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_7719528
_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         'C29 H46 I Mo N3 O3 P2, C H2 Cl2'
_chemical_formula_sum            'C30 H48 Cl2 I Mo N3 O3 P2'
_chemical_formula_weight         854.39
_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             2025-06-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-08-14 deposited with the CCDC.	2025-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.191(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8257(6)
_cell_length_b                   14.8939(4)
_cell_length_c                   17.2162(7)
_cell_measurement_reflns_used    14826
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.6760
_cell_measurement_theta_min      1.9010
_cell_volume                     3520.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.44.92a (Rigaku OD, 2025)'
_computing_data_collection       'CrysAlisPro 1.171.44.92a (Rigaku OD, 2025)'
_computing_data_reduction        'CrysAlisPro 1.171.44.92a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (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 0.994
_diffrn_measured_fraction_theta_max 0.789
_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    -76.00 -26.00   0.50   40.46    --   -4.50 -46.00  74.00  100
  2  \w      2.00  64.00   0.50   40.46    --   -4.50  46.00-136.00  124
  3  \w    -10.00  36.00   0.50   40.46    --    5.90 -99.00-120.00   92
  4  \w      5.00  31.00   0.50   40.46    --    5.90 -99.00 -30.00   52
  5  \w     -1.00  78.00   0.50   40.46    --    5.90  37.00-180.00  158
  6  \w     -6.00  36.00   0.50   40.46    --    5.90 -99.00   0.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, SynergyCustom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0440836000
_diffrn_orient_matrix_UB_12      -0.0233014000
_diffrn_orient_matrix_UB_13      0.0065435000
_diffrn_orient_matrix_UB_21      0.0188422000
_diffrn_orient_matrix_UB_22      0.0142364000
_diffrn_orient_matrix_UB_23      0.0424682000
_diffrn_orient_matrix_UB_31      -0.0193710000
_diffrn_orient_matrix_UB_32      -0.0390091000
_diffrn_orient_matrix_UB_33      0.0114232000
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33562
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.989
_diffrn_reflns_theta_min         2.018
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.92a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.220
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         8840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0729P)^2^+2.7338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6756
_reflns_number_total             8840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02036k3.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7719525--7719529.cif.'
_cod_database_code               7719528
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C30 H50 N3 O3 Mo I P2'
_chemical_oxdiff_usercomment     'CSD: REHYOV'
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.657
_diffrn_oxdiff_digest_od_ed
;

;
_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), C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B), C1M(H1MA,H1MB)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C12(H12), C14(H14), C1B(H1B)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C),
 C19(H19A,H19B,H19C), C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,H1DC), C1F(H1FA,H1FB,
 H1FC), C1H(H1HA,H1HB,H1HC), C1J(H1JA,H1JB,H1JC), C1K(H1KA,H1KB,H1KC), C1L(H1LA,
 H1LB,H1LC)
;
_shelx_res_checksum              75935
_shelx_hkl_checksum              3422
_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 1.672
_oxdiff_exptl_absorpt_empirical_full_min 0.687