#------------------------------------------------------------------------------
#$Date: 2019-12-26 21:54:54 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246123 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/18/2311806.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_2311806
loop_
_publ_author_name
'Bouchene, Rafika'
'Bouacida, Sofiane'
'Berrah, Fadila'
'Roisnel, Thierry'
_publ_section_title
;
 A simple hydrated salt with a complex hydrogen-bonding network:
 tetrakis(5-amino-3-carboxy-4H-1,2,4-triazol-1-ium)
 hexachloridocadmate(II) tetrahydrate.
;
_journal_coeditor_code           KU3133
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              672
_journal_page_last               676
_journal_paper_doi               10.1107/S2053229614012819
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '4C3 H5 N4 O2 + , Cd Cl6 4- , 4H2 O'
_chemical_formula_moiety         '4(C3 H5 N4 O2 +), Cd Cl6 4-, 4(H2 O)'
_chemical_formula_sum            'C12 H28 Cd Cl6 N16 O12'
_chemical_formula_weight         913.61
_chemical_name_systematic
;
Tetrakis(5-amino-3-carboxy-4H-1,2,4-triazol-1-ium)
hexachloridocadmate(II) tetrahydrate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                109.352(2)
_cell_angle_beta                 110.768(2)
_cell_angle_gamma                96.643(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4373(4)
_cell_length_b                   9.5334(4)
_cell_length_c                   10.4848(5)
_cell_measurement_reflns_used    6410
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.39
_cell_volume                     802.59(6)
_computing_cell_refinement       'APEX2 (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2001)'
_computing_data_reduction        'APEX2 (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9881
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.990
_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_constraints    6
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3565
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0262
_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)+(0.0383P)²+0.4658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                3334
_reflns_number_total             3565
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ku3133sup1.cif
_cod_data_source_block           I
_cod_database_code               2311806
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -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_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
O O8 0.02998(17) 0.48245(17) 0.21876(16) 0.0197(4) Uani d . 1.000
O O9 0.04705(18) 0.63653(18) 0.44236(17) 0.0226(5) Uani d . 1.000
N N1 0.5168(2) 0.4977(2) 0.7572(2) 0.0200(5) Uani d . 1.000
N N3 0.38211(19) 0.3574(2) 0.49436(19) 0.0163(5) Uani d . 1.000
N N4 0.2601(2) 0.3625(2) 0.37738(19) 0.0168(5) Uani d . 1.000
N N6 0.30201(19) 0.54971(19) 0.59112(19) 0.0149(5) Uani d . 1.000
C C2 0.4084(2) 0.4698(2) 0.6243(2) 0.0158(6) Uani d . 1.000
C C5 0.2146(2) 0.4796(2) 0.4397(2) 0.0146(5) Uani d . 1.000
C C7 0.0855(2) 0.5325(2) 0.3534(2) 0.0158(6) Uani d . 1.000
O O17 0.36683(17) 0.77460(17) 0.40758(16) 0.0193(4) Uani d . 1.000
O O18 0.34338(18) 0.98366(18) 0.57315(17) 0.0240(4) Uani d . 1.000
N N10 -0.0893(2) 0.8048(2) -0.0370(2) 0.0221(5) Uani d . 1.000
