#------------------------------------------------------------------------------
#$Date: 2025-04-05 06:15:48 +0300 (Sat, 05 Apr 2025) $
#$Revision: 298919 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/78/7717851.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_7717851
loop_
_publ_author_name
'Lachguar, Abdelhak'
'Neumann, Till'
'Pichugov, Andrey V.'
'Jeanneau, Erwann'
'Veyre, Laurent'
'Thieuleux, Chloé'
'Camp, Clément'
_publ_section_title
;
 Catalytic H/D exchange of (hetero)arenes with early-late polyhydride
 heterobimetallic complexes: impact of transition metal pairs.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3804
_journal_page_last               3811
_journal_paper_doi               10.1039/d4dt03171g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C25 H48 Hf Os'
_chemical_formula_sum            'C25 H48 Hf Os'
_chemical_formula_weight         717.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-15
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_audit_update_record
;
2024-11-04 deposited with the CCDC.	2025-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.428(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0703(2)
_cell_length_b                   11.9968(2)
_cell_length_c                   18.9180(4)
_cell_measurement_reflns_used    24681
_cell_measurement_temperature    100.1(2)
_cell_measurement_theta_max      30.5610
_cell_measurement_theta_min      2.3660
_cell_volume                     2797.47(9)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.120a 64-bit (release 16-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  39.00   0.50    2.14    --    7.11  57.00 120.00   90
  2  ω    -85.00 -40.00   0.50    2.14    --   -6.25 -19.00 -60.00   90
  3  ω    -85.00 -40.00   0.50    2.14    --   -6.25 -19.00 -30.00   90
  4  ω     25.00  86.00   0.50    2.14    --    7.11  13.00 -92.00  122
  5  ω     25.00  72.00   0.50    2.14    --   -6.25  13.00 -92.00   94
  6  ω     -6.00  32.00   0.50    2.14    --    7.11  57.00 -30.00   76
  7  ω    -73.00 -40.00   0.50    2.14    --    7.11 -19.00   0.00   66
  8  ω    -73.00 -40.00   0.50    2.14    --    7.11 -19.00-120.00   66
  9  ω     -4.00  42.00   0.50    2.14    --    7.11 -99.00 120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0517303000
_diffrn_orient_matrix_UB_12      0.0101840000
_diffrn_orient_matrix_UB_13      0.0269733000
_diffrn_orient_matrix_UB_21      0.0234733000
_diffrn_orient_matrix_UB_22      0.0004445000
_diffrn_orient_matrix_UB_23      -0.0288411000
_diffrn_orient_matrix_UB_31      -0.0092198000
_diffrn_orient_matrix_UB_32      0.0582412000
_diffrn_orient_matrix_UB_33      -0.0045150000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34091
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.420
_diffrn_reflns_theta_min         2.369
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.328
_exptl_crystal_size_min          0.085
_refine_diff_density_max         2.228
_refine_diff_density_min         -2.610
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.00053(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         7148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0284
_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)+(0.0563P)²+0.2244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6451
_reflns_number_total             7148
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03171g2.cif
_cod_data_source_block           al159_autored
_cod_depositor_comments          'Adding full bibliography for 7717851.cif.'
_cod_database_code               7717851
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H192 Os4 Ta4 '
_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   0.541
_shelx_estimated_absorpt_t_min   0.121
_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.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C11(H11A,H11B), C21(H21A,H21B)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C18(H18A,H18B,
 H18C), C25(H25A,H25B,H25C), C7(H7A,H7B,H7C), C20(H20A,H20B,H20C), C9(H9A,H9B,
 H9C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C10(H10A,H10B,
 H10C), C13(H13A,H13B,H13C), C6(H6A,H6B,H6C)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id AL159
_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 2.477
_oxdiff_exptl_absorpt_empirical_full_min 0.572
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Os1 Os 0.49852(2) 0.60983(2) 0.74675(2) 0.01170(6) Uani 1 1 d . . . . .
Hf1 Hf 0.33839(2) 0.62427(2) 0.61472(2) 0.01188(6) Uani 1 1 d . . . . .
C19 C -0.0098(3) 0.6048(3) 0.6365(3) 0.0257(9) Uani 1 1 d . . . . .
H19A H -0.030691 0.680958 0.618761 0.039 Uiso 1 1 calc R U . . .
H19B H -0.043742 0.584748 0.673738 0.039 Uiso 1 1 calc R U . . .
