# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_JK717
_database_code_depnum_ccdc_archive 'CCDC 1436226'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;

_vrf_PLAT331_I                   
;
PROBLEM:  Small Average Phenyl C-C Dist. C894 -C899 1.33 Ang.
RFESPONSE: In benzene of solvation.  Possible unrefined disorder.
;
_vrf_PLAT342_I                   
;
PROBLEM:  Low Bond Precision on C-C Bonds ............... 0.0207 Ang.
RFESPONSE: Typical for uranium compounds
;
_vrf_PLAT971_I                   
;
PROBLEM:  Check Calcd Residual Density 1.64A From C15 2.94 eA-3
RFESPONSE: Tried to place atom there with no success
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H58 O4 Si2 P2 S2 U1,3(C6 H6)'
_chemical_formula_sum            'C72 H76 O4 P2 S2 Si2 U'
_chemical_formula_weight         1425.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.9048(7)
_cell_length_b                   11.6124(4)
_cell_length_c                   25.6316(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.099(2)
_cell_angle_gamma                90
_cell_volume                     6790.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    35035
_cell_measurement_theta_min      5.393
_cell_measurement_theta_max      70.181
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             2888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    8.446
_shelx_estimated_absorpt_T_min   0.283
_shelx_estimated_absorpt_T_max   0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.017
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35035
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         5.393
_diffrn_reflns_theta_max         70.181
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_special_details          'crystal mosaicity 0.62'
_diffrn_measurement_details      
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             6290
_reflns_number_gt                5831
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'local programs'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0969P)²+20.1313P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6290
_refine_ls_number_parameters     378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1614
_refine_ls_wR_factor_gt          0.1515
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.61712(2) 0.7500 0.05501(14) Uani 1 2 d S T P . .
S1 S 0.50135(10) 0.78031(18) 0.67069(8) 0.0788(5) Uani 1 1 d . . . . .
P1 P 0.49434(9) 0.37185(14) 0.65028(7) 0.0597(4) Uani 1 1 d . . . . .
Si1 Si 0.34026(9) 0.63537(18) 0.71111(9) 0.0669(5) Uani 1 1 d . . . . .
O1 O 0.4080(2) 0.6079(5) 0.7338(2) 0.0710(14) Uani 1 1 d . . . . .
O2 O 0.5064(2) 0.4704(4) 0.68772(18) 0.0656(11) Uani 1 1 d . . . . .
C10 C 0.5742(4) 0.7948(7) 0.6545(3) 0.0738(19) Uani 1 1 d . . . . .
C11 C 0.6018(5) 0.9029(8) 0.6541(4) 0.087(3) Uani 1 1 d . . . . .
H11 H 0.5811 0.9691 0.6641 0.105 Uiso 1 1 calc R U . . .
C12 C 0.6568(6) 0.9151(11) 0.6399(5) 0.104(3) Uani 1 1 d . . . . .
H12 H 0.6736 0.9898 0.6390 0.125 Uiso 1 1 calc R U . . .
C13 C 0.6891(5) 0.8205(13) 0.6267(4) 0.108(3) Uani 1 1 d . . . . .
H13 H 0.7283 0.8290 0.6178 0.129 Uiso 1 1 calc R U . . .
C14 C 0.6631(5) 0.7141(10) 0.6268(4) 0.095(3) Uani 1 1 d . . . . .
H14 H 0.6846 0.6486 0.6171 0.114 Uiso 1 1 calc R U . . .
C15 C 0.6067(4) 0.6998(8) 0.6405(3) 0.079(2) Uani 1 1 d . . . . .
H15 H 0.5899 0.6250 0.6403 0.095 Uiso 1 1 calc R U . . .
C1A C 0.3299(5) 0.5979(9) 0.6406(4) 0.094(3) Uani 1 1 d . . . . .
H1A1 H 0.3545 0.6479 0.6209 0.141 Uiso 1 1 calc R U . . .
H1A2 H 0.2886 0.6086 0.6277 0.141 Uiso 1 1 calc R U . . .
H1A3 H 0.3410 0.5173 0.6358 0.141 Uiso 1 1 calc R U . . .
C1B C 0.2882(4) 0.5456(9) 0.7461(4) 0.090(2) Uani 1 1 d . . . . .
H1B1 H 0.2996 0.4644 0.7446 0.135 Uiso 1 1 calc R U . . .
H1B2 H 0.2484 0.5552 0.7293 0.135 Uiso 1 1 calc R U . . .
H1B3 H 0.2893 0.5701 0.7828 0.135 Uiso 1 1 calc R U . . .
C1C C 0.3254(5) 0.7907(8) 0.7204(4) 0.095(3) Uani 1 1 d . . . . .
H1C1 H 0.3296 0.8090 0.7579 0.142 Uiso 1 1 calc R U . . .
H1C2 H 0.2853 0.8086 0.7059 0.142 Uiso 1 1 calc R U . . .
H1C3 H 0.3533 0.8367 0.7024 0.142 Uiso 1 1 calc R U . . .
C20 C 0.4548(3) 0.4202(7) 0.5907(3) 0.0635(16) Uani 1 1 d . . . . .
C21 C 0.4208(4) 0.3444(8) 0.5580(3) 0.078(2) Uani 1 1 d . . . . .
H21 H 0.4154 0.2670 0.5686 0.094 Uiso 1 1 calc R U . . .
C22 C 0.3957(4) 0.3822(7) 0.5111(4) 0.073(2) Uani 1 1 d . . . . .
H22 H 0.3734 0.3304 0.4886 0.088 Uiso 1 1 calc R U . . .
C23 C 0.4023(4) 0.4937(10) 0.4959(4) 0.094(3) Uani 1 1 d . . . . .
H23 H 0.3842 0.5188 0.4631 0.113 Uiso 1 1 calc R U . . .
C24 C 0.4347(4) 0.5699(9) 0.5273(3) 0.084(2) Uani 1 1 d . . . . .
H24 H 0.4387 0.6475 0.5164 0.101 Uiso 1 1 calc R U . . .
C25 C 0.4614(4) 0.5336(8) 0.5750(3) 0.077(2) Uani 1 1 d . . . . .
H25 H 0.4841 0.5858 0.5969 0.093 Uiso 1 1 calc R U . . .
C30 C 0.5624(3) 0.3154(6) 0.6317(3) 0.0618(15) Uani 1 1 d . . . . .
C31 C 0.5649(4) 0.2322(7) 0.5934(3) 0.0757(19) Uani 1 1 d . . . . .
H31 H 0.5299 0.1983 0.5779 0.091 Uiso 1 1 calc R U . . .
C32 C 0.6191(4) 0.1981(8) 0.5776(3) 0.080(2) Uani 1 1 d . . . . .
H32 H 0.6211 0.1399 0.5517 0.096 Uiso 1 1 calc R U . . .
C33 C 0.6694(4) 0.2488(9) 0.5996(4) 0.092(3) Uani 1 1 d . . . . .
H33 H 0.7061 0.2248 0.5888 0.110 Uiso 1 1 calc R U . . .
C34 C 0.6682(4) 0.3333(10) 0.6368(4) 0.089(3) Uani 1 1 d . . . . .
H34 H 0.7035 0.3690 0.6508 0.107 Uiso 1 1 calc R U . . .
C35 C 0.6140(4) 0.3666(8) 0.6540(4) 0.078(2) Uani 1 1 d . . . . .
H35 H 0.6125 0.4235 0.6805 0.094 Uiso 1 1 calc R U . . .
C40 C 0.4521(3) 0.2610(6) 0.6783(3) 0.0654(16) Uani 1 1 d . . . . .
C41 C 0.4691(4) 0.1482(8) 0.6817(5) 0.089(3) Uani 1 1 d . . . . .
H41 H 0.5037 0.1237 0.6672 0.107 Uiso 1 1 calc R U . . .
C42 C 0.4348(5) 0.0694(9) 0.7067(5) 0.102(3) Uani 1 1 d . . . . .
H42 H 0.4469 -0.0088 0.7096 0.122 Uiso 1 1 calc R U . . .
C43 C 0.3848(5) 0.1022(7) 0.7270(4) 0.080(2) Uani 1 1 d . . . . .
H43 H 0.3614 0.0473 0.7431 0.096 Uiso 1 1 calc R U . . .
C44 C 0.3684(4) 0.2156(7) 0.7240(4) 0.089(3) Uani 1 1 d . . . . .
H44 H 0.3339 0.2401 0.7389 0.106 Uiso 1 1 calc R U . . .
C45 C 0.4016(4) 0.2941(8) 0.6997(4) 0.085(2) Uani 1 1 d . . . . .
H45 H 0.3897 0.3724 0.6976 0.102 Uiso 1 1 calc R U . . .
C894 C 0.2866(14) 1.1133(19) 0.5523(18) 0.193(12) Uani 1 1 d . . . . .
H894 H 0.2815 1.1943 0.5542 0.232 Uiso 1 1 calc R U . . .
C895 C 0.2640(8) 1.051(3) 0.5087(9) 0.179(9) Uani 1 1 d . . . . .
H895 H 0.2440 1.0895 0.4795 0.215 Uiso 1 1 calc R U . . .
C896 C 0.2709(8) 0.935(3) 0.5088(8) 0.151(7) Uani 1 1 d . . . . .
H896 H 0.2521 0.8904 0.4811 0.181 Uiso 1 1 calc R U . . .
C897 C 0.3022(11) 0.8851(16) 0.5452(15) 0.175(10) Uani 1 1 d . . . . .
H897 H 0.3102 0.8051 0.5428 0.210 Uiso 1 1 calc R U . . .
C898 C 0.3247(11) 0.947(4) 0.5883(10) 0.194(11) Uani 1 1 d . . . . .
H898 H 0.3471 0.9096 0.6163 0.232 Uiso 1 1 calc R U . . .
C899 C 0.3146(12) 1.058(4) 0.5900(11) 0.181(11) Uani 1 1 d . . . . .
H899 H 0.3287 1.0991 0.6206 0.217 Uiso 1 1 calc R U . . .
C997 C 0.4777(6) 0.9445(11) 0.5407(4) 0.110(3) Uani 1 1 d . . . . .
H997 H 0.4622 0.9061 0.5691 0.132 Uiso 1 1 calc R U . . .
C998 C 0.4452(5) 1.0330(10) 0.5140(4) 0.105(3) Uani 1 1 d . . . . .
H998 H 0.4078 1.0548 0.5240 0.126 Uiso 1 1 calc R U . . .
C999 C 0.5312(7) 0.9139(11) 0.5262(5) 0.108(4) Uani 1 1 d . . . . .
H999 H 0.5525 0.8540 0.5446 0.129 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.113(5) 2_656 ?
U1 O1 2.113(5) . ?
U1 O2 2.348(5) 2_656 ?
U1 O2 2.348(5) . ?
U1 S1 2.7812(19) . ?
U1 S1 2.7813(19) 2_656 ?
S1 C10 1.763(9) . ?
P1 O2 1.503(5) . ?
P1 C30 1.793(7) . ?
P1 C20 1.795(7) . ?
P1 C40 1.798(8) . ?
Si1 O1 1.640(6) . ?
Si1 C1A 1.855(10) . ?
Si1 C1C 1.855(9) . ?
Si1 C1B 1.872(9) . ?
C10 C15 1.396(12) . ?
C10 C11 1.406(13) . ?
C11 C12 1.350(17) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.372(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(13) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C1A H1A1 0.9800 . ?
C1A H1A2 0.9800 . ?
C1A H1A3 0.9800 . ?
C1B H1B1 0.9800 . ?
C1B H1B2 0.9800 . ?
C1B H1B3 0.9800 . ?
C1C H1C1 0.9800 . ?
C1C H1C2 0.9800 . ?
C1C H1C3 0.9800 . ?
C20 C25 1.388(12) . ?
C20 C21 1.402(11) . ?
C21 C22 1.359(12) . ?
C21 H21 0.9500 . ?
C22 C23 1.364(13) . ?
C22 H22 0.9500 . ?
C23 C24 1.369(14) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(11) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C31 1.382(10) . ?
C30 C35 1.400(12) . ?
C31 C32 1.396(11) . ?
C31 H31 0.9500 . ?
C32 C33 1.370(13) . ?
C32 H32 0.9500 . ?
C33 C34 1.370(14) . ?
C33 H33 0.9500 . ?
C34 C35 1.408(14) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C41 1.367(11) . ?
C40 C45 1.377(11) . ?
C41 C42 1.398(14) . ?
C41 H41 0.9500 . ?
