# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2016572'
loop_
_audit_author_name
_audit_author_address
'Roberto Centore'
;University of Naples Federico II
Italy
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
'4-Methyl-7-(2-pyrazinyl)-2H-[1,2,4]triazolo[3,2-c][1,2,4]-triazole hydrate'
_chemical_formula_moiety         '(c8 H7 N7), (H2 O)'
_chemical_formula_sum            'C8 H9 N7 O'
_chemical_formula_weight         219.22

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.4070(13)
_cell_length_b                   8.507(3)
_cell_length_c                   11.507(5)
_cell_angle_alpha                109.32(3)
_cell_angle_beta                 93.16(3)
_cell_angle_gamma                96.25(3)
_cell_volume                     494.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    145
_cell_measurement_theta_min      4.464
_cell_measurement_theta_max      23.490

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.108
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_process_details   
;
 SADABS (Bruker, 2001)
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;

_diffrn_reflns_number            5361
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.614
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2218
_reflns_number_gt                1572
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius, 1999)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg et al., 2003)
;
_computing_structure_solution    
;
SIR97 (Altomare et al., 1999)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 2012) and 
Mercury (Macrae et al., 2006)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'


_refine_special_details          
;
 Reflection 0 1 0 was omitted from refinement, because its
 experimental intensity was affected by large error due to 
 the beamstop.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+0.1189P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2218
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1380
_refine_ls_wR_factor_gt          0.1198
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5135(3) 0.2634(2) 0.00133(16) 0.0360(4) Uani 1 1 d . . . . .
C2 C 0.4166(4) 0.1128(2) -0.09136(17) 0.0432(4) Uani 1 1 d . . . . .
H2 H 0.269796 0.052789 -0.081357 0.052 Uiso 1 1 calc R U . . .
C3 C 0.7395(4) 0.1449(3) -0.20156(18) 0.0512(5) Uani 1 1 d . . . . .
H3 H 0.825602 0.106223 -0.271060 0.061 Uiso 1 1 calc R U . . .
C4 C 0.8338(4) 0.2944(3) -0.11103(18) 0.0466(5) Uani 1 1 d . . . . .
H4 H 0.980169 0.354398 -0.121485 0.056 Uiso 1 1 calc R U . . .
C5 C 0.3919(3) 0.3248(2) 0.11421(16) 0.0367(4) Uani 1 1 d . . . . .
C6 C 0.3148(3) 0.4792(2) 0.30039(16) 0.0400(4) Uani 1 1 d . . . . .
C7 C 0.6043(4) 0.6768(2) 0.36800(17) 0.0453(5) Uani 1 1 d . . . . .
C8 C 0.7618(5) 0.8309(3) 0.4530(2) 0.0636(6) Uani 1 1 d . . . . .
H8A H 0.931673 0.829589 0.432892 0.095 Uiso 1 1 calc R U . . .
H8B H 0.754223 0.834023 0.536850 0.095 Uiso 1 1 calc R U . . .
H8C H 0.700906 0.928590 0.443980 0.095 Uiso 1 1 calc R U . . .
N1 N 0.1840(3) 0.2512(2) 0.13811(14) 0.0439(4) Uani 1 1 d . . . . .
N2 N 0.1361(3) 0.3470(2) 0.25365(15) 0.0469(4) Uani 1 1 d . . . . .
H2N H -0.005(4) 0.315(3) 0.288(2) 0.056 Uiso 1 1 d . U . . .
N3 N 0.3865(3) 0.6121(2) 0.40076(14) 0.0457(4) Uani 1 1 d . . . . .
N4 N 0.6705(3) 0.5967(2) 0.25673(14) 0.0437(4) Uani 1 1 d . . . . .
N5 N 0.4765(3) 0.46712(18) 0.21365(13) 0.0375(4) Uani 1 1 d . . . . .
N6 N 0.7211(3) 0.3554(2) -0.00872(14) 0.0417(4) Uani 1 1 d . . . . .
N7 N 0.5288(3) 0.0532(2) -0.19347(15) 0.0494(4) Uani 1 1 d . . . . .
O1 O 0.2608(3) -0.2525(2) -0.35458(16) 0.0695(5) Uani 1 1 d . . . . .
H1O H 0.364(6) -0.161(4) -0.314(3) 0.083 Uiso 1 1 d . U . . .
H2O H 0.286(5) -0.294(4) -0.433(3) 0.083 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N6 1.330(2) . ?
C1 C2 1.394(3) . ?
C1 C5 1.453(2) . ?
C2 N7 1.326(2) . ?
C2 H2 0.9300 . ?
C3 N7 1.335(3) . ?
C3 C4 1.373(3) . ?
C3 H3 0.9300 . ?
C4 N6 1.331(3) . ?
C4 H4 0.9300 . ?
C5 N1 1.314(2) . ?
C5 N5 1.375(2) . ?
C6 N3 1.324(2) . ?
C6 N2 1.339(2) . ?
C6 N5 1.349(2) . ?
C7 N4 1.326(2) . ?
C7 N3 1.370(2) . ?
C7 C8 1.489(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 N2 1.366(2) . ?
N2 H2N 0.93(2) . ?
N4 N5 1.375(2) . ?
O1 H1O 0.88(3) . ?
O1 H2O 0.88(3) . ?

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
N6 C1 C2 121.80(17) . . ?
N6 C1 C5 117.37(15) . . ?
C2 C1 C5 120.83(16) . . ?
N7 C2 C1 121.52(17) . . ?
N7 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
N7 C3 C4 122.41(18) . . ?
N7 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
N6 C4 C3 121.68(18) . . ?
N6 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
N1 C5 N5 108.98(15) . . ?
N1 C5 C1 125.21(16) . . ?
N5 C5 C1 125.81(16) . . ?
N3 C6 N2 141.99(17) . . ?
N3 C6 N5 111.50(16) . . ?
N2 C6 N5 106.50(16) . . ?
N4 C7 N3 117.32(17) . . ?
N4 C7 C8 120.83(18) . . ?
N3 C7 C8 121.85(18) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 N1 N2 106.70(15) . . ?
C6 N2 N1 109.99(15) . . ?
C6 N2 H2N 130.1(14) . . ?
N1 N2 H2N 119.9(14) . . ?
C6 N3 C7 100.79(15) . . ?
C7 N4 N5 100.50(15) . . ?
C6 N5 C5 107.83(15) . . ?
C6 N5 N4 109.89(14) . . ?
C5 N5 N4 142.23(15) . . ?
C1 N6 C4 116.39(16) . . ?
C2 N7 C3 116.18(16) . . ?
H1O O1 H2O 113(3) . . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 C1 C2 N7 0.8(3) . . . . ?
C5 C1 C2 N7 -178.31(17) . . . . ?
N7 C3 C4 N6 0.9(3) . . . . ?
N6 C1 C5 N1 178.75(17) . . . . ?
C2 C1 C5 N1 -2.1(3) . . . . ?
N6 C1 C5 N5 -2.2(3) . . . . ?
C2 C1 C5 N5 176.98(17) . . . . ?
N5 C5 N1 N2 -0.2(2) . . . . ?
C1 C5 N1 N2 179.04(17) . . . . ?
N3 C6 N2 N1 -178.3(3) . . . . ?
N5 C6 N2 N1 0.1(2) . . . . ?
C5 N1 N2 C6 0.0(2) . . . . ?
N2 C6 N3 C7 177.6(3) . . . . ?
N5 C6 N3 C7 -0.8(2) . . . . ?
N4 C7 N3 C6 0.6(2) . . . . ?
C8 C7 N3 C6 -179.5(2) . . . . ?
N3 C7 N4 N5 -0.2(2) . . . . ?
C8 C7 N4 N5 179.9(2) . . . . ?
N3 C6 N5 C5 178.70(16) . . . . ?
N2 C6 N5 C5 -0.2(2) . . . . ?
N3 C6 N5 N4 0.7(2) . . . . ?
N2 C6 N5 N4 -178.18(15) . . . . ?
N1 C5 N5 C6 0.3(2) . . . . ?
C1 C5 N5 C6 -178.94(17) . . . . ?
N1 C5 N5 N4 177.1(2) . . . . ?
C1 C5 N5 N4 -2.1(4) . . . . ?
C7 N4 N5 C6 -0.3(2) . . . . ?
C7 N4 N5 C5 -177.1(2) . . . . ?
C2 C1 N6 C4 -1.2(3) . . . . ?
C5 C1 N6 C4 177.93(17) . . . . ?
C3 C4 N6 C1 0.4(3) . . . . ?
C1 C2 N7 C3 0.5(3) . . . . ?
C4 C3 N7 C2 -1.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4 N4 0.93 2.60 3.440(3) 151.1 2_765
N2 H2N O1 0.93(2) 1.74(3) 2.668(2) 178(2) 2
O1 H1O N7 0.88(3) 1.97(3) 2.827(3) 166(3) .
O1 H2O N3 0.88(3) 1.95(3) 2.820(3) 172(3) 1_544

_refine_diff_density_max         0.215
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.044


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol-water'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2016575'
loop_
_audit_author_name
_audit_author_address
'Roberto Centore'
;University of Naples Federico II
Italy
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
'Sodium 4-Methyl-7-(2-pyrazinyl)-[1,2,4]triazolo[3,2-c][1,2,4]-triazolate'
_chemical_formula_moiety         '(Na)+, (C8 H6 N7)-, 3(H2O)'
_chemical_formula_sum            'C8 H12 N7 Na O3'
_chemical_formula_weight         277.24

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'
Na Na 0.0362 0.0249 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8520(9)
_cell_length_b                   9.1940(17)
_cell_length_c                   10.1550(16)
_cell_angle_alpha                72.687(18)
_cell_angle_beta                 81.788(18)
_cell_angle_gamma                86.177(14)
_cell_volume                     604.29(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    196
_cell_measurement_theta_min      3.787
_cell_measurement_theta_max      23.359

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.149
_shelx_estimated_absorpt_T_min   0.957
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   
;
 SADABS (Bruker, 2001)
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;


_diffrn_reflns_number            7679
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.647
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2748
_reflns_number_gt                2123
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius, 1999)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg et al., 2003)
;
_computing_structure_solution    
;
SIR97 (Altomare et al., 1999)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 2012) and 
Mercury (Macrae et al., 2006)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0423P)²+0.1971P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2748
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0997
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7611(2) 0.07398(17) 0.56119(15) 0.0234(3) Uani 1 1 d . . . . .
C2 C 0.7614(3) 0.07461(19) 0.69844(17) 0.0301(4) Uani 1 1 d . . . . .
H2 H 0.738860 -0.015900 0.769495 0.036 Uiso 1 1 calc R U . . .
C3 C 0.8244(3) 0.32587(19) 0.62475(18) 0.0313(4) Uani 1 1 d . . . . .
H3 H 0.847707 0.416216 0.642684 0.038 Uiso 1 1 calc R U . . .
C4 C 0.8235(3) 0.32605(18) 0.48879(18) 0.0311(4) Uani 1 1 d . . . . .
H4 H 0.845700 0.416958 0.418183 0.037 Uiso 1 1 calc R U . . .
C5 C 0.7290(2) -0.06643(17) 0.53130(15) 0.0240(3) Uani 1 1 d . . . . .
C6 C 0.7020(2) -0.23732(17) 0.42515(16) 0.0248(3) Uani 1 1 d . . . . .
C7 C 0.7372(2) -0.12686(18) 0.21064(16) 0.0270(3) Uani 1 1 d . . . . .
C8 C 0.7520(3) -0.1024(2) 0.05838(18) 0.0414(5) Uani 1 1 d . . . . .
H8A H 0.776879 0.002931 0.010387 0.062 Uiso 1 1 calc R U . . .
H8B H 0.630475 -0.129589 0.036138 0.062 Uiso 1 1 calc R U . . .
H8C H 0.858091 -0.164658 0.030135 0.062 Uiso 1 1 calc R U . . .
N1 N 0.6961(2) -0.20020(15) 0.62613(14) 0.0298(3) Uani 1 1 d . . . . .
N2 N 0.6786(2) -0.31053(15) 0.56162(14) 0.0304(3) Uani 1 1 d . . . . .
N3 N 0.7050(2) -0.26636(15) 0.30233(14) 0.0286(3) Uani 1 1 d . . . . .
N4 N 0.7554(2) -0.01092(15) 0.26238(13) 0.0261(3) Uani 1 1 d . . . . .
N5 N 0.73313(19) -0.08730(14) 0.40325(13) 0.0229(3) Uani 1 1 d . . . . .
N6 N 0.7922(2) 0.20092(15) 0.45479(13) 0.0270(3) Uani 1 1 d . . . . .
N7 N 0.7926(2) 0.19969(16) 0.73109(15) 0.0320(3) Uani 1 1 d . . . . .
Na1 Na 0.75240(11) 0.27278(7) 0.19353(7) 0.0349(2) Uani 1 1 d . . . . .
O1 O 0.7040(3) 0.33606(17) -0.04056(14) 0.0471(4) Uani 1 1 d . . . . .
H1A H 0.745(4) 0.285(3) -0.090(3) 0.057 Uiso 1 1 d . U . . .
H1B H 0.609(4) 0.388(3) -0.079(3) 0.057 Uiso 1 1 d . U . . .
O2 O 1.0723(3) 0.3638(2) 0.14959(18) 0.0578(4) Uani 1 1 d . . . . .
H2A H 1.152(4) 0.318(3) 0.204(3) 0.069 Uiso 1 1 d . U . . .
H2B H 1.114(4) 0.455(3) 0.110(3) 0.069 Uiso 1 1 d . U . . .
O3 O 0.5685(2) 0.49570(14) 0.21741(13) 0.0325(3) Uani 1 1 d . . . . .
H3A H 0.616(3) 0.563(3) 0.242(2) 0.039 Uiso 1 1 d . U . . .
H3B H 0.488(3) 0.452(2) 0.290(2) 0.039 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N6 1.339(2) . ?
C1 C2 1.396(2) . ?
C1 C5 1.448(2) . ?
C2 N7 1.326(2) . ?
C2 H2 0.9300 . ?
C3 N7 1.334(2) . ?
C3 C4 1.381(2) . ?
C3 H3 0.9300 . ?
C4 N6 1.334(2) . ?
C4 H4 0.9300 . ?
C5 N1 1.327(2) . ?
C5 N5 1.3660(19) . ?
C6 N2 1.340(2) . ?
C6 N3 1.348(2) . ?
C6 N5 1.3566(19) . ?
C7 N4 1.341(2) . ?
C7 N3 1.352(2) . ?
C7 C8 1.484(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 N2 1.3809(19) . ?
N4 N5 1.3845(17) . ?
N4 Na1 2.4909(15) . ?
N6 Na1 2.5864(15) . ?
Na1 O2 2.3340(18) . ?
Na1 O1 2.3400(15) . ?
Na1 O3 2.3898(15) . ?
Na1 H3B 2.65(2) . ?
O1 H1A 0.79(3) . ?
O1 H1B 0.85(2) . ?
O2 H2A 0.83(3) . ?
O2 H2B 0.86(3) . ?
O3 H3A 0.83(2) . ?
O3 H3B 0.86(2) . ?