H19C H -0.034048 0.553067 0.594036 0.039 Uiso 1 1 calc R U . . .
C3 C 0.6344(3) 0.6971(3) 0.83263(19) 0.0156(7) Uani 1 1 d . . . . .
C16 C 0.1692(3) 0.6291(3) 0.6143(2) 0.0176(7) Uani 1 1 d . . . . .
H16A H 0.146861 0.707454 0.601421 0.021 Uiso 1 1 calc R U . . .
H16B H 0.128658 0.585119 0.569500 0.021 Uiso 1 1 calc R U . . .
C17 C 0.1144(3) 0.5980(3) 0.6723(2) 0.0190(7) Uani 1 1 d . . . . .
C15 C 0.4694(3) 0.9229(3) 0.6258(2) 0.0193(7) Uani 1 1 d . . . . .
H15A H 0.470242 0.887542 0.672673 0.029 Uiso 1 1 calc R U . . .
H15B H 0.476699 1.003790 0.632878 0.029 Uiso 1 1 calc R U . . .
H15C H 0.529872 0.894342 0.611357 0.029 Uiso 1 1 calc R U . . .
C23 C 0.4616(3) 0.3284(3) 0.5878(2) 0.0261(8) Uani 1 1 d . . . . .
H23A H 0.471371 0.355395 0.638507 0.039 Uiso 1 1 calc R U . . .
H23B H 0.519500 0.358079 0.571019 0.039 Uiso 1 1 calc R U . . .
H23C H 0.464350 0.246751 0.588022 0.039 Uiso 1 1 calc R U . . .
C22 C 0.3512(3) 0.3674(3) 0.5343(2) 0.0183(7) Uani 1 1 d . . . . .
C11 C 0.3514(3) 0.7707(3) 0.54646(19) 0.0163(7) Uani 1 1 d . . . . .
H11A H 0.414544 0.753555 0.530488 0.020 Uiso 1 1 calc R U . . .
H11B H 0.287110 0.764766 0.500568 0.020 Uiso 1 1 calc R U . . .
C12 C 0.3617(3) 0.8963(3) 0.5637(2) 0.0142(7) Uani 1 1 d . . . . .
C18 C 0.1459(3) 0.4795(3) 0.6997(2) 0.0263(8) Uani 1 1 d . . . . .
H18A H 0.108783 0.458571 0.735053 0.039 Uiso 1 1 calc R U . . .
H18B H 0.224520 0.475373 0.724825 0.039 Uiso 1 1 calc R U . . .
H18C H 0.124493 0.428325 0.656911 0.039 Uiso 1 1 calc R U . . .
C5 C 0.6327(3) 0.5043(3) 0.82009(18) 0.0139(6) Uani 1 1 d . . . . .
C4 C 0.6766(3) 0.6060(3) 0.80056(19) 0.0133(6) Uani 1 1 d . . . . .
C25 C 0.2609(3) 0.3186(3) 0.5603(2) 0.0273(8) Uani 1 1 d . . . . .
H25A H 0.264744 0.236994 0.560056 0.041 Uiso 1 1 calc R U . . .
H25B H 0.190087 0.342891 0.526163 0.041 Uiso 1 1 calc R U . . .
H25C H 0.270272 0.344692 0.611112 0.041 Uiso 1 1 calc R U . . .
C7 C 0.5106(3) 0.7160(3) 0.9163(2) 0.0231(8) Uani 1 1 d . . . . .
H7A H 0.499509 0.793359 0.898810 0.035 Uiso 1 1 calc R U . . .
H7B H 0.556185 0.714547 0.969232 0.035 Uiso 1 1 calc R U . . .
H7C H 0.440256 0.681691 0.910707 0.035 Uiso 1 1 calc R U . . .
C20 C 0.1505(3) 0.6781(3) 0.7386(2) 0.0275(8) Uani 1 1 d . . . . .
H20A H 0.128546 0.754154 0.721159 0.041 Uiso 1 1 calc R U . . .
H20B H 0.229630 0.675001 0.761673 0.041 Uiso 1 1 calc R U . . .
H20C H 0.116605 0.656745 0.775684 0.041 Uiso 1 1 calc R U . . .
C21 C 0.3431(3) 0.4950(3) 0.5314(2) 0.0191(7) Uani 1 1 d . . . . .
H21A H 0.276866 0.509741 0.488087 0.023 Uiso 1 1 calc R U . . .