C42 C43 1.355(15) . ?
C42 H42 0.9500 . ?
C43 C44 1.370(11) . ?
C43 H43 0.9500 . ?
C44 C45 1.371(12) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C894 C899 1.29(4) . ?
C894 C895 1.39(4) . ?
C894 H894 0.9500 . ?
C895 C896 1.36(3) . ?
C895 H895 0.9500 . ?
C896 C897 1.26(3) . ?
C896 H896 0.9500 . ?
C897 C898 1.38(4) . ?
C897 H897 0.9500 . ?
C898 C899 1.31(3) . ?
C898 H898 0.9500 . ?
C899 H899 0.9500 . ?
C997 C999 1.359(19) . ?
C997 C998 1.411(17) . ?
C997 H997 0.9500 . ?
C998 C999 1.354(17) 5_676 ?
C998 H998 0.9500 . ?
C999 C998 1.354(17) 5_676 ?
C999 H999 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 174.2(3) 2_656 . ?
O1 U1 O2 87.2(2) 2_656 2_656 ?
O1 U1 O2 88.6(2) . 2_656 ?
O1 U1 O2 88.6(2) 2_656 . ?
O1 U1 O2 87.2(2) . . ?
O2 U1 O2 86.9(3) 2_656 . ?
O1 U1 S1 95.88(17) 2_656 . ?
O1 U1 S1 88.08(17) . . ?
O2 U1 S1 175.30(12) 2_656 . ?
O2 U1 S1 89.56(14) . . ?
O1 U1 S1 88.08(17) 2_656 2_656 ?
O1 U1 S1 95.88(17) . 2_656 ?
O2 U1 S1 89.56(14) 2_656 2_656 ?
O2 U1 S1 175.30(12) . 2_656 ?
S1 U1 S1 94.10(9) . 2_656 ?
C10 S1 U1 108.0(3) . . ?
O2 P1 C30 109.5(3) . . ?
O2 P1 C20 110.8(3) . . ?
C30 P1 C20 105.8(3) . . ?
O2 P1 C40 111.4(3) . . ?
C30 P1 C40 110.8(3) . . ?
C20 P1 C40 108.4(4) . . ?
O1 Si1 C1A 109.6(4) . . ?
O1 Si1 C1C 108.8(4) . . ?
C1A Si1 C1C 110.2(5) . . ?
O1 Si1 C1B 110.2(4) . . ?
C1A Si1 C1B 107.7(5) . . ?
C1C Si1 C1B 110.3(5) . . ?
Si1 O1 U1 162.8(4) . . ?
P1 O2 U1 165.4(3) . . ?
C15 C10 C11 117.0(9) . . ?
C15 C10 S1 121.6(7) . . ?
C11 C10 S1 121.4(7) . . ?
C12 C11 C10 121.7(11) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C13 121.0(11) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 118.3(11) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C13 C14 C15 121.7(10) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C14 C15 C10 120.3(9) . . ?
C14 C15 H15 119.9 . . ?
C10 C15 H15 119.9 . . ?
Si1 C1A H1A1 109.5 . . ?
Si1 C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 109.5 . . ?
Si1 C1A H1A3 109.5 . . ?
H1A1 C1A H1A3 109.5 . . ?
H1A2 C1A H1A3 109.5 . . ?
Si1 C1B H1B1 109.5 . . ?
Si1 C1B H1B2 109.5 . . ?
H1B1 C1B H1B2 109.5 . . ?
Si1 C1B H1B3 109.5 . . ?
H1B1 C1B H1B3 109.5 . . ?
H1B2 C1B H1B3 109.5 . . ?
Si1 C1C H1C1 109.5 . . ?
Si1 C1C H1C2 109.5 . . ?
H1C1 C1C H1C2 109.5 . . ?
Si1 C1C H1C3 109.5 . . ?
H1C1 C1C H1C3 109.5 . . ?
H1C2 C1C H1C3 109.5 . . ?
C25 C20 C21 119.4(7) . . ?
C25 C20 P1 118.9(6) . . ?
C21 C20 P1 121.6(7) . . ?
C22 C21 C20 119.6(8) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C23 120.7(8) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C24 120.9(8) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C23 C24 C25 119.7(10) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C20 119.6(9) . . ?
C24 C25 H25 120.2 . . ?
C20 C25 H25 120.2 . . ?
C31 C30 C35 120.0(7) . . ?
C31 C30 P1 122.4(6) . . ?
C35 C30 P1 117.3(6) . . ?
C30 C31 C32 120.0(8) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C33 C32 C31 119.6(8) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 121.8(8) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C35 119.2(9) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C30 C35 C34 119.5(9) . . ?
C30 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C41 C40 C45 119.1(8) . . ?
C41 C40 P1 123.4(7) . . ?
C45 C40 P1 117.4(6) . . ?
C40 C41 C42 119.2(9) . . ?
C40 C41 H41 120.4 . . ?
C42 C41 H41 120.4 . . ?
C43 C42 C41 121.4(9) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C42 C43 C44 119.0(9) . . ?
C42 C43 H43 120.5 . . ?
C44 C43 H43 120.5 . . ?
C43 C44 C45 120.3(9) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C40 121.0(8) . . ?
C44 C45 H45 119.5 . . ?
C40 C45 H45 119.5 . . ?
C899 C894 C895 118(2) . . ?
C899 C894 H894 120.9 . . ?
C895 C894 H894 120.9 . . ?
C896 C895 C894 119(2) . . ?
C896 C895 H895 120.7 . . ?
C894 C895 H895 120.7 . . ?
C897 C896 C895 121(2) . . ?
C897 C896 H896 119.5 . . ?
C895 C896 H896 119.5 . . ?
C896 C897 C898 120(2) . . ?
C896 C897 H897 120.0 . . ?
C898 C897 H897 120.0 . . ?
C899 C898 C897 119(2) . . ?
C899 C898 H898 120.5 . . ?
C897 C898 H898 120.5 . . ?
C894 C899 C898 123(3) . . ?
C894 C899 H899 118.5 . . ?
C898 C899 H899 118.5 . . ?
C999 C997 C998 120.5(11) . . ?
C999 C997 H997 119.7 . . ?
C998 C997 H997 119.7 . . ?
C999 C998 C997 118.1(12) 5_676 . ?
C999 C998 H998 120.9 5_676 . ?
C997 C998 H998 120.9 . . ?
C998 C999 C997 121.4(11) 5_676 . ?
C998 C999 H999 119.3 5_676 . ?
C997 C999 H999 119.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1A Si1 O1 U1 73.8(13) . . . . ?
C1C Si1 O1 U1 -46.8(14) . . . . ?
C1B Si1 O1 U1 -167.9(12) . . . . ?
C30 P1 O2 U1 -165.7(12) . . . . ?
C20 P1 O2 U1 77.9(13) . . . . ?
C40 P1 O2 U1 -42.8(13) . . . . ?
U1 S1 C10 C15 54.5(7) . . . . ?
U1 S1 C10 C11 -126.8(7) . . . . ?
C15 C10 C11 C12 1.2(14) . . . . ?
S1 C10 C11 C12 -177.6(8) . . . . ?
C10 C11 C12 C13 -2.1(17) . . . . ?
C11 C12 C13 C14 2.0(17) . . . . ?
C12 C13 C14 C15 -1.2(16) . . . . ?
C13 C14 C15 C10 0.3(15) . . . . ?
C11 C10 C15 C14 -0.3(12) . . . . ?
S1 C10 C15 C14 178.4(7) . . . . ?
O2 P1 C20 C25 27.3(7) . . . . ?
C30 P1 C20 C25 -91.3(7) . . . . ?
C40 P1 C20 C25 149.8(6) . . . . ?
O2 P1 C20 C21 -157.1(6) . . . . ?
C30 P1 C20 C21 84.3(7) . . . . ?
C40 P1 C20 C21 -34.6(8) . . . . ?
C25 C20 C21 C22 1.2(13) . . . . ?
P1 C20 C21 C22 -174.4(7) . . . . ?
C20 C21 C22 C23 -1.2(14) . . . . ?
C21 C22 C23 C24 0.4(15) . . . . ?
C22 C23 C24 C25 0.4(15) . . . . ?
C23 C24 C25 C20 -0.5(13) . . . . ?
C21 C20 C25 C24 -0.3(12) . . . . ?
P1 C20 C25 C24 175.3(7) . . . . ?
O2 P1 C30 C31 -173.0(6) . . . . ?
C20 P1 C30 C31 -53.5(7) . . . . ?
C40 P1 C30 C31 63.8(7) . . . . ?
O2 P1 C30 C35 1.0(7) . . . . ?
C20 P1 C30 C35 120.4(7) . . . . ?
C40 P1 C30 C35 -122.3(7) . . . . ?
C35 C30 C31 C32 1.1(12) . . . . ?
P1 C30 C31 C32 174.9(7) . . . . ?
C30 C31 C32 C33 -1.1(13) . . . . ?
C31 C32 C33 C34 -0.3(15) . . . . ?
C32 C33 C34 C35 1.8(16) . . . . ?
C31 C30 C35 C34 0.4(13) . . . . ?
P1 C30 C35 C34 -173.7(7) . . . . ?
C33 C34 C35 C30 -1.9(15) . . . . ?
O2 P1 C40 C41 -125.7(8) . . . . ?
C30 P1 C40 C41 -3.5(9) . . . . ?
C20 P1 C40 C41 112.2(8) . . . . ?
O2 P1 C40 C45 50.9(7) . . . . ?
C30 P1 C40 C45 173.0(6) . . . . ?
C20 P1 C40 C45 -71.3(7) . . . . ?
C45 C40 C41 C42 0.1(15) . . . . ?
P1 C40 C41 C42 176.6(8) . . . . ?
C40 C41 C42 C43 0.9(18) . . . . ?
C41 C42 C43 C44 -1.7(18) . . . . ?
C42 C43 C44 C45 1.5(16) . . . . ?
C43 C44 C45 C40 -0.5(16) . . . . ?
C41 C40 C45 C44 -0.2(14) . . . . ?
P1 C40 C45 C44 -176.9(8) . . . . ?
C899 C894 C895 C896 2(4) . . . . ?
C894 C895 C896 C897 -7(3) . . . . ?
C895 C896 C897 C898 7(3) . . . . ?
C896 C897 C898 C899 -2(4) . . . . ?
C895 C894 C899 C898 3(4) . . . . ?
C897 C898 C899 C894 -3(4) . . . . ?
C999 C997 C998 C999 0(2) . . . 5_676 ?
C998 C997 C999 C998 0(2) . . . 5_676 ?

_refine_diff_density_max         3.046
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.142


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Benzene'
_chemical_properties_physical    'Air-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JK725
_database_code_depnum_ccdc_archive 'CCDC 1436227'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;

_vrf_PLAT411_I                   
;
PROBLEM:  Short Inter H...H Contact H43 .. H99H .. 1.76 Ang.
          Short Inter H...H Contact H32 .. H89G .. 1.80 Ang.
RFESPONSE: Very disordered THF, Unable to properly model, but did not want to squeeze
;
_vrf_PLAT733_I                   
;
PROBLEM:  Torsion Calc -179.5(16), Rep -180(**) ...... 9.90 su-Rat
RFESPONSE: Also associated with disorder THF. We opted not to squeeze
;
_vrf_PLAT971_I                   
;
PROBLEM:  Check Calcd Residual Density 0.93A From U1 2.62 eA-3
RFESPONSE: Common issue for uranium
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C12 H10 Cl2 P2 U1,2(C18 H15 O1 Si1),2(H2 O1),4(C4 H8 O1),4(C6 H5)'
_chemical_formula_sum            'C88 H92 Cl2 O8 P2 Si2 U'
_chemical_formula_weight         1704.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   29.2654(7)
_cell_length_b                   18.0309(4)
_cell_length_c                   15.5926(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.090(2)
_cell_angle_gamma                90
_cell_volume                     8226.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    46906
_cell_measurement_theta_min      2.879
_cell_measurement_theta_max      72.299
_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_F_000             3472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    7.225
_shelx_estimated_absorpt_T_min   0.239
_shelx_estimated_absorpt_T_max   1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.013
_exptl_absorpt_correction_T_max  0.236
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46906
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.879
_diffrn_reflns_theta_max         72.299
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_special_details          'crystal mosaicity 0.40'
_diffrn_measurement_details      
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             7812
_reflns_number_gt                7255
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'local programs'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1003P)²+37.3361P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7812
_refine_ls_number_parameters     450
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1694
_refine_ls_wR_factor_gt          0.1657
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.74624(2) 0.2500 0.03704(13) Uani 1 2 d S T P . .
