#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/19/8101959.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_8101959
loop_
_publ_author_name
'Zhang, W.-J.'
'Liu, Z.-H.'
_publ_section_title
;
Crystal structure of pyridinium tetrahydroxyhexaoxopentaborate pyridine 
hemisolvate, (C₅H₆N)[B₅O₆(OH)₄] · ½C₅H₅N
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              189
_journal_page_last               190
_journal_volume                  221
_journal_year                    2006
_chemical_formula_moiety         'C5H6N, B5H4O10, 0.5C5H5N'
_chemical_formula_sum            'C7.5 H12.5 B5 N1.5 O10'
_chemical_formula_weight         337.74
_chemical_name_common            'pyridine pentaborate pyridine hemisolvate'
_chemical_name_systematic
; 
pyridinium tetrahydroxyhexaoxopentaborate pyridine hemisolvate
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.478(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.485(10)
_cell_length_b                   11.554(7)
_cell_length_c                   17.811(11)
_cell_measurement_reflns_used    1188
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.781
_cell_measurement_theta_min      2.317
_cell_volume                     2985(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7589
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.9514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0550
_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/[σ²(Fo²)+(0.0701P)²+3.8237P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1785
_reflns_number_gt                1189
_reflns_number_total             2633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1763.cff
_cod_data_source_block           C7.5H12.5B5N1.5O10WJZ
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      C12/c1
_cod_database_code               8101959
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.7814(3) 0.3862(4) 0.6981(3) 0.0373(11) Uani 1 8 f d . . .
B2 B 0.7596(3) 0.4875(4) 0.8137(3) 0.0403(12) Uani 1 8 f d . . .
B3 B 0.7483(3) 0.2834(4) 0.8079(3) 0.0424(12) Uani 1 8 f d . . .
B4 B 0.9059(3) 0.3932(5) 0.6399(3) 0.0443(12) Uani 1 8 f d . . .
B5 B 0.7495(3) 0.3967(4) 0.5527(3) 0.0423(12) Uani 1 8 f d . . .
N1 N 0.4667(4) 0.7812(6) 0.4824(3) 0.1063(18) Uani 1 8 f d DU . .
H1 H 0.4157 0.8062 0.4856 0.128 Uiso 1 8 f calc R . .
N2 N 0.5000 0.3781(9) 0.7500 0.147(3) Uani 1 4 e d SDU . .
O1 O 0.76950(19) 0.4905(2) 0.74095(15) 0.0409(7) Uani 1 8 f d . . .
O2 O 0.7522(2) 0.3848(2) 0.84937(15) 0.0488(8) Uani 1 8 f d . . .
O3 O 0.76067(19) 0.2822(2) 0.73597(15) 0.0409(7) Uani 1 8 f d . . .
O4 O 0.87915(17) 0.3822(2) 0.70363(14) 0.0406(7) Uani 1 8 f d . . .
O5 O 0.84223(19) 0.4003(3) 0.56332(16) 0.0551(9) Uani 1 8 f d . . .
O6 O 0.72016(17) 0.3916(2) 0.61515(14) 0.0408(7) Uani 1 8 f d . . .
O7 O 0.7558(2) 0.5860(2) 0.85386(16) 0.0546(9) Uani 1 8 f d . . .
H7 H 0.7603 0.6423 0.8274 0.082 Uiso 1 8 f calc R . .
O8 O 0.7298(2) 0.1859(3) 0.84099(17) 0.0613(10) Uani 1 8 f d . . .
H8 H 0.7278 0.1308 0.8114 0.092 Uiso 1 8 f calc R . .
O9 O 0.9955(2) 0.3973(3) 0.64539(17) 0.0698(11) Uani 1 8 f d . . .
H9 H 1.0288 0.3929 0.6926 0.105 Uiso 1 8 f calc R . .
O10 O 0.68594(19) 0.4007(3) 0.47719(15) 0.0543(9) Uani 1 8 f d . . .
H10 H 0.7124 0.4034 0.4446 0.081 Uiso 1 8 f calc R . .
