Salts of the Bis(catecholato)borate Anion with Organic Cations
Clegg, William; Scott, Andrew J.; Lawlor, Fiona J.; Norman, Nicholas C.; Marder, Todd B.; Dai, Chaoyang; Nguyen, Paul; Acta Crystallographica Section C 54 (1998) 1875–1880; doi:10.1107/S0108270198009810

data_2007930
_publ_section_title
;
 Salts of the Bis(catecholato)borate Anion with Organic Cations
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1875
_journal_page_last               1880
_journal_paper_doi               10.1107/S0108270198009810
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C6 H8 N +, C12 H8 B O4 -'
_chemical_formula_sum            'C18 H16 B N O4'
_chemical_formula_weight         321.13
_chemical_name_systematic
;
 2-methylpyridinium bis(pyrocatecholato-O,O')borate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.187(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5204(10)
_cell_length_b                   17.061(2)
_cell_length_c                   12.2921(17)
_cell_measurement_reflns_used    3393
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.39
_cell_volume                     1576.0(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.027
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4758
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.308
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -1.4(13)
_refine_ls_extinction_coef       0.0040(7)
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2468
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0417P)^2^+1.7798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.111
_reflns_number_gt                2277
_reflns_number_total             2468
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1497.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2007930