Synthesis and Stability of Reactive Salts of Dodecafluoro-closo-dodecaborate(2-)
Sergei V. Ivanov; Susie M. Miller; Oren P. Anderson; Konstantin A. Solntsev; Steven H. Strauss; Journal of the American Chemical Society 125 (2003) 4694–4695; doi:10.1021/ja0296374

data_4113668
_publ_section_title
;
 Synthesis and Stability of Reactive Salts of
 Dodecafluoro-closo-dodecaborate(2-)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4694
_journal_page_last               4695
_journal_paper_doi               10.1021/ja0296374
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C38 H30 B12 F12'
_chemical_formula_weight         844.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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            8
_cell_length_a                   19.102(2)
_cell_length_b                   19.102(2)
_cell_length_c                   20.535(3)
_cell_measurement_temperature    293(2)
_cell_volume                     7492.9(16)
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1502
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16408
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_F_000             3408
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.00022(14)
_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   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                835
_reflns_number_total             1358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0296374si20021211_062230.cif
_cod_data_source_block           142
_cod_original_cell_volume        7492.5(16)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4113668