Guanidinium and Imidazolium Borates Containing the First Examples of an Isolated Nonaborate Oxoanion: [B~9~O~12~(OH)~6~]^3^
David M. Schubert; Mandana Z. Visi; Carolyn B. Knobler; Inorganic Chemistry 39 (2000) 2250–2251; doi:10.1021/ic000217u

data_4320961
_publ_contact_author
;
Schubert, D. M.,
US Borax Inc.
26877 Tourney Road, Valencia, CA 91355-1847, USA
;
_publ_contact_author_fax         661-287-6014
_publ_contact_author_phone       661-287-6074
_publ_section_title
;
 Guanidinium and Imidazolium Borates Containing the First Examples of an
 Isolated Nonaborate Oxoanion: [B~9~O~12~(OH)~6~]^3^
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2250
_journal_page_last               2251
_journal_paper_doi               10.1021/ic000217u
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C9 H21 B9 N6 O18'
_chemical_formula_weight         598.61
_chemical_name_common
;
imidazolium nonaborate
;
_chemical_name_systematic
;
[C~3~H~5~N~2~]~3~ [B~9~O~12~(OH)~6~
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.170(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.622(3)
_cell_length_b                   9.3324(15)
_cell_length_c                   15.570(3)
_cell_measurement_temperature    373(2)
_cell_volume                     2414.8(7)
_computing_cell_refinement       'Bruker SMART 1000'
_computing_data_collection       'Bruker SMART 1000'
_computing_data_reduction        'Bruker SMART 1000'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'Bruker SMART 1000 and UCLA programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.1032
_diffrn_reflns_av_sigmaI/netI    0.1445
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15207
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.146
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00230(19)
_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   0.819
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0124P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                2863
_reflns_number_total             5756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000217u_1.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      'P 1 21/a 1'
_cod_database_code               4320961