#------------------------------------------------------------------------------
#$Date: 2024-06-01 01:12:21 +0300 (Sat, 01 Jun 2024) $
#$Revision: 292131 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571732.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1571732
loop_
_publ_author_name
'Ye, Christopher Z.'
'Del Rosal, Iker'
'Kelly, Sheridon N.'
'Brackbill, I. Joseph'
'Maron, Laurent'
'Camp, Cl\'ement'
'Arnold, John'
_publ_section_title
;
 Photolysis-driven bond activation by thorium and uranium tetraosmate
 polyhydride complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D4SC02380C
_journal_year                    2024
_chemical_formula_moiety         'C46 H64 Os4 Th'
_chemical_formula_sum            'C46 H64 Os4 Th'
_chemical_formula_weight         1609.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           138
_space_group_name_Hall           '-P 4ac 2ac'
_space_group_name_H-M_alt        'P 42/n c m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-08 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7391(15)
_cell_length_b                   13.7391(15)
_cell_length_c                   25.158(3)
_cell_measurement_reflns_used    53451
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.042
_cell_measurement_theta_min      2.304
_cell_volume                     4748.9(9)
_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)'
_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       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_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_source                   'Advanced Light Source, station 12.2.1'
_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 \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.204
_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_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0445
_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/[\s^2^(Fo^2^)+73.6242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2047
_reflns_number_total             2317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02380c2.cif
_cod_data_source_block           czy_ii_175_0m
_cod_original_cell_volume        4748.8(12)
_cod_original_sg_symbol_H-M      'P 42/n c m'
_cod_database_code               1571732
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.096
_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)
;
_shelx_res_file
;
    czy_ii_175_0m.res created by SHELXL-2014/7

TITL czy_ii_175_0m_a.res in P4(2)/ncm
REM Old TITL CZY_II_175_0m in P42/ncm #138
REM SHELXT solution in P4(2)/ncm
REM R1 0.347, Rweak 0.042, Alpha 0.064, Orientation as input
REM Formula found by SHELXT: C45 Os2 Th2
CELL 0.7288 13.7391 13.7391 25.1577 90 90 90
ZERR 4 0.0015 0 0.0027 0 0 0
LATT 1
SYMM 0.5-X,0.5-Y,+Z
SYMM 0.5-Y,+X,0.5+Z
SYMM +Y,0.5-X,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,-Y,0.5-Z
SYMM 0.5+Y,0.5+X,-Z
SYMM -Y,-X,-Z
SFAC C H Os Th
DISP C 0.0034 0.0017 11.92
DISP H 0 0 0.67
DISP Os -1.2848 7.9466 33486.29
DISP Th -7.9004 9.3112 39457.97
UNIT 184 256 16 4
EQIV $1 1.5-Y,1.5-X,+Z
DFIX 0.96 C12 H12c
DFIX 1.37 C13 C14 C16 C17 C17 C18
DANG 2.37 C13 C15 C15 C17 C16 C18
DFIX 1.38 C13 C18
DANG 2.38 C13 C17
DFIX 1.36 C14 C15 C15 C16
DANG 2.36 C14 C16
FLAT C13 C14 C15 C16 C17 C18
RIGU C13 C14 C15 C16 C17 C18

L.S. 10 0 0
PLAN  30
SIZE 0.3 0.02 0.02
TEMP -173.15
CONF
FREE Th1 H12c
FREE Th1 H12c_$1
list 4
MORE -1
BOND $H
fmap 2 53
acta
SHEL 100 0.83
OMIT 0 0 2
OMIT 0 1 2
OMIT 1 1 0
REM <olex2.extras>
REM <HklSrc "%.\\CZY_II_175_0m.hkl">
REM </olex2.extras>

