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_4315778
_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         'Bi9 O14, 5(C F3 O3 S)'
_chemical_formula_sum            'C5 Bi9 F15 O29 S5'
_chemical_formula_weight         2850.17
_chemical_name_common            'trifluoromethylsolfonate bismuth oxide'
_chemical_name_systematic
;
pentakis-trifluoromethylsolfonate nonabismuth tetradecaoxide
;
_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   undef
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 99.665(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.463(6)
_cell_length_b                   10.114(4)
_cell_length_c                   23.924(9)
_cell_measurement_reflns_used    4811
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.3
_cell_volume                     4166(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia,1997), ATOMS (Dowty,1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker SmartApex'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      NFRAMES=606,606,606,50,1206,50
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0504448
_diffrn_orient_matrix_UB_12      0.0464910
_diffrn_orient_matrix_UB_13      -0.0004523
_diffrn_orient_matrix_UB_21      0.0136726
_diffrn_orient_matrix_UB_22      -0.0106860
_diffrn_orient_matrix_UB_23      0.0420443
_diffrn_orient_matrix_UB_31      0.0253517
_diffrn_orient_matrix_UB_32      -0.0866021
_diffrn_orient_matrix_UB_33      -0.0054649
_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  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23984
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.37
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.15
_exptl_absorpt_coefficient_mu    38.279
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP (Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4896
_exptl_crystal_id                'Dan/Scott B2O3+F3CSO3H+NH4OH Crystal#3'
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.335
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5161
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0115P)^2^], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                3573
_reflns_number_total             5161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1004402_si_003.cif
_cod_data_source_block           SLUG-16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4315778
_diffrn_measurement_total_frames-ccd 3124
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    5.156
_diffrn_measurement_frame_time-ccd 10
_diffrn_measurement_total_time-ccd 11.72
_diffrn_measurement_frame_size-ccd 512