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
N6 C1 C2 121.43(14) . . ?
N6 C1 C5 118.56(13) . . ?
C2 C1 C5 120.01(14) . . ?
N7 C2 C1 122.32(15) . . ?
N7 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
N7 C3 C4 121.84(15) . . ?
N7 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
N6 C4 C3 122.57(15) . . ?
N6 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
N1 C5 N5 107.85(13) . . ?
N1 C5 C1 125.03(13) . . ?
N5 C5 C1 127.09(13) . . ?
N2 C6 N3 139.71(14) . . ?
N2 C6 N5 110.43(14) . . ?
N3 C6 N5 109.85(13) . . ?
N4 C7 N3 117.49(14) . . ?
N4 C7 C8 121.04(15) . . ?
N3 C7 C8 121.47(15) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 N1 N2 109.86(13) . . ?
C6 N2 N1 105.21(12) . . ?
C6 N3 C7 101.94(12) . . ?
C7 N4 N5 100.09(12) . . ?
C7 N4 Na1 141.20(10) . . ?
N5 N4 Na1 117.40(9) . . ?
C6 N5 C5 106.65(12) . . ?
C6 N5 N4 110.61(12) . . ?
C5 N5 N4 142.73(13) . . ?
C4 N6 C1 115.75(13) . . ?
C4 N6 Na1 109.67(10) . . ?
C1 N6 Na1 133.78(10) . . ?
C2 N7 C3 116.09(14) . . ?
O2 Na1 O1 95.31(7) . . ?
O2 Na1 O3 100.14(6) . . ?
O1 Na1 O3 90.53(6) . . ?
O2 Na1 N4 111.08(6) . . ?
O1 Na1 N4 101.90(6) . . ?
O3 Na1 N4 144.85(6) . . ?
O2 Na1 N6 86.76(6) . . ?
O1 Na1 N6 177.89(6) . . ?
O3 Na1 N6 88.69(5) . . ?
N4 Na1 N6 77.69(5) . . ?
O2 Na1 H3B 113.2(5) . . ?
O1 Na1 H3B 102.1(5) . . ?
O3 Na1 H3B 18.8(5) . . ?
N4 Na1 H3B 126.6(5) . . ?
N6 Na1 H3B 76.7(5) . . ?
Na1 O1 H1A 123.2(18) . . ?
Na1 O1 H1B 128.0(17) . . ?
H1A O1 H1B 104(2) . . ?
Na1 O2 H2A 117.3(19) . . ?
Na1 O2 H2B 130.0(18) . . ?
H2A O2 H2B 108(3) . . ?
Na1 O3 H3A 122.5(14) . . ?
Na1 O3 H3B 97.7(14) . . ?
H3A O3 H3B 102.6(19) . . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 C1 C2 N7 -0.2(3) . . . . ?
C5 C1 C2 N7 179.12(15) . . . . ?
N7 C3 C4 N6 -0.4(3) . . . . ?
N6 C1 C5 N1 -179.88(15) . . . . ?
C2 C1 C5 N1 0.8(2) . . . . ?
N6 C1 C5 N5 2.5(2) . . . . ?
C2 C1 C5 N5 -176.84(15) . . . . ?
N5 C5 N1 N2 0.08(18) . . . . ?
C1 C5 N1 N2 -177.96(14) . . . . ?
N3 C6 N2 N1 179.70(19) . . . . ?
N5 C6 N2 N1 0.02(17) . . . . ?
C5 N1 N2 C6 -0.06(17) . . . . ?
N2 C6 N3 C7 179.8(2) . . . . ?
N5 C6 N3 C7 -0.54(17) . . . . ?
N4 C7 N3 C6 0.08(19) . . . . ?
C8 C7 N3 C6 -179.95(16) . . . . ?
N3 C7 N4 N5 0.38(18) . . . . ?
C8 C7 N4 N5 -179.58(15) . . . . ?
N3 C7 N4 Na1 -164.92(12) . . . . ?
C8 C7 N4 Na1 15.1(3) . . . . ?
N2 C6 N5 C5 0.03(17) . . . . ?
N3 C6 N5 C5 -179.75(13) . . . . ?
N2 C6 N5 N4 -179.39(13) . . . . ?
N3 C6 N5 N4 0.83(17) . . . . ?
N1 C5 N5 C6 -0.07(17) . . . . ?
C1 C5 N5 C6 177.92(15) . . . . ?
N1 C5 N5 N4 179.03(18) . . . . ?
C1 C5 N5 N4 -3.0(3) . . . . ?
C7 N4 N5 C6 -0.70(16) . . . . ?
Na1 N4 N5 C6 168.98(10) . . . . ?
C7 N4 N5 C5 -179.78(19) . . . . ?
Na1 N4 N5 C5 -10.1(3) . . . . ?
C3 C4 N6 C1 0.1(2) . . . . ?
C3 C4 N6 Na1 171.23(13) . . . . ?
C2 C1 N6 C4 0.2(2) . . . . ?
C5 C1 N6 C4 -179.11(14) . . . . ?
C2 C1 N6 Na1 -168.27(12) . . . . ?
C5 C1 N6 Na1 12.4(2) . . . . ?
C1 C2 N7 C3 -0.1(2) . . . . ?
C4 C3 N7 C2 0.4(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C3 H3 N2 0.93 2.64 3.324(2) 130.5 1_565
O1 H1A N7 0.79(3) 2.17(3) 2.923(2) 160(2) 1_554
O1 H1B O3 0.85(2) 2.00(3) 2.8326(19) 164(2) 2_665
O2 H2A N1 0.83(3) 2.12(3) 2.940(2) 168(3) 2_756
O2 H2B O1 0.86(3) 2.24(3) 3.074(2) 164(2) 2_765
O3 H3A N3 0.83(2) 2.01(2) 2.8338(19) 174(2) 1_565

_refine_diff_density_max         0.244
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.043


_chemical_compound_source        
'Slow cooling to room temperature of a hot saturated NaOH water solution.'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2016574'
loop_
_audit_author_name
_audit_author_address
'Roberto Centore'
;University of Naples Federico II
Italy
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
"Bis([4-Methyl-7-(2-pyrazinyl)-3H-[1,2,4]triazolo[3,2-c][1,2,4]-triazole k²-N1,N6-k¹-N2'-triaquo-k¹-N7-pentabromodizincate]Zinc(II)) dihydrate"
_chemical_formula_moiety         'C16 H26 Br12 N14 O6 Zn6, 2(H2 O)'
_chemical_formula_sum            'C16 H30 Br12 N14 O8 Zn6'
_chemical_formula_weight         1897.68

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'
Br Br -0.2901 2.4595 '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'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.282(3)
_cell_length_b                   10.500(9)
_cell_length_c                   13.206(12)
_cell_angle_alpha                107.35(7)
_cell_angle_beta                 90.60(6)
_cell_angle_gamma                101.75(4)
_cell_volume                     1199.3(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    248
_cell_measurement_theta_min      2.362
_cell_measurement_theta_max      28.031

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.628
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    12.999
_shelx_estimated_absorpt_T_min   0.356
_shelx_estimated_absorpt_T_max   0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_T_max  0.490
_exptl_absorpt_process_details   
;
 SADABS (Bruker, 2001)
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;

_diffrn_reflns_number            15578
_diffrn_reflns_av_unetI/netI     0.1256
_diffrn_reflns_av_R_equivalents  0.1149
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.669
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5460
_reflns_number_gt                3230
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius, 1999)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg et al., 2003)
;
_computing_structure_solution    
;
SIR97 (Altomare et al., 1999)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 2012) and 
Mercury (Macrae et al., 2006)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+8.1912P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5460
_refine_ls_number_parameters     254
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1316
_refine_ls_wR_factor_gt          0.1082
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3723(11) 0.4395(10) 0.7044(7) 0.013(2) Uani 1 1 d . . . . .
C2 C 0.3493(12) 0.3898(11) 0.5947(7) 0.018(2) Uani 1 1 d . . . . .
H2 H 0.392438 0.316787 0.556354 0.021 Uiso 1 1 calc R U . . .
C3 C 0.2099(11) 0.5469(11) 0.5978(8) 0.018(2) Uani 1 1 d . . . . .
H3 H 0.150921 0.586389 0.561787 0.021 Uiso 1 1 calc R U . . .
C4 C 0.2345(12) 0.5991(11) 0.7085(8) 0.020(2) Uani 1 1 d . . . . .
H4 H 0.193843 0.674315 0.745821 0.024 Uiso 1 1 calc R U . . .
C5 C 0.4573(11) 0.3876(10) 0.7655(7) 0.015(2) Uani 1 1 d . . . . .
C6 C 0.6031(11) 0.2749(10) 0.8143(7) 0.013(2) Uani 1 1 d . . . . .
C7 C 0.6495(12) 0.1352(11) 0.6648(8) 0.019(2) Uani 1 1 d . . . . .
C8 C 0.7195(13) 0.0347(12) 0.5894(9) 0.024(2) Uani 1 1 d . . . . .
H8A H 0.654381 -0.010119 0.524132 0.037 Uiso 1 1 calc R U . . .
H8B H 0.736272 -0.034127 0.621929 0.037 Uiso 1 1 calc R U . . .
H8C H 0.814007 0.081715 0.572162 0.037 Uiso 1 1 calc R U . . .
Br1 Br 0.15290(14) 0.51385(13) 0.30783(9) 0.0298(3) Uani 1 1 d . . . . .
Br2 Br 0.42003(13) 0.25841(14) 0.32721(9) 0.0306(3) Uani 1 1 d . . . . .
Br3 Br -0.01031(12) 0.18880(11) 0.39600(8) 0.0208(2) Uani 1 1 d . . . . .
Br4 Br 0.12160(13) 0.01946(12) 0.12271(8) 0.0246(3) Uani 1 1 d . . . . .
Br5 Br -0.09047(16) -0.20130(12) 0.28697(10) 0.0369(3) Uani 1 1 d . . . . .
Br6 Br -0.31330(12) 0.00208(12) 0.15393(9) 0.0262(3) Uani 1 1 d . . . . .
N1 N 0.4861(9) 0.4333(8) 0.8711(6) 0.0112(16) Uani 1 1 d . . . . .
N2 N 0.5772(10) 0.3670(9) 0.9032(6) 0.0166(18) Uani 1 1 d . . . . .
N3 N 0.6804(10) 0.1767(9) 0.7748(6) 0.0185(19) Uani 1 1 d . . . . .
H3A H 0.737773 0.145760 0.810885 0.022 Uiso 1 1 calc R U . . .
N4 N 0.5570(10) 0.1965(9) 0.6336(7) 0.0190(19) Uani 1 1 d . . . . .
N5 N 0.5300(9) 0.2846(9) 0.7292(6) 0.0159(18) Uani 1 1 d . . . . .
N6 N 0.3140(9) 0.5450(9) 0.7624(6) 0.0142(17) Uani 1 1 d . . . . .
N7 N 0.2664(10) 0.4440(9) 0.5418(6) 0.0183(19) Uani 1 1 d . . . . .
Zn1 Zn 0.36574(13) 0.59748(12) 0.93682(9) 0.0147(3) Uani 1 1 d . . . . .
Zn2 Zn 0.21204(14) 0.34834(13) 0.37883(9) 0.0190(3) Uani 1 1 d . . . . .
Zn3 Zn -0.08077(14) -0.00709(13) 0.22850(9) 0.0198(3) Uani 1 1 d . . . . .
O1 O 0.1673(9) 0.4576(8) 0.9334(6) 0.0257(18) Uani 1 1 d . . . . .
H1A H 0.125454 0.410496 0.963134 0.031 Uiso 1 1 d R U . . .
H1B H 0.147054 0.410896 0.864233 0.031 Uiso 1 1 d R U . . .
O2 O 0.2453(8) 0.7487(8) 0.9740(5) 0.0228(17) Uani 1 1 d . . . . .
H2A H 0.181200 0.774659 1.012165 0.027 Uiso 1 1 d R U . . .
H2B H 0.263194 0.813985 0.940563 0.027 Uiso 1 1 d R U . . .
O3 O 0.5511(9) 0.7466(8) 0.9251(6) 0.0267(18) Uani 1 1 d . . . . .
H3B H 0.572835 0.770422 0.872487 0.032 Uiso 1 1 d R U . . .
H3C H 0.587133 0.814799 0.986185 0.032 Uiso 1 1 d R U . . .
O4 O 0.0556(9) 0.3043(8) 0.0649(6) 0.0309(19) Uani 1 1 d . . . . .
H4A H 0.078797 0.242462 0.080596 0.037 Uiso 1 1 d R U . . .
H4B H 0.082446 0.362046 0.131934 0.037 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N6 1.361(12) . ?
C1 C2 1.384(13) . ?
C1 C5 1.412(14) . ?
C2 N7 1.344(13) . ?
C2 H2 0.9500 . ?
C3 N7 1.324(14) . ?
C3 C4 1.397(14) . ?
C3 H3 0.9500 . ?
C4 N6 1.333(13) . ?
C4 H4 0.9500 . ?
C5 N1 1.337(11) . ?
C5 N5 1.360(12) . ?
C6 N2 1.340(12) . ?
C6 N5 1.346(12) . ?
C6 N3 1.355(13) . ?
C7 N4 1.303(13) . ?
C7 N3 1.394(12) . ?
C7 C8 1.481(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Br1 Zn2 2.356(2) . ?
Br2 Zn2 2.339(2) . ?
Br3 Zn2 2.438(2) . ?
Br3 Zn3 2.502(3) . ?
Br4 Zn3 2.373(2) . ?
Br5 Zn3 2.372(3) . ?
Br6 Zn3 2.395(2) . ?
N1 N2 1.337(11) . ?
N1 Zn1 2.210(8) . ?
N2 Zn1 2.076(8) 2_667 ?
N3 H3A 0.8800 . ?
N4 N5 1.384(11) . ?
N6 Zn1 2.225(8) . ?
N7 Zn2 2.092(8) . ?
Zn1 O2 2.070(8) . ?
Zn1 O1 2.100(8) . ?
Zn1 O3 2.118(8) . ?
O1 H1A 0.7683 . ?
O1 H1B 0.8953 . ?
O2 H2A 0.8196 . ?
O2 H2B 0.9099 . ?
O3 H3B 0.8202 . ?
O3 H3C 0.9100 . ?
O4 H4A 0.8043 . ?
O4 H4B 0.9100 . ?

