#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/28/2212805.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_2212805
loop_
_publ_author_name
'Min Li'
'Hui Xu'
'Zhen-Ling Wang'
'Heng-Zhen Shi'
_publ_section_title
;
 A new non-metal borophosphate with a supramolecular network
;
_journal_coeditor_code           CF2088
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1696
_journal_page_last               o1698
_journal_paper_doi               10.1107/S160053680701029X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C4 H12 N2 2+, H4 B2 O16 P4 2-'
_chemical_formula_moiety         'C4 H12 N2 2+, H4 B2 O16 P4 2-'
_chemical_formula_sum            'C4 H16 B2 N2 O16 P4'
_chemical_formula_weight         493.69
_chemical_name_systematic
;
catena-poly[hemi(piperazine-1,4-diium) [boron-di-μ-hydrogenphosphato-
κ⁴O:O']]
;
_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
_cell_angle_alpha                89.510(2)
_cell_angle_beta                 84.514(2)
_cell_angle_gamma                88.697(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3433(10)
_cell_length_b                   10.1179(13)
_cell_length_c                   10.5228(14)
_cell_measurement_reflns_used    2443
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.79
_cell_volume                     778.03(18)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_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            5963
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.426
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         2876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0316
_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)+(0.0406P)²+0.712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                2424
_reflns_number_total             2876
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf2088.cif
_cod_data_source_block           I
_cod_database_code               2212805
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
P P1 0.42963(8) 0.50205(6) 0.67864(6) 0.01232(16) Uani d . 1
P P2 0.06302(8) 0.30552(6) 0.44962(6) 0.01184(16) Uani d . 1
P P3 0.56363(9) 0.81378(6) 0.97631(6) 0.01386(17) Uani d . 1
P P4 0.98552(8) 1.06796(6) 0.81318(6) 0.01277(16) Uani d . 1
B B1 0.2375(4) 0.5449(3) 0.4661(3) 0.0131(6) Uani d . 1
B B2 0.7594(4) 1.0311(3) 1.0326(3) 0.0134(6) Uani d . 1
O O1 0.4829(3) 0.64730(17) 0.69034(18) 0.0203(4) Uani d . 1
H H1 0.5279 0.6575 0.7579 0.030 Uiso calc R 1
O O2 0.3670(2) 0.43791(18) 0.80281(17) 0.0206(4) Uani d . 1
O O3 0.2685(2) 0.50034(17) 0.59469(16) 0.0174(4) Uani d . 1
O O4 0.4075(2) 0.57938(16) 0.38951(17) 0.0166(4) Uani d . 1
O O5 0.1243(2) 0.66728(17) 0.47089(16) 0.0160(4) Uani d . 1
O O6 0.1416(2) 0.44118(16) 0.40246(16) 0.0139(4) Uani d . 1
