# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_twin5
_database_code_depnum_ccdc_archive 'CCDC 2346841'
loop_
_audit_author_name
_audit_author_address
'Christopher Ye'
;UC Berkeley
United States of America
;
_audit_update_record             
;
2024-04-08 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 Os4 Th'
_chemical_formula_weight         1533.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
H H 0.0000 0.0000
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
Os Os -1.2848 7.9466
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
Th Th -7.9004 9.3112
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   23.163(2)
_cell_length_b                   12.6413(11)
_cell_length_c                   15.7810(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.796(3)
_cell_angle_gamma                90
_cell_volume                     4618.6(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0921
_cell_measurement_theta_min      2.2853
_shelx_estimated_absorpt_T_max   0.864
_shelx_estimated_absorpt_T_min   0.520
_exptl_absorpt_coefficient_mu    15.063
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11258
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         29.119
_diffrn_reflns_theta_min         1.882
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker D8 with PHOTONII detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9690
_reflns_number_total             11258
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT v8.40a'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'Bruker SAINT v8.40a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.774
_refine_diff_density_min         -2.363
_refine_diff_density_rms         0.391
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         11258
_refine_ls_number_restraints     206
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0387
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0351P)²+24.6766P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0862
_refine_special_details          
;
 Several crystals were tried and this was the best crystal. The diffraction
 pattern showed twinning. Using Cell_now two orientation matrices were
 determined, the relationship between these components was determined to be
 180 degrees about reciprocal axis 0 0 1.  The data were integrated using the
 two matrices in SAINT, TWINABS was used to produce a merged HKLF4 file,
 for structure solution and refinement along with an HKLF5 for
 structure refinement. The HKLF5 file contained the merged reflections first
 component and those that overlapped with this component, which were split
 into 2 reflection. TWINABS indicated the twin faction to be 51:49 The structure
 was solved and refined using the HKLF4 file, the final refinement was done on
 the HKLF5 file.

 All non-hydrogen atoms were refined anisotropically. Hydrogen
 atoms were found in the rotational fourier map on the carbon atoms
 constrained and refined using a riding model. Displacement parameter
 restraints were used in modelling the Cp* groups.

 Refined as a 2-component twin.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Dual space'
_atom_sites_solution_secondary   difmap
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
Th1 Th 0.74944(2) 0.49712(3) 0.18454(3) 0.00891(7) Uani 1 1 d . . . . .
Os1 Os 0.82262(2) 0.64022(3) 0.07840(3) 0.01075(9) Uani 1 1 d . . . . .
C1 C 0.8930(5) 0.6555(8) -0.0134(6) 0.0143(18) Uani 1 1 d . U . . .
C2 C 0.9110(5) 0.7012(8) 0.0669(6) 0.0166(19) Uani 1 1 d . U . . .
C3 C 0.8738(4) 0.7890(8) 0.0816(7) 0.0135(17) Uani 1 1 d . U . . .
C4 C 0.8337(5) 0.7979(8) 0.0112(6) 0.0152(19) Uani 1 1 d . U . . .
C5 C 0.8457(5) 0.7148(8) -0.0487(7) 0.0163(18) Uani 1 1 d . U . . .
C6 C 0.9245(5) 0.5670(9) -0.0588(8) 0.026(3) Uani 1 1 d . U . . .
H6A H 0.896705 0.526261 -0.093692 0.039 Uiso 1 1 calc R U . . .
H6B H 0.943316 0.520206 -0.016821 0.039 Uiso 1 1 calc R U . . .
H6C H 0.953728 0.597638 -0.095102 0.039 Uiso 1 1 calc R U . . .
C7 C 0.9634(5) 0.6691(10) 0.1184(8) 0.031(3) Uani 1 1 d . U . . .
H7A H 0.996780 0.710178 0.100545 0.047 Uiso 1 1 calc R U . . .
H7B H 0.970867 0.593566 0.109975 0.047 Uiso 1 1 calc R U . . .
H7C H 0.956950 0.682485 0.178570 0.047 Uiso 1 1 calc R U . . .
C8 C 0.8797(5) 0.8661(9) 0.1544(8) 0.026(3) Uani 1 1 d . U . . .
H8A H 0.901292 0.928365 0.136461 0.040 Uiso 1 1 calc R U . . .
H8B H 0.900321 0.832089 0.202250 0.040 Uiso 1 1 calc R U . . .
H8C H 0.841189 0.887758 0.171789 0.040 Uiso 1 1 calc R U . . .
C9 C 0.7886(5) 0.8836(9) -0.0012(7) 0.023(2) Uani 1 1 d . U . . .
H9A H 0.781286 0.917127 0.053465 0.035 Uiso 1 1 calc R U . . .
H9B H 0.752688 0.852376 -0.024225 0.035 Uiso 1 1 calc R U . . .
H9C H 0.802543 0.936860 -0.040749 0.035 Uiso 1 1 calc R U . . .
C10 C 0.8166(5) 0.7020(10) -0.1330(6) 0.025(3) Uani 1 1 d . U . . .
H10A H 0.837839 0.741377 -0.175435 0.037 Uiso 1 1 calc R U . . .
H10B H 0.777004 0.729201 -0.131083 0.037 Uiso 1 1 calc R U . . .
H10C H 0.815562 0.626827 -0.148251 0.037 Uiso 1 1 calc R U . . .
Os2 Os 0.66104(2) 0.62391(3) 0.28010(3) 0.01192(9) Uani 1 1 d . . . . .
C11 C 0.6271(4) 0.7343(8) 0.3841(6) 0.015(2) Uani 1 1 d . U . . .
C12 C 0.6206(5) 0.7846(8) 0.3038(7) 0.022(3) Uani 1 1 d . . . . .
C13 C 0.5826(5) 0.7207(10) 0.2513(7) 0.027(3) Uani 1 1 d . . . . .
C14 C 0.5686(5) 0.6288(9) 0.2989(8) 0.025(3) Uani 1 1 d . . . . .
C15 C 0.5961(5) 0.6351(9) 0.3814(7) 0.021(2) Uani 1 1 d . . . . .
C16 C 0.6568(5) 0.7809(10) 0.4616(7) 0.031(3) Uani 1 1 d . . . . .
H16A H 0.694368 0.809724 0.446368 0.046 Uiso 1 1 calc R U . . .
H16B H 0.662537 0.725693 0.504670 0.046 Uiso 1 1 calc R U . . .
H16C H 0.632917 0.837579 0.484265 0.046 Uiso 1 1 calc R U . . .
C17 C 0.6446(6) 0.8899(9) 0.2800(10) 0.042(4) Uani 1 1 d . . . . .
H17A H 0.614726 0.944228 0.285058 0.064 Uiso 1 1 calc R U . . .
H17B H 0.657332 0.887431 0.221392 0.064 Uiso 1 1 calc R U . . .
H17C H 0.677566 0.907155 0.317994 0.064 Uiso 1 1 calc R U . . .
C18 C 0.5591(6) 0.7503(12) 0.1652(7) 0.038(3) Uani 1 1 d . . . . .
H18A H 0.555891 0.686810 0.129690 0.057 Uiso 1 1 calc R U . . .
H18B H 0.585189 0.801029 0.139112 0.057 Uiso 1 1 calc R U . . .
H18C H 0.520884 0.782441 0.170244 0.057 Uiso 1 1 calc R U . . .
C19 C 0.5247(5) 0.5445(10) 0.2719(10) 0.039(3) Uani 1 1 d . . . . .
H19A H 0.485683 0.569561 0.283328 0.059 Uiso 1 1 calc R U . . .
H19B H 0.532527 0.479349 0.303889 0.059 Uiso 1 1 calc R U . . .
H19C H 0.527744 0.530427 0.211146 0.059 Uiso 1 1 calc R U . . .
C20 C 0.5850(6) 0.5632(10) 0.4545(8) 0.036(3) Uani 1 1 d . . . . .
H20A H 0.547230 0.579533 0.477481 0.053 Uiso 1 1 calc R U . . .
H20B H 0.615152 0.573394 0.498780 0.053 Uiso 1 1 calc R U . . .
H20C H 0.585455 0.489529 0.435184 0.053 Uiso 1 1 calc R U . . .
Os3 Os 0.67650(2) 0.34728(3) 0.07763(3) 0.01105(8) Uani 1 1 d . . . . .
C21 C 0.6670(4) 0.1934(8) 0.0033(6) 0.014(2) Uani 1 1 d . . . . .
C22 C 0.6500(4) 0.2808(8) -0.0521(6) 0.014(2) Uani 1 1 d . . . . .
C23 C 0.6037(5) 0.3330(9) -0.0158(7) 0.021(2) Uani 1 1 d . . . . .
C24 C 0.5877(4) 0.2808(8) 0.0620(7) 0.019(2) Uani 1 1 d . . . . .
C25 C 0.6294(4) 0.1930(8) 0.0738(7) 0.017(2) Uani 1 1 d . . . . .
C26 C 0.7128(5) 0.1131(9) -0.0146(7) 0.024(3) Uani 1 1 d . . . . .
H26A H 0.729562 0.086445 0.039065 0.035 Uiso 1 1 calc R U . . .
H26B H 0.743165 0.146294 -0.047413 0.035 Uiso 1 1 calc R U . . .
H26C H 0.695701 0.054315 -0.047071 0.035 Uiso 1 1 calc R U . . .
C27 C 0.6739(5) 0.3035(9) -0.1369(6) 0.022(2) Uani 1 1 d . . . . .
H27A H 0.653577 0.260488 -0.180006 0.033 Uiso 1 1 calc R U . . .
H27B H 0.715133 0.286404 -0.135974 0.033 Uiso 1 1 calc R U . . .
H27C H 0.668533 0.378660 -0.150310 0.033 Uiso 1 1 calc R U . . .
C28 C 0.5678(5) 0.4250(10) -0.0543(9) 0.034(3) Uani 1 1 d . . . . .
H28A H 0.592727 0.470293 -0.087793 0.051 Uiso 1 1 calc R U . . .
H28B H 0.551220 0.466616 -0.008665 0.051 Uiso 1 1 calc R U . . .
H28C H 0.536584 0.396445 -0.090967 0.051 Uiso 1 1 calc R U . . .
C29 C 0.5375(5) 0.3021(11) 0.1151(9) 0.034(3) Uani 1 1 d . . . . .
H29A H 0.527487 0.377340 0.111587 0.051 Uiso 1 1 calc R U . . .
H29B H 0.547214 0.283500 0.174104 0.051 Uiso 1 1 calc R U . . .
H29C H 0.504518 0.259579 0.094725 0.051 Uiso 1 1 calc R U . . .
C30 C 0.6282(5) 0.1120(9) 0.1410(8) 0.026(3) Uani 1 1 d . . . . .
H30A H 0.600062 0.057127 0.124978 0.039 Uiso 1 1 calc R U . . .
H30B H 0.617135 0.145064 0.194280 0.039 Uiso 1 1 calc R U . . .
H30C H 0.666595 0.080185 0.148414 0.039 Uiso 1 1 calc R U . . .
Os4 Os 0.83785(2) 0.37815(3) 0.29316(3) 0.01256(9) Uani 1 1 d . . . . .
C31 C 0.8688(5) 0.2478(9) 0.3875(7) 0.022(2) Uani 1 1 d . U . . .
C32 C 0.8897(5) 0.2304(8) 0.3032(7) 0.0183(19) Uani 1 1 d . U . . .
C33 C 0.9253(4) 0.3173(9) 0.2814(7) 0.021(2) Uani 1 1 d . U . . .
C34 C 0.9263(5) 0.3893(9) 0.3529(8) 0.026(2) Uani 1 1 d . U . . .
C35 C 0.8908(5) 0.3454(10) 0.4152(8) 0.027(2) Uani 1 1 d . U . . .
C36 C 0.8333(5) 0.1718(10) 0.4365(9) 0.037(3) Uani 1 1 d . U . . .
H36A H 0.858951 0.124905 0.469911 0.056 Uiso 1 1 calc R U . . .
H36B H 0.809290 0.129446 0.397180 0.056 Uiso 1 1 calc R U . . .
H36C H 0.808549 0.211092 0.474639 0.056 Uiso 1 1 calc R U . . .
C37 C 0.8822(6) 0.1307(9) 0.2515(8) 0.032(3) Uani 1 1 d . U . . .
H37A H 0.888378 0.146381 0.191690 0.048 Uiso 1 1 calc R U . . .
H37B H 0.843002 0.103226 0.257846 0.048 Uiso 1 1 calc R U . . .
H37C H 0.910313 0.077647 0.271545 0.048 Uiso 1 1 calc R U . . .
C38 C 0.9602(5) 0.3280(11) 0.2047(8) 0.036(3) Uani 1 1 d . U . . .
H38A H 0.999361 0.301339 0.216858 0.054 Uiso 1 1 calc R U . . .
H38B H 0.962168 0.402643 0.188289 0.054 Uiso 1 1 calc R U . . .
H38C H 0.942306 0.287005 0.158149 0.054 Uiso 1 1 calc R U . . .
C39 C 0.9626(6) 0.4912(11) 0.3640(10) 0.047(3) Uani 1 1 d . U . . .
H39A H 0.941099 0.543119 0.396565 0.070 Uiso 1 1 calc R U . . .
H39B H 0.970706 0.520560 0.308090 0.070 Uiso 1 1 calc R U . . .
H39C H 0.999096 0.474530 0.394187 0.070 Uiso 1 1 calc R U . . .
C40 C 0.8869(6) 0.3896(11) 0.5037(7) 0.040(3) Uani 1 1 d . U . . .
H40A H 0.922273 0.372579 0.536525 0.060 Uiso 1 1 calc R U . . .
H40B H 0.853601 0.358356 0.531334 0.060 Uiso 1 1 calc R U . . .
H40C H 0.882146 0.466576 0.500786 0.060 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
Th1 Os1 3.0214(5) . ?
Th1 Os2 3.0379(6) . ?
Th1 Os3 3.0183(6) . ?
Th1 Os4 3.0289(6) . ?
Os1 C1 2.223(10) . ?
Os1 C2 2.200(10) . ?
Os1 C3 2.223(9) . ?
Os1 C4 2.276(10) . ?
Os1 C5 2.295(10) . ?
C1 C2 1.442(14) . ?
C1 C5 1.427(15) . ?
C1 C6 1.528(14) . ?
C2 C3 1.428(14) . ?
C2 C7 1.496(15) . ?
C3 C4 1.431(14) . ?
C3 C8 1.509(15) . ?
C4 C5 1.446(14) . ?
C4 C9 1.514(15) . ?
C5 C10 1.481(14) . ?
Os2 C11 2.311(9) . ?
Os2 C12 2.273(10) . ?
Os2 C13 2.225(11) . ?
Os2 C14 2.173(11) . ?
Os2 C15 2.234(11) . ?
C11 C12 1.422(15) . ?
C11 C15 1.444(15) . ?
C11 C16 1.504(14) . ?
C12 C13 1.437(17) . ?
C12 C17 1.496(15) . ?
C13 C14 1.427(16) . ?
C13 C18 1.496(16) . ?
C14 C15 1.434(17) . ?
C14 C19 1.524(16) . ?
C15 C20 1.498(15) . ?
Os3 C21 2.279(10) . ?
Os3 C22 2.279(10) . ?
Os3 C23 2.213(10) . ?
Os3 C24 2.227(10) . ?
Os3 C25 2.235(10) . ?
C21 C22 1.455(14) . ?
C21 C25 1.434(14) . ?
C21 C26 1.502(15) . ?
C22 C23 1.398(15) . ?
C22 C27 1.492(14) . ?
C23 C24 1.451(16) . ?
C23 C28 1.543(16) . ?
C24 C25 1.480(15) . ?
C24 C29 1.480(15) . ?
C25 C30 1.474(15) . ?
Os4 C31 2.320(10) . ?
Os4 C32 2.224(10) . ?
Os4 C33 2.179(10) . ?
Os4 C34 2.233(11) . ?
Os4 C35 2.289(11) . ?
C31 C32 1.447(15) . ?
C31 C35 1.400(17) . ?
C31 C36 1.496(16) . ?
C32 C33 1.420(16) . ?
C32 C37 1.509(15) . ?
C33 C34 1.450(16) . ?
C33 C38 1.484(15) . ?
C34 C35 1.414(17) . ?
C34 C39 1.546(17) . ?
C35 C40 1.510(16) . ?

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
Os1 Th1 Os2 110.969(16) . . ?
Os1 Th1 Os4 103.291(17) . . ?
Os3 Th1 Os1 112.319(16) . . ?
Os3 Th1 Os2 103.557(17) . . ?
Os3 Th1 Os4 111.188(17) . . ?
Os4 Th1 Os2 115.805(16) . . ?
C1 Os1 Th1 148.1(3) . . ?
C1 Os1 C3 62.6(4) . . ?
C1 Os1 C4 61.6(4) . . ?
C1 Os1 C5 36.8(4) . . ?
C2 Os1 Th1 142.7(3) . . ?
C2 Os1 C1 38.0(4) . . ?
C2 Os1 C3 37.7(4) . . ?
C2 Os1 C4 62.4(4) . . ?
C2 Os1 C5 62.7(4) . . ?
C3 Os1 Th1 143.3(3) . . ?
C3 Os1 C4 37.1(4) . . ?
C3 Os1 C5 62.2(4) . . ?
C4 Os1 Th1 148.9(3) . . ?
C4 Os1 C5 36.9(4) . . ?
C5 Os1 Th1 151.7(3) . . ?
C2 C1 Os1 70.1(6) . . ?
C2 C1 C6 125.2(10) . . ?
C5 C1 Os1 74.3(6) . . ?
C5 C1 C2 109.3(9) . . ?
C5 C1 C6 125.0(10) . . ?
C6 C1 Os1 127.8(7) . . ?
C1 C2 Os1 71.8(6) . . ?
C1 C2 C7 125.2(10) . . ?
C3 C2 Os1 72.0(6) . . ?
C3 C2 C1 107.1(9) . . ?
C3 C2 C7 127.3(10) . . ?
C7 C2 Os1 127.0(8) . . ?
C2 C3 Os1 70.3(6) . . ?
C2 C3 C4 108.4(9) . . ?
C2 C3 C8 125.8(10) . . ?
C4 C3 Os1 73.5(6) . . ?
C4 C3 C8 125.5(9) . . ?
C8 C3 Os1 126.8(7) . . ?
C3 C4 Os1 69.4(5) . . ?
C3 C4 C5 108.5(9) . . ?
C3 C4 C9 125.9(10) . . ?
C5 C4 Os1 72.3(6) . . ?
C5 C4 C9 125.6(9) . . ?
C9 C4 Os1 126.8(7) . . ?
C1 C5 Os1 68.9(5) . . ?
C1 C5 C4 106.7(9) . . ?
C1 C5 C10 128.0(10) . . ?
C4 C5 Os1 70.9(6) . . ?
C4 C5 C10 125.1(10) . . ?
C10 C5 Os1 128.9(7) . . ?
C11 Os2 Th1 157.0(3) . . ?
C12 Os2 Th1 147.3(3) . . ?
C12 Os2 C11 36.1(4) . . ?
C13 Os2 Th1 138.3(3) . . ?
C13 Os2 C11 61.3(4) . . ?
C13 Os2 C12 37.2(4) . . ?
C13 Os2 C15 63.1(4) . . ?
C14 Os2 Th1 140.0(3) . . ?
C14 Os2 C11 61.8(4) . . ?
C14 Os2 C12 62.5(4) . . ?
C14 Os2 C13 37.8(4) . . ?
C14 Os2 C15 38.0(4) . . ?
C15 Os2 Th1 150.3(3) . . ?
C15 Os2 C11 37.0(4) . . ?
C15 Os2 C12 62.3(4) . . ?
C12 C11 Os2 70.5(5) . . ?
C12 C11 C15 108.8(9) . . ?
C12 C11 C16 125.7(10) . . ?