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
N6 C1 C2 121.7(9) . . ?
N6 C1 C5 114.4(8) . . ?
C2 C1 C5 123.8(9) . . ?
N7 C2 C1 120.6(10) . . ?
N7 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
N7 C3 C4 121.8(9) . . ?
N7 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
N6 C4 C3 121.1(10) . . ?
N6 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
N1 C5 N5 106.1(8) . . ?
N1 C5 C1 126.5(9) . . ?
N5 C5 C1 127.4(9) . . ?
N2 C6 N5 110.3(8) . . ?
N2 C6 N3 144.2(9) . . ?
N5 C6 N3 105.5(8) . . ?
N4 C7 N3 113.9(9) . . ?
N4 C7 C8 122.6(9) . . ?
N3 C7 C8 123.4(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Zn2 Br3 Zn3 111.08(9) . . ?
N2 N1 C5 111.5(8) . . ?
N2 N1 Zn1 140.2(6) . . ?
C5 N1 Zn1 108.3(6) . . ?
N1 N2 C6 105.1(8) . . ?
N1 N2 Zn1 121.9(6) . 2_667 ?
C6 N2 Zn1 132.7(7) . 2_667 ?
C6 N3 C7 105.4(8) . . ?
C6 N3 H3A 127.3 . . ?
C7 N3 H3A 127.3 . . ?
C7 N4 N5 101.7(8) . . ?
C6 N5 C5 107.1(8) . . ?
C6 N5 N4 113.5(8) . . ?
C5 N5 N4 139.2(8) . . ?
C4 N6 C1 116.8(8) . . ?
C4 N6 Zn1 130.0(7) . . ?
C1 N6 Zn1 113.1(6) . . ?
C3 N7 C2 117.9(8) . . ?
C3 N7 Zn2 122.8(7) . . ?
C2 N7 Zn2 118.8(7) . . ?
O2 Zn1 N2 91.1(3) . 2_667 ?
O2 Zn1 O1 87.2(3) . . ?
N2 Zn1 O1 94.6(3) 2_667 . ?
O2 Zn1 O3 88.4(3) . . ?
N2 Zn1 O3 91.8(3) 2_667 . ?
O1 Zn1 O3 172.3(3) . . ?
O2 Zn1 N1 171.1(3) . . ?
N2 Zn1 N1 97.8(3) 2_667 . ?
O1 Zn1 N1 92.7(3) . . ?
O3 Zn1 N1 90.6(3) . . ?
O2 Zn1 N6 93.6(3) . . ?
N2 Zn1 N6 175.2(3) 2_667 . ?
O1 Zn1 N6 85.3(3) . . ?
O3 Zn1 N6 88.7(3) . . ?
N1 Zn1 N6 77.5(3) . . ?
N7 Zn2 Br2 101.4(3) . . ?
N7 Zn2 Br1 106.9(3) . . ?
Br2 Zn2 Br1 119.90(8) . . ?
N7 Zn2 Br3 96.6(3) . . ?
Br2 Zn2 Br3 117.03(8) . . ?
Br1 Zn2 Br3 110.93(8) . . ?
Br5 Zn3 Br4 110.39(8) . . ?
Br5 Zn3 Br6 113.46(8) . . ?
Br4 Zn3 Br6 115.61(8) . . ?
Br5 Zn3 Br3 103.32(9) . . ?
Br4 Zn3 Br3 104.37(8) . . ?
Br6 Zn3 Br3 108.52(9) . . ?
Zn1 O1 H1A 143.4 . . ?
Zn1 O1 H1B 103.6 . . ?
H1A O1 H1B 105.3 . . ?
Zn1 O2 H2A 141.6 . . ?
Zn1 O2 H2B 118.2 . . ?
H2A O2 H2B 100.2 . . ?
Zn1 O3 H3B 126.9 . . ?
Zn1 O3 H3C 116.4 . . ?
H3B O3 H3C 111.3 . . ?
H4A O4 H4B 91.5 . . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 C1 C2 N7 -0.8(16) . . . . ?
C5 C1 C2 N7 179.7(10) . . . . ?
N7 C3 C4 N6 -1.4(17) . . . . ?
N6 C1 C5 N1 -1.2(15) . . . . ?
C2 C1 C5 N1 178.3(10) . . . . ?
N6 C1 C5 N5 -179.0(10) . . . . ?
C2 C1 C5 N5 0.6(17) . . . . ?
N5 C5 N1 N2 1.9(11) . . . . ?
C1 C5 N1 N2 -176.3(10) . . . . ?
N5 C5 N1 Zn1 -178.3(6) . . . . ?
C1 C5 N1 Zn1 3.6(13) . . . . ?
C5 N1 N2 C6 -1.3(11) . . . . ?
Zn1 N1 N2 C6 178.9(8) . . . . ?
C5 N1 N2 Zn1 -175.8(7) . . . 2_667 ?
Zn1 N1 N2 Zn1 4.4(14) . . . 2_667 ?
N5 C6 N2 N1 0.2(11) . . . . ?
N3 C6 N2 N1 176.4(15) . . . . ?
N5 C6 N2 Zn1 173.8(7) . . . 2_667 ?
N3 C6 N2 Zn1 -10(2) . . . 2_667 ?
N2 C6 N3 C7 -175.0(15) . . . . ?
N5 C6 N3 C7 1.3(11) . . . . ?
N4 C7 N3 C6 -1.8(12) . . . . ?
C8 C7 N3 C6 175.9(11) . . . . ?
N3 C7 N4 N5 1.4(12) . . . . ?
C8 C7 N4 N5 -176.3(10) . . . . ?
N2 C6 N5 C5 0.9(12) . . . . ?
N3 C6 N5 C5 -176.8(9) . . . . ?
N2 C6 N5 N4 177.2(8) . . . . ?
N3 C6 N5 N4 -0.5(12) . . . . ?
N1 C5 N5 C6 -1.6(11) . . . . ?
C1 C5 N5 C6 176.5(10) . . . . ?
N1 C5 N5 N4 -176.4(11) . . . . ?
C1 C5 N5 N4 2(2) . . . . ?
C7 N4 N5 C6 -0.5(12) . . . . ?
C7 N4 N5 C5 174.0(13) . . . . ?
C3 C4 N6 C1 1.5(15) . . . . ?
C3 C4 N6 Zn1 -177.2(8) . . . . ?
C2 C1 N6 C4 -0.5(15) . . . . ?
C5 C1 N6 C4 179.1(9) . . . . ?
C2 C1 N6 Zn1 178.5(8) . . . . ?
C5 C1 N6 Zn1 -2.0(11) . . . . ?
C4 C3 N7 C2 0.1(15) . . . . ?
C4 C3 N7 Zn2 172.6(8) . . . . ?
C1 C2 N7 C3 0.9(15) . . . . ?
C1 C2 N7 Zn2 -171.9(8) . . . . ?

_refine_diff_density_max         1.210
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.268


_exptl_crystal_recrystallization_method 
'Slow evaporation of a water/ethanol solution.'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2016573'
loop_
_audit_author_name
_audit_author_address
'Roberto Centore'
;University of Naples Federico II
Italy
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
'4-Methyl-7-(2-pyrazinyl)-2H-3H-7H[1,2,4]triazolo[3,2-c][1,2,4]-triazolium tetrachlorozincate'
_chemical_formula_moiety         '2(C8 H9 N7)2+, 2(Zn1 Cl4)2-'
_chemical_formula_sum            'C16 H18 Cl8 N14 Zn2'
_chemical_formula_weight         820.78

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'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   8.7870(17)
_cell_length_b                   16.250(4)
_cell_length_c                   41.341(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5903(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    135
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      25.78

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.387
_shelx_estimated_absorpt_T_min   0.449
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_process_details   
;
 SADABS (Bruker, 2001)
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;

_diffrn_reflns_number            48632
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         2.370
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6987
_reflns_number_gt                5297
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius, 1999)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg et al., 2003)
;
_computing_structure_solution    
;
SIR97 (Altomare et al., 1999)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 2012) and 
Mercury (Macrae et al., 2006)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'

