#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/19/8101994.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_8101994
loop_
_publ_author_name
'Du, Z.-X.'
'Han, M.-L.'
'Feng, X.'
_publ_section_title
;
Crystal structure of tetrakis(melaminium) 1,2,4,5-benzenetetracarboxylate 
octahydrate, (C₃H₇N₆)₄[C₆H₂(COO)₄] · 8H₂O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              313
_journal_page_last               315
_journal_volume                  221
_journal_year                    2006
_chemical_formula_structural     '(C3H7N6)4[C6H2(COO)4] &#x00B7; 8H2O'
_chemical_formula_sum            'C22 H46 N24 O16'
_chemical_formula_weight         902.82
_chemical_name_systematic
' tetrakis(melaminium) 1,2,4,5-benzenetetracarboxylate octahydrate'
_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                105.8790(10)
_cell_angle_beta                 91.6080(10)
_cell_angle_gamma                96.2540(10)
_cell_formula_units_Z            1
_cell_length_a                   7.0706(6)
_cell_length_b                   9.7952(8)
_cell_length_c                   14.7895(12)
_cell_measurement_reflns_used    4774
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     977.55(14)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0106
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9056
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_correction_T_min  0.9406
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0490
_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)+(0.0800P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1500
_reflns_number_gt                3932
_reflns_number_total             4691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1807.cff
_cod_data_source_block           a
_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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101994
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
O1 O 0.5065(2) 0.77166(15) 0.65581(9) 0.0439(3) Uani 1 2 i d . . .
O2 O 0.2004(2) 0.7809(2) 0.62091(11) 0.0564(4) Uani 1 2 i d . . .
O3 O 0.3680(3) 1.08183(17) 0.74586(9) 0.0554(5) Uani 1 2 i d . . .
O4 O 0.2371(2) 1.22944(14) 0.67959(9) 0.0422(3) Uani 1 2 i d . . .
C7 C 0.5206(3) 0.85569(16) 0.47301(10) 0.0290(3) Uani 1 2 i d . . .
H7 H 0.5344 0.7588 0.4551 0.035 Uiso 1 2 i calc R . .
C8 C 0.4375(2) 0.91376(16) 0.55704(10) 0.0264(3) Uani 1 2 i d . . .
C9 C 0.4166(2) 1.05955(16) 0.58489(10) 0.0265(3) Uani 1 2 i d . . .
C10 C 0.3757(3) 0.81516(17) 0.61621(11) 0.0318(4) Uani 1 2 i d . . .
C11 C 0.3345(3) 1.12862(17) 0.67790(11) 0.0313(4) Uani 1 2 i d . . .
N1 N 0.3079(2) 0.41288(14) 0.07577(9) 0.0268(3) Uani 1 2 i d . . .
N2 N 0.39726(19) 0.17443(13) 0.01954(9) 0.0251(3) Uani 1 2 i d . . .
N3 N 0.3877(2) 0.28531(14) 0.18171(9) 0.0260(3) Uani 1 2 i d . . .
H3' H 0.4017 0.2814 0.2388 0.031 Uiso 1 2 i d R . .
N4 N 0.3052(2) 0.51309(16) 0.23622(10) 0.0371(4) Uani 1 2 i d . . .
H4A H 0.2698 0.5900 0.2274 0.044 Uiso 1 2 i d R . .
H4B H 0.3223 0.5061 0.2925 0.044 Uiso 1 2 i d R . .
N5 N 0.3156(2) 0.30192(15) -0.08141(10) 0.0327(3) Uani 1 2 i d . . .
H5A H 0.3342 0.2302 -0.1275 0.039 Uiso 1 2 i d R . .
H5B H 0.2803 0.3775 -0.0923 0.039 Uiso 1 2 i d R . .
N6 N 0.4737(2) 0.05796(15) 0.12887(10) 0.0307(3) Uani 1 2 i d . . .
H6A H 0.4949 -0.0151 0.0843 0.037 Uiso 1 2 i d R . .
H6B H 0.4878 0.0570 0.1867 0.037 Uiso 1 2 i d R . .
C1 C 0.3332(2) 0.40543(16) 0.16319(11) 0.0252(3) Uani 1 2 i d . . .