C15 C11 Os2 68.6(6) . . ?
C15 C11 C16 125.3(10) . . ?
C16 C11 Os2 131.0(7) . . ?
C11 C12 Os2 73.4(5) . . ?
C11 C12 C13 108.0(9) . . ?
C11 C12 C17 126.3(11) . . ?
C13 C12 Os2 69.6(6) . . ?
C13 C12 C17 125.5(11) . . ?
C17 C12 Os2 126.5(8) . . ?
C12 C13 Os2 73.2(6) . . ?
C12 C13 C18 125.6(12) . . ?
C14 C13 Os2 69.1(6) . . ?
C14 C13 C12 107.4(10) . . ?
C14 C13 C18 126.9(13) . . ?
C18 C13 Os2 126.5(8) . . ?
C13 C14 Os2 73.1(7) . . ?
C13 C14 C15 109.3(10) . . ?
C13 C14 C19 125.7(12) . . ?
C15 C14 Os2 73.3(6) . . ?
C15 C14 C19 124.5(11) . . ?
C19 C14 Os2 126.4(8) . . ?
C11 C15 Os2 74.4(6) . . ?
C11 C15 C20 127.0(11) . . ?
C14 C15 Os2 68.7(6) . . ?
C14 C15 C11 106.4(9) . . ?
C14 C15 C20 125.7(11) . . ?
C20 C15 Os2 130.4(8) . . ?
C21 Os3 Th1 150.1(3) . . ?
C22 Os3 Th1 149.7(2) . . ?
C22 Os3 C21 37.2(3) . . ?
C23 Os3 Th1 145.6(3) . . ?
C23 Os3 C21 61.8(4) . . ?
C23 Os3 C22 36.2(4) . . ?
C23 Os3 C24 38.1(4) . . ?
C23 Os3 C25 63.2(4) . . ?
C24 Os3 Th1 142.9(3) . . ?
C24 Os3 C21 63.1(4) . . ?
C24 Os3 C22 62.6(4) . . ?
C24 Os3 C25 38.7(4) . . ?
C25 Os3 Th1 145.8(3) . . ?
C25 Os3 C21 37.0(4) . . ?
C25 Os3 C22 62.4(4) . . ?
C22 C21 Os3 71.4(5) . . ?
C22 C21 C26 125.5(10) . . ?
C25 C21 Os3 69.8(5) . . ?
C25 C21 C22 108.0(9) . . ?
C25 C21 C26 126.4(10) . . ?
C26 C21 Os3 128.0(7) . . ?
C21 C22 Os3 71.4(5) . . ?
C21 C22 C27 125.7(10) . . ?
C23 C22 Os3 69.3(6) . . ?
C23 C22 C21 108.0(9) . . ?
C23 C22 C27 126.0(10) . . ?
C27 C22 Os3 129.6(7) . . ?
C22 C23 Os3 74.5(6) . . ?
C22 C23 C24 110.5(10) . . ?
C22 C23 C28 127.3(11) . . ?
C24 C23 Os3 71.5(6) . . ?
C24 C23 C28 121.9(11) . . ?
C28 C23 Os3 126.2(8) . . ?
C23 C24 Os3 70.4(6) . . ?
C23 C24 C25 105.4(9) . . ?
C23 C24 C29 128.4(11) . . ?
C25 C24 Os3 70.9(5) . . ?
C25 C24 C29 125.9(10) . . ?
C29 C24 Os3 127.4(8) . . ?
C21 C25 Os3 73.2(6) . . ?
C21 C25 C24 108.0(9) . . ?
C21 C25 C30 125.9(10) . . ?
C24 C25 Os3 70.4(5) . . ?
C30 C25 Os3 127.3(7) . . ?
C30 C25 C24 125.8(10) . . ?
C31 Os4 Th1 155.0(3) . . ?
C32 Os4 Th1 144.3(3) . . ?
C32 Os4 C31 37.1(4) . . ?
C32 Os4 C34 62.4(4) . . ?
C32 Os4 C35 60.9(4) . . ?
C33 Os4 Th1 137.8(3) . . ?
C33 Os4 C31 62.3(4) . . ?
C33 Os4 C32 37.6(4) . . ?
C33 Os4 C34 38.3(4) . . ?
C33 Os4 C35 62.2(4) . . ?
C34 Os4 Th1 143.4(3) . . ?
C34 Os4 C31 60.8(4) . . ?
C34 Os4 C35 36.4(4) . . ?
C35 Os4 Th1 154.3(3) . . ?
C35 Os4 C31 35.4(4) . . ?
C32 C31 Os4 67.9(5) . . ?
C32 C31 C36 125.7(11) . . ?
C35 C31 Os4 71.1(6) . . ?
C35 C31 C32 106.9(10) . . ?
C35 C31 C36 127.3(11) . . ?
C36 C31 Os4 128.7(8) . . ?
C31 C32 Os4 75.1(6) . . ?
C31 C32 C37 125.9(10) . . ?
C33 C32 Os4 69.5(6) . . ?
C33 C32 C31 108.6(10) . . ?
C33 C32 C37 125.0(10) . . ?
C37 C32 Os4 127.6(8) . . ?
C32 C33 Os4 72.9(6) . . ?
C32 C33 C34 107.0(10) . . ?
C32 C33 C38 127.1(11) . . ?
C34 C33 Os4 72.8(6) . . ?
C34 C33 C38 125.6(11) . . ?
C38 C33 Os4 124.7(8) . . ?
C33 C34 Os4 68.8(6) . . ?
C33 C34 C39 127.3(12) . . ?
C35 C34 Os4 73.9(7) . . ?
C35 C34 C33 107.4(10) . . ?
C35 C34 C39 125.1(12) . . ?
C39 C34 Os4 126.1(8) . . ?
C31 C35 Os4 73.5(6) . . ?
C31 C35 C34 110.0(10) . . ?
C31 C35 C40 125.7(12) . . ?
C34 C35 Os4 69.7(6) . . ?
C34 C35 C40 123.5(12) . . ?
C40 C35 Os4 131.7(7) . . ?

_vrf_PLAT213_twin5               
;
PROBLEM: Atom C33             has ADP max/min Ratio .....        4.8 oblate
RESPONSE: Displacement restraints were used in modelling some of the Cp* groups. 
 The difference map contained artifact peaks due not being able to model the
 twinning perfectly. These peaks interfered with some of the Cp* carbon atoms
 displacement parameters.
;
####################################################################### 
# 
# 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_czy_ii_3-th
_database_code_depnum_ccdc_archive 'CCDC 2346844'
loop_
_audit_author_name
_audit_author_address
'Christopher Ye'
;UC Berkeley
United States of America
;
_audit_update_record             
;
2024-04-08 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_audit_creation_date             2024-03-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H59 Os4 Th, C6 H14'
_chemical_formula_sum            'C46 H73 Os4 Th'
_chemical_formula_weight         1618.88
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Th Os C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   18.6052(5)
_cell_length_b                   9.9998(3)
_cell_length_c                   13.3830(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2489.88(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15674
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.6960
_cell_measurement_theta_min      3.3370
_shelx_estimated_absorpt_T_max   0.559
_shelx_estimated_absorpt_T_min   0.178
_exptl_absorpt_coefficient_mu    13.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1486
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27906
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         2.991
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     40.00  87.00   0.50    2.34    --    8.14-179.00-180.00   94
  2  ω     40.00  71.00   0.50    2.34    --    8.14-179.00 -30.00   62
  3  ω    -60.00 -23.00   0.50    2.34    --    8.14   0.00-150.00   74
  4  ω    -18.00  16.00   0.50    2.34    --    8.14   0.00-150.00   68
  5  ω      0.00  37.00   0.50    2.34    --    8.14  77.00  90.00   74
  6  ω    -14.00  14.00   0.50    2.34    --   -7.82  29.00  14.00   56
  7  ω    -40.00  12.00   0.50    2.34    --   -7.82 -77.00-120.00  104
  8  ω    -29.00  -4.00   0.50    2.34    --   -7.82 -95.00  73.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0059482000
_diffrn_orient_matrix_UB_12      0.0565539000
_diffrn_orient_matrix_UB_13      0.0309499000
_diffrn_orient_matrix_UB_21      -0.0131306000
_diffrn_orient_matrix_UB_22      0.0424370000
_diffrn_orient_matrix_UB_23      -0.0383205000
_diffrn_orient_matrix_UB_31      -0.0352863000
_diffrn_orient_matrix_UB_32      -0.0063326000
_diffrn_orient_matrix_UB_33      0.0194723000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.854
_reflns_number_gt                6851
_reflns_number_total             7260
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.132
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 
;
 Flack x determined using 2863 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         7260
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0216
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0249P)²+0.4399P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0470
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C28 \\sim C27 \\sim C26 \\sim C25 \\sim C24 \\sim C23: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C27) = Uanis(C28)
3. Others
 Sof(H7BD)=Sof(H7BE)=Sof(H1BC)=Sof(H1BD)=Sof(H1BE)=Sof(Th2)=0.5*(1-FVAR(2))
 Sof(Th1)=Sof(H7AC)=Sof(H7AB)=Sof(H7AA)=Sof(H1AA)=Sof(H1AB)=0.5*FVAR(2)
 Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C27(0.5) H27A(0.5)
 H27B(0.5) C26(0.5) H26A(0.5) H26B(0.5) C25(0.5) H25A(0.5) H25B(0.5) C24(0.5)
 H24A(0.5) H24B(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7BD,H7BE), C1(H1AA,H1AB), C27(H27A,H27B), C26(H26A,H26B), C25(H25A,H25B),
 C24(H24A,H24B)
4.b Me refined with riding coordinates:
 C7(H7AC,H7AB,H7AA), C1(H1BC,H1BD,H1BE), C28(H28A,H28B,H28C)
4.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C5(H5A,H5B,
 H5C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C6(H6A,
 H6B,H6C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Th1 Th 0.500000 0.42487(3) 0.50049(2) 0.01676(10) Uani 0.9206(15) 2 d S T P A 1
Os1 Os 0.500000 0.56343(3) 0.30556(2) 0.01546(7) Uani 1 2 d S T P A .
Os2 Os 0.500000 0.32122(3) 0.26980(3) 0.01654(7) Uani 1 2 d S T P A .
Os3 Os 0.35835(2) 0.34607(2) 0.59472(2) 0.02039(6) Uani 1 1 d . . . . .
C2 C 0.500000 0.7147(9) 0.4281(7) 0.0210(17) Uani 1 2 d S T P A .
C9 C 0.4378(3) 0.1340(6) 0.2704(5) 0.0231(12) Uani 1 1 d . . . . .
C10 C 0.4603(3) 0.1637(6) 0.1710(5) 0.0230(12) Uani 1 1 d . . . . .
C3 C 0.4377(3) 0.7325(6) 0.3665(5) 0.0192(11) Uani 1 1 d . . . . .
C4 C 0.4611(3) 0.7636(5) 0.2665(5) 0.0202(11) Uani 1 1 d . . . . .
C16 C 0.2401(3) 0.3894(7) 0.6110(5) 0.0259(13) Uani 1 1 d . . . . .
C7 C 0.500000 0.0631(9) 0.4370(7) 0.028(2) Uani 1 2 d S T P . .
H7AC H 0.549431 0.060059 0.462153 0.041 Uiso 0.4603(8) 1 calc R U P A 1
H7AB H 0.471147 0.122217 0.479417 0.041 Uiso 0.4603(8) 1 calc R U P A 1
H7AA H 0.479422 -0.027095 0.437946 0.041 Uiso 0.4603(8) 1 calc R U P A 1
H7BD H 0.544128 0.014610 0.456845 0.033 Uiso 0.0397(8) 1 calc R U P A 2
H7BE H 0.455872 0.014610 0.456845 0.033 Uiso 0.0397(8) 1 calc R U P A 2
C17 C 0.2730(4) 0.3981(8) 0.7063(5) 0.0271(14) Uani 1 1 d . . . . .
C8 C 0.500000 0.1152(9) 0.3323(7) 0.0222(18) Uani 1 2 d S T P A .
C15 C 0.2479(3) 0.2568(8) 0.5741(5) 0.0281(14) Uani 1 1 d . . . . .
C22 C 0.2725(4) 0.5159(8) 0.7737(6) 0.0391(17) Uani 1 1 d . . . . .
H22A H 0.316287 0.516070 0.814370 0.059 Uiso 1 1 calc R U . . .
H22B H 0.230335 0.511561 0.817486 0.059 Uiso 1 1 calc R U . . .
H22C H 0.270494 0.597931 0.733716 0.059 Uiso 1 1 calc R U . . .
C21 C 0.1970(4) 0.4993(9) 0.5647(5) 0.0385(18) Uani 1 1 d . . . . .
H21A H 0.224168 0.583111 0.568083 0.058 Uiso 1 1 calc R U . . .
H21B H 0.151578 0.509478 0.601071 0.058 Uiso 1 1 calc R U . . .
H21C H 0.186948 0.477366 0.494743 0.058 Uiso 1 1 calc R U . . .
C11 C 0.3614(3) 0.1190(8) 0.3049(6) 0.0321(15) Uani 1 1 d . . . . .
H11A H 0.357843 0.144662 0.375349 0.048 Uiso 1 1 calc R U . . .
H11B H 0.346328 0.025696 0.296983 0.048 Uiso 1 1 calc R U . . .
H11C H 0.330209 0.176840 0.264690 0.048 Uiso 1 1 calc R U . . .
C5 C 0.3616(3) 0.7321(7) 0.4024(6) 0.0292(15) Uani 1 1 d . . . . .
H5A H 0.329226 0.719746 0.345382 0.044 Uiso 1 1 calc R U . . .
H5B H 0.350965 0.817424 0.435154 0.044 Uiso 1 1 calc R U . . .
H5C H 0.354873 0.658800 0.450045 0.044 Uiso 1 1 calc R U . . .
C13 C 0.3014(3) 0.2663(8) 0.7301(5) 0.0274(14) Uani 1 1 d . . . . .
C1 C 0.500000 0.6738(10) 0.5356(7) 0.0260(19) Uani 1 2 d S T P . .
H1BC H 0.450391 0.668986 0.559991 0.039 Uiso 0.0397(8) 1 calc R U P A 2
H1BD H 0.522843 0.586002 0.542408 0.039 Uiso 0.0397(8) 1 calc R U P A 2
H1BE H 0.526766 0.739808 0.574997 0.039 Uiso 0.0397(8) 1 calc R U P A 2
H1AA H 0.456363 0.703642 0.571652 0.031 Uiso 0.4603(8) 1 calc R U P A 1
H1AB H 0.543637 0.703642 0.571652 0.031 Uiso 0.4603(8) 1 calc R U P A 1
C20 C 0.2148(4) 0.2016(9) 0.4791(5) 0.0375(18) Uani 1 1 d . . . . .
H20A H 0.208327 0.274239 0.430746 0.056 Uiso 1 1 calc R U . . .
H20B H 0.168098 0.161370 0.494455 0.056 Uiso 1 1 calc R U . . .
H20C H 0.246701 0.133495 0.450587 0.056 Uiso 1 1 calc R U . . .
C18 C 0.3338(4) 0.2261(10) 0.8285(5) 0.043(2) Uani 1 1 d . . . . .
H18A H 0.367028 0.151268 0.818225 0.064 Uiso 1 1 calc R U . . .
H18B H 0.295559 0.198741 0.874521 0.064 Uiso 1 1 calc R U . . .
H18C H 0.360030 0.302070 0.857057 0.064 Uiso 1 1 calc R U . . .
C12 C 0.4144(4) 0.1791(7) 0.0808(6) 0.0330(15) Uani 1 1 d . . . . .
H12A H 0.437548 0.240800 0.033868 0.050 Uiso 1 1 calc R U . . .
H12B H 0.367417 0.214805 0.100324 0.050 Uiso 1 1 calc R U . . .
H12C H 0.408029 0.091800 0.048706 0.050 Uiso 1 1 calc R U . . .
C14 C 0.2855(3) 0.1800(7) 0.6474(5) 0.0277(14) Uani 1 1 d . . . . .
C6 C 0.4152(4) 0.7989(7) 0.1791(5) 0.0274(14) Uani 1 1 d . . . . .
H6A H 0.416122 0.895974 0.168953 0.041 Uiso 1 1 calc R U . . .
H6B H 0.365764 0.769807 0.191553 0.041 Uiso 1 1 calc R U . . .
H6C H 0.433722 0.754190 0.119183 0.041 Uiso 1 1 calc R U . . .
C19 C 0.2984(5) 0.0311(8) 0.6426(7) 0.047(2) Uani 1 1 d . . . . .
H19A H 0.318961 0.007879 0.577464 0.070 Uiso 1 1 calc R U . . .
H19B H 0.252660 -0.016218 0.651485 0.070 Uiso 1 1 calc R U . . .
H19C H 0.331778 0.004832 0.695687 0.070 Uiso 1 1 calc R U . . .
Th2 Th 0.500000 0.3300(4) 0.4797(3) 0.0185(13) Uani 0.0794(15) 2 d S T P A 2
C28 C 0.498(4) 1.018(2) 0.728(2) 0.091(6) Uani 0.5 1 d . U P B -3
H28A H 0.536431 1.064546 0.691710 0.137 Uiso 0.5 1 calc R U P B -3
H28B H 0.460485 0.990737 0.681205 0.137 Uiso 0.5 1 calc R U P B -3
H28C H 0.477477 1.079008 0.778112 0.137 Uiso 0.5 1 calc R U P B -3
C27 C 0.5291(12) 0.894(3) 0.781(3) 0.091(6) Uani 0.5 1 d . U P B -3
H27A H 0.550258 0.832673 0.730895 0.109 Uiso 0.5 1 calc R U P B -3
H27B H 0.567313 0.921269 0.828159 0.109 Uiso 0.5 1 calc R U P B -3
C26 C 0.4707(14) 0.828(3) 0.834(3) 0.092(9) Uani 0.5 1 d . U P B -3
H26A H 0.432600 0.808040 0.784703 0.110 Uiso 0.5 1 calc R U P B -3
H26B H 0.450288 0.894139 0.881583 0.110 Uiso 0.5 1 calc R U P B -3
C25 C 0.4848(16) 0.704(2) 0.8907(17) 0.071(9) Uani 0.5 1 d . U P B -3
H25A H 0.524096 0.722661 0.938719 0.085 Uiso 0.5 1 calc R U P B -3
H25B H 0.441345 0.683101 0.930350 0.085 Uiso 0.5 1 calc R U P B -3
C24 C 0.504(3) 0.5874(17) 0.8352(16) 0.067(6) Uani 0.5 1 d . U P B -3
H24A H 0.551869 0.601996 0.805244 0.080 Uiso 0.5 1 calc R U P B -3
H24B H 0.469177 0.577102 0.779680 0.080 Uiso 0.5 1 calc R U P B -3
C23 C 0.506(3) 0.4580(19) 0.893(2) 0.084(9) Uani 0.5 1 d . U P B -3
H23A H 0.474896 0.391911 0.860473 0.125 Uiso 0.5 1 calc R U P B -3
H23B H 0.488636 0.473731 0.961452 0.125 Uiso 0.5 1 calc R U P B -3
H23C H 0.555279 0.424279 0.895495 0.125 Uiso 0.5 1 calc R U P B -3


_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
Th1 Os1 2.9539(4) . ?
Th1 Os2 3.2567(5) . ?
Th1 Os3 3.0260(3) . ?
Th1 Os3 3.0259(3) 4_655 ?
Th1 C2 3.055(9) . ?
Th1 C1 2.534(10) . ?
Th1 H1BD 1.758(10) 4_655 ?
Os1 Os2 2.4689(4) . ?
Os1 C2 2.231(9) . ?
Os1 C3 2.206(6) . ?
Os1 C3 2.206(6) 4_655 ?
Os1 C4 2.192(6) 4_655 ?
Os1 C4 2.192(6) . ?
