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_1575157
_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         'C7 H16 N2 O'
_chemical_formula_sum            'C7 H16 N2 O'
_chemical_formula_weight         144.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-10
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2024-12-16 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9756(3)
_cell_length_b                   11.6881(3)
_cell_length_c                   15.1321(4)
_cell_measurement_reflns_used    3341
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      73.0150
_cell_measurement_theta_min      5.8350
_cell_volume                     1764.34(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.138a 64-bit (release 24-09-2024))'
_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(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 0.997
_diffrn_measured_fraction_theta_max 0.959
_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     17.00  42.00   0.50    5.00    --   52.69-103.00 161.00   50
  2  \w    -55.00 -30.00   0.50    5.00    --  -53.88 103.00 -97.00   50
  3  \w    -31.00   1.00   0.50    5.00    --  -54.50 103.00 -97.00   64
  4  \w    -54.00 -29.00   0.50    5.00    --  -77.16 103.00 -97.00   50
  5  \w     36.00  61.00   0.50   10.00    --   97.76-103.00 161.00   50
  6  \w    -13.00  13.00   0.50    5.00    --   52.69 -38.00 -30.00   52
  7  \w    -16.00  15.00   0.50    5.00    --  -53.88  38.00  90.00   62
  8  \w    -19.00  17.00   0.50    5.00    --  -54.50  38.00 -30.00   72
  9  \w    -15.00  14.00   0.50    5.00    --  -54.50  38.00-120.00   58
 10  \w    -16.00  17.00   0.50    5.00    --  -54.50  38.00-150.00   66
 11  \w    -65.00 -15.00   0.50    5.00    --  -77.16  77.00 120.00  100
 12  \w    -55.00 -23.00   0.50    5.00    --  -77.16  77.00  30.00   64
 13  \w     38.00  65.00   0.50   10.00    --   97.76 -77.00 120.00   54
 14  \w     99.00 140.00   0.50   10.00    --   97.76  19.00-120.00   82
 15  \w     36.00  73.00   0.50   10.00    --   97.76 -77.00-120.00   74
 16  \w     41.00  66.00   0.50   10.00    --   97.76 -77.00  60.00   50
 17  \w     36.00  64.00   0.50   10.00    --   97.76 -77.00 -30.00   56
 18  \w     37.00  63.00   0.50   10.00    --   97.76 -77.00  30.00   52
 19  \w     61.00  86.00   0.50   10.00    --   97.76 -99.00 -90.00   50
 20  \w     37.00  75.00   0.50   10.00    --   97.76 -77.00-180.00   76
 21  \w    109.00 140.00   0.50   10.00    --   97.76  19.00   0.00   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      -0.0763694000
_diffrn_orient_matrix_UB_12      -0.0408394000
_diffrn_orient_matrix_UB_13      -0.0827368000
_diffrn_orient_matrix_UB_21      0.0545767000
_diffrn_orient_matrix_UB_22      0.1032350000
_diffrn_orient_matrix_UB_23      -0.0521737000
_diffrn_orient_matrix_UB_31      0.1225252000
_diffrn_orient_matrix_UB_32      -0.0711524000
_diffrn_orient_matrix_UB_33      -0.0282809000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8064
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.130
_diffrn_reflns_theta_min         5.848
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69391
_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    1.086
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1454
_reflns_number_total             1722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03465e2.cif
_cod_data_source_block           zd299_2
_cod_depositor_comments
'Adding full bibliography for 1575153--1575159.cif.'
_cod_database_code               1575157
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H120 N8 O16 '
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C1(H1A,H1B,H1C), C6(H6A,
 H6B,H6C)
;
_shelx_res_checksum              52359
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZD299_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 1.595
_oxdiff_exptl_absorpt_empirical_full_min 0.598