#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/19/4321993.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_4321993
loop_
_publ_author_name
'Matthew A. Withersby'
'Alexander J. Blake'
'Neil R. Champness'
'Paul A. Cooke'
'Peter Hubberstey'
'Wan-Sheung Li'
'Martin Schröder'
_publ_section_title
;
 Solvent Control in the Synthesis of
 3,6-Bis(pyridin-3-yl)-1,2,4,5-tetrazine-Bridged Cadmium(II) and Zinc(II)
 Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2259
_journal_page_last               2266
_journal_paper_doi               10.1021/ic980898h
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C19 H14 Cl2 N11 O6 Zn'
_chemical_formula_weight         628.68
_chemical_name_common            {[Zn2(mu-3,3-pytz)3(NO3)4](CH2Cl2)}n
_chemical_name_systematic
; 
3,6-bis(Pyrid-3-yl)1,2,4,5-tetrazine Zinc Nitrate Dichloromethane adduct 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.79(3)
_cell_angle_beta                 102.39(3)
_cell_angle_gamma                101.13(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1110(18)
_cell_length_b                   12.474(3)
_cell_length_c                   13.171(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     1216.7(8)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe & Cie, 1997a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1997b)'
_computing_molecular_graphics    'SHELXTL/PC (version 5.03)(Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.785
_diffrn_measured_fraction_theta_max 0.785
_diffrn_measurement_device_type  'Enraf Nonius FAST'
_diffrn_measurement_method       'area detector 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  0.0803
_diffrn_reflns_av_sigmaI/netI    0.1111
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5217
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'deep pink'
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         3355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0507P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                2554
_reflns_number_total             3355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980898h_6.cif
_cod_data_source_block           znpzpra
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'geometrically placed' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1216.7(4)
_cod_database_code               4321993
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.09797(7) 0.65996(6) 0.83541(5) 0.0112(2) Uani 1 d . . .
Cl1 Cl -0.5670(3) -0.0177(2) 0.7030(2) 0.0786(8) Uani 1 d . . .
N1 N 0.0162(5) 0.0784(4) 0.3669(4) 0.0175(11) Uani 1 d . . .
Cl2 Cl -0.6158(2) 0.1091(2) 0.56799(18) 0.0525(5) Uani 1 d . . .
N2 N 0.0513(5) 1.0276(4) 1.2644(4) 0.0189(11) Uani 1 d . . .
C3 C 0.1662(6) 1.1065(5) 1.2569(5) 0.0129(12) Uani 1 d . . .
N4 N 0.2525(5) 1.2266(4) 1.3445(4) 0.0158(11) Uani 1 d . . .
N5 N 0.2165(5) 0.2788(4) 0.4469(4) 0.0149(11) Uani 1 d . . .
C6 C 0.0958(6) 0.2006(5) 0.4508(5) 0.0112(12) Uani 1 d . . .
N10 N 0.2140(6) 0.6743(4) 0.6722(4) 0.0209(12) Uani 1 d . . .
C11 C -0.6405(8) 0.0972(7) 0.6922(7) 0.0411(18) Uani 1 d . . .
H1SA H -0.5837 0.1820 0.7693 0.049 Uiso 1 calc R . .
H1SB H -0.7554 0.0734 0.6813 0.049 Uiso 1 calc R . .
O11 O 0.0720(5) 0.6719(4) 0.6655(4) 0.0257(10) Uani 1 d . . .
O12 O 0.2986(5) 0.6818(4) 0.7669(4) 0.0276(10) Uani 1 d . . .
O13 O 0.2627(5) 0.6708(4) 0.5920(4) 0.0442(13) Uani 1 d . . .
N20 N 0.2644(5) 0.6850(4) 1.0528(4) 0.0173(11) Uani 1 d . . .
O21 O 0.1165(4) 0.6590(4) 0.9966(3) 0.0175(9) Uani 1 d . . .
O22 O 0.3613(5) 0.7024(4) 1.0027(4) 0.0298(11) Uani 1 d . . .
O23 O 0.3055(4) 0.6914(4) 1.1508(4) 0.0291(10) Uani 1 d . . .
N31 N 0.0620(5) 0.4543(4) 0.7367(4) 0.0127(10) Uani 1 d . . .
C32 C 0.0913(6) 0.3923(5) 0.6316(4) 0.0107(12) Uani 1 d . . .
H1A H 0.1396 0.4420 0.6031 0.013 Uiso 1 calc R . .