_refine_special_details          
;
 The tetrachlorozincate anions lie in special position on 
 crystallographic mirror planes. There two independent 
 organic cations and four independent half anions. Each anion 
 is disordered over two positions, both lying on mirror planes.
 The split positions were refined with some constraints: the 
 same anisotropic displacement parameter was assumed for 
 correspondent atoms of the split positions, while coordinates 
 were refined without constraints. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0456P)²+34.4475P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6987
_refine_ls_number_parameters     420
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.1768
_refine_ls_wR_factor_gt          0.1662
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.1106(7) -0.0454(4) 0.18335(13) 0.0345(12) Uani 1 1 d . . . . .
C2A C 0.0115(8) -0.0901(4) 0.16381(15) 0.0432(15) Uani 1 1 d . . . . .
H2A H 0.024957 -0.093268 0.141532 0.052 Uiso 1 1 calc R U . . .
C3A C -0.1218(8) -0.1288(4) 0.21017(18) 0.0518(17) Uani 1 1 d . . . . .
H3A H -0.202582 -0.156568 0.219770 0.062 Uiso 1 1 calc R U . . .
C4A C -0.0190(7) -0.0876(4) 0.22795(17) 0.0461(15) Uani 1 1 d . . . . .
H4A H -0.029127 -0.088894 0.250332 0.055 Uiso 1 1 calc R U . . .
C5A C 0.2303(6) 0.0032(3) 0.16843(14) 0.0338(12) Uani 1 1 d . . . . .
C6A C 0.4270(7) 0.0836(4) 0.16316(14) 0.0351(13) Uani 1 1 d . . . . .
C7A C 0.5232(7) 0.0968(4) 0.21144(15) 0.0381(13) Uani 1 1 d . . . . .
C8A C 0.6212(9) 0.1262(5) 0.23678(18) 0.062(2) Uani 1 1 d . . . . .
H8A1 H 0.562098 0.136546 0.255879 0.092 Uiso 1 1 calc R U . . .
H8A2 H 0.669658 0.176220 0.229954 0.092 Uiso 1 1 calc R U . . .
H8A3 H 0.697299 0.085481 0.241413 0.092 Uiso 1 1 calc R U . . .
C1B C 0.5934(7) -0.0480(4) 0.06758(14) 0.0364(13) Uani 1 1 d . . . . .
C2B C 0.5014(8) -0.093000 0.08854(15) 0.0435(15) Uani 1 1 d . . . . .
H2B H 0.522745 -0.096523 0.110527 0.052 Uiso 1 1 calc R U . . .
C3B C 0.3537(8) -0.1316(5) 0.04425(19) 0.0545(18) Uani 1 1 d . . . . .
H3B H 0.269959 -0.159250 0.035831 0.065 Uiso 1 1 calc R U . . .
C4B C 0.4520(7) -0.0906(4) 0.02485(18) 0.0479(16) Uani 1 1 d . . . . .
H4B H 0.435993 -0.092684 0.002624 0.057 Uiso 1 1 calc R U . . .
C5B C 0.7162(7) 0.0020(4) 0.08060(14) 0.0366(13) Uani 1 1 d . . . . .
C6B C 0.9142(7) 0.0816(4) 0.08347(14) 0.0377(13) Uani 1 1 d . . . . .
C7B C 0.9994(8) 0.0952(4) 0.03442(16) 0.0449(15) Uani 1 1 d . . . . .
C8B C 1.0948(10) 0.1250(5) 0.00860(19) 0.067(2) Uani 1 1 d . . . . .
H8B1 H 1.050666 0.110217 -0.011832 0.101 Uiso 1 1 calc R U . . .
H8B2 H 1.194095 0.100851 0.010418 0.101 Uiso 1 1 calc R U . . .
H8B3 H 1.103025 0.183802 0.010020 0.101 Uiso 1 1 calc R U . . .
N1A N 0.2373(6) 0.0188(4) 0.13780(12) 0.0432(13) Uani 1 1 d . . . . .
N2A N 0.3646(6) 0.0699(4) 0.13461(13) 0.0481(14) Uani 1 1 d . . . . .
H2A1 H 0.397382 0.089708 0.116620 0.058 Uiso 1 1 calc R U . . .
N3A N 0.5438(6) 0.1175(3) 0.17841(12) 0.0402(12) Uani 1 1 d . . . . .
H3NA H 0.637723 0.142741 0.173292 0.048 Uiso 1 1 d R U . . .
N4A N 0.4029(5) 0.0505(3) 0.21566(11) 0.0339(11) Uani 1 1 d . . . . .
N5A N 0.3446(5) 0.0428(3) 0.18500(11) 0.0331(10) Uani 1 1 d . . . . .
N6A N 0.0972(6) -0.0449(3) 0.21546(12) 0.0386(11) Uani 1 1 d . . . . .
N7A N -0.1032(7) -0.1282(4) 0.17850(14) 0.0518(15) Uani 1 1 d . . . . .
H7A H -0.168676 -0.153702 0.166748 0.062 Uiso 1 1 calc R U . . .
N1B N 0.7319(6) 0.0169(4) 0.11134(12) 0.0467(13) Uani 1 1 d . . . . .
N2B N 0.8595(7) 0.0674(4) 0.11279(13) 0.0523(15) Uani 1 1 d . . . . .
H2B1 H 0.897657 0.086836 0.130362 0.063 Uiso 1 1 calc R U . . .
N3B N 1.0275(6) 0.1159(3) 0.06712(13) 0.0459(13) Uani 1 1 d . . . . .
H3NB H 1.111665 0.140293 0.074935 0.055 Uiso 1 1 d R U . . .
N4B N 0.8766(6) 0.0501(3) 0.03139(11) 0.0370(11) Uani 1 1 d . . . . .
N5B N 0.8256(6) 0.0422(3) 0.06274(11) 0.0360(11) Uani 1 1 d . . . . .
N6B N 0.5697(6) -0.0477(3) 0.03573(12) 0.0379(11) Uani 1 1 d . . . . .
N7B N 0.3818(7) -0.1307(4) 0.07562(14) 0.0519(14) Uani 1 1 d . . . . .
H7B H 0.319545 -0.155736 0.088312 0.062 Uiso 1 1 calc R U . . .
Zn1 Zn 0.3871(3) -0.250000 0.17979(5) 0.0299(4) Uani 0.885(8) 2 d S T P A 1
Cl1 Cl 0.2189(4) -0.250000 0.22160(9) 0.0464(8) Uani 0.885(8) 2 d S T P A 1
Cl2 Cl 0.2531(4) -0.250000 0.13127(7) 0.0422(7) Uani 0.885(8) 2 d S T P A 1
Cl3 Cl 0.5200(3) -0.13001(15) 0.18053(7) 0.0416(5) Uani 0.885(8) 1 d . . P A 1
Zn1B Zn 0.4315(18) -0.250000 0.1794(5) 0.0299(4) Uani 0.115(8) 2 d S T P A 2
Cl1B Cl 0.201(4) -0.250000 0.2088(7) 0.0464(8) Uani 0.115(8) 2 d S T P A 2
Cl2B Cl 0.328(3) -0.250000 0.1273(6) 0.0422(7) Uani 0.115(8) 2 d S T P A 2
Cl3B Cl 0.569(2) -0.1359(14) 0.1836(6) 0.0416(5) Uani 0.115(8) 1 d . . P A 2
Zn2 Zn 0.0647(2) 0.250000 0.17089(4) 0.0312(3) Uani 0.919(5) 2 d S T P B 3
Cl4 Cl 0.2767(3) 0.250000 0.20079(8) 0.0386(6) Uani 0.919(5) 2 d S T P B 3
Cl5 Cl 0.1315(4) 0.250000 0.11782(6) 0.0469(7) Uani 0.919(5) 2 d S T P B 3
Cl6 Cl -0.0798(3) 0.13557(12) 0.18085(5) 0.0373(4) Uani 0.919(5) 1 d . . P B 3
Zn2B Zn 0.113(2) 0.250000 0.1712(6) 0.0312(3) Uani 0.081(5) 2 d S T P B 4
Cl4B Cl 0.245(3) 0.250000 0.2158(9) 0.0386(6) Uani 0.081(5) 2 d S T P B 4
Cl5B Cl 0.235(4) 0.250000 0.1205(7) 0.0469(7) Uani 0.081(5) 2 d S T P B 4
Cl6B Cl -0.027(3) 0.1327(16) 0.1739(6) 0.0373(4) Uani 0.081(5) 1 d . . P B 4
Zn3 Zn 0.5491(3) 0.250000 0.07026(4) 0.0313(4) Uani 0.894(9) 2 d S T P C 5
Cl7 Cl 0.6371(5) 0.250000 0.12260(7) 0.0461(8) Uani 0.894(9) 2 d S T P C 5
Cl8 Cl 0.7377(4) 0.250000 0.03243(10) 0.0466(8) Uani 0.894(9) 2 d S T P C 5
Cl9 Cl 0.4061(4) 0.13339(12) 0.06406(6) 0.0348(5) Uani 0.894(9) 1 d . . P C 5
Zn3B Zn 0.599(2) 0.250000 0.0718(4) 0.0313(4) Uani 0.106(9) 2 d S T P C 6
Cl7B Cl 0.710(4) 0.250000 0.1195(7) 0.0461(8) Uani 0.106(9) 2 d S T P C 6
Cl8B Cl 0.777(3) 0.250000 0.0456(8) 0.0466(8) Uani 0.106(9) 2 d S T P C 6
Cl9B Cl 0.459(3) 0.1309(12) 0.0698(5) 0.0348(5) Uani 0.106(9) 1 d . . P C 6
Zn4 Zn 0.87026(19) -0.250000 0.07947(4) 0.0306(3) Uani 0.902(5) 2 d S T P D 7
Cl10 Cl 0.7477(3) -0.250000 0.12856(6) 0.0407(6) Uani 0.902(5) 2 d S T P D 7
Cl11 Cl 0.6818(3) -0.250000 0.04360(7) 0.0365(6) Uani 0.902(5) 2 d S T P D 7
Cl12 Cl 1.0088(2) -0.13200(11) 0.07751(5) 0.0377(5) Uani 0.902(5) 1 d . . P D 7
Zn4B Zn 0.9175(18) -0.250000 0.0746(4) 0.0306(3) Uani 0.098(5) 2 d S T P D 8
Cl13 Cl 0.840(3) -0.250000 0.1294(5) 0.0407(6) Uani 0.098(5) 2 d S T P D 8
Cl14 Cl 0.718(3) -0.250000 0.0341(7) 0.0365(6) Uani 0.098(5) 2 d S T P D 8
Cl15 Cl 1.062(2) -0.1356(12) 0.0669(5) 0.0377(5) Uani 0.098(5) 1 d . . P D 8


