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_7719525
_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, C26 H44 Mo N3 O P2, 2(C4 H8 O)'
_chemical_formula_sum            'C34 H59 I Mo N3 O3 P2'
_chemical_formula_weight         842.62
_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             2025-06-26
_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                 96.190(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7864(4)
_cell_length_b                   12.2202(3)
_cell_length_c                   17.8968(5)
_cell_measurement_reflns_used    13268
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.1690
_cell_measurement_theta_min      2.1090
_cell_volume                     3867.25(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.779
_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    -69.00  13.00   0.50    4.86    --    5.71 -19.00 144.00  164
  2  \w     -3.00  80.00   0.50    4.86    --    5.71  19.00 -47.00  166
  3  \w    -60.00   2.00   0.50    4.86    --   -4.78 -57.00  60.00  124
  4  \w    -18.00   7.00   0.50    4.86    --    5.71 -37.00 -90.00   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      -0.0132628000
_diffrn_orient_matrix_UB_12      -0.0094363000
_diffrn_orient_matrix_UB_13      -0.0382714000
_diffrn_orient_matrix_UB_21      0.0375339000
_diffrn_orient_matrix_UB_22      -0.0107895000
_diffrn_orient_matrix_UB_23      -0.0078610000
_diffrn_orient_matrix_UB_31      -0.0049625000
_diffrn_orient_matrix_UB_32      -0.0562416000
_diffrn_orient_matrix_UB_33      0.0079248000
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33552
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.068
_diffrn_reflns_theta_min         2.026
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42278
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       needle
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.527
_refine_diff_density_min         -1.968
_refine_diff_density_rms         0.105
_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     551
_refine_ls_number_reflns         9675
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0432P)^2^+7.8468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7523
_reflns_number_total             9675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02036k3.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7719525--7719529.cif.'
_cod_database_code               7719525
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.573
_diffrn_oxdiff_digest_hkl
;
0172d2f1caaf1377a2631deb93e269bd2e1797
;
_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
O2 \\sim C30 \\sim C29 \\sim C28 \\sim C27: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 N2, C3B, C3A, P1B, P1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13B, C11B, C12B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C30, C29, C28, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(P1B)=Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C13B)=Sof(H13A)=
 Sof(H13B)=Sof(H13C)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11B)=
 Sof(C15B)=Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C16B)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(C17B)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=1-FVAR(1)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=
 Sof(C15A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11A)=
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(P1A)=FVAR(1)
 Fixed Sof: O3(0.5) O4(0.5) C14(0.5) H14G(0.5) H14H(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C16(0.5) H16G(0.5) H16H(0.5) C12(0.5)
 H12G(0.5) H12H(0.5) C31(0.5) H31A(0.5) H31B(0.5) C18(0.5) H18G(0.5) H18H(0.5)
 C17(0.5) H17G(0.5) H17H(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C10(H10A,H10B), C29(H29A,H29B), C28(H28A,H28B), C27(H27A,
 H27B), C30(H30A,H30B), C3B(H3BA,H3BB), C14(H14G,H14H), C3(H3A,H3B), C11(H11A,
 H11B), C16(H16G,H16H), C12(H12G,H12H), C31(H31A,H31B), C18(H18G,H18H),
 C17(H17G,H17H)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C6(H6)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C14B(H14A,H14B,H14C),
 C13B(H13A,H13B,H13C), C12B(H12A,H12B,H12C), C18B(H18A,H18B,H18C), C16B(H16A,
 H16B,H16C), C17B(H17A,H17B,H17C), C18A(H18D,H18E,H18F), C16A(H16D,H16E,H16F),
 C17A(H17D,H17E,H17F), C12A(H12D,H12E,H12F), C14A(H14D,H14E,H14F), C13A(H13D,
 H13E,H13F)
;
_shelx_res_checksum              5162
_shelx_hkl_checksum              63671
_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 1.624
_oxdiff_exptl_absorpt_empirical_full_min 0.726