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_1569253
_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         C21H33IMoN2O3P2
_chemical_formula_sum            'C21 H33 I Mo N2 O3 P2'
_chemical_formula_weight         646.27
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9591(3)
_cell_length_b                   13.17384(15)
_cell_length_c                   14.86566(17)
_cell_measurement_reflns_used    11349
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      75.1090
_cell_measurement_theta_min      4.7530
_cell_volume                     5083.77(10)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14290
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.437
_diffrn_reflns_theta_min         4.798
_exptl_absorpt_coefficient_mu    15.143
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.46836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, hexane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
; 
 Flack x determined using 1130 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.018(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2568
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+9.7299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                2523
_reflns_number_total             2568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01925j2.cif
_cod_data_source_block           MoCO3
_cod_depositor_comments
'Adding full bibliography for 1569251--1569256.cif.'
_cod_database_code               1569253
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              51167
_shelx_hkl_checksum              13579