Bis[(<i>m</i>-phenylenedimethylene)diammonium] tetradecaborate
Jiang, Xiao; Wu, Shu-Li; Shao, Zhi-Dong; Liang, Yun-Xiao; Acta Crystallographica Section E 64 (2008) o2129–; doi:10.1107/S1600536808033333

data_2219787
_publ_section_title
;
 Bis[(<i>m</i>-phenylenedimethylene)diammonium] tetradecaborate
;
_journal_coeditor_code           BT2801
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2129
_journal_paper_doi               10.1107/S1600536808033333
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '2C8 H14 N2 2+ , B14 H6 O26 4-'
_chemical_formula_moiety         '2C8 H14 N2 2+ , B14 H6 O26 4-'
_chemical_formula_sum            'C16 H34 B14 N4 O26'
_chemical_formula_weight         849.81
_chemical_name_systematic
;
Bis[(m-phenylenedimethylene)diammonium] tetradecaborate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                109.68(3)
_cell_angle_beta                 108.24(3)
_cell_angle_gamma                102.19(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1025(18)
_cell_length_b                   10.293(2)
_cell_length_c                   10.942(2)
_cell_measurement_reflns_used    4940
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      54.92
_cell_measurement_theta_min      6.73
_cell_volume                     857.4(5)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'Crystal Structure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6803
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.458
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0299P)^2^+1.2547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                2002
_reflns_number_total             3009
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2801.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               2219787
_cod_database_fobs_code          2219787