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_7719526
_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, C30 H52 Mo N3 P2, C4 H8 O'
_chemical_formula_sum            'C34 H60 I Mo N3 O P2'
_chemical_formula_weight         811.63
_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
_audit_creation_date             2025-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-08-14 deposited with the CCDC.	2025-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.652(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4356(5)
_cell_length_b                   11.5583(3)
_cell_length_c                   20.5278(6)
_cell_measurement_reflns_used    13967
_cell_measurement_temperature    93.00
_cell_measurement_theta_max      31.1260
_cell_measurement_theta_min      2.1440
_cell_volume                     3817.8(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      93.00
_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 0.818
_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    -51.00 -25.00   0.50    5.28    --   -4.62 -17.00  92.00   52
  2  \w    -18.00  71.00   0.50    5.28    --   -4.62  17.00 -98.00  178
  3  \w    -71.00   7.00   0.50    5.28    --   -4.62 -37.00 -90.00  156
  4  \w      2.00  27.00   0.50    5.28    --    5.56 -99.00-150.00   50
  5  \w    -11.00  27.00   0.50    5.28    --    5.56 -99.00 120.00   76
  6  \w    -10.00  35.00   0.50    5.28    --    5.56 -99.00  90.00   90
;
_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      0.0429130000
_diffrn_orient_matrix_UB_12      0.0137823000
_diffrn_orient_matrix_UB_13      0.0127558000
_diffrn_orient_matrix_UB_21      -0.0015250000
_diffrn_orient_matrix_UB_22      -0.0008311000
_diffrn_orient_matrix_UB_23      -0.0350496000
_diffrn_orient_matrix_UB_31      -0.0098658000
_diffrn_orient_matrix_UB_32      0.0597864000
_diffrn_orient_matrix_UB_33      -0.0034266000
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.818
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38372
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.759
_diffrn_reflns_theta_min         1.951
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72164
_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_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.661
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         9755
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0808P)^2^+16.9851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6673
_reflns_number_total             9755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02036k3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7719525--7719529.cif.'
_cod_database_code               7719526
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C30H52P2MoN3I
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.786
_diffrn_oxdiff_digest_hkl
;
019b27b8be9ab2894b207980e39bc26297aa3e
;
_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. Restrained distances
 C13-O1
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C39 \\sim C38 \\sim C13 \\sim C10: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C13, C10, C39, C38, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C22(H22A,H22B), C3(H3A,H3B), C4(H4A,H4B), C39(H39A,H39B),
 C38(H38A,H38B), C13(H13A,H13B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C7(H7), C8(H8), C11(H11), C1(H1)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C25(H25A,
 H25B,H25C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C5(H5A,H5B,H5C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              95382
_shelx_hkl_checksum              75407
_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 1.222
_oxdiff_exptl_absorpt_empirical_full_min 0.748