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_2007934
_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         'C12 H9 N2 +,C12 H8 B O4 -,C H2 Cl2'
_chemical_formula_sum            'C25 H19 B Cl2 N2 O4'
_chemical_formula_weight         493.13
_chemical_name_systematic
'1,10-phenanthrolinium bis(pyrocatecholato-O,O')borate dichloromethane solvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                96.361(2)
_cell_angle_beta                 107.932(2)
_cell_angle_gamma                115.848(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3594(11)
_cell_length_b                   11.0153(11)
_cell_length_c                   12.0742(13)
_cell_measurement_reflns_used    3565
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      2.14
_cell_volume                     1130.4(2)
_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 0.984
_diffrn_measured_fraction_theta_max 0.938
_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  0.035
_diffrn_reflns_av_sigmaI/netI    0.041
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6167
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.457
_refine_ls_extinction_coef       0.0051(9)
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.060
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0166P)^2^+0.9928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.100
_reflns_number_gt                3501
_reflns_number_total             4331
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1497.cif
_cod_data_source_block           5
_cod_database_code               2007934