#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/85/2018525.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_2018525
loop_
_publ_author_name
'Domasevitch, Konstantin V.'
_publ_section_title
;
 4,4'-Bi(1H-pyrazol-2-ium) tetrachloridoaurate(III) chloride: a
 three-dimensional cationic cooperite-like framework with multiple
 pyrazolium--chloride hydrogen-bonding interactions
;
_journal_coeditor_code           EM3049
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m169
_journal_page_last               m172
_journal_paper_doi               10.1107/S0108270112024389
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C6 H8 N4) [Au Cl4] Cl'
_chemical_formula_moiety         'C6 H8 N4 2+, Au Cl4 -, Cl -'
_chemical_formula_sum            'C6 H8 Au Cl5 N4'
_chemical_formula_weight         510.38
_chemical_name_systematic
;
4,4'-Bi(1H-pyrazol-2-ium) tetrachloridoaurate(III) chloride
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.533(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5768(8)
_cell_length_b                   16.0166(9)
_cell_length_c                   7.1617(5)
_cell_measurement_reflns_used    6076
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      3.19
_cell_volume                     1350.99(17)
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'φ oscillation 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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6076
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    11.856
_exptl_absorpt_correction_T_max  0.4150
_exptl_absorpt_correction_T_min  0.3555
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.306
_refine_ls_extinction_coef       0.0026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0267
_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)+(0.0433P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                1798
_reflns_number_total             1967
_reflns_threshold_expression     I>2σ(I)
_iucr_refine_instructions_details
;
TITL ip107 in C2c
CELL  0.71073  12.5768  16.0166   7.1617   90.000  110.533   90.000
ZERR     4.00   0.0008   0.0009   0.0005    0.000    0.010    0.000
LATT   7
SYMM  - X,   Y, 1/2 - Z
SFAC  C    H    CL   AU   N
UNIT  24   32   20   4    16
MERG   2
OMIT     0
OMIT    -2   0   2
SHEL 0.71 8
FMAP   2
PLAN    8
SIZE     0.09   0.11   0.11
ACTA
BOND   $H
EQIV $1 1-X, 1-Y, 2-Z
EQIV $2 0.5+X, -0.5+Y, 1+Z
EQIV $3 0.5-X, -0.5+Y, 1.5-Z
EQIV $4 -X, 1-Y, 1-Z
RTAB H..O H1N CL1
RTAB H..O H2N CL1_$1
RTAB H..O H2N CL4_$2
RTAB H..O H3 CL4_$2
RTAB H..O H3 CL2_$3
RTAB O..O N1 CL1
RTAB O..O N2 CL1_$1
RTAB O..O N2 CL4_$2
RTAB O..O C3 CL4_$2
RTAB O..O C3 CL2_$3
RTAB XHY N1 H1N CL1
RTAB XHY N2 H2N CL1_$1
RTAB XHY N2 H2N CL4_$2
RTAB XHY C3 H3 CL4_$2
RTAB XHY C3 H3 CL2_$3
BIND AU1 CL3_$4
CONF
LIST   4
L.S.   4
TEMP   -60.00
WGHT    0.043300
EXTI    0.002609
FVAR       0.10194
AU1   4    0.000000    0.569379    0.250000    10.50000    0.02773    0.02806 =
         0.02129    0.00000    0.00728    0.00000
CL1   3    0.500000    0.565871    0.750000    10.50000    0.03758    0.02175 =
         0.02204    0.00000   -0.00424    0.00000
CL2   3    0.186363    0.570620    0.455687    11.00000    0.02913    0.04296 =
         0.03657    0.00001    0.00701   -0.00013
CL3   3    0.000000    0.426382    0.250000    10.50000    0.03709    0.02692 =
         0.04960    0.00000    0.01831    0.00000
CL4   3    0.000000    0.712372    0.250000    10.50000    0.07253    0.02791 =
         0.03288    0.00000   -0.01323    0.00000
N1    5    0.360344    0.400674    0.701142    11.00000    0.03313    0.02786 =
         0.03743   -0.01178    0.00990   -0.00813
AFIX  43
H1N   2    0.379032    0.453206    0.715912    11.00000   -1.50000
AFIX   0
N2    5    0.393053    0.342893    0.843781    11.00000    0.02905    0.03899 =
         0.02581   -0.01044   -0.00078   -0.00333
AFIX  43
H2N   2    0.437899    0.351496    0.965997    11.00000   -1.50000
AFIX   0
C1    1    0.294100    0.364834    0.531499    11.00000    0.03061    0.02709 =
         0.02725   -0.00230    0.00416   -0.00198
AFIX  43
H1    2    0.261186    0.391651    0.407781    11.00000   -1.20000
AFIX   0
C2    1    0.282601    0.281611    0.570085    11.00000    0.02509    0.02457 =
