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_1571734
_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         '0.333(C30 H45 Os3), C30 H45 Os3 U'
_chemical_formula_sum            'C40 H60 Os4 U'
_chemical_formula_weight         1539.71
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-05-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_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            8
_cell_length_a                   21.395(2)
_cell_length_b                   21.395(2)
_cell_length_c                   21.395(2)
_cell_measurement_reflns_used    125415
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.804
_cell_measurement_theta_min      1.952
_cell_volume                     9793.5(16)
_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 0.999
_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  0.1087
_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_source                   'Advanced Light Source, station 12.2.1'
_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 \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.089
_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
_refine_diff_density_max         1.352
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.301
_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_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0342
_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/[\s^2^(Fo^2^)+(0.0530P)^2^+52.5146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3289
_reflns_number_total             3605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02380c2.cif
_cod_data_source_block           czy_ii_125_0m
_cod_depositor_comments
'Adding full bibliography for 1571730--1571734.cif.'
_cod_original_cell_volume        9793(3)
_cod_database_code               1571734
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.368
_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)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12621
_shelx_fab_checksum              69635
_olex2_submission_special_instructions 'No special instructions were received'