#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/55/2225577.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2225577
loop_
_publ_author_name
'Wang, Guo-Ming'
'Wang, Pei'
'Li, Zeng-Xin'
'Li, Hui'
'Liu, Hui-Luan'
_publ_section_title
;
 Bis(ethylenediammonium) tetradecaborate
;
_journal_coeditor_code           HY2288
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o798
_journal_page_last               o799
_journal_paper_doi               10.1107/S1600536810008494
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '2C2 H10 N2 2+, B14 H6 O26 4-'
_chemical_formula_moiety         '2(C2 H10 N2 2+), B14 H6 O26 4-'
_chemical_formula_sum            'C4 H26 B14 N4 O26'
_chemical_formula_weight         697.63
_chemical_name_systematic
;
Bis(ethylenediammonium) 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           SHELXL-97
_cell_angle_alpha                95.085(2)
_cell_angle_beta                 96.942(3)
_cell_angle_gamma                116.856(4)
_cell_formula_units_Z            1
_cell_length_a                   8.4849(3)
_cell_length_b                   8.8387(3)
_cell_length_c                   10.0406(2)
_cell_measurement_reflns_used    5101
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.07
_cell_volume                     658.08(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5101
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.9935
_exptl_absorpt_correction_T_min  0.9556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0431
_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)+(0.0518P)²+0.1264P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                2033
_reflns_number_total             2541
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2288.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        658.08(3)
_cod_database_code               2225577
_cod_database_fobs_code          2225577
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B B1 -0.5849(3) -0.5170(3) 0.8129(2) 0.0190(5) Uani d . 1 . .
B B2 -0.4605(3) -0.2456(3) 0.9547(2) 0.0180(5) Uani d . 1 . .
B B3 -0.2914(3) -0.2948(3) 0.7854(2) 0.0166(5) Uani d . 1 . .
B B4 -0.2007(3) -0.1473(3) 0.5881(2) 0.0166(5) Uani d . 1 . .
B B5 0.0303(3) -0.1771(3) 0.7443(2) 0.0175(5) Uani d . 1 . .
B B6 0.3485(3) 0.0104(3) 0.8520(2) 0.0174(5) Uani d . 1 . .
B B7 0.2775(3) -0.2278(3) 0.6835(2) 0.0189(5) Uani d . 1 . .
O O1 -0.73216(19) -0.67207(18) 0.76829(15) 0.0286(4) Uani d . 1 . .
H H1F -0.7172 -0.7203 0.7011 0.043 Uiso calc R 1 . .
O O2 -0.42739(18) -0.47558(17) 0.77218(13) 0.0203(3) Uani d . 1 . .
O O3 -0.60553(17) -0.40525(18) 0.90605(14) 0.0232(3) Uani d . 1 . .
O O4 -0.48111(18) -0.15100(18) 1.06075(14) 0.0211(3) Uani d . 1 . .
O O5 -0.31106(17) -0.18999(17) 0.90041(13) 0.0188(3) Uani d . 1 . .
O O6 -0.11436(17) -0.27927(17) 0.80925(13) 0.0175(3) Uani d . 1 . .
O O7 -0.32891(17) -0.23425(18) 0.65880(13) 0.0218(3) Uani d . 1 . .
O O8 -0.25158(18) -0.10364(18) 0.46895(14) 0.0245(4) Uani d . 1 . .
H H8A -0.1620 -0.0404 0.4401 0.037 Uiso calc R 1 . .
O O9 -0.02594(18) -0.10073(19) 0.63517(14) 0.0246(4) Uani d . 1 . .
O O10 0.10144(17) -0.28587(18) 0.68168(14) 0.0230(3) Uani d . 1 . .
O O11 0.17413(17) -0.03462(17) 0.84417(13) 0.0196(3) Uani d . 1 . .
O O12 0.40563(17) -0.08058(18) 0.76988(14) 0.0221(3) Uani d . 1 . .
O O13 0.33259(18) -0.31501(19) 0.59850(14) 0.0248(4) Uani d . 1 . .
H H13A 0.4399 -0.2832 0.6234 0.037 Uiso calc R 1 . .
C C1 0.8308(3) 0.2448(3) 0.7230(2) 0.0251(5) Uani d . 1 . .
H H1A 0.9116 0.2282 0.6699 0.030 Uiso calc R 1 . .
H H1B 0.7200 0.1376 0.7087 0.030 Uiso calc R 1 . .
C C2 0.9149(3) 0.2927(3) 0.8712(2) 0.0248(5) Uani d . 1 . .
H H2A 1.0184 0.4058 0.8868 0.030 Uiso calc R 1 . .
H H2B 0.8291 0.2977 0.9248 0.030 Uiso calc R 1 . .
N N1 0.7928(3) 0.3808(2) 0.67745(18) 0.0284(4) Uani d . 1 . .
H H1C 0.7433 0.3510 0.5897 0.043 Uiso calc R 1 . .
H H1D 0.8947 0.4789 0.6897 0.043 Uiso calc R 1 . .
H H1E 0.7173 0.3948 0.7254 0.043 Uiso calc R 1 . .
N N2 0.9717(2) 0.1666(2) 0.91544(17) 0.0236(4) Uani d . 1 . .
H H2C 1.0208 0.1977 1.0033 0.035 Uiso calc R 1 . .
H H2D 1.0518 0.1633 0.8673 0.035 Uiso calc R 1 . .
H H2E 0.8765 0.0631 0.9024 0.035 Uiso calc R 1 . .
