#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/19/4321989.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_4321989
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 H14.5 Cd N11 O6.5'
_chemical_formula_weight         613.32
_chemical_name_common            {[Cd2(mu-3,3'-pytz)3(NO3)4](EtOH)}n
_chemical_name_systematic
; 
 3,6-bis(pyridy-3-yl)-1,2,4,5-tetrazine Cadmium nitrate ethanol 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                86.76(3)
_cell_angle_beta                 79.04(3)
_cell_angle_gamma                88.14(2)
_cell_formula_units_Z            2
_cell_length_a                   9.060(3)
_cell_length_b                   9.848(3)
_cell_length_c                   13.208(4)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      14
_cell_volume                     1154.8(6)
_computing_cell_refinement       'STADI-4 (stoe & cie, 1996a)'
_computing_data_collection       'STADI-4 (stoe & cie, 1996a)'
_computing_data_reduction        'X-RED (stoe & cie, 1996b)'
_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      297(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE STADI-4 FOUR-CIRCLE DIFFRACTOMETER'
_diffrn_measurement_method       'omega theta'
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8132
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        +-4.8%
_diffrn_standards_interval_time  '60 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.8550
_exptl_absorpt_correction_T_min  0.7935
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Block
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Deep Pink'
_exptl_crystal_F_000             611
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0315
_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)+(0.0547P)²+0.7408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                3569
_reflns_number_total             4066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980898h_2.cif
_cod_data_source_block           cdtznt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.7408P] 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^)+(0.0547P)^2^+0.7408P] 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_primary' value 'direct methods' was changed to
'direct'.

'_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_formula_sum        'C19 H14.50 Cd N11 O6.50'
_cod_database_code               4321989
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
Cd1 Cd 0.49479(3) -0.08926(2) 0.75903(2) 0.03562(10) Uani 1 d . . .
N1 N 0.8182(4) -0.5813(3) 0.7659(3) 0.0483(8) Uani 1 d . . .
N2 N 0.8649(4) -0.7039(3) 0.7369(3) 0.0490(8) Uani 1 d . . .
C3 C 0.9920(4) -0.7518(4) 0.7631(3) 0.0365(8) Uani 1 d . . .
N4 N 1.0679(4) -0.6908(3) 0.8246(3) 0.0512(9) Uani 1 d . . .
N5 N 1.0221(4) -0.5674(3) 0.8534(3) 0.0517(9) Uani 1 d . . .
C6 C 0.9025(4) -0.5138(4) 0.8184(3) 0.0399(8) Uani 1 d . . .
N10 N 0.3106(4) -0.2043(4) 0.9413(3) 0.0481(8) Uani 1 d . . .
O11 O 0.3563(4) -0.0834(3) 0.9323(2) 0.0546(7) Uani 1 d . . .
O12 O 0.3556(4) -0.2774(3) 0.8675(3) 0.0674(9) Uani 1 d . . .
O13 O 0.2253(4) -0.2428(5) 1.0189(3) 0.0909(13) Uani 1 d . . .
N20 N 0.6351(4) -0.1666(4) 0.5613(3) 0.0497(8) Uani 1 d . . .
O21 O 0.5553(4) -0.2452(3) 0.6269(2) 0.0560(7) Uani 1 d . . .
O22 O 0.6518(4) -0.0496(3) 0.5872(2) 0.0669(9) Uani 1 d . . .
O23 O 0.6928(5) -0.2054(4) 0.4767(3) 0.0824(11) Uani 1 d . . .
N31 N 0.6990(3) -0.1793(3) 0.8228(2) 0.0417(7) Uani 1 d . . .
C32 C 0.7420(4) -0.3084(4) 0.8051(3) 0.0426(8) Uani 1 d . . .
H32A H 0.6898 -0.3572 0.7656 0.051 Uiso 1 calc R . .
C33 C 0.8598(4) -0.3732(4) 0.8424(3) 0.0402(8) Uani 1 d . . .
C34 C 0.9366(5) -0.2992(4) 0.9017(3) 0.0511(10) Uani 1 d . . .
H34A H 1.0165 -0.3388 0.9285 0.061 Uiso 1 calc R . .
C35 C 0.8923(5) -0.1661(4) 0.9203(3) 0.0552(11) Uani 1 d . . .
H35A H 0.9416 -0.1149 0.9602 0.066 Uiso 1 calc R . .
C36 C 0.7749(5) -0.1104(4) 0.8794(3) 0.0478(9) Uani 1 d . . .