N N12 -0.0140(2) 0.9749(2) 0.21443(19) 0.0168(5) Uani d . 1.000
N N13 0.0971(2) 1.0018(2) 0.35292(19) 0.0166(5) Uani d . 1.000
N N15 0.11457(19) 0.80514(19) 0.17750(19) 0.0147(5) Uani d . 1.000
C C11 -0.0037(2) 0.8572(2) 0.1073(2) 0.0154(6) Uani d . 1.000
C C14 0.1725(2) 0.8976(2) 0.3251(2) 0.0142(5) Uani d . 1.000
C C16 0.3058(2) 0.8787(2) 0.4405(2) 0.0157(6) Uani d . 1.000
Cd Cd1 0.50000 1.00000 0.00000 0.01410(10) Uani d S 1.000
Cl Cl1 0.39747(6) 1.08296(6) 0.21183(5) 0.01750(10) Uani d . 1.000
Cl Cl2 0.22928(5) 0.80659(5) -0.18305(5) 0.01730(10) Uani d . 1.000
Cl Cl3 0.58603(6) 0.77248(6) 0.07099(6) 0.01870(10) Uani d . 1.000
O O1W 0.82954(18) 0.75504(19) 0.35604(18) 0.0223(5) Uani d D 1.000
O O2W 0.25195(18) 0.60899(19) 0.04346(18) 0.0211(5) Uani d D 1.000
H H1A 0.58030 0.44020 0.76700 0.0240 Uiso c R 1.000
H H1B 0.52390 0.57330 0.83420 0.0240 Uiso c R 1.000
H H3 0.43530 0.29020 0.48540 0.0190 Uiso c R 1.000
H H6 0.29100 0.62890 0.65260 0.0180 Uiso c R 1.000
H H9 -0.02400 0.66430 0.39310 0.0340 Uiso c R 1.000
H H10A -0.16120 0.84710 -0.07140 0.0270 Uiso c R 1.000
H H10B -0.07330 0.72810 -0.09700 0.0270 Uiso c R 1.000
H H12 -0.08190 1.02720 0.19840 0.0200 Uiso c R 1.000
H H15 0.14690 0.72890 0.13710 0.0180 Uiso c R 1.000
H H18 0.41730 0.97020 0.63430 0.0360 Uiso c R 1.000
H H1WA 0.769(3) 0.757(3) 0.279(2) 0.0270 Uiso d D 1.000
H H1WB 0.848(3) 0.834(2) 0.429(2) 0.0270 Uiso d D 1.000
H H2WB 0.329(2) 0.656(3) 0.040(3) 0.0250 Uiso d D 1.000
H H2WA 0.183(3) 0.567(3) -0.044(2) 0.0250 Uiso d D 1.000
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'
Cd Cd -0.8075 1.2024 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 ' 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
Cl1 Cd1 Cl2 2_675 . 89.93(2) .
Cl2 Cd1 Cl2 . 2_675 180.00 .
Cl2 Cd1 Cl3 . 2_675 92.78(2) .
Cl1 Cd1 Cl3 2_675 . 88.79(2) .
Cl2 Cd1 Cl3 2_675 . 92.78(2) .
Cl3 Cd1 Cl3 . 2_675 180.00 .
Cl1 Cd1 Cl2 2_675 2_675 90.07(2) .
Cl1 Cd1 Cl3 2_675 2_675 91.21(2) .
Cl2 Cd1 Cl3 2_675 2_675 87.22(2) .
Cl1 Cd1 Cl2 . . 90.07(2) yes
Cl1 Cd1 Cl3 . . 91.21(2) yes
Cl1 Cd1 Cl1 . 2_675 180.00 .
Cl1 Cd1 Cl2 . 2_675 89.93(2) .
Cl1 Cd1 Cl3 . 2_675 88.79(2) .
Cl2 Cd1 Cl3 . . 87.22(2) yes
C7 O9 H9 . . 109.00 no
C16 O18 H18 . . 109.00 no
H1WA O1W H1WB . . 112(2) no
H2WB O2W H2WA . . 106(3) no
N4 N3 C2 . . 111.88(18) yes
N3 N4 C5 . . 103.69(16) yes
C2 N6 C5 . . 106.42(17) yes
C2 N1 H1B . . 120.00 no
C2 N1 H1A . . 120.00 no
H1A N1 H1B . . 120.00 no
C2 N3 H3 . . 124.00 no
N4 N3 H3 . . 124.00 no
C5 N6 H6 . . 127.00 no
C2 N6 H6 . . 127.00 no
N13 N12 C11 . . 111.70(18) yes
N12 N13 C14 . . 103.32(17) yes
C11 N15 C14 . . 106.23(17) yes
H10A N10 H10B . . 120.00 no
C11 N10 H10B . . 120.00 no
C11 N10 H10A . . 120.00 no
N13 N12 H12 . . 124.00 no
C11 N12 H12 . . 124.00 no
C11 N15 H15 . . 127.00 no
C14 N15 H15 . . 127.00 no
N1 C2 N3 . . 127.3(2) .
N1 C2 N6 . . 126.93(19) .
N3 C2 N6 . . 105.78(17) .
N6 C5 C7 . . 124.95(18) .
N4 C5 C7 . . 122.80(17) .
N4 C5 N6 . . 112.23(18) .
O9 C7 C5 . . 110.75(16) .
O8 C7 C5 . . 121.89(19) .
O8 C7 O9 . . 127.4(2) .
N12 C11 N15 . . 105.95(16) .
N10 C11 N15 . . 126.93(19) .
N10 C11 N12 . . 127.1(2) .
N15 C14 C16 . . 122.97(18) .
N13 C14 C16 . . 124.24(17) .
N13 C14 N15 . . 112.78(18) .
O17 C16 O18 . . 127.29(19) .
O17 C16 C14 . . 120.89(17) .
O18 C16 C14 . . 111.82(18) .
