Synthesis and Characterization of O,N-Chelated Vanadium(IV) Oxo Phenolate Complexes: Electronic Effect of Meta and Para Substituents on the Vanadium Center
Henk Hagen; Antonio Barbon; Ernst E. van Faassen; Bert T. G. Lutz; Jaap Boersma; Anthony L. Spek; Gerard van Koten; Inorganic Chemistry 38 (1999) 4079–4086; doi:10.1021/ic9901564

data_4322235
_publ_contact_author_address
;
    Bijvoet Center for Biomolecular Research
    Department of Crystal and Structural Chemistry
    Utrecht University
    Padualaan 8
    3584 CH Utrecht
    The Netherlands
;
_publ_contact_author_email       spea@chem.uu.nl
_publ_contact_author_fax         '+31 30 2533940'
_publ_contact_author_name        '   Dr. A.L. Spek'
_publ_contact_author_phone       '+31 30 2532538'
_publ_section_title
;
 Synthesis and Characterization of O,N-Chelated Vanadium(IV) Oxo Phenolate
 Complexes: Electronic Effect of Meta and Para Substituents on the
 Vanadium Center
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4079
_journal_page_last               4086
_journal_paper_doi               10.1021/ic9901564
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C13 H22 Cl2 N2 O2 V, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C13.5 H23 Cl3 N2 O2 V'
_chemical_formula_weight         402.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 113.206(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9977(15)
_cell_length_b                   15.7445(9)
_cell_length_c                   14.4986(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    225
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     3776.0(4)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'Locally modified CAD4-Version 5 Software'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      225
_diffrn_measurement_device_type  CAD4T
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6721
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.96
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'de Meulenaer & Tompa'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    'H-atom refinement: see text '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                3369
_reflns_number_total             4329
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic9901564_2.cif
_cod_data_source_block           s1661c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

2020-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C27 H46 Cl6 N4 O4 V2'
_cod_original_formula_weight         805.26
_cod_original_formula_moiety         '2(C13 H22 Cl2 N2 O2 V), C H2 Cl2'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4322235