Reduction of CS2 to an ethanetetrathiolate by a hydride-bridged uranium–iridium heterobimetallic complex
Ye, Christopher Z.; Del Rosal, Iker; Ouellette, Erik T.; Hohloch, Stephan; Maron, Laurent; Camp, Clément; Arnold, John; Chemical Communications 60 (2024) 12377–12380; doi:10.1039/D4CC02482F

data_7133930
_publ_section_title
;
 Reduction of CS2 to an ethanetetrathiolate by a hydride-bridged
 uranium--iridium heterobimetallic complex
;
_journal_issue                   85
_journal_name_full               'Chemical Communications'
_journal_page_first              12377
_journal_page_last               12380
_journal_paper_doi               10.1039/D4CC02482F
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C44 H76 Ir U, 0.5(C6 H18 O Si2)'
_chemical_formula_sum            'C47 H85 Ir O0.5 Si U'
_chemical_formula_weight         1116.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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
;
2024-04-20 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                105.679(4)
_cell_angle_beta                 96.253(4)
_cell_angle_gamma                96.290(4)
_cell_formula_units_Z            2
_cell_length_a                   12.0803(12)
_cell_length_b                   12.3459(12)
_cell_length_c                   16.9963(17)
_cell_measurement_reflns_used    42447
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.522
_cell_measurement_theta_min      2.310
_cell_volume                     2400.3(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0666
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42447
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         30.522
_diffrn_reflns_theta_min         2.310
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.541
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1034 before and 0.0849 after correction.
The Ratio of minimum to maximum transmission is 0.8351.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       rod
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.948
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         13551
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11274
_reflns_number_total             13551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02482f2.cif
_cod_data_source_block           czy_ii_019_0m
_cod_original_formula_sum        'C47 H85 Ir O0.50 Si U'
_cod_database_code               7133930
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.612
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-C46 = Si1-C45 = Si1-C48 = Si2-C49 = Si2-C50 = Si2-C47
 1.86 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C45, Si1, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: Si1(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) O47(0.5) C46(0.5)
 H46A(0.5) H46B(0.5) H46C(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) Si2(0.5)
 C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
 C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5)
5.a Ternary CH refined with riding coordinates:
 C6(H6), C32(H32), C26(H26), C23(H23), C29(H29), C15(H15), C9(H9), C12(H12)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C1(H1)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C44(H44A,H44B,H44C), C31(H31A,H31B,H31C),
 C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C28(H28A,
 H28B,H28C), C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C34(H34A,H34B,H34C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C25(H25A,H25B,
 H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C),
 C49(H49A,H49B,H49C)
;
_shelx_res_checksum              51270
_shelx_hkl_checksum              94155
_olex2_submission_special_instructions 'No special instructions were received'