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_4131182
_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            'C76 H118 N8 O P2 V2'
_chemical_formula_weight         1323.60
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   29.3330(12)
_cell_length_b                   29.3330(12)
_cell_length_c                   23.1240(10)
_cell_measurement_reflns_used    9617
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.30
_cell_volume                     17230.8(12)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            179237
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.066
_diffrn_reflns_theta_max         25.066
_diffrn_reflns_theta_min         1.191
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6426
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.104
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.6993
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0688P)^2^+61.9736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5872
_reflns_number_total             6811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10545_si_003.cif
_cod_data_source_block           X8_16036
_cod_original_cell_volume        17230.8(16)
_cod_database_code               4131182
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.937
_shelx_estimated_absorpt_t_max   0.966
_shelx_res_checksum              24578
_shelx_hkl_checksum              97230