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_4311970
_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_moiety         '[C68 H90 O6 P2 V], 3.25 MeCN'
_chemical_formula_sum            'C74.5 H99.75 N3.25 O6 P2 V'
_chemical_formula_weight         1249.71
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.47(1)
_cell_angle_beta                 70.57(1)
_cell_angle_gamma                74.30(1)
_cell_formula_units_Z            4
_cell_length_a                   17.3782(8)
_cell_length_b                   20.5903(8)
_cell_length_c                   22.8046(10)
_cell_measurement_temperature    100(2)
_cell_volume                     7290.9(8)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '932 images at 1.0 deg. in \w and 20 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            138406
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_correction_T_min  0.9075
_exptl_absorpt_correction_type   'Gaussian, face-indexed'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             2682
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1645
_refine_ls_number_reflns         33437
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.411
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+7.0348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                25183
_reflns_number_total             33437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040052f_4.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0425P)^2^+7.0348P] 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^)+(0.0425P)^2^+7.0348P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7290.9(5)
_cod_original_formula_sum        'C74.50 H99.75 N3.25 O6 P2 V'
_cod_database_code               4311970