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1A N6A 1.333(7) . ?
C1A C2A 1.393(8) . ?
C1A C5A 1.453(8) . ?
C2A N7A 1.329(9) . ?
C2A H2A 0.9300 . ?
C3A N7A 1.320(9) . ?
C3A C4A 1.343(9) . ?
C3A H3A 0.9300 . ?
C4A N6A 1.338(8) . ?
C4A H4A 0.9300 . ?
C5A N1A 1.293(7) . ?
C5A N5A 1.375(7) . ?
C6A N2A 1.320(8) . ?
C6A N3A 1.325(8) . ?
C6A N5A 1.334(7) . ?
C7A N4A 1.308(7) . ?
C7A N3A 1.418(8) . ?
C7A C8A 1.438(9) . ?
C8A H8A1 0.9600 . ?
C8A H8A2 0.9600 . ?
C8A H8A3 0.9600 . ?
C1B N6B 1.333(7) . ?
C1B C2B 1.393(8) . ?
C1B C5B 1.454(8) . ?
C2B N7B 1.329(8) . ?
C2B H2B 0.9300 . ?
C3B N7B 1.320(9) . ?
C3B C4B 1.353(10) . ?
C3B H3B 0.9300 . ?
C4B N6B 1.326(8) . ?
C4B H4B 0.9300 . ?
C5B N1B 1.301(8) . ?
C5B N5B 1.377(7) . ?
C6B N5B 1.323(8) . ?
C6B N2B 1.324(8) . ?
C6B N3B 1.327(8) . ?
C7B N4B 1.311(8) . ?
C7B N3B 1.415(8) . ?
C7B C8B 1.441(9) . ?
C8B H8B1 0.9600 . ?
C8B H8B2 0.9600 . ?
C8B H8B3 0.9600 . ?
N1A N2A 1.400(7) . ?
N2A H2A1 0.8600 . ?
N3A H3NA 0.9454 . ?
N4A N5A 1.373(6) . ?
N7A H7A 0.8600 . ?
N1B N2B 1.391(8) . ?
N2B H2B1 0.8600 . ?
N3B H3NB 0.8986 . ?
N4B N5B 1.377(6) . ?
N7B H7B 0.8600 . ?
Zn1 Cl3 2.273(2) . ?
Zn1 Cl3 2.273(2) 8 ?
Zn1 Cl1 2.274(3) . ?
Zn1 Cl2 2.326(3) . ?
Zn1B Cl3B 2.22(2) 8 ?
Zn1B Cl3B 2.22(2) . ?
Zn1B Cl2B 2.34(3) . ?
Zn1B Cl1B 2.36(3) . ?
Zn2 Cl4 2.236(3) . ?
Zn2 Cl5 2.271(3) . ?
Zn2 Cl6 2.2890(18) 8_565 ?
Zn2 Cl6 2.2890(19) . ?
Zn2B Cl4B 2.18(4) . ?
Zn2B Cl6B 2.27(3) . ?
Zn2B Cl6B 2.27(3) 8_565 ?
Zn2B Cl5B 2.36(4) . ?
Zn3 Cl8 2.278(4) . ?
Zn3 Cl9 2.2878(19) 8_565 ?
Zn3 Cl9 2.2878(19) . ?
Zn3 Cl7 2.298(3) . ?
Zn3B Cl8B 1.90(3) . ?
Zn3B Cl7B 2.20(3) . ?
Zn3B Cl9B 2.29(2) . ?
Zn3B Cl9B 2.29(2) 8_565 ?
Zn4 Cl11 2.223(3) . ?
Zn4 Cl12 2.2726(18) 8 ?
Zn4 Cl12 2.2726(18) . ?
Zn4 Cl10 2.298(3) . ?
Zn4B Cl15 2.273(19) . ?
Zn4B Cl15 2.273(19) 8 ?
Zn4B Cl13 2.36(3) . ?
Zn4B Cl14 2.43(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
N6A C1A C2A 121.7(6) . . ?
N6A C1A C5A 118.9(5) . . ?
C2A C1A C5A 119.3(5) . . ?
N7A C2A C1A 116.9(6) . . ?
N7A C2A H2A 121.6 . . ?
C1A C2A H2A 121.6 . . ?
N7A C3A C4A 117.1(6) . . ?
N7A C3A H3A 121.5 . . ?
C4A C3A H3A 121.5 . . ?
N6A C4A C3A 124.1(7) . . ?
N6A C4A H4A 117.9 . . ?
C3A C4A H4A 117.9 . . ?
N1A C5A N5A 111.2(5) . . ?
N1A C5A C1A 123.8(5) . . ?
N5A C5A C1A 124.8(5) . . ?
N2A C6A N3A 144.8(6) . . ?
N2A C6A N5A 107.2(5) . . ?
N3A C6A N5A 107.8(5) . . ?
N4A C7A N3A 111.6(5) . . ?
N4A C7A C8A 125.3(6) . . ?
N3A C7A C8A 123.1(6) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
N6B C1B C2B 121.7(6) . . ?
N6B C1B C5B 118.7(5) . . ?
C2B C1B C5B 119.6(6) . . ?
N7B C2B C1B 116.8(6) . . ?
N7B C2B H2B 121.6 . . ?
C1B C2B H2B 121.6 . . ?
N7B C3B C4B 117.3(7) . . ?
N7B C3B H3B 121.4 . . ?
C4B C3B H3B 121.4 . . ?
N6B C4B C3B 123.7(7) . . ?
N6B C4B H4B 118.1 . . ?
C3B C4B H4B 118.1 . . ?
N1B C5B N5B 111.2(5) . . ?
N1B C5B C1B 123.0(5) . . ?
N5B C5B C1B 125.8(5) . . ?
N5B C6B N2B 107.1(5) . . ?
N5B C6B N3B 108.4(5) . . ?
N2B C6B N3B 144.3(6) . . ?
N4B C7B N3B 111.6(6) . . ?
N4B C7B C8B 126.6(6) . . ?
N3B C7B C8B 121.8(6) . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C5A N1A N2A 104.3(5) . . ?
C6A N2A N1A 110.3(5) . . ?
C6A N2A H2A1 124.8 . . ?
N1A N2A H2A1 124.8 . . ?
C6A N3A C7A 105.1(5) . . ?
C6A N3A H3NA 138.6 . . ?
C7A N3A H3NA 115.5 . . ?
C7A N4A N5A 103.3(5) . . ?
C6A N5A N4A 112.1(5) . . ?
C6A N5A C5A 106.9(5) . . ?
N4A N5A C5A 140.8(5) . . ?
C1A N6A C4A 116.7(5) . . ?
C3A N7A C2A 123.4(6) . . ?
C3A N7A H7A 118.3 . . ?
C2A N7A H7A 118.3 . . ?
C5B N1B N2B 103.7(5) . . ?
C6B N2B N1B 110.8(5) . . ?
C6B N2B H2B1 124.6 . . ?
N1B N2B H2B1 124.6 . . ?
C6B N3B C7B 104.8(5) . . ?
C6B N3B H3NB 128.3 . . ?
C7B N3B H3NB 126.3 . . ?
C7B N4B N5B 103.3(5) . . ?
C6B N5B C5B 107.0(5) . . ?
C6B N5B N4B 111.9(5) . . ?
C5B N5B N4B 140.9(5) . . ?
C4B N6B C1B 117.1(6) . . ?
C3B N7B C2B 123.2(6) . . ?
C3B N7B H7B 118.4 . . ?
C2B N7B H7B 118.4 . . ?
Cl3 Zn1 Cl3 118.15(10) . 8 ?
Cl3 Zn1 Cl1 108.89(9) . . ?
Cl3 Zn1 Cl1 108.88(9) 8 . ?
Cl3 Zn1 Cl2 105.76(9) . . ?
Cl3 Zn1 Cl2 105.77(9) 8 . ?
Cl1 Zn1 Cl2 109.05(15) . . ?
Cl3B Zn1B Cl3B 113.1(11) 8 . ?
Cl3B Zn1B Cl2B 106.5(9) 8 . ?
Cl3B Zn1B Cl2B 106.5(9) . . ?
Cl3B Zn1B Cl1B 115.4(8) 8 . ?
Cl3B Zn1B Cl1B 115.4(8) . . ?
Cl2B Zn1B Cl1B 98.1(10) . . ?
Cl4 Zn2 Cl5 108.59(14) . . ?
Cl4 Zn2 Cl6 111.27(7) . . ?
Cl5 Zn2 Cl6 108.49(8) . . ?
Cl6 Zn2 Cl6 108.65(11) 8_565 . ?
Cl4B Zn2B Cl6B 104.3(10) . . ?
Cl4B Zn2B Cl5B 120.7(15) . . ?
Cl6B Zn2B Cl5B 106.8(10) . . ?
Cl6B Zn2B Cl5B 106.8(10) 8_565 . ?
Cl8 Zn3 Cl9 108.81(8) . . ?
Cl9 Zn3 Cl9 111.84(10) 8_565 . ?
Cl8 Zn3 Cl7 113.68(13) . . ?
Cl9 Zn3 Cl7 106.87(8) 8_565 . ?
Cl9 Zn3 Cl7 106.87(8) . . ?
Cl8B Zn3B Cl7B 98.3(14) . . ?
Cl8B Zn3B Cl9B 114.9(8) . . ?
Cl7B Zn3B Cl9B 105.6(8) . . ?
Cl11 Zn4 Cl12 112.04(6) . . ?
Cl12 Zn4 Cl12 115.07(10) 8 . ?
Cl11 Zn4 Cl10 103.88(10) . . ?
Cl12 Zn4 Cl10 106.41(7) 8 . ?
Cl12 Zn4 Cl10 106.41(7) . . ?
Cl15 Zn4B Cl15 109.7(11) . 8 ?
Cl15 Zn4B Cl13 107.2(7) . . ?
Cl15 Zn4B Cl13 107.2(7) 8 . ?
Cl15 Zn4B Cl14 107.9(7) . . ?
Cl15 Zn4B Cl14 107.9(7) 8 . ?
Cl13 Zn4B Cl14 116.9(10) . . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6A C1A C2A N7A 4.2(9) . . . . ?
C5A C1A C2A N7A -174.8(6) . . . . ?
N7A C3A C4A N6A 1.8(11) . . . . ?
N6A C1A C5A N1A -167.3(6) . . . . ?
C2A C1A C5A N1A 11.6(9) . . . . ?
N6A C1A C5A N5A 8.3(9) . . . . ?
C2A C1A C5A N5A -172.7(6) . . . . ?
N6B C1B C2B N7B -5.0(8) . . . . ?
C5B C1B C2B N7B 173.3(5) . . . . ?
N7B C3B C4B N6B -2.6(11) . . . . ?
N6B C1B C5B N1B 167.9(6) . . . . ?
C2B C1B C5B N1B -10.4(9) . . . . ?
N6B C1B C5B N5B -9.3(9) . . . . ?
C2B C1B C5B N5B 172.4(5) . . . . ?
N5A C5A N1A N2A 1.0(7) . . . . ?
C1A C5A N1A N2A 177.2(5) . . . . ?
N3A C6A N2A N1A 174.0(8) . . . . ?
N5A C6A N2A N1A 0.0(7) . . . . ?
C5A N1A N2A C6A -0.7(7) . . . . ?
N2A C6A N3A C7A -176.0(9) . . . . ?
N5A C6A N3A C7A -2.1(6) . . . . ?
N4A C7A N3A C6A 2.0(7) . . . . ?
C8A C7A N3A C6A -176.0(6) . . . . ?
N3A C7A N4A N5A -1.0(6) . . . . ?
C8A C7A N4A N5A 177.0(6) . . . . ?
N2A C6A N5A N4A 177.9(5) . . . . ?
N3A C6A N5A N4A 1.6(7) . . . . ?
N2A C6A N5A C5A 0.6(6) . . . . ?
N3A C6A N5A C5A -175.8(5) . . . . ?
C7A N4A N5A C6A -0.3(6) . . . . ?
C7A N4A N5A C5A 175.7(7) . . . . ?
N1A C5A N5A C6A -1.0(7) . . . . ?
C1A C5A N5A C6A -177.2(5) . . . . ?
N1A C5A N5A N4A -177.2(6) . . . . ?
C1A C5A N5A N4A 6.7(11) . . . . ?
C2A C1A N6A C4A -1.8(9) . . . . ?
C5A C1A N6A C4A 177.1(6) . . . . ?
C3A C4A N6A C1A -1.2(10) . . . . ?
C4A C3A N7A C2A 0.8(11) . . . . ?
C1A C2A N7A C3A -3.6(10) . . . . ?
N5B C5B N1B N2B -1.3(7) . . . . ?
C1B C5B N1B N2B -178.8(5) . . . . ?
N5B C6B N2B N1B 0.4(7) . . . . ?
N3B C6B N2B N1B -174.1(9) . . . . ?
C5B N1B N2B C6B 0.6(7) . . . . ?
N5B C6B N3B C7B 0.9(7) . . . . ?
N2B C6B N3B C7B 175.3(9) . . . . ?
N4B C7B N3B C6B -0.6(7) . . . . ?
C8B C7B N3B C6B 176.9(7) . . . . ?
N3B C7B N4B N5B 0.1(7) . . . . ?
C8B C7B N4B N5B -177.2(7) . . . . ?
N2B C6B N5B C5B -1.1(7) . . . . ?
N3B C6B N5B C5B 175.5(5) . . . . ?
N2B C6B N5B N4B -177.5(5) . . . . ?
N3B C6B N5B N4B -0.9(7) . . . . ?
N1B C5B N5B C6B 1.6(7) . . . . ?
C1B C5B N5B C6B 179.1(6) . . . . ?
N1B C5B N5B N4B 176.2(7) . . . . ?
C1B C5B N5B N4B -6.4(11) . . . . ?
C7B N4B N5B C6B 0.4(7) . . . . ?
C7B N4B N5B C5B -174.0(7) . . . . ?
C3B C4B N6B C1B 2.2(10) . . . . ?
C2B C1B N6B C4B 1.7(8) . . . . ?
C5B C1B N6B C4B -176.6(6) . . . . ?
C4B C3B N7B C2B -1.1(10) . . . . ?
C1B C2B N7B C3B 4.7(9) . . . . ?

_refine_diff_density_max         1.131
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.123


_exptl_crystal_recrystallization_method 
'Slow cooling to room temperature of a hot solution in water/HCl (37 %)l'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2016576'
loop_
_audit_author_name
_audit_author_address
'Roberto Centore'
;University of Naples Federico II
Italy
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
'4-Methyl-7-(2-pyrazinyl)-2H-3H-7H[1,2,4]triazolo[3,2-c][1,2,4]-triazolium hexachlorostannate dihydrate'
_chemical_formula_moiety         '(C8 H9 N7)2+, (Sn1 Cl6)2-, 2(H2 O)'
_chemical_formula_sum            'C8 H13 Cl6 N7 O2 Sn'
_chemical_formula_weight         570.64

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'
Sn Sn -0.6537 1.4246 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   12.1370(19)
_cell_length_b                   15.2500(11)
_cell_length_c                   10.851(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2008.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    345
_cell_measurement_theta_min      2.691
_cell_measurement_theta_max      30.693

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.087
_shelx_estimated_absorpt_T_min   0.489
_shelx_estimated_absorpt_T_max   0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_process_details   
;
 SADABS (Bruker, 2001)
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;

_diffrn_reflns_number            8930
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.155
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4002
_reflns_number_gt                3640
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius, 1999)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg et al., 2003)
;
_computing_structure_solution    
;
SIR97 (Altomare et al., 1999)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 2012),  
Mercury (Macrae et al., 2006), and 
VESTA (Momma & Izumi, 2014)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'


_refine_special_details          
;
 Refined as a 2-component inversion twin.
 One of the two water molecules is disordered over 
 two sites. The split positions were refined with sum of 
 occupation factors equal to 1 (21 and -21) and with some 
 restraints on the anisotropic displacement parameters of the 
 split O atoms. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0084P)²+1.5974P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.29(3)
_refine_ls_number_reflns         4002
_refine_ls_number_parameters     229
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0550
_refine_ls_wR_factor_gt          0.0514
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2435(3) 0.3161(3) 0.1421(5) 0.0218(10) Uani 1 1 d . . . . .
C2 C 0.2996(4) 0.3601(3) 0.0495(5) 0.0271(12) Uani 1 1 d . . . . .
H2 H 0.377602 0.364942 0.049991 0.033 Uiso 1 1 calc R U . . .
C3 C 0.1291(4) 0.3857(4) -0.0446(6) 0.0411(15) Uani 1 1 d . . . . .
H3 H 0.087551 0.408066 -0.111856 0.049 Uiso 1 1 calc R U . . .
C4 C 0.0784(4) 0.3426(4) 0.0511(5) 0.0381(14) Uani 1 1 d . . . . .
H4 H 0.000490 0.337014 0.050453 0.046 Uiso 1 1 calc R U . . .
C5 C 0.3070(3) 0.2758(3) 0.2396(4) 0.0218(11) Uani 1 1 d . . . . .
C6 C 0.3551(4) 0.2086(3) 0.4083(5) 0.0246(11) Uani 1 1 d . . . . .
C7 C 0.2049(4) 0.1807(3) 0.5054(5) 0.0292(11) Uani 1 1 d . . . . .
C8 C 0.1309(5) 0.1488(5) 0.6045(7) 0.0464(16) Uani 1 1 d . . . . .
H8A H 0.142803 0.183719 0.679193 0.070 Uiso 1 1 calc R U . . .
H8B H 0.146978 0.087090 0.621860 0.070 Uiso 1 1 calc R U . . .
H8C H 0.054068 0.154701 0.578015 0.070 Uiso 1 1 calc R U . . .
N1 N 0.4154(3) 0.2705(2) 0.2371(4) 0.0252(10) Uani 1 1 d . . . . .
N2 N 0.4442(3) 0.2290(3) 0.3424(4) 0.0262(9) Uani 1 1 d . . . . .
H2A H 0.512295 0.216971 0.364444 0.031 Uiso 1 1 calc R U . . .
N3 N 0.3176(3) 0.1689(2) 0.5093(5) 0.0258(9) Uani 1 1 d . . . . .
H3A H 0.356180 0.141262 0.565941 0.031 Uiso 1 1 calc R U . . .
N4 N 0.1711(3) 0.2209(3) 0.4077(4) 0.0241(9) Uani 1 1 d . . . . .
N5 N 0.2687(3) 0.2381(2) 0.3453(4) 0.0190(8) Uani 1 1 d . . . . .
N6 N 0.1352(3) 0.3080(3) 0.1457(4) 0.0263(9) Uani 1 1 d . . . . .
N7 N 0.2391(3) 0.3953(3) -0.0402(4) 0.0361(11) Uani 1 1 d . . . . .
H7 H 0.272190 0.425805 -0.098315 0.043 Uiso 1 1 calc R U . . .
O1 O 0.3917(3) 0.5017(3) -0.1246(4) 0.0499(12) Uani 1 1 d . . . . .
H1A H 0.461464 0.492691 -0.108867 0.060 Uiso 1 1 d R U . . .
H1B H 0.396340 0.525895 -0.197821 0.060 Uiso 1 1 d R U . . .
Sn1 Sn 0.24878(3) 0.51004(2) 0.52238(8) 0.01867(8) Uani 1 1 d . . . . .
Cl1 Cl 0.41355(9) 0.57908(8) 0.60162(13) 0.0321(3) Uani 1 1 d . . . . .
Cl2 Cl 0.34403(10) 0.47267(9) 0.33462(12) 0.0335(3) Uani 1 1 d . . . . .
Cl3 Cl 0.08017(9) 0.44650(7) 0.43819(12) 0.0289(3) Uani 1 1 d . . . . .
Cl4 Cl 0.14904(9) 0.54654(8) 0.71102(11) 0.0264(3) Uani 1 1 d . . . . .
Cl5 Cl 0.19644(10) 0.65029(7) 0.43114(12) 0.0287(3) Uani 1 1 d . . . . .
Cl6 Cl 0.29922(11) 0.37233(8) 0.61597(14) 0.0354(3) Uani 1 1 d . . . . .
O2A O 0.0662(10) 0.5947(10) 0.1866(8) 0.047(4) Uani 0.48(2) 1 d . U P A 1
H20B H 0.089864 0.561792 0.251188 0.056 Uiso 0.48(2) 1 d R U P A 1
H21A H 0.008862 0.560415 0.181318 0.056 Uiso 0.48(2) 1 d R U P A 1
O2B O 0.1024(8) 0.5455(9) 0.1640(9) 0.042(3) Uani 0.52(2) 1 d . U P A 2
H30B H 0.092227 0.558264 0.251215 0.050 Uiso 0.52(2) 1 d R U P A 2
H31B H 0.161265 0.508196 0.184739 0.050 Uiso 0.52(2) 1 d R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N6 1.320(6) . ?
C1 C2 1.387(7) . ?
C1 C5 1.445(7) . ?
C2 N7 1.332(7) . ?
C2 H2 0.9500 . ?
C3 N7 1.345(7) . ?
C3 C4 1.375(8) . ?
C3 H3 0.9500 . ?
C4 N6 1.344(6) . ?
C4 H4 0.9500 . ?
C5 N1 1.319(5) . ?
C5 N5 1.364(6) . ?
C6 N5 1.331(6) . ?
C6 N2 1.332(6) . ?
C6 N3 1.332(7) . ?
C7 N4 1.292(6) . ?
C7 N3 1.381(6) . ?
C7 C8 1.483(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N1 N2 1.353(6) . ?
N2 H2A 0.8800 . ?
N3 H3A 0.8800 . ?
N4 N5 1.390(5) . ?
N7 H7 0.8800 . ?
O1 H1A 0.8753 . ?
O1 H1B 0.8773 . ?
Sn1 Cl2 2.4108(16) . ?
Sn1 Cl6 2.4117(13) . ?
Sn1 Cl1 2.4182(12) . ?
Sn1 Cl5 2.4409(12) . ?
Sn1 Cl3 2.4416(12) . ?
Sn1 Cl4 2.4424(15) . ?
O2A H20B 0.9086 . ?
O2A H21A 0.8721 . ?
O2B H30B 0.9739 . ?
O2B H31B 0.9403 . ?

