A versatile strategy for the formation of hydride-bridged actinide-iridium multimetallics.
Ye, Christopher Z.; Del Rosal, Iker; Boreen, Michael A.; Ouellette, Erik T.; Russo, Dominic R.; Maron, Laurent; Arnold, John; Camp, Clément; Chemical science 14 (2023) 861–868; doi:10.1039/d2sc04903a

data_1568134
_publ_section_title
;
 A versatile strategy for the formation of hydride-bridged
 actinide-iridium multimetallics.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              861
_journal_page_last               868
_journal_paper_doi               10.1039/d2sc04903a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C40 H60 Ir4 Th'
_chemical_formula_sum            'C40 H60 Ir4 Th'
_chemical_formula_weight         1541.72
_chemical_melting_point          444
_chemical_name_systematic        Th{[(\m-H2)(H)IrCp*]2[(\m-H)3IrCp*]2}
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-03-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-29 deposited with the CCDC.	2022-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.339(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6424(17)
_cell_length_b                   19.070(2)
_cell_length_c                   17.520(2)
_cell_measurement_reflns_used    9167
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.097
_cell_measurement_theta_min      1.639
_cell_volume                     4452.7(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9167
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.097
_diffrn_reflns_theta_min         1.639
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    16.233
_exptl_absorpt_correction_T_max  0.746223
_exptl_absorpt_correction_T_min  0.400583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 84284 reflections, Rint = 0.0999
 (29858 with I > 3sig(I), Rint = 0.0726)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.300
_exptl_crystal_description       plate
_exptl_crystal_F_000             2792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.005
_refine_diff_density_max         3.443
_refine_diff_density_min         -3.007
_refine_diff_density_rms         0.458
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         9167
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0556P)^2^+282.9104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6572
_reflns_number_total             9167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04903a2.cif
_cod_data_source_block           czy_ii_027_b_0m
_cod_depositor_comments
'Adding full bibliography for 1568133--1568135.cif.'
_cod_original_cell_volume        4452.8(10)
_cod_database_code               1568134
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.246
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.783(3)
 0.217(3)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C14, C13, C12, C11, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34, C35, C31, C32, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C24, C25, C21, C22, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C20, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C36(H36A,H36B,H36C), C18(H18A,H18B,H18C),
 C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C),
  C16(H16A,H16B,H16C), C40(H40A,H40B,H40C), C8(H8A,H8B,H8C), C28(H28A,H28B,
 H28C), C20(H20A,H20B,H20C), C37(H37A,H37B,H37C), C17(H17A,H17B,H17C), C29(H29A,
 H29B,H29C), C39(H39A,H39B,H39C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C),
 C38(H38A,H38B,H38C)
;
_shelx_res_checksum              21285
_shelx_hkl_checksum              7089
_olex2_submission_special_instructions 'No special instructions were received'