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#$Date: 2023-03-06 11:12:09 +0200 (Mon, 06 Mar 2023) $
#$Revision: 281658 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/68/8106838.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8106838
loop_
_publ_author_name
'Zhu, Guang-Zhou'
'Li, Chun-Ling'
'Wang, Ao-Lan'
'Wang, Shi-Yu'
'Zou, Dan-Ling'
'Zhang, Xiao-Jing'
'Yang, Feng-Lei'
_publ_section_title
;
 Crystal structure of tris(3-(2-pyridyl)pyrazole)zinc(II)tetrachlorido
 zincate(II), C24H21Cl4N9Zn2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              241
_journal_page_last               242
_journal_paper_doi               10.1515/ncrs-2015-0104
_journal_volume                  231
_journal_year                    2016
_chemical_formula_sum            'C24 H21 Cl4 N9 Zn2'
_chemical_formula_weight         708.04
_chemical_name_systematic
; 
[Tri(3-(2-pyridyl)pyrazole)zinc(II)] Zinc(II) Tetrachloride 
;
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   13.3310(13)
_cell_length_b                   13.3310(13)
_cell_length_c                   58.070(9)
_cell_measurement_temperature    296(2)
_cell_volume                     8937.3(19)
_computing_cell_refinement       'SMART (Bruker 2001)'
_computing_data_collection       'SMART (Bruker 2001)'
_computing_data_reduction        'SMART (Bruker 2001)'
_computing_molecular_graphics    'SHELXTL(Sheldrick, 1997)'
_computing_publication_material  'SHELXTL(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            36116
_diffrn_reflns_theta_full        26.62
_diffrn_reflns_theta_max         26.62
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.148
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0408
_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+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1491
_reflns_number_gt                1307
_reflns_number_total             2032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2015-0104_suppl.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               8106838
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
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 0.6667 0.3333 0.014268(11) 0.0521(3) Uani 1 3 d S . .
Cl1 Cl 0.49952(8) 0.31332(9) -0.000307(14) 0.0771(4) Uani 1 1 d . . .
Cl2 Cl 0.6667 0.3333 0.05277(2) 0.0547(4) Uani 1 3 d S . .
Zn2 Zn 0.0000 0.0000 0.085141(11) 0.0468(3) Uani 1 3 d S . .
N1 N 0.1432(2) 0.0145(2) 0.06411(5) 0.0584(7) Uani 1 1 d . . .
N2 N 0.1506(2) 0.1195(2) 0.10328(4) 0.0516(6) Uani 1 1 d . . .
N3 N 0.1761(2) 0.1794(2) 0.12302(5) 0.0660(8) Uani 1 1 d . . .
H3A H 0.1250 0.1765 0.1324 0.079 Uiso 1 1 calc R . .
C1 C 0.1363(4) -0.0394(3) 0.04417(7) 0.0800(10) Uani 1 1 d . . .
H1A H 0.0632 -0.0949 0.0390 0.096 Uiso 1 1 calc R . .
C2 C 0.2273(5) -0.0185(4) 0.03121(9) 0.1042(14) Uani 1 1 d . . .
H2A H 0.2177 -0.0573 0.0174 0.125 Uiso 1 1 calc R . .
C3 C 0.3344(5) 0.0610(5) 0.03884(9) 0.1034(15) Uani 1 1 d . . .
H3B H 0.3995 0.0763 0.0302 0.124 Uiso 1 1 calc R . .
C4 C 0.3472(3) 0.1187(3) 0.05920(8) 0.0843(12) Uani 1 1 d . . .
H4A H 0.4202 0.1736 0.0645 0.101 Uiso 1 1 calc R . .
C5 C 0.2488(3) 0.0933(3) 0.07164(6) 0.0570(8) Uani 1 1 d . . .
C6 C 0.2512(3) 0.1476(3) 0.09353(6) 0.0548(8) Uani 1 1 d . . .
C7 C 0.3424(3) 0.2270(3) 0.10740(8) 0.0829(12) Uani 1 1 d . . .
H7A H 0.4214 0.2612 0.1045 0.100 Uiso 1 1 calc R . .
C8 C 0.2893(4) 0.2435(3) 0.12637(8) 0.0866(12) Uani 1 1 d . . .
H8A H 0.3260 0.2904 0.1390 0.104 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
Cl2 Zn1 Cl1 111.88(3) . 2_655
Cl2 Zn1 Cl1 111.88(3) . 3_665
Cl1 Zn1 Cl1 106.96(3) 2_655 3_665
Cl2 Zn1 Cl1 111.88(3) . .
Cl1 Zn1 Cl1 106.96(3) 2_655 .
Cl1 Zn1 Cl1 106.96(3) 3_665 .
N2 Zn2 N2 97.38(9) . 3
N2 Zn2 N2 97.38(9) . 2
N2 Zn2 N2 97.38(9) 3 2
N2 Zn2 N1 165.42(9) . 3
N2 Zn2 N1 75.79(10) 3 3
N2 Zn2 N1 96.29(10) 2 3
N2 Zn2 N1 96.29(10) . 2
N2 Zn2 N1 165.42(9) 3 2
N2 Zn2 N1 75.79(9) 2 2
N1 Zn2 N1 91.98(10) 3 2
N2 Zn2 N1 75.79(10) . .
N2 Zn2 N1 96.29(9) 3 .
N2 Zn2 N1 165.42(9) 2 .
N1 Zn2 N1 91.98(10) 3 .