O O7 0.1839(2) 0.22481(17) 0.52817(17) 0.0176(4) Uani d . 1
O O8 0.0244(3) 0.23977(18) 0.32408(17) 0.0227(4) Uani d . 1
H H8 0.0536 0.1612 0.3263 0.034 Uiso calc R 1
O O9 0.6164(3) 0.69944(18) 0.89065(19) 0.0262(5) Uani d . 1
O O10 0.4918(3) 0.7706(2) 1.11273(19) 0.0269(5) Uani d . 1
H H10 0.5482 0.7040 1.1329 0.040 Uiso calc R 1
O O11 0.7342(2) 0.89789(17) 0.98443(18) 0.0189(4) Uani d . 1
O O12 0.8617(2) 1.02598(17) 1.14493(16) 0.0172(4) Uani d . 1
O O13 0.5861(2) 1.09856(17) 1.07686(16) 0.0156(4) Uani d . 1
O O14 0.8575(2) 1.10984(17) 0.93127(16) 0.0164(4) Uani d . 1
O O15 1.0700(3) 1.20272(18) 0.76941(17) 0.0231(4) Uani d . 1
H H15 1.1007 1.2008 0.6924 0.035 Uiso calc R 1
O O16 0.8975(2) 1.00171(18) 0.70898(17) 0.0209(4) Uani d . 1
N N1 0.9916(3) 0.5199(2) 0.8664(2) 0.0238(5) Uani d . 1
H H1A 0.9391 0.5572 0.8006 0.029 Uiso calc R 1
H H1B 1.0872 0.4695 0.8339 0.029 Uiso calc R 1
N N2 0.5450(3) 0.1303(2) 0.5369(2) 0.0291(6) Uani d . 1
H H2A 0.4471 0.1774 0.5152 0.035 Uiso calc R 1
H H2B 0.6208 0.1862 0.5705 0.035 Uiso calc R 1
C C1 0.8561(4) 0.4342(3) 0.9410(3) 0.0215(6) Uani d . 1
H H1C 0.8186 0.3648 0.8867 0.026 Uiso calc R 1
H H1D 0.7484 0.4866 0.9708 0.026 Uiso calc R 1
C C2 0.9407(4) 0.3738(3) 1.0533(3) 0.0243(6) Uani d . 1
H H2C 0.8505 0.3221 1.1041 0.029 Uiso calc R 1
H H2D 1.0417 0.3152 1.0232 0.029 Uiso calc R 1
C C3 0.6406(4) 0.0681(3) 0.4210(3) 0.0251(6) Uani d . 1
H H3A 0.7508 0.0221 0.4429 0.030 Uiso calc R 1
H H3B 0.6760 0.1359 0.3582 0.030 Uiso calc R 1
C C4 0.4840(4) 0.0283(3) 0.6347(3) 0.0279(7) Uani d . 1
H H4A 0.4195 0.0712 0.7085 0.034 Uiso calc R 1
H H4B 0.5898 -0.0188 0.6624 0.034 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'
P P 0.1023 0.0942 '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 P1 O1 . . 114.04(11) y
O2 P1 O3 . . 107.33(10) y
O1 P1 O3 . . 107.01(10) y
O2 P1 O4 . 2_666 109.78(10) ?
O1 P1 O4 . 2_666 110.05(10) ?
O3 P1 O4 . 2_666 108.42(10) ?
O7 P2 O8 . . 114.12(11) y
O7 P2 O6 . . 115.00(10) y
O8 P2 O6 . . 102.30(10) y
O7 P2 O5 . 2_566 109.16(10) ?
O8 P2 O5 . 2_566 107.85(10) ?
O6 P2 O5 . 2_566 107.95(9) ?
O9 P3 O11 . . 108.07(11) y
O9 P3 O13 . 2_677 111.37(10) ?
O11 P3 O13 . 2_677 108.33(10) ?
O9 P3 O10 . . 112.84(12) y
O11 P3 O10 . . 108.50(11) y
O13 P3 O10 2_677 . 107.62(10) ?
O16 P4 O14 . . 116.28(10) y
O16 P4 O12 . 2_777 107.93(10) ?
O14 P4 O12 . 2_777 109.42(10) ?
O16 P4 O15 . . 112.34(11) y
O14 P4 O15 . . 101.35(10) y
O12 P4 O15 2_777 . 109.28(11) ?
O3 B1 O4 . . 112.6(2) y
O3 B1 O5 . . 110.6(2) y
O4 B1 O5 . . 104.90(19) y
O3 B1 O6 . . 109.1(2) y
O4 B1 O6 . . 110.6(2) y
O5 B1 O6 . . 108.9(2) y
O12 B2 O11 . . 110.9(2) y
O12 B2 O13 . . 104.4(2) y
O11 B2 O13 . . 113.0(2) y
O12 B2 O14 . . 110.0(2) y
O11 B2 O14 . . 109.0(2) y
O13 B2 O14 . . 109.6(2) y
P1 O1 H1 . . 109.5 ?
