# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_trzncl_1
_database_code_depnum_ccdc_archive 'CCDC 2195223'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2022-10-09 downloaded from the CCDC.
;
_audit_creation_date             2019-10-21
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]zinc(II) diperchlorate dihydrate'
_chemical_formula_moiety         'C26 H26 N10 Zn, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C26 H30 Cl2 N10 O10 Zn'
_chemical_formula_weight         778.87
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x+1/2, z+1/2'
3 '-x+1/2, -y+1/2, z'
4 'y+1/2, -x, z+1/2'
5 '-x, -y, -z'
6 'y, -x-1/2, -z-1/2'
7 'x-1/2, y-1/2, -z'
8 '-y-1/2, x, -z-1/2'

_cell_length_a                   9.6587(2)
_cell_length_b                   9.6587(2)
_cell_length_c                   18.0240(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1681.47(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3451
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.88
_cell_measurement_theta_max      71.37
_exptl_absorpt_coefficient_mu    3.080
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7596
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         72.89
_diffrn_reflns_theta_min         4.91
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                1445
_reflns_number_total             1658
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1658
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0731
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1255P)²+4.9791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2168
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains one-quarter of a complex dication, with Zn1 on
 the -4 site 3/4, 3/4, 1/4 and N2 and C5 on the C₂ axis 3/4, 3/4, z. The
 ClO₄⁻ half-anion is disordered over two sites spanning the C₂ axis
 3/4, 1/4, z. These were modelled with occupancies of 0.35 and 0.15, using 
 the refined restraints Cl---O = 1.44(2) and O...O = 2.35(2) Å. The isotropic
 displacement ellipsoids of the Cl and O atoms in each partial anion were
 also constrained to be approximately equal (SHELXL SIMU restraint). 
 The unique water half-molecule is crystallographically ordered in this 
 refinement. All non-H atoms except the disordered anion were refined 
 anisotropically, and C- and N-bound H atoms were placed in calculated 
 positions and refined using a riding model. The disordered water H atoms
 are not included in the model, but are accounted for in the molecular
 weight and density calculations.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1A-O13A = Cl1A-O14A = Cl1A-O15A = Cl1A-O16A
 1.43787 with sigma of 0.02
 Cl1B-O13B = Cl1B-O14B = Cl1B-O15B = Cl1B-O16B
 1.43787 with sigma of 0.02
 O13A-O14A = O13A-O15A = O13A-O16A = O14A-O15A = O14A-O16A = O15A-O16A
 2.348042 with sigma of 0.02
 O13B-O14B = O13B-O15B = O13B-O16B = O14B-O15B = O14B-O16B = O15B-O16B
 2.348042 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim O13A \\sim O14A \\sim O15A \\sim O16A \\sim Cl1B \\sim O13B \\sim O14B \\sim O15B \\sim O16B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl1A(0.35) O13A(0.35) O14A(0.35) O15A(0.35) O16A(0.35) Cl1B(0.15)
 O13B(0.15) O14B(0.15) O15B(0.15) O16B(0.15) O17(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), N8(H8), C10(H10)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.7500 0.7500 0.2500 0.0243(4) Uani 1 4 d S . .
N2 N 0.7500 0.7500 0.1329(3) 0.0342(12) Uani 1 2 d S . .
C3 C 0.7974(5) 0.6386(5) 0.0961(3) 0.0439(11) Uani 1 1 d . . .
C4 C 0.7988(7) 0.6365(7) 0.0187(3) 0.0670(18) Uani 1 1 d . . .
H4 H 0.8329 0.5581 -0.0074 0.080 Uiso 1 1 calc R . .
C5 C 0.7500 0.7500 -0.0192(5) 0.082(3) Uani 1 2 d S . .
H5 H 0.7500 0.7500 -0.0719 0.098 Uiso 1 2 calc SR . .
C6 C 0.8420(5) 0.5271(5) 0.1446(3) 0.0395(10) Uani 1 1 d . . .
N7 N 0.8324(4) 0.5487(3) 0.2177(2) 0.0328(8) Uani 1 1 d . . .
N8 N 0.8781(4) 0.4299(4) 0.2492(2) 0.0406(10) Uani 1 1 d . . .
H8 H 0.8822 0.4151 0.2973 0.049 Uiso 1 1 calc R . .
C9 C 0.9167(5) 0.3364(5) 0.1968(4) 0.0504(14) Uani 1 1 d . . .
C10 C 0.8949(5) 0.3950(5) 0.1295(4) 0.0529(14) Uani 1 1 d . . .
H10 H 0.9119 0.3551 0.0822 0.063 Uiso 1 1 calc R . .
C11 C 0.9710(6) 0.1967(6) 0.2194(5) 0.0726(19) Uani 1 1 d . . .
H11A H 0.9267 0.1248 0.1893 0.109 Uiso 1 1 calc R . .
H11B H 0.9503 0.1806 0.2720 0.109 Uiso 1 1 calc R . .
H11C H 1.0714 0.1937 0.2118 0.109 Uiso 1 1 calc R . .
Cl1A Cl 0.8339(5) 0.3270(5) 0.4401(2) 0.0440(12) Uiso 0.35 1 d PDU . 1
O13A O 0.8633(12) 0.3985(13) 0.5093(6) 0.059(3) Uiso 0.35 1 d PDU A 1
O14A O 0.7052(10) 0.3784(11) 0.4078(6) 0.057(2) Uiso 0.35 1 d PDU . 1
O15A O 0.9462(12) 0.3437(14) 0.3903(6) 0.066(3) Uiso 0.35 1 d PDU B 1
O16A O 0.8214(10) 0.1808(9) 0.4511(6) 0.047(2) Uiso 0.35 1 d PDU . 1
Cl1B Cl 0.8271(11) 0.3587(12) 0.4460(6) 0.048(3) Uiso 0.15 1 d PDU . 2
O13B O 0.717(3) 0.467(3) 0.443(2) 0.132(11) Uiso 0.15 1 d PDU C 2
O14B O 0.766(2) 0.244(2) 0.4089(8) 0.034(3) Uiso 0.15 1 d PDU . 2
O15B O 0.939(2) 0.413(3) 0.4010(13) 0.032(6) Uiso 0.15 1 d PDU D 2
O16B O 0.871(3) 0.346(3) 0.5194(10) 0.070(7) Uiso 0.15 1 d PDU E 2
O17 O 0.9146(14) 0.4572(13) 0.4113(6) 0.079(3) Uani 0.50 1 d P F 3


_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
Zn1 N2 2.110(5) . ?
Zn1 N7 2.179(3) . ?
N2 C3 1.345(5) . ?
C3 C4 1.396(7) . ?
C3 C6 1.453(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.375(8) . ?
C5 H5 0.9500 . ?
C6 N7 1.337(6) . ?
C6 C10 1.401(6) . ?
N7 N8 1.355(5) . ?
N8 H8 0.8800 . ?
N8 C9 1.359(7) . ?
C9 C10 1.354(9) . ?
C9 C11 1.504(7) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
Cl1A O13A 1.454(10) . ?
Cl1A O14A 1.459(10) . ?
Cl1A O15A 1.416(11) . ?
Cl1A O16A 1.431(10) . ?
Cl1B O13B 1.491(17) . ?
Cl1B O14B 1.420(17) . ?
Cl1B O15B 1.450(16) . ?
Cl1B O16B 1.394(16) . ?

