Synthesis and Characterization of Vanadium(V)-Phosphinimide Complexes
Sarah B. Hawkeswood; Douglas W. Stephan; Inorganic Chemistry 42 (2003) 5429–5433; doi:10.1021/ic030151d

data_4314020
_publ_section_title
;
 Synthesis and Characterization of Vanadium(V)-Phosphinimide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5429
_journal_page_last               5433
_journal_paper_doi               10.1021/ic030151d
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C60 H50 Cl2 N4 P3 V'
_chemical_formula_weight         1041.79
_space_group_IT_number           148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.646(6)
_cell_length_b                   13.646(6)
_cell_length_c                   47.73(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     7697(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            11106
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.145121
_exptl_absorpt_correction_T_min  0.108540
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                1497
_reflns_number_total             2441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030151d_1.cif
_cod_data_source_block           '[(Ph3PN)3VCl]Cl'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4314020