B1 O3 P1 . . 135.78(16) ?
B1 O4 P1 . 2_666 134.29(16) ?
B1 O5 P2 . 2_566 128.08(16) ?
B1 O6 P2 . . 132.53(16) ?
P2 O8 H8 . . 109.5 ?
P3 O10 H10 . . 109.5 ?
B2 O11 P3 . . 132.70(16) ?
B2 O12 P4 . 2_777 133.11(16) ?
B2 O13 P3 . 2_677 139.54(17) ?
B2 O14 P4 . . 131.14(16) ?
P4 O15 H15 . . 109.5 ?
C1 N1 C2 . 2_767 112.1(2) ?
C1 N1 H1A . . 109.2 ?
C2 N1 H1A 2_767 . 109.2 ?
C1 N1 H1B . . 109.2 ?
C2 N1 H1B 2_767 . 109.2 ?
H1A N1 H1B . . 107.9 ?
C3 N2 C4 . . 111.2(2) ?
C3 N2 H2A . . 109.4 ?
C4 N2 H2A . . 109.4 ?
C3 N2 H2B . . 109.4 ?
C4 N2 H2B . . 109.4 ?
H2A N2 H2B . . 108.0 ?
N1 C1 C2 . . 109.8(2) ?
N1 C1 H1C . . 109.7 ?
C2 C1 H1C . . 109.7 ?
N1 C1 H1D . . 109.7 ?
C2 C1 H1D . . 109.7 ?
H1C C1 H1D . . 108.2 ?
N1 C2 C1 2_767 . 110.0(2) ?
N1 C2 H2C 2_767 . 109.7 ?
C1 C2 H2C . . 109.7 ?
N1 C2 H2D 2_767 . 109.7 ?
C1 C2 H2D . . 109.7 ?
H2C C2 H2D . . 108.2 ?
N2 C3 C4 . 2_656 109.9(2) ?
N2 C3 H3A . . 109.7 ?
C4 C3 H3A 2_656 . 109.7 ?
N2 C3 H3B . . 109.7 ?
C4 C3 H3B 2_656 . 109.7 ?
H3A C3 H3B . . 108.2 ?
N2 C4 C3 . 2_656 110.1(2) ?
N2 C4 H4A . . 109.6 ?
C3 C4 H4A 2_656 . 109.6 ?
N2 C4 H4B . . 109.6 ?
C3 C4 H4B 2_656 . 109.6 ?
H4A C4 H4B . . 108.2 ?
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
P1 O2 . 1.4914(18) y
P1 O1 . 1.5383(18) y
P1 O3 . 1.5431(18) y
P1 O4 2_666 1.5573(18) ?
P2 O7 . 1.4947(18) y
P2 O8 . 1.5374(18) y
P2 O6 . 1.5597(17) y
P2 O5 2_566 1.5603(17) ?
P3 O9 . 1.4939(19) y
P3 O11 . 1.5398(18) y
P3 O13 2_677 1.5405(17) ?
P3 O10 . 1.544(2) y
P4 O16 . 1.4955(18) y
P4 O14 . 1.5411(18) y
P4 O12 2_777 1.5475(17) ?
P4 O15 . 1.5585(19) y
B1 O3 . 1.460(3) y
B1 O4 . 1.467(3) y
B1 O5 . 1.474(3) y
B1 O6 . 1.477(3) y
B2 O12 . 1.460(3) y
B2 O11 . 1.465(3) y
B2 O13 . 1.468(3) y
B2 O14 . 1.468(3) y
O1 H1 . 0.820 ?
O4 P1 2_666 1.5572(18) ?
O5 P2 2_566 1.5603(17) ?
O8 H8 . 0.820 ?
O10 H10 . 0.820 ?
O12 P4 2_777 1.5475(17) ?
O13 P3 2_677 1.5405(17) ?
O15 H15 . 0.820 ?
N1 C1 . 1.495(3) ?