N1 Zn2 N1 91.98(10) 2 .
C5 N1 C1 117.7(3) . .
C5 N1 Zn2 114.5(2) . .
C1 N1 Zn2 127.6(2) . .
C6 N2 N3 106.1(3) . .
C6 N2 Zn2 116.4(2) . .
N3 N2 Zn2 137.5(2) . .
C8 N3 N2 112.2(3) . .
C8 N3 H3A 123.9 . .
N2 N3 H3A 123.9 . .
C2 C1 N1 124.3(4) . .
C2 C1 H1A 117.8 . .
N1 C1 H1A 117.8 . .
C1 C2 C3 118.1(5) . .
C1 C2 H2A 121.0 . .
C3 C2 H2A 121.0 . .
C2 C3 C4 120.3(4) . .
C2 C3 H3B 119.8 . .
C4 C3 H3B 119.8 . .
C3 C4 C5 118.4(4) . .
C3 C4 H4A 120.8 . .
C5 C4 H4A 120.8 . .
N1 C5 C4 121.2(4) . .
N1 C5 C6 115.3(3) . .
C4 C5 C6 123.5(4) . .
N2 C6 C7 109.9(3) . .
N2 C6 C5 117.7(3) . .
C7 C6 C5 132.4(3) . .
C8 C7 C6 105.0(3) . .
C8 C7 H7A 127.5 . .
C6 C7 H7A 127.5 . .
N3 C8 C7 106.8(3) . .
N3 C8 H8A 126.6 . .
C7 C8 H8A 126.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 Cl2 2.2360(17) .
Zn1 Cl1 2.2712(9) 2_655
Zn1 Cl1 2.2712(9) 3_665
Zn1 Cl1 2.2712(9) .
Zn2 N2 2.116(2) .
Zn2 N2 2.116(2) 3
Zn2 N2 2.116(2) 2
Zn2 N1 2.192(2) 3
Zn2 N1 2.192(2) 2
Zn2 N1 2.192(2) .
N1 C5 1.340(4) .
N1 C1 1.341(4) .
N2 C6 1.326(4) .
N2 N3 1.340(3) .
N3 C8 1.325(4) .
N3 H3A 0.8600 .
C1 C2 1.333(5) .
C1 H1A 0.9300 .
C2 C3 1.359(6) .
C2 H2A 0.9300 .
C3 C4 1.374(6) .
C3 H3B 0.9300 .
C4 C5 1.383(4) .
C4 H4A 0.9300 .
C5 C6 1.455(5) .
C6 C7 1.400(5) .
C7 C8 1.385(6) .
C7 H7A 0.9300 .
C8 H8A 0.9300 .
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
N2 Zn2 N1 C5 -4.55(19) . . . .
N2 Zn2 N1 C5 -100.6(2) 3 . . .
N2 Zn2 N1 C5 58.9(5) 2 . . .
N1 Zn2 N1 C5 -176.5(2) 3 . . .
N1 Zn2 N1 C5 91.4(3) 2 . . .
N2 Zn2 N1 C1 -179.3(3) . . . .
N2 Zn2 N1 C1 84.7(3) 3 . . .
N2 Zn2 N1 C1 -115.8(4) 2 . . .
N1 Zn2 N1 C1 8.8(3) 3 . . .
N1 Zn2 N1 C1 -83.3(2) 2 . . .
N2 Zn2 N2 C6 97.3(2) 3 . . .
N2 Zn2 N2 C6 -164.2(2) 2 . . .
N1 Zn2 N2 C6 36.4(5) 3 . . .
N1 Zn2 N2 C6 -87.8(2) 2 . . .
N1 Zn2 N2 C6 2.69(19) . . . .
N2 Zn2 N2 N3 -82.7(2) 3 . . .
N2 Zn2 N2 N3 15.7(3) 2 . . .
N1 Zn2 N2 N3 -143.7(4) 3 . . .
N1 Zn2 N2 N3 92.1(3) 2 . . .
N1 Zn2 N2 N3 -177.4(3) . . . .
C6 N2 N3 C8 -0.8(3) . . . .
Zn2 N2 N3 C8 179.3(2) . . . .
C5 N1 C1 C2 -1.0(5) . . . .
Zn2 N1 C1 C2 173.6(3) . . . .
N1 C1 C2 C3 1.2(7) . . . .
C1 C2 C3 C4 -0.9(7) . . . .
C2 C3 C4 C5 0.4(6) . . . .
C1 N1 C5 C4 0.4(4) . . . .
Zn2 N1 C5 C4 -174.9(2) . . . .
C1 N1 C5 C6 -179.1(3) . . . .
Zn2 N1 C5 C6 5.6(3) . . . .
C3 C4 C5 N1 -0.1(5) . . . .
C3 C4 C5 C6 179.3(3) . . . .
N3 N2 C6 C7 -0.1(3) . . . .
Zn2 N2 C6 C7 179.9(2) . . . .
N3 N2 C6 C5 179.4(2) . . . .
Zn2 N2 C6 C5 -0.6(3) . . . .
N1 C5 C6 N2 -3.5(4) . . . .
C4 C5 C6 N2 177.1(3) . . . .
N1 C5 C6 C7 175.9(3) . . . .
C4 C5 C6 C7 -3.6(5) . . . .
N2 C6 C7 C8 0.8(4) . . . .
C5 C6 C7 C8 -178.5(3) . . . .
N2 N3 C8 C7 1.3(4) . . . .
C6 C7 C8 N3 -1.3(4) . . . .
