Macropolyhedral boron-containing cluster chemistry. The [S2B18H19]− anion, and the reversible dismantling and regeneration of an apical boron cluster site with cluster connectivity six
Jelínek, Tomáš; Cisařová, Ivana; Štíbr, Bohumil; Kennedy, John D.; Thornton-Pett, Mark; Journal of the Chemical Society, Dalton Transactions  (1998) 2965–; doi:10.1039/a805791e

data_7028051
_publ_section_title
;
 Macropolyhedral boron-containing cluster chemistry. The
 [S2B18H19]&#x2212; anion, and the reversible dismantling and regeneration
 of an apical boron cluster site with cluster connectivity six
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2965
_journal_paper_doi               10.1039/a805791e
_journal_year                    1998
_chemical_formula_sum            'C36 H49 B18 N P2 S2'
_chemical_formula_weight         816.40
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             96-06-28
_audit_creation_method           'STADI4, X-RED'
_cell_angle_alpha                70.977(6)
_cell_angle_beta                 88.202(6)
_cell_angle_gamma                80.321(6)
_cell_formula_units_Z            2
_cell_length_a                   10.9228(8)
_cell_length_b                   14.2190(12)
_cell_length_c                   15.3204(10)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      39.4
_cell_measurement_theta_min      30.1
_cell_volume                     2216.8(3)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
;
 Variable 2theta:omega scans, ratio = 1.00
 Min and max omega scan width = 1.45, 1.70
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5851
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        6.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  0.6678
_exptl_absorpt_correction_T_min  0.4427
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.28  

    H   K   L   2Theta   Chi   Imin/Imax
    0  -2  -1    12.8    87.4    0.675
    0   2   1    12.8   -87.4    0.669
    0  -4  -2    25.7    87.4    0.674
    0   4   2    25.7   -87.4    0.705
    0   7   2    45.4   -80.5    0.742
    0  -7  -2    45.4    80.5    0.630
    0   8   5    54.1   -80.9    0.772
    0  -8  -5    54.1    80.9    0.674
    1  10   4    65.8   -81.1    0.756
   -1 -10  -4    65.8    81.1    0.496
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.297
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         5851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.211
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+1.3332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                4941
_reflns_number_total             5851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            e805791sup1.cif
_cod_data_source_block           TJ2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028051
_audit_contact_author            'J. Richter'