#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179312 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/09/4320962.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320962
loop_
_publ_author_name
'David M. Schubert'
'Mandana Z. Visi'
'Carolyn B. Knobler'
_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: [B₉O₁₂(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            'C3 H24 B9 N9 O18'
_chemical_formula_weight         571.60
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.073(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.452(7)
_cell_length_b                   9.100(4)
_cell_length_c                   15.266(7)
_cell_volume                     2276.6(17)
_computing_molecular_graphics    ORTEP
_computing_publication_material  'UCLA package and SHELX93'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1383
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2994
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.153
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_F_000             1176
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0015(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.938
_refine_ls_goodness_of_fit_obs   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2994
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.941
_refine_ls_restrained_S_obs      1.020
_refine_ls_R_factor_all          0.1940
_refine_ls_R_factor_obs          0.0659
_refine_ls_shift/esd_max         0.048
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0120P)²+13.8729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1821
_refine_ls_wR_factor_obs         0.1235
_reflns_number_observed          1257
_reflns_number_total             2994
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000217u_2.cif
_cod_data_source_block           shelx93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+13.8729P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+13.8729P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2276.7(17)
_cod_database_code               4320962
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
O1 O 0.2009(2) 0.2665(3) 0.8809(2) 0.0487(9) Uani 1 d D .
H1 H 0.1716(2) 0.3347(3) 0.8937(2) 0.073 Uiso 1 calc RD .
B1 B 0.2804(3) 0.3071(6) 0.8958(3) 0.0334(11) Uiso 1 d . .
O2 O 0.3392(2) 0.2102(3) 0.8791(2) 0.0353(7) Uani 1 d . .
B3 B 0.4268(3) 0.2524(5) 0.8872(3) 0.0305(11) Uiso 1 d . .
O4 O 0.4392(2) 0.3740(3) 0.9529(2) 0.0358(7) Uani 1 d . .
O5 O 0.3946(2) 0.6115(4) 0.9956(2) 0.0540(10) Uani 1 d D .
H5 H 0.4434(2) 0.6195(4) 1.0114(2) 0.081 Uiso 1 calc RD .
B5 B 0.3799(3) 0.4760(6) 0.9598(3) 0.0363(12) Uiso 1 d . .
O6 O 0.3000(2) 0.4462(3) 0.9288(2) 0.0397(8) Uani 1 d . .
O7 O 0.4532(2) 0.3026(3) 0.8051(2) 0.0309(7) Uani 1 d . .
B8 B 0.5000 0.2113(7) 0.7500 0.0275(14) Uiso 1 d S .
O9 O 0.5561(2) 0.1131(3) 0.8048(2) 0.0367(8) Uani 1 d . .
O10 O 0.5793(2) -0.0467(4) 0.9238(2) 0.0489(9) Uani 1 d D .
H10 H 0.5614(2) -0.0649(4) 0.9711(2) 0.073 Uiso 1 calc RD .
B10 B 0.5358(3) 0.0670(5) 0.8835(3) 0.0270(10) Uiso 1 d . .
O11 O 0.4730(2) 0.1253(3) 0.9237(2) 0.0336(7) Uani 1 d . .
C1C C 0.2579(3) 0.3450(5) 0.6510(3) 0.0401(11) Uani 1 d . .
N1C N 0.2773(2) 0.2060(4) 0.6552(3) 0.0489(11) Uani 1 d D .
H1C1 H 0.3195(2) 0.1777(4) 0.6881(3) 0.059 Uiso 1 calc RD .
H1C2 H 0.2478(2) 0.1427(4) 0.6250(3) 0.059 Uiso 1 calc RD .
N2C N 0.3028(2) 0.4419(5) 0.6972(3) 0.0531(11) Uani 1 d D .
H2C1 H 0.3450(2) 0.4137(5) 0.7301(3) 0.064 Uiso 1 calc RD .
H2C2 H 0.2900(2) 0.5335(5) 0.6944(3) 0.064 Uiso 1 calc RD .
