Synthesis, Structure, and Reactivity of closo-2,3,4,5,6,7,8,9,10,11-Decahydroxy-1,12-bis(sulfonic acid)-1,12-dicarbadodecaborane(12)
Axel Herzog; Carolyn B. Knobler; M. Frederick Hawthorne; Journal of the American Chemical Society 123 (2001) 12791–12797; doi:10.1021/ja011917g

data_4115856
_publ_contact_author
;
Hawthorne, M. F.,
Department of Chemistry and Biochemistry,
University of California,
Los Angeles, CA 90095-1569.  U. S. A.
;
_publ_contact_author_email       mfh@chem.ucla.edu
_publ_contact_author_fax         310-825-5490
_publ_contact_author_phone       310-825-7378
_publ_section_title
;
 Synthesis, Structure, and Reactivity of
 closo-2,3,4,5,6,7,8,9,10,11-Decahydroxy-1,12-bis(sulfonic
 acid)-1,12-dicarbadodecaborane(12)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12791
_journal_page_last               12797
_journal_paper_doi               10.1021/ja011917g
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         'K2 C2(SO3)2B10(OH)10 (H2O)2'
_chemical_formula_sum            'C2 H14 B10 K2 O18 S2'
_chemical_formula_weight         576.55
_chemical_name_common
;
 bispotassium salt of closo-B-1,12-decahydroxy-bis(sulfonic acid)-p-carborane
dihydrate
;
_chemical_name_systematic
; 
 K2 closo-2,3,4,5,6,7,8,9,10,11-decahydroxy-1,12-bis(sulfonic acid)-
1,12-dicarbadodecaborane(12) (H2O)2
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 126.471(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3129(18)
_cell_length_b                   10.0702(13)
_cell_length_c                   8.8975(12)
_cell_measurement_reflns_used    903
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      3.02
_cell_volume                     887.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2957
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  1.
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   'Bruker software'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.158
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0028(10)
_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   0.516
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.516
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.839
_refine_ls_shift/su_mean         0.048
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+8.2859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                1004
_reflns_number_total             1121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011917g_1.cif
_cod_data_source_block           compound19(H2O)2
_cod_database_code               4115856