C2 C 0.3415(2) 0.29595(16) 0.00614(11) 0.0241(3) Uani 1 2 i d . . .
C3 C 0.4197(2) 0.17160(16) 0.10857(10) 0.0235(3) Uani 1 2 i d . . .
N7 N 0.1134(2) 0.74510(14) 0.79465(9) 0.0278(3) Uani 1 2 i d . . .
H7' H 0.1036 0.7625 0.7409 0.033 Uiso 1 2 i d R . .
N8 N 0.1858(2) 0.58772(14) 0.88237(9) 0.0273(3) Uani 1 2 i d . . .
N9 N 0.08855(19) 0.81946(14) 0.95865(9) 0.0263(3) Uani 1 2 i d . . .
N10 N 0.0205(2) 0.96550(15) 0.86681(10) 0.0324(3) Uani 1 2 i d . . .
H10A H -0.0057 1.0296 0.9160 0.039 Uiso 1 2 i d R . .
H10B H 0.0116 0.9805 0.8123 0.039 Uiso 1 2 i d R . .
N11 N 0.2054(2) 0.52640(16) 0.72134(10) 0.0355(3) Uani 1 2 i d . . .
H11A H 0.2416 0.4456 0.7219 0.043 Uiso 1 2 i d R . .
H11B H 0.1932 0.5478 0.6690 0.043 Uiso 1 2 i d R . .
N12 N 0.1640(2) 0.66497(16) 1.04139(10) 0.0353(3) Uani 1 2 i d . . .
H12A H 0.1401 0.7272 1.0919 0.042 Uiso 1 2 i d R . .
H12B H 0.2000 0.5852 1.0445 0.042 Uiso 1 2 i d R . .
C4 C 0.0741(2) 0.84427(16) 0.87508(11) 0.0246(3) Uani 1 2 i d . . .
C5 C 0.1685(2) 0.61774(16) 0.80088(11) 0.0256(3) Uani 1 2 i d . . .
C6 C 0.1458(2) 0.69185(16) 0.95921(11) 0.0253(3) Uani 1 2 i d . . .
O5 O 0.8645(3) 0.9300(2) 0.67432(12) 0.0612(4) Uani 1 2 i d G . .
H1W H 0.7589 0.8761 0.6612 0.092 Uiso 1 2 i d G . .
H2W H 0.9467 0.8938 0.6371 0.092 Uiso 1 2 i d G . .
O6 O 0.3124(5) 0.4941(3) 0.42646(17) 0.1188(11) Uani 1 2 i d . . .
H3W H 0.2907 0.4574 0.4716 0.178 Uiso 1 2 i d R . .
H4W H 0.1967 0.4605 0.4273 0.178 Uiso 1 2 i d R . .
O7 O 0.9236(4) 0.6733(3) 0.47058(16) 0.0945(7) Uani 1 2 i d . . .
H5W H 0.9975 0.7404 0.5081 0.142 Uiso 1 2 i d R . .
H6W H 0.8762 0.7019 0.4265 0.142 Uiso 1 2 i d R . .
O8 O 0.8790(3) 0.22674(17) 0.76052(11) 0.0527(4) Uani 1 2 i d G . .
H7W H 0.8245 0.1436 0.7322 0.079 Uiso 1 2 i d G . .
H8W H 0.9928 0.2359 0.7440 0.079 Uiso 1 2 i d G . .
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 C7 C9 121.14(14) . 2_676 ?
C8 C7 H7 119.4 . . ?
C9 C7 H7 119.4 2_676 . ?
C7 C8 C9 119.97(14) . . ?
C7 C8 C10 117.82(14) . . ?
C9 C8 C10 122.19(14) . . ?
C7 C9 C8 118.89(13) 2_676 . ?
C7 C9 C11 119.33(13) 2_676 . ?
C8 C9 C11 121.74(13) . . ?
O1 C10 O2 125.06(16) . . ?
O1 C10 C8 116.26(16) . . ?
O2 C10 C8 118.66(15) . . ?
O3 C11 O4 125.16(15) . . ?
O3 C11 C9 117.92(14) . . ?
O4 C11 C9 116.92(14) . . ?
C1 N1 C2 116.34(13) . . ?