Os1 Th2 3.299(4) . ?
Os2 C9 2.200(6) 4_655 ?
Os2 C9 2.201(6) . ?
Os2 C10 2.185(6) . ?
Os2 C10 2.185(6) 4_655 ?
Os2 C8 2.224(9) . ?
Os2 Th2 2.810(4) . ?
Os3 C16 2.254(6) . ?
Os3 C17 2.241(6) . ?
Os3 C15 2.257(6) . ?
Os3 C13 2.245(6) . ?
Os3 C14 2.256(6) . ?
Os3 Th2 3.0563(19) . ?
C2 C3 1.434(8) 4_655 ?
C2 C3 1.434(8) . ?
C2 C1 1.496(14) . ?
C9 C10 1.426(9) . ?
C9 C8 1.435(8) . ?
C9 C11 1.502(8) . ?
C10 C10 1.478(13) 4_655 ?
C10 C12 1.486(9) . ?
C3 C4 1.440(9) . ?
C3 C5 1.494(8) . ?
C4 C4 1.447(11) 4_655 ?
C4 C6 1.491(9) . ?
C16 C17 1.419(9) . ?
C16 C15 1.422(10) . ?
C16 C21 1.494(10) . ?
C7 H7AC 0.9800 4_655 ?
C7 H7AC 0.9800 . ?
C7 H7AB 0.9800 4_655 ?
C7 H7AB 0.9800 . ?
C7 H7AA 0.9800 4_655 ?
C7 H7AA 0.9800 . ?
C7 H7BD 0.9900 . ?
C7 H7BE 0.9900 . ?
C7 C8 1.494(13) . ?
C7 Th2 2.729(10) . ?
C17 C22 1.484(10) . ?
C17 C13 1.455(10) . ?
C8 Th2 2.917(9) . ?
C15 C20 1.517(9) . ?
C15 C14 1.429(10) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C13 C18 1.504(9) . ?
C13 C14 1.434(10) . ?
C1 H1BC 0.9799 4_655 ?
C1 H1BC 0.9800 . ?
C1 H1BD 0.9800 . ?
C1 H1BD 0.9800 4_655 ?
C1 H1BE 0.9800 . ?
C1 H1BE 0.9800 4_655 ?
C1 H1AA 0.9900 . ?
C1 H1AB 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 C19 1.510(10) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 C27 1.54(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.46(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C25 1.48(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.43(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.51(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
Os1 Th1 Os2 46.532(10) . . ?
Os1 Th1 Os3 119.354(7) . . ?
Os1 Th1 Os3 119.355(7) . 4_655 ?
Os1 Th1 C2 43.54(17) . . ?
Os1 Th1 H1BD 81.5(3) . 4_655 ?
Os2 Th1 H1BD 126.5(3) . 4_655 ?
Os3 Th1 Os2 108.192(9) 4_655 . ?
Os3 Th1 Os2 108.192(9) . . ?
Os3 Th1 Os3 121.132(14) 4_655 . ?
Os3 Th1 C2 112.28(6) 4_655 . ?
Os3 Th1 C2 112.28(6) . . ?
Os3 Th1 H1BD 83.98(17) . 4_655 ?
Os3 Th1 H1BD 108.43(18) 4_655 4_655 ?
C2 Th1 Os2 90.07(17) . . ?
C2 Th1 H1BD 39.8(3) . 4_655 ?
C1 Th1 Os1 72.7(2) . . ?
C1 Th1 Os2 119.3(2) . . ?
C1 Th1 Os3 100.28(10) . 4_655 ?
C1 Th1 Os3 100.28(11) . . ?
C1 Th1 C2 29.2(3) . . ?
C1 Th1 H1BD 16.32(10) . 4_655 ?
Os2 Os1 Th1 73.203(14) . . ?
Os2 Os1 Th2 56.13(7) . . ?
C2 Os1 Th1 70.7(2) . . ?
C2 Os1 Os2 143.9(2) . . ?
C2 Os1 Th2 87.7(2) . . ?
C3 Os1 Th1 91.90(16) . . ?
C3 Os1 Th1 91.90(16) 4_655 . ?
C3 Os1 Os2 145.45(15) 4_655 . ?
C3 Os1 Os2 145.45(15) . . ?
C3 Os1 C2 37.7(2) 4_655 . ?
C3 Os1 C2 37.7(2) . . ?
C3 Os1 C3 63.4(3) 4_655 . ?
C3 Os1 Th2 106.34(17) . . ?
C3 Os1 Th2 106.34(17) 4_655 . ?
C4 Os1 Th1 129.70(17) 4_655 . ?
C4 Os1 Th1 129.70(17) . . ?
C4 Os1 Os2 148.20(15) 4_655 . ?
C4 Os1 Os2 148.20(15) . . ?
C4 Os1 C2 63.6(3) 4_655 . ?
C4 Os1 C2 63.6(3) . . ?
C4 Os1 C3 38.2(2) 4_655 4_655 ?
C4 Os1 C3 64.0(2) 4_655 . ?
C4 Os1 C3 64.0(2) . 4_655 ?
C4 Os1 C3 38.2(2) . . ?
C4 Os1 C4 38.6(3) 4_655 . ?
C4 Os1 Th2 144.56(18) 4_655 . ?
C4 Os1 Th2 144.56(18) . . ?
Os1 Os2 Th1 60.265(12) . . ?
Os1 Os2 Th2 77.03(9) . . ?
C9 Os2 Th1 105.50(18) 4_655 . ?
C9 Os2 Th1 105.50(18) . . ?
C9 Os2 Os1 146.49(16) 4_655 . ?
C9 Os2 Os1 146.49(16) . . ?
C9 Os2 C9 63.4(3) 4_655 . ?
C9 Os2 C8 37.9(2) . . ?
C9 Os2 C8 37.9(2) 4_655 . ?
C9 Os2 Th2 91.3(2) . . ?
C9 Os2 Th2 91.3(2) 4_655 . ?
C10 Os2 Th1 143.42(17) 4_655 . ?
C10 Os2 Th1 143.42(17) . . ?
C10 Os2 Os1 145.53(17) . . ?
C10 Os2 Os1 145.53(17) 4_655 . ?
C10 Os2 C9 37.9(2) 4_655 4_655 ?
C10 Os2 C9 64.3(2) 4_655 . ?
C10 Os2 C9 64.3(2) . 4_655 ?
C10 Os2 C9 37.9(2) . . ?
C10 Os2 C10 39.5(3) . 4_655 ?
C10 Os2 C8 63.9(3) . . ?
C10 Os2 C8 63.9(3) 4_655 . ?
C10 Os2 Th2 128.85(18) 4_655 . ?
C10 Os2 Th2 128.85(18) . . ?
C8 Os2 Th1 86.5(2) . . ?
C8 Os2 Os1 146.7(2) . . ?
C8 Os2 Th2 69.7(2) . . ?
C16 Os3 Th1 147.22(18) . . ?
C16 Os3 C15 36.8(3) . . ?
C16 Os3 C14 61.6(2) . . ?
C16 Os3 Th2 154.27(18) . . ?
C17 Os3 Th1 146.55(19) . . ?
C17 Os3 C16 36.8(2) . . ?
C17 Os3 C15 61.9(2) . . ?
C17 Os3 C13 37.8(3) . . ?
C17 Os3 C14 62.4(3) . . ?
C17 Os3 Th2 163.50(19) . . ?
C15 Os3 Th1 147.64(15) . . ?
C15 Os3 Th2 134.63(17) . . ?
C13 Os3 Th1 147.12(16) . . ?
C13 Os3 C16 61.9(2) . . ?
C13 Os3 C15 61.9(2) . . ?
C13 Os3 C14 37.1(3) . . ?
C13 Os3 Th2 142.62(18) . . ?
C14 Os3 Th1 147.67(17) . . ?
C14 Os3 C15 36.9(2) . . ?
C14 Os3 Th2 129.54(18) . . ?
Os1 C2 Th1 65.8(2) . . ?
C3 C2 Th1 107.5(4) 4_655 . ?
C3 C2 Th1 107.5(4) . . ?
C3 C2 Os1 70.2(4) . . ?
C3 C2 Os1 70.2(4) 4_655 . ?
C3 C2 C3 107.9(8) 4_655 . ?
C3 C2 C1 126.0(4) 4_655 . ?
C3 C2 C1 126.0(4) . . ?
C1 C2 Th1 55.7(5) . . ?
C1 C2 Os1 121.5(6) . . ?
C10 C9 Os2 70.4(3) . . ?
C10 C9 C8 109.2(6) . . ?
C10 C9 C11 125.8(6) . . ?
C8 C9 Os2 71.9(4) . . ?
C8 C9 C11 124.9(7) . . ?
C11 C9 Os2 125.7(4) . . ?
C9 C10 Os2 71.6(4) . . ?
C9 C10 C10 107.1(4) . 4_655 ?
C9 C10 C12 127.7(6) . . ?
C10 C10 Os2 70.24(17) 4_655 . ?
C10 C10 C12 125.0(4) 4_655 . ?
C12 C10 Os2 127.7(4) . . ?
C2 C3 Os1 72.1(4) . . ?
C2 C3 C4 108.5(5) . . ?
C2 C3 C5 125.5(6) . . ?
C4 C3 Os1 70.3(3) . . ?
C4 C3 C5 125.8(6) . . ?
C5 C3 Os1 127.9(4) . . ?
C3 C4 Os1 71.4(3) . . ?
C3 C4 C4 107.6(3) . 4_655 ?
C3 C4 C6 127.4(5) . . ?
C4 C4 Os1 70.72(14) 4_655 . ?
C4 C4 C6 124.9(4) 4_655 . ?
C6 C4 Os1 126.3(4) . . ?
C17 C16 Os3 71.1(3) . . ?
C17 C16 C15 109.0(6) . . ?
C17 C16 C21 124.0(7) . . ?
C15 C16 Os3 71.7(3) . . ?
C15 C16 C21 126.7(6) . . ?
C21 C16 Os3 128.7(5) . . ?
H7AC C7 H7AC 139.6 . 4_655 ?
H7AC C7 H7AB 46.0 . 4_655 ?
H7AC C7 H7AB 109.5 . . ?
H7AC C7 H7AB 109.5 4_655 4_655 ?
H7AC C7 H7AA 66.4 . 4_655 ?
H7AC C7 H7AA 109.5 . . ?
H7AC C7 H7AA 109.5 4_655 4_655 ?
H7AB C7 H7AC 46.0 . 4_655 ?
H7AB C7 H7AB 66.4 . 4_655 ?
H7AB C7 H7AA 109.5 . . ?
H7AB C7 H7AA 109.5 4_655 4_655 ?
H7AB C7 H7AA 139.6 . 4_655 ?
H7AA C7 H7AC 66.4 . 4_655 ?
H7AA C7 H7AB 139.6 . 4_655 ?
H7AA C7 H7AA 46.0 . 4_655 ?
H7BD C7 H7BE 112.1 . . ?
C8 C7 H7AC 109.47(5) . 4_655 ?
C8 C7 H7AC 109.5 . . ?
C8 C7 H7AB 109.5 . . ?
C8 C7 H7AB 109.5(4) . 4_655 ?
C8 C7 H7AA 109.5(4) . 4_655 ?
C8 C7 H7AA 109.5 . . ?
C8 C7 H7BD 115.0 . . ?
C8 C7 H7BE 115.0 . . ?
C8 C7 Th2 81.7(5) . . ?
Th2 C7 H7BD 115.0 . . ?
Th2 C7 H7BE 115.0 . . ?
C16 C17 Os3 72.1(3) . . ?
C16 C17 C22 126.3(7) . . ?
C16 C17 C13 107.3(6) . . ?
C22 C17 Os3 126.4(5) . . ?
C13 C17 Os3 71.2(3) . . ?
C13 C17 C22 126.1(6) . . ?
Os2 C8 Th2 64.7(2) . . ?
C9 C8 Os2 70.2(4) . . ?
C9 C8 Os2 70.2(4) 4_655 . ?
C9 C8 C9 107.4(8) . 4_655 ?
C9 C8 C7 125.9(4) 4_655 . ?
C9 C8 C7 125.9(4) . . ?
C9 C8 Th2 107.1(4) 4_655 . ?
C9 C8 Th2 107.1(4) . . ?
C7 C8 Os2 132.5(6) . . ?
C7 C8 Th2 67.8(5) . . ?
C16 C15 Os3 71.5(4) . . ?
C16 C15 C20 126.1(6) . . ?
C16 C15 C14 108.2(6) . . ?
C20 C15 Os3 128.0(4) . . ?
C14 C15 Os3 71.5(3) . . ?
C14 C15 C20 125.4(7) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C17 C13 Os3 70.9(4) . . ?
C17 C13 C18 125.4(7) . . ?
C18 C13 Os3 127.8(5) . . ?
C14 C13 Os3 71.9(4) . . ?
C14 C13 C17 107.6(6) . . ?
C14 C13 C18 126.7(7) . . ?
Th1 C1 H1BC 90.75(7) . 4_655 ?
Th1 C1 H1BD 30.28(11) . 4_655 ?
Th1 C1 H1BE 139.57(14) . 4_655 ?
Th1 C1 H1AA 112.7 . . ?
Th1 C1 H1AB 112.7 . . ?
C2 C1 Th1 95.1(6) . . ?
C2 C1 H1BC 109.5 . . ?
C2 C1 H1BC 109.47(2) . 4_655 ?
C2 C1 H1BD 109.5 . . ?
C2 C1 H1BD 109.5(5) . 4_655 ?
C2 C1 H1BE 109.5 . . ?
C2 C1 H1BE 109.5(4) . 4_655 ?
C2 C1 H1AA 112.7 . . ?
C2 C1 H1AB 112.7 . . ?
H1BC C1 H1BD 109.5 . . ?
H1BC C1 H1BE 109.5 . . ?
H1BD C1 H1BE 109.5 . . ?
H1AA C1 H1BC 128.7 . 4_655 ?
H1AA C1 H1BD 82.5 . 4_655 ?
H1AA C1 H1BE 28.3 . 4_655 ?
H1AA C1 H1AB 110.2 . . ?
H1AB C1 H1BC 23.2 . 4_655 ?
H1AB C1 H1BD 125.5 . 4_655 ?
H1AB C1 H1BE 87.3 . 4_655 ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C14 Os3 71.6(4) . . ?
C15 C14 C13 107.9(6) . . ?
C15 C14 C19 125.3(7) . . ?
C13 C14 Os3 71.0(4) . . ?
C13 C14 C19 126.4(7) . . ?
C19 C14 Os3 128.1(5) . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Os1 Th2 H7AB 133.2(3) . 4_655 ?
Os2 Th2 Os1 46.84(6) . . ?
Os2 Th2 Os3 120.34(6) . 4_655 ?
Os2 Th2 Os3 120.34(6) . . ?
Os2 Th2 H7AB 88.2(3) . 4_655 ?
Os2 Th2 C8 45.65(19) . . ?
Os3 Th2 Os1 108.58(9) . . ?
Os3 Th2 Os1 108.58(9) 4_655 . ?
Os3 Th2 Os3 119.15(12) 4_655 . ?
Os3 Th2 H7AB 80.57(15) 4_655 4_655 ?
Os3 Th2 H7AB 105.51(19) . 4_655 ?
C7 Th2 Os1 122.9(2) . . ?
C7 Th2 Os2 76.1(2) . . ?
C7 Th2 Os3 99.03(13) . 4_655 ?
C7 Th2 Os3 99.03(13) . . ?
C7 Th2 H7AB 18.72(9) . 4_655 ?
C7 Th2 C8 30.5(3) . . ?
C8 Th2 Os1 92.5(2) . . ?
C8 Th2 Os3 112.30(11) . . ?
C8 Th2 Os3 112.30(11) . 4_655 ?
C8 Th2 H7AB 44.4(3) . 4_655 ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
C28 C27 H27A 110.1 . . ?
C28 C27 H27B 110.1 . . ?
H27A C27 H27B 108.4 . . ?
C26 C27 C28 108(3) . . ?
C26 C27 H27A 110.1 . . ?
C26 C27 H27B 110.1 . . ?
C27 C26 H26A 107.4 . . ?
C27 C26 H26B 107.4 . . ?
C27 C26 C25 120(2) . . ?
H26A C26 H26B 106.9 . . ?
C25 C26 H26A 107.4 . . ?
C25 C26 H26B 107.4 . . ?
C26 C25 H25A 107.9 . . ?
C26 C25 H25B 107.9 . . ?
H25A C25 H25B 107.2 . . ?
C24 C25 C26 118(2) . . ?
C24 C25 H25A 107.9 . . ?
C24 C25 H25B 107.9 . . ?
C25 C24 H24A 108.3 . . ?
C25 C24 H24B 108.3 . . ?
C25 C24 C23 116.1(18) . . ?
H24A C24 H24B 107.4 . . ?
C23 C24 H24A 108.3 . . ?
C23 C24 H24B 108.3 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 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
Th1 C2 C3 Os1 -55.2(3) . . . . ?
Th1 C2 C3 C4 -116.5(4) . . . . ?
Th1 C2 C3 C5 68.9(7) . . . . ?
Os1 C2 C3 C4 -61.3(4) . . . . ?
Os1 C2 C3 C5 124.2(6) . . . . ?
Os1 C2 C1 Th1 0.000(2) . . . . ?
Os1 C3 C4 C4 -61.84(15) . . . 4_655 ?
Os1 C3 C4 C6 122.0(6) . . . . ?
Os2 C9 C10 C10 61.66(16) . . . 4_655 ?
Os2 C9 C10 C12 -123.8(7) . . . . ?
Os2 C9 C8 C9 -60.6(6) . . . 4_655 ?
Os2 C9 C8 C7 128.7(8) . . . . ?
Os2 C9 C8 Th2 54.1(3) . . . . ?
Os3 C16 C17 C22 122.5(7) . . . . ?
Os3 C16 C17 C13 -62.9(4) . . . . ?
Os3 C16 C15 C20 -124.1(6) . . . . ?
Os3 C16 C15 C14 62.5(4) . . . . ?
Os3 C17 C13 C18 123.4(7) . . . . ?
Os3 C17 C13 C14 -63.0(4) . . . . ?
Os3 C15 C14 C13 62.1(4) . . . . ?
Os3 C15 C14 C19 -124.2(7) . . . . ?
Os3 C13 C14 C15 -62.4(4) . . . . ?
Os3 C13 C14 C19 123.9(7) . . . . ?
C2 C3 C4 Os1 62.4(5) . . . . ?
C2 C3 C4 C4 0.5(6) . . . 4_655 ?
C2 C3 C4 C6 -175.7(6) . . . . ?
C10 C9 C8 Os2 60.9(4) . . . . ?
C10 C9 C8 C9 0.3(9) . . . 4_655 ?
C10 C9 C8 C7 -170.4(8) . . . . ?
C10 C9 C8 Th2 115.0(5) . . . . ?
C3 C2 C3 Os1 60.4(6) 4_655 . . . ?
C3 C2 C3 C4 -0.9(9) 4_655 . . . ?
C3 C2 C3 C5 -175.4(4) 4_655 . . . ?
C3 C2 C1 Th1 -87.4(8) 4_655 . . . ?
C3 C2 C1 Th1 87.4(8) . . . . ?
C16 C17 C13 Os3 63.5(4) . . . . ?
C16 C17 C13 C18 -173.2(6) . . . . ?
C16 C17 C13 C14 0.5(7) . . . . ?
C16 C15 C14 Os3 -62.5(4) . . . . ?
C16 C15 C14 C13 -0.4(7) . . . . ?
C16 C15 C14 C19 173.4(6) . . . . ?
C17 C16 C15 Os3 -61.7(4) . . . . ?
C17 C16 C15 C20 174.2(6) . . . . ?
C17 C16 C15 C14 0.7(7) . . . . ?
C17 C13 C14 Os3 62.3(4) . . . . ?
C17 C13 C14 C15 -0.1(7) . . . . ?