         0.02056   -0.00322    0.00161   -0.00278
C3    1    0.346385    0.269954    0.770045    11.00000    0.03082    0.03277 =
         0.02186   -0.00043    0.00117   -0.00141
AFIX  43
H3    2    0.355103    0.219496    0.840898    11.00000   -1.20000
HKLF    4
REM  ip107 in C2c
REM R1 =  0.0267 for   1798 Fo > 4sig(Fo)  and  0.0293 for all   1967 data
REM     76 parameters refined using      0 restraints
END
WGHT      0.0433      0.0000
REM Highest difference peak  1.687,  deepest hole -1.306,  1-sigma level  0.182
Q1    1  -0.0397  0.6134  0.2377  11.00000  0.05    1.69
Q2    1  -0.0384  0.5274  0.2380  11.00000  0.05    1.62
Q3    1  -0.0368  0.5702  0.0935  11.00000  0.05    1.17
Q4    1   0.1215  0.5689  0.3162  11.00000  0.05    1.17
Q5    1   0.0379  0.5701  0.1251  11.00000  0.05    0.84
Q6    1   0.4015  0.2007  0.6279  11.00000  0.05    0.60
Q7    1  -0.1060  0.4305  0.0861  11.00000  0.05    0.52
Q8    1  -0.0440  0.4307  0.0979  11.00000  0.05    0.48
;
_cod_data_source_file            em3049.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2018525
_cod_database_fobs_code          2018525
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_symmetry_multiplicity
Au Au1 0.0000 0.569379(12) 0.2500 0.02604(9) Uani d S 1 2
Cl Cl1 0.5000 0.56587(7) 0.7500 0.0310(2) Uani d S 1 2
Cl Cl2 0.18636(8) 0.57062(7) 0.45569(15) 0.0374(2) Uani d . 1 1
Cl Cl3 0.0000 0.42638(9) 0.2500 0.0370(3) Uani d S 1 2
Cl Cl4 0.0000 0.71237(10) 0.2500 0.0529(4) Uani d S 1 2
N N1 0.3603(3) 0.4007(2) 0.7011(5) 0.0335(6) Uani d . 1 1
H H1N 0.3790 0.4532 0.7159 0.050 Uiso calc R 1 1
N N2 0.3931(3) 0.3429(2) 0.8438(5) 0.0341(7) Uani d . 1 1
H H2N 0.4379 0.3515 0.9660 0.051 Uiso calc R 1 1
C C1 0.2941(3) 0.3648(2) 0.5315(5) 0.0299(7) Uani d . 1 1
H H1 0.2612 0.3917 0.4078 0.036 Uiso calc R 1 1
C C2 0.2826(3) 0.2816(2) 0.5701(4) 0.0251(6) Uani d . 1 1
C C3 0.3464(3) 0.2700(3) 0.7700(5) 0.0306(7) Uani d . 1 1
H H3 0.3551 0.2195 0.8409 0.037 Uiso calc R 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Au1 0.02773(11) 0.02806(12) 0.02129(10) 0.000 0.00728(6) 0.000
Cl1 0.0376(5) 0.0217(5) 0.0220(5) 0.000 -0.0042(4) 0.000
Cl2 0.0291(4) 0.0430(5) 0.0366(4) -0.0001(3) 0.0070(3) 0.0000(4)
Cl3 0.0371(6) 0.0269(6) 0.0496(7) 0.000 0.0183(5) 0.000
Cl4 0.0725(10) 0.0279(7) 0.0329(6) 0.000 -0.0132(6) 0.000
N1 0.0331(14) 0.0279(15) 0.0374(15) -0.0081(12) 0.0099(12) -0.0118(13)
N2 0.0291(13) 0.0390(18) 0.0258(13) -0.0033(13) -0.0008(11) -0.0104(12)
C1 0.0306(15) 0.0271(17) 0.0273(15) -0.0020(12) 0.0042(12) -0.0023(12)
C2 0.0251(13) 0.0246(16) 0.0206(13) -0.0028(12) 0.0016(10) -0.0032(12)
C3 0.0308(15) 0.0328(19) 0.0219(14) -0.0014(13) 0.0012(12) -0.0004(13)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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'
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
Cl2 Au1 Cl2 . 2 179.00(5) y
Cl2 Au1 Cl4 . . 89.50(3) y
Cl2 Au1 Cl4 2 . 89.50(3) ?
Cl2 Au1 Cl3 . . 90.50(3) y
Cl2 Au1 Cl3 2 . 90.50(3) ?
Cl4 Au1 Cl3 . . 180.0 ?
N2 N1 C1 . . 109.0(3) ?
N2 N1 H1N . . 125.5 ?
C1 N1 H1N . . 125.5 ?
C3 N2 N1 . . 109.3(3) ?
C3 N2 H2N . . 125.3 ?
N1 N2 H2N . . 125.3 ?
N1 C1 C2 . . 108.0(3) ?
N1 C1 H1 . . 126.0 ?
C2 C1 H1 . . 126.0 ?
C1 C2 C3 . . 105.9(3) ?
C1 C2 C2 . 7_556 127.3(4) ?
C3 C2 C2 . 7_556 126.8(4) ?
N2 C3 C2 . . 107.8(3) ?
N2 C3 H3 . . 126.1 ?
C2 C3 H3 . . 126.1 ?
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
N1 N2 . 1.332(5) y
N1 C1 . 1.338(4) y
N1 H1N . 0.8700 ?
N2 C3 . 1.331(5) y
N2 H2N . 0.8700 ?
C1 C2 . 1.379(5) y
C1 H1 . 0.9400 ?
C2 C3 . 1.387(4) y
C2 C2 7_556 1.459(6) y
C3 H3 . 0.9400 ?
Au1 Cl2 . 2.2895(10) y
Au1 Cl2 2 2.2895(10) ?
Au1 Cl4 . 2.2903(16) y
Au1 Cl3 . 2.2903(14) y
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
N1 H1N Cl1 . 0.87 2.32 3.127(3) 155 yes
N2 H2N Cl1 5_667 0.87 2.32 3.109(3) 151 yes
N2 H2N Cl4 3_546 0.87 2.93 3.449(4) 120 yes
C3 H3 Cl4 3_546 0.94 2.86 3.426(3) 120 yes
C3 H3 Cl2 4_546 0.94 2.93 3.846(4) 164 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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C1 N1 N2 C3 . . -1.6(5)
N2 N1 C1 C2 . . 1.4(4)
N1 C1 C2 C3 . . -0.7(4)
N1 C1 C2 C2 . 7_556 179.6(4)
N1 N2 C3 C2 . . 1.1(4)
C1 C2 C3 N2 . . -0.2(4)
C2 C2 C3 N2 7_556 . 179.5(4)
