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_1571733
_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 U'
_chemical_formula_sum            'C40 H59 Os4 U'
_chemical_formula_weight         1538.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-10
_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                 113.731(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.875(4)
_cell_length_b                   10.0269(10)
_cell_length_c                   23.315(2)
_cell_measurement_reflns_used    52702
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.042
_cell_measurement_theta_min      1.821
_cell_volume                     8747.7(15)
_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)'
_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       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_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_source                   'Advanced Light Source, station 12.2.1'
_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 \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.337
_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
_refine_diff_density_max         1.899
_refine_diff_density_min         -2.543
_refine_diff_density_rms         0.172
_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_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0178P)^2^+154.2928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6813
_reflns_number_total             7991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02380c2.cif
_cod_data_source_block           czy_72236_0m
_cod_depositor_comments
'Adding full bibliography for 1571730--1571734.cif.'
_cod_database_code               1571733
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.679
_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)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54449
_shelx_fab_checksum              44088
_olex2_submission_special_instructions 'No special instructions were received'