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
Cd1 Cl1 2_675 2.6517(5) .
Cd1 Cl2 2_675 2.5881(5) .
Cd1 Cl3 2_675 2.6395(6) .
Cd1 Cl1 . 2.6517(5) yes
Cd1 Cl2 . 2.5881(5) yes
Cd1 Cl3 . 2.6395(6) yes
O8 C7 . 1.211(2) yes
O9 C7 . 1.302(3) yes
O9 H9 . 0.8200 no
O17 C16 . 1.217(3) yes
O18 C16 . 1.307(2) yes
O18 H18 . 0.8200 no
O1W H1WB . 0.82(2) no
O1W H1WA . 0.82(2) no
O2W H2WB . 0.83(3) no
O2W H2WA . 0.835(19) no
N1 C2 . 1.319(3) yes
N3 N4 . 1.372(3) yes
N3 C2 . 1.341(3) yes
N4 C5 . 1.298(3) yes
N6 C5 . 1.374(2) yes
N6 C2 . 1.347(3) yes
N1 H1B . 0.8600 no
N1 H1A . 0.8600 no
N3 H3 . 0.8600 no
N6 H6 . 0.8600 no
N10 C11 . 1.315(3) yes
N12 N13 . 1.373(3) yes
N12 C11 . 1.341(3) yes
N13 C14 . 1.303(3) yes
N15 C14 . 1.362(2) yes
N15 C11 . 1.350(3) yes
N10 H10A . 0.8600 no
N10 H10B . 0.8600 no
N12 H12 . 0.8600 no
N15 H15 . 0.8600 no
C5 C7 . 1.490(3) no
C14 C16 . 1.482(3) no
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
O9 H9 O1W 1_455 0.82 1.71 2.491(3) 158 yes
O18 H18 Cl1 2_676 0.82 2.16 2.977(2) 176 yes
O1W H1WA Cl3 . 0.82(2) 2.32(2) 3.128(2) 175(3) yes
O1W H1WB N13 2_676 0.82(2) 2.13(2) 2.934(2) 164(2) yes
O2W H2WA O8 2_565 0.83(2) 2.05(2) 2.844(2) 158(3) yes
O2W H2WB Cl3 . 0.83(3) 2.41(2) 3.221(2) 167(3) yes
N1 H1A O2W 2_666 0.86 2.29 2.976(3) 137 yes
N1 H1A O17 2_666 0.86 2.49 3.156(3) 135 yes
N1 H1B Cl3 1_556 0.86 2.39 3.237(2) 170 yes
N3 H3 Cl1 1_545 0.86 2.76 3.301(2) 122 yes
N3 H3 O17 2_666 0.86 2.09 2.842(3) 146 yes
N6 H6 Cl2 1_556 0.86 2.28 3.126(2) 170 yes
N10 H10A Cl1 2_575 0.86 2.50 3.347(2) 168 yes
N10 H10B O8 2_565 0.86 2.17 3.016(3) 170 yes
N10 H10B N4 2_565 0.86 2.60 3.071(2) 115 yes
N12 H12 Cl2 2_575 0.86 2.23 3.088(2) 171 yes
N15 H15 O2W . 0.86 1.86 2.695(3) 163 yes
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_publ_flag
C2 N3 N4 C5 0.1(2) no
N4 N3 C2 N1 -179.7(2) no
N4 N3 C2 N6 -0.2(2) no
N3 N4 C5 N6 0.1(2) no
N3 N4 C5 C7 178.15(19) no
C5 N6 C2 N1 179.7(2) no
C5 N6 C2 N3 0.3(2) no
C2 N6 C5 N4 -0.2(3) no
C2 N6 C5 C7 -178.24(19) no
N13 N12 C11 N15 0.9(2) no
C11 N12 N13 C14 -0.1(3) no
N13 N12 C11 N10 -178.0(2) no
N12 N13 C14 N15 -0.8(2) no
N12 N13 C14 C16 -180.0(2) no
C14 N15 C11 N10 177.6(2) no
C14 N15 C11 N12 -1.3(2) no
C11 N15 C14 N13 1.3(3) no
C11 N15 C14 C16 -179.45(19) no
N4 C5 C7 O8 -10.2(3) no
N6 C5 C7 O9 -11.5(3) no
N4 C5 C7 O9 170.7(2) no
N6 C5 C7 O8 167.7(2) no
N13 C14 C16 O17 176.8(2) no
N13 C14 C16 O18 -2.9(3) no
N15 C14 C16 O17 -2.3(3) no
N15 C14 C16 O18 178.01(19) no
