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_1569252
_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         C31H46IMoN3P3,I
_chemical_formula_sum            'C31 H46 I2 Mo N3 P3'
_chemical_formula_weight         903.36
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 103.547(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.1147(11)
_cell_length_b                   12.0242(4)
_cell_length_c                   19.6739(7)
_cell_measurement_reflns_used    9261
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      62.69
_cell_measurement_theta_min      2.83
_cell_volume                     7385.8(4)
_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      300(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32171
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        63.015
_diffrn_reflns_theta_max         63.015
_diffrn_reflns_theta_min         3.939
_exptl_absorpt_coefficient_mu    17.436
_exptl_absorpt_correction_T_max  0.3138
_exptl_absorpt_correction_T_min  0.1315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       plate
_exptl_crystal_F_000             3568
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, hexane'
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5755
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0628
_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^)+(0.1028P)^2^+82.7405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4473
_reflns_number_total             5755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01925j2.cif
_cod_data_source_block           MoNPMePh2
_cod_depositor_comments
'Adding full bibliography for 1569251--1569256.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1569252
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.109
_shelx_estimated_absorpt_t_max   0.614
_shelx_res_checksum              24011
_shelx_hkl_checksum              40012