H21B H 0.404321 0.518321 0.515080 0.023 Uiso 1 1 calc R U . . .
C9 C 0.7620(3) 0.6141(3) 0.7644(3) 0.0239(8) Uani 1 1 d . . . . .
H9A H 0.757593 0.548942 0.732325 0.036 Uiso 1 1 calc R U . . .
H9B H 0.833686 0.616630 0.803249 0.036 Uiso 1 1 calc R U . . .
H9C H 0.750736 0.682051 0.734048 0.036 Uiso 1 1 calc R U . . .
C8 C 0.6666(3) 0.8175(3) 0.8320(2) 0.0229(8) Uani 1 1 d . . . . .
H8A H 0.673177 0.835637 0.783144 0.034 Uiso 1 1 calc R U . . .
H8B H 0.736356 0.830120 0.871482 0.034 Uiso 1 1 calc R U . . .
H8C H 0.611108 0.865127 0.840788 0.034 Uiso 1 1 calc R U . . .
C14 C 0.2672(3) 0.9337(3) 0.5889(2) 0.0241(8) Uani 1 1 d . . . . .
H14A H 0.271099 0.894996 0.635351 0.036 Uiso 1 1 calc R U . . .
H14B H 0.198397 0.915687 0.549796 0.036 Uiso 1 1 calc R U . . .
H14C H 0.271672 1.014330 0.597678 0.036 Uiso 1 1 calc R U . . .
C24 C 0.3366(3) 0.3225(3) 0.4556(2) 0.0244(8) Uani 1 1 d . . . . .
H24A H 0.392922 0.353639 0.437801 0.037 Uiso 1 1 calc R U . . .
H24B H 0.264939 0.344084 0.421268 0.037 Uiso 1 1 calc R U . . .
H24C H 0.342426 0.241023 0.457397 0.037 Uiso 1 1 calc R U . . .
C10 C 0.6626(3) 0.3886(3) 0.8043(2) 0.0224(8) Uani 1 1 d . . . . .
H10A H 0.606911 0.336187 0.807727 0.034 Uiso 1 1 calc R U . . .
H10B H 0.732736 0.368295 0.841161 0.034 Uiso 1 1 calc R U . . .
H10C H 0.667659 0.385728 0.753846 0.034 Uiso 1 1 calc R U . . .
C2 C 0.5656(3) 0.6520(3) 0.8706(2) 0.0164(7) Uani 1 1 d . . . . .
C13 C 0.3566(3) 0.9624(3) 0.4933(2) 0.0220(7) Uani 1 1 d . . . . .
H13A H 0.366261 1.041934 0.505582 0.033 Uiso 1 1 calc R U . . .
H13B H 0.285916 0.950590 0.454558 0.033 Uiso 1 1 calc R U . . .
H13C H 0.414289 0.937004 0.474798 0.033 Uiso 1 1 calc R U . . .
C1 C 0.5655(2) 0.5331(3) 0.86329(18) 0.0148(6) Uani 1 1 d . . . . .
C6 C 0.5111(3) 0.4531(3) 0.9005(2) 0.0222(8) Uani 1 1 d . . . . .
H6A H 0.448310 0.489426 0.907976 0.033 Uiso 1 1 calc R U . . .
H6B H 0.562483 0.430401 0.949083 0.033 Uiso 1 1 calc R U . . .
H6C H 0.486889 0.387252 0.868613 0.033 Uiso 1 1 calc R U . . .
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'
Hf Hf -0.5830 6.1852 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 0 0.0740
0 0 0 0.0106
-2 -1 1 0.1369
18 2 -8 0.1714
2 1 -1 0.2061
-2 1 1 0.1399
2 -2 -1 0.1995
3 -16 -6 0.2382
-3 17 1 0.1927
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
C3 Os1 Hf1 146.66(9) . . ?
C3 Os1 C5 62.79(12) . . ?
C3 Os1 C2 37.07(12) . . ?
C3 Os1 C1 61.82(12) . . ?
C5 Os1 Hf1 145.58(9) . . ?
C5 Os1 C2 62.02(12) . . ?
C5 Os1 C1 36.87(11) . . ?
C4 Os1 Hf1 143.91(9) . . ?
C4 Os1 C3 38.00(12) . . ?
C4 Os1 C5 38.04(11) . . ?
C4 Os1 C2 62.77(12) . . ?
C4 Os1 C1 62.53(12) . . ?
C2 Os1 Hf1 149.60(8) . . ?