C17 C13 C14 C19 -173.8(6) . . . . ?
C8 C9 C10 Os2 -61.8(5) . . . . ?
C8 C9 C10 C10 -0.2(6) . . . 4_655 ?
C8 C9 C10 C12 174.3(6) . . . . ?
C15 C16 C17 Os3 62.1(4) . . . . ?
C15 C16 C17 C22 -175.4(6) . . . . ?
C15 C16 C17 C13 -0.8(7) . . . . ?
C22 C17 C13 Os3 -121.9(7) . . . . ?
C22 C17 C13 C18 1.5(11) . . . . ?
C22 C17 C13 C14 175.2(6) . . . . ?
C21 C16 C17 Os3 -124.5(6) . . . . ?
C21 C16 C17 C22 -2.0(10) . . . . ?
C21 C16 C17 C13 172.6(6) . . . . ?
C21 C16 C15 Os3 125.1(7) . . . . ?
C21 C16 C15 C20 1.1(10) . . . . ?
C21 C16 C15 C14 -172.4(6) . . . . ?
C11 C9 C10 Os2 120.5(6) . . . . ?
C11 C9 C10 C10 -177.8(5) . . . 4_655 ?
C11 C9 C10 C12 -3.3(10) . . . . ?
C11 C9 C8 Os2 -121.4(6) . . . . ?
C11 C9 C8 C9 177.9(4) . . . 4_655 ?
C11 C9 C8 C7 7.3(12) . . . . ?
C11 C9 C8 Th2 -67.3(7) . . . . ?
C5 C3 C4 Os1 -123.1(6) . . . . ?
C5 C3 C4 C4 175.1(5) . . . 4_655 ?
C5 C3 C4 C6 -1.1(10) . . . . ?
C1 C2 C3 Os1 -115.1(9) . . . . ?
C1 C2 C3 C4 -176.4(8) . . . . ?
C1 C2 C3 C5 9.0(12) . . . . ?
C20 C15 C14 Os3 124.0(6) . . . . ?
C20 C15 C14 C13 -173.9(6) . . . . ?
C20 C15 C14 C19 -0.1(10) . . . . ?
C18 C13 C14 Os3 -124.1(7) . . . . ?
C18 C13 C14 C15 173.5(6) . . . . ?
C18 C13 C14 C19 -0.2(11) . . . . ?
Th2 C7 C8 Os2 0.000(1) . . . . ?
Th2 C7 C8 C9 -95.5(8) . . . . ?
Th2 C7 C8 C9 95.5(8) . . . 4_655 ?
C28 C27 C26 C25 179(3) . . . . ?
C27 C26 C25 C24 -67(5) . . . . ?
C26 C25 C24 C23 -170(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.046
_oxdiff_exptl_absorpt_empirical_full_min 0.657
####################################################################### 
# 
# 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_czy_ii_175_0m
_database_code_depnum_ccdc_archive 'CCDC 2346845'
loop_
_audit_author_name
_audit_author_address
'Christopher Ye'
;UC Berkeley
United States of America
;
_audit_update_record             
;
2024-04-08 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-30
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H64 Os4 Th'
_chemical_formula_sum            'C46 H64 Os4 Th'
_chemical_formula_weight         1609.81
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Os Os -1.2848 7.9466 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Th Th -7.9004 9.3112 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           138
_space_group_name_H-M_alt        'P 42/n c m'
_space_group_name_Hall           '-P 4ac 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z+1/2'
'y, -x+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'y+1/2, x+1/2, -z'
'-y, -x, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z-1/2'
'-y, x-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
'-y-1/2, -x-1/2, z'
'y, x, z'

_cell_length_a                   13.7391(15)
_cell_length_b                   13.7391(15)
_cell_length_c                   25.158(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4748.8(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    53451
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.042
_cell_measurement_theta_min      2.304
_shelx_estimated_absorpt_T_max   0.758
_shelx_estimated_absorpt_T_min   0.096
_exptl_absorpt_coefficient_mu    14.656
_exptl_absorpt_correction_T_max  0.6985
_exptl_absorpt_correction_T_min  0.2861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1894 before and 0.1317 after correction.
The Ratio of minimum to maximum transmission is 0.4096.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             2936
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1416
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53451
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         2.304
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II CPAD detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2047
_reflns_number_total             2317
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2317
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0445
_refine_ls_restrained_S_all      1.200
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+73.6242P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1101
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C12-H12C
 0.96 with sigma of 0.02
 C13-C14 = C16-C17 = C17-C18
 1.37 with sigma of 0.02
 C13-C18
 1.38 with sigma of 0.02
 C14-C15 = C15-C16
 1.36 with sigma of 0.02
 C13-C15 = C15-C17 = C16-C18
 2.37 with sigma of 0.04
 C13-C17
 2.38 with sigma of 0.04
 C14-C16
 2.36 with sigma of 0.04
2. Restrained planarity
 C13, C14, C15, C16, C17, C18
 with sigma of 0.1
3. Rigid body (RIGU) restrains
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Th1(0.25) H4A(0.5) H4B(0.5) H4C(0.5) H12A(0.5) H12B(0.5)
 H12C(0.25) C13(0.25) H13(0.25) C14(0.25) H14(0.25) C15(0.25) H15(0.25)
 C16(0.25) H16(0.25) C17(0.25) H17(0.25) C18(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C),
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Os2 Os 0.68686(3) 0.81314(3) 0.49324(2) 0.03428(19) Uani 1 2 d S T P . .
Os1 Os 0.60450(3) 0.60450(3) 0.33764(2) 0.0435(2) Uani 1 2 d S T P B .
Th1 Th 0.72670(5) 0.77330(5) 0.38049(4) 0.0318(3) Uani 0.5 2 d S T P B .
C7 C 0.6308(8) 0.9433(8) 0.5327(4) 0.043(3) Uani 1 1 d . . . . .
C10 C 0.6725(10) 0.9895(11) 0.5809(5) 0.063(4) Uani 1 1 d . . . . .
H10A H 0.6281 1.0402 0.5938 0.095 Uiso 1 1 calc R U . . .
H10B H 0.7356 1.0186 0.5722 0.095 Uiso 1 1 calc R U . . .
H10C H 0.6812 0.9401 0.6086 0.095 Uiso 1 1 calc R U . . .
C5 C 0.6253(13) 0.3605(10) 0.3465(6) 0.078(5) Uani 1 1 d . . . . .
H5A H 0.6917 0.3680 0.3328 0.117 Uiso 1 1 calc R U . . .
H5B H 0.5965 0.3010 0.3319 0.117 Uiso 1 1 calc R U . . .
H5C H 0.6271 0.3561 0.3854 0.117 Uiso 1 1 calc R U . . .
C1 C 0.4938(8) 0.4938(8) 0.3620(7) 0.053(5) Uani 1 2 d S T P B .
C2 C 0.5655(10) 0.4461(9) 0.3304(5) 0.052(3) Uani 1 1 d . . . . .
C3 C 0.5632(11) 0.4872(11) 0.2786(5) 0.067(4) Uani 1 1 d . . . . .
C4 C 0.4652(10) 0.4652(10) 0.4178(7) 0.061(5) Uani 1 2 d S T P . .
H4A H 0.5234 0.4458 0.4377 0.091 Uiso 0.5 1 calc R U P A -1
H4B H 0.4194 0.4105 0.4164 0.091 Uiso 0.5 1 calc R U P A -1
H4C H 0.4342 0.5206 0.4355 0.091 Uiso 0.5 1 calc R U P A -1
C8 C 0.6528(8) 0.9654(8) 0.4781(4) 0.039(3) Uani 1 1 d . . . . .
C6 C 0.6179(14) 0.4558(14) 0.2316(6) 0.095(6) Uani 1 1 d . . . . .
H6A H 0.5778 0.4112 0.2105 0.143 Uiso 1 1 calc R U . . .
H6B H 0.6775 0.4225 0.2428 0.143 Uiso 1 1 calc R U . . .
H6C H 0.6348 0.5128 0.2100 0.143 Uiso 1 1 calc R U . . .
C11 C 0.7225(10) 1.0446(9) 0.4604(6) 0.058(3) Uani 1 1 d . . . . .
H11A H 0.7790 1.0458 0.4842 0.087 Uiso 1 1 calc R U . . .
H11B H 0.6894 1.1077 0.4616 0.087 Uiso 1 1 calc R U . . .
H11C H 0.7442 1.0313 0.4240 0.087 Uiso 1 1 calc R U . . .
C12 C 0.5878(9) 0.9122(9) 0.3865(6) 0.051(5) Uani 1 2 d DS T P . .
H12A H 0.6084 0.9754 0.3714 0.062 Uiso 0.5 1 calc R U P B .
H12B H 0.5246 0.8916 0.3714 0.062 Uiso 0.5 1 calc R U P . .
C9 C 0.5902(7) 0.9098(7) 0.4453(6) 0.037(4) Uani 1 2 d S T P B .
H12C H 0.604(15) 0.896(15) 0.350(4) 0.04(9) Uiso 0.5 2 d DS . P . .
C13 C 0.648(5) 0.757(5) 0.251(2) 0.051(18) Uani 0.25 1 d D U P B -1
H13 H 0.5913 0.7883 0.2639 0.061 Uiso 0.25 1 calc R U P B -1
C14 C 0.691(4) 0.791(5) 0.205(2) 0.10(3) Uani 0.25 1 d D U P B -1
H14 H 0.6641 0.8456 0.1870 0.119 Uiso 0.25 1 calc R U P B -1
C15 C 0.773(3) 0.747(3) 0.1860(11) 0.052(14) Uani 0.25 1 d D U P B -1
H15 H 0.8034 0.7711 0.1547 0.062 Uiso 0.25 1 calc R U P B -1
C16 C 0.810(3) 0.669(3) 0.2118(13) 0.033(11) Uani 0.25 1 d D U P B -1
H16 H 0.8664 0.6378 0.1979 0.040 Uiso 0.25 1 calc R U P B -1
C17 C 0.769(5) 0.635(5) 0.2576(18) 0.049(15) Uani 0.25 1 d D U P B -1
H17 H 0.7978 0.5816 0.2758 0.059 Uiso 0.25 1 calc R U P B -1
C18 C 0.685(4) 0.677(5) 0.2776(11) 0.040(8) Uani 0.25 1 d D U P B -1


_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
Os2 Os2 2.4537(12) 2_665 ?
Os2 Th1 3.2965(12) 2_665 ?
Os2 Th1 2.9403(11) . ?
Os2 C7 2.186(10) 15_775 ?
Os2 C7 2.186(10) . ?
Os2 C8 2.177(10) 15_775 ?
Os2 C8 2.177(10) . ?
Os2 C9 2.231(14) . ?
Os1 Th1 3.0593(7) . ?
Os1 Th1 3.0593(8) 2_665 ?
Os1 C1 2.237(16) . ?
Os1 C2 2.248(11) 16 ?
Os1 C2 2.248(11) . ?
Os1 C3 2.264(12) . ?
Os1 C3 2.264(12) 16 ?
Os1 C18 2.12(3) . ?
Th1 Os2 3.2966(12) 2_665 ?
Th1 Os1 3.0593(8) 2_665 ?
Th1 Th1 0.906(2) 2_665 ?
Th1 C12 2.702(17) . ?
Th1 C9 3.113(15) . ?
Th1 H12C 2.5(3) . ?
Th1 C18 2.96(3) . ?
C7 C7 1.44(2) 15_775 ?
C7 C10 1.483(16) . ?
C7 C8 1.439(15) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 C2 1.49(2) . ?
C1 C2 1.426(16) 16 ?
C1 C2 1.426(16) . ?
C1 C4 1.51(2) . ?
C2 C3 1.420(17) . ?
C3 C3 1.48(3) 16 ?
C3 C6 1.467(19) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C8 C11 1.517(16) . ?
C8 C9 1.416(14) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C9 1.48(2) . ?
C12 H12C 0.96(2) . ?
C9 C8 1.416(14) 15_775 ?
C13 H13 0.9500 . ?
C13 C14 1.37(2) . ?
C13 C18 1.390(19) . ?
C14 H14 0.9500 . ?
C14 C15 1.364(19) . ?
C15 H15 0.9500 . ?
C15 C16 1.355(19) . ?
C16 H16 0.9500 . ?
C16 C17 1.370(19) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(19) . ?

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
Os2 Os2 Th1 59.37(2) 2_665 2_665 ?
Os2 Os2 Th1 74.74(2) 2_665 . ?
Th1 Os2 Th1 15.37(4) . 2_665 ?
C7 Os2 Os2 145.9(3) 15_775 2_665 ?
C7 Os2 Os2 145.9(3) . 2_665 ?
C7 Os2 Th1 144.4(3) 15_775 2_665 ?
C7 Os2 Th1 131.0(3) . . ?
C7 Os2 Th1 131.0(3) 15_775 . ?
C7 Os2 Th1 144.4(3) . 2_665 ?
C7 Os2 C7 38.4(6) . 15_775 ?
C7 Os2 C9 63.2(5) 15_775 . ?
C7 Os2 C9 63.2(5) . . ?
C8 Os2 Os2 146.2(3) . 2_665 ?
C8 Os2 Os2 146.2(3) 15_775 2_665 ?
C8 Os2 Th1 92.9(3) . . ?
C8 Os2 Th1 105.9(3) 15_775 2_665 ?
C8 Os2 Th1 105.9(3) . 2_665 ?
C8 Os2 Th1 92.9(3) 15_775 . ?
C8 Os2 C7 38.5(4) . . ?
C8 Os2 C7 38.5(4) 15_775 15_775 ?
C8 Os2 C7 64.2(4) . 15_775 ?
C8 Os2 C7 64.2(4) 15_775 . ?
C8 Os2 C8 63.7(6) . 15_775 ?
C8 Os2 C9 37.4(3) 15_775 . ?
C8 Os2 C9 37.4(3) . . ?
C9 Os2 Os2 147.3(4) . 2_665 ?
C9 Os2 Th1 87.9(4) . 2_665 ?
C9 Os2 Th1 72.5(4) . . ?
Th1 Os1 Th1 17.02(4) . 2_665 ?
C1 Os1 Th1 142.4(4) . 2_665 ?
C1 Os1 Th1 142.4(4) . . ?
C1 Os1 C2 37.1(4) . . ?
C1 Os1 C2 37.1(4) . 16 ?
C1 Os1 C3 61.6(5) . . ?
C1 Os1 C3 61.6(5) . 16 ?
C2 Os1 Th1 153.3(3) 16 2_665 ?
C2 Os1 Th1 137.8(4) . 2_665 ?
C2 Os1 Th1 137.8(4) 16 . ?
C2 Os1 Th1 153.3(3) . . ?
C2 Os1 C2 62.1(7) . 16 ?
C2 Os1 C3 36.7(5) 16 16 ?
C2 Os1 C3 62.2(5) . 16 ?
C2 Os1 C3 36.7(5) . . ?
C2 Os1 C3 62.2(5) 16 . ?
C3 Os1 Th1 155.3(3) 16 2_665 ?
C3 Os1 Th1 144.3(4) . 2_665 ?
C3 Os1 Th1 155.3(3) . . ?
C3 Os1 Th1 144.3(4) 16 . ?
C3 Os1 C3 38.0(8) 16 . ?
C18 Os1 Th1 66.2(9) . 2_665 ?
C18 Os1 Th1 66.9(8) . . ?
C18 Os1 C1 150.4(9) . . ?
C18 Os1 C2 121.4(16) . . ?
C18 Os1 C2 124.1(17) . 16 ?
C18 Os1 C3 91.4(12) . 16 ?
C18 Os1 C3 89.9(11) . . ?
Os2 Th1 Os2 45.89(3) . 2_665 ?
Os2 Th1 Os1 112.27(2) . . ?
Os2 Th1 Os1 112.27(2) . 2_665 ?
Os2 Th1 C9 43.1(3) . . ?
Os2 Th1 H12C 92.3(6) . . ?
Os2 Th1 H12C 138.2(6) 2_665 . ?
Os2 Th1 C18 152.9(5) . . ?
Os1 Th1 Os2 103.17(2) . 2_665 ?
Os1 Th1 Os2 103.17(2) 2_665 2_665 ?
Os1 Th1 Os1 135.06(4) . 2_665 ?
Os1 Th1 C9 108.10(7) . . ?
Os1 Th1 C9 108.10(7) 2_665 . ?
Os1 Th1 H12C 92.0(2) . . ?
Os1 Th1 H12C 92.0(2) 2_665 . ?
Th1 Th1 Os2 59.36(2) 2_665 2_665 ?
Th1 Th1 Os2 105.26(2) 2_665 . ?
Th1 Th1 Os1 81.49(2) 2_665 . ?
Th1 Th1 Os1 81.49(2) 2_665 2_665 ?
Th1 Th1 C12 176.8(3) 2_665 . ?
Th1 Th1 C9 148.4(3) 2_665 . ?
Th1 Th1 H12C 162.4(6) 2_665 . ?
Th1 Th1 C18 79.6(17) 2_665 . ?
C12 Th1 Os2 117.4(4) . 2_665 ?
C12 Th1 Os2 71.5(3) . . ?
C12 Th1 Os1 99.65(12) . . ?
C12 Th1 Os1 99.65(12) . 2_665 ?
C12 Th1 C9 28.4(4) . . ?
C12 Th1 H12C 20.8(5) . . ?
C12 Th1 C18 103.2(17) . . ?
C9 Th1 Os2 89.0(3) . 2_665 ?
C9 Th1 H12C 49.2(7) . . ?
C18 Th1 Os2 131.3(15) . 2_665 ?
C18 Th1 Os1 94.7(5) . 2_665 ?
C18 Th1 Os1 41.3(5) . . ?
C18 Th1 C9 127.7(16) . . ?
C18 Th1 H12C 84.7(18) . . ?
C7 C7 Os2 70.8(3) 15_775 . ?
C7 C7 C10 125.1(8) 15_775 . ?
C7 C7 C8 107.3(7) 15_775 . ?
C10 C7 Os2 125.8(8) . . ?
C8 C7 Os2 70.4(6) . . ?
C8 C7 C10 127.5(12) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
C2 C1 Os1 71.9(8) 16 . ?
C2 C1 Os1 71.9(8) . . ?
C2 C1 C2 108.9(15) 16 . ?
C2 C1 C4 125.4(8) . . ?
C2 C1 C4 125.4(8) 16 . ?
C4 C1 Os1 127.5(12) . . ?
C5 C2 Os1 127.6(10) . . ?
C1 C2 Os1 71.0(8) . . ?
C1 C2 C5 126.3(12) . . ?
C3 C2 Os1 72.2(7) . . ?
C3 C2 C5 125.2(13) . . ?
C3 C2 C1 108.2(13) . . ?
C2 C3 Os1 71.1(7) . . ?
C2 C3 C3 107.3(9) . 16 ?
C2 C3 C6 127.7(15) . . ?
C3 C3 Os1 71.0(4) 16 . ?
C6 C3 Os1 127.6(11) . . ?
C6 C3 C3 124.8(10) . 16 ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C7 C8 Os2 71.1(6) . . ?
C7 C8 C11 124.4(11) . . ?
C11 C8 Os2 127.2(8) . . ?
C9 C8 Os2 73.4(7) . . ?
C9 C8 C7 108.4(10) . . ?
C9 C8 C11 126.8(11) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Th1 C12 H12A 113.4 . . ?
Th1 C12 H12B 113.4 . . ?
Th1 C12 H12C 68(10) . . ?
H12A C12 H12B 110.7 . . ?
H12A C12 H12C 76.7 . . ?
H12B C12 H12C 76.7 . . ?
C9 C12 Th1 91.4(10) . . ?
C9 C12 H12A 113.4 . . ?
C9 C12 H12B 113.4 . . ?
C9 C12 H12C 160(10) . . ?
Os2 C9 Th1 64.3(4) . . ?
