Pb4V6O16(SeO3)3(H2O), Pb2VO2(SeO3)2Cl, and PbVO2(SeO3)F: New Lead(II)-Vanadium(V) Mixed-Metal Selenites Featuring Novel Anionic Skeletons.
Cao, Xue-Li; Kong, Fang; Hu, Chun-Li; Xu, Xiang; Mao, Jiang-Gao; Inorganic chemistry 53 (2014) 8816–8824; doi:10.1021/ic501548m

data_4340645
_publ_section_title
;
 Pb4V6O16(SeO3)3(H2O), Pb2VO2(SeO3)2Cl, and PbVO2(SeO3)F: New
 Lead(II)-Vanadium(V) Mixed-Metal Selenites Featuring Novel Anionic
 Skeletons.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8816
_journal_page_last               8824
_journal_paper_doi               10.1021/ic501548m
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'H2 O26 Pb4 Se3 V6'
_chemical_formula_weight         1789.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 94.887(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.13620(10)
_cell_length_b                   21.3103(4)
_cell_length_c                   7.20040(10)
_cell_measurement_reflns_used    4972
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2319
_cell_measurement_theta_min      4.1456
_cell_volume                     1091.02(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6930
_diffrn_reflns_theta_full        74.39
_diffrn_reflns_theta_max         74.39
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    86.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31965
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       FLAKE
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.846
_refine_diff_density_min         -1.827
_refine_diff_density_rms         0.338
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.036(10)
_refine_ls_extinction_coef       0.00010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3823
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                3745
_reflns_number_total             3823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501548m_si_002.cif
_cod_data_source_block           Pb4V6Se3O25(H2O)
_cod_depositor_comments
'Adding full bibliography for 4340645--4340647.cif.'
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4340645