Cl1 Cl 0.5000 0.89472(12) 0.2500 0.0593(6) Uani 1 2 d S T P . .
Cl2 Cl 0.5000 0.59824(13) 0.2500 0.0656(7) Uani 1 2 d S T P . .
P1 P 0.54897(5) 0.76763(9) 0.47548(10) 0.0425(3) Uani 1 1 d . . . . .
Si1 Si 0.61901(6) 0.73473(12) 0.16792(14) 0.0524(4) Uani 1 1 d . . . . .
O1 O 0.56672(17) 0.7473(2) 0.2007(4) 0.0466(12) Uani 1 1 d . . . . .
O2 O 0.5279(2) 0.74875(19) 0.3878(4) 0.0491(12) Uani 1 1 d . . . . .
C10 C 0.6178(2) 0.6753(4) 0.0690(4) 0.0598(17) Uani 1 1 d . . . . .
C11 C 0.5772(2) 0.6668(4) 0.0213(4) 0.0598(16) Uani 1 1 d . . . . .
H11 H 0.5500 0.6886 0.0417 0.072 Uiso 1 1 calc R U . . .
C12 C 0.5759(3) 0.6274(5) -0.0547(5) 0.073(2) Uani 1 1 d . . . . .
H12 H 0.5480 0.6231 -0.0863 0.088 Uiso 1 1 calc R U . . .
C13 C 0.6148(3) 0.5944(6) -0.0850(5) 0.086(3) Uani 1 1 d . . . . .
H13 H 0.6140 0.5684 -0.1379 0.103 Uiso 1 1 calc R U . . .
C14 C 0.6542(3) 0.5994(7) -0.0388(6) 0.101(3) Uani 1 1 d . . . . .
H14 H 0.6811 0.5760 -0.0589 0.121 Uiso 1 1 calc R U . . .
C15 C 0.6555(3) 0.6387(6) 0.0383(6) 0.090(3) Uani 1 1 d . . . . .
H15 H 0.6833 0.6402 0.0708 0.108 Uiso 1 1 calc R U . . .
C20 C 0.6450(3) 0.8261(6) 0.1400(5) 0.074(2) Uani 1 1 d . . . . .
C21 C 0.6847(4) 0.8319(8) 0.0908(6) 0.117(5) Uani 1 1 d . . . . .
H21 H 0.7001 0.7885 0.0721 0.141 Uiso 1 1 calc R U . . .
C22 C 0.7011(6) 0.9017(12) 0.0700(10) 0.153(8) Uani 1 1 d . . . . .
H22 H 0.7285 0.9045 0.0385 0.183 Uiso 1 1 calc R U . . .
C23 C 0.6810(6) 0.9650(11) 0.0913(11) 0.152(9) Uani 1 1 d . . . . .
H23 H 0.6928 1.0114 0.0730 0.183 Uiso 1 1 calc R U . . .
C24 C 0.6415(4) 0.9612(7) 0.1420(10) 0.139(6) Uani 1 1 d . . . . .
H24 H 0.6272 1.0054 0.1608 0.167 Uiso 1 1 calc R U . . .
C25 C 0.6236(3) 0.8920(6) 0.1645(7) 0.094(3) Uani 1 1 d . . . . .
H25 H 0.5964 0.8898 0.1968 0.113 Uiso 1 1 calc R U . . .
C30 C 0.6538(2) 0.6868(4) 0.2533(4) 0.0583(16) Uani 1 1 d . . . . .
C31 C 0.7003(3) 0.6974(6) 0.2660(6) 0.081(2) Uani 1 1 d . . . . .
H31 H 0.7158 0.7320 0.2312 0.097 Uiso 1 1 calc R U . . .
C32 C 0.7246(4) 0.6585(8) 0.3287(8) 0.108(4) Uani 1 1 d . . . . .
H32 H 0.7567 0.6655 0.3347 0.130 Uiso 1 1 calc R U . . .
C33 C 0.7028(4) 0.6101(7) 0.3820(6) 0.098(3) Uani 1 1 d . . . . .
H33 H 0.7195 0.5842 0.4254 0.117 Uiso 1 1 calc R U . . .
C34 C 0.6574(4) 0.5998(7) 0.3723(6) 0.090(3) Uani 1 1 d . . . . .
H34 H 0.6419 0.5673 0.4100 0.108 Uiso 1 1 calc R U . . .
C35 C 0.6328(3) 0.6368(5) 0.3067(6) 0.079(2) Uani 1 1 d . . . . .
H35 H 0.6011 0.6271 0.2990 0.095 Uiso 1 1 calc R U . . .
C40 C 0.6068(2) 0.7974(4) 0.4660(4) 0.0516(14) Uani 1 1 d . . . . .
C41 C 0.6153(3) 0.8533(5) 0.4084(6) 0.081(2) Uani 1 1 d . . . . .
H41 H 0.5909 0.8744 0.3757 0.097 Uiso 1 1 calc R U . . .
C42 C 0.6602(4) 0.8794(7) 0.3981(8) 0.099(4) Uani 1 1 d . . . . .
H42 H 0.6666 0.9175 0.3580 0.119 Uiso 1 1 calc R U . . .
C43 C 0.6950(3) 0.8481(6) 0.4477(6) 0.085(3) Uani 1 1 d . . . . .
H43 H 0.7253 0.8666 0.4429 0.102 Uiso 1 1 calc R U . . .
C44 C 0.6867(3) 0.7921(6) 0.5025(6) 0.082(2) Uani 1 1 d . . . . .
H44 H 0.7111 0.7706 0.5350 0.098 Uiso 1 1 calc R U . . .
C45 C 0.6423(3) 0.7659(5) 0.5111(6) 0.0636(19) Uani 1 1 d . . . . .
H45 H 0.6366 0.7257 0.5488 0.076 Uiso 1 1 calc R U . . .
C50 C 0.5188(2) 0.8431(4) 0.5244(4) 0.0503(14) Uani 1 1 d . . . . .
C51 C 0.4751(2) 0.8622(4) 0.4928(5) 0.0625(17) Uani 1 1 d . . . . .
H51 H 0.4615 0.8351 0.4468 0.075 Uiso 1 1 calc R U . . .
C52 C 0.4525(3) 0.9205(5) 0.5291(6) 0.080(2) Uani 1 1 d . . . . .
H52 H 0.4230 0.9341 0.5077 0.096 Uiso 1 1 calc R U . . .
C53 C 0.4721(3) 0.9596(5) 0.5967(6) 0.089(3) Uani 1 1 d . . . . .
H53 H 0.4558 0.9993 0.6222 0.106 Uiso 1 1 calc R U . . .
C54 C 0.5153(3) 0.9413(5) 0.6272(6) 0.081(2) Uani 1 1 d . . . . .
H54 H 0.5288 0.9689 0.6729 0.097 Uiso 1 1 calc R U . . .
C55 C 0.5388(3) 0.8827(4) 0.5913(5) 0.0626(17) Uani 1 1 d . . . . .
H55 H 0.5684 0.8698 0.6124 0.075 Uiso 1 1 calc R U . . .
C60 C 0.5479(2) 0.6879(4) 0.5441(4) 0.0480(13) Uani 1 1 d . . . . .
C61 C 0.5482(2) 0.6178(4) 0.5051(5) 0.0605(16) Uani 1 1 d . . . . .
H61 H 0.5483 0.6133 0.4444 0.073 Uiso 1 1 calc R U . . .
C62 C 0.5483(3) 0.5544(5) 0.5577(7) 0.085(3) Uani 1 1 d . . . . .
H62 H 0.5473 0.5065 0.5324 0.101 Uiso 1 1 calc R U . . .
C63 C 0.5498(3) 0.5613(6) 0.6450(6) 0.084(3) Uani 1 1 d . . . . .
H63 H 0.5515 0.5185 0.6803 0.101 Uiso 1 1 calc R U . . .
C64 C 0.5490(3) 0.6300(7) 0.6808(6) 0.092(3) Uani 1 1 d . . . . .
H64 H 0.5486 0.6341 0.7415 0.110 Uiso 1 1 calc R U . . .
C65 C 0.5486(3) 0.6937(5) 0.6327(5) 0.070(2) Uani 1 1 d . . . . .
H65 H 0.5487 0.7409 0.6596 0.084 Uiso 1 1 calc R U . . .
O8 O 0.3757(6) 0.1741(10) 0.2616(8) 0.221(7) Uani 1 1 d G . . . .
C891 C 0.3941(6) 0.2010(17) 0.1915(10) 0.32(2) Uani 1 1 d G . . . .
H89A H 0.4242 0.1776 0.1817 0.385 Uiso 1 1 calc R U . . .
H89B H 0.3985 0.2552 0.1967 0.385 Uiso 1 1 calc R U . . .
C892 C 0.3636(7) 0.1846(18) 0.1237(9) 0.297(18) Uani 1 1 d G . . . .
H89C H 0.3694 0.1349 0.0993 0.356 Uiso 1 1 calc R U . . .
H89D H 0.3652 0.2222 0.0775 0.356 Uiso 1 1 calc R U . . .
C893 C 0.3213(5) 0.187(2) 0.1652(13) 0.291(19) Uani 1 1 d G . . . .
H89E H 0.3103 0.2388 0.1712 0.349 Uiso 1 1 calc R U . . .
H89F H 0.2978 0.1575 0.1343 0.349 Uiso 1 1 calc R U . . .
C894 C 0.3328(7) 0.1559(19) 0.2452(12) 0.58(6) Uani 1 1 d G U . . .
H89G H 0.3127 0.1758 0.2902 0.701 Uiso 1 1 calc R U . . .
H89H H 0.3293 0.1013 0.2432 0.701 Uiso 1 1 calc R U . . .
O9 O 0.6812(4) 0.4301(11) 0.1137(9) 0.373(19) Uani 1 1 d G . . . .
C991 C 0.6829(6) 0.4115(13) 0.1978(11) 0.45(4) Uani 1 1 d G . . . .
H99A H 0.6780 0.3575 0.2049 0.539 Uiso 1 1 calc R U . . .
H99B H 0.6590 0.4383 0.2296 0.539 Uiso 1 1 calc R U . . .
C992 C 0.7277(6) 0.4322(13) 0.2293(7) 0.215(13) Uani 1 1 d G . . . .
H99C H 0.7501 0.3919 0.2205 0.258 Uiso 1 1 calc R U . . .
H99D H 0.7273 0.4454 0.2908 0.258 Uiso 1 1 calc R U . . .
C993 C 0.7373(4) 0.4958(9) 0.1765(11) 0.225(12) Uani 1 1 d G . . . .
H99E H 0.7227 0.5412 0.1988 0.271 Uiso 1 1 calc R U . . .
H99F H 0.7706 0.5043 0.1721 0.271 Uiso 1 1 calc R U . . .
C994 C 0.7173(4) 0.4737(7) 0.0954(8) 0.121(4) Uani 1 1 d G . . . .
H99G H 0.7072 0.5177 0.0622 0.145 Uiso 1 1 calc R U . . .
H99H H 0.7398 0.4459 0.0613 0.145 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.112(5) 2_655 ?
U1 O1 2.112(5) . ?
U1 O2 2.285(6) 2_655 ?
U1 O2 2.285(6) . ?
U1 Cl2 2.669(2) . ?
U1 Cl1 2.677(2) . ?
P1 O2 1.527(6) . ?
P1 C40 1.785(6) . ?
P1 C60 1.793(6) . ?
P1 C50 1.799(7) . ?
Si1 O1 1.638(5) . ?
Si1 C20 1.870(9) . ?
Si1 C30 1.872(7) . ?
Si1 C10 1.878(8) . ?
C10 C15 1.379(10) . ?
C10 C11 1.397(10) . ?
C11 C12 1.382(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.350(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.396(13) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C20 C25 1.400(14) . ?
C20 C21 1.408(12) . ?
C21 C22 1.39(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.33(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.42(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.400(13) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C35 1.379(11) . ?
C30 C31 1.384(10) . ?
C31 C32 1.389(14) . ?
C31 H31 0.9500 . ?
C32 C33 1.371(16) . ?
C32 H32 0.9500 . ?
C33 C34 1.348(15) . ?
C33 H33 0.9500 . ?
C34 C35 1.408(12) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C45 1.366(10) . ?
C40 C41 1.376(10) . ?
C41 C42 1.408(12) . ?
