Synthesis and Characterization of New Oxidopolysulfidovanadates
Mehtap Emirdag-Eanes; James A. Ibers; Inorganic Chemistry 40 (2001) 6910–6912; doi:10.1021/ic010809s

data_4320788
_publ_section_title
;
 Synthesis and Characterization of New Oxidopolysulfidovanadates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6910
_journal_page_last               6912
_journal_paper_doi               10.1021/ic010809s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C2 H9.2 K6 O6.6 S19 V4'
_chemical_formula_weight         1186.39
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.127(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.047(3)
_cell_length_b                   12.5355(11)
_cell_length_c                   8.7822(8)
_cell_measurement_reflns_used    5445
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.62
_cell_volume                     3412.9(5)
_computing_cell_refinement       'SMART version 5.054 (Bruker, 2000)'
_computing_data_collection       'SMART version 5.054 (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus version 6.02A (Bruker, 2000)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       \w
_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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19942
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_T_max  0.8903
_exptl_absorpt_correction_T_min  0.7276
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+5.6382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                3050
_reflns_number_total             4217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010809s_3.cif
_cod_data_source_block           k6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C2 H9.20 K6 O6.60 S19 V4'
_cod_database_code               4320788