Polyhedral monocarbaborane chemistry. Carboxylic acid derivatives of the [closo-2-CB9H10]- anion.
Franken, Andreas; Kilner, Colin A; Kennedy, John D; Chemical communications (Cambridge, England)  (2004) 328–329; doi:10.1039/b311853n

data_7102447
_publ_section_title
;
 Polyhedral monocarbaborane chemistry. Carboxylic acid derivatives of
 the [closo-2-CB9H10]- anion.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              328
_journal_page_last               329
_journal_paper_doi               10.1039/b311853n
_journal_year                    2004
_chemical_formula_moiety
;
3(C8H20N)+, 2(C8H14B9O2)-, Br-
;
_chemical_formula_sum            'C40 H88 B18 Br N3 O4'
_chemical_formula_weight         949.62
_chemical_name_common
'(NEt4)+(2-(HOOC-C6H4)-closo-2-CB9H9)- * (NEt4)+Br-'
_chemical_name_systematic
;
?
;
_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                 103.3860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.2400(4)
_cell_length_b                   20.6240(4)
_cell_length_c                   11.8850(2)
_cell_measurement_reflns_used    51672
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     5541.74(17)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 1997)
XSeed (Barbour, 2001)
;
_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 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_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  0.1082
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            54783
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.9330
_exptl_absorpt_correction_T_min  0.7994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.195
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6354
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0709P)^2^+13.7191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                4834
_reflns_number_total             6354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311853n.txt
_cod_data_source_block           c:AFXV93A
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7102447