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
N2 Zn1 N2 180.00 6_576 . ?
N2 Zn1 N7 74.51(10) . . ?
N2 Zn1 N7 105.49(10) . 6_576 ?
N7 Zn1 N7 149.0(2) . 3_665 ?
N7 Zn1 N7 94.09(5) 6_576 . ?
C3 N2 Zn1 119.6(3) . . ?
C3 N2 C3 120.8(6) . 3_665 ?
N2 C3 C4 120.6(5) . . ?
N2 C3 C6 113.4(4) . . ?
C4 C3 C6 126.1(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(6) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C4 120.5(8) 3_665 . ?
C4 C5 H5 119.8 . . ?
N7 C6 C3 117.2(4) . . ?
N7 C6 C10 111.1(5) . . ?
C10 C6 C3 131.8(5) . . ?
C6 N7 Zn1 115.4(3) . . ?
C6 N7 N8 104.9(4) . . ?
N8 N7 Zn1 139.7(3) . . ?
N7 N8 H8 124.4 . . ?
N7 N8 C9 111.2(4) . . ?
C9 N8 H8 124.4 . . ?
N8 C9 C11 120.2(6) . . ?
C10 C9 N8 107.6(4) . . ?
C10 C9 C11 132.2(6) . . ?
C6 C10 H10 127.4 . . ?
C9 C10 C6 105.3(5) . . ?
C9 C10 H10 127.4 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O13A Cl1A O14A 110.3(7) . . ?
O15A Cl1A O13A 109.9(7) . . ?
O15A Cl1A O14A 111.2(7) . . ?
O15A Cl1A O16A 105.3(7) . . ?
O16A Cl1A O13A 111.4(7) . . ?
O16A Cl1A O14A 108.6(6) . . ?
O14B Cl1B O13B 103.1(13) . . ?
O14B Cl1B O15B 109.2(12) . . ?
O15B Cl1B O13B 104.9(14) . . ?
O16B Cl1B O13B 108.3(14) . . ?
O16B Cl1B O14B 120.5(14) . . ?
O16B Cl1B O15B 109.6(13) . . ?

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
N8 H8 O15A 0.88 1.92 2.756(13) 159.3 .
N8 H8 O15B 0.88 1.95 2.80(3) 163.8 .
N8 H8 O17 0.88 2.12 2.955(13) 158.7 .


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_trzncl_2
_database_code_depnum_ccdc_archive 'CCDC 2195224'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2022-10-09 downloaded from the CCDC.
;
_audit_creation_date             2019-10-21
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]zinc(II) diperchlorate (phase B)'
_chemical_formula_moiety         'C26 H26 N10 Zn, 2(Cl O4)'
_chemical_formula_sum            'C26 H26 Cl2 N10 O8 Zn'
_chemical_formula_weight         742.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x+1/2, z+1/2'
3 '-x+1/2, -y+1/2, z'
4 'y+1/2, -x, z+1/2'
5 '-x, -y, -z'
6 'y, -x-1/2, -z-1/2'
7 'x-1/2, y-1/2, -z'
8 '-y-1/2, x, -z-1/2'

_cell_length_a                   9.5847(3)
_cell_length_b                   9.5847(3)
_cell_length_c                   18.4386(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1693.89(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2820
_cell_measurement_temperature    350(2)
_cell_measurement_theta_min      4.58
_cell_measurement_theta_max      71.68
_exptl_absorpt_coefficient_mu    2.986
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6514
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.49
_diffrn_reflns_theta_min         4.80
_diffrn_ambient_temperature      350(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                1341
_reflns_number_total             1689
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1689
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0645
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1327P)²+0.5382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1977
_refine_ls_wR_factor_ref         0.2147
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains one-quarter of a complex dication, with Cu1 on
 the -4 site 3/4, 3/4, 1/4 and N2 and C5 on the C₂ axis 3/4, 3/4, z. The
 ClO₄⁻ half-anion is disordered over two sites spanning the C₂ axis
 3/4, 1/4, z. These were modelled with occupancies of 0.25 and 0.25, using 
 the refined restraints Cl---O = 1.43(2) and O...O = 2.34(2) Å. The isotropic
 displacement ellipsoids of the Cl and O atoms in each partial anion were
 also constrained to be approximately equal (SHELXL SIMU restraint). 
 All crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a riding
 model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1A-O13A = Cl1A-O14A = Cl1A-O15A = Cl1A-O16A
 1.43328 with sigma of 0.02
 Cl1B-O13B = Cl1B-O14B = Cl1B-O15B = Cl1B-O16B
 1.43328 with sigma of 0.02
 O13A-O14A = O13A-O15A = O13A-O16A = O14A-O15A = O14A-O16A = O15A-O16A
 2.340546 with sigma of 0.02
 O13B-O14B = O13B-O15B = O13B-O16B = O14B-O15B = O14B-O16B = O15B-O16B
 2.340546 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim O13A \\sim O14A \\sim O15A \\sim O16A \\sim Cl1B \\sim O13B \\sim O14B \\sim O15B \\sim O16B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl1A(0.25) O13A(0.25) O14A(0.25) O15A(0.25) O16A(0.25) Cl1B(0.25)
 O13B(0.25) O14B(0.25) O15B(0.25) O16B(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), N8(H8), C10(H10)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.7500 0.7500 0.2500 0.0631(4) Uani 1 4 d S . .
N2 N 0.7500 0.7500 0.3634(3) 0.0686(11) Uani 1 2 d S . .
C3 C 0.7052(5) 0.6376(4) 0.4000(2) 0.0816(11) Uani 1 1 d . . .
C4 C 0.7044(8) 0.6340(6) 0.4743(3) 0.123(2) Uani 1 1 d . . .
H4 H 0.6736 0.5547 0.4986 0.147 Uiso 1 1 calc R . .
C5 C 0.7500 0.7500 0.5131(5) 0.142(5) Uani 1 2 d S . .
H5 H 0.7500 0.7500 0.5635 0.171 Uiso 1 2 calc SR . .
C6 C 0.6602(4) 0.5236(4) 0.3529(2) 0.0760(10) Uani 1 1 d . . .
N7 N 0.6753(3) 0.5395(3) 0.28225(19) 0.0687(8) Uani 1 1 d . . .
N8 N 0.6267(4) 0.4211(4) 0.25284(19) 0.0755(9) Uani 1 1 d . . .
H8 H 0.6243 0.4048 0.2070 0.091 Uiso 1 1 calc R . .
C9 C 0.5820(4) 0.3307(4) 0.3041(3) 0.0843(12) Uani 1 1 d . . .
C10 C 0.6020(5) 0.3938(5) 0.3684(3) 0.0885(12) Uani 1 1 d . . .
H10 H 0.5812 0.3580 0.4141 0.106 Uiso 1 1 calc R . .
C11 C 0.5226(6) 0.1919(5) 0.2841(4) 0.1138(18) Uani 1 1 d . . .
H11A H 0.5712 0.1558 0.2426 0.171 Uiso 1 1 calc R . .
H11B H 0.4254 0.2021 0.2727 0.171 Uiso 1 1 calc R . .
H11C H 0.5330 0.1287 0.3241 0.171 Uiso 1 1 calc R . .
Cl1A Cl 0.7881(10) 0.2068(9) 0.0793(5) 0.121(3) Uiso 0.25 1 d PDU A -1
O13A O 0.809(2) 0.215(2) 0.0036(8) 0.127(5) Uiso 0.25 1 d PDU A -1
O14A O 0.6522(19) 0.142(2) 0.0888(13) 0.155(7) Uiso 0.25 1 d PDU A -1
O15A O 0.780(3) 0.348(2) 0.1134(13) 0.162(7) Uiso 0.25 1 d PDU A -1
O16A O 0.892(2) 0.131(3) 0.1103(11) 0.149(6) Uiso 0.25 1 d PDU A -1
Cl1B Cl 0.7312(8) 0.2505(10) 0.0840(2) 0.0756(12) Uiso 0.25 1 d PDU B -2
O13B O 0.737(2) 0.2147(17) 0.0098(6) 0.102(4) Uiso 0.25 1 d PDU B -2
O14B O 0.633(2) 0.185(3) 0.1252(12) 0.157(8) Uiso 0.25 1 d PDU B -2
O15B O 0.709(3) 0.4019(17) 0.0922(13) 0.176(8) Uiso 0.25 1 d PDU B -2
O16B O 0.8773(16) 0.228(3) 0.1123(10) 0.127(5) Uiso 0.25 1 d PDU B -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
Zn1 N2 2.092(5) . ?
Zn1 N7 2.222(3) . ?
N2 C3 1.342(5) . ?
C3 C4 1.370(7) . ?
C3 C6 1.460(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(8) . ?
C5 H5 0.9300 . ?
C6 N7 1.320(6) . ?
C6 C10 1.393(6) . ?
N7 N8 1.341(5) . ?
N8 H8 0.8600 . ?
N8 C9 1.352(6) . ?
C9 C10 1.346(7) . ?
C9 C11 1.493(6) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
Cl1A O13A 1.412(14) . ?
Cl1A O14A 1.453(16) . ?
Cl1A O15A 1.493(16) . ?
Cl1A O16A 1.362(15) . ?
Cl1B O13B 1.412(11) . ?
Cl1B O14B 1.360(15) . ?
Cl1B O15B 1.474(16) . ?
Cl1B O16B 1.510(15) . ?

