Nonoxovanadium(IV) and Oxovanadium(V) Complexes with Mixed O, X, O-Donor Ligands (X = S, Se, P, or PO)
Tapan K. Paine; Thomas Weyhermüller; Leonardo D. Slep; Frank Neese; Eckhard Bill; Eberhard Bothe; Karl Wieghardt; Phalguni Chaudhuri; Inorganic Chemistry 43 (2004) 7324–7338; doi:10.1021/ic040052f

data_4311967
_publ_section_title
;
 Nonoxovanadium(IV) and Oxovanadium(V) Complexes with Mixed O, X, O-Donor
 Ligands (X = S, Se, P, or PO)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7324
_journal_page_last               7338
_journal_paper_doi               10.1021/ic040052f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C56 H80 O4 S2 V'
_chemical_formula_weight         932.26
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6860(12)
_cell_length_b                   15.4480(12)
_cell_length_c                   18.1817(12)
_cell_measurement_reflns_used    11380
_cell_measurement_temperature    100(2)
_cell_volume                     5529.2(7)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa CCD-Detector'
_diffrn_measurement_method       '\w-scan,94 images a 1.0 deg/ 180sec'
_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  0.1129
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40108
_diffrn_reflns_theta_max         33.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_type   'MulScanAbs,Platon Program Suite 1999'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       'opaque needle'
_exptl_crystal_F_000             2012
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         10340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_obs          0.0506
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+1.9263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1483
_refine_ls_wR_factor_obs         0.1207
_reflns_number_observed          7406
_reflns_number_total             10392
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic040052f_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+1.9263P] 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^)+(0.0463P)^2^+1.9263P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4311967