WGHT    0.000000   73.624191
FVAR       0.13061
OS2   3    0.686858    0.813142    0.493239    10.50000    0.03704    0.03704 =
         0.02877   -0.00050    0.00050    0.01055
OS1   3    0.604501    0.604501    0.337638    10.50000    0.05137    0.05137 =
         0.02773    0.00006    0.00006   -0.01734
TH1   4    0.726697    0.773303    0.380487    10.25000    0.03501    0.03501 =
         0.02549   -0.00086    0.00086   -0.00293
C7    1    0.630759    0.943273    0.532724    11.00000    0.04567    0.03835 =
         0.04431   -0.01009    0.00310    0.01384
C10   1    0.672461    0.989454    0.580916    11.00000    0.04888    0.08769 =
         0.05335   -0.01961   -0.00464    0.01707
AFIX 137
H10A  2    0.628139    1.040160    0.593751    11.00000   -1.50000
H10B  2    0.735579    1.018585    0.572189    11.00000   -1.50000
H10C  2    0.681213    0.940125    0.608644    11.00000   -1.50000
AFIX   0
C5    1    0.625324    0.360469    0.346507    11.00000    0.10252    0.04169 =
         0.08905   -0.01023    0.02086   -0.01516
AFIX 137
H5A   2    0.691687    0.368027    0.332835    11.00000   -1.50000
H5B   2    0.596460    0.300970    0.331908    11.00000   -1.50000
H5C   2    0.627113    0.356128    0.385376    11.00000   -1.50000
AFIX   0
C1    1    0.493773    0.493773    0.361970    10.50000    0.05667    0.05667 =
         0.04517   -0.00546   -0.00546   -0.03927
C2    1    0.565531    0.446127    0.330375    11.00000    0.07171    0.03500 =
         0.04872   -0.01429   -0.00316   -0.01592
C3    1    0.563164    0.487237    0.278607    11.00000    0.08319    0.08308 =
         0.03581   -0.01337    0.00009   -0.03433
C4    1    0.465185    0.465185    0.417801    10.50000    0.06039    0.06039 =
         0.06217    0.01205    0.01205   -0.01972
PART -1
AFIX 137
H4A   2    0.523378    0.445848    0.437698    10.50000   -1.50000
H4B   2    0.419446    0.410508    0.416429    10.50000   -1.50000
H4C   2    0.434181    0.520649    0.435499    10.50000   -1.50000
AFIX   0
PART 0
C8    1    0.652820    0.965365    0.478130    11.00000    0.03935    0.02921 =
         0.04829   -0.00463    0.00578    0.00977
C6    1    0.617869    0.455845    0.231576    11.00000    0.12741    0.10144 =
         0.05624   -0.03916    0.01099   -0.03509
AFIX 137
H6A   2    0.577819    0.411236    0.210468    11.00000   -1.50000
H6B   2    0.677496    0.422526    0.242799    11.00000   -1.50000
H6C   2    0.634846    0.512798    0.210033    11.00000   -1.50000
AFIX   0
C11   1    0.722525    1.044577    0.460400    11.00000    0.05352    0.05072 =
         0.06985    0.00074    0.01293    0.00269
AFIX 137
H11A  2    0.779011    1.045850    0.484177    11.00000   -1.50000
H11B  2    0.689422    1.107723    0.461573    11.00000   -1.50000
H11C  2    0.744179    1.031338    0.423996    11.00000   -1.50000
AFIX   0
C12   1    0.587848    0.912152    0.386523    10.50000    0.05645    0.05645 =
         0.04119   -0.00260    0.00260    0.01700
AFIX  23
H12A  2    0.608403    0.975429    0.371410    10.50000   -1.20000
H12B  2    0.524571    0.891597    0.371410    10.50000   -1.20000
AFIX   0
C9    1    0.590233    0.909767    0.445304    10.50000    0.04092    0.04092 =
         0.02979    0.00005   -0.00005    0.01369
H12C  2    0.603693    0.896307    0.350369    10.25000    0.04362
PART -1
C13   1    0.647876    0.756892    0.250603    10.25000    0.03836    0.06549 =
         0.04916   -0.00132    0.02327   -0.00664
AFIX  43
H13   2    0.591261    0.788297    0.263863    10.25000   -1.20000
AFIX   0
C14   1    0.691064    0.791267    0.205122    10.25000    0.08361    0.12204 =
         0.09200    0.04876    0.07030    0.04698
AFIX  43
H14   2    0.664060    0.845601    0.187011    10.25000   -1.20000
AFIX   0
C15   1    0.772870    0.747196    0.185996    10.25000    0.03870    0.07444 =
         0.04218   -0.00249    0.02207   -0.00104
AFIX  43
H15   2    0.803396    0.771089    0.154727    10.25000   -1.20000
AFIX   0
C16   1    0.810369    0.669194    0.211810    10.25000    0.01902    0.05412 =
         0.02711   -0.02064    0.00538   -0.01970
AFIX  43
H16   2    0.866425    0.637755    0.197881    10.25000   -1.20000
AFIX   0
C17   1    0.768885    0.634849    0.257643    10.25000    0.03650    0.07043 =
         0.03998   -0.00596    0.01730   -0.00491
AFIX  43
H17   2    0.797821    0.581585    0.275811    10.25000   -1.20000
AFIX   0
C18   1    0.685376    0.677039    0.277624    10.25000    0.02783    0.05107 =
         0.04240   -0.01156    0.01466   -0.01716
HKLF 4

REM  czy_ii_175_0m_a.res in P4(2)/ncm
REM R1 =  0.0445 for    2047 Fo > 4sig(Fo)  and  0.0510 for all    2317 data
REM    177 parameters refined using     51 restraints

