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_7719529
_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         '2(I), 2(C25 H44 Mo N3 O2 P2), 2(C4 H8 O)'
_chemical_formula_sum            'C58 H104 I2 Mo2 N6 O6 P4'
_chemical_formula_weight         1551.03
_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             2025-05-21
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-08-14 deposited with the CCDC.	2025-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.114(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9072(5)
_cell_length_b                   12.0684(2)
_cell_length_c                   25.0037(5)
_cell_measurement_reflns_used    29796
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.2140
_cell_measurement_theta_min      1.9430
_cell_volume                     6843.2(2)
_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 0.810
_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     -5.00  33.00   0.50    0.99    --    5.71 -99.00 120.00   76
  2  \w    -11.00  26.00   0.50    0.99    --    5.71 -96.00 -55.00   74
  3  \w    -67.00  16.00   0.50    0.99    --    5.71 -37.00-150.00  166
  4  \w    -18.00  19.00   0.50    0.99    --    5.71  96.00  53.00   74
  5  \w    -76.00  10.00   0.50    0.99    --   -4.62 -57.00-150.00  172
  6  \w    -32.00  -7.00   0.50    0.99    --   -4.62  96.00  53.00   50
;
_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      0.0082634000
_diffrn_orient_matrix_UB_12      -0.0551929000
_diffrn_orient_matrix_UB_13      0.0072372000
_diffrn_orient_matrix_UB_21      0.0205316000
_diffrn_orient_matrix_UB_22      0.0006440000
_diffrn_orient_matrix_UB_23      -0.0187802000
_diffrn_orient_matrix_UB_31      0.0220706000
_diffrn_orient_matrix_UB_32      0.0201151000
_diffrn_orient_matrix_UB_33      0.0204280000
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            68921
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.054
_diffrn_reflns_theta_min         1.877
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.411
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82785
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.494
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         17771
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0440P)^2^+26.2799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13200
_reflns_number_total             17771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02036k3.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7719525--7719529.cif.'
_cod_database_code               7719529
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.677
_shelx_estimated_absorpt_t_min   0.677
_diffrn_oxdiff_digest_hkl
;
0136240a0c477efb5270f529383941d6433b53
;
_reflns_odcompleteness_completeness 99.94
_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. Uiso/Uaniso restraints and constraints
Mo3 \\sim P3 \\sim P4: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 Mo3, P4, P3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Mo3)=1-FVAR(1)
 Sof(Mo2)=FVAR(1)
 Sof(I1A)=1-FVAR(2)
 Sof(I1)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C16(H16A,H16B), C49(H49A,H49B), C59(H59A,H59B), C77(H77A,
 H77B), C76(H76A,H76B), C75(H75A,H75B), C78(H78A,H78B), C72(H72A,H72B),
 C73(H73A,H73B), C70(H70A,H70B), C71(H71A,H71B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C41(H41), C8(H8), C6(H6), C39(H39), C42(H42), C40(H40), C7(H7)
5.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C23(H23A,H23B,H23C), C63(H63A,H63B,H63C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C), C19(H19A,H19B,H19C), C29(H29A,H29B,H29C),
 C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C56(H56A,H56B,H56C), C21(H21A,H21B,
 H21C), C30(H30A,H30B,H30C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C52(H52A,
 H52B,H52C), C25(H25A,H25B,H25C), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C),
 C53(H53A,H53B,H53C), C58(H58A,H58B,H58C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82922
_shelx_hkl_checksum              32777
_shelx_fab_checksum              82468
_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 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.867