C41 H41 0.9500 . ?
C42 C43 1.385(14) . ?
C42 H42 0.9500 . ?
C43 C44 1.348(13) . ?
C43 H43 0.9500 . ?
C44 C45 1.393(12) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C50 C55 1.385(9) . ?
C50 C51 1.403(9) . ?
C51 C52 1.370(10) . ?
C51 H51 0.9500 . ?
C52 C53 1.384(12) . ?
C52 H52 0.9500 . ?
C53 C54 1.381(12) . ?
C53 H53 0.9500 . ?
C54 C55 1.385(11) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C60 C65 1.385(10) . ?
C60 C61 1.402(10) . ?
C61 C62 1.407(11) . ?
C61 H61 0.9500 . ?
C62 C63 1.366(14) . ?
C62 H62 0.9500 . ?
C63 C64 1.359(14) . ?
C63 H63 0.9500 . ?
C64 C65 1.371(12) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
O8 C894 1.320(9) . ?
O8 C891 1.320(9) . ?
C891 C892 1.404(9) . ?
C891 H89A 0.9900 . ?
C891 H89B 0.9900 . ?
C892 C893 1.407(9) . ?
C892 H89C 0.9900 . ?
C892 H89D 0.9900 . ?
C893 C894 1.404(9) . ?
C893 H89E 0.9900 . ?
C893 H89F 0.9900 . ?
C894 H89G 0.9900 . ?
C894 H89H 0.9900 . ?
O9 C994 1.354(7) . ?
O9 C991 1.354(7) . ?
C991 C992 1.440(7) . ?
C991 H99A 0.9900 . ?
C991 H99B 0.9900 . ?
C992 C993 1.443(7) . ?
C992 H99C 0.9900 . ?
C992 H99D 0.9900 . ?
C993 C994 1.440(7) . ?
C993 H99E 0.9900 . ?
C993 H99F 0.9900 . ?
C994 H99G 0.9900 . ?
C994 H99H 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 178.9(2) 2_655 . ?
O1 U1 O2 91.5(2) 2_655 2_655 ?
O1 U1 O2 88.5(2) . 2_655 ?
O1 U1 O2 88.5(2) 2_655 . ?
O1 U1 O2 91.5(2) . . ?
O2 U1 O2 177.73(17) 2_655 . ?
O1 U1 Cl2 90.53(10) 2_655 . ?
O1 U1 Cl2 90.54(10) . . ?
O2 U1 Cl2 91.14(9) 2_655 . ?
O2 U1 Cl2 91.13(9) . . ?
O1 U1 Cl1 89.47(10) 2_655 . ?
O1 U1 Cl1 89.46(10) . . ?
O2 U1 Cl1 88.86(9) 2_655 . ?
O2 U1 Cl1 88.87(9) . . ?
Cl2 U1 Cl1 180.0 . . ?
O2 P1 C40 111.1(3) . . ?
O2 P1 C60 110.1(3) . . ?
C40 P1 C60 108.5(3) . . ?
O2 P1 C50 110.8(3) . . ?
C40 P1 C50 106.4(3) . . ?
C60 P1 C50 109.9(3) . . ?
O1 Si1 C20 109.7(3) . . ?
O1 Si1 C30 109.9(3) . . ?
C20 Si1 C30 110.8(3) . . ?
O1 Si1 C10 109.4(3) . . ?
C20 Si1 C10 108.2(4) . . ?
C30 Si1 C10 108.8(3) . . ?
Si1 O1 U1 171.0(3) . . ?
P1 O2 U1 167.8(2) . . ?
C15 C10 C11 116.1(7) . . ?
C15 C10 Si1 123.8(6) . . ?
C11 C10 Si1 120.1(5) . . ?
C12 C11 C10 121.5(7) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C12 C11 120.4(8) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 119.5(8) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 120.1(8) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 C14 122.3(8) . . ?
C10 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C25 C20 C21 117.7(10) . . ?
C25 C20 Si1 119.8(6) . . ?
C21 C20 Si1 122.4(9) . . ?
C22 C21 C20 119.1(15) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C23 C22 C21 124.4(15) . . ?
C23 C22 H22 117.8 . . ?
C21 C22 H22 117.8 . . ?
C22 C23 C24 117.8(13) . . ?
C22 C23 H23 121.1 . . ?
C24 C23 H23 121.1 . . ?
C25 C24 C23 119.9(15) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C20 C25 C24 121.0(11) . . ?
C20 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C35 C30 C31 116.8(7) . . ?
C35 C30 Si1 119.3(6) . . ?
C31 C30 Si1 123.9(6) . . ?
C30 C31 C32 121.4(10) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 H31 119.3 . . ?
C33 C32 C31 120.6(10) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 119.3(9) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C35 120.3(11) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C30 C35 C34 121.5(9) . . ?
C30 C35 H35 119.3 . . ?
C34 C35 H35 119.3 . . ?
C45 C40 C41 119.7(7) . . ?
C45 C40 P1 123.0(6) . . ?
C41 C40 P1 117.2(5) . . ?
C40 C41 C42 120.0(8) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 118.5(9) . . ?
C43 C42 H42 120.7 . . ?
C41 C42 H42 120.7 . . ?
C44 C43 C42 121.3(8) . . ?
C44 C43 H43 119.4 . . ?
C42 C43 H43 119.4 . . ?
C43 C44 C45 119.7(8) . . ?
C43 C44 H44 120.2 . . ?
C45 C44 H44 120.2 . . ?
C40 C45 C44 120.7(8) . . ?
C40 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C55 C50 C51 120.4(6) . . ?
C55 C50 P1 120.3(5) . . ?
C51 C50 P1 119.2(5) . . ?
C52 C51 C50 119.2(7) . . ?
C52 C51 H51 120.4 . . ?
C50 C51 H51 120.4 . . ?
C51 C52 C53 120.6(8) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 H52 119.7 . . ?
C54 C53 C52 120.2(7) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
C53 C54 C55 120.2(8) . . ?
C53 C54 H54 119.9 . . ?
C55 C54 H54 119.9 . . ?
C50 C55 C54 119.4(7) . . ?
C50 C55 H55 120.3 . . ?
C54 C55 H55 120.3 . . ?
C65 C60 C61 120.0(6) . . ?
C65 C60 P1 122.3(6) . . ?
C61 C60 P1 117.6(5) . . ?
C60 C61 C62 118.7(8) . . ?
C60 C61 H61 120.7 . . ?
C62 C61 H61 120.7 . . ?
C63 C62 C61 120.4(9) . . ?
C63 C62 H62 119.8 . . ?
C61 C62 H62 119.8 . . ?
C64 C63 C62 119.5(8) . . ?
C64 C63 H63 120.3 . . ?
C62 C63 H63 120.3 . . ?
C63 C64 C65 122.5(9) . . ?
C63 C64 H64 118.7 . . ?
C65 C64 H64 118.7 . . ?
C64 C65 C60 118.9(9) . . ?
C64 C65 H65 120.6 . . ?
C60 C65 H65 120.6 . . ?
C894 O8 C891 109.5 . . ?
O8 C891 C892 106.4 . . ?
O8 C891 H89A 110.4 . . ?
C892 C891 H89A 110.4 . . ?
O8 C891 H89B 110.4 . . ?
C892 C891 H89B 110.4 . . ?
H89A C891 H89B 108.6 . . ?
C891 C892 C893 101.5 . . ?
C891 C892 H89C 111.5 . . ?
C893 C892 H89C 111.5 . . ?
C891 C892 H89D 111.5 . . ?
C893 C892 H89D 111.5 . . ?
H89C C892 H89D 109.3 . . ?
C894 C893 C892 101.5 . . ?
C894 C893 H89E 111.5 . . ?
C892 C893 H89E 111.5 . . ?
C894 C893 H89F 111.5 . . ?
C892 C893 H89F 111.5 . . ?
H89E C893 H89F 109.3 . . ?
O8 C894 C893 106.4 . . ?
O8 C894 H89G 110.4 . . ?
C893 C894 H89G 110.4 . . ?
O8 C894 H89H 110.4 . . ?
C893 C894 H89H 110.4 . . ?
H89G C894 H89H 108.6 . . ?
C994 O9 C991 109.5 . . ?
O9 C991 C992 106.4 . . ?
O9 C991 H99A 110.4 . . ?
C992 C991 H99A 110.4 . . ?
O9 C991 H99B 110.4 . . ?
C992 C991 H99B 110.4 . . ?
H99A C991 H99B 108.6 . . ?
C991 C992 C993 101.5 . . ?
C991 C992 H99C 111.5 . . ?
C993 C992 H99C 111.5 . . ?
C991 C992 H99D 111.5 . . ?
C993 C992 H99D 111.5 . . ?
H99C C992 H99D 109.3 . . ?
C994 C993 C992 101.5 . . ?
C994 C993 H99E 111.5 . . ?
C992 C993 H99E 111.5 . . ?
C994 C993 H99F 111.5 . . ?
C992 C993 H99F 111.5 . . ?
H99E C993 H99F 109.3 . . ?
O9 C994 C993 106.4 . . ?
O9 C994 H99G 110.4 . . ?
C993 C994 H99G 110.4 . . ?
O9 C994 H99H 110.4 . . ?
C993 C994 H99H 110.4 . . ?
H99G C994 H99H 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C40 P1 O2 U1 -59.4(19) . . . . ?
C60 P1 O2 U1 -180(100) . . . . ?
C50 P1 O2 U1 58.6(19) . . . . ?
O1 Si1 C10 C15 -162.5(7) . . . . ?
C20 Si1 C10 C15 78.0(8) . . . . ?
C30 Si1 C10 C15 -42.4(8) . . . . ?
O1 Si1 C10 C11 18.2(7) . . . . ?
C20 Si1 C10 C11 -101.3(6) . . . . ?
C30 Si1 C10 C11 138.3(6) . . . . ?
C15 C10 C11 C12 -3.6(12) . . . . ?
Si1 C10 C11 C12 175.8(6) . . . . ?
C10 C11 C12 C13 0.9(13) . . . . ?
C11 C12 C13 C14 1.5(16) . . . . ?
C12 C13 C14 C15 -1.0(18) . . . . ?
C11 C10 C15 C14 4.1(15) . . . . ?
Si1 C10 C15 C14 -175.2(9) . . . . ?
C13 C14 C15 C10 -1.9(18) . . . . ?
O1 Si1 C20 C25 12.7(8) . . . . ?
C30 Si1 C20 C25 -108.9(7) . . . . ?
C10 Si1 C20 C25 132.0(7) . . . . ?
O1 Si1 C20 C21 -164.0(7) . . . . ?
C30 Si1 C20 C21 74.4(8) . . . . ?
C10 Si1 C20 C21 -44.7(8) . . . . ?
C25 C20 C21 C22 1.0(15) . . . . ?
Si1 C20 C21 C22 177.7(9) . . . . ?
C20 C21 C22 C23 -2(2) . . . . ?
C21 C22 C23 C24 3(3) . . . . ?
C22 C23 C24 C25 -3(2) . . . . ?
C21 C20 C25 C24 -1.1(14) . . . . ?
Si1 C20 C25 C24 -178.0(8) . . . . ?
C23 C24 C25 C20 2.2(17) . . . . ?
O1 Si1 C30 C35 32.3(7) . . . . ?
C20 Si1 C30 C35 153.7(7) . . . . ?
C10 Si1 C30 C35 -87.5(7) . . . . ?
O1 Si1 C30 C31 -148.7(7) . . . . ?
C20 Si1 C30 C31 -27.3(8) . . . . ?
C10 Si1 C30 C31 91.5(7) . . . . ?
C35 C30 C31 C32 1.1(13) . . . . ?
Si1 C30 C31 C32 -177.9(8) . . . . ?
C30 C31 C32 C33 -2.4(16) . . . . ?
C31 C32 C33 C34 0.9(17) . . . . ?
C32 C33 C34 C35 1.6(17) . . . . ?
C31 C30 C35 C34 1.6(13) . . . . ?
Si1 C30 C35 C34 -179.4(7) . . . . ?
C33 C34 C35 C30 -3.0(16) . . . . ?
O2 P1 C40 C45 -126.2(7) . . . . ?
C60 P1 C40 C45 -5.0(8) . . . . ?
C50 P1 C40 C45 113.2(7) . . . . ?
O2 P1 C40 C41 52.0(7) . . . . ?
C60 P1 C40 C41 173.2(6) . . . . ?
C50 P1 C40 C41 -68.6(7) . . . . ?
