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_4115859
_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         'Na2 C2 (SO3)2 B10 (OH)10 (H2O)4'
_chemical_formula_sum            'C2 H18 B10 Na2 O20 S2'
_chemical_formula_weight         580.36
_chemical_name_common
;
bissodium salt of closo-B-decahydroxy-1,12-bis(sulfonic acid)-p-carborane
;
_chemical_name_systematic
; 
 bissodium salt of 
closo-2,3,4,5,6,7,8,9,10,11-decahydroxy-1,12-bis-(sulfonic acid)-
1,12-dicarbadodecaborane(12) 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.579(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.282(5)
_cell_length_b                   7.343(2)
_cell_length_c                   16.735(5)
_cell_measurement_reflns_used    968
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      23.088
_cell_measurement_theta_min      2.50
_cell_volume                     1952.8(10)
_computing_cell_refinement       'Bruker software'
_computing_data_collection       'Bruker software'
_computing_data_reduction        'Bruker software'
_computing_molecular_graphics    'Bruker software'
_computing_publication_material  'Bruker software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker Smart ccd'
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6209
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details
;
SADABS is supplied with the Bruker SMART software
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_description       needle
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0000(3)
_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   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2335
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.281
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                1646
_reflns_number_total             2335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011917g_4.cif
_cod_data_source_block           compound18.(H2O)4
_cod_original_cell_volume        1952.9(10)
_cod_database_code               4115859