C8 C9 Os2 69.2(7) 15_775 . ?
C8 C9 Os2 69.2(7) . . ?
C8 C9 Th1 105.3(8) 15_775 . ?
C8 C9 Th1 105.3(8) . . ?
C8 C9 C8 108.4(13) 15_775 . ?
C8 C9 C12 125.8(7) 15_775 . ?
C8 C9 C12 125.8(7) . . ?
C12 C9 Os2 124.5(11) . . ?
C12 C9 Th1 60.2(8) . . ?
C14 C13 H13 119.4 . . ?
C14 C13 C18 121(3) . . ?
C18 C13 H13 119.4 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 120(3) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 120.2 . . ?
C16 C15 C14 120(2) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121(2) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 121(2) . . ?
C18 C17 H17 119.7 . . ?
Os1 C18 Th1 71.9(7) . . ?
C13 C18 Os1 122(4) . . ?
C13 C18 Th1 98(4) . . ?
C17 C18 Os1 120(4) . . ?
C17 C18 Th1 110(4) . . ?
C17 C18 C13 117(2) . . ?

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
Os2 C7 C8 C11 -122.7(11) . . . . ?
Os2 C7 C8 C9 64.4(9) . . . . ?
Os2 C8 C9 Th1 -54.2(4) . . . . ?
Os2 C8 C9 C8 58.2(10) . . . 15_775 ?
Os2 C8 C9 C12 -118.2(15) . . . . ?
Os1 C1 C2 C5 123.3(14) . . . . ?
Os1 C1 C2 C3 -63.1(9) . . . . ?
Os1 C2 C3 C3 -62.1(4) . . . 16 ?
Os1 C2 C3 C6 123.4(15) . . . . ?
Th1 C12 C9 Os2 0.000(3) . . . . ?
Th1 C12 C9 C8 87.9(14) . . . . ?
Th1 C12 C9 C8 -87.9(14) . . . 15_775 ?
C7 C7 C8 Os2 -61.5(3) 15_775 . . . ?
C7 C7 C8 C11 175.8(9) 15_775 . . . ?
C7 C7 C8 C9 2.9(10) 15_775 . . . ?
C7 C8 C9 Os2 -62.9(8) . . . . ?
C7 C8 C9 Th1 -117.1(8) . . . . ?
C7 C8 C9 C8 -4.7(16) . . . 15_775 ?
C7 C8 C9 C12 178.9(14) . . . . ?
C10 C7 C8 Os2 120.6(12) . . . . ?
C10 C7 C8 C11 -2.1(18) . . . . ?
C10 C7 C8 C9 -175.0(12) . . . . ?
C5 C2 C3 Os1 -123.9(14) . . . . ?
C5 C2 C3 C3 173.9(11) . . . 16 ?
C5 C2 C3 C6 -1(2) . . . . ?
C1 C2 C3 Os1 62.3(9) . . . . ?
C1 C2 C3 C3 0.2(11) . . . 16 ?
C1 C2 C3 C6 -174.3(14) . . . . ?
C2 C1 C2 Os1 62.8(11) 16 . . . ?
C2 C1 C2 C5 -174.0(9) 16 . . . ?
C2 C1 C2 C3 -0.3(18) 16 . . . ?
C4 C1 C2 Os1 -123.6(16) . . . . ?
C4 C1 C2 C5 0(2) . . . . ?
C4 C1 C2 C3 173.4(15) . . . . ?
C11 C8 C9 Os2 124.4(12) . . . . ?
C11 C8 C9 Th1 70.3(13) . . . . ?
C11 C8 C9 C8 -177.4(8) . . . 15_775 ?
C11 C8 C9 C12 6(2) . . . . ?
C13 C14 C15 C16 1(3) . . . . ?
C14 C13 C18 Os1 -167(2) . . . . ?
C14 C13 C18 Th1 119(3) . . . . ?
C14 C13 C18 C17 1(4) . . . . ?
C14 C15 C16 C17 -2(5) . . . . ?
C15 C16 C17 C18 2(6) . . . . ?
C16 C17 C18 Os1 166(3) . . . . ?
C16 C17 C18 Th1 -114(5) . . . . ?
C16 C17 C18 C13 -2(5) . . . . ?
C18 C13 C14 C15 -1(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_czy_72236_0m
_database_code_depnum_ccdc_archive 'CCDC 2346843'
loop_
_audit_author_name
_audit_author_address
'Christopher Ye'
;UC Berkeley
United States of America
;
_audit_update_record             
;
2024-04-08 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C40 H59 Os4 U'
_chemical_formula_sum            'C40 H59 Os4 U'
_chemical_formula_weight         1538.70
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Os Os -1.2848 7.9466 'Calculated using XDISP in WinGX (Farrugia, 1999)'
U U -10.9608 4.1580 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   40.875(4)
_cell_length_b                   10.0269(10)
_cell_length_c                   23.315(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.731(4)
_cell_angle_gamma                90
_cell_volume                     8747.7(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    52702
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.042
_cell_measurement_theta_min      1.821
_shelx_estimated_absorpt_T_max   0.767
_shelx_estimated_absorpt_T_min   0.679
_exptl_absorpt_coefficient_mu    13.975
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.7902.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5560
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52702
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         1.821
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6813
_reflns_number_total             7991
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.899
_refine_diff_density_min         -2.543
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     186
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0178P)²+154.2928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0701
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H6C-U1
 3.275 with sigma of 0.02
 H6B-U1
 3.227 with sigma of 0.02
 H6A-U1
 1.792 with sigma of 0.02
 U1A-H27C
 1.735 with sigma of 0.02
 U1A-H27A
 3.154 with sigma of 0.02
 U1A-H27B
 3.235 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C34A \\sim C35A \\sim C31A \\sim C32A \\sim C33A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C35, C31, C32, C33, C34, C40, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37A, C36A, C40A, C39A, C38A, C33A, C34A, C35A, C31A, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C33A)=Sof(C32A)=Sof(C31A)=Sof(C34A)=Sof(C35A)=Sof(C38A)=Sof(H38A)=
 Sof(H38B)=Sof(H38C)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40A)=
 Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C31)=Sof(C35)=Sof(C34)=Sof(C32)=Sof(C33)=Sof(C38)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C39)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(1)
 Sof(U1A)=1-FVAR(2)
 Sof(U1)=FVAR(2)
 Fixed Sof: H6A(0.5) H27C(0.5)
5.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C29(H29A,H29B,H29C), C8(H8A,H8B,H8C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C9(H9A,H9B,H9C),
  C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C20(H20A,H20B,H20C), C16(H16A,H16B,
 H16C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C38A(H38A,H38B,H38C), C39A(H39A,H39B,H39C), C38(H38D,H38E,H38F), C39(H39D,H39E,
 H39F), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C36(H36A,H36B,H36C),
 C40A(H40D,H40E,H40F), C37A(H37D,H37E,H37F), C36A(H36D,H36E,H36F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Os3 Os 0.42003(2) 0.47753(3) 0.49327(2) 0.02019(7) Uani 1 1 d . . . . .
Os4 Os 0.41174(2) 0.71765(3) 0.50552(2) 0.02565(8) Uani 1 1 d . . . . .
Os2 Os 0.38008(2) 0.66266(5) 0.27598(2) 0.04710(11) Uani 1 1 d . . . . .
Os1 Os 0.28859(2) 0.53915(5) 0.36821(2) 0.05274(12) Uani 1 1 d . . . . .
U1 U 0.35976(2) 0.65292(7) 0.38723(3) 0.0318(2) Uani 0.5345(13) 1 d D . P A 4
U1A U 0.36336(2) 0.54494(8) 0.37735(3) 0.0271(3) Uani 0.4655(13) 1 d D . P A 3
C3 C 0.4381(2) 0.9102(7) 0.5379(5) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.4152(2) 0.9211(7) 0.4718(5) 0.039(2) Uani 1 1 d . . . . .
C22 C 0.4017(2) 0.2972(7) 0.4326(4) 0.0288(17) Uani 1 1 d . . . . .
C24 C 0.4341(2) 0.2826(7) 0.5408(4) 0.0264(17) Uani 1 1 d . . . . .
C1 C 0.3790(2) 0.9003(7) 0.4642(4) 0.0348(19) Uani 1 1 d . . . . .
C7 C 0.4277(3) 0.9630(8) 0.4226(5) 0.047(2) Uani 1 1 d . . . . .
H7A H 0.4512 0.9233 0.4314 0.071 Uiso 1 1 calc R U . . .
H7B H 0.4296 1.0604 0.4225 0.071 Uiso 1 1 calc R U . . .
H7C H 0.4106 0.9328 0.3815 0.071 Uiso 1 1 calc R U . . .
C21 C 0.4389(2) 0.3232(7) 0.4465(4) 0.0274(17) Uani 1 1 d . . . . .
C6 C 0.3472(3) 0.9066(8) 0.4045(5) 0.055(3) Uani 1 1 d . . . . .
H6A H 0.3432 0.8192 0.3840 0.082 Uiso 0.5 1 calc DR U P . .
H6B H 0.3510 0.9735 0.3771 0.082 Uiso 1 1 calc DR U . . .
H6C H 0.3263 0.9312 0.4128 0.082 Uiso 1 1 calc DR U . . .
C23 C 0.3992(2) 0.2729(7) 0.4919(4) 0.0277(17) Uani 1 1 d . . . . .
C29 C 0.4436(2) 0.2601(8) 0.6090(4) 0.0345(19) Uani 1 1 d . . . . .
H29A H 0.4649 0.3121 0.6337 0.052 Uiso 1 1 calc R U . . .
H29B H 0.4483 0.1652 0.6187 0.052 Uiso 1 1 calc R U . . .
H29C H 0.4236 0.2884 0.6194 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3797(2) 0.8717(7) 0.5250(4) 0.039(2) Uani 1 1 d . . . . .
C4 C 0.4156(2) 0.8797(7) 0.5707(4) 0.036(2) Uani 1 1 d . . . . .
C25 C 0.4591(2) 0.3137(7) 0.5124(4) 0.0255(16) Uani 1 1 d . . . . .
C8 C 0.4774(2) 0.9364(8) 0.5667(5) 0.054(3) Uani 1 1 d . . . . .
H8A H 0.4881 0.8911 0.6073 0.081 Uiso 1 1 calc R U . . .
H8B H 0.4817 1.0326 0.5727 0.081 Uiso 1 1 calc R U . . .
H8C H 0.4883 0.9026 0.5390 0.081 Uiso 1 1 calc R U . . .
C26 C 0.4536(2) 0.3419(8) 0.3976(4) 0.040(2) Uani 1 1 d . . . . .
H26A H 0.4399 0.4110 0.3679 0.060 Uiso 1 1 calc R U . . .
H26B H 0.4519 0.2578 0.3752 0.060 Uiso 1 1 calc R U . . .
H26C H 0.4787 0.3692 0.4178 0.060 Uiso 1 1 calc R U . . .
C28 C 0.3658(2) 0.2395(7) 0.5005(4) 0.0337(19) Uani 1 1 d . . . . .
H28A H 0.3677 0.2730 0.5411 0.051 Uiso 1 1 calc R U . . .
H28B H 0.3626 0.1425 0.4989 0.051 Uiso 1 1 calc R U . . .
H28C H 0.3453 0.2811 0.4669 0.051 Uiso 1 1 calc R U . . .
C12 C 0.4182(3) 0.6323(12) 0.2308(5) 0.058(3) Uani 1 1 d . . . . .
C30 C 0.4983(2) 0.3272(8) 0.5459(4) 0.0344(19) Uani 1 1 d . . . . .
H30A H 0.5074 0.3863 0.5222 0.052 Uiso 1 1 calc R U . . .
H30B H 0.5095 0.2393 0.5502 0.052 Uiso 1 1 calc R U . . .
H30C H 0.5040 0.3650 0.5876 0.052 Uiso 1 1 calc R U . . .
C11 C 0.3831(3) 0.5991(12) 0.1863(5) 0.066(3) Uani 1 1 d . . . . .
C9 C 0.4282(3) 0.8650(9) 0.6401(5) 0.051(2) Uani 1 1 d . . . . .
H9A H 0.4113 0.8094 0.6496 0.077 Uiso 1 1 calc R U . . .
H9B H 0.4298 0.9532 0.6591 0.077 Uiso 1 1 calc R U . . .
H9C H 0.4519 0.8229 0.6570 0.077 Uiso 1 1 calc R U . . .
C13 C 0.4180(2) 0.7686(12) 0.2448(4) 0.049(3) Uani 1 1 d . . . . .
C17 C 0.4502(4) 0.5390(16) 0.2526(7) 0.112(6) Uani 1 1 d . . . . .
H17A H 0.4681 0.5702 0.2928 0.168 Uiso 1 1 calc R U . . .
H17B H 0.4607 0.5378 0.2214 0.168 Uiso 1 1 calc R U . . .
H17C H 0.4425 0.4488 0.2575 0.168 Uiso 1 1 calc R U . . .
C27 C 0.3724(2) 0.2897(7) 0.3695(4) 0.042(2) Uani 1 1 d . . . . .
H27A H 0.3531 0.2335 0.3711 0.063 Uiso 1 1 calc DR U . . .
H27B H 0.3814 0.2512 0.3401 0.063 Uiso 1 1 calc DR U . . .
H27C H 0.3631 0.3795 0.3556 0.063 Uiso 0.5 1 calc DR U P . .
C20 C 0.3236(3) 0.7305(17) 0.1268(5) 0.094(5) Uani 1 1 d . . . . .
H20A H 0.3122 0.6428 0.1160 0.141 Uiso 1 1 calc R U . . .
H20B H 0.3235 0.7732 0.0889 0.141 Uiso 1 1 calc R U . . .
H20C H 0.3104 0.7863 0.1447 0.141 Uiso 1 1 calc R U . . .
C14 C 0.3831(3) 0.8196(10) 0.2097(4) 0.048(2) Uani 1 1 d . . . . .
C16 C 0.3725(5) 0.4672(15) 0.1540(8) 0.121(6) Uani 1 1 d . . . . .
H16A H 0.3850 0.3956 0.1833 0.182 Uiso 1 1 calc R U . . .
H16B H 0.3790 0.4645 0.1179 0.182 Uiso 1 1 calc R U . . .
H16C H 0.3466 0.4552 0.1398 0.182 Uiso 1 1 calc R U . . .
C10 C 0.3468(2) 0.8476(9) 0.5379(4) 0.042(2) Uani 1 1 d . . . . .
H10A H 0.3288 0.8013 0.5021 0.064 Uiso 1 1 calc R U . . .
H10B H 0.3372 0.9332 0.5443 0.064 Uiso 1 1 calc R U . . .
H10C H 0.3532 0.7926 0.5756 0.064 Uiso 1 1 calc R U . . .
C15 C 0.3622(2) 0.7138(13) 0.1747(4) 0.055(3) Uani 1 1 d . . . . .
C18 C 0.4501(3) 0.8505(14) 0.2845(5) 0.075(4) Uani 1 1 d . . . . .
H18A H 0.4423 0.9394 0.2912 0.113 Uiso 1 1 calc R U . . .
H18B H 0.4663 0.8589 0.2632 0.113 Uiso 1 1 calc R U . . .
H18C H 0.4626 0.8066 0.3251 0.113 Uiso 1 1 calc R U . . .
C19 C 0.3714(4) 0.9627(12) 0.2096(7) 0.090(4) Uani 1 1 d . . . . .
H19A H 0.3478 0.9645 0.2115 0.135 Uiso 1 1 calc R U . . .
H19B H 0.3699 1.0069 0.1712 0.135 Uiso 1 1 calc R U . . .
H19C H 0.3887 1.0094 0.2461 0.135 Uiso 1 1 calc R U . . .
C33A C 0.2537(11) 0.524(4) 0.420(2) 0.058(7) Uani 0.466(15) 1 d . U P A 2
C32A C 0.2344(9) 0.591(4) 0.3667(16) 0.059(6) Uani 0.466(15) 1 d . U P A 2
C31A C 0.2292(7) 0.513(5) 0.3104(13) 0.058(5) Uani 0.466(15) 1 d . U P A 2
C34A C 0.2559(6) 0.385(3) 0.4052(12) 0.053(5) Uani 0.466(15) 1 d . U P A 2
C35A C 0.2425(7) 0.381(4) 0.3376(15) 0.057(5) Uani 0.466(15) 1 d . U P A 2
C31 C 0.2357(6) 0.442(3) 0.3132(15) 0.067(5) Uani 0.534(15) 1 d . U P A 1
C35 C 0.2548(6) 0.386(3) 0.3749(16) 0.065(5) Uani 0.534(15) 1 d . U P A 1
C34 C 0.2559(8) 0.487(3) 0.4174(18) 0.055(5) Uani 0.534(15) 1 d . U P A 1
C32 C 0.2284(5) 0.585(3) 0.3227(15) 0.059(5) Uani 0.534(15) 1 d . U P A 1
C33 C 0.2413(7) 0.611(3) 0.3834(13) 0.054(5) Uani 0.534(15) 1 d . U P A 1
C38A C 0.2631(7) 0.564(3) 0.4873(11) 0.068(7) Uani 0.466(15) 1 d . U P A 2
H38A H 0.2677 0.6597 0.4919 0.102 Uiso 0.466(15) 1 calc R U P A 2
H38B H 0.2845 0.5152 0.5148 0.102 Uiso 0.466(15) 1 calc R U P A 2
H38C H 0.2431 0.5418 0.4987 0.102 Uiso 0.466(15) 1 calc R U P A 2
C39A C 0.2701(6) 0.268(3) 0.4461(13) 0.071(7) Uani 0.466(15) 1 d . U P A 2
H39A H 0.2851 0.2977 0.4886 0.107 Uiso 0.466(15) 1 calc R U P A 2
H39B H 0.2844 0.2131 0.4299 0.107 Uiso 0.466(15) 1 calc R U P A 2
H39C H 0.2502 0.2145 0.4470 0.107 Uiso 0.466(15) 1 calc R U P A 2
C38 C 0.2349(7) 0.737(3) 0.4102(14) 0.087(7) Uani 0.534(15) 1 d . U P A 1
H38D H 0.2130 0.7286 0.4176 0.131 Uiso 0.534(15) 1 calc R U P A 1
H38E H 0.2323 0.8098 0.3809 0.131 Uiso 0.534(15) 1 calc R U P A 1
H38F H 0.2552 0.7546 0.4500 0.131 Uiso 0.534(15) 1 calc R U P A 1
C39 C 0.2685(7) 0.458(3) 0.4842(12) 0.089(7) Uani 0.534(15) 1 d . U P A 1
H39D H 0.2482 0.4320 0.4940 0.134 Uiso 0.534(15) 1 calc R U P A 1
H39E H 0.2799 0.5378 0.5084 0.134 Uiso 0.534(15) 1 calc R U P A 1
H39F H 0.2859 0.3852 0.4950 0.134 Uiso 0.534(15) 1 calc R U P A 1
C37 C 0.2060(5) 0.671(3) 0.2679(12) 0.092(7) Uani 0.534(15) 1 d . U P A 1
H37A H 0.2122 0.6520 0.2323 0.138 Uiso 0.534(15) 1 calc R U P A 1
H37B H 0.2106 0.7652 0.2795 0.138 Uiso 0.534(15) 1 calc R U P A 1
H37C H 0.1807 0.6515 0.2564 0.138 Uiso 0.534(15) 1 calc R U P A 1
C40 C 0.2658(6) 0.241(2) 0.3883(15) 0.096(8) Uani 0.534(15) 1 d . U P A 1
H40A H 0.2447 0.1859 0.3814 0.144 Uiso 0.534(15) 1 calc R U P A 1
H40B H 0.2830 0.2312 0.4319 0.144 Uiso 0.534(15) 1 calc R U P A 1
H40C H 0.2769 0.2107 0.3603 0.144 Uiso 0.534(15) 1 calc R U P A 1
C36 C 0.2262(7) 0.359(4) 0.2526(14) 0.118(10) Uani 0.534(15) 1 d . U P A 1
H36A H 0.2434 0.2861 0.2605 0.176 Uiso 0.534(15) 1 calc R U P A 1
H36B H 0.2271 0.4164 0.2192 0.176 Uiso 0.534(15) 1 calc R U P A 1
H36C H 0.2021 0.3223 0.2398 0.176 Uiso 0.534(15) 1 calc R U P A 1
C40A C 0.2375(8) 0.248(3) 0.3021(15) 0.092(8) Uani 0.466(15) 1 d . U P A 2
H40D H 0.2130 0.2160 0.2903 0.138 Uiso 0.466(15) 1 calc R U P A 2
H40E H 0.2543 0.1818 0.3292 0.138 Uiso 0.466(15) 1 calc R U P A 2
H40F H 0.2420 0.2611 0.2643 0.138 Uiso 0.466(15) 1 calc R U P A 2
C37A C 0.2234(11) 0.734(4) 0.3612(18) 0.118(12) Uani 0.466(15) 1 d . U P A 2
H37D H 0.2031 0.7439 0.3731 0.178 Uiso 0.466(15) 1 calc R U P A 2
H37E H 0.2164 0.7637 0.3178 0.178 Uiso 0.466(15) 1 calc R U P A 2
H37F H 0.2434 0.7884 0.3890 0.178 Uiso 0.466(15) 1 calc R U P A 2
C36A C 0.2094(7) 0.535(4) 0.2435(12) 0.105(9) Uani 0.466(15) 1 d . U P A 2
H36D H 0.1880 0.4786 0.2282 0.157 Uiso 0.466(15) 1 calc R U P A 2
H36E H 0.2246 0.5126 0.2213 0.157 Uiso 0.466(15) 1 calc R U P A 2
H36F H 0.2023 0.6289 0.2361 0.157 Uiso 0.466(15) 1 calc R U P A 2


_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
Os3 Os4 2.4639(4) . ?
