Photolysis-driven bond activation by thorium and uranium tetraosmate polyhydride complexes.
Ye, Christopher Z.; Del Rosal, Iker; Kelly, Sheridon N.; Brackbill, I. Joseph; Maron, Laurent; Camp, Clément; Arnold, John; Chemical science 15 (2024) 9784–9792; doi:10.1039/d4sc02380c

data_1571731
_publ_section_title
;
 Photolysis-driven bond activation by thorium and uranium tetraosmate
 polyhydride complexes.
;
_journal_issue                   25
_journal_name_full               'Chemical science'
_journal_page_first              9784
_journal_page_last               9792
_journal_paper_doi               10.1039/d4sc02380c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C40 H59 Os4 Th, C6 H14'
_chemical_formula_sum            'C46 H73 Os4 Th'
_chemical_formula_weight         1618.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_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            2
_cell_length_a                   18.6052(5)
_cell_length_b                   9.9998(3)
_cell_length_c                   13.3830(4)
_cell_measurement_reflns_used    15674
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.6960
_cell_measurement_theta_min      3.3370
_cell_volume                     2489.88(12)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     40.00  87.00   0.50    2.34    --    8.14-179.00-180.00   94
  2  \w     40.00  71.00   0.50    2.34    --    8.14-179.00 -30.00   62
  3  \w    -60.00 -23.00   0.50    2.34    --    8.14   0.00-150.00   74
  4  \w    -18.00  16.00   0.50    2.34    --    8.14   0.00-150.00   68
  5  \w      0.00  37.00   0.50    2.34    --    8.14  77.00  90.00   74
  6  \w    -14.00  14.00   0.50    2.34    --   -7.82  29.00  14.00   56
  7  \w    -40.00  12.00   0.50    2.34    --   -7.82 -77.00-120.00  104
  8  \w    -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       '\w 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_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_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_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_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.159
_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
_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_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_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0216
_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^)+(0.0249P)^2^+0.4399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0470
_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_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02380c2.cif
_cod_data_source_block           czy_ii_3-th
_cod_depositor_comments
'Adding full bibliography for 1571730--1571734.cif.'
_cod_database_code               1571731
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Th Os C H'
_shelx_estimated_absorpt_t_max   0.559
_shelx_estimated_absorpt_t_min   0.178
_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)
;
_shelx_res_checksum              6922
_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