N1 C2 2_767 1.496(3) ?
N1 H1A . 0.900 ?
N1 H1B . 0.900 ?
N2 C3 . 1.486(4) ?
N2 C4 . 1.497(4) ?
N2 H2A . 0.900 ?
N2 H2B . 0.900 ?
C1 C2 . 1.506(4) ?
C1 H1C . 0.970 ?
C1 H1D . 0.970 ?
C2 N1 2_767 1.497(3) ?
C2 H2C . 0.970 ?
C2 H2D . 0.970 ?
C3 C4 2_656 1.512(4) ?
C3 H3A . 0.970 ?
C3 H3B . 0.970 ?
C4 C3 2_656 1.512(4) ?
C4 H4A . 0.970 ?
C4 H4B . 0.970 ?
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
O1 H1 O9 . 0.82 1.66 2.474(3) 173
O8 H8 O16 2_666 0.82 1.71 2.516(3) 165
O10 H10 O2 2_667 0.82 1.71 2.522(3) 169
O15 H15 O7 1_665 0.82 1.79 2.605(3) 170
N1 H1B O2 1_655 0.90 2.07 2.878(3) 149
N1 H1A O6 2_666 0.90 2.27 3.100(3) 153
N1 H1A O8 2_666 0.90 2.43 3.145(3) 136
N2 H2A O7 . 0.90 1.97 2.807(3) 154
N2 H2B O4 2_666 0.90 2.41 3.080(3) 131
N2 H2B O5 2_666 0.90 2.42 3.207(3) 146
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O4 B1 O3 P1 . . 12.7(3)
O5 B1 O3 P1 . . -104.3(2)
O6 B1 O3 P1 . . 135.9(2)
O2 P1 O3 B1 . . -179.7(2)
O1 P1 O3 B1 . . 57.5(3)
O4 P1 O3 B1 2_666 . -61.2(3)
O3 B1 O4 P1 . 2_666 74.6(3)
O5 B1 O4 P1 . 2_666 -165.11(17)
O6 B1 O4 P1 . 2_666 -47.8(3)
O3 B1 O5 P2 . 2_566 -51.5(3)
O4 B1 O5 P2 . 2_566 -173.21(15)
O6 B1 O5 P2 . 2_566 68.4(3)
O3 B1 O6 P2 . . 4.1(3)
O4 B1 O6 P2 . . 128.56(19)
O5 B1 O6 P2 . . -116.7(2)
O7 P2 O6 B1 . . -43.1(2)
O8 P2 O6 B1 . . -167.4(2)
O5 P2 O6 B1 2_566 . 79.0(2)
O12 B2 O11 P3 . . 113.9(2)
O13 B2 O11 P3 . . -2.8(3)
O14 B2 O11 P3 . . -124.9(2)
O9 P3 O11 B2 . . 166.8(2)
O13 P3 O11 B2 2_677 . 46.0(2)
O10 P3 O11 B2 . . -70.6(2)
O11 B2 O12 P4 . 2_777 32.2(3)
O13 B2 O12 P4 . 2_777 154.16(17)
O14 B2 O12 P4 . 2_777 -88.4(3)
O12 B2 O13 P3 . 2_677 151.9(2)
O11 B2 O13 P3 . 2_677 -87.5(3)
O14 B2 O13 P3 . 2_677 34.2(3)
O12 B2 O14 P4 . . 98.3(2)
O11 B2 O14 P4 . . -23.5(3)
O13 B2 O14 P4 . . -147.55(17)
O16 P4 O14 B2 . . 70.1(2)
O12 P4 O14 B2 2_777 . -52.4(2)
O15 P4 O14 B2 . . -167.8(2)
C2 N1 C1 C2 2_767 . -57.4(3)
N1 C1 C2 N1 . 2_767 56.2(3)
C4 N2 C3 C4 . 2_656 57.8(3)
C3 N2 C4 C3 . 2_656 -57.9(3)
