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_7133931
_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         'C90 H152 Ir2 S4 U2, C6 H14'
_chemical_formula_sum            'C96 H166 Ir2 S4 U2'
_chemical_formula_weight         2308.98
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-04-05
_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                90
_cell_angle_beta                 99.352(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.472(3)
_cell_length_b                   18.083(2)
_cell_length_c                   17.948(2)
_cell_measurement_reflns_used    61141
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.097
_cell_measurement_theta_min      2.310
_cell_volume                     9438.1(18)
_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 0.999
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61141
_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         27.097
_diffrn_reflns_theta_min         2.310
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    4.687
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1605 before and 0.0711 after correction.
The Ratio of minimum to maximum transmission is 0.8372.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.264
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9655
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+75.6581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8562
_reflns_number_total             9655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02482f2.cif
_cod_data_source_block           czy_ii_128_0m
_cod_original_cell_volume        9437.7(18)
_cod_database_code               7133931
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.651
_shelx_estimated_absorpt_t_min   0.454
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C48-C47 = C47-C46
 1.54 with sigma of 0.01
 Ir1-HB
 1.53 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C27, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13, C14, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H16A)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(H16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C16(H16), C16(H16A), C24(H24), C27(H27), C30(H30),
  C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C48(H48A,H48B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C20(H20)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C17B(H17D,H17E,
 H17F), C18(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              66645
_shelx_hkl_checksum              81677
_olex2_submission_special_instructions 'No special instructions were received'