END

WGHT      0.0000     73.5743

REM Highest difference peak  1.077,  deepest hole -1.371,  1-sigma level  0.204
Q1    1   0.7500  0.7500  0.5438  10.25000  0.05    1.08
Q2    1   0.8469  0.8891  0.4623  11.00000  0.05    0.85
Q3    1   0.6688  0.6688  0.4814  10.50000  0.05    0.76
Q4    1   0.7981  0.7981  0.4972  10.50000  0.05    0.74
Q5    1   0.6075  0.8925  0.3385  10.50000  0.05    0.72
Q6    1   0.6874  0.8126  0.4448  10.50000  0.05    0.68
Q7    1   0.8279  0.8280  0.2002  10.50000  0.05    0.67
Q8    1   0.7264  0.5651  0.3464  11.00000  0.05    0.65
Q9    1   0.6755  0.4989  0.1802  11.00000  0.05    0.65
Q10   1   0.6586  0.7181  0.4562  11.00000  0.05    0.65
Q11   1   0.6595  0.6595  0.3820  10.50000  0.05    0.64
Q12   1   0.7474  0.8572  0.4545  11.00000  0.05    0.63
Q13   1   0.7196  0.4009  0.3232  11.00000  0.05    0.62
Q14   1   0.6759  0.6759  0.2986  10.50000  0.05    0.59
Q15   1   0.6208  0.6010  0.2207  11.00000  0.05    0.59
Q16   1   0.5525  0.7801  0.3774  11.00000  0.05    0.58
Q17   1   0.7500  0.7500  0.4573  10.25000  0.05    0.58
Q18   1   0.6120  0.6120  0.4190  10.50000  0.05    0.58
Q19   1   0.5307  0.5307  0.1711  10.50000  0.05    0.57
Q20   1   0.5757  0.9243  0.6402  10.50000  0.05    0.55
Q21   1   0.8011  1.0122  0.4968  11.00000  0.05    0.55
Q22   1   0.5980  1.0440  0.5003  11.00000  0.05    0.55
Q23   1   0.7381  0.8762  0.4270  11.00000  0.05    0.55
Q24   1   0.6932  0.8068  0.5445  10.50000  0.05    0.55
Q25   1   0.7658  0.9772  0.4849  11.00000  0.05    0.54
Q26   1   0.6406  0.5666  0.1797  11.00000  0.05    0.52
Q27   1   0.4006  0.4006  0.4572  10.50000  0.05    0.52
Q28   1   0.7062  1.0979  0.4549  11.00000  0.05    0.52
Q29   1   0.6062  0.7080  0.3222  11.00000  0.05    0.50
Q30   1   0.6584  0.8416  0.3991  10.50000  0.05    0.50
;
_shelx_res_checksum              74509
_olex2_submission_special_instructions 'No special instructions were received'
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'
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
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os2 0.0370(2) 0.0370(2) 0.0288(3) -0.00050(16) 0.00050(16) 0.0105(3)
Os1 0.0514(3) 0.0514(3) 0.0277(3) 0.00006(18) 0.00006(18) -0.0173(3)
Th1 0.0350(4) 0.0350(4) 0.0255(5) -0.0009(3) 0.0009(3) -0.0029(5)
C7 0.046(7) 0.038(6) 0.044(6) -0.010(5) 0.003(5) 0.014(5)
C10 0.049(8) 0.088(11) 0.053(8) -0.020(7) -0.005(6) 0.017(7)
C5 0.103(13) 0.042(8) 0.089(11) -0.010(8) 0.021(10) -0.015(8)
C1 0.057(7) 0.057(7) 0.045(9) -0.005(5) -0.005(5) -0.039(9)
C2 0.072(9) 0.035(6) 0.049(7) -0.014(5) -0.003(6) -0.016(6)
C3 0.083(10) 0.083(10) 0.036(6) -0.013(6) 0.000(6) -0.034(8)
C4 0.060(8) 0.060(8) 0.062(11) 0.012(6) 0.012(6) -0.020(10)
C8 0.039(6) 0.029(6) 0.048(6) -0.005(5) 0.006(5) 0.010(5)
C6 0.127(17) 0.101(14) 0.056(9) -0.039(9) 0.011(10) -0.035(12)
C11 0.054(8) 0.051(8) 0.070(8) 0.001(7) 0.013(7) 0.003(6)
C12 0.056(7) 0.056(7) 0.041(9) -0.003(5) 0.003(5) 0.017(9)
C9 0.041(5) 0.041(5) 0.030(7) 0.000(4) 0.000(4) 0.014(7)
C13 0.04(2) 0.07(3) 0.05(3) 0.00(2) 0.02(2) -0.01(2)
C14 0.08(4) 0.12(5) 0.09(3) 0.05(3) 0.07(4) 0.05(4)
C15 0.04(3) 0.07(3) 0.042(12) -0.002(15) 0.022(14) -0.001(19)
C16 0.019(18) 0.05(3) 0.027(13) -0.021(12) 0.005(11) -0.02(2)
C17 0.04(2) 0.07(3) 0.040(19) -0.01(2) 0.017(17) 0.00(2)
C18 0.03(2) 0.05(3) 0.042(13) -0.012(15) 0.015(15) -0.017(13)
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)'
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_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_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) . . . . ?