Antimony Oxide Hydroxide Ethanedisulfonate: a Cationic Layered Metal Oxide for Lewis Acid Applications
Claudia H. Swanson; Harris A. Shaikh; David L. Rogow; Allen G. Oliver; Charles F. Campana; Scott R. J. Oliver; Journal of the American Chemical Society 130 (2008) 11737–11741; doi:10.1021/ja802420h

data_4108262
_publ_contact_author_address
;
Department of Chemistry and Biochemistry,
University of California, Santa Cruz,
1156 High Street,
Santa Cruz, CA 95064
USA
;
_publ_contact_author_email       soliver@chemsitry.ucsc.edu
_publ_contact_author_fax         '+1 831 459 2935'
_publ_contact_author_name        'Scott R. J. Oliver'
_publ_contact_author_phone       '+1 831 459 4676'
_publ_section_title
;
 Antimony Oxide Hydroxide Ethanedisulfonate: a Cationic Layered Metal
 Oxide for Lewis Acid Applications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11737
_journal_page_last               11741
_journal_paper_doi               10.1021/ja802420h
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '(Sb4 O6 H2),(C2 H4 O6 S2), 0.5(H2 O)'
_chemical_formula_sum            'C2 H7.5 O12.5 S2 Sb4'
_chemical_formula_weight         782.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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            4
_cell_length_a                   21.8217(9)
_cell_length_b                   7.2520(3)
_cell_length_c                   8.7815(4)
_cell_measurement_reflns_used    6869
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.96
_cell_volume                     1389.68(10)
_computing_cell_refinement       'Bruker SAINT v7.34'
_computing_data_collection       'Bruker APEX-II v2.1'
_computing_data_reduction        'Bruker 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12944
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    8.053
_exptl_absorpt_correction_T_max  0.6436
_exptl_absorpt_correction_T_min  0.3251
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Sheldrick, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.741
_exptl_crystal_description       plate
_exptl_crystal_F_000             1422
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.430
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.430
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0407
_reflns_number_gt                1605
_reflns_number_total             1731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802420h-file002.cif
_cod_data_source_block           xsc06002
_cod_original_formula_sum        'C2 H7.50 O12.50 S2 Sb4'
_cod_database_code               4108262