C3 N2 C2 116.09(13) . . ?
C3 N3 C1 119.49(13) . . ?
C3 N3 H3' 120.3 . . ?
C1 N3 H3' 120.3 . . ?
C1 N4 H4A 120.0 . . ?
C1 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C2 N5 H5A 119.9 . . ?
C2 N5 H5B 120.1 . . ?
H5A N5 H5B 120.0 . . ?
C3 N6 H6A 120.0 . . ?
C3 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
N4 C1 N1 121.39(14) . . ?
N4 C1 N3 117.32(14) . . ?
N1 C1 N3 121.29(14) . . ?
N5 C2 N2 117.76(14) . . ?
N5 C2 N1 116.85(13) . . ?
N2 C2 N1 125.39(14) . . ?
N6 C3 N2 120.64(14) . . ?
N6 C3 N3 117.96(13) . . ?
N2 C3 N3 121.40(13) . . ?
C4 N7 C5 119.28(13) . . ?
C4 N7 H7' 120.4 . . ?
C5 N7 H7' 120.3 . . ?
C5 N8 C6 115.40(13) . . ?
C4 N9 C6 115.99(13) . . ?
C4 N10 H10A 120.0 . . ?
C4 N10 H10B 120.1 . . ?
H10A N10 H10B 120.0 . . ?
C5 N11 H11A 120.0 . . ?
C5 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C6 N12 H12A 120.0 . . ?
C6 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N10 C4 N9 120.83(14) . . ?
N10 C4 N7 117.89(14) . . ?
N9 C4 N7 121.27(13) . . ?
N11 C5 N8 121.29(14) . . ?
N11 C5 N7 116.76(14) . . ?
N8 C5 N7 121.95(14) . . ?
N12 C6 N9 117.40(14) . . ?
N12 C6 N8 116.50(13) . . ?
N9 C6 N8 126.10(14) . . ?
H1W O5 H2W 109.5 . . ?
H3W O6 H4W 66.2 . . ?
H5W O7 H6W 110.6 . . ?
H7W O8 H8W 109.6 . . ?
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
O1 C10 1.254(2) . ?
O2 C10 1.257(2) . ?
O3 C11 1.240(2) . ?
O4 C11 1.259(2) . ?
C7 C8 1.393(2) . ?
C7 C9 1.396(2) 2_676 ?
C7 H7 0.9300 . ?
C8 C9 1.399(2) . ?
C8 C10 1.510(2) . ?
C9 C7 1.396(2) 2_676 ?
C9 C11 1.519(2) . ?
N1 C1 1.323(2) . ?
N1 C2 1.3624(19) . ?
N2 C3 1.3301(19) . ?
N2 C2 1.3559(19) . ?
N3 C3 1.3679(19) . ?
N3 C1 1.3701(19) . ?
N3 H3' 0.8597 . ?
N4 C1 1.324(2) . ?
N4 H4A 0.8604 . ?
N4 H4B 0.8599 . ?
N5 C2 1.321(2) . ?
N5 H5A 0.8597 . ?
N5 H5B 0.8602 . ?
N6 C3 1.3205(19) . ?
N6 H6A 0.8602 . ?
N6 H6B 0.8607 . ?
N7 C4 1.371(2) . ?
N7 C5 1.3723(19) . ?
N7 H7' 0.8603 . ?
N8 C5 1.322(2) . ?
N8 C6 1.3633(19) . ?
N9 C4 1.327(2) . ?
N9 C6 1.3572(19) . ?
N10 C4 1.320(2) . ?
N10 H10A 0.8604 . ?
N10 H10B 0.8597 . ?
N11 C5 1.321(2) . ?
N11 H11A 0.8603 . ?
N11 H11B 0.8597 . ?
N12 C6 1.318(2) . ?
N12 H12A 0.8592 . ?
N12 H12B 0.8602 . ?
O5 H1W 0.8507 . ?
O5 H2W 0.8506 . ?
O6 H3W 0.8499 . ?
O6 H4W 0.8500 . ?
O7 H5W 0.8503 . ?
O7 H6W 0.8515 . ?
O8 H7W 0.8501 . ?
O8 H8W 0.8504 . ?