Os3 U1 3.2204(7) . ?
Os3 U1A 2.8439(7) . ?
Os3 C22 2.232(7) . ?
Os3 C24 2.206(7) . ?
Os3 C21 2.203(7) . ?
Os3 C23 2.217(7) . ?
Os3 C25 2.207(7) . ?
Os4 U1 2.7974(7) . ?
Os4 U1A 3.3292(8) . ?
Os4 C3 2.192(7) . ?
Os4 C2 2.211(8) . ?
Os4 C1 2.244(7) . ?
Os4 C5 2.188(7) . ?
Os4 C4 2.186(8) . ?
Os2 U1 3.0264(7) . ?
Os2 U1A 2.9571(7) . ?
Os2 C12 2.226(9) . ?
Os2 C11 2.236(10) . ?
Os2 C13 2.229(8) . ?
Os2 C14 2.243(8) . ?
Os2 C15 2.232(9) . ?
Os1 U1 2.9873(7) . ?
Os1 U1A 2.9777(8) . ?
Os1 C33A 2.21(4) . ?
Os1 C32A 2.26(4) . ?
Os1 C31A 2.27(2) . ?
Os1 C34A 2.42(3) . ?
Os1 C35A 2.34(3) . ?
Os1 C31 2.24(2) . ?
Os1 C35 2.11(2) . ?
Os1 C34 2.15(3) . ?
Os1 C32 2.30(2) . ?
Os1 C33 2.22(3) . ?
U1 C1 2.975(8) . ?
U1A C22 2.943(7) . ?
C3 C2 1.450(13) . ?
C3 C4 1.447(11) . ?
C3 C8 1.494(11) . ?
C2 C1 1.431(11) . ?
C2 C7 1.494(11) . ?
C22 C21 1.444(11) . ?
C22 C23 1.449(10) . ?
C22 C27 1.479(11) . ?
C24 C23 1.427(11) . ?
C24 C29 1.494(11) . ?
C24 C25 1.457(10) . ?
C1 C6 1.475(13) . ?
C1 C5 1.437(12) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C21 C25 1.426(11) . ?
C21 C26 1.500(10) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C23 C28 1.493(10) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C5 C4 1.427(12) . ?
C5 C10 1.509(11) . ?
C4 C9 1.494(13) . ?
C25 C30 1.481(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C12 C11 1.432(16) . ?
C12 C13 1.405(15) . ?
C12 C17 1.520(14) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C11 C16 1.496(17) . ?
C11 C15 1.393(15) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C13 C14 1.424(13) . ?
C13 C18 1.509(14) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C15 1.531(14) . ?
C14 C15 1.401(15) . ?
C14 C19 1.513(15) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C33A C32A 1.35(6) . ?
C33A C34A 1.45(5) . ?
C33A C38A 1.51(4) . ?
C32A C31A 1.47(4) . ?
C32A C37A 1.50(5) . ?
C31A C35A 1.47(5) . ?
C31A C36A 1.46(4) . ?
C34A C35A 1.44(4) . ?
C34A C39A 1.48(4) . ?
C35A C40A 1.54(4) . ?
C31 C35 1.45(4) . ?
C31 C32 1.50(4) . ?
C31 C36 1.55(4) . ?
C35 C34 1.41(5) . ?
C35 C40 1.52(3) . ?
C34 C33 1.46(4) . ?
C34 C39 1.46(4) . ?
C32 C33 1.32(4) . ?
C32 C37 1.51(3) . ?
C33 C38 1.48(4) . ?
C38A H38A 0.9800 . ?
C38A H38B 0.9800 . ?
C38A H38C 0.9800 . ?
C39A H39A 0.9800 . ?
C39A H39B 0.9800 . ?
C39A H39C 0.9800 . ?
C38 H38D 0.9800 . ?
C38 H38E 0.9800 . ?
C38 H38F 0.9800 . ?
C39 H39D 0.9800 . ?
C39 H39E 0.9800 . ?
C39 H39F 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C40A H40D 0.9800 . ?
C40A H40E 0.9800 . ?
C40A H40F 0.9800 . ?
C37A H37D 0.9800 . ?
C37A H37E 0.9800 . ?
C37A H37F 0.9800 . ?
C36A H36D 0.9800 . ?
C36A H36E 0.9800 . ?
C36A H36F 0.9800 . ?

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
Os4 Os3 U1 57.114(17) . . ?
Os4 Os3 U1A 77.323(19) . . ?
C22 Os3 Os4 147.0(2) . . ?
C22 Os3 U1 89.9(2) . . ?
C22 Os3 U1A 69.7(2) . . ?
C24 Os3 Os4 145.86(19) . . ?
C24 Os3 U1 146.5(2) . . ?
C24 Os3 U1A 129.5(2) . . ?
C24 Os3 C22 63.5(3) . . ?
C24 Os3 C23 37.6(3) . . ?
C24 Os3 C25 38.6(3) . . ?
C21 Os3 Os4 146.65(18) . . ?
C21 Os3 U1 108.4(2) . . ?
C21 Os3 U1A 90.6(2) . . ?
C21 Os3 C22 38.0(3) . . ?
C21 Os3 C24 63.5(3) . . ?
C21 Os3 C23 63.4(3) . . ?
C21 Os3 C25 37.7(3) . . ?
C23 Os3 Os4 146.71(19) . . ?
C23 Os3 U1 108.9(2) . . ?
C23 Os3 U1A 92.6(2) . . ?
C23 Os3 C22 38.0(3) . . ?
C25 Os3 Os4 145.65(19) . . ?
C25 Os3 U1 146.0(2) . . ?
C25 Os3 U1A 128.0(2) . . ?
C25 Os3 C22 63.6(3) . . ?
C25 Os3 C23 63.7(3) . . ?
Os3 Os4 U1 75.184(18) . . ?
Os3 Os4 U1A 56.452(16) . . ?
C3 Os4 Os3 146.0(2) . . ?
C3 Os4 U1 128.1(3) . . ?
C3 Os4 U1A 143.1(3) . . ?
C3 Os4 C2 38.5(3) . . ?
C3 Os4 C1 63.6(3) . . ?
C2 Os4 Os3 146.0(2) . . ?
C2 Os4 U1 89.7(3) . . ?
C2 Os4 U1A 105.1(3) . . ?
C2 Os4 C1 37.5(3) . . ?
C1 Os4 Os3 146.5(2) . . ?
C1 Os4 U1 71.4(2) . . ?
C1 Os4 U1A 90.2(2) . . ?
C5 Os4 Os3 146.7(2) . . ?
C5 Os4 U1 95.1(3) . . ?
C5 Os4 U1A 111.4(2) . . ?
C5 Os4 C3 63.9(3) . . ?
C5 Os4 C2 63.4(3) . . ?
C5 Os4 C1 37.8(3) . . ?
C4 Os4 Os3 146.3(2) . . ?
C4 Os4 U1 132.2(2) . . ?
C4 Os4 U1A 149.4(2) . . ?
C4 Os4 C3 38.6(3) . . ?
C4 Os4 C2 64.2(3) . . ?
C4 Os4 C1 63.6(3) . . ?
C4 Os4 C5 38.1(3) . . ?
C12 Os2 U1 152.5(3) . . ?
C12 Os2 U1A 139.0(2) . . ?
C12 Os2 C11 37.4(4) . . ?
C12 Os2 C13 36.8(4) . . ?
C12 Os2 C14 61.7(3) . . ?
C12 Os2 C15 61.6(3) . . ?
C11 Os2 U1 158.4(3) . . ?
C11 Os2 U1A 138.7(3) . . ?
C11 Os2 C14 61.1(4) . . ?
C13 Os2 U1 139.6(3) . . ?
C13 Os2 U1A 149.9(2) . . ?
C13 Os2 C11 61.6(4) . . ?
C13 Os2 C14 37.1(3) . . ?
C13 Os2 C15 61.4(3) . . ?
C14 Os2 U1 136.3(3) . . ?
C14 Os2 U1A 157.7(2) . . ?
C15 Os2 U1 145.9(2) . . ?
C15 Os2 U1A 148.7(3) . . ?
C15 Os2 C11 36.3(4) . . ?
C15 Os2 C14 36.5(4) . . ?
C33A Os1 C32A 35.2(15) . . ?
C33A Os1 C31A 63.0(13) . . ?
C33A Os1 C34A 36.1(11) . . ?
C33A Os1 C35A 60.2(11) . . ?
C32A Os1 C31A 37.8(11) . . ?
C32A Os1 C34A 58.3(13) . . ?
C32A Os1 C35A 59.1(12) . . ?
C31A Os1 C34A 61.6(11) . . ?
C31A Os1 C35A 37.1(12) . . ?
C35A Os1 C34A 35.3(9) . . ?
C31 Os1 C32 38.5(9) . . ?
C35 Os1 C31 38.7(9) . . ?
C35 Os1 C34 38.6(12) . . ?
C35 Os1 C32 64.5(9) . . ?
C35 Os1 C33 65.5(12) . . ?
C34 Os1 C31 62.4(12) . . ?
C34 Os1 C32 60.9(11) . . ?
C34 Os1 C33 39.0(11) . . ?
C33 Os1 C31 62.0(11) . . ?
C33 Os1 C32 33.9(10) . . ?
Os4 U1 Os3 47.702(13) . . ?
Os4 U1 Os2 118.43(2) . . ?
Os4 U1 Os1 122.88(2) . . ?
Os4 U1 C1 45.61(16) . . ?
Os2 U1 Os3 106.66(2) . . ?
Os1 U1 Os3 107.68(2) . . ?
Os1 U1 Os2 118.15(2) . . ?
C1 U1 Os3 93.29(16) . . ?
C1 U1 Os2 113.11(16) . . ?
C1 U1 Os1 114.42(16) . . ?
Os3 U1A Os4 46.225(13) . . ?
Os3 U1A Os2 119.52(2) . . ?
Os3 U1A Os1 118.90(2) . . ?
Os3 U1A C22 45.32(14) . . ?
Os2 U1A Os4 105.36(2) . . ?
Os2 U1A Os1 120.74(2) . . ?
Os1 U1A Os4 107.23(2) . . ?
C22 U1A Os4 91.54(14) . . ?
C22 U1A Os2 115.66(15) . . ?
C22 U1A Os1 111.43(15) . . ?
C2 C3 Os4 71.4(4) . . ?
C2 C3 C8 125.7(8) . . ?
C4 C3 Os4 70.5(4) . . ?
C4 C3 C2 107.5(7) . . ?
C4 C3 C8 126.7(9) . . ?
C8 C3 Os4 126.9(5) . . ?
C3 C2 Os4 70.1(4) . . ?
C3 C2 C7 124.2(8) . . ?
C1 C2 Os4 72.5(4) . . ?
C1 C2 C3 108.4(7) . . ?
C1 C2 C7 127.0(9) . . ?
C7 C2 Os4 128.6(6) . . ?
Os3 C22 U1A 64.98(17) . . ?
C21 C22 Os3 69.9(4) . . ?
C21 C22 U1A 105.8(4) . . ?
C21 C22 C23 106.8(6) . . ?
C21 C22 C27 126.2(7) . . ?
C23 C22 Os3 70.5(4) . . ?
C23 C22 U1A 109.2(5) . . ?
C23 C22 C27 126.9(7) . . ?
C27 C22 Os3 127.0(5) . . ?
C27 C22 U1A 62.1(4) . . ?
C23 C24 Os3 71.6(4) . . ?
C23 C24 C29 125.9(7) . . ?
C23 C24 C25 108.1(6) . . ?
C29 C24 Os3 124.9(5) . . ?
C25 C24 Os3 70.8(4) . . ?
C25 C24 C29 126.0(7) . . ?
Os4 C1 U1 63.00(18) . . ?
C2 C1 Os4 70.0(4) . . ?
C2 C1 U1 101.9(5) . . ?
C2 C1 C6 125.9(8) . . ?
C2 C1 C5 107.3(8) . . ?
C6 C1 Os4 126.0(5) . . ?
C6 C1 U1 63.1(4) . . ?
C5 C1 Os4 69.0(4) . . ?
C5 C1 U1 108.9(5) . . ?
C5 C1 C6 126.8(8) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C22 C21 Os3 72.1(4) . . ?
C22 C21 C26 124.1(7) . . ?
C25 C21 Os3 71.3(4) . . ?
C25 C21 C22 109.3(6) . . ?
C25 C21 C26 126.3(7) . . ?
C26 C21 Os3 128.0(5) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C22 C23 Os3 71.5(4) . . ?
C22 C23 C28 125.8(7) . . ?
C24 C23 Os3 70.7(4) . . ?
C24 C23 C22 108.6(6) . . ?
C24 C23 C28 125.6(7) . . ?
C28 C23 Os3 124.9(5) . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C1 C5 Os4 73.2(4) . . ?
C1 C5 C10 124.3(8) . . ?
C4 C5 Os4 70.9(4) . . ?
C4 C5 C1 109.3(7) . . ?
C4 C5 C10 126.2(8) . . ?
C10 C5 Os4 125.7(6) . . ?
C3 C4 Os4 70.9(4) . . ?
C3 C4 C9 125.2(8) . . ?
C5 C4 Os4 71.0(5) . . ?
C5 C4 C3 107.4(8) . . ?
C5 C4 C9 127.3(8) . . ?
C9 C4 Os4 125.2(6) . . ?
C24 C25 Os3 70.7(4) . . ?
C24 C25 C30 126.0(7) . . ?
C21 C25 Os3 71.0(4) . . ?
C21 C25 C24 107.2(6) . . ?
C21 C25 C30 126.7(7) . . ?
C30 C25 Os3 125.5(5) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C11 C12 Os2 71.7(5) . . ?
C11 C12 C17 125.2(13) . . ?
C13 C12 Os2 71.8(5) . . ?
C13 C12 C11 107.3(9) . . ?
C13 C12 C17 127.3(12) . . ?
C17 C12 Os2 126.8(7) . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C12 C11 Os2 70.9(6) . . ?
C12 C11 C16 124.9(13) . . ?
C16 C11 Os2 127.5(9) . . ?
C15 C11 Os2 71.7(5) . . ?
C15 C11 C12 107.9(10) . . ?
C15 C11 C16 127.0(13) . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C13 Os2 71.5(5) . . ?
C12 C13 C14 108.3(9) . . ?
C12 C13 C18 126.0(10) . . ?
C14 C13 Os2 71.9(5) . . ?
C14 C13 C18 125.4(11) . . ?
C18 C13 Os2 127.4(6) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
C13 C14 Os2 70.9(5) . . ?
C13 C14 C19 125.9(11) . . ?
C15 C14 Os2 71.3(5) . . ?
C15 C14 C13 107.4(9) . . ?
C15 C14 C19 126.7(10) . . ?
C19 C14 Os2 124.1(7) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C11 C15 Os2 72.0(6) . . ?
C11 C15 C20 127.1(12) . . ?
C11 C15 C14 109.2(9) . . ?
C20 C15 Os2 126.9(6) . . ?
C14 C15 Os2 72.2(5) . . ?
C14 C15 C20 123.4(11) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C32A C33A Os1 74(2) . . ?
C32A C33A C34A 109(3) . . ?
C32A C33A C38A 129(3) . . ?
C34A C33A Os1 79.7(16) . . ?
C34A C33A C38A 119(3) . . ?
C38A C33A Os1 127(2) . . ?
C33A C32A Os1 71(2) . . ?
C33A C32A C31A 112(4) . . ?
C33A C32A C37A 127(3) . . ?
C31A C32A Os1 71.4(17) . . ?
C31A C32A C37A 120(4) . . ?
C37A C32A Os1 119(3) . . ?
C32A C31A Os1 70.8(16) . . ?
C32A C31A C35A 101(3) . . ?
C35A C31A Os1 74.1(14) . . ?
C36A C31A Os1 128.3(18) . . ?
C36A C31A C32A 134(4) . . ?
C36A C31A C35A 123(4) . . ?
C33A C34A Os1 64.3(18) . . ?
C33A C34A C39A 131(3) . . ?
C35A C34A Os1 69.4(14) . . ?
C35A C34A C33A 105(3) . . ?
C35A C34A C39A 124(3) . . ?
C39A C34A Os1 127.7(15) . . ?
C31A C35A Os1 68.7(14) . . ?
C31A C35A C40A 127(3) . . ?
C34A C35A Os1 75.3(15) . . ?
C34A C35A C31A 111(2) . . ?
C34A C35A C40A 121(3) . . ?
C40A C35A Os1 131.8(15) . . ?
C35 C31 Os1 65.7(12) . . ?
C35 C31 C32 106(2) . . ?
C35 C31 C36 122(3) . . ?
C32 C31 Os1 72.9(12) . . ?
C32 C31 C36 131(3) . . ?
C36 C31 Os1 125.9(19) . . ?
C31 C35 Os1 75.6(14) . . ?
C31 C35 C40 125(3) . . ?
C34 C35 Os1 72.1(17) . . ?
C34 C35 C31 106(3) . . ?
C34 C35 C40 129(3) . . ?
C40 C35 Os1 124.3(16) . . ?
C35 C34 Os1 69.3(17) . . ?
C35 C34 C33 110(3) . . ?
C35 C34 C39 120(3) . . ?
C33 C34 Os1 73.3(18) . . ?
C39 C34 Os1 126.1(19) . . ?
C39 C34 C33 130(3) . . ?
C31 C32 Os1 68.6(11) . . ?
C31 C32 C37 121(3) . . ?
C33 C32 Os1 69.7(15) . . ?
C33 C32 C31 109(2) . . ?
C33 C32 C37 130(3) . . ?
C37 C32 Os1 132.6(16) . . ?
C34 C33 Os1 67.7(17) . . ?
C34 C33 C38 127(3) . . ?
C32 C33 Os1 76.4(17) . . ?
C32 C33 C34 109(3) . . ?
C32 C33 C38 124(3) . . ?
C38 C33 Os1 131.0(19) . . ?
C33A C38A H38A 109.5 . . ?
C33A C38A H38B 109.5 . . ?