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
N6 C1 C2 123.7(4) . . ?
N6 C1 C5 118.0(4) . . ?
C2 C1 C5 118.3(4) . . ?
N7 C2 C1 117.0(5) . . ?
N7 C2 H2 121.5 . . ?
C1 C2 H2 121.5 . . ?
N7 C3 C4 118.0(5) . . ?
N7 C3 H3 121.0 . . ?
C4 C3 H3 121.0 . . ?
N6 C4 C3 122.4(5) . . ?
N6 C4 H4 118.8 . . ?
C3 C4 H4 118.8 . . ?
N1 C5 N5 109.4(4) . . ?
N1 C5 C1 122.9(4) . . ?
N5 C5 C1 127.7(4) . . ?
N5 C6 N2 106.6(4) . . ?
N5 C6 N3 107.9(4) . . ?
N2 C6 N3 145.5(4) . . ?
N4 C7 N3 113.7(4) . . ?
N4 C7 C8 124.0(5) . . ?
N3 C7 C8 122.3(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 N1 N2 105.6(4) . . ?
C6 N2 N1 110.7(4) . . ?
C6 N2 H2A 124.6 . . ?
N1 N2 H2A 124.6 . . ?
C6 N3 C7 104.7(4) . . ?
C6 N3 H3A 127.6 . . ?
C7 N3 H3A 127.6 . . ?
C7 N4 N5 102.7(4) . . ?
C6 N5 C5 107.8(4) . . ?
C6 N5 N4 111.0(4) . . ?
C5 N5 N4 141.3(4) . . ?
C1 N6 C4 116.8(4) . . ?
C2 N7 C3 121.9(5) . . ?
C2 N7 H7 119.0 . . ?
C3 N7 H7 119.0 . . ?
H1A O1 H1B 100.4 . . ?
Cl2 Sn1 Cl6 91.62(5) . . ?
Cl2 Sn1 Cl1 90.39(5) . . ?
Cl6 Sn1 Cl1 91.11(5) . . ?
Cl2 Sn1 Cl5 89.38(5) . . ?
Cl6 Sn1 Cl5 178.99(7) . . ?
Cl1 Sn1 Cl5 88.74(4) . . ?
Cl2 Sn1 Cl3 89.54(5) . . ?
Cl6 Sn1 Cl3 91.42(4) . . ?
Cl1 Sn1 Cl3 177.47(5) . . ?
Cl5 Sn1 Cl3 88.73(4) . . ?
Cl2 Sn1 Cl4 178.88(5) . . ?
Cl6 Sn1 Cl4 88.36(6) . . ?
Cl1 Sn1 Cl4 90.72(5) . . ?
Cl5 Sn1 Cl4 90.65(4) . . ?
Cl3 Sn1 Cl4 89.35(5) . . ?
H20B O2A H21A 88.4 . . ?
H30B O2B H31B 89.1 . . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 C1 C2 N7 -0.3(8) . . . . ?
C5 C1 C2 N7 178.9(4) . . . . ?
N7 C3 C4 N6 -2.0(9) . . . . ?
N6 C1 C5 N1 171.4(4) . . . . ?
C2 C1 C5 N1 -7.9(7) . . . . ?
N6 C1 C5 N5 -8.5(7) . . . . ?
C2 C1 C5 N5 172.2(5) . . . . ?
N5 C5 N1 N2 0.1(5) . . . . ?
C1 C5 N1 N2 -179.8(4) . . . . ?
N5 C6 N2 N1 -0.6(5) . . . . ?
N3 C6 N2 N1 176.6(7) . . . . ?
C5 N1 N2 C6 0.3(5) . . . . ?
N5 C6 N3 C7 -3.0(5) . . . . ?
N2 C6 N3 C7 179.8(7) . . . . ?
N4 C7 N3 C6 2.8(6) . . . . ?
C8 C7 N3 C6 -177.7(5) . . . . ?
N3 C7 N4 N5 -1.3(5) . . . . ?
C8 C7 N4 N5 179.2(5) . . . . ?
N2 C6 N5 C5 0.6(5) . . . . ?
N3 C6 N5 C5 -177.7(4) . . . . ?
N2 C6 N5 N4 -179.3(4) . . . . ?
N3 C6 N5 N4 2.4(5) . . . . ?
N1 C5 N5 C6 -0.5(5) . . . . ?
C1 C5 N5 C6 179.4(4) . . . . ?
N1 C5 N5 N4 179.4(5) . . . . ?
C1 C5 N5 N4 -0.7(9) . . . . ?
C7 N4 N5 C6 -0.7(5) . . . . ?
C7 N4 N5 C5 179.5(6) . . . . ?
C2 C1 N6 C4 2.2(7) . . . . ?
C5 C1 N6 C4 -177.1(5) . . . . ?
C3 C4 N6 C1 -1.0(8) . . . . ?
C1 C2 N7 C3 -2.9(8) . . . . ?
C4 C3 N7 C2 4.0(9) . . . . ?

_refine_diff_density_max         0.410
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.080


_exptl_crystal_recrystallization_method 
'Slow evaporation of a solution containing water, ethanol and 10 drops of HCl 37 %.'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2016577'
loop_
_audit_author_name
_audit_author_address
'Roberto Centore'
;University of Naples Federico II
Italy
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
'4-Methyl-7-(2-pyrazinyl)-2H-3H[1,2,4]triazolo[3,2-c][1,2,4]-triazolium chloride'
_chemical_formula_moiety         '(C8 H8 N7)+, (Cl)-'
_chemical_formula_sum            'C8 H8 Cl N7'
_chemical_formula_weight         237.66

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   5.290(2)
_cell_length_b                   16.438(4)
_cell_length_c                   12.291(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.96(2)
_cell_angle_gamma                90
_cell_volume                     1016.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    185
_cell_measurement_theta_min      4.427
_cell_measurement_theta_max      22.461

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.359
_shelx_estimated_absorpt_T_min   0.870
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   
;
 SADABS (Bruker, 2001)
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;

_diffrn_reflns_number            10090
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.030
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2313
_reflns_number_gt                1472
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius, 1999)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg et al., 2003)
;
_computing_structure_solution    
;
SIR97 (Altomare et al., 1999)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 2012) and 
Mercury (Macrae et al., 2006)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0303P)²+0.5709P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2313
_refine_ls_number_parameters     152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0862
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5630(5) 0.13084(14) 0.44535(19) 0.0253(5) Uani 1 1 d . . . . .
C2 C 0.5685(5) 0.20215(15) 0.5069(2) 0.0315(6) Uani 1 1 d . . . . .
H2 H 0.418164 0.235040 0.488640 0.038 Uiso 1 1 calc R U . . .
C3 C 0.9893(6) 0.17432(16) 0.6127(2) 0.0364(6) Uani 1 1 d . . . . .
H3 H 1.144672 0.188380 0.669707 0.044 Uiso 1 1 calc R U . . .
C4 C 0.9831(5) 0.10245(16) 0.5544(2) 0.0358(6) Uani 1 1 d . . . . .
H4 H 1.131770 0.068840 0.574655 0.043 Uiso 1 1 calc R U . . .
C5 C 0.3271(5) 0.11042(14) 0.35090(18) 0.0271(5) Uani 1 1 d . . . . .
C6 C 0.0371(5) 0.04507(15) 0.21314(19) 0.0301(6) Uani 1 1 d . . . . .
C7 C 0.2127(5) -0.07070(15) 0.1978(2) 0.0313(6) Uani 1 1 d . . . . .
C8 C 0.2474(6) -0.15109(16) 0.1498(2) 0.0429(7) Uani 1 1 d . . . . .
H8A H 0.389430 -0.179975 0.203674 0.064 Uiso 1 1 calc R U . . .
H8B H 0.289280 -0.143613 0.079827 0.064 Uiso 1 1 calc R U . . .
H8C H 0.085863 -0.181799 0.134827 0.064 Uiso 1 1 calc R U . . .
N1 N 0.1272(5) 0.16008(13) 0.30833(17) 0.0360(5) Uani 1 1 d . . . . .
N2 N -0.0561(5) 0.11819(14) 0.22271(18) 0.0380(6) Uani 1 1 d . . . . .
H2N H -0.211(6) 0.1385(17) 0.178(2) 0.046 Uiso 1 1 d . U . . .
N3 N -0.0109(5) -0.02366(13) 0.15258(17) 0.0326(5) Uani 1 1 d . . . . .
H3N H -0.148(6) -0.0372(16) 0.091(2) 0.039 Uiso 1 1 d . U . . .
N4 N 0.3927(4) -0.03630(11) 0.28386(16) 0.0301(5) Uani 1 1 d . . . . .
N5 N 0.2742(4) 0.03750(11) 0.29255(15) 0.0260(5) Uani 1 1 d . . . . .
N6 N 0.7675(4) 0.07966(12) 0.46890(16) 0.0317(5) Uani 1 1 d . . . . .
N7 N 0.7822(5) 0.22455(12) 0.59075(18) 0.0360(5) Uani 1 1 d . . . . .
Cl1 Cl -0.61223(14) 0.10317(4) 0.05792(5) 0.0414(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N6 1.330(3) . ?
C1 C2 1.390(3) . ?
C1 C5 1.457(3) . ?
C2 N7 1.326(3) . ?
C2 H2 0.9300 . ?
C3 N7 1.332(3) . ?
C3 C4 1.377(4) . ?
C3 H3 0.9300 . ?
C4 N6 1.344(3) . ?
C4 H4 0.9300 . ?
C5 N1 1.310(3) . ?
C5 N5 1.380(3) . ?
C6 N2 1.318(3) . ?
C6 N3 1.334(3) . ?
C6 N5 1.337(3) . ?
C7 N4 1.313(3) . ?
C7 N3 1.379(3) . ?
C7 C8 1.481(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 N2 1.376(3) . ?
N2 H2N 0.90(3) . ?
N3 H3N 0.90(3) . ?
N4 N5 1.385(3) . ?

