#------------------------------------------------------------------------------
#$Date: 2019-10-28 09:23:29 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219800 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/22/72/2227285.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_2227285
loop_
_publ_author_name
'Hemissi, Hanène'
'Rzaigui, Mohammed'
'Al-Deyab, Salem S.'
_publ_section_title
;
 Bis(homopiperazine-1,4-diium) cyclotetraphosphate--telluric acid (1/2)
;
_journal_coeditor_code           BV2159
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2712
_journal_paper_doi               10.1107/S1600536810038225
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '2C5 H14 N2 2+, P4 O12 4-, 2Te (O H)6'
_chemical_formula_moiety         '2(C5 H14 N2 2+), O12 P4 4-, 2(H6 O6 Te)'
_chemical_formula_sum            'C10 H40 N4 O24 P4 Te2'
_chemical_formula_weight         979.54
_chemical_name_systematic
;
Bis(piperazine-1,4-diium) cyclotetraphosphate--telluric acid (1/2)
;
_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                 101.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.826(3)
_cell_length_b                   8.3600(13)
_cell_length_c                   17.030(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.86
_cell_measurement_theta_min      9.01
_cell_volume                     2903.9(15)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1996)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'Non-profiled ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            8219
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.986
_refine_diff_density_min         -1.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         6346
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0482P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                4847
_reflns_number_total             6346
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bv2159.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         489.77
_cod_original_formula_moiety         'C5 H14 N2 2+, 0.5(O12 P4 4-), H6 O6 Te'
_cod_original_formula_iupac          'C5 H14 N2 2+, 0.5P4 O12 4-, Te (O H)6'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        2903.9(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C5 H20 N2 O12 P2 Te '
_cod_database_code               2227285
_cod_database_fobs_code          2227285
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_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
C C5 0.17222(12) 0.3358(3) 0.92873(16) 0.0227(5) Uani d . 1 . .
H H5A 0.1782 0.2247 0.9450 0.027 Uiso calc R 1 . .
H H5B 0.1909 0.4014 0.9747 0.027 Uiso calc R 1 . .
C C4 0.20920(13) 0.3672(3) 0.86247(18) 0.0253(5) Uani d . 1 . .
H H4A 0.1880 0.4538 0.8291 0.030 Uiso calc R 1 . .
H H4B 0.2535 0.4010 0.8860 0.030 Uiso calc R 1 . .
H H3 -0.0202(13) 0.058(5) 0.080(2) 0.060(14) Uiso d D 1 . .
H H4 -0.0415(18) 0.298(4) 0.1851(19) 0.039(11) Uiso d D 1 . .
H H1 0.1244(7) 0.217(4) 0.2504(13) 0.027(9) Uiso d D 1 . .
H H6 0.0994(18) 0.505(3) 0.1086(14) 0.053(13) Uiso d D 1 . .
H H2 -0.0171(9) 0.333(4) 0.0087(11) 0.024(8) Uiso d D 1 . .
H H5 0.1230(13) 0.094(3) 0.068(2) 0.047(12) Uiso d D 1 . .
Te Te1 0.053963(7) 0.257312(16) 0.128185(8) 0.01399(4) Uani d D 1 . .
P P1 0.35495(3) 0.28147(6) 0.49522(3) 0.01199(9) Uani d . 1 . .
P P2 0.26836(3) 0.30733(7) 0.61119(3) 0.01214(9) Uani d . 1 . .
O O10 0.32281(8) 0.22730(19) 0.56907(10) 0.0161(3) Uani d . 1 . .
O O7 0.29316(8) 0.3056(2) 0.42301(10) 0.0167(3) Uani d . 1 . .
O O9 0.39402(8) 0.1419(2) 0.47840(11) 0.0199(3) Uani d . 1 . .
O O1 0.08267(8) 0.2069(2) 0.23924(11) 0.0200(3) Uani d D 1 . .
O O11 0.25530(8) 0.4740(2) 0.58395(11) 0.0197(3) Uani d . 1 . .
N N2 0.21224(11) 0.2239(2) 0.81152(15) 0.0223(4) Uani d . 1 . .
H H2A 0.2422 0.2419 0.7812 0.027 Uiso calc R 1 . .
H H2B 0.2264 0.1404 0.8438 0.027 Uiso calc R 1 . .
O O4 -0.02504(9) 0.3469(2) 0.15028(12) 0.0239(4) Uani d D 1 . .
