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_1575155
_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         'C19 H33 Ir Mo N3 O'
_chemical_formula_sum            'C19 H33 Ir Mo N3 O'
_chemical_formula_weight         607.62
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-04
_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                 104.700(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4733(2)
_cell_length_b                   14.1270(3)
_cell_length_c                   15.9700(3)
_cell_measurement_reflns_used    24702
_cell_measurement_temperature    100.02(16)
_cell_measurement_theta_max      30.4650
_cell_measurement_theta_min      2.4670
_cell_volume                     2285.52(8)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(16)
_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 0.872
_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     -7.00  38.00   0.50    2.00    --   -2.19  57.00 -60.00   90
  2  \w     -7.00  38.00   0.50    2.00    --   -2.19  57.00  30.00   90
  3  \w     -1.00  71.00   0.50    2.00    --   -2.19  39.00 140.00  144
  4  \w    -74.00 -40.00   0.50    2.00    --   -2.19 -19.00 120.00   68
  5  \w    -75.00  -3.00   0.50    2.00    --   -2.19 -39.00 -13.00  144
  6  \w    -74.00 -40.00   0.50    2.00    --   -2.19 -19.00  90.00   68
  7  \w    -74.00 -40.00   0.50    2.00    --   -2.19 -19.00 -60.00   68
  8  \w    -74.00 -40.00   0.50    2.00    --   -2.19 -19.00 150.00   68
  9  \w    -74.00 -40.00   0.50    2.00    --   -2.19 -19.00 -90.00   68
 10  \w    -74.00 -40.00   0.50    2.00    --   -2.19 -19.00-120.00   68
 11  \w    -74.00 -40.00   0.50    2.00    --   -2.19 -19.00-150.00   68
 12  \w    -70.00 -40.00   0.50    2.00    --    2.66 -19.00-180.00   60
 13  \w    -70.00 -40.00   0.50    2.00    --    2.66 -19.00-120.00   60
 14  \w     -1.00  63.00   0.50    2.00    --    2.66  19.00 -90.00  128
;
_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      -0.0442410000
_diffrn_orient_matrix_UB_12      -0.0109268000
_diffrn_orient_matrix_UB_13      -0.0404053000
_diffrn_orient_matrix_UB_21      -0.0431613000
_diffrn_orient_matrix_UB_22      -0.0220831000
_diffrn_orient_matrix_UB_23      0.0218106000
_diffrn_orient_matrix_UB_31      -0.0328198000
_diffrn_orient_matrix_UB_32      0.0437652000
_diffrn_orient_matrix_UB_33      0.0009424000
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.124a (Rigaku Oxford Diffraction, 2024)
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    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.127
_refine_diff_density_max         3.224
_refine_diff_density_min         -1.926
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         6080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0474P)^2^+7.1396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5164
_reflns_number_total             6080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03465e2.cif
_cod_data_source_block           zd222_autored
_cod_depositor_comments
'Adding full bibliography for 1575153--1575159.cif.'
_cod_database_code               1575155
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C110 H100 N10 O10 I0 Ta1 Mo1 Ir1 '
_shelx_estimated_absorpt_t_max   0.498
_shelx_estimated_absorpt_t_min   0.140
_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.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              30455
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZD222
_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 4.603
_oxdiff_exptl_absorpt_empirical_full_min 0.574