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_4314021
_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            'C15 H26 Cl2 N2 P V'
_chemical_formula_weight         387.19
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 93.9520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.0233(5)
_cell_length_b                   8.7868(2)
_cell_length_c                   15.51160(10)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3946.39(12)
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9748
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.152542
_exptl_absorpt_correction_T_min  0.099208
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.36(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5453
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.193
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                4042
_reflns_number_total             5453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030151d_2.cif
_cod_data_source_block           (i-Pr3PN)(PhN)VCl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'momoclinic' was replaced with
'monoclinic' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314021