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
N2 Zn1 N2 180.00 . 6_576 ?
N2 Zn1 N7 74.48(9) . . ?
N2 Zn1 N7 105.52(9) . 6_576 ?
N7 Zn1 N7 94.11(5) . 6_576 ?
N7 Zn1 N7 148.96(18) 3_665 . ?
C3 N2 Zn1 120.2(3) . . ?
C3 N2 C3 119.7(5) 3_665 . ?
N2 C3 C4 121.6(5) . . ?
N2 C3 C6 113.4(4) . . ?
C4 C3 C6 125.0(4) . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(6) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C4 118.2(8) 3_665 . ?
C4 C5 H5 120.9 . . ?
N7 C6 C3 117.9(3) . . ?
N7 C6 C10 110.4(4) . . ?
C10 C6 C3 131.6(4) . . ?
C6 N7 Zn1 113.8(2) . . ?
C6 N7 N8 105.3(3) . . ?
N8 N7 Zn1 140.5(3) . . ?
N7 N8 H8 124.1 . . ?
N7 N8 C9 111.7(4) . . ?
C9 N8 H8 124.1 . . ?
N8 C9 C11 121.3(5) . . ?
C10 C9 N8 106.4(4) . . ?
C10 C9 C11 132.3(5) . . ?
C6 C10 H10 126.9 . . ?
C9 C10 C6 106.1(4) . . ?
C9 C10 H10 126.9 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O13A Cl1A O14A 105.8(12) . . ?
O13A Cl1A O15A 111.9(12) . . ?
O14A Cl1A O15A 107.0(12) . . ?
O16A Cl1A O13A 109.9(11) . . ?
O16A Cl1A O14A 112.1(13) . . ?
O16A Cl1A O15A 110.2(12) . . ?
O13B Cl1B O15B 110.2(11) . . ?
O13B Cl1B O16B 105.2(10) . . ?
O14B Cl1B O13B 117.3(12) . . ?
O14B Cl1B O15B 107.1(12) . . ?
O14B Cl1B O16B 112.5(11) . . ?
O15B Cl1B O16B 103.7(11) . . ?

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
N8 H8 O15A 0.86 2.35 3.05(2) 138.4 .
N8 H8 O16A 0.86 1.82 2.681(19) 176.6 3_655
N8 H8 O15B 0.86 2.27 3.07(2) 155.5 .
N8 H8 O16B 0.86 2.16 2.960(19) 154.4 3_655


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_trzncl_3
_database_code_depnum_ccdc_archive 'CCDC 2195225'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2022-10-09 downloaded from the CCDC.
;
_audit_creation_date             2019-11-13
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]zinc(II) diperchlorate (phase B)'
_chemical_formula_moiety         'C26 H26 N10 Zn, Cl2 O8'
_chemical_formula_sum            'C26 H26 Cl2 N10 O8 Zn'
_chemical_formula_weight         742.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x+1/2, z+1/2'
3 '-x+1/2, -y+1/2, z'
4 'y+1/2, -x, z+1/2'
5 '-x, -y, -z'
6 'y, -x-1/2, -z-1/2'
7 'x-1/2, y-1/2, -z'
8 '-y-1/2, x, -z-1/2'

_cell_length_a                   9.5643(1)
_cell_length_b                   9.5643(1)
_cell_length_c                   18.4259(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1685.52(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5636
_cell_measurement_temperature    300(2)
_cell_measurement_theta_min      5.19
_cell_measurement_theta_max      71.91
_exptl_absorpt_coefficient_mu    3.000
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13490
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.14
_diffrn_reflns_theta_min         4.80
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                1397
_reflns_number_total             1684
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1684
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0501
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0968P)²+0.6092P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1598
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains one-quarter of a complex dication, with Cu1 on
 the -4 site 3/4, 3/4, 1/4 and N2 and C5 on the C₂ axis 3/4, 3/4, z. The
 ClO₄⁻ half-anion is disordered over two sites spanning the C₂ axis
 3/4, 1/4, z. These were modelled with occupancies of 0.25 and 0.25, using 
 the refined restraints Cl---O = 1.43(2) and O...O = 2.34(2) Å. The isotropic
 displacement ellipsoids of the Cl and O atoms in each partial anion were
 also constrained to be approximately equal (SHELXL SIMU restraint). 
 All crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a riding
 model. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1A-O13A = Cl1A-O14A = Cl1A-O15A = Cl1A-O16A
 1.44068 with sigma of 0.02
 Cl1B-O13B = Cl1B-O14B = Cl1B-O15B = Cl1B-O16B
 1.44068 with sigma of 0.02
 O13A-O14A = O13A-O15A = O13A-O16A = O14A-O15A = O14A-O16A = O15A-O16A
 2.35263 with sigma of 0.02
 O13B-O14B = O13B-O15B = O13B-O16B = O14B-O15B = O14B-O16B = O15B-O16B
 2.35263 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim O13A \\sim O14A \\sim O15A \\sim O16A \\sim Cl1B \\sim O13B \\sim O14B \\sim O15B \\sim O16B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl1A(0.25) O13A(0.25) O14A(0.25) O15A(0.25) O16A(0.25) Cl1B(0.25)
 O13B(0.25) O14B(0.25) O15B(0.25) O16B(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), N8(H8), C10(H10)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.7500 0.7500 0.2500 0.0545(3) Uani 1 4 d S . .
N2 N 0.7500 0.7500 0.3639(2) 0.0605(8) Uani 1 2 d S . .
C3 C 0.7052(4) 0.6373(3) 0.40041(19) 0.0716(8) Uani 1 1 d . . .
C4 C 0.7050(5) 0.6339(5) 0.4751(2) 0.1062(15) Uani 1 1 d . . .
H4 H 0.6750 0.5546 0.4998 0.127 Uiso 1 1 calc R . .
C5 C 0.7500 0.7500 0.5127(4) 0.117(3) Uani 1 2 d S . .
H5 H 0.7500 0.7500 0.5632 0.140 Uiso 1 2 calc SR . .
C6 C 0.6601(3) 0.5225(3) 0.35309(19) 0.0651(7) Uani 1 1 d . . .
N7 N 0.6754(2) 0.5392(2) 0.28229(15) 0.0600(6) Uani 1 1 d . . .
N8 N 0.6270(3) 0.4197(3) 0.25247(15) 0.0644(7) Uani 1 1 d . . .
H8 H 0.6251 0.4033 0.2066 0.077 Uiso 1 1 calc R . .
C9 C 0.5819(3) 0.3293(3) 0.3036(2) 0.0726(9) Uani 1 1 d . . .
C10 C 0.6012(4) 0.3920(3) 0.3687(2) 0.0768(9) Uani 1 1 d . . .
H10 H 0.5797 0.3560 0.4143 0.092 Uiso 1 1 calc R . .
C11 C 0.5218(4) 0.1898(4) 0.2842(3) 0.0978(13) Uani 1 1 d . . .
H11A H 0.5377 0.1715 0.2336 0.147 Uiso 1 1 calc R . .
H11B H 0.4232 0.1898 0.2938 0.147 Uiso 1 1 calc R . .
H11C H 0.5661 0.1184 0.3127 0.147 Uiso 1 1 calc R . .
Cl1A Cl 0.7845(8) 0.2144(7) 0.0799(3) 0.0967(18) Uiso 0.25 1 d PDU A -1
O13A O 0.8037(17) 0.220(2) 0.0031(7) 0.119(5) Uiso 0.25 1 d PDU A -1
O14A O 0.6487(16) 0.150(2) 0.0907(11) 0.142(6) Uiso 0.25 1 d PDU A -1
O15A O 0.775(2) 0.3655(16) 0.1111(10) 0.131(5) Uiso 0.25 1 d PDU A -1
O16A O 0.8931(15) 0.151(2) 0.1109(8) 0.120(4) Uiso 0.25 1 d PDU A -1
Cl1B Cl 0.7334(8) 0.2472(10) 0.08419(18) 0.0676(10) Uiso 0.25 1 d PDU B -2
O13B O 0.7413(19) 0.2164(14) 0.0097(5) 0.092(4) Uiso 0.25 1 d PDU B -2
O14B O 0.6425(19) 0.175(2) 0.1260(10) 0.136(5) Uiso 0.25 1 d PDU B -2
O15B O 0.696(3) 0.3979(15) 0.0974(10) 0.145(6) Uiso 0.25 1 d PDU B -2
O16B O 0.8802(13) 0.238(2) 0.1146(7) 0.109(4) Uiso 0.25 1 d PDU B -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
Zn1 N2 2.098(4) . ?
Zn1 N7 2.220(2) . ?
N2 C3 1.341(4) . ?
C3 C4 1.377(5) . ?
C3 C6 1.467(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.378(6) . ?
C5 H5 0.9300 . ?
C6 N7 1.322(4) . ?
C6 C10 1.399(4) . ?
N7 N8 1.349(3) . ?
N8 H8 0.8600 . ?
N8 C9 1.350(4) . ?
C9 C10 1.355(5) . ?
C9 C11 1.496(5) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
Cl1A O13A 1.428(13) . ?
Cl1A O14A 1.449(14) . ?
Cl1A O15A 1.558(13) . ?
Cl1A O16A 1.329(13) . ?
Cl1B O13B 1.405(10) . ?
Cl1B O14B 1.352(13) . ?
Cl1B O15B 1.504(14) . ?
Cl1B O16B 1.515(13) . ?

