Reactivity of a molybdenum-nitride complex bearing an NHC-based PCP-type pincer ligand toward unsaturated substrates.
Miyazaki, Tomoyuki; Suginome, Shun; Nakamura, Taiji; Tanaka, Hiromasa; Yoshizawa, Kazunari; Nishibayashi, Yoshiaki; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15864–15872; doi:10.1039/d5dt02036k

data_7719527
_publ_section_title
;
 Reactivity of a molybdenum-nitride complex bearing an NHC-based PCP-type
 pincer ligand toward unsaturated substrates.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15864
_journal_page_last               15872
_journal_paper_doi               10.1039/d5dt02036k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'I, C27 H48 Mo N3 P2, C4 H8 O'
_chemical_formula_sum            'C31 H56 I Mo N3 O P2'
_chemical_formula_weight         771.56
_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             2023-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-08-14 deposited with the CCDC.	2025-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.724(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3696(3)
_cell_length_b                   11.6652(3)
_cell_length_c                   22.8440(5)
_cell_measurement_reflns_used    19899
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.1560
_cell_measurement_theta_min      2.1590
_cell_volume                     3544.96(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.803
_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    -60.00  10.00   0.50    2.02    --   -4.78 -57.00 -60.00  140
  2  \w    -18.00  33.00   0.50    2.02    --   -4.78  34.00 -26.00  102
  3  \w    -31.00  11.00   0.50    2.02    --   -4.78 -77.00  90.00   84
  4  \w    -76.00   6.00   0.50    2.02    --   -4.78 -34.00 176.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0517323000
_diffrn_orient_matrix_UB_12      -0.0070839000
_diffrn_orient_matrix_UB_13      0.0036256000
_diffrn_orient_matrix_UB_21      -0.0077886000
_diffrn_orient_matrix_UB_22      -0.0259077000
_diffrn_orient_matrix_UB_23      -0.0281732000
_diffrn_orient_matrix_UB_31      0.0103954000
_diffrn_orient_matrix_UB_32      -0.0545271000
_diffrn_orient_matrix_UB_33      0.0129204000
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30065
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.836
_diffrn_reflns_theta_min         2.238
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         8945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+3.1683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7682
_reflns_number_total             8945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02036k3.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7719525--7719529.cif.'
_cod_original_cell_volume        3544.95(14)
_cod_database_code               7719527
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         Mo1P2I1C50H30N3
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.686
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C22(H22A,H22B), C36(H36A,H36B), C12(H12A,H12B),
 C35(H35A,H35B), C34(H34A,H34B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C6(H6), C5(H5)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C15(H15A,H15B,H15C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C20(H20A,
 H20B,H20C), C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              20886
_shelx_hkl_checksum              75316
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.705