Tetraethylammonium 12-phenylethynylcarba-<i>closo</i>-dodecaborate, [Et~4~N][12-PhCC-<i>closo</i>-CB~11~H~11~]
Finze, Maik; Reiss, Guido J.; Acta Crystallographica Section E 65 (2009) o1048–; doi:10.1107/S1600536809013300

data_2221593
_publ_section_title
;
 Tetraethylammonium 12-phenylethynylcarba-<i>closo</i>-dodecaborate,
 [Et~4~N][12-PhCC-<i>closo</i>-CB~11~H~11~]
;
_journal_coeditor_code           BR2103
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1048
_journal_paper_doi               10.1107/S1600536809013300
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C8 H20 N +, C9 H16 B11 -'
_chemical_formula_moiety         'C8 H20 N +, C9 H16 B11 -'
_chemical_formula_sum            'C17 H36 B11 N'
_chemical_formula_weight         373.38
_chemical_melting_point          433
_chemical_name_systematic
;
Tetraethylammonium 12-phenylethynylcarba-<i>closo</i>-dodecaborate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.032(7)
_cell_angle_beta                 79.899(7)
_cell_angle_gamma                71.553(7)
_cell_formula_units_Z            2
_cell_length_a                   8.8201(6)
_cell_length_b                   12.0929(11)
_cell_length_c                   12.1858(11)
_cell_measurement_reflns_used    4623
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.73
_cell_measurement_theta_min      6.80
_cell_volume                     1206.82(18)
_computing_cell_refinement       'CrysAlis RED (Kuma, 2000)'
_computing_data_collection       'CrysAlis CCD (Kuma, 2000)'
_computing_data_reduction        'CrysAlis RED (Kuma, 2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe Stadi CCD'
_diffrn_measurement_method       \w
_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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17081
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.051
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.155
_refine_ls_extinction_coef       0.037(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.01P)^2^+0.45P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                3228
_reflns_number_total             4219
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2103.cif
_cod_data_source_block           I
_cod_database_code               2221593
_cod_database_fobs_code          2221593