C45 C40 C41 C42 -1.8(14) . . . . ?
P1 C40 C41 C42 179.9(9) . . . . ?
C40 C41 C42 C43 -0.9(17) . . . . ?
C41 C42 C43 C44 2.5(18) . . . . ?
C42 C43 C44 C45 -1.4(16) . . . . ?
C41 C40 C45 C44 3.0(13) . . . . ?
P1 C40 C45 C44 -178.8(7) . . . . ?
C43 C44 C45 C40 -1.4(15) . . . . ?
O2 P1 C50 C55 -162.1(6) . . . . ?
C40 P1 C50 C55 -41.2(7) . . . . ?
C60 P1 C50 C55 76.1(6) . . . . ?
O2 P1 C50 C51 16.7(7) . . . . ?
C40 P1 C50 C51 137.6(6) . . . . ?
C60 P1 C50 C51 -105.1(6) . . . . ?
C55 C50 C51 C52 -0.2(12) . . . . ?
P1 C50 C51 C52 -178.9(7) . . . . ?
C50 C51 C52 C53 -0.6(14) . . . . ?
C51 C52 C53 C54 1.3(16) . . . . ?
C52 C53 C54 C55 -1.2(16) . . . . ?
C51 C50 C55 C54 0.3(12) . . . . ?
P1 C50 C55 C54 179.1(7) . . . . ?
C53 C54 C55 C50 0.4(14) . . . . ?
O2 P1 C60 C65 -155.7(6) . . . . ?
C40 P1 C60 C65 82.5(6) . . . . ?
C50 P1 C60 C65 -33.4(6) . . . . ?
O2 P1 C60 C61 26.8(6) . . . . ?
C40 P1 C60 C61 -95.0(5) . . . . ?
C50 P1 C60 C61 149.1(5) . . . . ?
C65 C60 C61 C62 1.2(10) . . . . ?
P1 C60 C61 C62 178.8(5) . . . . ?
C60 C61 C62 C63 -2.4(12) . . . . ?
C61 C62 C63 C64 3.2(13) . . . . ?
C62 C63 C64 C65 -2.8(15) . . . . ?
C63 C64 C65 C60 1.6(14) . . . . ?
C61 C60 C65 C64 -0.8(11) . . . . ?
P1 C60 C65 C64 -178.2(7) . . . . ?
C894 O8 C891 C892 -12.4 . . . . ?
O8 C891 C892 C893 31.5 . . . . ?
C891 C892 C893 C894 -37.4 . . . . ?
C891 O8 C894 C893 -12.3 . . . . ?
C892 C893 C894 O8 31.5 . . . . ?
C994 O9 C991 C992 -12.3 . . . . ?
O9 C991 C992 C993 31.5 . . . . ?
C991 C992 C993 C994 -37.4 . . . . ?
C991 O9 C994 C993 -12.4 . . . . ?
C992 C993 C994 O9 31.5 . . . . ?

_refine_diff_density_max         2.541
_refine_diff_density_min         -2.366
_refine_diff_density_rms         0.143


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Hygroscopic, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JK755
_database_code_depnum_ccdc_archive 'CCDC 1436228'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;

_vrf_PLAT971_I                   
;
PROBLEM:  Check Calcd Residual Density 1.04A From U1 4.21 eA-3
          Check Calcd Residual Density 1.02A From O2 3.70 eA-3
RFESPONSE: Common issue with uranium
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C6 H5 P1 S2 Si1 U1,C3 H9 O1 Si1,2(C1 F3),8(H2 O1),2(C4 H8 O1),3(C1 H3),2(C6 H5)'
_chemical_formula_sum            'C34 H49 F6 O11 P S2 Si2 U'
_chemical_formula_weight         1137.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.0951(3)
_cell_length_b                   18.5493(4)
_cell_length_c                   17.7595(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.3790(10)
_cell_angle_gamma                90
_cell_volume                     4639.29(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    53002
_cell_measurement_theta_min      3.941
_cell_measurement_theta_max      67.875
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_F_000             2248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    12.173
_shelx_estimated_absorpt_T_min   0.195
_shelx_estimated_absorpt_T_max   0.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53002
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.941
_diffrn_reflns_theta_max         67.875
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_special_details          'crystal mosaicity 0.27'
_diffrn_measurement_details      
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             8289
_reflns_number_gt                7883
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'local programs'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0792P)²+18.9372P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8289
_refine_ls_number_parameters     520
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1247
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.26385(2) 0.77108(2) 0.53580(2) 0.02627(10) Uani 1 1 d . . . . .
S1 S 0.26404(12) 0.88536(9) 0.35913(9) 0.0404(4) Uani 1 1 d . . . . .
S2 S 0.28667(16) 0.78799(9) 0.74636(10) 0.0500(4) Uani 1 1 d . . . . .
P1 P 0.25636(10) 0.56886(7) 0.58224(8) 0.0272(3) Uani 1 1 d . . . . .
Si1 Si -0.00056(14) 0.78439(11) 0.52553(12) 0.0438(4) Uani 1 1 d . . . . .
Si2 Si 0.52765(16) 0.77088(10) 0.53140(14) 0.0486(5) Uani 1 1 d . . . . .
F1 F 0.3466(6) 1.0026(3) 0.4048(5) 0.124(3) Uani 1 1 d . . . . .
F2 F 0.2574(5) 1.0153(3) 0.3070(3) 0.096(2) Uani 1 1 d . . . . .
F3 F 0.1956(7) 1.0032(4) 0.4130(4) 0.121(3) Uani 1 1 d . . . . .
F4 F 0.2456(5) 0.6596(3) 0.7959(3) 0.0812(16) Uani 1 1 d . . . . .
F5 F 0.2452(5) 0.7441(4) 0.8784(3) 0.0811(16) Uani 1 1 d . . . . .
F6 F 0.1314(4) 0.7346(4) 0.7952(4) 0.092(2) Uani 1 1 d . . . . .
O1 O 0.1175(4) 0.7778(2) 0.5286(3) 0.0423(12) Uani 1 1 d . . . . .
O2 O 0.4095(4) 0.7675(2) 0.5375(3) 0.0410(11) Uani 1 1 d . . . . .
O3 O 0.2552(3) 0.6480(2) 0.5634(2) 0.0340(9) Uani 1 1 d . . . . .
O4 O 0.2771(4) 0.8599(3) 0.4362(3) 0.0556(13) Uani 1 1 d . . . . .
O5 O 0.3430(5) 0.8712(4) 0.3147(4) 0.083(2) Uani 1 1 d . . . . .
O6 O 0.1735(5) 0.8707(4) 0.3263(4) 0.080(2) Uani 1 1 d . . . . .
O7 O 0.2585(4) 0.7607(2) 0.6719(3) 0.0496(13) Uani 1 1 d . . . . .
O8 O 0.3852(5) 0.7757(4) 0.7657(5) 0.079(2) Uani 1 1 d . . . . .
O9 O 0.2519(6) 0.8570(3) 0.7628(3) 0.0755(19) Uani 1 1 d . . . . .
O10 O 0.2580(3) 0.7078(3) 0.4127(3) 0.0439(11) Uani 1 1 d . . . . .
O11 O 0.2725(3) 0.8935(2) 0.5890(3) 0.0405(10) Uani 1 1 d . . . . .
C10 C -0.0537(7) 0.6991(6) 0.4903(6) 0.071(2) Uani 1 1 d . . . . .
H10G H -0.0445 0.6948 0.4361 0.106 Uiso 1 1 calc R U . . .
H10H H -0.1218 0.6988 0.4995 0.106 Uiso 1 1 calc R U . . .
H10I H -0.0229 0.6583 0.5167 0.106 Uiso 1 1 calc R U . . .
C11 C -0.0358(8) 0.8600(7) 0.4619(7) 0.094(4) Uani 1 1 d . . . . .
H11Z H -0.0108 0.9053 0.4829 0.141 Uiso 1 1 calc R U . . .
H11Y H -0.1053 0.8627 0.4571 0.141 Uiso 1 1 calc R U . . .
H11G H -0.0101 0.8519 0.4122 0.141 Uiso 1 1 calc R U . . .
C12 C -0.0383(7) 0.8016(7) 0.6228(6) 0.084(3) Uani 1 1 d . . . . .
H12A H 0.0001 0.7723 0.6584 0.126 Uiso 1 1 calc R U . . .
H12B H -0.1054 0.7889 0.6263 0.126 Uiso 1 1 calc R U . . .
H12C H -0.0294 0.8528 0.6349 0.126 Uiso 1 1 calc R U . . .
C20 C 0.5686(6) 0.6872(5) 0.4843(6) 0.066(2) Uani 1 1 d . . . . .
H20A H 0.5374 0.6452 0.5059 0.099 Uiso 1 1 calc R U . . .
H20B H 0.6376 0.6825 0.4921 0.099 Uiso 1 1 calc R U . . .
H20C H 0.5523 0.6899 0.4302 0.099 Uiso 1 1 calc R U . . .
C21 C 0.5810(8) 0.7782(9) 0.6304(8) 0.114(6) Uani 1 1 d . . . . .
H21A H 0.5552 0.8207 0.6551 0.170 Uiso 1 1 calc R U . . .
H21B H 0.6502 0.7828 0.6285 0.170 Uiso 1 1 calc R U . . .
H21C H 0.5655 0.7348 0.6589 0.170 Uiso 1 1 calc R U . . .
C22 C 0.5565(7) 0.8512(5) 0.4733(7) 0.078(3) Uani 1 1 d . . . . .
H22A H 0.5228 0.8478 0.4240 0.118 Uiso 1 1 calc R U . . .
H22B H 0.6251 0.8528 0.4662 0.118 Uiso 1 1 calc R U . . .
H22C H 0.5369 0.8951 0.4990 0.118 Uiso 1 1 calc R U . . .
C30 C 0.1485(4) 0.5446(3) 0.6271(3) 0.0315(12) Uani 1 1 d . . . . .
C31 C 0.0956(4) 0.5996(4) 0.6572(4) 0.0392(14) Uani 1 1 d . . . . .
H31 H 0.1129 0.6485 0.6496 0.047 Uiso 1 1 calc R U . . .
C32 C 0.0175(5) 0.5833(4) 0.6983(4) 0.0453(16) Uani 1 1 d . . . . .
H32 H -0.0186 0.6208 0.7197 0.054 Uiso 1 1 calc R U . . .
C33 C -0.0079(5) 0.5121(4) 0.7084(4) 0.0524(18) Uani 1 1 d . . . . .
H33 H -0.0616 0.5010 0.7367 0.063 Uiso 1 1 calc R U . . .
C34 C 0.0435(5) 0.4571(4) 0.6779(4) 0.0484(17) Uani 1 1 d . . . . .
H34 H 0.0247 0.4084 0.6847 0.058 Uiso 1 1 calc R U . . .
C35 C 0.1232(5) 0.4727(3) 0.6368(4) 0.0408(15) Uani 1 1 d . . . . .
H35 H 0.1595 0.4351 0.6159 0.049 Uiso 1 1 calc R U . . .
C40 C 0.3531(4) 0.5481(3) 0.6479(3) 0.0334(13) Uani 1 1 d . . . . .
C41 C 0.4026(4) 0.6044(4) 0.6840(4) 0.0423(15) Uani 1 1 d . . . . .
H41 H 0.3886 0.6531 0.6712 0.051 Uiso 1 1 calc R U . . .
C42 C 0.4720(5) 0.5885(5) 0.7385(4) 0.055(2) Uani 1 1 d . . . . .
H42 H 0.5065 0.6265 0.7630 0.066 Uiso 1 1 calc R U . . .
C43 C 0.4917(5) 0.5186(6) 0.7576(4) 0.062(2) Uani 1 1 d . . . . .
H43 H 0.5390 0.5085 0.7958 0.075 Uiso 1 1 calc R U . . .
C44 C 0.4436(5) 0.4620(5) 0.7220(4) 0.057(2) Uani 1 1 d . . . . .
H44 H 0.4582 0.4136 0.7354 0.068 Uiso 1 1 calc R U . . .
C45 C 0.3745(5) 0.4766(4) 0.6671(4) 0.0407(14) Uani 1 1 d . . . . .
H45 H 0.3414 0.4381 0.6423 0.049 Uiso 1 1 calc R U . . .
C50 C 0.2722(4) 0.5137(3) 0.5005(3) 0.0293(11) Uani 1 1 d . . . . .
C51 C 0.1995(5) 0.4765(4) 0.4635(4) 0.0424(15) Uani 1 1 d . . . . .
