Synthesis, Structural Characterization, and MO Calculations of Vanadium Imido Complexes Containing Bidentate Phosphine Coligands
Francisco Montilla; Angeles Monge; Enrique Gutiérrez-Puebla; Antonio Pastor; Diego del Río; Norge Cruz Hernández; Javier Fernández Sanz; Agustín Galindo; Inorganic Chemistry 38 (1999) 4462–4466; doi:10.1021/ic9900152

data_4322251
_publ_contact_author
;
        Agust\'in Galindo
        Departamento de Qu\'imica Inorg\'anica
        Universidad de Sevilla
        Aptdo. 553
    41071 SEVILLA
        Spain
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_publ_contact_author_email       galindo@cica.es
_publ_contact_author_fax         '34 1 95 4557156'
_publ_contact_author_phone       '34 1 95 455-7165'
_publ_section_title
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 Synthesis, Structural Characterization, and MO Calculations of Vanadium
 Imido Complexes Containing Bidentate Phosphine Coligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4462
_journal_page_last               4466
_journal_paper_doi               10.1021/ic9900152
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C22 H41 Cl3 N P2 V'
_chemical_formula_weight         538.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.954(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7387(14)
_cell_length_b                   10.6738(10)
_cell_length_c                   16.999(3)
_cell_measurement_temperature    153(2)
_cell_volume                     2673.9(6)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SAINT (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL 5.0 (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'SMART Siemens'
_diffrn_measurement_method       'omega scans'
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.1123
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5692
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0.05%
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.983
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_obs          0.0544
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1175
_refine_ls_wR_factor_obs         0.1046
_reflns_number_observed          2308
_reflns_number_total             3304
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9900152.cif
_cod_data_source_block           PMR8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2673.8(6)
_cod_original_formula_sum        'C22 H41 Cl3 N1 P2 V1'
_cod_database_code               4322251