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
N2 Zn1 N2 180.00 . 6_576 ?
N2 Zn1 N7 105.54(7) . 6_576 ?
N2 Zn1 N7 74.46(7) . . ?
N7 Zn1 N7 148.91(14) 3_665 . ?
N7 Zn1 N7 94.12(4) 6_576 . ?
C3 N2 Zn1 120.1(2) . . ?
C3 N2 C3 119.7(4) 3_665 . ?
N2 C3 C4 121.4(3) . . ?
N2 C3 C6 113.4(3) . . ?
C4 C3 C6 125.2(3) . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.9(4) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C4 119.7(6) 3_665 . ?
C4 C5 H5 120.2 . . ?
N7 C6 C3 117.6(3) . . ?
N7 C6 C10 110.8(3) . . ?
C10 C6 C3 131.6(3) . . ?
C6 N7 Zn1 114.17(19) . . ?
C6 N7 N8 105.2(2) . . ?
N8 N7 Zn1 140.3(2) . . ?
N7 N8 H8 124.2 . . ?
N7 N8 C9 111.6(3) . . ?
C9 N8 H8 124.2 . . ?
N8 C9 C10 106.9(3) . . ?
N8 C9 C11 121.8(4) . . ?
C10 C9 C11 131.2(4) . . ?
C6 C10 H10 127.3 . . ?
C9 C10 C6 105.5(3) . . ?
C9 C10 H10 127.3 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O13A Cl1A O14A 105.5(10) . . ?
O13A Cl1A O15A 109.7(10) . . ?
O14A Cl1A O15A 106.9(9) . . ?
O16A Cl1A O13A 109.9(9) . . ?
O16A Cl1A O14A 116.8(11) . . ?
O16A Cl1A O15A 107.8(10) . . ?
O13B Cl1B O15B 111.8(10) . . ?
O13B Cl1B O16B 107.4(10) . . ?
O14B Cl1B O13B 119.0(10) . . ?
O14B Cl1B O15B 104.2(11) . . ?
O14B Cl1B O16B 110.8(10) . . ?
O15B Cl1B O16B 102.4(9) . . ?

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
N8 H8 O15A 0.86 2.30 3.011(17) 140.1 .
N8 H8 O16A 0.86 1.85 2.704(14) 172.7 3_655
N8 H8 O15B 0.86 2.12 2.940(19) 158.2 .
N8 H8 O16B 0.86 2.17 2.955(14) 152.0 3_655


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_trzncl_5
_database_code_depnum_ccdc_archive 'CCDC 2195227'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2022-10-09 downloaded from the CCDC.
;
_audit_creation_date             2019-12-20
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]zinc(II) diperchlorate (phase B)'
_chemical_formula_moiety         'C26 H26 N10 Zn, 2(Cl O4)'
_chemical_formula_sum            'C26 H26 Cl2 N10 O8 Zn'
_chemical_formula_weight         742.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x+1/2, z+1/2'
3 '-x+1/2, -y+1/2, z'
4 'y+1/2, -x, z+1/2'
5 '-x, -y, -z'
6 'y, -x-1/2, -z-1/2'
7 'x-1/2, y-1/2, -z'
8 '-y-1/2, x, -z-1/2'

_cell_length_a                   9.5249(9)
_cell_length_b                   9.5249(9)
_cell_length_c                   18.346(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1664.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4388
_cell_measurement_temperature    200(2)
_cell_measurement_theta_min      4.65
_cell_measurement_theta_max      72.09
_exptl_absorpt_coefficient_mu    3.038
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16789
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.14
_diffrn_reflns_theta_min         4.82
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                1297
_reflns_number_total             1667
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.759
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.312
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1667
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0935
_refine_ls_restrained_S_all      1.336
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2912
_refine_ls_wR_factor_ref         0.3099
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 This structure is noisier and less precise than the 250 K refinement from 
 the same crystal. Since the crystal had transformed to a twinned triclinic
 phase at 120 K, this measurement at 200 K might be close to the phase 
 transition temperature.

 The asymmetric unit contains one-quarter of a complex dication, with Cu1 on
 the -4 site 3/4, 3/4, 1/4 and N2 and C5 on the C₂ axis 3/4, 3/4, z. The
 ClO₄⁻ half-anion is disordered over two sites spanning the C₂ axis
 3/4, 1/4, z. These were modelled with occupancies of 0.25 and 0.25, using 
 the refined restraints Cl---O = 1.43(2) and O...O = 2.34(2) Å. All 
 crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a riding
 model. 