C33A C38A H38C 109.5 . . ?
H38A C38A H38B 109.5 . . ?
H38A C38A H38C 109.5 . . ?
H38B C38A H38C 109.5 . . ?
C34A C39A H39A 109.5 . . ?
C34A C39A H39B 109.5 . . ?
C34A C39A H39C 109.5 . . ?
H39A C39A H39B 109.5 . . ?
H39A C39A H39C 109.5 . . ?
H39B C39A H39C 109.5 . . ?
C33 C38 H38D 109.5 . . ?
C33 C38 H38E 109.5 . . ?
C33 C38 H38F 109.5 . . ?
H38D C38 H38E 109.5 . . ?
H38D C38 H38F 109.5 . . ?
H38E C38 H38F 109.5 . . ?
C34 C39 H39D 109.5 . . ?
C34 C39 H39E 109.5 . . ?
C34 C39 H39F 109.5 . . ?
H39D C39 H39E 109.5 . . ?
H39D C39 H39F 109.5 . . ?
H39E C39 H39F 109.5 . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C40 H40A 109.5 . . ?
C35 C40 H40B 109.5 . . ?
C35 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
C31 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35A C40A H40D 109.5 . . ?
C35A C40A H40E 109.5 . . ?
C35A C40A H40F 109.5 . . ?
H40D C40A H40E 109.5 . . ?
H40D C40A H40F 109.5 . . ?
H40E C40A H40F 109.5 . . ?
C32A C37A H37D 109.5 . . ?
C32A C37A H37E 109.5 . . ?
C32A C37A H37F 109.5 . . ?
H37D C37A H37E 109.5 . . ?
H37D C37A H37F 109.5 . . ?
H37E C37A H37F 109.5 . . ?
C31A C36A H36D 109.5 . . ?
C31A C36A H36E 109.5 . . ?
C31A C36A H36F 109.5 . . ?
H36D C36A H36E 109.5 . . ?
H36D C36A H36F 109.5 . . ?
H36E C36A H36F 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
Os3 C22 C21 C25 61.9(5) . . . . ?
Os3 C22 C21 C26 -124.2(7) . . . . ?
Os3 C22 C23 C24 -61.4(5) . . . . ?
Os3 C22 C23 C28 120.2(7) . . . . ?
Os3 C24 C23 C22 61.9(5) . . . . ?
Os3 C24 C23 C28 -119.7(7) . . . . ?
Os3 C24 C25 C21 -61.9(5) . . . . ?
Os3 C24 C25 C30 120.4(7) . . . . ?
Os3 C21 C25 C24 61.7(5) . . . . ?
Os3 C21 C25 C30 -120.6(7) . . . . ?
Os4 C3 C2 C1 62.8(5) . . . . ?
Os4 C3 C2 C7 -123.8(7) . . . . ?
Os4 C3 C4 C5 -62.0(5) . . . . ?
Os4 C3 C4 C9 120.2(8) . . . . ?
Os4 C2 C1 U1 -55.2(3) . . . . ?
Os4 C2 C1 C6 -120.5(7) . . . . ?
Os4 C2 C1 C5 59.1(5) . . . . ?
Os4 C1 C5 C4 62.1(5) . . . . ?
Os4 C1 C5 C10 -122.1(8) . . . . ?
Os4 C5 C4 C3 62.0(5) . . . . ?
Os4 C5 C4 C9 -120.3(8) . . . . ?
Os2 C12 C11 C16 -122.9(12) . . . . ?
Os2 C12 C11 C15 62.5(6) . . . . ?
Os2 C12 C13 C14 -62.9(6) . . . . ?
Os2 C12 C13 C18 123.2(9) . . . . ?
Os2 C11 C15 C20 -123.0(10) . . . . ?
Os2 C11 C15 C14 63.0(6) . . . . ?
Os2 C13 C14 C15 -62.4(6) . . . . ?
Os2 C13 C14 C19 118.9(9) . . . . ?
Os2 C14 C15 C11 -62.9(7) . . . . ?
Os2 C14 C15 C20 122.9(8) . . . . ?
Os1 C33A C32A C31A 59(2) . . . . ?
Os1 C33A C32A C37A -112(4) . . . . ?
Os1 C33A C34A C35A -58.1(17) . . . . ?
Os1 C33A C34A C39A 119(2) . . . . ?
Os1 C32A C31A C35A 68.6(15) . . . . ?
Os1 C32A C31A C36A -125(3) . . . . ?
Os1 C31A C35A C34A 63.7(16) . . . . ?
Os1 C31A C35A C40A -127(2) . . . . ?
Os1 C34A C35A C31A -59.7(15) . . . . ?
Os1 C34A C35A C40A 130(2) . . . . ?
Os1 C31 C35 C34 66.3(17) . . . . ?
Os1 C31 C35 C40 -122(2) . . . . ?
Os1 C31 C32 C33 -58.1(17) . . . . ?
Os1 C31 C32 C37 127.8(19) . . . . ?
Os1 C35 C34 C33 62.5(19) . . . . ?
Os1 C35 C34 C39 -121(2) . . . . ?
Os1 C34 C33 C32 66.1(19) . . . . ?
Os1 C34 C33 C38 -125(3) . . . . ?
Os1 C32 C33 C34 -60.5(18) . . . . ?
Os1 C32 C33 C38 131(3) . . . . ?
U1 C1 C5 Os4 49.8(3) . . . . ?
U1 C1 C5 C4 111.9(6) . . . . ?
U1 C1 C5 C10 -72.3(8) . . . . ?
U1A C22 C21 Os3 55.2(3) . . . . ?
U1A C22 C21 C25 117.1(5) . . . . ?
U1A C22 C21 C26 -69.1(7) . . . . ?
U1A C22 C23 Os3 -53.2(3) . . . . ?
U1A C22 C23 C24 -114.6(5) . . . . ?
U1A C22 C23 C28 67.0(8) . . . . ?
C3 C2 C1 Os4 -61.2(5) . . . . ?
C3 C2 C1 U1 -116.5(5) . . . . ?
C3 C2 C1 C6 178.2(7) . . . . ?
C3 C2 C1 C5 -2.1(8) . . . . ?
C2 C3 C4 Os4 62.3(5) . . . . ?
C2 C3 C4 C5 0.2(8) . . . . ?
C2 C3 C4 C9 -177.6(7) . . . . ?
C2 C1 C5 Os4 -59.8(5) . . . . ?
C2 C1 C5 C4 2.3(8) . . . . ?
C2 C1 C5 C10 178.1(7) . . . . ?
C22 C21 C25 Os3 -62.4(5) . . . . ?
C22 C21 C25 C24 -0.7(8) . . . . ?
C22 C21 C25 C30 177.0(7) . . . . ?
C1 C5 C4 Os4 -63.5(5) . . . . ?
C1 C5 C4 C3 -1.6(8) . . . . ?
C1 C5 C4 C9 176.2(7) . . . . ?
C7 C2 C1 Os4 125.5(8) . . . . ?
C7 C2 C1 U1 70.3(8) . . . . ?
C7 C2 C1 C6 5.0(13) . . . . ?
C7 C2 C1 C5 -175.3(7) . . . . ?
C21 C22 C23 Os3 60.8(5) . . . . ?
C21 C22 C23 C24 -0.6(8) . . . . ?
C21 C22 C23 C28 -179.0(7) . . . . ?
C6 C1 C5 Os4 119.9(8) . . . . ?
C6 C1 C5 C4 -178.0(7) . . . . ?
C6 C1 C5 C10 -2.2(12) . . . . ?
C23 C22 C21 Os3 -61.2(5) . . . . ?
C23 C22 C21 C25 0.8(8) . . . . ?
C23 C22 C21 C26 174.6(7) . . . . ?
C23 C24 C25 Os3 62.3(5) . . . . ?
C23 C24 C25 C21 0.3(8) . . . . ?
C23 C24 C25 C30 -177.4(7) . . . . ?
C29 C24 C23 Os3 120.2(7) . . . . ?
C29 C24 C23 C22 -177.9(7) . . . . ?
C29 C24 C23 C28 0.5(12) . . . . ?
C29 C24 C25 Os3 -119.7(7) . . . . ?
C29 C24 C25 C21 178.4(7) . . . . ?
C29 C24 C25 C30 0.7(11) . . . . ?
C4 C3 C2 Os4 -61.6(5) . . . . ?
C4 C3 C2 C1 1.2(8) . . . . ?
C4 C3 C2 C7 174.6(7) . . . . ?
C25 C24 C23 Os3 -61.7(5) . . . . ?
C25 C24 C23 C22 0.2(8) . . . . ?
C25 C24 C23 C28 178.6(7) . . . . ?
C8 C3 C2 Os4 122.6(8) . . . . ?
C8 C3 C2 C1 -174.6(7) . . . . ?
C8 C3 C2 C7 -1.2(12) . . . . ?
C8 C3 C4 Os4 -122.0(8) . . . . ?
C8 C3 C4 C5 176.0(7) . . . . ?
C8 C3 C4 C9 -1.9(12) . . . . ?
C26 C21 C25 Os3 123.9(7) . . . . ?
C26 C21 C25 C24 -174.3(7) . . . . ?
C26 C21 C25 C30 3.3(12) . . . . ?
C12 C11 C15 Os2 -62.0(7) . . . . ?
C12 C11 C15 C20 174.9(9) . . . . ?
C12 C11 C15 C14 1.0(11) . . . . ?
C12 C13 C14 Os2 62.6(6) . . . . ?
C12 C13 C14 C15 0.2(10) . . . . ?
C12 C13 C14 C19 -178.5(9) . . . . ?
C11 C12 C13 Os2 63.3(6) . . . . ?
C11 C12 C13 C14 0.4(10) . . . . ?
C11 C12 C13 C18 -173.5(8) . . . . ?
C13 C12 C11 Os2 -63.4(6) . . . . ?
C13 C12 C11 C16 173.7(11) . . . . ?
C13 C12 C11 C15 -0.8(11) . . . . ?
C13 C14 C15 Os2 62.1(6) . . . . ?
C13 C14 C15 C11 -0.8(10) . . . . ?
C13 C14 C15 C20 -175.0(8) . . . . ?
C17 C12 C11 Os2 122.6(10) . . . . ?
C17 C12 C11 C16 -0.3(17) . . . . ?
C17 C12 C11 C15 -174.9(9) . . . . ?
C17 C12 C13 Os2 -122.8(10) . . . . ?
C17 C12 C13 C14 174.3(9) . . . . ?
C17 C12 C13 C18 0.4(15) . . . . ?
C27 C22 C21 Os3 121.8(7) . . . . ?
C27 C22 C21 C25 -176.2(7) . . . . ?
C27 C22 C21 C26 -2.4(11) . . . . ?
C27 C22 C23 Os3 -122.2(7) . . . . ?
C27 C22 C23 C24 176.4(7) . . . . ?
C27 C22 C23 C28 -2.0(12) . . . . ?
C16 C11 C15 Os2 123.6(12) . . . . ?
C16 C11 C15 C20 0.5(17) . . . . ?
C16 C11 C15 C14 -173.4(11) . . . . ?
C10 C5 C4 Os4 120.8(8) . . . . ?
C10 C5 C4 C3 -177.3(7) . . . . ?
C10 C5 C4 C9 0.5(13) . . . . ?
C18 C13 C14 Os2 -123.5(9) . . . . ?
C18 C13 C14 C15 174.1(8) . . . . ?
C18 C13 C14 C19 -4.6(14) . . . . ?
C19 C14 C15 Os2 -119.2(9) . . . . ?
C19 C14 C15 C11 177.9(9) . . . . ?
C19 C14 C15 C20 3.7(14) . . . . ?
C33A C32A C31A Os1 -59(3) . . . . ?
C33A C32A C31A C35A 10(3) . . . . ?
C33A C32A C31A C36A 176(3) . . . . ?
C33A C34A C35A Os1 54.8(19) . . . . ?
C33A C34A C35A C31A -5(3) . . . . ?
C33A C34A C35A C40A -175(2) . . . . ?
C32A C33A C34A Os1 69(3) . . . . ?
C32A C33A C34A C35A 11(3) . . . . ?
C32A C33A C34A C39A -172(3) . . . . ?
C32A C31A C35A Os1 -66.1(17) . . . . ?
C32A C31A C35A C34A -2(2) . . . . ?
C32A C31A C35A C40A 167(2) . . . . ?
C34A C33A C32A Os1 -73(2) . . . . ?
C34A C33A C32A C31A -13(4) . . . . ?
C34A C33A C32A C37A 175(3) . . . . ?
C31 C35 C34 Os1 -68.7(16) . . . . ?
C31 C35 C34 C33 -6(3) . . . . ?
C31 C35 C34 C39 171(2) . . . . ?
C31 C32 C33 Os1 57.4(15) . . . . ?
C31 C32 C33 C34 -3(3) . . . . ?
C31 C32 C33 C38 -172(2) . . . . ?
C35 C31 C32 Os1 57.4(14) . . . . ?
C35 C31 C32 C33 -1(2) . . . . ?
C35 C31 C32 C37 -174.9(19) . . . . ?
C35 C34 C33 Os1 -60.0(19) . . . . ?
C35 C34 C33 C32 6(3) . . . . ?
C35 C34 C33 C38 175(3) . . . . ?
C32 C31 C35 Os1 -62.0(14) . . . . ?
C32 C31 C35 C34 4(2) . . . . ?
C32 C31 C35 C40 176(2) . . . . ?
C38A C33A C32A Os1 125(4) . . . . ?
C38A C33A C32A C31A -176(3) . . . . ?
C38A C33A C32A C37A 13(7) . . . . ?
C38A C33A C34A Os1 -127(3) . . . . ?
C38A C33A C34A C35A 175(3) . . . . ?
C38A C33A C34A C39A -8(5) . . . . ?
C39A C34A C35A Os1 -122(2) . . . . ?
C39A C34A C35A C31A 178(2) . . . . ?
C39A C34A C35A C40A 8(3) . . . . ?
C39 C34 C33 Os1 123(3) . . . . ?
C39 C34 C33 C32 -170(3) . . . . ?
C39 C34 C33 C38 -2(5) . . . . ?
C37 C32 C33 Os1 -129(2) . . . . ?
C37 C32 C33 C34 170(2) . . . . ?
C37 C32 C33 C38 1(4) . . . . ?
C40 C35 C34 Os1 120(2) . . . . ?
C40 C35 C34 C33 -178(2) . . . . ?
C40 C35 C34 C39 -1(4) . . . . ?
C36 C31 C35 Os1 118(2) . . . . ?
C36 C31 C35 C34 -175(2) . . . . ?
C36 C31 C35 C40 -4(4) . . . . ?
C36 C31 C32 Os1 -123(3) . . . . ?
C36 C31 C32 C33 179(3) . . . . ?
C36 C31 C32 C37 5(4) . . . . ?
C37A C32A C31A Os1 113(3) . . . . ?
C37A C32A C31A C35A -178(3) . . . . ?
C37A C32A C31A C36A -12(5) . . . . ?
C36A C31A C35A Os1 126(2) . . . . ?
C36A C31A C35A C34A -171(2) . . . . ?
C36A C31A C35A C40A -1(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.238 0.250 121.5 0.0 ?
2 0.000 0.238 0.750 121.5 0.0 ?
3 0.158 0.050 0.986 7.2 0.0 ?
4 0.158 0.950 0.486 7.2 0.0 ?
5 0.195 -0.006 0.285 14.8 6.1 ?
6 0.195 0.006 0.785 14.8 6.1 ?
7 0.305 0.494 0.215 14.8 6.4 ?
8 0.305 0.506 0.715 14.8 6.5 ?
9 0.342 0.450 0.014 7.2 0.0 ?
10 0.342 0.550 0.514 7.2 0.0 ?
11 0.500 0.262 0.250 121.5 0.0 ?
12 0.500 0.738 0.750 121.5 0.0 ?
13 0.658 0.450 0.486 7.2 0.0 ?
14 0.658 0.550 0.986 7.2 0.0 ?
15 0.695 0.494 0.285 14.8 6.1 ?
16 0.695 0.506 0.785 14.8 6.1 ?
17 0.805 -0.006 0.215 14.8 6.4 ?
18 0.805 0.006 0.715 14.8 6.5 ?
19 0.842 0.050 0.514 7.2 0.0 ?
20 0.842 0.950 0.014 7.2 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_czy_ii_125_0m
_database_code_depnum_ccdc_archive 'CCDC 2346842'
loop_
_audit_author_name
_audit_author_address
'Christopher Ye'
;UC Berkeley
United States of America
;
_audit_update_record             
;
2024-04-08 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_audit_creation_date             2023-05-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.333(C30 H45 Os3), C30 H45 Os3 U'
_chemical_formula_sum            'C40 H60 Os4 U'
_chemical_formula_weight         1539.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Os Os -1.2848 7.9466 'Calculated using XDISP in WinGX (Farrugia, 1999)'
U U -10.9608 4.1580 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   21.395(2)
_cell_length_b                   21.395(2)
_cell_length_c                   21.395(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9793(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    125415
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.804
_cell_measurement_theta_min      1.952
_shelx_estimated_absorpt_T_max   0.574
_shelx_estimated_absorpt_T_min   0.368
_exptl_absorpt_coefficient_mu    12.483
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.4843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1747 before and 0.1221 after correction.
The Ratio of minimum to maximum transmission is 0.6509.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1087
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            125415
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.804
_diffrn_reflns_theta_min         1.952
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II CPAD detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3289
_reflns_number_total             3605
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.352
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.301
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3605
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0530P)²+52.5146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0986
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid body (RIGU) restrains
 C2, C3, C4, C5, C6, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
2. Others
 Fixed Sof: C2(0.3333) C3(0.3333) C4(0.3333) C5(0.3333) C6(0.3333) C7(0.3333)
 H7A(0.3333) H7B(0.3333) H7C(0.3333) C8(0.3333) H8A(0.3333) H8B(0.3333)
 H8C(0.3333) C9(0.3333) H9A(0.3333) H9B(0.3333) H9C(0.3333) C10(0.3333)
 H10A(0.3333) H10B(0.3333) H10C(0.3333) C11(0.3333) H11A(0.3333) H11B(0.3333)
 H11C(0.3333)
3.a Idealised Me refined as rotating group:
 C00B(H00A,H00B,H00C), C00C(H00D,H00E,H00F), C00D(H00G,H00H,H00I), C00E(H00J,
 H00K,H00L), C00F(H00M,H00N,H00O), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,
 H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Os2 Os 0.60228(2) 0.60228(2) 0.60228(2) 0.02370(12) Uani 1 3 d S T P . .
U1 U 0.68186(2) 0.68186(2) 0.68186(2) 0.02398(12) Uani 1 3 d S T P . .
Os1 Os 0.66991(2) 0.64662(2) 0.81463(2) 0.02869(11) Uani 1 1 d . . . . .
C004 C 0.6185(4) 0.6593(4) 0.9058(3) 0.0380(16) Uani 1 1 d . . . . .
C005 C 0.6807(3) 0.6832(4) 0.9118(3) 0.0368(16) Uani 1 1 d . . . . .
C006 C 0.6876(4) 0.5771(4) 0.8904(3) 0.0404(18) Uani 1 1 d . . . . .
C008 C 0.6227(4) 0.5949(4) 0.8925(3) 0.0387(17) Uani 1 1 d . . . . .
C00A C 0.7233(3) 0.6345(4) 0.9026(3) 0.0362(16) Uani 1 1 d . . . . .
C00B C 0.7120(6) 0.5131(5) 0.8837(4) 0.064(3) Uani 1 1 d . . . . .
H00A H 0.6800 0.4864 0.8647 0.096 Uiso 1 1 calc R U . . .
H00B H 0.7231 0.4966 0.9249 0.096 Uiso 1 1 calc R U . . .
H00C H 0.7492 0.5137 0.8569 0.096 Uiso 1 1 calc R U . . .