H36A H 0.7468 -0.0202 0.8916 0.057 Uiso 1 calc R . .
N61 N 0.2616(3) -0.0430(3) 0.7123(2) 0.0418(7) Uani 1 d . . .
C62 C 0.1890(4) 0.0700(4) 0.7487(3) 0.0389(8) Uani 1 d . . .
H62 H 0.2321 0.1199 0.7928 0.047 Uiso 1 calc R . .
C63 C 1.0541(4) -0.8835(4) 0.7247(3) 0.0372(8) Uani 1 d . . .
C64 C 0.9872(5) -0.9603(4) 0.6623(3) 0.0496(10) Uani 1 d . . .
H64 H 0.8958 -0.9325 0.6447 0.059 Uiso 1 calc R . .
C65 C 1.0583(5) -1.0784(5) 0.6266(4) 0.0573(11) Uani 1 d . . .
H65 H 1.0147 -1.1325 0.5853 0.069 Uiso 1 calc R . .
C66 C 0.1955(5) -0.1165(4) 0.6528(3) 0.0515(10) Uani 1 d . . .
H66 H 0.2430 -0.1962 0.6278 0.062 Uiso 1 calc R . .
N101 N 0.3838(4) 0.5255(3) 0.5787(3) 0.0534(9) Uani 1 d . . .
N105 N 0.6102(4) 0.4068(3) 0.5110(3) 0.0560(9) Uani 1 d . . .
C106 C 0.4942(4) 0.4346(4) 0.5869(3) 0.0447(9) Uani 1 d . . .
N131 N 0.5254(3) 0.1445(3) 0.7741(2) 0.0404(7) Uani 1 d . . .
C132 C 0.5339(4) 0.2217(4) 0.6876(3) 0.0426(8) Uani 1 d . . .
H13A H 0.5721 0.1830 0.6250 0.051 Uiso 1 calc R . .
C133 C 0.4884(4) 0.3577(4) 0.6864(3) 0.0439(9) Uani 1 d . . .
C134 C 0.4340(5) 0.4161(4) 0.7795(4) 0.0540(10) Uani 1 d . . .
H13B H 0.3990 0.5059 0.7810 0.065 Uiso 1 calc R . .
C135 C 0.4328(5) 0.3388(4) 0.8701(4) 0.0564(11) Uani 1 d . . .
H13C H 0.4015 0.3765 0.9338 0.068 Uiso 1 calc R . .
C136 C 0.4790(4) 0.2045(4) 0.8638(3) 0.0470(9) Uani 1 d . . .
H13D H 0.4782 0.1525 0.9249 0.056 Uiso 1 calc R . .
O10 O 0.0544(13) 0.5595(11) 0.6165(9) 0.121(3) Uiso 0.50 d P . .
C11 C -0.0134(9) 0.5718(8) 0.5250(6) 0.112(2) Uiso 1 d . . .
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'
Cd Cd -0.8075 1.2024 '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
N31 Cd1 N61 166.95(11) . . y
N31 Cd1 N131 100.80(11) . . y
N61 Cd1 N131 89.99(11) . . y
N31 Cd1 O21 86.99(11) . . y
N61 Cd1 O21 90.25(11) . . y
N131 Cd1 O21 136.29(11) . . y
N31 Cd1 O11 89.10(11) . . y
N61 Cd1 O11 84.58(11) . . y
N131 Cd1 O11 84.74(11) . . y
O21 Cd1 O11 138.73(10) . . y
N31 Cd1 O22 90.83(12) . . y
N61 Cd1 O22 97.62(12) . . y
N131 Cd1 O22 84.06(11) . . y
O21 Cd1 O22 52.63(11) . . y
O11 Cd1 O22 168.59(10) . . y
N31 Cd1 O12 84.19(12) . . y
N61 Cd1 O12 82.94(12) . . y
N131 Cd1 O12 136.31(11) . . y
O21 Cd1 O12 86.99(11) . . y
O11 Cd1 O12 51.75(10) . . y
O22 Cd1 O12 139.57(11) . . y
N2 N1 C6 117.9(3) . . ?
N1 N2 C3 117.2(3) . . ?
N2 C3 N4 124.8(3) . . ?
N2 C3 C63 118.7(3) . . ?
N4 C3 C63 116.5(3) . . ?
N5 N4 C3 117.9(3) . . ?
N4 N5 C6 117.0(3) . . ?
N5 C6 N1 124.5(3) . . ?
N5 C6 C33 117.1(3) . . ?