O O6 0.09666(11) 0.4585(2) 0.15090(12) 0.0273(4) Uani d D 1 . .
O O8 0.38702(8) 0.4392(2) 0.51103(11) 0.0197(3) Uani d . 1 . .
O O12 0.28855(8) 0.2710(2) 0.69789(10) 0.0217(3) Uani d . 1 . .
O O2 0.02429(9) 0.3119(3) 0.01751(11) 0.0229(4) Uani d D 1 . .
O O5 0.13208(8) 0.1739(3) 0.10185(12) 0.0254(4) Uani d D 1 . .
C C3 0.14949(14) 0.1782(3) 0.75778(16) 0.0268(5) Uani d . 1 . .
H H3A 0.1564 0.0813 0.7292 0.032 Uiso calc R 1 . .
H H3B 0.1368 0.2621 0.7183 0.032 Uiso calc R 1 . .
N N1 0.10076(10) 0.3697(3) 0.90552(13) 0.0211(4) Uani d . 1 . .
H H1A 0.0817 0.3340 0.9451 0.025 Uiso calc R 1 . .
H H1B 0.0955 0.4765 0.9031 0.025 Uiso calc R 1 . .
C C2 0.09384(13) 0.1504(3) 0.80154(17) 0.0245(5) Uani d . 1 . .
H H2C 0.0595 0.0911 0.7665 0.029 Uiso calc R 1 . .
H H2D 0.1099 0.0841 0.8481 0.029 Uiso calc R 1 . .
O O3 0.01479(9) 0.0496(2) 0.11451(13) 0.0253(4) Uani d D 1 . .
C C1 0.06439(13) 0.3009(4) 0.82876(18) 0.0289(5) Uani d . 1 . .
H H1C 0.0619 0.3812 0.7871 0.035 Uiso calc R 1 . .
H H1D 0.0199 0.2775 0.8344 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 0.0015 0.0009 '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'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.9710 1.0960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 5 3
-1 -5 3
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
N1 C5 C4 . . 113.7(2) ?
N1 C5 H5A . . 108.8 ?
C4 C5 H5A . . 108.8 ?
N1 C5 H5B . . 108.8 ?
C4 C5 H5B . . 108.8 ?
H5A C5 H5B . . 107.7 ?
N2 C4 C5 . . 112.5(2) ?
N2 C4 H4A . . 109.1 ?
C5 C4 H4A . . 109.1 ?
N2 C4 H4B . . 109.1 ?
C5 C4 H4B . . 109.1 ?
H4A C4 H4B . . 107.8 ?
O5 Te1 O6 . . 89.15(9) ?
O5 Te1 O1 . . 92.34(9) ?
O6 Te1 O1 . . 87.36(8) ?
O5 Te1 O3 . . 90.15(9) ?
O6 Te1 O3 . . 175.03(9) ?
O1 Te1 O3 . . 87.75(9) ?
O5 Te1 O4 . . 177.38(9) ?
O6 Te1 O4 . . 89.95(9) ?
O1 Te1 O4 . . 90.08(8) ?
O3 Te1 O4 . . 90.96(8) ?
O5 Te1 O2 . . 88.67(9) ?
O6 Te1 O2 . . 91.96(9) ?
O1 Te1 O2 . . 178.78(8) ?
O3 Te1 O2 . . 92.94(9) ?
O4 Te1 O2 . . 88.91(8) ?
O8 P1 O9 . . 119.45(10) ?
O8 P1 O7 . . 106.91(10) ?
O9 P1 O7 . . 109.72(10) ?
O8 P1 O10 . . 110.71(10) ?
O9 P1 O10 . . 105.15(10) ?
O7 P1 O10 . . 103.86(9) ?
O11 P2 O12 . . 120.22(11) ?
O11 P2 O7 . 7_556 111.00(9) ?
O12 P2 O7 . 7_556 106.65(10) ?
O11 P2 O10 . . 110.78(10) ?
O12 P2 O10 . . 106.01(10) ?
O7 P2 O10 7_556 . 100.20(9) ?
P1 O10 P2 . . 132.59(11) ?
P1 O7 P2 . 7_556 131.58(11) ?
Te1 O1 H1 . . 107.4(15) ?
C3 N2 C4 . . 115.5(2) ?
C3 N2 H2A . . 108.4 ?
C4 N2 H2A . . 108.4 ?
C3 N2 H2B . . 108.4 ?
