Monocarbaborane chemistry. Preparation and characterisation of [4-CB8H9]‒, the ‘missing’ closo-carbaborane anion
Jelínek, Tomáš; Kilner, Colin A.; Thornton-Pett, Mark; Kennedy, John D.; Štíbr, Bohumil; Schanz, Hans-Jörg; Wrackmeyer, Bernd; Holub, Josef; Bakardjiev, Mario; Hnyk, Drahomír; Ormsby, Daniel L.; Chemical Communications  (2001) 1756–; doi:10.1039/b103408c

data_7114687
_publ_section_title
;
 Monocarbaborane chemistry. Preparation and characterisation of
 [4-CB8H9]--, the &#x2018;missing&#x2019; closo-carbaborane anion
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1756
_journal_paper_doi               10.1039/b103408c
_journal_year                    2001
_chemical_formula_sum            'C20 H27 B8 P'
_chemical_formula_weight         384.87
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 107.7840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.7338(2)
_cell_length_b                   14.1571(3)
_cell_length_c                   22.7377(4)
_cell_measurement_temperature    150(2)
_cell_volume                     4516.17(14)
_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)'
_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 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31515
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.9863
_exptl_absorpt_correction_T_min  0.9444
_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    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0033(13)
_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   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8821
_refine_ls_number_restraints     343
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0604P)^2^+2.5492P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1491
_reflns_number_gt                6775
_reflns_number_total             8821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103408c.txt
_cod_data_source_block           tom31e
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               7114687