Phosphinidene Reactivity of a Transient Vanadium P≡N Complex.
Courtemanche, Marc-André; Transue, Wesley J.; Cummins, Christopher C.; Journal of the American Chemical Society 138 (2016) 16220–16223; doi:10.1021/jacs.6b10545

data_4131178
_publ_section_title
;
 Phosphinidene Reactivity of a Transient Vanadium P\\tb N Complex.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16220
_journal_page_last               16223
_journal_paper_doi               10.1021/jacs.6b10545
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C46 H58 N4 P S2 V'
_chemical_formula_weight         812.99
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.6160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6897(7)
_cell_length_b                   11.2855(6)
_cell_length_c                   26.2745(13)
_cell_measurement_reflns_used    9449
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.43
_cell_volume                     4351.3(4)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            260543
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.617
_diffrn_reflns_theta_min         1.388
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.4843
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         13289
_refine_ls_number_restraints     3195
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+3.5958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11170
_reflns_number_total             13289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10545_si_002.cif
_cod_data_source_block           X8_16026
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4131178
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.939
_shelx_res_checksum              94702
_shelx_hkl_checksum              22519