[<i>N</i>-(4-Chlorobenzoyl)-<i>N</i>'-(picolinylidene)hydrazinato]dioxovanadium(V)
Pal, Satyanarayan; Pal, Samudranil; Acta Crystallographica Section C 57 (2001) 141–142; doi:10.1107/S0108270100017418

data_2011749
_publ_section_title
'[<i>N</i>-(4-Chlorobenzoyl)-<i>N</i>'-(picolinylidene)hydrazinato]dioxovanadium(V)'
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              141
_journal_page_last               142
_journal_paper_doi               10.1107/S0108270100017418
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[V O2 (C13 H9 Cl N3 O1)]'
_chemical_formula_moiety         'C13 H9 Cl N3 O3 V'
_chemical_formula_sum            'C13 H9 Cl N3 O3 V'
_chemical_formula_weight         341.62
_chemical_name_systematic
'[N-(4-chlorobenzoyl)-N'-(picolinylidene)hydrazinato]dioxovanadium(V)'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.636(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   7.1139(9)
_cell_length_b                   39.501(5)
_cell_length_c                   14.7094(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      9.5
_cell_volume                     4105.7(8)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'Xtal3.4 (Hall et al., 1995)'
_computing_molecular_graphics    'ORTEX6a (McArdle, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Enraf-Nonius MACH3 four-circle'
_diffrn_measurement_method       'Profile data from \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .018
_diffrn_reflns_av_sigmaI/netI    .0880
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7956
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .932
_exptl_absorpt_correction_T_max  .990
_exptl_absorpt_correction_T_min  .884
_exptl_absorpt_correction_type   'empirical based on \y scan'
_exptl_absorpt_process_details   '(DATCOR; Reibenspies, 1989)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .36
_exptl_crystal_size_min          .32
_refine_diff_density_max         .303
_refine_diff_density_min         -.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          .144
_refine_ls_R_factor_gt           .049
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0418P)^2^+1.7700P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .126
_reflns_number_gt                3565
_reflns_number_total             7219
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1436.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0418P)^2^+1.7700P] 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^)+(0.0418P)^2^+1.7700P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2011749
_cod_database_fobs_code          2011749