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_4311972
_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_analytical     '[C56 H82 O8 Se2 V2], 4 CH3CN'
_chemical_formula_sum            'C64 H94 N4 O8 Se2 V2'
_chemical_formula_weight         1307.23
_chemical_name_systematic
; 
  ? 
;
_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'
_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                 95.310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.625(2)
_cell_length_b                   9.6819(9)
_cell_length_c                   20.108(2)
_cell_measurement_reflns_used    3765
_cell_measurement_temperature    100(2)
_cell_volume                     3416.6(6)
_computing_cell_refinement       'Siemens SAINT 5'
_computing_data_collection       'Siemens SAINT 5'
_computing_data_reduction        'Siemens SAINT 5'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w-scan,0.3 deg./frame'
_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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25476
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   'SADABS, G.M.Sheldrick 1994'
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       opaque
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_obs          0.0496
_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^)+(0.0621P)^2^+1.7864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1287
_refine_ls_wR_factor_obs         0.1120
_reflns_number_observed          3941
_reflns_number_total             5953
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic040052f_6.cif
_cod_data_source_block           6
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+1.7864P] 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^)+(0.0621P)^2^+1.7864P] 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               4311972