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'
N N 0.0061 0.0033 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 B1 O1 . . 122.44(19) ?
O2 B1 O3 . . 121.71(19) ?
O1 B1 O3 . . 115.84(18) ?
O5 B2 O4 . . 123.39(19) ?
O5 B2 O3 . . 121.17(18) ?
O4 B2 O3 . . 115.44(18) ?
O6 B3 O2 . . 110.41(17) ?
O6 B3 O7 . . 112.48(16) ?
O2 B3 O7 . . 106.77(16) ?
O6 B3 O5 . . 109.26(16) ?
O2 B3 O5 . . 109.91(16) ?
O7 B3 O5 . . 107.96(16) ?
O7 B4 O9 . . 120.90(18) ?
O7 B4 O8 . . 117.95(18) ?
O9 B4 O8 . . 121.13(18) ?
O6 B5 O11 . . 110.14(16) ?
O6 B5 O9 . . 112.55(16) ?
O11 B5 O9 . . 107.35(16) ?
O6 B5 O10 . . 109.49(17) ?
O11 B5 O10 . . 109.92(16) ?
O9 B5 O10 . . 107.33(16) ?
O11 B6 O4 . 2_557 122.59(19) ?
O11 B6 O12 . . 121.46(19) ?
O4 B6 O12 2_557 . 115.93(18) ?
O10 B7 O13 . . 119.34(19) ?
O10 B7 O12 . . 121.74(19) ?
O13 B7 O12 . . 118.91(18) ?
B1 O1 H1F . . 109.5 ?
B1 O2 B3 . . 120.65(17) ?
B2 O3 B1 . . 118.42(16) ?
B2 O4 B6 . 2_557 127.25(17) ?
B2 O5 B3 . . 122.53(16) ?
B5 O6 B3 . . 125.67(16) ?
B4 O7 B3 . . 122.80(16) ?
B4 O8 H8A . . 109.5 ?
B4 O9 B5 . . 122.54(16) ?
B7 O10 B5 . . 121.89(17) ?
B6 O11 B5 . . 123.54(16) ?
B6 O12 B7 . . 118.51(17) ?
B7 O13 H13A . . 109.5 ?
N1 C1 C2 . . 110.38(17) ?
N1 C1 H1A . . 109.6 ?
C2 C1 H1A . . 109.6 ?
N1 C1 H1B . . 109.6 ?
C2 C1 H1B . . 109.6 ?
H1A C1 H1B . . 108.1 ?
N2 C2 C1 . . 111.20(17) ?
N2 C2 H2A . . 109.4 ?
C1 C2 H2A . . 109.4 ?
N2 C2 H2B . . 109.4 ?
C1 C2 H2B . . 109.4 ?
H2A C2 H2B . . 108.0 ?
C1 N1 H1C . . 109.5 ?
C1 N1 H1D . . 109.5 ?
H1C N1 H1D . . 109.5 ?
C1 N1 H1E . . 109.5 ?
H1C N1 H1E . . 109.5 ?
H1D N1 H1E . . 109.5 ?
C2 N2 H2C . . 109.5 ?
C2 N2 H2D . . 109.5 ?
H2C N2 H2D . . 109.5 ?
C2 N2 H2E . . 109.5 ?
H2C N2 H2E . . 109.5 ?
H2D N2 H2E . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
B1 O2 . 1.343(3) ?
B1 O1 . 1.360(3) ?
B1 O3 . 1.383(3) ?
B2 O5 . 1.341(3) ?
B2 O4 . 1.372(3) ?
B2 O3 . 1.381(3) ?
B3 O6 . 1.433(3) ?
B3 O2 . 1.471(3) ?
B3 O7 . 1.476(3) ?
B3 O5 . 1.489(3) ?
B4 O7 . 1.344(3) ?
B4 O9 . 1.355(3) ?
B4 O8 . 1.369(3) ?
B5 O6 . 1.430(3) ?
B5 O11 . 1.474(3) ?
B5 O9 . 1.477(3) ?
B5 O10 . 1.480(3) ?
B6 O11 . 1.337(3) ?
B6 O4 2_557 1.372(3) ?
B6 O12 . 1.376(3) ?
B7 O10 . 1.340(3) ?
B7 O13 . 1.359(3) ?
B7 O12 . 1.386(3) ?
O1 H1F . 0.8200 ?
O4 B6 2_557 1.372(3) ?
O8 H8A . 0.8200 ?
O13 H13A . 0.8200 ?
C1 N1 . 1.474(3) ?
C1 C2 . 1.503(3) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 N2 . 1.481(3) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
N1 H1C . 0.8900 ?
N1 H1D . 0.8900 ?
N1 H1E . 0.8900 ?
N2 H2C . 0.8900 ?
N2 H2D . 0.8900 ?
N2 H2E . 0.8900 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1F O8 2_446 0.82 2.11 2.909(2) 165 yes
O8 H8A O9 2_556 0.82 1.83 2.6433(19) 176 yes
O13 H13A O7 1_655 0.82 1.79 2.6030(18) 172 yes
N1 H1C O13 2_656 0.89 1.87 2.755(2) 172 yes
N1 H1D O10 1_665 0.89 2.04 2.919(2) 168 yes
N1 H1E O2 1_665 0.89 2.09 2.892(2) 150 yes
N2 H2C O6 2_657 0.89 1.89 2.777(2) 174 yes
N2 H2D O1 1_765 0.89 2.18 2.926(2) 141 yes
N2 H2E O5 1_655 0.89 2.08 2.951(2) 168 yes