C2 Os1 C1 36.73(11) . . ?
C1 Os1 Hf1 149.13(8) . . ?
C16 Hf1 Os1 118.39(10) . . ?
C16 Hf1 C11 104.33(12) . . ?
C16 Hf1 C21 106.21(13) . . ?
C11 Hf1 Os1 113.97(9) . . ?
C11 Hf1 C21 96.56(13) . . ?
C21 Hf1 Os1 114.72(9) . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
C4 C3 Os1 70.23(18) . . ?
C4 C3 C8 125.1(3) . . ?
C8 C3 Os1 127.0(2) . . ?
C2 C3 Os1 72.95(19) . . ?
C2 C3 C4 108.4(3) . . ?
C2 C3 C8 126.2(3) . . ?
Hf1 C16 H16A 103.8 . . ?
Hf1 C16 H16B 103.8 . . ?
H16A C16 H16B 105.4 . . ?
C17 C16 Hf1 133.8(3) . . ?
C17 C16 H16A 103.8 . . ?
C17 C16 H16B 103.8 . . ?
C19 C17 C16 110.2(3) . . ?
C18 C17 C19 109.0(3) . . ?
C18 C17 C16 109.4(3) . . ?
C18 C17 C20 109.5(3) . . ?
C20 C17 C19 108.7(3) . . ?
C20 C17 C16 110.0(3) . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
C23 C22 C25 109.0(3) . . ?
C21 C22 C23 111.5(3) . . ?
C21 C22 C25 109.8(3) . . ?
C21 C22 C24 109.4(3) . . ?
C24 C22 C23 108.7(3) . . ?
C24 C22 C25 108.4(3) . . ?
Hf1 C11 H11A 104.2 . . ?
Hf1 C11 H11B 104.2 . . ?
H11A C11 H11B 105.5 . . ?
C12 C11 Hf1 132.0(2) . . ?
C12 C11 H11A 104.2 . . ?
C12 C11 H11B 104.2 . . ?
C15 C12 C11 111.0(3) . . ?
C14 C12 C15 109.3(3) . . ?
C14 C12 C11 109.3(3) . . ?
C14 C12 C13 108.2(3) . . ?
C13 C12 C15 108.7(3) . . ?
C13 C12 C11 110.3(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C4 C5 Os1 70.07(18) . . ?
C4 C5 C10 125.4(3) . . ?
C10 C5 Os1 127.2(3) . . ?
C1 C5 Os1 73.28(18) . . ?
C1 C5 C4 108.2(3) . . ?
C1 C5 C10 126.1(3) . . ?
C3 C4 Os1 71.77(18) . . ?
C3 C4 C5 106.9(3) . . ?
C3 C4 C9 126.2(3) . . ?
C5 C4 Os1 71.89(18) . . ?
C5 C4 C9 126.2(3) . . ?
C9 C4 Os1 128.4(3) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Hf1 C21 H21A 103.8 . . ?
Hf1 C21 H21B 103.8 . . ?
C22 C21 Hf1 133.5(3) . . ?
C22 C21 H21A 103.8 . . ?
C22 C21 H21B 103.8 . . ?
H21A C21 H21B 105.4 . . ?
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 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 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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 . . ?
C3 C2 Os1 69.98(19) . . ?
C3 C2 C7 126.5(3) . . ?
C3 C2 C1 108.0(3) . . ?
C7 C2 Os1 127.8(2) . . ?
C1 C2 Os1 72.01(19) . . ?
C1 C2 C7 125.2(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 C1 Os1 69.84(18) . . ?
C5 C1 C2 108.4(3) . . ?
C5 C1 C6 126.2(3) . . ?
C2 C1 Os1 71.26(19) . . ?
C2 C1 C6 125.2(3) . . ?
C6 C1 Os1 128.5(2) . . ?
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 . . ?
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
Os1 Hf1 2.6780(2) . ?
Os1 C3 2.229(3) . ?
Os1 C5 2.233(3) . ?
Os1 C4 2.209(3) . ?
Os1 C2 2.268(4) . ?
Os1 C1 2.278(3) . ?
Hf1 C16 2.210(3) . ?
Hf1 C11 2.220(3) . ?
Hf1 C21 2.227(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 C17 1.540(5) . ?
C3 C4 1.445(5) . ?
C3 C8 1.506(5) . ?
C3 C2 1.430(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.541(5) . ?
C17 C18 1.521(5) . ?