C4 N2 H2B . . 108.4 ?
H2A N2 H2B . . 107.5 ?
Te1 O4 H4 . . 116(3) ?
Te1 O6 H6 . . 110.3(17) ?
Te1 O2 H2 . . 109.4(13) ?
Te1 O5 H5 . . 110.6(16) ?
N2 C3 C2 . . 113.6(2) ?
N2 C3 H3A . . 108.8 ?
C2 C3 H3A . . 108.8 ?
N2 C3 H3B . . 108.8 ?
C2 C3 H3B . . 108.8 ?
H3A C3 H3B . . 107.7 ?
C1 N1 C5 . . 117.7(2) ?
C1 N1 H1A . . 107.9 ?
C5 N1 H1A . . 107.9 ?
C1 N1 H1B . . 107.9 ?
C5 N1 H1B . . 107.9 ?
H1A N1 H1B . . 107.2 ?
C1 C2 C3 . . 114.8(2) ?
C1 C2 H2C . . 108.6 ?
C3 C2 H2C . . 108.6 ?
C1 C2 H2D . . 108.6 ?
C3 C2 H2D . . 108.6 ?
H2C C2 H2D . . 107.5 ?
Te1 O3 H3 . . 107(3) ?
N1 C1 C2 . . 115.1(2) ?
N1 C1 H1C . . 108.5 ?
C2 C1 H1C . . 108.5 ?
N1 C1 H1D . . 108.5 ?
C2 C1 H1D . . 108.5 ?
H1C C1 H1D . . 107.5 ?
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
C5 N1 . 1.488(3) ?
C5 C4 . 1.512(4) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C4 N2 . 1.488(3) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
Te1 O5 . 1.9050(18) ?
Te1 O6 . 1.9050(18) ?
Te1 O1 . 1.9119(19) ?
Te1 O3 . 1.9124(18) ?
Te1 O4 . 1.9130(18) ?
Te1 O2 . 1.916(2) ?
P1 O8 . 1.4784(17) ?
P1 O9 . 1.4831(17) ?
P1 O7 . 1.6028(18) ?
P1 O10 . 1.6046(18) ?
P2 O11 . 1.4766(18) ?
P2 O12 . 1.4825(19) ?
P2 O7 7_556 1.6033(17) ?
P2 O10 . 1.6052(17) ?
O7 P2 7_556 1.6033(17) ?
O1 H1 . 0.855(13) ?
N2 C3 . 1.486(4) ?
N2 H2A . 0.9000 ?
N2 H2B . 0.9000 ?
O4 H4 . 0.846(18) ?
O6 H6 . 0.830(17) ?
O2 H2 . 0.862(16) ?
O5 H5 . 0.874(17) ?
C3 C2 . 1.517(4) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
N1 C1 . 1.488(4) ?
N1 H1A . 0.9000 ?
N1 H1B . 0.9000 ?
C2 C1 . 1.513(4) ?
C2 H2C . 0.9700 ?
C2 H2D . 0.9700 ?
O3 H3 . 0.840(19) ?
C1 H1C . 0.9700 ?
C1 H1D . 0.9700 ?
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 H1 O12 7_556 0.856(16) 1.851(17) 2.686(3) 165(2) yes
N1 H1B O4 5_566 0.90 2.15 2.898(3) 140 yes
N1 H1B O9 4_556 0.90 2.42 3.002(3) 123 yes
N1 H1A O2 1_556 0.90 1.89 2.763(3) 162 yes
O2 H2 O9 8_455 0.86(2) 1.831(19) 2.688(3) 172(3) yes
N2 H2A O12 . 0.90 1.89 2.769(3) 167 yes
N2 H2B O11 4_546 0.90 1.85 2.739(3) 172 yes
O3 H3 O8 8_455 0.84(3) 2.05(3) 2.881(3) 170(4) yes
O4 H4 O1 2_555 0.85(3) 1.85(3) 2.695(3) 175(3) yes
O5 H5 O8 4_545 0.87(3) 1.85(3) 2.719(3) 172(3) yes
O6 H6 O9 4_555 0.83(3) 1.90(2) 2.722(3) 171(3) yes
C2 H2C O1 6_556 0.97 2.60 3.162(3) 117 yes
C4 H4B O5 7_556 0.97 2.43 3.256(4) 142 yes
C5 H5B O11 6_566 0.97 2.31 3.265(4) 168 yes