C1 C 0.5025(5) 0.6827(6) 0.5185(4) 0.0807(17) Uani 1 8 f d DU . .
H1A H 0.4734 0.6426 0.5482 0.097 Uiso 1 8 f calc R . .
C2 C 0.5780(5) 0.6421(5) 0.5123(4) 0.0885(18) Uani 1 8 f d DU . .
H2 H 0.6024 0.5731 0.5379 0.106 Uiso 1 8 f calc R . .
C3 C 0.6218(4) 0.6985(6) 0.4692(4) 0.0874(18) Uani 1 8 f d DU . .
H3 H 0.6747 0.6675 0.4639 0.105 Uiso 1 8 f calc R . .
C4 C 0.5878(5) 0.7997(6) 0.4345(4) 0.0894(18) Uani 1 8 f d DU . .
H4 H 0.6182 0.8404 0.4061 0.107 Uiso 1 8 f calc R . .
C5 C 0.5090(5) 0.8428(6) 0.4407(4) 0.0960(19) Uani 1 8 f d DU . .
H5 H 0.4848 0.9129 0.4169 0.115 Uiso 1 8 f calc R . .
C6 C 0.5337(5) 0.4406(7) 0.7000(5) 0.109(2) Uani 1 8 f d DU . .
H6 H 0.5596 0.4006 0.6678 0.131 Uiso 1 8 f calc R . .
C7 C 0.5305(5) 0.5512(8) 0.6961(6) 0.135(3) Uani 1 8 f d DU . .
H7A H 0.5480 0.5924 0.6589 0.162 Uiso 1 8 f calc R . .
C8 C 0.5000 0.6043(12) 0.7500 0.163(4) Uani 1 4 e d SDU . .
H8A H 0.5000 0.6848 0.7500 0.195 Uiso 1 4 e calc SR . .
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
_geom_angle_publ_flag
O6 B1 O3 109.4(3) . . ?
O6 B1 O1 109.7(3) . . ?
O3 B1 O1 110.2(3) . . ?
O6 B1 O4 110.9(3) . . ?
O3 B1 O4 109.1(3) . . ?
O1 B1 O4 107.5(3) . . ?
O1 B2 O7 121.5(4) . . ?
O1 B2 O2 121.4(4) . . ?
O7 B2 O2 117.1(4) . . ?
O8 B3 O3 121.7(4) . . ?
O8 B3 O2 116.9(4) . . ?
O3 B3 O2 121.3(4) . . ?
O4 B4 O9 123.5(4) . . ?
O4 B4 O5 121.1(4) . . ?
O9 B4 O5 115.5(4) . . ?
O6 B5 O10 118.9(4) . . ?
O6 B5 O5 121.6(4) . . ?
O10 B5 O5 119.5(4) . . ?
C1 N1 C5 121.0(6) . . ?
C1 N1 H1 119.5 . . ?
C5 N1 H1 119.5 . . ?
C6 N2 C6 117.1(10) . 2_656 ?
B2 O1 B1 123.4(3) . . ?
B2 O2 B3 118.9(3) . . ?
B3 O3 B1 123.4(3) . . ?
B4 O4 B1 123.4(3) . . ?
B4 O5 B5 119.0(3) . . ?
B5 O6 B1 123.8(3) . . ?
B2 O7 H7 109.5 . . ?
B3 O8 H8 109.5 . . ?
B4 O9 H9 109.5 . . ?
B5 O10 H10 109.5 . . ?
C2 C1 N1 120.2(6) . . ?
C2 C1 H1A 119.9 . . ?
N1 C1 H1A 119.9 . . ?
C1 C2 C3 121.2(6) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C4 C3 C2 119.2(6) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 120.0(6) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 118.3(6) . . ?
N1 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C7 C6 N2 122.7(9) . . ?
C7 C6 H6 118.7 . . ?
N2 C6 H6 118.7 . . ?
C6 C7 C8 115.4(10) . . ?
C6 C7 H7A 122.3 . . ?
C8 C7 H7A 122.3 . . ?
C7 C8 C7 126.2(13) . 2_656 ?