C33 C 0.0552(6) 0.2618(5) 0.5642(5) 0.0127(12) Uani 1 d . . .
C34 C -0.0186(6) 0.1862(5) 0.6032(5) 0.0196(13) Uani 1 d . . .
H3A H -0.0468 0.0951 0.5578 0.024 Uiso 1 calc R . .
C35 C -0.0488(7) 0.2500(6) 0.7108(5) 0.0247(15) Uani 1 d . . .
H5A H -0.0981 0.2029 0.7412 0.030 Uiso 1 calc R . .
C36 C -0.0072(6) 0.3816(5) 0.7733(5) 0.0156(13) Uani 1 d . . .
H4A H -0.0291 0.4231 0.8469 0.019 Uiso 1 calc R . .
N61 N 0.1660(5) 0.8683(4) 0.9471(4) 0.0148(11) Uani 1 d . . .
C62 C 0.1363(6) 0.9240(5) 1.0537(5) 0.0140(12) Uani 1 d . . .
H10A H 0.0650 0.8705 1.0678 0.017 Uiso 1 calc R . .
C63 C 0.2029(6) 1.0520(5) 1.1415(5) 0.0120(12) Uani 1 d . . .
C64 C 0.3094(6) 1.1324(5) 1.1242(5) 0.0157(13) Uani 1 d . . .
H8A H 0.3607 1.2214 1.1849 0.019 Uiso 1 calc R . .
C65 C 0.3381(6) 1.0772(5) 1.0143(5) 0.0190(13) Uani 1 d . . .
H7A H 0.4078 1.1287 0.9974 0.023 Uiso 1 calc R . .
C66 C 0.2653(6) 0.9493(5) 0.9318(5) 0.0180(13) Uani 1 d . . .
H6A H 0.2863 0.9143 0.8574 0.022 Uiso 1 calc R . .
N101 N -0.3500(5) 0.5856(4) 1.0415(4) 0.0184(11) Uani 1 d . . .
N105 N -0.5940(5) 0.4295(5) 0.8791(4) 0.0174(11) Uani 1 d . . .
C106 C -0.4472(6) 0.5148(5) 0.9231(5) 0.0149(13) Uani 1 d . . .
N131 N -0.1549(5) 0.6024(4) 0.7906(4) 0.0106(10) Uani 1 d . . .
C132 C -0.2239(6) 0.5975(5) 0.8706(5) 0.0125(12) Uani 1 d . . .
H12A H -0.1605 0.6442 0.9552 0.015 Uiso 1 calc R . .
C133 C -0.3830(6) 0.5271(5) 0.8341(5) 0.0120(12) Uani 1 d . . .
C134 C -0.4766(6) 0.4620(6) 0.7101(5) 0.0185(13) Uani 1 d . . .
H14A H -0.5867 0.4147 0.6826 0.022 Uiso 1 calc R . .
C135 C -0.4083(6) 0.4669(6) 0.6278(5) 0.0190(14) Uani 1 d . . .
H15A H -0.4699 0.4229 0.5431 0.023 Uiso 1 calc R . .
C136 C -0.2484(6) 0.5372(5) 0.6716(5) 0.0150(13) Uani 1 d . . .
H16A H -0.2015 0.5399 0.6146 0.018 Uiso 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O21 Zn1 N131 87.91(15) . . y
O21 Zn1 N61 87.34(15) . . y
N131 Zn1 N61 101.28(16) . . y
O21 Zn1 N31 89.66(15) . . y
N131 Zn1 N31 85.65(16) . . y
N61 Zn1 N31 172.33(16) . . y
O21 Zn1 O12 125.08(15) . . y
N131 Zn1 O12 145.89(16) . . y
N61 Zn1 O12 89.82(15) . . y
N31 Zn1 O12 86.13(14) . . y
O21 Zn1 O11 176.32(14) . . y
N131 Zn1 O11 90.62(15) . . y
N61 Zn1 O11 89.63(15) . . y
N31 Zn1 O11 93.60(15) . . y
O12 Zn1 O11 56.97(14) . . y
C6 N1 N2 117.4(4) . 1_544 ?
N1 N2 C3 116.8(5) 1_566 . ?
N4 C3 N2 125.4(4) . . ?
N4 C3 C63 117.3(4) . . ?
N2 C3 C63 117.3(5) . . ?
C3 N4 N5 118.0(4) . 1_566 ?
N4 N5 C6 115.9(4) 1_544 . ?