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
N6 C1 C2 122.4(2) . . ?
N6 C1 C5 117.8(2) . . ?
C2 C1 C5 119.8(2) . . ?
N7 C2 C1 121.8(2) . . ?
N7 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
N7 C3 C4 122.7(2) . . ?
N7 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
N6 C4 C3 121.6(2) . . ?
N6 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
N1 C5 N5 108.9(2) . . ?
N1 C5 C1 124.2(2) . . ?
N5 C5 C1 126.9(2) . . ?
N2 C6 N3 144.1(2) . . ?
N2 C6 N5 108.2(2) . . ?
N3 C6 N5 107.6(2) . . ?
N4 C7 N3 113.7(2) . . ?
N4 C7 C8 123.8(3) . . ?
N3 C7 C8 122.4(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 N1 N2 106.6(2) . . ?
C6 N2 N1 109.3(2) . . ?
C6 N2 H2N 125.3(18) . . ?
N1 N2 H2N 125.3(18) . . ?
C6 N3 C7 105.0(2) . . ?
C6 N3 H3N 130.0(17) . . ?
C7 N3 H3N 124.8(17) . . ?
C7 N4 N5 101.9(2) . . ?
C6 N5 C5 107.0(2) . . ?
C6 N5 N4 111.75(19) . . ?
C5 N5 N4 141.0(2) . . ?
C1 N6 C4 115.5(2) . . ?
C2 N7 C3 115.9(2) . . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 C1 C2 N7 2.1(4) . . . . ?
C5 C1 C2 N7 -177.6(2) . . . . ?
N7 C3 C4 N6 1.9(4) . . . . ?
N6 C1 C5 N1 -170.1(2) . . . . ?
C2 C1 C5 N1 9.5(4) . . . . ?
N6 C1 C5 N5 10.4(4) . . . . ?
C2 C1 C5 N5 -169.9(2) . . . . ?
N5 C5 N1 N2 0.6(3) . . . . ?
C1 C5 N1 N2 -179.0(2) . . . . ?
N3 C6 N2 N1 -175.7(3) . . . . ?
N5 C6 N2 N1 1.6(3) . . . . ?
C5 N1 N2 C6 -1.3(3) . . . . ?
N2 C6 N3 C7 175.4(4) . . . . ?
N5 C6 N3 C7 -1.9(3) . . . . ?
N4 C7 N3 C6 1.5(3) . . . . ?
C8 C7 N3 C6 -176.4(2) . . . . ?
N3 C7 N4 N5 -0.4(3) . . . . ?
C8 C7 N4 N5 177.4(2) . . . . ?
N2 C6 N5 C5 -1.2(3) . . . . ?
N3 C6 N5 C5 177.1(2) . . . . ?
N2 C6 N5 N4 -176.5(2) . . . . ?
N3 C6 N5 N4 1.8(3) . . . . ?
N1 C5 N5 C6 0.4(3) . . . . ?
C1 C5 N5 C6 179.9(2) . . . . ?
N1 C5 N5 N4 173.5(3) . . . . ?
C1 C5 N5 N4 -7.0(5) . . . . ?
C7 N4 N5 C6 -0.8(3) . . . . ?
C7 N4 N5 C5 -173.8(3) . . . . ?
C2 C1 N6 C4 -1.7(3) . . . . ?
C5 C1 N6 C4 178.0(2) . . . . ?
C3 C4 N6 C1 -0.2(4) . . . . ?
C1 C2 N7 C3 -0.4(4) . . . . ?
C4 C3 N7 C2 -1.5(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2 Cl1 0.93 2.81 3.452(3) 127.0 4_666
C4 H4 N4 0.93 2.63 3.462(4) 148.6 3_756
C4 H4 N6 0.93 2.59 3.319(3) 135.7 3_756
C8 H8B Cl1 0.96 2.83 3.729(3) 156.2 3
N2 H2N N7 0.90(3) 2.49(3) 3.031(3) 119(2) 4_465
N2 H2N Cl1 0.90(3) 2.25(3) 3.024(3) 143(2) .
N3 H3N Cl1 0.90(3) 2.17(3) 3.032(2) 160(2) 3_455

_refine_diff_density_max         0.258
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.068


_exptl_crystal_recrystallization_method 
'Slow cooling to room temperature of a solution containing water and few drops of HCl 1M.'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 2016578'
loop_
_audit_author_name
_audit_author_address
'Roberto Centore'
;University of Naples Federico II
Italy
;
_audit_update_record             
;
2020-07-15 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
"Bis([4-Methyl-7-(2-pyrazinyl)-3H-[1,2,4]triazolo[3,2-c][1,2,4]-triazole k²-N1,N6-k¹-N2']dichlorideZinc(II)) pentahydrate"
_chemical_formula_moiety         
'C16 H16.73 Cl2.64 Cu2 N14 O1.36, C16 H14 Cl4 Cu2 N14, 1.364(Cl)'
_chemical_formula_sum            'C32 H48 Cl8 Cu4 N28 O10'
_chemical_formula_weight         1522.78

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_space_group_crystal_system      triclinic

_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.745(2)
_cell_length_b                   11.371(3)
_cell_length_c                   12.811(2)
_cell_angle_alpha                71.003(12)
_cell_angle_beta                 76.242(15)
_cell_angle_gamma                73.412(16)
_cell_volume                     1400.2(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    245
_cell_measurement_theta_min      3.740
_cell_measurement_theta_max      27.151

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.958
_shelx_estimated_absorpt_T_min   0.508
_shelx_estimated_absorpt_T_max   0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_process_details   
;
 SADABS (Bruker, 2001)
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;

_diffrn_reflns_number            18414
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.093
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6353
_reflns_number_gt                4537
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius, 1999)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg et al., 2003)
;
_computing_structure_solution    
;
SIR97 (Altomare et al., 1999)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
Ortep-3 for Windows (Farrugia, 2012) and 
Mercury (Macrae et al., 2006)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'


_refine_special_details          
;
 In the coordination sphere of Cu1B one coordination position 
 is shared between a water molecule and a chloride ion. The two 
 split ligands were refined with SOF 21 for water and -21 for 
 chloride. Moreover, there is a nonncoordinated water molecule 
 (-21) and a noncoordinated chloride ion (-21). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+1.7643P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6353
_refine_ls_number_parameters     409
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0861
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.1207(3) 0.8678(3) 0.2812(3) 0.0235(7) Uani 1 1 d . . . . .
C2A C 0.1573(4) 0.8525(3) 0.3819(3) 0.0350(9) Uani 1 1 d . . . . .
H2A H 0.143745 0.923457 0.407681 0.042 Uiso 1 1 calc R U . . .
C3A C 0.2278(4) 0.6410(3) 0.4019(3) 0.0342(9) Uani 1 1 d . . . . .
H3A H 0.266359 0.559795 0.442402 0.041 Uiso 1 1 calc R U . . .
C4A C 0.1899(3) 0.6541(3) 0.3013(3) 0.0277(7) Uani 1 1 d . . . . .
H4A H 0.201874 0.582513 0.276876 0.033 Uiso 1 1 calc R U . . .
C5A C 0.0642(3) 0.9895(3) 0.2078(3) 0.0243(7) Uani 1 1 d . . . . .
C6A C -0.0145(3) 1.1878(3) 0.1286(3) 0.0254(7) Uani 1 1 d . . . . .
C7A C -0.0057(3) 1.2890(3) 0.2442(3) 0.0259(7) Uani 1 1 d . . . . .
C8A C -0.0213(4) 1.3965(4) 0.2907(3) 0.0376(9) Uani 1 1 d . . . . .
H8A1 H -0.112632 1.438728 0.301567 0.056 Uiso 1 1 calc R U . . .
H8A2 H 0.028274 1.455994 0.239604 0.056 Uiso 1 1 calc R U . . .
H8A3 H 0.010167 1.364644 0.361078 0.056 Uiso 1 1 calc R U . . .
N1A N 0.0320(3) 0.9964(2) 0.1128(2) 0.0246(6) Uani 1 1 d . . . . .
N2A N -0.0196(3) 1.1228(2) 0.0603(2) 0.0246(6) Uani 1 1 d . . . . .
N3A N -0.0417(3) 1.3055(3) 0.1428(2) 0.0272(6) Uani 1 1 d . . . . .
H3NA H -0.084(4) 1.372(4) 0.102(3) 0.033 Uiso 1 1 d . U . . .
N4A N 0.0422(3) 1.1697(3) 0.2944(2) 0.0297(7) Uani 1 1 d . . . . .
N5A N 0.0358(3) 1.1076(3) 0.2198(2) 0.0258(6) Uani 1 1 d . . . . .
N6A N 0.1367(3) 0.7688(3) 0.2403(2) 0.0237(6) Uani 1 1 d . . . . .
N7A N 0.2117(3) 0.7376(3) 0.4427(3) 0.0387(8) Uani 1 1 d . . . . .
Cl1A Cl -0.14711(10) 0.76125(9) 0.19737(8) 0.0378(2) Uani 1 1 d . . . . .
Cl2A Cl 0.18165(9) 0.62706(8) 0.06037(7) 0.0313(2) Uani 1 1 d . . . . .
Cu1A Cu 0.06896(4) 0.81528(4) 0.09168(3) 0.02433(11) Uani 1 1 d . . . . .
C1B C 0.6425(3) 0.2684(3) 0.2556(3) 0.0238(7) Uani 1 1 d . . . . .
C2B C 0.6943(4) 0.2127(3) 0.3535(3) 0.0315(8) Uani 1 1 d . . . . .
H2B H 0.694296 0.263669 0.397416 0.038 Uiso 1 1 calc R U . . .
C3B C 0.7418(4) 0.0195(3) 0.3209(3) 0.0398(10) Uani 1 1 d . . . . .
H3B H 0.773840 -0.068447 0.342683 0.048 Uiso 1 1 calc R U . . .
C4B C 0.6933(4) 0.0743(3) 0.2213(3) 0.0332(8) Uani 1 1 d . . . . .
H4B H 0.696507 0.023025 0.176623 0.040 Uiso 1 1 calc R U . . .
C5B C 0.5873(3) 0.4023(3) 0.2132(3) 0.0232(7) Uani 1 1 d . . . . .
C6B C 0.5200(3) 0.6072(3) 0.1828(3) 0.0231(7) Uani 1 1 d . . . . .
C7B C 0.5556(3) 0.6469(3) 0.3269(3) 0.0274(7) Uani 1 1 d . . . . .
C8B C 0.5586(4) 0.7214(4) 0.4012(3) 0.0363(9) Uani 1 1 d . . . . .
H8B1 H 0.575032 0.664581 0.473065 0.054 Uiso 1 1 calc R U . . .
H8B2 H 0.475512 0.780725 0.409553 0.054 Uiso 1 1 calc R U . . .
H8B3 H 0.627260 0.767339 0.369208 0.054 Uiso 1 1 calc R U . . .
N1B N 0.5440(3) 0.4493(2) 0.1165(2) 0.0236(6) Uani 1 1 d . . . . .
N2B N 0.4993(3) 0.5805(2) 0.0957(2) 0.0234(6) Uani 1 1 d . . . . .
N3B N 0.5085(3) 0.7033(3) 0.2273(2) 0.0269(6) Uani 1 1 d . . . . .
H3NB H 0.483(4) 0.775(4) 0.203(3) 0.032 Uiso 1 1 d . U . . .
N4B N 0.5960(3) 0.5222(3) 0.3493(2) 0.0288(7) Uani 1 1 d . . . . .
N5B N 0.5718(3) 0.5002(3) 0.2566(2) 0.0230(6) Uani 1 1 d . . . . .
N6B N 0.6419(3) 0.1989(3) 0.1881(2) 0.0271(6) Uani 1 1 d . . . . .
N7B N 0.7445(4) 0.0874(3) 0.3869(3) 0.0417(8) Uani 1 1 d . . . . .
Cl1B Cl 0.3224(8) 0.2655(7) 0.1338(8) 0.0254(12) Uani 0.318(3) 1 d . . P A 1
Cl3B Cl 0.31400(16) 0.33088(15) 0.35654(13) 0.0480(5) Uani 0.682(3) 1 d . . P A
1
Cl2B Cl 0.63102(11) 0.13520(8) -0.02360(8) 0.0417(2) Uani 1 1 d . . . . .
Cu1B Cu 0.56279(5) 0.30586(4) 0.04482(3) 0.02848(12) Uani 1 1 d . . . . .
O1W O 0.4325(5) 0.9645(4) 0.2050(4) 0.0813(14) Uani 1 1 d D . . . .
H1OA H 0.422(6) 0.995(6) 0.261(4) 0.098 Uiso 1 1 d D U . . .
H1OB H 0.353(4) 0.966(6) 0.206(5) 0.098 Uiso 1 1 d D U . . .
O2W O 0.8224(3) 0.5587(3) 0.0794(3) 0.0484(8) Uani 1 1 d D . . . .
H2OA H 0.831(5) 0.613(4) 0.107(4) 0.058 Uiso 1 1 d D U . . .
H2OB H 0.798(5) 0.594(4) 0.019(3) 0.058 Uiso 1 1 d D U . . .
O3W O 0.0887(4) 0.3797(4) 0.5407(3) 0.0814(12) Uani 1 1 d . . . . .
H3OA H 0.152841 0.365136 0.488359 0.098 Uiso 1 1 d R U . . .
H3OB H 0.113558 0.375884 0.600034 0.098 Uiso 1 1 d R U . . .
O4W O 0.4145(5) 1.0468(4) 0.3924(4) 0.1182(19) Uani 1 1 d . . . . .
H4OA H 0.369821 1.009754 0.453281 0.142 Uiso 1 1 d R U . . .
H4OB H 0.396945 1.118116 0.413920 0.142 Uiso 1 1 d R U . . .
O1B O 0.3389(10) 0.2951(8) 0.1212(10) 0.029(2) Uani 0.682(3) 1 d . . P A 2
H28 H 0.322022 0.269659 0.196358 0.035 Uiso 0.682(3) 1 d R U P A 2
H39 H 0.338081 0.233830 0.091491 0.035 Uiso 0.682(3) 1 d R U P A 2
O4B O 0.2613(7) 0.1484(7) 0.0399(7) 0.034(2) Uani 0.318(3) 1 d . U P A 2
H4BA H 0.303621 0.070001 0.049587 0.041 Uiso 0.318(3) 1 d R U P A 2
H4BB H 0.230395 0.170457 -0.021442 0.041 Uiso 0.318(3) 1 d R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1A N6A 1.342(4) . ?
C1A C2A 1.380(4) . ?
C1A C5A 1.453(4) . ?
C2A N7A 1.332(4) . ?
C2A H2A 0.9300 . ?
C3A N7A 1.316(5) . ?
C3A C4A 1.392(5) . ?
C3A H3A 0.9300 . ?
C4A N6A 1.328(4) . ?
C4A H4A 0.9300 . ?
C5A N1A 1.315(4) . ?
C5A N5A 1.341(4) . ?
C6A N2A 1.336(4) . ?
C6A N5A 1.347(4) . ?
C6A N3A 1.348(4) . ?
C7A N4A 1.307(4) . ?
C7A N3A 1.382(4) . ?
C7A C8A 1.480(5) . ?
C8A H8A1 0.9600 . ?
C8A H8A2 0.9600 . ?
C8A H8A3 0.9600 . ?
N1A N2A 1.385(4) . ?
N1A Cu1A 2.078(3) . ?
N2A Cu1A 1.988(3) 2_575 ?
N3A H3NA 0.84(4) . ?
N4A N5A 1.384(4) . ?
N6A Cu1A 2.054(3) . ?
Cl1A Cu1A 2.5256(12) . ?
Cl2A Cu1A 2.2485(10) . ?
C1B N6B 1.351(4) . ?
C1B C2B 1.378(4) . ?
C1B C5B 1.436(4) . ?
C2B N7B 1.333(5) . ?
C2B H2B 0.9300 . ?
C3B N7B 1.326(5) . ?
C3B C4B 1.378(5) . ?
C3B H3B 0.9300 . ?
C4B N6B 1.330(4) . ?
C4B H4B 0.9300 . ?
C5B N1B 1.318(4) . ?
C5B N5B 1.353(4) . ?
C6B N2B 1.328(4) . ?
C6B N5B 1.341(4) . ?
C6B N3B 1.352(4) . ?
C7B N4B 1.313(4) . ?
C7B N3B 1.373(4) . ?
C7B C8B 1.477(5) . ?
C8B H8B1 0.9600 . ?
C8B H8B2 0.9600 . ?
C8B H8B3 0.9600 . ?
N1B N2B 1.386(4) . ?
N1B Cu1B 2.060(3) . ?
N2B Cu1B 1.981(3) 2_665 ?
N3B H3NB 0.77(4) . ?
N4B N5B 1.384(4) . ?
N6B Cu1B 2.066(3) . ?
Cl1B Cu1B 2.668(8) . ?
Cl2B Cu1B 2.2497(11) . ?
Cu1B O1B 2.394(10) . ?
O1W H1OA 0.86(3) . ?
O1W H1OB 0.84(3) . ?
O2W H2OA 0.84(3) . ?
O2W H2OB 0.82(3) . ?
O3W H3OA 0.8599 . ?
O3W H3OB 0.8481 . ?
O4W H4OA 0.8597 . ?
O4W H4OB 0.8954 . ?
O1B H28 0.8996 . ?
O1B H39 0.8994 . ?
O4B H4BA 0.8600 . ?
O4B H4BB 0.8598 . ?

