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_1575159
_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 H45 Ir Mo N4 O2'
_chemical_formula_sum            'C24 H45 Ir Mo N4 O2'
_chemical_formula_weight         709.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-28
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2024-12-16 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.443(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3416(2)
_cell_length_b                   18.4312(4)
_cell_length_c                   14.9177(3)
_cell_measurement_reflns_used    51684
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      29.8340
_cell_measurement_theta_min      2.4230
_cell_volume                     2753.57(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.125a 64-bit (release 04-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.124a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(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 0.999
_diffrn_measured_fraction_theta_max 0.937
_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     -3.00  55.00   0.50   18.00    --   10.72-105.00 140.00  116
  2  \w    -94.00 -40.00   0.50   18.00    --  -10.09 -19.00 -90.00  108
  3  \w    -94.00 -40.00   0.50   18.00    --  -10.09 -19.00 -30.00  108
  4  \w    -94.00 -40.00   0.50   18.00    --  -10.09 -19.00  30.00  108
  5  \w    -73.00 -39.00   0.50   18.00    --  -10.09 137.00 -33.28   68
  6  \w      8.00  43.00   0.50   18.00    --  -10.09-122.00 127.25   70
  7  \w    -73.00 -38.00   0.50   18.00    --  -10.09 136.00  99.36   70
  8  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00 150.00   66
  9  \w     -7.00  38.00   0.50   18.00    --   10.72  57.00   0.00   90
 10  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00-150.00   66
 11  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00-180.00   66
 12  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00 -60.00   66
 13  \w    -59.00  24.00   0.50   18.00    --   10.72 -57.00  30.00  166
 14  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00-120.00   66
 15  \w     -7.00  38.00   0.50   18.00    --   10.72  57.00-180.00   90
 16  \w    -59.00  24.00   0.50   18.00    --   10.72 -57.00  30.00  166
 17  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00 -90.00   66
 18  \w     -7.00  38.00   0.50   18.00    --   10.72  57.00 -60.00   90
 19  \w    -94.00 -40.00   0.50   18.00    --  -10.09 -19.00 150.00  108
 20  \w    -67.00 -32.00   0.50   18.00    --  -10.09 126.00 -62.34   70
 21  \w    -28.00  38.00   0.50   18.00    --  -10.09  57.00 -30.00  132
 22  \w    -73.00 -38.00   0.50   18.00    --  -10.09 136.00   8.97   70
 23  \w     13.00  49.00   0.50   18.00    --  -10.09-130.00 161.35   72
 24  \w    -68.00 -33.00   0.50   18.00    --  -10.09 128.00-173.40   70
 25  \w    -67.00 -32.00   0.50   18.00    --  -10.09 126.00-131.28   70
 26  \w     -7.00  38.00   0.50   18.00    --   10.72  57.00 120.00   90
 27  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00   0.00   66
 28  \w     -3.00  55.00   0.50   18.00    --   10.72-105.00 -25.69  116
 29  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00 120.00   66
 30  \w     -7.00  38.00   0.50   18.00    --   10.72  57.00-120.00   90
 31  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00  90.00   66
 32  \w    -73.00 -40.00   0.50   18.00    --   10.72 -19.00 -30.00   66
 33  \w    -67.00 -32.00   0.50   18.00    --  -10.09 126.00 102.41   70
 34  \w    -28.00  38.00   0.50   18.00    --  -10.09  57.00  90.00  132
 35  \w    -94.00 -40.00   0.50   18.00    --  -10.09 -19.00  60.00  108
 36  \w    -94.00 -40.00   0.50   18.00    --  -10.09 -19.00 -60.00  108
 37  \w    -94.00 -63.00   0.50   18.00    --  -10.09 -19.00 120.00   62
 38  \w     -7.00  51.00   0.50   18.00    --   10.72 -99.00-120.00  116
;
_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      -0.0226564000
_diffrn_orient_matrix_UB_12      -0.0364443000
_diffrn_orient_matrix_UB_13      -0.0028428000
_diffrn_orient_matrix_UB_21      0.0339967000
_diffrn_orient_matrix_UB_22      -0.0070359000
_diffrn_orient_matrix_UB_23      -0.0349165000
_diffrn_orient_matrix_UB_31      0.0578834000
_diffrn_orient_matrix_UB_32      -0.0101550000
_diffrn_orient_matrix_UB_33      0.0343824000
_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  0.0767
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            119373
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.940
_diffrn_reflns_theta_min         2.314
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.124a (Rigaku Oxford Diffraction, 2024)
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    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.447
_refine_diff_density_min         -2.891
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         7504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+39.0068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6502
_reflns_number_total             7504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03465e2.cif
_cod_data_source_block           zd225_2
_cod_depositor_comments
'Adding full bibliography for 1575153--1575159.cif.'
_cod_original_cell_volume        2753.56(11)
_cod_database_code               1575159
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo Ir C H N O'
_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:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              39595
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZD225
_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 3.708
_oxdiff_exptl_absorpt_empirical_full_min 0.464