C7 C8 H8A 116.9 . . ?
C7 C8 H8A 116.9 2_656 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 O6 1.452(5) . ?
B1 O3 1.467(5) . ?
B1 O1 1.471(5) . ?
B1 O4 1.483(5) . ?
B2 O1 1.356(5) . ?
B2 O7 1.357(5) . ?
B2 O2 1.370(5) . ?
B3 O8 1.347(5) . ?
B3 O3 1.360(5) . ?
B3 O2 1.376(5) . ?
B4 O4 1.345(5) . ?
B4 O9 1.356(5) . ?
B4 O5 1.377(5) . ?
B5 O6 1.342(5) . ?
B5 O10 1.361(5) . ?
B5 O5 1.382(5) . ?
N1 C1 1.330(7) . ?
N1 C5 1.352(7) . ?
N1 H1 0.8600 . ?
N2 C6 1.383(8) . ?
N2 C6 1.383(8) 2_656 ?
O7 H7 0.8200 . ?
O8 H8 0.8200 . ?
O9 H9 0.8200 . ?
O10 H10 0.8200 . ?
C1 C2 1.299(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.355(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.341(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.357(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.280(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.356(9) . ?
C7 H7A 0.9300 . ?
C8 C7 1.356(9) 2_656 ?
C8 H8A 0.9300 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O5 0.86 2.35 3.103(6) 147.2 3_455
O7 H7 O3 0.82 1.93 2.734(4) 165.5 4_656
O8 H8 O1 0.82 1.88 2.691(4) 170.6 4_646
O9 H9 O4 0.82 1.90 2.716(4) 171.6 2_756
O10 H10 O7 0.82 1.96 2.772(4) 170.8 6_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 B2 O1 B1 174.9(4) . . . . ?
O2 B2 O1 B1 -5.7(6) . . . . ?
O6 B1 O1 B2 133.0(4) . . . . ?
O3 B1 O1 B2 12.5(5) . . . . ?
O4 B1 O1 B2 -106.3(4) . . . . ?
O1 B2 O2 B3 -4.6(6) . . . . ?
O7 B2 O2 B3 174.8(4) . . . . ?
O8 B3 O2 B2 -172.2(4) . . . . ?
O3 B3 O2 B2 6.6(6) . . . . ?
O8 B3 O3 B1 -179.6(4) . . . . ?
O2 B3 O3 B1 1.7(6) . . . . ?
O6 B1 O3 B3 -131.1(4) . . . . ?
O1 B1 O3 B3 -10.5(5) . . . . ?
O4 B1 O3 B3 107.4(4) . . . . ?
O9 B4 O4 B1 175.4(4) . . . . ?
O5 B4 O4 B1 -5.0(7) . . . . ?
O6 B1 O4 B4 5.7(6) . . . . ?
O3 B1 O4 B4 126.3(4) . . . . ?
O1 B1 O4 B4 -114.2(4) . . . . ?
O4 B4 O5 B5 0.4(7) . . . . ?
O9 B4 O5 B5 180.0(4) . . . . ?
O6 B5 O5 B4 3.0(7) . . . . ?
O10 B5 O5 B4 -178.4(4) . . . . ?
O10 B5 O6 B1 179.6(4) . . . . ?
O5 B5 O6 B1 -1.8(7) . . . . ?
O3 B1 O6 B5 -122.7(4) . . . . ?
O1 B1 O6 B5 116.3(4) . . . . ?
O4 B1 O6 B5 -2.3(6) . . . . ?
C5 N1 C1 C2 -2.0(10) . . . . ?
N1 C1 C2 C3 -0.1(10) . . . . ?
C1 C2 C3 C4 2.0(10) . . . . ?
C2 C3 C4 C5 -1.9(10) . . . . ?
C1 N1 C5 C4 2.0(9) . . . . ?
C3 C4 C5 N1 -0.1(10) . . . . ?
C6 N2 C6 C7 -3.3(6) 2_656 . . . ?
N2 C6 C7 C8 6.1(11) . . . . ?
C6 C7 C8 C7 -3.0(6) . . . 2_656 ?