 The highest residual Fourier peak of +1.8 e.Å⁻³ is 1.1 Å from Zn1, 
 on the crystallographic C₂ axis bisecting the organic ligand.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1A-O13A = Cl1A-O14A = Cl1A-O15A = Cl1A-O16A
 1.42869 with sigma of 0.02
 Cl1B-O13B = Cl1B-O14B = Cl1B-O15B = Cl1B-O16B
 1.42869 with sigma of 0.02
 O13A-O14A = O13A-O15A = O13A-O16A = O14A-O15A = O14A-O16A = O15A-O16A
 2.333051 with sigma of 0.02
 O13B-O14B = O13B-O15B = O13B-O16B = O14B-O15B = O14B-O16B = O15B-O16B
 2.333051 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim O13A \\sim O14A \\sim O15A \\sim O16A \\sim Cl1B \\sim O13B \\sim O14B \\sim O15B \\sim O16B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl1A(0.25) O13A(0.25) O14A(0.25) O15A(0.25) O16A(0.25) Cl1B(0.25)
 O13B(0.25) O14B(0.25) O15B(0.25) O16B(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), N8(H8), C10(H10)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.7500 0.7500 0.2500 0.0503(6) Uani 1 4 d S . .
N2 N 0.7500 0.7500 0.1357(4) 0.0521(13) Uani 1 2 d S . .
C3 C 0.7953(6) 0.6354(5) 0.0983(3) 0.0693(13) Uani 1 1 d . . .
C4 C 0.7971(9) 0.6330(7) 0.0233(4) 0.096(2) Uani 1 1 d . . .
H4 H 0.8300 0.5526 -0.0022 0.116 Uiso 1 1 calc R . .
C5 C 0.7500 0.7500 -0.0143(6) 0.098(4) Uani 1 2 d S . .
H5 H 0.7500 0.7500 -0.0661 0.118 Uiso 1 2 calc SR . .
C6 C 0.8403(5) 0.5220(5) 0.1464(3) 0.0615(12) Uani 1 1 d . . .
N7 N 0.8237(4) 0.5374(4) 0.2172(2) 0.0563(10) Uani 1 1 d . . .
N8 N 0.8726(5) 0.4192(4) 0.2478(2) 0.0573(11) Uani 1 1 d . . .
H8 H 0.8750 0.4031 0.2951 0.069 Uiso 1 1 calc R . .
C9 C 0.9182(5) 0.3272(5) 0.1959(3) 0.0665(14) Uani 1 1 d . . .
C10 C 0.8990(6) 0.3905(5) 0.1304(3) 0.0691(13) Uani 1 1 d . . .
H10 H 0.9207 0.3535 0.0836 0.083 Uiso 1 1 calc R . .
C11 C 0.9788(6) 0.1874(6) 0.2155(5) 0.0853(18) Uani 1 1 d . . .
H11A H 0.9297 0.1135 0.1885 0.128 Uiso 1 1 calc R . .
H11B H 0.9678 0.1714 0.2680 0.128 Uiso 1 1 calc R . .
H11C H 1.0788 0.1858 0.2029 0.128 Uiso 1 1 calc R . .
Cl1A Cl 0.7652(12) 0.2520(14) 0.4151(3) 0.0620(16) Uiso 0.25 1 d PDU A -1
O13A O 0.741(3) 0.272(3) 0.4899(7) 0.096(6) Uiso 0.25 1 d PDU A -1
O14A O 0.756(3) 0.1096(15) 0.3935(11) 0.103(6) Uiso 0.25 1 d PDU A -1
O15A O 0.8972(16) 0.309(2) 0.3921(10) 0.096(5) Uiso 0.25 1 d PDU A -1
O16A O 0.659(2) 0.330(2) 0.3742(13) 0.129(8) Uiso 0.25 1 d PDU A -1
Cl1B Cl 0.7806(12) 0.2796(10) 0.4197(5) 0.091(3) Uiso 0.25 1 d PDU B -2
O13B O 0.851(3) 0.150(2) 0.3985(13) 0.117(7) Uiso 0.25 1 d PDU B -2
O14B O 0.783(2) 0.284(2) 0.4971(7) 0.096(6) Uiso 0.25 1 d PDU B -2
O15B O 0.850(3) 0.3967(19) 0.3915(11) 0.109(6) Uiso 0.25 1 d PDU B -2
O16B O 0.6399(19) 0.269(3) 0.3910(14) 0.135(8) Uiso 0.25 1 d PDU B -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
Zn1 N2 2.096(7) . ?
Zn1 N7 2.226(3) . ?
N2 C3 1.360(6) . ?
C3 C4 1.377(9) . ?
C3 C6 1.458(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(9) . ?
C5 H5 0.9500 . ?
C6 N7 1.318(7) . ?
C6 C10 1.403(7) . ?
N7 N8 1.342(5) . ?
N8 H8 0.8800 . ?
N8 C9 1.365(7) . ?
C9 C10 1.358(8) . ?
C9 C11 1.495(7) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
Cl1A O13A 1.405(11) . ?
Cl1A O14A 1.416(14) . ?
Cl1A O15A 1.434(13) . ?
Cl1A O16A 1.462(14) . ?
Cl1B O13B 1.460(13) . ?
Cl1B O14B 1.420(13) . ?
Cl1B O15B 1.395(13) . ?
Cl1B O16B 1.444(14) . ?

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
N2 Zn1 N2 180.00 . 6_576 ?
N2 Zn1 N7 105.67(11) . 6_576 ?
N2 Zn1 N7 74.33(11) . . ?
N7 Zn1 N7 148.7(2) 3_665 . ?
N7 Zn1 N7 94.19(6) . 6_576 ?
C3 N2 Zn1 120.3(3) . . ?
C3 N2 C3 119.4(7) . 3_665 ?
N2 C3 C4 121.5(5) . . ?
N2 C3 C6 112.5(5) . . ?
C4 C3 C6 126.0(5) . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.7(6) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 C4 120.3(10) 3_665 . ?
C4 C5 H5 119.9 . . ?
N7 C6 C3 118.6(4) . . ?
N7 C6 C10 110.7(5) . . ?
C10 C6 C3 130.7(5) . . ?
C6 N7 Zn1 113.9(3) . . ?
C6 N7 N8 106.1(4) . . ?
N8 N7 Zn1 139.5(3) . . ?
N7 N8 H8 124.5 . . ?
N7 N8 C9 110.9(4) . . ?
C9 N8 H8 124.5 . . ?
N8 C9 C11 121.8(6) . . ?
C10 C9 N8 106.9(4) . . ?
C10 C9 C11 131.3(6) . . ?
C6 C10 H10 127.3 . . ?
C9 C10 C6 105.4(5) . . ?
C9 C10 H10 127.3 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O13A Cl1A O14A 113.2(11) . . ?
O13A Cl1A O15A 112.3(11) . . ?
O13A Cl1A O16A 108.7(11) . . ?
O14A Cl1A O15A 109.6(10) . . ?
O14A Cl1A O16A 107.4(10) . . ?
O15A Cl1A O16A 105.3(10) . . ?
O14B Cl1B O13B 106.4(10) . . ?
O14B Cl1B O16B 112.6(11) . . ?
O15B Cl1B O13B 111.2(11) . . ?
O15B Cl1B O14B 109.9(10) . . ?
O15B Cl1B O16B 111.0(11) . . ?
O16B Cl1B O13B 105.7(10) . . ?

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
N8 H8 O14A 0.88 2.18 2.93(2) 143.1 3_655
N8 H8 O15A 0.88 2.00 2.86(2) 162.8 .
N8 H8 O15B 0.88 1.79 2.653(19) 167.8 .


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_trzncl_4
_database_code_depnum_ccdc_archive 'CCDC 2195226'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2022-10-09 downloaded from the CCDC.
;
_audit_creation_date             2019-10-22
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]zinc(II) diperchlorate (phase B)'
_chemical_formula_moiety         'C26 H26 N10 Zn, 2(Cl O4)'
_chemical_formula_sum            'C26 H26 Cl2 N10 O8 Zn'
_chemical_formula_weight         742.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x+1/2, z+1/2'
3 '-x+1/2, -y+1/2, z'
4 'y+1/2, -x, z+1/2'
5 '-x, -y, -z'
6 'y, -x-1/2, -z-1/2'
7 'x-1/2, y-1/2, -z'
8 '-y-1/2, x, -z-1/2'

_cell_length_a                   9.5298(3)
_cell_length_b                   9.5298(3)
_cell_length_c                   18.3840(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1669.58(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6203
_cell_measurement_temperature    250(2)
_cell_measurement_theta_min      4.62
_cell_measurement_theta_max      72.71
_exptl_absorpt_coefficient_mu    3.029
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12