H51 H 0.1374 0.4769 0.4823 0.051 Uiso 1 1 calc R U . . .
C52 C 0.2181(5) 0.4380(4) 0.3978(4) 0.0490(17) Uani 1 1 d . . . . .
H52 H 0.1683 0.4119 0.3724 0.059 Uiso 1 1 calc R U . . .
C53 C 0.3072(5) 0.4375(4) 0.3697(4) 0.0465(16) Uani 1 1 d . . . . .
H53 H 0.3188 0.4112 0.3251 0.056 Uiso 1 1 calc R U . . .
C54 C 0.3801(5) 0.4751(4) 0.4059(4) 0.0472(17) Uani 1 1 d . . . . .
H54 H 0.4417 0.4754 0.3860 0.057 Uiso 1 1 calc R U . . .
C55 C 0.3626(5) 0.5131(3) 0.4727(4) 0.0379(14) Uani 1 1 d . . . . .
H55 H 0.4128 0.5383 0.4986 0.045 Uiso 1 1 calc R U . . .
C60 C 0.2260(7) 0.7277(4) 0.8079(5) 0.060(2) Uani 1 1 d . . . . .
C70 C 0.2666(8) 0.9809(5) 0.3718(5) 0.068(2) Uani 1 1 d . . . . .
C100 C 0.1699(6) 0.6815(4) 0.3768(4) 0.0529(18) Uani 1 1 d . . . . .
H10E H 0.1288 0.7220 0.3596 0.063 Uiso 1 1 calc R U . . .
H10F H 0.1346 0.6511 0.4119 0.063 Uiso 1 1 calc R U . . .
C101 C 0.2024(7) 0.6375(5) 0.3103(5) 0.064(2) Uani 1 1 d . . . . .
H10J H 0.2121 0.5863 0.3245 0.077 Uiso 1 1 calc R U . . .
H10K H 0.1554 0.6401 0.2674 0.077 Uiso 1 1 calc R U . . .
C102 C 0.2925(7) 0.6713(6) 0.2910(5) 0.073(3) Uani 1 1 d . . . . .
H10C H 0.2813 0.7145 0.2591 0.087 Uiso 1 1 calc R U . . .
H10D H 0.3331 0.6370 0.2643 0.087 Uiso 1 1 calc R U . . .
C103 C 0.3370(6) 0.6915(4) 0.3668(4) 0.0497(17) Uani 1 1 d . . . . .
H10A H 0.3747 0.6510 0.3884 0.060 Uiso 1 1 calc R U . . .
H10B H 0.3788 0.7341 0.3623 0.060 Uiso 1 1 calc R U . . .
C111 C 0.1896(5) 0.9376(4) 0.6003(5) 0.0538(19) Uani 1 1 d . . . . .
H11C H 0.1541 0.9193 0.6433 0.065 Uiso 1 1 calc R U . . .
H11D H 0.1469 0.9374 0.5547 0.065 Uiso 1 1 calc R U . . .
C112 C 0.2269(7) 1.0135(5) 0.6167(8) 0.087(4) Uani 1 1 d . . . . .
H11E H 0.2244 1.0433 0.5704 0.104 Uiso 1 1 calc R U . . .
H11F H 0.1892 1.0375 0.6553 0.104 Uiso 1 1 calc R U . . .
C113 C 0.3212(7) 1.0031(5) 0.6433(9) 0.101(5) Uani 1 1 d . . . . .
H11X H 0.3241 0.9993 0.6990 0.121 Uiso 1 1 calc R U . . .
H11W H 0.3611 1.0443 0.6287 0.121 Uiso 1 1 calc R U . . .
C114 C 0.3570(6) 0.9342(4) 0.6088(5) 0.0532(18) Uani 1 1 d . . . . .
H11A H 0.3933 0.9447 0.5635 0.064 Uiso 1 1 calc R U . . .
H11B H 0.3983 0.9073 0.6455 0.064 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 2.053(6) . ?
U1 O1 2.066(6) . ?
U1 O3 2.339(4) . ?
U1 O7 2.429(5) . ?
U1 O4 2.430(5) . ?
U1 O11 2.461(4) . ?
U1 O10 2.480(5) . ?
S1 O6 1.407(6) . ?
S1 O5 1.415(6) . ?
S1 O4 1.452(5) . ?
S1 C70 1.786(9) . ?
S2 O9 1.405(6) . ?
S2 O8 1.435(8) . ?
S2 O7 1.455(5) . ?
S2 C60 1.804(9) . ?
P1 O3 1.506(4) . ?
P1 C50 1.797(6) . ?
P1 C40 1.799(6) . ?
P1 C30 1.803(6) . ?
Si1 O1 1.667(6) . ?
Si1 C10 1.849(9) . ?
Si1 C12 1.855(10) . ?
Si1 C11 1.856(10) . ?
Si2 O2 1.675(6) . ?
Si2 C20 1.866(9) . ?
Si2 C22 1.867(10) . ?
Si2 C21 1.888(12) . ?
F1 C70 1.313(12) . ?
F2 C70 1.316(9) . ?
F3 C70 1.331(12) . ?
F4 C60 1.312(10) . ?
F5 C60 1.305(10) . ?
F6 C60 1.349(12) . ?
O10 C103 1.439(9) . ?
O10 C100 1.456(9) . ?
O11 C114 1.440(8) . ?
O11 C111 1.446(8) . ?
C10 H10G 0.9800 . ?
C10 H10H 0.9800 . ?
C10 H10I 0.9800 . ?
C11 H11Z 0.9800 . ?
C11 H11Y 0.9800 . ?
C11 H11G 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C30 C31 1.385(9) . ?
C30 C35 1.392(9) . ?
C31 C32 1.378(9) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(11) . ?
C32 H32 0.9500 . ?
C33 C34 1.375(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.395(9) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C41 1.398(9) . ?
C40 C45 1.399(9) . ?
C41 C42 1.380(10) . ?
C41 H41 0.9500 . ?
C42 C43 1.366(13) . ?
C42 H42 0.9500 . ?
C43 C44 1.387(13) . ?
C43 H43 0.9500 . ?
C44 C45 1.374(10) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C50 C51 1.380(9) . ?
C50 C55 1.386(8) . ?
C51 C52 1.401(10) . ?
C51 H51 0.9500 . ?
C52 C53 1.371(10) . ?
C52 H52 0.9500 . ?
C53 C54 1.379(10) . ?
C53 H53 0.9500 . ?
C54 C55 1.410(9) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C100 C101 1.523(11) . ?
C100 H10E 0.9900 . ?
C100 H10F 0.9900 . ?
C101 C102 1.469(13) . ?
C101 H10J 0.9900 . ?
C101 H10K 0.9900 . ?
C102 C103 1.508(11) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C103 H10A 0.9900 . ?
C103 H10B 0.9900 . ?
C111 C112 1.527(11) . ?
C111 H11C 0.9900 . ?
C111 H11D 0.9900 . ?
C112 C113 1.406(14) . ?
C112 H11E 0.9900 . ?
C112 H11F 0.9900 . ?
C113 C114 1.513(11) . ?
C113 H11X 0.9900 . ?
C113 H11W 0.9900 . ?
C114 H11A 0.9900 . ?
C114 H11B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 176.85(17) . . ?
O2 U1 O3 91.49(15) . . ?
O1 U1 O3 90.66(16) . . ?
O2 U1 O7 93.1(2) . . ?
O1 U1 O7 89.7(2) . . ?
O3 U1 O7 73.17(15) . . ?
O2 U1 O4 85.74(19) . . ?
O1 U1 O4 91.18(19) . . ?
O3 U1 O4 145.11(17) . . ?
O7 U1 O4 141.67(17) . . ?
O2 U1 O11 89.46(16) . . ?
O1 U1 O11 90.08(16) . . ?
O3 U1 O11 145.34(15) . . ?
O7 U1 O11 72.19(15) . . ?
O4 U1 O11 69.50(16) . . ?
O2 U1 O10 89.68(18) . . ?
O1 U1 O10 88.70(18) . . ?
O3 U1 O10 73.90(16) . . ?
O7 U1 O10 147.01(15) . . ?
O4 U1 O10 71.31(17) . . ?
O11 U1 O10 140.76(16) . . ?
O6 S1 O5 117.0(5) . . ?
O6 S1 O4 113.9(4) . . ?
O5 S1 O4 113.1(4) . . ?
O6 S1 C70 104.9(5) . . ?
O5 S1 C70 104.0(5) . . ?
O4 S1 C70 101.7(4) . . ?
O9 S2 O8 115.9(4) . . ?
O9 S2 O7 114.9(4) . . ?
O8 S2 O7 112.7(4) . . ?
O9 S2 C60 105.1(4) . . ?
O8 S2 C60 103.6(5) . . ?
O7 S2 C60 102.5(4) . . ?
O3 P1 C50 112.1(3) . . ?
O3 P1 C40 110.7(3) . . ?
C50 P1 C40 106.5(3) . . ?
O3 P1 C30 109.9(3) . . ?
C50 P1 C30 110.5(3) . . ?
C40 P1 C30 106.9(3) . . ?
O1 Si1 C10 109.8(4) . . ?
O1 Si1 C12 107.9(4) . . ?
C10 Si1 C12 109.6(5) . . ?
O1 Si1 C11 108.5(4) . . ?
C10 Si1 C11 110.3(6) . . ?
C12 Si1 C11 110.9(6) . . ?
O2 Si2 C20 109.0(3) . . ?
O2 Si2 C22 107.8(4) . . ?
C20 Si2 C22 109.7(5) . . ?
O2 Si2 C21 107.5(4) . . ?
C20 Si2 C21 111.0(6) . . ?
C22 Si2 C21 111.7(6) . . ?
Si1 O1 U1 178.1(3) . . ?
Si2 O2 U1 173.9(3) . . ?
P1 O3 U1 176.4(3) . . ?
S1 O4 U1 153.6(3) . . ?
S2 O7 U1 149.1(3) . . ?
C103 O10 C100 110.3(5) . . ?
C103 O10 U1 126.9(4) . . ?
C100 O10 U1 122.7(4) . . ?
C114 O11 C111 109.6(5) . . ?
C114 O11 U1 127.1(4) . . ?
C111 O11 U1 123.2(4) . . ?
Si1 C10 H10G 109.5 . . ?
Si1 C10 H10H 109.5 . . ?
H10G C10 H10H 109.5 . . ?
Si1 C10 H10I 109.5 . . ?
H10G C10 H10I 109.5 . . ?
H10H C10 H10I 109.5 . . ?
Si1 C11 H11Z 109.5 . . ?
Si1 C11 H11Y 109.5 . . ?
H11Z C11 H11Y 109.5 . . ?
Si1 C11 H11G 109.5 . . ?
H11Z C11 H11G 109.5 . . ?
H11Y C11 H11G 109.5 . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C31 C30 C35 120.9(6) . . ?
C31 C30 P1 117.7(5) . . ?
C35 C30 P1 121.3(5) . . ?
C32 C31 C30 119.8(6) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C31 C32 C33 119.7(6) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C34 C33 C32 121.0(6) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 120.0(7) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C30 C35 C34 118.6(6) . . ?
C30 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
C41 C40 C45 119.9(6) . . ?
C41 C40 P1 119.2(5) . . ?
C45 C40 P1 120.8(5) . . ?
C42 C41 C40 119.2(7) . . ?
C42 C41 H41 120.4 . . ?
C40 C41 H41 120.4 . . ?
C43 C42 C41 120.5(8) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C42 C43 C44 121.0(7) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 H43 119.5 . . ?
C45 C44 C43 119.6(8) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C44 C45 C40 119.9(7) . . ?
C44 C45 H45 120.1 . . ?
C40 C45 H45 120.1 . . ?
C51 C50 C55 120.1(6) . . ?
C51 C50 P1 123.7(5) . . ?
C55 C50 P1 116.1(4) . . ?
C50 C51 C52 119.5(6) . . ?
C50 C51 H51 120.3 . . ?
C52 C51 H51 120.3 . . ?
C53 C52 C51 120.7(6) . . ?
C53 C52 H52 119.6 . . ?
C51 C52 H52 119.6 . . ?
C52 C53 C54 120.2(6) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C53 C54 C55 119.5(7) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
C50 C55 C54 120.0(6) . . ?
C50 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
F5 C60 F4 110.0(8) . . ?
F5 C60 F6 107.7(8) . . ?
F4 C60 F6 106.1(8) . . ?
F5 C60 S2 110.6(6) . . ?
