Synergistic C-H bond activation across molybdenum-iridium multiply bonded complexes: a cascade of transformations.
Dubrawski, Zachary; Del Rosal, Iker; Jeanneau, Erwann; Maron, Laurent; Thieuleux, Chloé; Camp, Clément; Chemical science 16 (2025) 14564–14577; doi:10.1039/d5sc03465e

data_1575154
_publ_section_title
;
 Synergistic C-H bond activation across molybdenum-iridium multiply bonded
 complexes: a cascade of transformations.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              14564
_journal_page_last               14577
_journal_paper_doi               10.1039/d5sc03465e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C24 H42 Ir2 Mo N2'
_chemical_formula_sum            'C24 H42 Ir2 Mo N2'
_chemical_formula_weight         838.93
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-17
_audit_creation_method
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_audit_update_record
;
2024-12-16 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                86.4790(10)
_cell_angle_beta                 80.4780(10)
_cell_angle_gamma                80.6460(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3728(2)
_cell_length_b                   11.1282(2)
_cell_length_c                   11.9391(2)
_cell_measurement_reflns_used    36432
_cell_measurement_temperature    100.1(4)
_cell_measurement_theta_max      30.4000
_cell_measurement_theta_min      2.4360
_cell_volume                     1340.23(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.93a 64-bit (release 17-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.838
_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    -33.00  20.00   0.50    2.69    --    6.38 -68.00-102.00  106
  2  \w    -16.00  39.00   0.50    2.69    --   -5.37  57.00 -90.00  110
  3  \w    -60.00   6.00   0.50    2.69    --   -5.37 -57.00 120.00  132
  4  \w    -60.00   6.00   0.50    2.69    --   -5.37 -57.00-180.00  132
  5  \w    -60.00   6.00   0.50    2.69    --   -5.37 -57.00  30.00  132
  6  \w    -60.00   6.00   0.50    2.69    --   -5.37 -57.00 -90.00  132
  7  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00-150.00   62
  8  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00 -60.00   62
  9  \w    -21.00  25.00   0.50    2.69    --    6.38 -77.00  30.00   92
 10  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00 120.00   62
 11  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00 150.00   62
 12  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00-180.00   62
 13  \w    -14.00  73.00   0.50    2.69    --   -5.37  38.00-150.00  174
 14  \w    -21.00  25.00   0.50    2.69    --    6.38 -77.00-150.00   92
 15  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00-120.00   62
 16  \w    -21.00  25.00   0.50    2.69    --    6.38 -77.00   0.00   92
 17  \w    -21.00  25.00   0.50    2.69    --    6.38 -77.00  60.00   92
 18  \w    -21.00  25.00   0.50    2.69    --    6.38 -77.00-180.00   92
 19  \w    -21.00  25.00   0.50    2.69    --    6.38 -77.00 120.00   92
 20  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00 -30.00   62
 21  \w    -21.00  25.00   0.50    2.69    --    6.38 -77.00 -60.00   92
 22  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00  90.00   62
 23  \w    -14.00  73.00   0.50    2.69    --   -5.37  38.00 120.00  174
 24  \w    -14.00  73.00   0.50    2.69    --   -5.37  38.00   0.00  174
 25  \w    -83.00 -40.00   0.50    2.69    --   -5.37 -19.00-150.00   86
 26  \w    -21.00  25.00   0.50    2.69    --    6.38 -77.00  90.00   92
 27  \w    -71.00 -40.00   0.50    2.69    --    6.38 -19.00 -90.00   62
;
_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      0.0028588000
_diffrn_orient_matrix_UB_12      -0.0521735000
_diffrn_orient_matrix_UB_13      0.0372799000
_diffrn_orient_matrix_UB_21      -0.0464981000
_diffrn_orient_matrix_UB_22      -0.0227165000
_diffrn_orient_matrix_UB_23      -0.0271576000
_diffrn_orient_matrix_UB_31      0.0524907000
_diffrn_orient_matrix_UB_32      -0.0306603000
_diffrn_orient_matrix_UB_33      -0.0388085000
_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  0.0840
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36487
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.615
_diffrn_reflns_theta_min         2.440
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.378
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.92a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.152
_refine_diff_density_max         3.306
_refine_diff_density_min         -3.973
_refine_diff_density_rms         0.325
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         6919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6208
_reflns_number_total             6919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03465e2.cif
_cod_data_source_block           zd025_autored
_cod_depositor_comments
'Adding full bibliography for 1575153--1575159.cif.'
_cod_database_code               1575154
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H42 N2 Mo1 Ir2 '
_shelx_estimated_absorpt_t_max   0.301
_shelx_estimated_absorpt_t_min   0.132
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C23(H23A,H23B,
 H23C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C17(H17A,
 H17B,H17C), C21(H21A,H21B,H21C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,
 H7C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              10031
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZD025
_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 4.608
_oxdiff_exptl_absorpt_empirical_full_min 0.432