_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17110
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.21
_diffrn_reflns_theta_min         4.81
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_gt                1408
_reflns_number_total             1683
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1683
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0533
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.8420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1697
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains one-quarter of a complex dication, with Cu1 on
 the -4 site 3/4, 3/4, 1/4 and N2 and C5 on the C₂ axis 3/4, 3/4, z. The
 ClO₄⁻ half-anion is disordered over two sites spanning the C₂ axis
 3/4, 1/4, z. These were modelled with occupancies of 0.25 and 0.25, using 
 the refined restraints Cl---O = 1.43(2) and O...O = 2.34(2) Å. All 
 crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a riding
 model. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1A-O13A = Cl1A-O14A = Cl1A-O15A = Cl1A-O16A
 1.44477 with sigma of 0.02
 Cl1B-O13B = Cl1B-O14B = Cl1B-O15B = Cl1B-O16B
 1.44477 with sigma of 0.02
 O13A-O14A = O13A-O15A = O13A-O16A = O14A-O15A = O14A-O16A = O15A-O16A
 2.359309 with sigma of 0.02
 O13B-O14B = O13B-O15B = O13B-O16B = O14B-O15B = O14B-O16B = O15B-O16B
 2.359309 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim O13A \\sim O14A \\sim O15A \\sim O16A \\sim Cl1B \\sim O13B \\sim O14B \\sim O15B \\sim O16B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl1A(0.25) O13A(0.25) O14A(0.25) O15A(0.25) O16A(0.25) Cl1B(0.25)
 O13B(0.25) O14B(0.25) O15B(0.25) O16B(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), N8(H8), C10(H10)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.7500 0.7500 0.2500 0.0478(3) Uani 1 4 d S . .
N2 N 0.7500 0.7500 0.1358(2) 0.0522(9) Uani 1 2 d S . .
C3 C 0.7952(4) 0.6366(4) 0.0992(2) 0.0651(9) Uani 1 1 d . . .
C4 C 0.7960(6) 0.6338(5) 0.0242(2) 0.0954(15) Uani 1 1 d . . .
H4 H 0.8270 0.5547 -0.0006 0.114 Uiso 1 1 calc R . .
C5 C 0.7500 0.7500 -0.0132(4) 0.103(3) Uani 1 2 d S . .
H5 H 0.7500 0.7500 -0.0638 0.124 Uiso 1 2 calc SR . .
C6 C 0.8399(3) 0.5224(3) 0.1466(2) 0.0588(8) Uani 1 1 d . . .
N7 N 0.8243(2) 0.5386(2) 0.21779(16) 0.0532(6) Uani 1 1 d . . .
N8 N 0.8726(3) 0.4192(3) 0.24767(15) 0.0559(7) Uani 1 1 d . . .
H8 H 0.8745 0.4025 0.2936 0.067 Uiso 1 1 calc R . .
C9 C 0.9181(3) 0.3285(3) 0.1959(2) 0.0647(9) Uani 1 1 d . . .
C10 C 0.8990(4) 0.3913(4) 0.1309(2) 0.0680(9) Uani 1 1 d . . .
H10 H 0.9205 0.3551 0.0852 0.082 Uiso 1 1 calc R . .
C11 C 0.9783(4) 0.1886(4) 0.2161(3) 0.0846(13) Uani 1 1 d . . .
H11A H 0.9343 0.1165 0.1876 0.127 Uiso 1 1 calc R . .
H11B H 0.9618 0.1710 0.2668 0.127 Uiso 1 1 calc R . .
H11C H 1.0775 0.1885 0.2068 0.127 Uiso 1 1 calc R . .
Cl1A Cl 0.7665(7) 0.2494(9) 0.41584(18) 0.0574(10) Uiso 0.25 1 d PDU A -1
O13A O 0.7297(17) 0.2687(19) 0.4905(5) 0.084(4) Uiso 0.25 1 d PDU A -1
O14A O 0.746(2) 0.1068(11) 0.3923(8) 0.103(4) Uiso 0.25 1 d PDU A -1
O15A O 0.8960(12) 0.304(2) 0.3917(8) 0.100(4) Uiso 0.25 1 d PDU A -1
O16A O 0.6572(16) 0.3316(19) 0.3736(10) 0.136(7) Uiso 0.25 1 d PDU A -1
Cl1B Cl 0.7819(8) 0.2847(7) 0.4193(4) 0.091(2) Uiso 0.25 1 d PDU B -2
O13B O 0.837(2) 0.1391(14) 0.4040(9) 0.117(5) Uiso 0.25 1 d PDU B -2
O14B O 0.7875(18) 0.2962(16) 0.4970(6) 0.101(4) Uiso 0.25 1 d PDU B -2
O15B O 0.861(2) 0.3874(17) 0.3890(8) 0.122(5) Uiso 0.25 1 d PDU B -2
O16B O 0.6373(14) 0.277(3) 0.3891(10) 0.128(6) Uiso 0.25 1 d PDU B -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
Zn1 N2 2.099(4) . ?
Zn1 N7 2.216(2) . ?
N2 C3 1.344(4) . ?
C3 C4 1.379(6) . ?
C3 C6 1.458(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.375(6) . ?
C5 H5 0.9300 . ?
C6 N7 1.326(5) . ?
C6 C10 1.401(4) . ?
N7 N8 1.345(4) . ?
N8 H8 0.8600 . ?
N8 C9 1.356(4) . ?
C9 C10 1.349(6) . ?
C9 C11 1.499(5) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
Cl1A O13A 1.428(9) . ?
Cl1A O14A 1.439(12) . ?
Cl1A O15A 1.410(11) . ?
Cl1A O16A 1.517(12) . ?
Cl1B O13B 1.509(11) . ?
Cl1B O14B 1.433(11) . ?
Cl1B O15B 1.356(11) . ?
Cl1B O16B 1.487(12) . ?

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
N2 Zn1 N2 180.00 6_576 . ?
N2 Zn1 N7 74.50(7) . . ?
N2 Zn1 N7 105.50(7) . 6_576 ?
N7 Zn1 N7 149.00(15) . 3_665 ?
N7 Zn1 N7 94.09(4) 6_576 . ?
C3 N2 Zn1 120.1(2) . . ?
C3 N2 C3 119.8(4) . 3_665 ?
N2 C3 C4 121.2(4) . . ?
N2 C3 C6 113.2(3) . . ?
C4 C3 C6 125.6(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.9(4) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C4 120.0(6) . 3_665 ?
C4 C5 H5 120.0 . . ?
N7 C6 C3 118.1(3) . . ?
N7 C6 C10 110.7(3) . . ?
C10 C6 C3 131.3(4) . . ?
C6 N7 Zn1 113.9(2) . . ?
C6 N7 N8 105.4(2) . . ?
N8 N7 Zn1 140.3(2) . . ?
N7 N8 H8 124.4 . . ?
N7 N8 C9 111.2(3) . . ?
C9 N8 H8 124.4 . . ?
N8 C9 C11 121.0(4) . . ?
C10 C9 N8 107.2(3) . . ?
C10 C9 C11 131.8(4) . . ?
C6 C10 H10 127.3 . . ?
C9 C10 C6 105.5(3) . . ?
C9 C10 H10 127.3 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O13A Cl1A O14A 112.2(9) . . ?
O13A Cl1A O16A 104.9(8) . . ?
O14A Cl1A O16A 104.0(9) . . ?
O15A Cl1A O13A 118.0(9) . . ?
O15A Cl1A O14A 111.7(8) . . ?
O15A Cl1A O16A 104.4(9) . . ?
O14B Cl1B O13B 104.1(8) . . ?
O14B Cl1B O16B 114.2(9) . . ?
O15B Cl1B O13B 113.2(10) . . ?
O15B Cl1B O14B 109.5(8) . . ?
O15B Cl1B O16B 113.5(9) . . ?
O16B Cl1B O13B 101.8(8) . . ?

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
N8 H8 O14A 0.86 2.13 2.881(14) 144.9 3_655
N8 H8 O15A 0.86 2.04 2.875(15) 162.6 .
N8 H8 O15B 0.86 1.76 2.618(15) 172.0 .