F4 C60 S2 112.9(6) . . ?
F6 C60 S2 109.2(6) . . ?
F1 C70 F2 107.0(8) . . ?
F1 C70 F3 108.0(9) . . ?
F2 C70 F3 106.4(8) . . ?
F1 C70 S1 111.9(7) . . ?
F2 C70 S1 111.7(7) . . ?
F3 C70 S1 111.5(7) . . ?
O10 C100 C101 103.9(6) . . ?
O10 C100 H10E 111.0 . . ?
C101 C100 H10E 111.0 . . ?
O10 C100 H10F 111.0 . . ?
C101 C100 H10F 111.0 . . ?
H10E C100 H10F 109.0 . . ?
C102 C101 C100 104.0(7) . . ?
C102 C101 H10J 111.0 . . ?
C100 C101 H10J 111.0 . . ?
C102 C101 H10K 111.0 . . ?
C100 C101 H10K 111.0 . . ?
H10J C101 H10K 109.0 . . ?
C101 C102 C103 103.3(7) . . ?
C101 C102 H10C 111.1 . . ?
C103 C102 H10C 111.1 . . ?
C101 C102 H10D 111.1 . . ?
C103 C102 H10D 111.1 . . ?
H10C C102 H10D 109.1 . . ?
O10 C103 C102 104.8(7) . . ?
O10 C103 H10A 110.8 . . ?
C102 C103 H10A 110.8 . . ?
O10 C103 H10B 110.8 . . ?
C102 C103 H10B 110.8 . . ?
H10A C103 H10B 108.9 . . ?
O11 C111 C112 105.9(6) . . ?
O11 C111 H11C 110.6 . . ?
C112 C111 H11C 110.6 . . ?
O11 C111 H11D 110.6 . . ?
C112 C111 H11D 110.6 . . ?
H11C C111 H11D 108.7 . . ?
C113 C112 C111 104.5(7) . . ?
C113 C112 H11E 110.9 . . ?
C111 C112 H11E 110.9 . . ?
C113 C112 H11F 110.9 . . ?
C111 C112 H11F 110.9 . . ?
H11E C112 H11F 108.9 . . ?
C112 C113 C114 107.8(8) . . ?
C112 C113 H11X 110.1 . . ?
C114 C113 H11X 110.1 . . ?
C112 C113 H11W 110.1 . . ?
C114 C113 H11W 110.1 . . ?
H11X C113 H11W 108.5 . . ?
O11 C114 C113 104.8(7) . . ?
O11 C114 H11A 110.8 . . ?
C113 C114 H11A 110.8 . . ?
O11 C114 H11B 110.8 . . ?
C113 C114 H11B 110.8 . . ?
H11A C114 H11B 108.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 S1 O4 U1 44.8(10) . . . . ?
O5 S1 O4 U1 -92.0(9) . . . . ?
C70 S1 O4 U1 157.0(8) . . . . ?
O9 S2 O7 U1 64.4(8) . . . . ?
O8 S2 O7 U1 -71.4(8) . . . . ?
C60 S2 O7 U1 177.8(7) . . . . ?
O3 P1 C30 C31 -18.0(6) . . . . ?
C50 P1 C30 C31 -142.2(5) . . . . ?
C40 P1 C30 C31 102.2(5) . . . . ?
O3 P1 C30 C35 167.2(5) . . . . ?
C50 P1 C30 C35 42.9(6) . . . . ?
C40 P1 C30 C35 -72.6(6) . . . . ?
C35 C30 C31 C32 1.0(10) . . . . ?
P1 C30 C31 C32 -173.8(5) . . . . ?
C30 C31 C32 C33 -0.8(11) . . . . ?
C31 C32 C33 C34 -0.1(12) . . . . ?
C32 C33 C34 C35 0.7(12) . . . . ?
C31 C30 C35 C34 -0.3(10) . . . . ?
P1 C30 C35 C34 174.3(5) . . . . ?
C33 C34 C35 C30 -0.5(11) . . . . ?
O3 P1 C40 C41 11.8(6) . . . . ?
C50 P1 C40 C41 134.0(5) . . . . ?
C30 P1 C40 C41 -107.9(5) . . . . ?
O3 P1 C40 C45 -172.9(5) . . . . ?
C50 P1 C40 C45 -50.7(6) . . . . ?
C30 P1 C40 C45 67.4(6) . . . . ?
C45 C40 C41 C42 -0.2(9) . . . . ?
P1 C40 C41 C42 175.2(5) . . . . ?
C40 C41 C42 C43 -0.7(10) . . . . ?
C41 C42 C43 C44 1.1(12) . . . . ?
C42 C43 C44 C45 -0.6(12) . . . . ?
C43 C44 C45 C40 -0.2(11) . . . . ?
C41 C40 C45 C44 0.6(10) . . . . ?
P1 C40 C45 C44 -174.6(5) . . . . ?
O3 P1 C50 C51 -102.9(6) . . . . ?
C40 P1 C50 C51 135.8(5) . . . . ?
C30 P1 C50 C51 20.1(6) . . . . ?
O3 P1 C50 C55 73.6(5) . . . . ?
C40 P1 C50 C55 -47.7(5) . . . . ?
C30 P1 C50 C55 -163.5(5) . . . . ?
C55 C50 C51 C52 0.3(10) . . . . ?
P1 C50 C51 C52 176.6(5) . . . . ?
C50 C51 C52 C53 -0.6(11) . . . . ?
C51 C52 C53 C54 0.0(12) . . . . ?
C52 C53 C54 C55 1.0(11) . . . . ?
C51 C50 C55 C54 0.7(10) . . . . ?
P1 C50 C55 C54 -175.8(5) . . . . ?
C53 C54 C55 C50 -1.4(11) . . . . ?
O9 S2 C60 F5 -60.7(8) . . . . ?
O8 S2 C60 F5 61.4(8) . . . . ?
O7 S2 C60 F5 178.9(7) . . . . ?
O9 S2 C60 F4 175.5(7) . . . . ?
O8 S2 C60 F4 -62.4(8) . . . . ?
O7 S2 C60 F4 55.0(8) . . . . ?
O9 S2 C60 F6 57.6(7) . . . . ?
O8 S2 C60 F6 179.7(6) . . . . ?
O7 S2 C60 F6 -62.8(7) . . . . ?
O6 S1 C70 F1 177.7(7) . . . . ?
O5 S1 C70 F1 -58.9(8) . . . . ?
O4 S1 C70 F1 58.8(8) . . . . ?
O6 S1 C70 F2 -62.3(9) . . . . ?
O5 S1 C70 F2 61.1(9) . . . . ?
O4 S1 C70 F2 178.8(7) . . . . ?
O6 S1 C70 F3 56.6(8) . . . . ?
O5 S1 C70 F3 179.9(7) . . . . ?
O4 S1 C70 F3 -62.3(8) . . . . ?
C103 O10 C100 C101 8.2(8) . . . . ?
U1 O10 C100 C101 -171.7(5) . . . . ?
O10 C100 C101 C102 -28.3(9) . . . . ?
C100 C101 C102 C103 36.9(10) . . . . ?
C100 O10 C103 C102 14.5(9) . . . . ?
U1 O10 C103 C102 -165.6(5) . . . . ?
C101 C102 C103 O10 -32.1(10) . . . . ?
C114 O11 C111 C112 9.0(10) . . . . ?
U1 O11 C111 C112 -167.4(6) . . . . ?
O11 C111 C112 C113 -23.0(13) . . . . ?
C111 C112 C113 C114 27.8(14) . . . . ?
C111 O11 C114 C113 7.4(10) . . . . ?
U1 O11 C114 C113 -176.3(7) . . . . ?
C112 C113 C114 O11 -22.8(13) . . . . ?

_refine_diff_density_max         4.064
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.175


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF, Pentane'
_chemical_properties_physical    'Air-sensitive, Hygroscopic, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JK6202
_database_code_depnum_ccdc_archive 'CCDC 1436229'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;

_vrf_PLAT029_I                   
;
PROBLEM:  _diffrn_measured_fraction_theta_full Low ....... 0.934 Note
RFESPONSE: ?
;
_vrf_PLAT342_I                   
;
PROBLEM:  Low Bond Precision on C-C Bonds ............... 0.0228 Ang.
RFESPONSE: slight disorder in co-crystallized toluene
;
_vrf_PLAT911_I                   
;
PROBLEM:  Missing # FCF Refl Between THmin & STh/L= 0.600 317 Report
RFESPONSE: ?
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H48 I2 O4 P2 Si2 U1,C7 H8'
_chemical_formula_sum            'C49 H56 I2 O4 P2 Si2 U'
_chemical_formula_weight         1318.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3801(7)
_cell_length_b                   11.9238(9)
_cell_length_c                   12.6051(12)
_cell_angle_alpha                76.394(6)
_cell_angle_beta                 67.826(6)
_cell_angle_gamma                67.689(5)
_cell_volume                     1328.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    180581
_cell_measurement_theta_min      5.127
_cell_measurement_theta_max      67.849
_exptl_crystal_description       platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_F_000             638
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    19.020
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_T_max  0.467
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            180581
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.092
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         5.127
_diffrn_reflns_theta_max         67.849
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_special_details          'crystal mosaicity 0.27'
_diffrn_measurement_details      
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.934
_reflns_number_total             4519
_reflns_number_gt                4270
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'local programs'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0840P)²+5.6349P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4519
_refine_ls_number_parameters     276
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1498
_refine_ls_wR_factor_gt          0.1464
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.0000 0.0000 0.5000 0.04842(17) Uani 1 2 d S . P . .
I1 I 0.31047(7) -0.17725(6) 0.38230(6) 0.0728(2) Uani 1 1 d . . . . .
P1 P 0.1248(3) 0.2534(2) 0.28473(19) 0.0571(5) Uani 1 1 d . . . . .
Si1 Si -0.1122(5) -0.0883(6) 0.2972(3) 0.1234(18) Uani 1 1 d . . . . .
O1 O -0.0738(7) -0.0324(6) 0.3814(5) 0.0631(16) Uani 1 1 d . . . . .
O2 O 0.0633(8) 0.1601(6) 0.3693(5) 0.0638(16) Uani 1 1 d . . . . .
C1 C -0.032(3) -0.2753(18) 0.3483(19) 0.162(8) Uani 1 1 d . . . . .
H1A H 0.0369 -0.3166 0.2825 0.243 Uiso 1 1 calc R U . . .
H1B H -0.1126 -0.3075 0.3818 0.243 Uiso 1 1 calc R U . . .
H1C H 0.0154 -0.2874 0.4042 0.243 Uiso 1 1 calc R U . . .
C2 C -0.2969(19) -0.073(2) 0.3302(16) 0.140(7) Uani 1 1 d . . . . .
H2A H -0.3441 -0.0730 0.4121 0.209 Uiso 1 1 calc R U . . .
H2B H -0.3038 -0.1393 0.3047 0.209 Uiso 1 1 calc R U . . .
H2C H -0.3444 0.0028 0.2922 0.209 Uiso 1 1 calc R U . . .
C3 C 0.002(2) -0.098(3) 0.1597(16) 0.174(10) Uani 1 1 d . . . . .
H3A H -0.0261 -0.0211 0.1144 0.261 Uiso 1 1 calc R U . . .
H3B H -0.0036 -0.1608 0.1282 0.261 Uiso 1 1 calc R U . . .
H3C H 0.1012 -0.1162 0.1584 0.261 Uiso 1 1 calc R U . . .
C10 C 0.2389(11) 0.1950(9) 0.1495(8) 0.059(2) Uani 1 1 d . . . . .
C11 C 0.2048(13) 0.1151(10) 0.1109(8) 0.071(3) Uani 1 1 d . . . . .
H11 H 0.1269 0.0874 0.1580 0.085 Uiso 1 1 calc R U . . .
C12 C 0.2835(13) 0.0750(11) 0.0035(9) 0.078(3) Uani 1 1 d . . . . .
H12 H 0.2586 0.0203 -0.0206 0.094 Uiso 1 1 calc R U . . .
C13 C 0.3966(12) 0.1144(10) -0.0666(9) 0.074(3) Uani 1 1 d . . . . .
H13 H 0.4488 0.0872 -0.1391 0.089 Uiso 1 1 calc R U . . .
C14 C 0.4351(12) 0.1954(10) -0.0313(9) 0.071(3) Uani 1 1 d . . . . .
H14 H 0.5129 0.2228 -0.0797 0.086 Uiso 1 1 calc R U . . .
