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_1569251
_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         'C30H60IMoN3P3, I'
_chemical_formula_sum            'C30 H60 I2 Mo N3 P3'
_chemical_formula_weight         905.46
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_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                 101.483(3)
_cell_angle_gamma                90
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_cell_length_b                   20.5955(16)
_cell_length_c                   17.0359(13)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.44
_cell_volume                     3870.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0798
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
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_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28227
_diffrn_reflns_point_group_measured_fraction_full 0.995
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_diffrn_reflns_theta_full        25.082
_diffrn_reflns_theta_max         25.082
_diffrn_reflns_theta_min         2.094
_exptl_absorpt_coefficient_mu    2.081
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
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_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, hexane'
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_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.605
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_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         6841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0535P)^2^+1.4694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5950
_reflns_number_total             6841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01925j2.cif
_cod_data_source_block           MoNPBu3
_cod_depositor_comments
'Adding full bibliography for 1569251--1569256.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1569251
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.329
_shelx_estimated_absorpt_t_max   0.898
_shelx_res_checksum              81136
_shelx_hkl_checksum              83900