C00C C 0.7930(4) 0.6384(6) 0.9093(4) 0.062(3) Uani 1 1 d . . . . .
H00D H 0.8129 0.6103 0.8790 0.092 Uiso 1 1 calc R U . . .
H00E H 0.8050 0.6260 0.9518 0.092 Uiso 1 1 calc R U . . .
H00F H 0.8068 0.6814 0.9016 0.092 Uiso 1 1 calc R U . . .
C00D C 0.5594(4) 0.6961(5) 0.9156(5) 0.057(2) Uani 1 1 d . . . . .
H00G H 0.5599 0.7333 0.8888 0.086 Uiso 1 1 calc R U . . .
H00H H 0.5565 0.7089 0.9595 0.086 Uiso 1 1 calc R U . . .
H00I H 0.5232 0.6701 0.9049 0.086 Uiso 1 1 calc R U . . .
C00E C 0.5673(5) 0.5480(5) 0.8889(5) 0.064(3) Uani 1 1 d . . . . .
H00J H 0.5291 0.5704 0.8774 0.095 Uiso 1 1 calc R U . . .
H00K H 0.5616 0.5280 0.9297 0.095 Uiso 1 1 calc R U . . .
H00L H 0.5764 0.5160 0.8574 0.095 Uiso 1 1 calc R U . . .
C00F C 0.6962(5) 0.7489(4) 0.9320(4) 0.054(2) Uani 1 1 d . . . . .
H00M H 0.7272 0.7667 0.9034 0.082 Uiso 1 1 calc R U . . .
H00N H 0.7131 0.7482 0.9745 0.082 Uiso 1 1 calc R U . . .
H00O H 0.6582 0.7745 0.9310 0.082 Uiso 1 1 calc R U . . .
C2 C 0.5195(19) 0.5409(18) 0.5945(13) 0.023(4) Uani 0.3333 1 d . U P A -1
C3 C 0.579(2) 0.5093(13) 0.5676(18) 0.023(5) Uani 0.3333 1 d . U P A -1
C4 C 0.5966(15) 0.5419(16) 0.515(2) 0.020(5) Uani 0.3333 1 d . U P A -1
C5 C 0.5560(17) 0.5946(15) 0.5061(15) 0.026(6) Uani 0.3333 1 d . U P A -1
C6 C 0.5097(14) 0.5906(19) 0.5553(17) 0.018(5) Uani 0.3333 1 d . U P A -1
C7 C 0.4556(11) 0.6423(11) 0.5540(14) 0.041(5) Uani 0.3333 1 d . U P A -1
H7A H 0.4353 0.6442 0.5950 0.061 Uiso 0.3333 1 calc R U P A -1
H7B H 0.4247 0.6312 0.5221 0.061 Uiso 0.3333 1 calc R U P A -1
H7C H 0.4738 0.6832 0.5441 0.061 Uiso 0.3333 1 calc R U P A -1
C8 C 0.5609(15) 0.6362(12) 0.4496(11) 0.042(5) Uani 0.3333 1 d . U P A -1
H8A H 0.6030 0.6542 0.4475 0.063 Uiso 0.3333 1 calc R U P A -1
H8B H 0.5301 0.6700 0.4528 0.063 Uiso 0.3333 1 calc R U P A -1
H8C H 0.5528 0.6117 0.4118 0.063 Uiso 0.3333 1 calc R U P A -1
C9 C 0.6506(12) 0.5191(15) 0.4750(14) 0.051(6) Uani 0.3333 1 d . U P A -1
H9A H 0.6675 0.5541 0.4509 0.076 Uiso 0.3333 1 calc R U P A -1
H9B H 0.6356 0.4866 0.4464 0.076 Uiso 0.3333 1 calc R U P A -1
H9C H 0.6834 0.5017 0.5019 0.076 Uiso 0.3333 1 calc R U P A -1
C10 C 0.5957(15) 0.4507(10) 0.5999(14) 0.054(6) Uani 0.3333 1 d . U P A -1
H10A H 0.6407 0.4506 0.6085 0.081 Uiso 0.3333 1 calc R U P A -1
H10B H 0.5851 0.4149 0.5733 0.081 Uiso 0.3333 1 calc R U P A -1
H10C H 0.5727 0.4477 0.6394 0.081 Uiso 0.3333 1 calc R U P A -1
C11 C 0.4730(14) 0.5268(13) 0.6464(12) 0.047(5) Uani 0.3333 1 d . U P A -1
H11A H 0.4894 0.4931 0.6728 0.071 Uiso 0.3333 1 calc R U P A -1
H11B H 0.4331 0.5139 0.6281 0.071 Uiso 0.3333 1 calc R U P A -1
H11C H 0.4668 0.5644 0.6719 0.071 Uiso 0.3333 1 calc R U P A -1


_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
Os2 U1 2.9490(6) . ?
Os2 C2 2.21(3) . ?
Os2 C3 2.18(3) . ?
Os2 C4 2.27(4) . ?
Os2 C5 2.29(3) . ?
Os2 C6 2.23(4) . ?
U1 Os1 2.9501(4) 5 ?
U1 Os1 2.9501(4) . ?
U1 Os1 2.9501(4) 9 ?
Os1 C004 2.255(8) . ?
Os1 C005 2.234(7) . ?
Os1 C006 2.233(7) . ?
Os1 C008 2.240(7) . ?
Os1 C00A 2.216(6) . ?
C004 C005 1.432(11) . ?
C004 C008 1.410(11) . ?
C004 C00D 1.506(11) . ?
C005 C00A 1.397(11) . ?
C005 C00F 1.506(11) . ?
C006 C008 1.440(11) . ?
C006 C00A 1.469(12) . ?
C006 C00B 1.473(12) . ?
C008 C00E 1.554(12) . ?
C00A C00C 1.502(11) . ?
C00B H00A 0.9800 . ?
C00B H00B 0.9800 . ?
C00B H00C 0.9800 . ?
C00C H00D 0.9800 . ?
C00C H00E 0.9800 . ?
C00C H00F 0.9800 . ?
C00D H00G 0.9800 . ?
C00D H00H 0.9800 . ?
C00D H00I 0.9800 . ?
C00E H00J 0.9800 . ?
C00E H00K 0.9800 . ?
C00E H00L 0.9800 . ?
C00F H00M 0.9800 . ?
C00F H00N 0.9800 . ?
C00F H00O 0.9800 . ?
C2 C3 1.54(4) . ?
C2 C6 1.37(3) . ?
C2 C11 1.52(4) . ?
C3 C4 1.37(4) . ?
C3 C10 1.48(4) . ?
C4 C5 1.44(4) . ?
C4 C9 1.52(4) . ?
C5 C6 1.45(4) . ?
C5 C8 1.51(4) . ?
C6 C7 1.60(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

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
C2 Os2 U1 148.1(8) . . ?
C2 Os2 C4 63.7(10) . . ?
C2 Os2 C5 62.8(10) . . ?
C2 Os2 C6 35.9(9) . . ?
C3 Os2 U1 148.9(8) . . ?
C3 Os2 C2 41.1(9) . . ?
C3 Os2 C4 35.9(10) . . ?
C3 Os2 C5 61.9(10) . . ?
C3 Os2 C6 62.6(10) . . ?
C4 Os2 U1 146.4(9) . . ?
C4 Os2 C5 36.8(9) . . ?
C5 Os2 U1 144.1(8) . . ?
C6 Os2 U1 146.7(9) . . ?
C6 Os2 C4 61.3(7) . . ?
C6 Os2 C5 37.3(10) . . ?
Os2 U1 Os1 110.998(9) . 9 ?
Os2 U1 Os1 110.998(9) . 5 ?
Os2 U1 Os1 110.999(9) . . ?
Os1 U1 Os1 107.902(9) 9 5 ?
Os1 U1 Os1 107.903(9) 9 . ?
Os1 U1 Os1 107.900(9) 5 . ?
C004 Os1 U1 147.61(19) . . ?
C005 Os1 U1 142.9(2) . . ?
C005 Os1 C004 37.2(3) . . ?
C005 Os1 C008 61.8(3) . . ?
C006 Os1 U1 148.76(19) . . ?
C006 Os1 C004 62.2(3) . . ?
C006 Os1 C005 62.6(3) . . ?
C006 Os1 C008 37.5(3) . . ?
C008 Os1 U1 151.8(2) . . ?
C008 Os1 C004 36.5(3) . . ?
C00A Os1 U1 143.40(19) . . ?
C00A Os1 C004 62.0(3) . . ?
C00A Os1 C005 36.6(3) . . ?
C00A Os1 C006 38.6(3) . . ?
C00A Os1 C008 62.8(3) . . ?
C005 C004 Os1 70.6(4) . . ?
C005 C004 C00D 125.6(8) . . ?
C008 C004 Os1 71.2(4) . . ?
C008 C004 C005 108.0(7) . . ?
C008 C004 C00D 126.3(8) . . ?
C00D C004 Os1 126.4(6) . . ?
C004 C005 Os1 72.2(4) . . ?
C004 C005 C00F 124.3(7) . . ?
C00A C005 Os1 71.0(4) . . ?
C00A C005 C004 109.0(7) . . ?
C00A C005 C00F 126.4(7) . . ?
C00F C005 Os1 128.0(6) . . ?
C008 C006 Os1 71.5(4) . . ?
C008 C006 C00A 105.9(6) . . ?
C008 C006 C00B 126.2(9) . . ?
C00A C006 Os1 70.1(4) . . ?
C00A C006 C00B 127.6(8) . . ?
C00B C006 Os1 127.5(5) . . ?
C004 C008 Os1 72.3(4) . . ?
C004 C008 C006 109.0(7) . . ?
C004 C008 C00E 126.3(8) . . ?
C006 C008 Os1 70.9(4) . . ?
C006 C008 C00E 124.3(8) . . ?
C00E C008 Os1 128.7(6) . . ?
C005 C00A Os1 72.4(4) . . ?
C005 C00A C006 108.1(6) . . ?
C005 C00A C00C 126.3(8) . . ?
C006 C00A Os1 71.4(4) . . ?
C006 C00A C00C 125.4(8) . . ?
C00C C00A Os1 125.9(5) . . ?
C006 C00B H00A 109.5 . . ?
C006 C00B H00B 109.5 . . ?
C006 C00B H00C 109.5 . . ?
H00A C00B H00B 109.5 . . ?
H00A C00B H00C 109.5 . . ?
H00B C00B H00C 109.5 . . ?
C00A C00C H00D 109.5 . . ?
C00A C00C H00E 109.5 . . ?
C00A C00C H00F 109.5 . . ?
H00D C00C H00E 109.5 . . ?
H00D C00C H00F 109.5 . . ?
H00E C00C H00F 109.5 . . ?
C004 C00D H00G 109.5 . . ?
C004 C00D H00H 109.5 . . ?
C004 C00D H00I 109.5 . . ?
H00G C00D H00H 109.5 . . ?
H00G C00D H00I 109.5 . . ?
H00H C00D H00I 109.5 . . ?
C008 C00E H00J 109.5 . . ?
C008 C00E H00K 109.5 . . ?
C008 C00E H00L 109.5 . . ?
H00J C00E H00K 109.5 . . ?
H00J C00E H00L 109.5 . . ?
H00K C00E H00L 109.5 . . ?
C005 C00F H00M 109.5 . . ?
C005 C00F H00N 109.5 . . ?
C005 C00F H00O 109.5 . . ?
H00M C00F H00N 109.5 . . ?
H00M C00F H00O 109.5 . . ?
H00N C00F H00O 109.5 . . ?
C3 C2 Os2 68.5(15) . . ?
C6 C2 Os2 72.9(17) . . ?
C6 C2 C3 104(3) . . ?
C6 C2 C11 120(4) . . ?
C11 C2 Os2 125.8(18) . . ?
C11 C2 C3 136(4) . . ?
C2 C3 Os2 70.5(15) . . ?
C4 C3 Os2 75.5(18) . . ?
C4 C3 C2 108(3) . . ?
C4 C3 C10 138(4) . . ?
C10 C3 Os2 123.8(19) . . ?
C10 C3 C2 114(4) . . ?
C3 C4 Os2 68.6(16) . . ?
C3 C4 C5 110(2) . . ?
C3 C4 C9 121(3) . . ?
C5 C4 Os2 72.4(18) . . ?
C5 C4 C9 129(4) . . ?
C9 C4 Os2 127(2) . . ?
C4 C5 Os2 70.8(19) . . ?
C4 C5 C6 106(2) . . ?
C4 C5 C8 122(3) . . ?
C6 C5 Os2 69(2) . . ?
C6 C5 C8 132(4) . . ?
C8 C5 Os2 130(2) . . ?
C2 C6 Os2 71.1(16) . . ?
C2 C6 C5 113(2) . . ?
C2 C6 C7 131(3) . . ?
C5 C6 Os2 73.4(19) . . ?
C5 C6 C7 116(3) . . ?
C7 C6 Os2 125(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C10 H10A 109.5 . . ?
C3 C10 H10B 109.5 . . ?
C3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C2 C11 H11A 109.5 . . ?
C2 C11 H11B 109.5 . . ?
C2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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
Os2 C2 C3 C4 -66.6(17) . . . . ?
Os2 C2 C3 C10 119(2) . . . . ?
Os2 C2 C6 C5 62(2) . . . . ?
Os2 C2 C6 C7 -120(3) . . . . ?
Os2 C3 C4 C5 -61(2) . . . . ?
Os2 C3 C4 C9 122(3) . . . . ?
Os2 C4 C5 C6 -61(2) . . . . ?
Os2 C4 C5 C8 126(3) . . . . ?
Os2 C5 C6 C2 -60.7(19) . . . . ?
Os2 C5 C6 C7 121(3) . . . . ?
Os1 C004 C005 C00A -61.8(5) . . . . ?
Os1 C004 C005 C00F 124.3(8) . . . . ?
Os1 C004 C008 C006 61.8(5) . . . . ?
Os1 C004 C008 C00E -125.5(8) . . . . ?
Os1 C005 C00A C006 -62.9(5) . . . . ?
Os1 C005 C00A C00C 122.1(8) . . . . ?
Os1 C006 C008 C004 -62.7(5) . . . . ?
Os1 C006 C008 C00E 124.5(8) . . . . ?
Os1 C006 C00A C005 63.5(5) . . . . ?
Os1 C006 C00A C00C -121.3(7) . . . . ?
C004 C005 C00A Os1 62.6(5) . . . . ?
C004 C005 C00A C006 -0.3(8) . . . . ?
C004 C005 C00A C00C -175.3(7) . . . . ?
C005 C004 C008 Os1 -61.3(5) . . . . ?
C005 C004 C008 C006 0.5(8) . . . . ?
C005 C004 C008 C00E 173.2(8) . . . . ?
C008 C004 C005 Os1 61.7(5) . . . . ?
C008 C004 C005 C00A -0.1(9) . . . . ?
C008 C004 C005 C00F -174.0(7) . . . . ?
C008 C006 C00A Os1 -63.0(5) . . . . ?
C008 C006 C00A C005 0.6(8) . . . . ?
C008 C006 C00A C00C 175.7(7) . . . . ?
C00A C006 C008 Os1 62.0(5) . . . . ?
C00A C006 C008 C004 -0.6(8) . . . . ?
C00A C006 C008 C00E -173.5(7) . . . . ?
C00B C006 C008 Os1 -123.4(7) . . . . ?
C00B C006 C008 C004 174.0(7) . . . . ?
C00B C006 C008 C00E 1.1(12) . . . . ?
C00B C006 C00A Os1 122.5(8) . . . . ?
C00B C006 C00A C005 -174.0(7) . . . . ?
C00B C006 C00A C00C 1.2(12) . . . . ?
C00D C004 C005 Os1 -121.4(8) . . . . ?
C00D C004 C005 C00A 176.8(7) . . . . ?
C00D C004 C005 C00F 2.9(12) . . . . ?
C00D C004 C008 Os1 121.8(8) . . . . ?
C00D C004 C008 C006 -176.4(8) . . . . ?
C00D C004 C008 C00E -3.7(13) . . . . ?
C00F C005 C00A Os1 -123.7(8) . . . . ?
C00F C005 C00A C006 173.5(7) . . . . ?
C00F C005 C00A C00C -1.6(13) . . . . ?
C2 C3 C4 Os2 63.3(15) . . . . ?
C2 C3 C4 C5 2(3) . . . . ?
C2 C3 C4 C9 -175(3) . . . . ?
C3 C2 C6 Os2 -61.9(14) . . . . ?
C3 C2 C6 C5 0(3) . . . . ?
C3 C2 C6 C7 178(3) . . . . ?
C3 C4 C5 Os2 58.7(18) . . . . ?
C3 C4 C5 C6 -2(2) . . . . ?
C3 C4 C5 C8 -175(3) . . . . ?
C4 C5 C6 Os2 62.0(19) . . . . ?
C4 C5 C6 C2 1(2) . . . . ?
C4 C5 C6 C7 -177(3) . . . . ?
C6 C2 C3 Os2 65.1(16) . . . . ?
C6 C2 C3 C4 -2(3) . . . . ?
C6 C2 C3 C10 -176(3) . . . . ?
C8 C5 C6 Os2 -126(4) . . . . ?
C8 C5 C6 C2 173(4) . . . . ?
C8 C5 C6 C7 -5(5) . . . . ?
C9 C4 C5 Os2 -124(4) . . . . ?
C9 C4 C5 C6 175(4) . . . . ?
C9 C4 C5 C8 2(5) . . . . ?
C10 C3 C4 Os2 -125(3) . . . . ?
C10 C3 C4 C5 174(4) . . . . ?
C10 C3 C4 C9 -3(5) . . . . ?
C11 C2 C3 Os2 -120(3) . . . . ?
C11 C2 C3 C4 174(3) . . . . ?
C11 C2 C3 C10 -1(4) . . . . ?
C11 C2 C6 Os2 122(2) . . . . ?
C11 C2 C6 C5 -176(3) . . . . ?
C11 C2 C6 C7 2(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.139 -0.139 0.861 204.3 23.1 ?
2 0.139 0.361 0.639 204.3 25.7 ?
3 0.139 0.139 0.139 204.3 21.7 ?
4 -0.139 0.639 0.361 204.3 21.7 ?
5 0.067 0.742 0.217 7.4 1.2 ?
6 0.067 0.758 0.717 7.4 0.0 ?
7 0.217 0.067 0.742 7.4 1.0 ?
8 0.217 0.433 0.242 7.4 0.0 ?
9 0.361 0.639 0.139 204.3 30.7 ?
10 0.361 0.861 0.639 204.3 21.7 ?
11 0.242 0.217 0.433 7.4 0.0 ?
12 0.242 0.283 0.933 7.4 0.6 ?
13 0.258 0.717 0.433 7.4 1.2 ?
14 0.258 0.783 0.933 7.4 0.0 ?
15 0.283 0.567 0.742 7.4 0.0 ?
16 0.283 0.933 0.242 7.4 1.1 ?
17 0.639 0.361 0.861 204.3 21.7 ?
18 0.639 0.139 0.361 204.3 25.9 ?
19 0.433 0.242 0.217 7.4 0.0 ?
20 0.433 0.258 0.717 7.4 0.5 ?
21 0.567 0.742 0.283 7.4 0.2 ?
22 0.567 0.758 0.783 7.4 1.4 ?
23 0.717 0.067 0.758 7.4 0.0 ?
24 0.717 0.433 0.258 7.4 1.2 ?
25 0.742 0.217 0.067 7.4 1.7 ?
26 0.742 0.283 0.567 7.4 0.0 ?
27 0.758 0.717 0.067 7.4 0.2 ?
28 0.758 0.783 0.567 7.4 1.1 ?
29 0.783 0.567 0.758 7.4 1.3 ?
30 0.783 0.933 0.258 7.4 0.0 ?
31 0.933 0.242 0.283 7.4 1.4 ?
32 0.933 0.258 0.783 7.4 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
