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_4314022
_publ_section_title
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 Synthesis and Characterization of Vanadium(V)-Phosphinimide Complexes
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_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            'C36 H54 N2 P V'
_chemical_formula_weight         596.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.73(3)
_cell_angle_beta                 73.30(3)
_cell_angle_gamma                63.48(3)
_cell_formula_units_Z            2
_cell_length_a                   12.220(3)
_cell_length_b                   13.049(6)
_cell_length_c                   13.108(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1777.6(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.468
_diffrn_measured_fraction_theta_max 0.468
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2935
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.152633
_exptl_absorpt_correction_T_min  0.088162
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+4.7081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1995
_reflns_number_gt                2178
_reflns_number_total             2935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030151d_3.cif
_cod_data_source_block           (t-Bu3PN)(C6H3i-Pr2N)VPh2
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'tricinic' was replaced with
'triclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1777.6(12)
_cod_database_code               4314022