A synthetic cycle for iminophosphorane synthesis involving direct intermolecular NP bond formation on N<sub>2</sub>-derived molybdenum nitride.
Jin, Li; Zhang, Guoqiang; Yang, Xiaoqin; Song, Jinyi; Wang, Jin; Liao, Qian; Chemical communications (Cambridge, England) 59 (2023) 7955–7958; doi:10.1039/d3cc01925j

data_1569255
_publ_section_title
;
 A synthetic cycle for iminophosphorane synthesis involving direct
 intermolecular N&#xe001;P bond formation on N<sub>2</sub>-derived
 molybdenum nitride.
;
_journal_issue                   51
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7955
_journal_page_last               7958
_journal_paper_doi               10.1039/d3cc01925j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         C26H44MoIN3P3,I
_chemical_formula_sum            'C26 H44 I2 Mo N3 P3'
_chemical_formula_weight         841.29
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-04-11 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.891(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0447(19)
_cell_length_b                   12.5657(13)
_cell_length_c                   16.0127(17)
_cell_measurement_reflns_used    1917
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.23
_cell_measurement_theta_min      2.48
_cell_volume                     3298.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0991
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25483
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.414
_diffrn_reflns_theta_max         24.414
_diffrn_reflns_theta_min         2.240
_exptl_absorpt_coefficient_mu    2.434
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, hexane'
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0491P)^2^+18.2406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4117
_reflns_number_total             5427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01925j2.cif
_cod_data_source_block           MoNPMe2Ph
_cod_depositor_comments
'Adding full bibliography for 1569251--1569256.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1569255
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.688
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              89202
_shelx_hkl_checksum              68750