Monocarbaborane anion chemistry. The substantiation of the C-arylated [PhCB6H6]‒ seven-vertex closo cluster anion by single-crystal synchrotron X-ray diffraction analysis
Franken, Andreas; Ormsby, Daniel L.; Kilner, Colin A.; Clegg, William; Thornton-Pett, Mark; Kennedy, John D.; Journal of the Chemical Society, Dalton Transactions  (2002) 2807–; doi:10.1039/b205016c

data_7011857
_publ_section_title
;
 Monocarbaborane anion chemistry. The substantiation of the C-arylated
 [PhCB6H6]-- seven-vertex closo cluster anion by single-crystal
 synchrotron X-ray diffraction analysis
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2807
_journal_paper_doi               10.1039/b205016c
_journal_year                    2002
_chemical_formula_sum            'C15 H31 B6 N'
_chemical_formula_weight         290.27
_chemical_name_systematic
; 
[NEt4]+[2-Ph-closo-2-CB6H6]-  
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   14.438(3)
_cell_length_b                   15.762(3)
_cell_length_c                   16.877(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3840.7(14)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker AXS SMART 1K CCD diffractometer'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6883
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10306
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.9845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+1.1144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1792
_refine_ls_wR_factor_ref         0.1877
_reflns_number_gt                3385
_reflns_number_total             4073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205016c.txt
_cod_data_source_block           global
_cod_original_cell_volume        3840.6(14)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7011857