Di-μ-dioxo-bis({1-[phenyl(2-pyridyl-κ<i>N</i>)methylene]-2-(pyrrolidin-1-ylthiocarbonyl-κ<i>S</i>)hydrazinato-κ<i>N</i>^1^}oxovanadium(V))
A. Sreekanth; Hoong-Kun Fun; Rohith P. John; M. R. Prathapachandra Kurup; Suchada Chantrapromma; Acta Crystallographica Section E 62 (2006) m1919–m1921; doi:10.1107/S1600536806026894

data_2209938
_publ_section_title
Di-\m-dioxo-bis({1-[phenyl(2-pyridyl-\k<i>N</i>)methylene]-2-(pyrrolidin-1-ylthiocarbonyl-\k<i>S</i>)hydrazinato-\k<i>N</i>^1^}oxovanadium(V))
_journal_coeditor_code           LH2125
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1919
_journal_page_last               m1921
_journal_paper_doi               10.1107/S1600536806026894
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[V2 (C17 H17 N4 S)2 O4]'
_chemical_formula_moiety         'C34 H34 N8 O4 S2 V2'
_chemical_formula_sum            'C34 H34 N8 O4 S2 V2'
_chemical_formula_weight         784.71
_chemical_name_common
;\m-dioxo-bis[Benzoyl pyridine N^4^,
 N^4^-(butane-1,4-diyl)thiosemicarbazonato-
\k^3^ N,N',S]oxovanadium(V)
;
_chemical_name_systematic
;
Di-\m-dioxo-bis({1-[phenyl(2-pyridyl-\kN)methylene]-2-(pyrrolidin-1-
ylthiocarbonyl-\kS)hydrazinato-\kN^1^}oxovanadium(V))
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.877(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3912(8)
_cell_length_b                   17.4103(14)
_cell_length_c                   11.0953(7)
_cell_measurement_reflns_used    3801
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.40
_cell_volume                     1757.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2003)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
;
Bruker SMART APEX2 CCD area-detector
;
_diffrn_measurement_method       \w
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9824
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Slab
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0428P)^2^+1.5976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                3129
_reflns_number_total             3801
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2125.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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2209938
_cod_database_fobs_code          2209938