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_trzncl_6
_database_code_depnum_ccdc_archive 'CCDC 2195228'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2022-10-09 downloaded from the CCDC.
;
_audit_creation_date             2019-12-20
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]zinc(II) diperchlorate (phase C)'
_chemical_formula_moiety         'C26 H26 N10 Zn, 2(Cl O4)'
_chemical_formula_sum            'C26 H26 Cl2 N10 O8 Zn'
_chemical_formula_weight         742.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   9.5028(8)
_cell_length_b                   9.5342(9)
_cell_length_c                   18.0673(12)
_cell_angle_alpha                80.147(7)
_cell_angle_beta                 84.097(7)
_cell_angle_gamma                89.098(7)
_cell_volume                     1604.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3117
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.65
_cell_measurement_theta_max      71.98
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 The crystal is a non-merohedral twin at this temperature, which was 
 resolved over four domains as described below.
;
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51778
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.48
_diffrn_reflns_theta_min         4.68
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_oxdiff_twin_items               4
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.2620 10251 5128 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.2434 10250 5097 nmt -1.0001 -0.0004 0.1073 -0.0002 -1.0004 0.1778 -0.0017
-0.0021 1.0002
3 0.2497 12932 2619 nmt 0.0032 1.0045 -0.0350 -0.9953 -0.0030 0.1423 -0.0016
-0.0012 1.0000
4 0.2450 12425 2968 nmt -0.0041 -1.0045 0.1436 0.9955 0.0024 0.0355 0.0001
-0.0003 0.9999
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -179.9985° 
 around [0.05 0.09 0.99] (reciprocal) or [-0.00 -0.00 1.00] (direct)
Component 3 rotated by -90.0442° 
 around [0.05 0.09 0.99] (reciprocal) or [-0.00 -0.00 1.00] (direct)
Component 4 rotated by 90.0035° 
 around [0.05 0.09 0.99] (reciprocal) or [-0.00 -0.00 1.00] (direct)
;
_reflns_number_gt                12631
_reflns_number_total             19048
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         19048
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0638
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1160P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.1942
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically and H atoms were
 placed in calculated positions and refined using a riding model.,Twin
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), N10(H10), C12(H12), N16(H16), C18(H18), C22(H22),
 C23(H23), C24(H24), N28(H28), C30(H30), N34(H34), C36(H36)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C37(H37A,H37B,
 H37C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.25113(4) 0.75057(4) 0.25249(2) 0.03315(11) Uani 1 1 d . . .
N2 N 0.2607(3) 0.7091(3) 0.37003(14) 0.0355(5) Uani 1 1 d . . .
C3 C 0.3064(3) 0.5830(3) 0.40455(17) 0.0386(7) Uani 1 1 d . . .
C4 C 0.3179(4) 0.5553(4) 0.4801(2) 0.0521(9) Uani 1 1 d . . .
H4 H 0.3494 0.4650 0.5036 0.063 Uiso 1 1 calc R . .
C5 C 0.2824(4) 0.6623(4) 0.5221(2) 0.0597(10) Uani 1 1 d . . .
H5 H 0.2923 0.6462 0.5746 0.072 Uiso 1 1 calc R . .
C6 C 0.2330(4) 0.7914(4) 0.48802(19) 0.0523(9) Uani 1 1 d . . .
H6 H 0.2071 0.8644 0.5166 0.063 Uiso 1 1 calc R . .
C7 C 0.2222(3) 0.8118(3) 0.41129(17) 0.0397(7) Uani 1 1 d . . .
C8 C 0.3416(3) 0.4814(3) 0.35201(18) 0.0376(7) Uani 1 1 d . . .
N9 N 0.3208(3) 0.5243(3) 0.28030(14) 0.0367(6) Uani 1 1 d . . .
N10 N 0.3625(3) 0.4131(3) 0.24599(16) 0.0396(6) Uani 1 1 d . . .
H10 H 0.3606 0.4130 0.1974 0.048 Uiso 1 1 calc R . .
C11 C 0.4073(3) 0.3026(3) 0.2946(2) 0.0451(8) Uani 1 1 d . . .
C12 C 0.3950(3) 0.3427(3) 0.3639(2) 0.0460(8) Uani 1 1 d . . .
H12 H 0.4178 0.2882 0.4102 0.055 Uiso 1 1 calc R . .
C13 C 0.4647(4) 0.1703(4) 0.2692(2) 0.0552(9) Uani 1 1 d . . .
H13A H 0.4345 0.1649 0.2195 0.083 Uiso 1 1 calc R . .
H13B H 0.4290 0.0870 0.3055 0.083 Uiso 1 1 calc R . .
H13C H 0.5683 0.1719 0.2658 0.083 Uiso 1 1 calc R . .
C14 C 0.1709(3) 0.9405(3) 0.36595(17) 0.0367(7) Uani 1 1 d . . .
N15 N 0.1742(3) 0.9443(2) 0.29194(14) 0.0357(6) Uani 1 1 d . . .
N16 N 0.1164(3) 1.0705(3) 0.26564(15) 0.0367(6) Uani 1 1 d . . .
H16 H 0.1053 1.1008 0.2178 0.044 Uiso 1 1 calc R . .
C17 C 0.0771(3) 1.1451(3) 0.32169(18) 0.0396(7) Uani 1 1 d . . .
C18 C 0.1116(3) 1.0641(3) 0.38752(18) 0.0404(7) Uani 1 1 d . . .
H18 H 0.0980 1.0869 0.4369 0.049 Uiso 1 1 calc R . .
C19 C 0.0085(4) 1.2870(4) 0.3073(2) 0.0514(8) Uani 1 1 d . . .
H19A H 0.0472 1.3389 0.2580 0.077 Uiso 1 1 calc R . .
H19B H 0.0269 1.3411 0.3468 0.077 Uiso 1 1 calc R . .
H19C H -0.0937 1.2747 0.3075 0.077 Uiso 1 1 calc R . .
N20 N 0.2557(3) 0.7480(3) 0.13653(14) 0.0373(6) Uani 1 1 d . . .
C21 C 0.3748(3) 0.7847(3) 0.08985(18) 0.0401(7) Uani 1 1 d . . .
C22 C 0.3856(4) 0.7707(4) 0.01496(18) 0.0477(8) Uani 1 1 d . . .
H22 H 0.4699 0.7976 -0.0170 0.057 Uiso 1 1 calc R . .
C23 C 0.2709(4) 0.7163(4) -0.0132(2) 0.0544(9) Uani 1 1 d . . .
H23 H 0.2765 0.7050 -0.0646 0.065 Uiso 1 1 calc R . .
C24 C 0.1487(4) 0.6789(4) 0.03437(19) 0.0505(8) Uani 1 1 d . . .
H24 H 0.0690 0.6428 0.0159 0.061 Uiso 1 1 calc R . .
C25 C 0.1449(3) 0.6950(3) 0.10902(18) 0.0405(7) Uani 1 1 d . . .
C26 C 0.4875(3) 0.8367(3) 0.12793(17) 0.0366(6) Uani 1 1 d . . .
N27 N 0.4644(2) 0.8284(3) 0.20315(14) 0.0359(6) Uani 1 1 d . . .
N28 N 0.5837(3) 0.8809(3) 0.22302(15) 0.0373(6) Uani 1 1 d . . .
H28 H 0.5974 0.8881 0.2697 0.045 Uiso 1 1 calc R . .
C29 C 0.6796(3) 0.9212(3) 0.16260(19) 0.0412(7) Uani 1 1 d . . .
C30 C 0.6209(3) 0.8938(3) 0.10111(18) 0.0405(7) Uani 1 1 d . . .
H30 H 0.6622 0.9102 0.0502 0.049 Uiso 1 1 calc R . .
C31 C 0.8210(3) 0.9840(4) 0.1707(2) 0.0488(8) Uani 1 1 d . . .
H31A H 0.8069 1.0790 0.1840 0.073 Uiso 1 1 calc R . .
H31B H 0.8813 0.9911 0.1229 0.073 Uiso 1 1 calc R . .
H31C H 0.8666 0.9225 0.2106 0.073 Uiso 1 1 calc R . .
C32 C 0.0250(3) 0.6577(3) 0.16689(18) 0.0387(7) Uani 1 1 d . . .
N33 N 0.0390(3) 0.6844(3) 0.23593(14) 0.0358(5) Uani 1 1 d . . .
N34 N -0.0835(3) 0.6421(3) 0.27676(15) 0.0371(6) Uani 1 1 d . . .
H34 H -0.1020 0.6466 0.3250 0.045 Uiso 1 1 calc R . .
C35 C -0.1758(3) 0.5918(3) 0.23510(18) 0.0387(7) Uani 1 1 d . . .