C15 C 0.3569(12) 0.2353(9) 0.0768(8) 0.067(2) Uani 1 1 d . . . . .
H15 H 0.3828 0.2890 0.1013 0.080 Uiso 1 1 calc R U . . .
C20 C -0.0240(12) 0.3839(9) 0.2571(8) 0.064(2) Uani 1 1 d . . . . .
C21 C -0.1665(13) 0.3943(10) 0.3275(10) 0.079(3) Uani 1 1 d . . . . .
H21 H -0.1853 0.3332 0.3865 0.095 Uiso 1 1 calc R U . . .
C22 C -0.2802(14) 0.4958(12) 0.3098(11) 0.092(4) Uani 1 1 d . . . . .
H22 H -0.3757 0.5045 0.3589 0.110 Uiso 1 1 calc R U . . .
C23 C -0.2542(16) 0.5840(12) 0.2206(12) 0.092(4) Uani 1 1 d . . . . .
H23 H -0.3319 0.6517 0.2088 0.111 Uiso 1 1 calc R U . . .
C24 C -0.1154(16) 0.5724(10) 0.1498(11) 0.089(4) Uani 1 1 d . . . . .
H24 H -0.0984 0.6327 0.0894 0.107 Uiso 1 1 calc R U . . .
C25 C 0.0019(14) 0.4723(10) 0.1658(10) 0.077(3) Uani 1 1 d . . . . .
H25 H 0.0968 0.4646 0.1160 0.092 Uiso 1 1 calc R U . . .
C30 C 0.2296(13) 0.3034(11) 0.3380(8) 0.072(3) Uani 1 1 d . . . . .
C31 C 0.1862(17) 0.4181(13) 0.3652(12) 0.095(4) Uani 1 1 d . . . . .
H31 H 0.1021 0.4762 0.3521 0.114 Uiso 1 1 calc R U . . .
C32 C 0.269(2) 0.4495(17) 0.4136(14) 0.118(5) Uani 1 1 d . . . . .
H32 H 0.2401 0.5283 0.4322 0.141 Uiso 1 1 calc R U . . .
C33 C 0.3901(19) 0.3639(19) 0.4323(13) 0.109(5) Uani 1 1 d . . . . .
H33 H 0.4449 0.3845 0.4638 0.131 Uiso 1 1 calc R U . . .
C34 C 0.4347(18) 0.247(2) 0.4057(13) 0.118(5) Uani 1 1 d . . . . .
H34 H 0.5170 0.1880 0.4212 0.141 Uiso 1 1 calc R U . . .
C35 C 0.3568(15) 0.2174(14) 0.3565(11) 0.091(4) Uani 1 1 d . . . . .
H35 H 0.3888 0.1394 0.3350 0.109 Uiso 1 1 calc R U . . .
C91 C 0.498(3) 0.492(2) 0.1111(18) 0.132(6) Uani 1 1 d . . . . .
H91 H 0.4952 0.4872 0.1867 0.158 Uiso 1 1 calc R U . . .
C92 C 0.617(3) 0.4182(19) 0.036(2) 0.131(7) Uani 1 1 d . . . . .
H92 H 0.6945 0.3636 0.0595 0.157 Uiso 0.5 1 d . U P . .
C93 C 0.383(3) 0.572(2) 0.075(2) 0.144(7) Uani 1 1 d . . . . .
H93 H 0.3035 0.6217 0.1268 0.173 Uiso 1 1 calc R U . . .
C97 C 0.741(5) 0.328(4) 0.073(4) 0.157(15) Uiso 0.5 1 d . . P . .
H97A H 0.8124 0.3658 0.0626 0.236 Uiso 0.5 1 calc R U P . .
H97B H 0.7858 0.2605 0.0279 0.236 Uiso 0.5 1 calc R U P . .
H97C H 0.7049 0.2995 0.1530 0.236 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.082(6) 2_556 ?
U1 O1 2.082(6) . ?
U1 O2 2.333(6) . ?
U1 O2 2.333(6) 2_556 ?
U1 I1 3.1222(7) 2_556 ?
U1 I1 3.1223(7) . ?
P1 O2 1.500(7) . ?
P1 C10 1.789(10) . ?
P1 C30 1.796(11) . ?
P1 C20 1.804(10) . ?
Si1 O1 1.607(7) . ?
Si1 C3 1.692(18) . ?
Si1 C2 1.745(16) . ?
Si1 C1 2.10(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C10 C11 1.368(14) . ?
C10 C15 1.401(14) . ?
C11 C12 1.379(14) . ?
C11 H11 0.9300 . ?
C12 C13 1.349(15) . ?
C12 H12 0.9300 . ?
C13 C14 1.387(16) . ?
C13 H13 0.9300 . ?
C14 C15 1.385(15) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C20 C21 1.383(16) . ?
C20 C25 1.385(14) . ?
C21 C22 1.377(16) . ?
C21 H21 0.9300 . ?
C22 C23 1.368(18) . ?
C22 H22 0.9300 . ?
C23 C24 1.353(18) . ?
C23 H23 0.9300 . ?
C24 C25 1.384(16) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C30 C31 1.351(17) . ?
C30 C35 1.393(17) . ?
C31 C32 1.413(19) . ?
C31 H31 0.9300 . ?
C32 C33 1.35(2) . ?
C32 H32 0.9300 . ?
C33 C34 1.38(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.362(19) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C91 C92 1.37(3) . ?
C91 C93 1.37(3) . ?
C91 H91 0.9300 . ?
C92 C93 1.38(3) 2_665 ?
C92 C97 1.48(5) . ?
C92 H92 0.92(2) . ?
C93 C92 1.38(3) 2_665 ?
C93 H93 0.9300 . ?
C97 H92 0.56(5) . ?
C97 H97A 0.9600 . ?
C97 H97B 0.9600 . ?
C97 H97C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 2_556 . ?
O1 U1 O2 91.8(2) 2_556 . ?
O1 U1 O2 88.2(2) . . ?
O1 U1 O2 88.2(2) 2_556 2_556 ?
O1 U1 O2 91.8(2) . 2_556 ?
O2 U1 O2 180.0 . 2_556 ?
O1 U1 I1 88.26(19) 2_556 2_556 ?
O1 U1 I1 91.74(19) . 2_556 ?
O2 U1 I1 90.92(16) . 2_556 ?
O2 U1 I1 89.08(16) 2_556 2_556 ?
O1 U1 I1 91.74(19) 2_556 . ?
O1 U1 I1 88.26(19) . . ?
O2 U1 I1 89.08(16) . . ?
O2 U1 I1 90.92(16) 2_556 . ?
I1 U1 I1 180.0 2_556 . ?
O2 P1 C10 111.2(4) . . ?
O2 P1 C30 111.7(4) . . ?
C10 P1 C30 108.9(5) . . ?
O2 P1 C20 109.4(5) . . ?
C10 P1 C20 106.9(4) . . ?
C30 P1 C20 108.6(5) . . ?
O1 Si1 C3 117.1(7) . . ?
O1 Si1 C2 116.4(7) . . ?
C3 Si1 C2 120.6(9) . . ?
O1 Si1 C1 100.7(7) . . ?
C3 Si1 C1 94.6(12) . . ?
C2 Si1 C1 99.1(10) . . ?
Si1 O1 U1 167.4(5) . . ?
P1 O2 U1 172.3(4) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C11 C10 C15 118.2(9) . . ?
C11 C10 P1 119.6(8) . . ?
C15 C10 P1 122.0(8) . . ?
C10 C11 C12 121.4(11) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C13 C12 C11 120.4(11) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 120.3(10) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 119.5(10) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C10 120.3(10) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
C21 C20 C25 119.7(10) . . ?
C21 C20 P1 119.1(8) . . ?
C25 C20 P1 121.2(9) . . ?
C22 C21 C20 119.5(11) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C23 C22 C21 120.7(13) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 119.9(12) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 121.1(11) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C20 119.1(12) . . ?
C24 C25 H25 120.4 . . ?
C20 C25 H25 120.4 . . ?
C31 C30 C35 119.8(11) . . ?
C31 C30 P1 122.6(10) . . ?
C35 C30 P1 117.6(9) . . ?
C30 C31 C32 119.8(14) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C33 C32 C31 119.2(15) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C32 C33 C34 121.5(14) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.3 . . ?
C35 C34 C33 119.2(16) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C30 120.5(14) . . ?
C34 C35 H35 119.7 . . ?
C30 C35 H35 119.7 . . ?
C92 C91 C93 120(2) . . ?
C92 C91 H91 120.0 . . ?
C93 C91 H91 120.0 . . ?
C91 C92 C93 118(2) . 2_665 ?
C91 C92 C97 121(3) . . ?
C93 C92 C97 121(3) 2_665 . ?
C91 C92 H92 121(3) . . ?
C93 C92 H92 121(3) 2_665 . ?
C97 C92 H92 1.3(18) . . ?
C91 C93 C92 122(2) . 2_665 ?
C91 C93 H93 119.0 . . ?
C92 C93 H93 119.0 2_665 . ?
C92 C97 H92 2(3) . . ?
C92 C97 H97A 109.5 . . ?
H92 C97 H97A 107.6 . . ?
C92 C97 H97B 109.5 . . ?
H92 C97 H97B 111.3 . . ?
H97A C97 H97B 109.5 . . ?
C92 C97 H97C 109.5 . . ?
H92 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 Si1 O1 U1 -93(2) . . . . ?
C2 Si1 O1 U1 113(2) . . . . ?
C1 Si1 O1 U1 7(2) . . . . ?
O2 P1 C10 C11 34.1(10) . . . . ?
C30 P1 C10 C11 157.6(8) . . . . ?
C20 P1 C10 C11 -85.3(9) . . . . ?
O2 P1 C10 C15 -150.8(8) . . . . ?
C30 P1 C10 C15 -27.2(10) . . . . ?
C20 P1 C10 C15 89.9(9) . . . . ?
C15 C10 C11 C12 -0.1(16) . . . . ?
P1 C10 C11 C12 175.2(9) . . . . ?
C10 C11 C12 C13 -0.3(18) . . . . ?
C11 C12 C13 C14 0.3(17) . . . . ?
C12 C13 C14 C15 0.2(16) . . . . ?
C13 C14 C15 C10 -0.6(15) . . . . ?
C11 C10 C15 C14 0.6(15) . . . . ?
P1 C10 C15 C14 -174.7(8) . . . . ?
O2 P1 C20 C21 12.1(10) . . . . ?
C10 P1 C20 C21 132.7(9) . . . . ?
C30 P1 C20 C21 -110.0(10) . . . . ?
O2 P1 C20 C25 -166.9(9) . . . . ?
C10 P1 C20 C25 -46.3(10) . . . . ?
C30 P1 C20 C25 71.0(10) . . . . ?
C25 C20 C21 C22 -3.4(18) . . . . ?
P1 C20 C21 C22 177.6(10) . . . . ?
C20 C21 C22 C23 2(2) . . . . ?
C21 C22 C23 C24 -1(2) . . . . ?
C22 C23 C24 C25 0(2) . . . . ?
C23 C24 C25 C20 -1.0(19) . . . . ?
C21 C20 C25 C24 2.6(17) . . . . ?
P1 C20 C25 C24 -178.4(9) . . . . ?
O2 P1 C30 C31 -112.9(11) . . . . ?
C10 P1 C30 C31 123.9(11) . . . . ?
C20 P1 C30 C31 7.9(12) . . . . ?
O2 P1 C30 C35 64.1(10) . . . . ?
C10 P1 C30 C35 -59.2(10) . . . . ?
C20 P1 C30 C35 -175.2(9) . . . . ?
C35 C30 C31 C32 -1(2) . . . . ?
P1 C30 C31 C32 176.0(11) . . . . ?
C30 C31 C32 C33 0(2) . . . . ?
C31 C32 C33 C34 0(3) . . . . ?
C32 C33 C34 C35 2(3) . . . . ?
C33 C34 C35 C30 -3(2) . . . . ?
C31 C30 C35 C34 3(2) . . . . ?
P1 C30 C35 C34 -174.5(11) . . . . ?
C93 C91 C92 C93 0(3) . . . 2_665 ?
C93 C91 C92 C97 -178(2) . . . . ?
C92 C91 C93 C92 0(3) . . . 2_665 ?

_refine_diff_density_max         1.577
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.161

_shelxl_version_number           2014/6


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene, Pentane'
_chemical_properties_physical    'Air-sensitive, Hygroscopic, Oxygen-sensitive'