Synthesis and Structural Characterization of a New Series of Vanadoselenites, [SexV4-xO12-x](4-x)- (x = 1, 2)
H. Nakano; T. Ozeki; A. Yagasaki; Inorganic Chemistry 40 (2001) 1816–1819; doi:10.1021/ic0010508

data_4319501
_publ_section_title
;
 Synthesis and Structural Characterization of a New Series of
 Vanadoselenites, [SexV4-xO12-x](4-x)- (x = 1, 2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1816
_journal_page_last               1819
_journal_paper_doi               10.1021/ic0010508
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C48 H109 N3 O11.5 Se V3'
_chemical_formula_weight         1144.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.328(5)
_cell_length_b                   44.099(9)
_cell_length_c                   12.287(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    93(2)
_cell_volume                     12098(5)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_sigmaI/netI    0.1110
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            96250
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7199
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4904
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.999
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(6)
_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     683
_refine_ls_number_reflns         28810
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      2.951
_refine_ls_R_factor_all          0.1805
_refine_ls_R_factor_gt           0.1210
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1899P)^2^+46.6033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3239
_refine_ls_wR_factor_ref         0.3575
_reflns_number_gt                16719
_reflns_number_total             28810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0010508_1.cif
_cod_data_source_block           sev3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        12098(4)
_cod_original_formula_sum        'C48 H109 N3 O11.50 Se V3'
_cod_database_code               4319501