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_4311971
_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_structural     '[C68 H91 O7 P2 V], CH2Cl2, MeCN'
_chemical_formula_sum            'C71 H96 Cl2 N O7 P2 V'
_chemical_formula_weight         1259.27
_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
_cell_angle_alpha                83.66(2)
_cell_angle_beta                 73.39(2)
_cell_angle_gamma                65.61(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5723(9)
_cell_length_b                   15.9764(12)
_cell_length_c                   18.0224(14)
_cell_measurement_reflns_used    5549
_cell_measurement_temperature    100(2)
_cell_volume                     3661.8(8)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_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, 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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39123
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.8687
_exptl_absorpt_correction_T_min  0.7499
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick, 1994'
_exptl_crystal_colour            'deep green'
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_refine_diff_density_max         1.448
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.250
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         23670
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.250
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_obs          0.0744
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2571
_refine_ls_wR_factor_obs         0.2341
_reflns_number_observed          14987
_reflns_number_total             23692
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic040052f_5.cif
_cod_data_source_block           5
_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^)+(0.1556P)^2^+0.0000P] 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^)+(0.1556P)^2^+0.0000P] 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        3661.8(5)
_cod_database_code               4311971