CO<sub>2</sub> cleavage by tantalum/M (M = iridium, osmium) heterobimetallic complexes.
Lachguar, Abdelhak; Ye, Christopher Z.; Kelly, Sheridon N.; Jeanneau, Erwann; Del Rosal, Iker; Maron, Laurent; Veyre, Laurent; Thieuleux, Chloé; Arnold, John; Camp, Clément; Chemical communications (Cambridge, England) 60 (2024) 7878–7881; doi:10.1039/d4cc02207f

data_7133285
_publ_section_title
;
 CO<sub>2</sub> cleavage by tantalum/M (M = iridium, osmium)
 heterobimetallic complexes.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7878
_journal_page_last               7881
_journal_paper_doi               10.1039/d4cc02207f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C25 H51 Os Ta'
_chemical_formula_sum            'C25 H51 Os Ta'
_chemical_formula_weight         722.80
_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
_audit_creation_date             2024-06-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.405(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7258(4)
_cell_length_b                   16.5130(2)
_cell_length_c                   19.8168(4)
_cell_measurement_reflns_used    32863
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.0350
_cell_measurement_theta_min      2.6670
_cell_volume                     5618.14(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      8.00  98.00   0.50   14.35    --   24.81  63.00-111.00  180
  2  \w    -47.00  42.00   0.50   14.35    --   24.81 -63.00 111.00  178
  3  \w    -97.00  -8.00   0.50   14.35    --  -25.20 -63.00 111.00  178
  4  \w     10.00  38.00   0.50   14.35    --   24.81  57.00  30.00   56
  5  \w    -50.00 -13.00   0.50   14.35    --   24.81 -19.00   0.00   74
  6  \w     10.00  38.00   0.50   14.35    --   24.81  57.00 120.00   56
  7  \w    -50.00 -13.00   0.50   14.35    --   24.81 -19.00 -30.00   74
  8  \w    -50.00 -13.00   0.50   14.35    --   24.81 -19.00-180.00   74
  9  \w      9.00  35.00   0.50   14.35    --   24.81  59.00  74.00   52
 10  \w    -77.00 -39.00   0.50   14.35    --  -25.20 134.00 -89.15   76
 11  \w    -50.00 -13.00   0.50   14.35    --   24.81 -19.00 150.00   74
 12  \w    -16.00  48.00   0.50   14.35    --   24.81 -77.00-120.00  128
 13  \w    -82.00 -51.00   0.50   14.35    --  -25.20 141.00 -51.73   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0179348000
_diffrn_orient_matrix_UB_12      0.0315698000
_diffrn_orient_matrix_UB_13      -0.0226626000
_diffrn_orient_matrix_UB_21      -0.0317779000
_diffrn_orient_matrix_UB_22      0.0000564000
_diffrn_orient_matrix_UB_23      0.0158099000
_diffrn_orient_matrix_UB_31      0.0194381000
_diffrn_orient_matrix_UB_32      0.0291372000
_diffrn_orient_matrix_UB_33      0.0244815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         1.851
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0165
_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^)+(0.0099P)^2^+15.0761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0337
_refine_ls_wR_factor_ref         0.0342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4817
_reflns_number_total             5159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02207f2.cif
_cod_data_source_block           al_003_c2_auto
_cod_depositor_comments
'Adding full bibliography for 7133285--7133286.cif.'
_cod_database_code               7133285
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C16(H16A,H16B), C11(H11A,H11B)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C14(H14A,H14B,
 H14C), C6(H6A,H6B,H6C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C7(H7A,H7B,
 H7C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C24(H24A,H24B,
 H24C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              38454
_shelx_hkl_checksum              71358
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.653
_oxdiff_exptl_absorpt_empirical_full_min 0.593