Hydrothermal Synthesis of Two Cationic Bismuthate Clusters: An Alkylenedisulfonate Bridged Hexamer, [Bi6O4(OH)4(H2O)2][(CH2)2(SO3)2]3 and a Rare Nonamer Templated by Triflate, [Bi9O8(OH)6][CF3SO3]5
David L. Rogow; Honghan Fei; Daniel P. Brennan; Mariko Ikehata; Peter Y. Zavalij; Allen G. Oliver; Scott R. J. Oliver; Inorganic Chemistry 49 (2010) 5619–5624; doi:10.1021/ic1004402

data_4315777
_publ_contact_author_address     '258 PSB'
_publ_contact_author_email       soliver@chemistry.ucsc.edu
_publ_contact_author_name        'Scott Oliver'
_publ_contact_author_phone       9-5448
_publ_section_title
;
 Hydrothermal Synthesis of Two Cationic Bismuthate Clusters: An
 Alkylenedisulfonate Bridged Hexamer, [Bi6O4(OH)4(H2O)2][(CH2)2(SO3)2]3
 and a Rare Nonamer Templated by Triflate, [Bi9O8(OH)6][CF3SO3]5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5619
_journal_page_last               5624
_journal_paper_doi               10.1021/ic1004402
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C6 H12 Bi6 O28 S6'
_chemical_formula_sum            'C6 H12 Bi6 O28 S6'
_chemical_formula_weight         1978.40
_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                 114.0620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5607(14)
_cell_length_b                   9.4615(11)
_cell_length_c                   13.7266(16)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.90
_cell_volume                     1489.6(3)
_computing_cell_refinement       'SAINT v7.34'
_computing_data_collection       'Bruker APEX-II v2.1'
_computing_data_reduction        'SAINT v7.34'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       \w/2\q-scans
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16758
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    35.847
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.348
_refine_diff_density_min         -2.420
_refine_diff_density_rms         0.308
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_extinction_coef       0.00158(6)
_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   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7425
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                7214
_reflns_number_total             7425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1004402_si_002.cif
_cod_data_source_block           SLUG-9
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4315777