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_7133286
_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         'C11 H18 O Os'
_chemical_formula_sum            'C11 H18 O Os'
_chemical_formula_weight         356.45
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-10
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2024-06-10 deposited with the CCDC.	2024-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.769(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1490(2)
_cell_length_b                   11.0276(2)
_cell_length_c                   13.2481(2)
_cell_measurement_reflns_used    20648
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      30.3780
_cell_measurement_theta_min      2.4220
_cell_volume                     1165.50(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.888
_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     -6.00  39.00   0.50    1.68    --    7.11  57.00-180.00   90
  2  \w    -19.00  39.00   0.50    1.68    --   -6.25  57.00-150.00  116
  3  \w     -6.00  39.00   0.50    1.68    --    7.11  57.00-120.00   90
  4  \w    -60.00   7.00   0.50    1.68    --   -6.25 -57.00 -90.00  134
  5  \w    -85.00 -40.00   0.50    1.68    --   -6.25 -19.00-150.00   90
  6  \w    -85.00 -44.00   0.50    1.68    --   -6.25 -18.00 -35.00   82
  7  \w      1.00  86.00   0.50    1.68    --    7.11  18.00 132.00  170
  8  \w      1.00  73.00   0.50    1.68    --   -6.25  18.00 132.00  144
  9  \w     -4.00  42.00   0.50    1.68    --    7.11 -99.00 -30.00   92
 10  \w     -4.00  42.00   0.50    1.68    --    7.11 -99.00-180.00   92
 11  \w     -4.00  42.00   0.50    1.68    --    7.11 -99.00  60.00   92
 12  \w     -4.00  42.00   0.50    1.68    --    7.11 -99.00 120.00   92
 13  \w    -73.00 -48.00   0.50    1.68    --    7.11 -19.00  60.00   50
 14  \w    -73.00 -40.00   0.50    1.68    --    7.11 -19.00  30.00   66
 15  \w    -72.00 -44.00   0.50    1.68    --    7.11 -18.00 -35.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0862945000
_diffrn_orient_matrix_UB_12      -0.0100409000
_diffrn_orient_matrix_UB_13      -0.0206514000
_diffrn_orient_matrix_UB_21      -0.0137231000
_diffrn_orient_matrix_UB_22      -0.0117520000
_diffrn_orient_matrix_UB_23      0.0502575000
_diffrn_orient_matrix_UB_31      -0.0165004000
_diffrn_orient_matrix_UB_32      0.0624391000
_diffrn_orient_matrix_UB_33      0.0061190000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26457
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.382
_diffrn_reflns_theta_min         2.424
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.191
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.00155(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3126
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+1.3111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2903
_reflns_number_total             3126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02207f2.cif
_cod_data_source_block           al143_2_autored
_cod_depositor_comments
'Adding full bibliography for 7133285--7133286.cif.'
_cod_database_code               7133286
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H60 O4 Os4 '
_shelx_estimated_absorpt_t_max   0.230
_shelx_estimated_absorpt_t_min   0.157
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
HA \\sim HB \\sim HC: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.08 within 1.7A
3. Rigid body (RIGU) restrains
 C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Uiso: HA(0.035) HB(0.035) HC(0.035)
5.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              77600
_shelx_hkl_checksum              31474
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id AL143_2
_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 1.402
_oxdiff_exptl_absorpt_empirical_full_min 0.724