C17 C20 1.526(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 C12 1.537(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 C22 1.534(5) . ?
C22 C25 1.538(5) . ?
C22 C21 1.533(5) . ?
C22 C24 1.534(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.538(4) . ?
C12 C14 1.531(5) . ?
C12 C13 1.533(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C5 C4 1.448(4) . ?
C5 C10 1.498(4) . ?
C5 C1 1.427(4) . ?
C4 C9 1.493(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 C2 1.507(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C2 C1 1.432(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C1 C6 1.502(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
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
Os1 C3 C4 C5 -63.7(2) . . . . ?
Os1 C3 C4 C9 124.7(4) . . . . ?
Os1 C3 C2 C7 -122.8(3) . . . . ?
Os1 C3 C2 C1 62.4(2) . . . . ?
Os1 C5 C4 C3 63.7(2) . . . . ?
Os1 C5 C4 C9 -124.8(4) . . . . ?
Os1 C5 C1 C2 -61.1(2) . . . . ?
Os1 C5 C1 C6 123.5(3) . . . . ?
Os1 C2 C1 C5 60.3(2) . . . . ?
Os1 C2 C1 C6 -124.4(3) . . . . ?
Hf1 C16 C17 C19 -172.5(2) . . . . ?
Hf1 C16 C17 C18 -52.7(4) . . . . ?
Hf1 C16 C17 C20 67.6(4) . . . . ?
Hf1 C11 C12 C15 65.1(4) . . . . ?
Hf1 C11 C12 C14 -55.6(4) . . . . ?
Hf1 C11 C12 C13 -174.4(2) . . . . ?
C3 C2 C1 Os1 -61.1(2) . . . . ?
C3 C2 C1 C5 -0.8(4) . . . . ?
C3 C2 C1 C6 174.6(3) . . . . ?
C23 C22 C21 Hf1 -66.8(4) . . . . ?
C4 C3 C2 Os1 -61.6(2) . . . . ?
C4 C3 C2 C7 175.6(3) . . . . ?
C4 C3 C2 C1 0.7(4) . . . . ?
C4 C5 C1 Os1 61.7(2) . . . . ?
C4 C5 C1 C2 0.6(4) . . . . ?
C4 C5 C1 C6 -174.7(3) . . . . ?
C25 C22 C21 Hf1 54.2(5) . . . . ?
C7 C2 C1 Os1 124.0(3) . . . . ?
C7 C2 C1 C5 -175.8(3) . . . . ?
C7 C2 C1 C6 -0.4(5) . . . . ?
C8 C3 C4 Os1 -121.9(3) . . . . ?
C8 C3 C4 C5 174.4(3) . . . . ?
C8 C3 C4 C9 2.8(6) . . . . ?
C8 C3 C2 Os1 123.7(3) . . . . ?
C8 C3 C2 C7 0.9(6) . . . . ?
C8 C3 C2 C1 -173.9(3) . . . . ?
C24 C22 C21 Hf1 173.0(3) . . . . ?
C10 C5 C4 Os1 122.1(4) . . . . ?
C10 C5 C4 C3 -174.3(3) . . . . ?
C10 C5 C4 C9 -2.7(6) . . . . ?
C10 C5 C1 Os1 -124.2(4) . . . . ?
C10 C5 C1 C2 174.6(3) . . . . ?
C10 C5 C1 C6 -0.7(6) . . . . ?
C2 C3 C4 Os1 63.4(2) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C2 C3 C4 C9 -171.9(3) . . . . ?
C1 C5 C4 Os1 -63.8(2) . . . . ?
C1 C5 C4 C3 -0.1(4) . . . . ?
C1 C5 C4 C9 171.4(3) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 -0.0000 -0.4998 -0.0135 0.0144 0.0023
0.0000 0.0000 0.4998 0.0135 -0.0144 -0.0023
-1.9989 -0.9997 0.9980 -0.0867 -0.0761 -0.0443
18.2325 2.3066 -7.6808 0.7595 0.6505 0.0009
1.9989 0.9997 -0.9980 0.0867 0.0761 0.0443
-1.9994 0.9989 0.5005 -0.0798 -0.0609 0.0744
1.9996 -1.9983 -0.5016 0.0696 0.0605 -0.1326
3.0015 -15.9895 -6.0148 -0.1698 0.2368 -0.9318
-3.0021 16.9884 0.5184 0.0317 -0.0779 1.0148
