Unprecedented [V2O]6+ core of a centrosymmetric thiosemicarbazonato dimer: spontaneous deoxygenation of oxovanadium(IV).
Shongwe, Musa S.; Al-Kharousi, Huda N R; Adams, Harry; Morris, Michael J.; Bill, Eckhard; Inorganic chemistry 45 (2006) 1103–1107; doi:10.1021/ic0511625

data_4340183
_publ_section_title
;
 Unprecedented [V2O]6+ core of a centrosymmetric thiosemicarbazonato
 dimer: spontaneous deoxygenation of oxovanadium(IV).
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1103
_journal_page_last               1107
_journal_paper_doi               10.1021/ic0511625
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C24 H34 Cl2 N14 O11 S4 V2'
_chemical_formula_weight         995.67
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.008(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.286(3)
_cell_length_b                   9.478(3)
_cell_length_c                   21.541(6)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    150(2)
_cell_volume                     1885.5(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0963
_diffrn_reflns_av_sigmaI/netI    0.1271
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11759
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_correction_T_min  0.7541
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.603
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4499
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0738
_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^)+(0.1021P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                2570
_reflns_number_total             4499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0511625si20051109_051029.cif
_cod_data_source_block           ims38m_[{V(daptsc)(MeOH)}2(&#x00B5;-O)](ClO4)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1885.5(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4340183