C36 C -0.1085(3) 0.5995(3) 0.16402(19) 0.0422(7) Uani 1 1 d . . .
H36 H -0.1445 0.5715 0.1216 0.051 Uiso 1 1 calc R . .
C37 C -0.3181(3) 0.5362(4) 0.2693(2) 0.0517(9) Uani 1 1 d . . .
H37A H -0.3151 0.4320 0.2810 0.078 Uiso 1 1 calc R . .
H37B H -0.3882 0.5657 0.2336 0.078 Uiso 1 1 calc R . .
H37C H -0.3443 0.5743 0.3159 0.078 Uiso 1 1 calc R . .
Cl38 Cl 0.22064(10) 0.27945(10) 0.08075(5) 0.0512(2) Uani 1 1 d . . .
O39 O 0.3306(4) 0.3679(4) 0.09737(17) 0.0819(9) Uani 1 1 d . . .
O40 O 0.0939(4) 0.2999(4) 0.12708(18) 0.0934(11) Uani 1 1 d . . .
O41 O 0.2650(4) 0.1366(3) 0.09689(17) 0.0836(10) Uani 1 1 d . . .
O42 O 0.2026(3) 0.3171(3) 0.00326(14) 0.0680(8) Uani 1 1 d . . .
Cl43 Cl 0.72208(10) 0.85549(10) 0.40866(5) 0.0524(2) Uani 1 1 d . . .
O44 O 0.6840(4) 0.8908(4) 0.48097(15) 0.0781(9) Uani 1 1 d . . .
O45 O 0.7572(3) 0.9795(4) 0.35514(17) 0.0821(10) Uani 1 1 d . . .
O46 O 0.6061(3) 0.7853(4) 0.38439(16) 0.0759(9) Uani 1 1 d . . .
O47 O 0.8430(3) 0.7601(3) 0.41306(17) 0.0755(8) 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
Zn1 N2 2.104(2) . ?
Zn1 N9 2.235(2) . ?
Zn1 N15 2.181(2) . ?
Zn1 N20 2.095(2) . ?
Zn1 N27 2.214(3) . ?
Zn1 N33 2.187(2) . ?
N2 C3 1.345(4) . ?
N2 C7 1.353(4) . ?
C3 C4 1.361(5) . ?
C3 C8 1.480(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.377(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(5) . ?
C7 C14 1.460(4) . ?
C8 N9 1.325(4) . ?
C8 C12 1.399(4) . ?
N9 N10 1.352(3) . ?
N10 H10 0.8800 . ?
N10 C11 1.345(4) . ?
C11 C12 1.363(5) . ?
C11 C13 1.492(4) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 N15 1.328(4) . ?
C14 C18 1.397(4) . ?
N15 N16 1.346(3) . ?
N16 H16 0.8800 . ?
N16 C17 1.353(4) . ?
C17 C18 1.370(5) . ?
C17 C19 1.487(4) . ?
C18 H18 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
N20 C21 1.352(4) . ?
N20 C25 1.350(4) . ?
C21 C22 1.376(5) . ?
C21 C26 1.467(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.391(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.385(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.380(5) . ?
C25 C32 1.469(5) . ?
C26 N27 1.343(4) . ?
C26 C30 1.394(4) . ?
N27 N28 1.352(3) . ?
N28 H28 0.8800 . ?
N28 C29 1.354(4) . ?
C29 C30 1.358(5) . ?
C29 C31 1.511(4) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N33 1.335(4) . ?
C32 C36 1.401(4) . ?
N33 N34 1.341(3) . ?
N34 H34 0.8800 . ?
N34 C35 1.356(4) . ?
C35 C36 1.365(5) . ?
C35 C37 1.493(4) . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
Cl38 O39 1.439(3) . ?
Cl38 O40 1.425(3) . ?
Cl38 O41 1.410(3) . ?
Cl38 O42 1.412(3) . ?
Cl43 O44 1.414(3) . ?
Cl43 O45 1.414(3) . ?
Cl43 O46 1.442(3) . ?
Cl43 O47 1.454(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
N2 Zn1 N9 73.91(9) . . ?
N2 Zn1 N15 74.90(9) . . ?
N2 Zn1 N27 105.57(9) . . ?
N2 Zn1 N33 105.24(10) . . ?
N15 Zn1 N9 148.59(9) . . ?
N15 Zn1 N27 97.99(9) . . ?
N15 Zn1 N33 93.06(9) . . ?
N20 Zn1 N2 168.09(9) . . ?
N20 Zn1 N9 94.18(9) . . ?
N20 Zn1 N15 116.99(9) . . ?
N20 Zn1 N27 74.56(10) . . ?
N20 Zn1 N33 74.62(10) . . ?
N27 Zn1 N9 93.83(9) . . ?
N33 Zn1 N9 91.53(9) . . ?
N33 Zn1 N27 149.01(9) . . ?
C3 N2 Zn1 121.0(2) . . ?
C3 N2 C7 119.6(3) . . ?
C7 N2 Zn1 119.5(2) . . ?
N2 C3 C4 122.1(3) . . ?
N2 C3 C8 113.0(3) . . ?
C4 C3 C8 125.0(3) . . ?
C3 C4 H4 120.8 . . ?
C3 C4 C5 118.3(3) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.5(3) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.9 . . ?
C5 C6 C7 118.2(3) . . ?
C7 C6 H6 120.9 . . ?
N2 C7 C6 121.3(3) . . ?
N2 C7 C14 112.8(3) . . ?
C6 C7 C14 125.8(3) . . ?
N9 C8 C3 117.2(3) . . ?
N9 C8 C12 111.4(3) . . ?
C12 C8 C3 131.4(3) . . ?
C8 N9 Zn1 114.74(19) . . ?
C8 N9 N10 104.5(2) . . ?
N10 N9 Zn1 140.5(2) . . ?
N9 N10 H10 123.9 . . ?
C11 N10 N9 112.3(3) . . ?
C11 N10 H10 123.9 . . ?
N10 C11 C12 106.7(3) . . ?
N10 C11 C13 122.0(3) . . ?
C12 C11 C13 131.2(3) . . ?
C8 C12 H12 127.4 . . ?
C11 C12 C8 105.1(3) . . ?
C11 C12 H12 127.4 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N15 C14 C7 117.8(3) . . ?
N15 C14 C18 111.6(3) . . ?
C18 C14 C7 130.6(3) . . ?
C14 N15 Zn1 114.97(18) . . ?
C14 N15 N16 104.9(2) . . ?
N16 N15 Zn1 139.9(2) . . ?
N15 N16 H16 124.1 . . ?
N15 N16 C17 111.8(3) . . ?
C17 N16 H16 124.1 . . ?
N16 C17 C18 107.0(3) . . ?
N16 C17 C19 122.2(3) . . ?
C18 C17 C19 130.9(3) . . ?
C14 C18 H18 127.6 . . ?
C17 C18 C14 104.7(3) . . ?
C17 C18 H18 127.6 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 N20 Zn1 120.5(2) . . ?
C25 N20 Zn1 120.0(2) . . ?
C25 N20 C21 119.1(3) . . ?
N20 C21 C22 121.8(3) . . ?
N20 C21 C26 113.0(3) . . ?
C22 C21 C26 125.1(3) . . ?
C21 C22 H22 120.6 . . ?
C21 C22 C23 118.9(3) . . ?
C23 C22 H22 120.6 . . ?
C22 C23 H23 120.3 . . ?
C24 C23 C22 119.5(3) . . ?
C24 C23 H23 120.3 . . ?
C23 C24 H24 120.6 . . ?
C25 C24 C23 118.8(3) . . ?
C25 C24 H24 120.6 . . ?
N20 C25 C24 121.9(3) . . ?
N20 C25 C32 112.5(3) . . ?
C24 C25 C32 125.5(3) . . ?
N27 C26 C21 117.1(3) . . ?
N27 C26 C30 110.7(3) . . ?
C30 C26 C21 132.2(3) . . ?
C26 N27 Zn1 114.48(18) . . ?
C26 N27 N28 104.6(2) . . ?
N28 N27 Zn1 140.8(2) . . ?
N27 N28 H28 124.0 . . ?
N27 N28 C29 111.9(3) . . ?
C29 N28 H28 124.0 . . ?
N28 C29 C30 106.8(3) . . ?
N28 C29 C31 121.6(3) . . ?
C30 C29 C31 131.6(3) . . ?
C26 C30 H30 127.0 . . ?
C29 C30 C26 105.9(3) . . ?
C29 C30 H30 127.0 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N33 C32 C25 117.1(3) . . ?
N33 C32 C36 110.8(3) . . ?
C36 C32 C25 132.0(3) . . ?
C32 N33 Zn1 114.8(2) . . ?
C32 N33 N34 105.0(2) . . ?
N34 N33 Zn1 139.47(19) . . ?
N33 N34 H34 123.9 . . ?
N33 N34 C35 112.2(3) . . ?
C35 N34 H34 123.9 . . ?
N34 C35 C36 106.5(3) . . ?
N34 C35 C37 121.5(3) . . ?
C36 C35 C37 131.9(3) . . ?
C32 C36 H36 127.3 . . ?
C35 C36 C32 105.4(3) . . ?
C35 C36 H36 127.3 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O40 Cl38 O39 109.1(2) . . ?
O41 Cl38 O39 107.8(2) . . ?
O41 Cl38 O40 110.0(2) . . ?
O41 Cl38 O42 110.14(18) . . ?
O42 Cl38 O39 108.12(19) . . ?
O42 Cl38 O40 111.56(19) . . ?
O44 Cl43 O46 110.30(19) . . ?
O44 Cl43 O47 108.55(19) . . ?
O45 Cl43 O44 110.6(2) . . ?
O45 Cl43 O46 108.40(19) . . ?
O45 Cl43 O47 109.8(2) . . ?
O46 Cl43 O47 109.21(19) . . ?

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
N10 H10 O39 0.88 1.98 2.838(4) 165.7 .
N16 H16 O40 0.88 2.30 3.053(5) 144.2 1_565
N28 H28 O46 0.88 2.15 2.931(4) 148.4 .
N34 H34 O47 0.88 2.09 2.896(4) 151.6 1_455


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