N3C N 0.1921(3) 0.3872(5) 0.6008(3) 0.0666(14) Uani 1 d D .
H3C1 H 0.1626(3) 0.3231(5) 0.5713(3) 0.080 Uiso 1 calc RD .
H3C2 H 0.1790(3) 0.4786(5) 0.5978(3) 0.080 Uiso 1 calc RD .
C1D C 0.5000 0.3326(8) 0.2500 0.099(4) Uani 1 d SD .
N1D N 0.5102(28) 0.3980(38) 0.3274(16) 0.083(12) Uani 0.50 d PD 1
H1D1 H 0.5014 0.4961 0.3380 0.100 Uiso 0.50 d P 1
H1D2 H 0.5285 0.3534 0.3785 0.100 Uiso 0.50 d P 1
N2D N 0.4737(25) 0.4150(31) 0.1824(16) 0.060(7) Uani 0.50 d PD 2
H2D1 H 0.4708 0.3696 0.1366 0.073 Uiso 0.50 d P 2
H2D2 H 0.4649 0.4995 0.1951 0.073 Uiso 0.50 d P 2
N3D N 0.5318(8) 0.1976(9) 0.2246(9) 0.100(5) Uani 0.50 d PD 3
H3D1 H 0.5124 0.1567 0.2026 0.120 Uiso 0.50 d P 3
H3D2 H 0.5349 0.1442 0.2852 0.120 Uiso 0.50 d P 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 B1 O1 119.1(4) . .
O2 B1 O6 121.1(4) . .
O1 B1 O6 119.8(4) . .
B1 O2 B3 121.4(4) . .
O7 B3 O11 113.3(3) . .
O7 B3 O2 112.0(3) . .
O11 B3 O2 107.1(3) . .
O7 B3 O4 108.4(4) . .
O11 B3 O4 107.1(3) . .
O2 B3 O4 108.7(3) . .
B5 O4 B3 120.1(3) . .
O4 B5 O5 123.1(4) . .
O4 B5 O6 120.4(4) . .
O5 B5 O6 116.5(4) . .
B5 O6 B1 119.1(4) . .
B3 O7 B8 122.7(3) . .
O7 B8 O7 110.1(5) 6_657 .
O7 B8 O9 109.6(2) 6_657 .
O7 B8 O9 110.6(2) . .
O7 B8 O9 110.6(2) 6_657 6_657
O7 B8 O9 109.6(2) . 6_657
O9 B8 O9 106.2(5) . 6_657
B10 O9 B8 119.9(3) . .
O9 B10 O11 123.0(4) . .
O9 B10 O10 118.4(4) . .
O11 B10 O10 118.7(4) . .
B10 O11 B3 121.7(3) . .
N1C C1C N2C 120.1(4) . .
N1C C1C N3C 119.5(4) . .
N2C C1C N3C 120.4(5) . .
N2D C1D N2D 110.5(27) 6_656 .
N1D C1D N1D 126.4(35) . 6_656
N3D C1D N3D 57.8(10) 6_656 .
N3D N3D C1D 61.1(5) 6_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 B1 1.358(6) .
B1 O2 1.349(5) .
B1 O6 1.390(6) .
O2 B3 1.487(5) .
B3 O7 1.436(5) .
B3 O11 1.467(6) .
B3 O4 1.496(6) .
O4 B5 1.357(6) .
O5 B5 1.362(6) .
B5 O6 1.383(6) .
O7 B8 1.451(5) .
B8 O7 1.451(5) 6_657
B8 O9 1.488(5) .
B8 O9 1.488(5) 6_657
O9 B10 1.343(5) .
O10 B10 1.373(5) .
B10 O11 1.356(5) .
C1C N1C 1.305(6) .
C1C N2C 1.315(6) .
C1C N3C 1.326(6) .
C1D N2D 1.317(13) 6_656
C1D N2D 1.317(13) .
C1D N1D 1.320(14) .
C1D N1D 1.320(14) 6_656
C1D N3D 1.403(10) 6_656
C1D N3D 1.403(10) .
N3D N3D 1.36(2) 6_656