N1 C6 N5 126.2(4) . . ?
N1 C6 C33 118.8(4) . . ?
N5 C6 C33 114.9(5) . . ?
O13 N10 O12 123.6(5) . . ?
O13 N10 O11 120.7(5) . . ?
O12 N10 O11 115.7(4) . . ?
Cl1 C11 Cl2 111.4(3) . . ?
N10 O11 Zn1 92.3(3) . . ?
N10 O12 Zn1 94.6(3) . . ?
O23 N20 O22 122.8(5) . . ?
O23 N20 O21 120.0(4) . . ?
O22 N20 O21 117.2(4) . . ?
N20 O21 Zn1 107.9(3) . . ?
C36 N31 C32 116.7(5) . . ?
C36 N31 Zn1 119.4(3) . . ?
C32 N31 Zn1 123.6(3) . . ?
N31 C32 C33 123.4(5) . . ?
C32 C33 C34 119.4(4) . . ?
C32 C33 C6 120.2(5) . . ?
C34 C33 C6 120.4(5) . . ?
C35 C34 C33 117.1(5) . . ?
C36 C35 C34 119.7(5) . . ?
N31 C36 C35 123.8(4) . . ?
C66 N61 C62 115.1(5) . . ?
C66 N61 Zn1 123.5(3) . . ?
C62 N61 Zn1 119.9(3) . . ?
N61 C62 C63 123.9(5) . . ?
C62 C63 C64 119.3(4) . . ?
C62 C63 C3 121.1(5) . . ?
C64 C63 C3 119.6(5) . . ?
C63 C64 C65 117.4(5) . . ?
C66 C65 C64 119.2(5) . . ?
N61 C66 C65 125.1(5) . . ?
N105 N101 C106 116.9(4) 2_467 . ?
N101 N105 C106 117.7(4) 2_467 . ?
N105 C106 N101 125.4(5) . . ?
N105 C106 C133 117.4(5) . . ?
N101 C106 C133 117.1(5) . . ?
C136 N131 C132 117.4(4) . . ?
C136 N131 Zn1 118.2(3) . . ?
C132 N131 Zn1 122.0(4) . . ?
N131 C132 C133 122.7(5) . . ?
C132 C133 C134 118.2(4) . . ?
C132 C133 C106 120.2(5) . . ?
C134 C133 C106 121.4(5) . . ?
C135 C134 C133 119.7(5) . . ?
C136 C135 C134 118.3(5) . . ?
N131 C136 C135 123.7(4) . . ?
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 O21 2.099(4) . y
Zn1 N131 2.134(4) . y
Zn1 N61 2.173(5) . y
Zn1 N31 2.182(4) . y
Zn1 O12 2.231(4) . y
Zn1 O11 2.276(4) . y
Cl1 C11 1.744(7) . ?
N1 C6 1.315(7) . ?
N1 N2 1.339(5) 1_544 ?
Cl2 C11 1.767(7) . ?
N2 N1 1.339(5) 1_566 ?
N2 C3 1.346(6) . ?
C3 N4 1.319(7) . ?
C3 C63 1.491(6) . ?
N4 N5 1.342(5) 1_566 ?
N5 N4 1.342(5) 1_544 ?
N5 C6 1.350(6) . ?
C6 C33 1.495(6) . ?
N10 O13 1.216(5) . ?
N10 O12 1.268(6) . ?
N10 O11 1.271(5) . ?
N20 O23 1.225(6) . ?
N20 O22 1.253(5) . ?
N20 O21 1.284(5) . ?
N31 C36 1.331(6) . ?
N31 C32 1.352(6) . ?
C32 C33 1.366(7) . ?
C33 C34 1.400(7) . ?
C34 C35 1.385(7) . ?
C35 C36 1.371(8) . ?
N61 C66 1.340(6) . ?
N61 C62 1.362(6) . ?
C62 C63 1.363(7) . ?
C63 C64 1.390(7) . ?
C64 C65 1.393(7) . ?
C65 C66 1.353(8) . ?
N101 N105 1.329(5) 2_467 ?
N101 C106 1.348(7) . ?
N105 N101 1.329(5) 2_467 ?
N105 C106 1.342(7) . ?
C106 C133 1.472(7) . ?
N131 C136 1.348(7) . ?
N131 C132 1.356(6) . ?
C132 C133 1.386(7) . ?
C133 C134 1.397(7) . ?
C134 C135 1.378(7) . ?
C135 C136 1.378(7) . ?
