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_1571732
_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         '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_depositor_comments
'Adding full bibliography for 1571730--1571734.cif.'
_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_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_checksum              74509
_olex2_submission_special_instructions 'No special instructions were received'