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
N6A C1A C2A 122.2(3) . . ?
N6A C1A C5A 112.9(3) . . ?
C2A C1A C5A 124.9(3) . . ?
N7A C2A C1A 121.0(3) . . ?
N7A C2A H2A 119.5 . . ?
C1A C2A H2A 119.5 . . ?
N7A C3A C4A 123.3(3) . . ?
N7A C3A H3A 118.3 . . ?
C4A C3A H3A 118.3 . . ?
N6A C4A C3A 120.0(3) . . ?
N6A C4A H4A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
N1A C5A N5A 108.8(3) . . ?
N1A C5A C1A 121.4(3) . . ?
N5A C5A C1A 129.9(3) . . ?
N2A C6A N5A 110.4(3) . . ?
N2A C6A N3A 144.0(3) . . ?
N5A C6A N3A 105.6(3) . . ?
N4A C7A N3A 113.4(3) . . ?
N4A C7A C8A 123.8(3) . . ?
N3A C7A C8A 122.8(3) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C5A N1A N2A 109.2(3) . . ?
C5A N1A Cu1A 110.5(2) . . ?
N2A N1A Cu1A 140.2(2) . . ?
C6A N2A N1A 104.8(2) . . ?
C6A N2A Cu1A 130.3(2) . 2_575 ?
N1A N2A Cu1A 124.6(2) . 2_575 ?
C6A N3A C7A 106.1(3) . . ?
C6A N3A H3NA 125(3) . . ?
C7A N3A H3NA 128(3) . . ?
C7A N4A N5A 102.0(3) . . ?
C5A N5A C6A 106.9(3) . . ?
C5A N5A N4A 140.2(3) . . ?
C6A N5A N4A 112.9(3) . . ?
C4A N6A C1A 116.9(3) . . ?
C4A N6A Cu1A 128.2(2) . . ?
C1A N6A Cu1A 114.8(2) . . ?
C3A N7A C2A 116.6(3) . . ?
N2A Cu1A N6A 172.06(12) 2_575 . ?
N2A Cu1A N1A 94.87(10) 2_575 . ?
N6A Cu1A N1A 80.25(10) . . ?
N2A Cu1A Cl2A 90.60(8) 2_575 . ?
N6A Cu1A Cl2A 91.97(8) . . ?
N1A Cu1A Cl2A 159.78(9) . . ?
N2A Cu1A Cl1A 96.95(9) 2_575 . ?
N6A Cu1A Cl1A 89.94(8) . . ?
N1A Cu1A Cl1A 97.63(9) . . ?
Cl2A Cu1A Cl1A 101.01(4) . . ?
N6B C1B C2B 121.5(3) . . ?
N6B C1B C5B 113.2(3) . . ?
C2B C1B C5B 125.3(3) . . ?
N7B C2B C1B 121.6(3) . . ?
N7B C2B H2B 119.2 . . ?
C1B C2B H2B 119.2 . . ?
N7B C3B C4B 122.6(3) . . ?
N7B C3B H3B 118.7 . . ?
C4B C3B H3B 118.7 . . ?
N6B C4B C3B 121.2(3) . . ?
N6B C4B H4B 119.4 . . ?
C3B C4B H4B 119.4 . . ?
N1B C5B N5B 108.1(3) . . ?
N1B C5B C1B 121.7(3) . . ?
N5B C5B C1B 130.1(3) . . ?
N2B C6B N5B 110.7(3) . . ?
N2B C6B N3B 143.8(3) . . ?
N5B C6B N3B 105.5(3) . . ?
N4B C7B N3B 113.9(3) . . ?
N4B C7B C8B 123.9(3) . . ?
N3B C7B C8B 122.2(3) . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C5B N1B N2B 109.2(3) . . ?
C5B N1B Cu1B 110.7(2) . . ?
N2B N1B Cu1B 140.07(19) . . ?
C6B N2B N1B 105.0(2) . . ?
C6B N2B Cu1B 130.9(2) . 2_665 ?
N1B N2B Cu1B 123.83(19) . 2_665 ?
C6B N3B C7B 105.9(3) . . ?
C6B N3B H3NB 129(3) . . ?
C7B N3B H3NB 126(3) . . ?
C7B N4B N5B 101.4(2) . . ?
C6B N5B C5B 106.9(3) . . ?
C6B N5B N4B 113.3(3) . . ?
C5B N5B N4B 139.7(3) . . ?
C4B N6B C1B 116.5(3) . . ?
C4B N6B Cu1B 129.6(2) . . ?
C1B N6B Cu1B 113.9(2) . . ?
C3B N7B C2B 116.5(3) . . ?
N2B Cu1B N1B 95.98(10) 2_665 . ?
N2B Cu1B N6B 173.94(12) 2_665 . ?
N1B Cu1B N6B 80.47(11) . . ?
N2B Cu1B Cl2B 92.39(8) 2_665 . ?
N1B Cu1B Cl2B 166.60(8) . . ?
N6B Cu1B Cl2B 90.25(8) . . ?
N2B Cu1B O1B 87.8(3) 2_665 . ?
N1B Cu1B O1B 90.2(3) . . ?
N6B Cu1B O1B 97.1(3) . . ?
Cl2B Cu1B O1B 100.6(3) . . ?
N2B Cu1B Cl1B 91.2(2) 2_665 . ?
N1B Cu1B Cl1B 95.3(2) . . ?
N6B Cu1B Cl1B 94.0(2) . . ?
Cl2B Cu1B Cl1B 95.0(2) . . ?
H1OA O1W H1OB 99(4) . . ?
H2OA O2W H2OB 109(4) . . ?
H3OA O3W H3OB 113.4 . . ?
H4OA O4W H4OB 91.8 . . ?
Cu1B O1B H28 114.6 . . ?
Cu1B O1B H39 95.9 . . ?
H28 O1B H39 111.3 . . ?
H4BA O4B H4BB 106.7 . . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6A C1A C2A N7A 0.6(6) . . . . ?
C5A C1A C2A N7A -178.2(4) . . . . ?
N7A C3A C4A N6A 1.2(6) . . . . ?
N6A C1A C5A N1A 0.9(5) . . . . ?
C2A C1A C5A N1A 179.8(4) . . . . ?
N6A C1A C5A N5A -179.1(3) . . . . ?
C2A C1A C5A N5A -0.2(6) . . . . ?
N5A C5A N1A N2A -0.2(4) . . . . ?
C1A C5A N1A N2A 179.8(3) . . . . ?
N5A C5A N1A Cu1A -178.4(2) . . . . ?
C1A C5A N1A Cu1A 1.6(4) . . . . ?
N5A C6A N2A N1A -0.7(4) . . . . ?
N3A C6A N2A N1A -180.0(5) . . . . ?
N5A C6A N2A Cu1A -174.4(2) . . . 2_575 ?
N3A C6A N2A Cu1A 6.4(8) . . . 2_575 ?
C5A N1A N2A C6A 0.6(4) . . . . ?
Cu1A N1A N2A C6A 177.9(3) . . . . ?
C5A N1A N2A Cu1A 174.7(2) . . . 2_575 ?
Cu1A N1A N2A Cu1A -8.0(5) . . . 2_575 ?
N2A C6A N3A C7A 179.1(5) . . . . ?
N5A C6A N3A C7A -0.1(4) . . . . ?
N4A C7A N3A C6A 0.1(4) . . . . ?
C8A C7A N3A C6A -179.4(3) . . . . ?
N3A C7A N4A N5A 0.0(4) . . . . ?
C8A C7A N4A N5A 179.5(3) . . . . ?
N1A C5A N5A C6A -0.3(4) . . . . ?
C1A C5A N5A C6A 179.7(4) . . . . ?
N1A C5A N5A N4A 179.8(4) . . . . ?
C1A C5A N5A N4A -0.2(7) . . . . ?
N2A C6A N5A C5A 0.7(4) . . . . ?
N3A C6A N5A C5A -179.8(3) . . . . ?
N2A C6A N5A N4A -179.4(3) . . . . ?
N3A C6A N5A N4A 0.1(4) . . . . ?
C7A N4A N5A C5A 179.9(4) . . . . ?
C7A N4A N5A C6A -0.1(4) . . . . ?
C3A C4A N6A C1A -0.8(5) . . . . ?
C3A C4A N6A Cu1A -178.6(3) . . . . ?
C2A C1A N6A C4A 0.0(5) . . . . ?
C5A C1A N6A C4A 178.9(3) . . . . ?
C2A C1A N6A Cu1A 178.1(3) . . . . ?
C5A C1A N6A Cu1A -3.0(4) . . . . ?
C4A C3A N7A C2A -0.6(6) . . . . ?
C1A C2A N7A C3A -0.3(6) . . . . ?
N6B C1B C2B N7B -1.0(6) . . . . ?
C5B C1B C2B N7B -179.6(4) . . . . ?
N7B C3B C4B N6B -2.4(7) . . . . ?
N6B C1B C5B N1B -1.3(5) . . . . ?
C2B C1B C5B N1B 177.4(3) . . . . ?
N6B C1B C5B N5B -179.7(3) . . . . ?
C2B C1B C5B N5B -1.0(6) . . . . ?
N5B C5B N1B N2B 0.1(4) . . . . ?
C1B C5B N1B N2B -178.6(3) . . . . ?
N5B C5B N1B Cu1B -179.6(2) . . . . ?
C1B C5B N1B Cu1B 1.7(4) . . . . ?
N5B C6B N2B N1B -1.4(4) . . . . ?
N3B C6B N2B N1B 178.7(5) . . . . ?
N5B C6B N2B Cu1B -175.4(2) . . . 2_665 ?
N3B C6B N2B Cu1B 4.7(7) . . . 2_665 ?
C5B N1B N2B C6B 0.8(4) . . . . ?
Cu1B N1B N2B C6B -179.7(3) . . . . ?
C5B N1B N2B Cu1B 175.3(2) . . . 2_665 ?
Cu1B N1B N2B Cu1B -5.2(5) . . . 2_665 ?
N2B C6B N3B C7B -179.9(5) . . . . ?
N5B C6B N3B C7B 0.2(4) . . . . ?
N4B C7B N3B C6B -0.1(4) . . . . ?
C8B C7B N3B C6B -179.6(3) . . . . ?
N3B C7B N4B N5B -0.1(4) . . . . ?
C8B C7B N4B N5B 179.4(3) . . . . ?
N2B C6B N5B C5B 1.4(4) . . . . ?
N3B C6B N5B C5B -178.6(3) . . . . ?
N2B C6B N5B N4B 179.8(3) . . . . ?
N3B C6B N5B N4B -0.3(4) . . . . ?
N1B C5B N5B C6B -0.9(4) . . . . ?
C1B C5B N5B C6B 177.7(3) . . . . ?
N1B C5B N5B N4B -178.5(4) . . . . ?
C1B C5B N5B N4B 0.0(7) . . . . ?
C7B N4B N5B C6B 0.2(4) . . . . ?
C7B N4B N5B C5B 177.8(4) . . . . ?
C3B C4B N6B C1B 1.3(6) . . . . ?
C3B C4B N6B Cu1B 180.0(3) . . . . ?
C2B C1B N6B C4B 0.3(5) . . . . ?
C5B C1B N6B C4B 179.1(3) . . . . ?
C2B C1B N6B Cu1B -178.6(3) . . . . ?
C5B C1B N6B Cu1B 0.2(4) . . . . ?
C4B C3B N7B C2B 1.7(6) . . . . ?
C1B C2B N7B C3B -0.1(6) . . . . ?

_refine_diff_density_max         0.465
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.085


_exptl_crystal_recrystallization_method 
'Slow evaporation from a water/ethanol solution.'