N1 C6 C33 118.4(3) . . ?
O13 N10 O12 123.3(4) . . ?
O13 N10 O11 119.6(4) . . ?
O12 N10 O11 117.0(3) . . ?
N10 O11 Cd1 97.7(2) . . ?
N10 O12 Cd1 93.4(2) . . ?
O23 N20 O22 122.1(4) . . ?
O23 N20 O21 120.7(4) . . ?
O22 N20 O21 117.1(3) . . ?
N20 O21 Cd1 97.0(2) . . ?
N20 O22 Cd1 93.2(2) . . ?
C36 N31 C32 117.6(3) . . ?
C36 N31 Cd1 123.4(2) . . ?
C32 N31 Cd1 119.0(2) . . ?
N31 C32 C33 123.6(4) . . ?
C32 C33 C34 117.6(3) . . ?
C32 C33 C6 120.7(3) . . ?
C34 C33 C6 121.7(3) . . ?
C35 C34 C33 119.0(4) . . ?
C36 C35 C34 119.2(4) . . ?
N31 C36 C35 123.0(4) . . ?
C66 N61 C62 117.4(3) . . ?
C66 N61 Cd1 126.6(2) . . ?
C62 N61 Cd1 116.0(2) . . ?
N61 C62 C63 123.8(3) . 1_465 ?
C62 C63 C64 118.1(3) 1_645 . ?
C62 C63 C3 118.4(3) 1_645 . ?
C64 C63 C3 123.4(3) . . ?
C65 C64 C63 118.7(4) . . ?
C64 C65 C66 119.5(4) . 1_645 ?
N61 C66 C65 122.4(4) . 1_465 ?
N105 N101 C106 117.3(4) 2_666 . ?
N101 N105 C106 117.6(3) 2_666 . ?
N101 C106 N105 125.1(4) . . ?
N101 C106 C133 117.9(4) . . ?
N105 C106 C133 117.0(3) . . ?
C132 N131 C136 117.6(3) . . ?
C132 N131 Cd1 115.8(2) . . ?
C136 N131 Cd1 121.7(3) . . ?
N131 C132 C133 122.8(4) . . ?
C134 C133 C132 118.7(4) . . ?
C134 C133 C106 121.7(3) . . ?
C132 C133 C106 119.5(4) . . ?
C135 C134 C133 118.8(4) . . ?
C134 C135 C136 118.4(4) . . ?
N131 C136 C135 123.5(4) . . ?
O10 C11 C11 105.6(9) . 2_566 ?
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
Cd1 N31 2.306(3) . y
Cd1 N61 2.335(3) . y
Cd1 N131 2.351(3) . y
Cd1 O21 2.364(3) . y
Cd1 O11 2.394(3) . y
Cd1 O22 2.456(3) . y
Cd1 O12 2.498(3) . y
N1 N2 1.320(4) . ?
N1 C6 1.339(5) . ?
N2 C3 1.329(4) . ?
C3 N4 1.337(5) . ?
C3 C63 1.475(5) . ?
N4 N5 1.324(4) . ?
N5 C6 1.338(5) . ?
C6 C33 1.461(5) . ?
N10 O13 1.211(5) . ?
N10 O12 1.242(5) . ?
N10 O11 1.264(4) . ?
N20 O23 1.217(4) . ?
N20 O22 1.243(4) . ?
N20 O21 1.263(5) . ?
N31 C36 1.333(5) . ?
N31 C32 1.338(5) . ?
C32 C33 1.381(5) . ?
C33 C34 1.390(6) . ?
C34 C35 1.380(6) . ?
C35 C36 1.368(6) . ?
N61 C66 1.332(5) . ?
N61 C62 1.339(5) . ?
C62 C63 1.378(5) 1_465 ?
C63 C62 1.378(5) 1_645 ?
C63 C64 1.382(5) . ?
C64 C65 1.374(6) . ?
C65 C66 1.387(6) 1_645 ?
C66 C65 1.387(6) 1_465 ?
N101 N105 1.319(5) 2_666 ?
N101 C106 1.337(5) . ?
N105 N101 1.319(5) 2_666 ?
N105 C106 1.340(5) . ?
C106 C133 1.473(6) . ?
N131 C132 1.327(5) . ?
N131 C136 1.343(5) . ?
C132 C133 1.389(5) . ?
C133 C134 1.385(6) . ?
C134 C135 1.379(6) . ?
C135 C136 1.377(6) . ?
O10 C11 1.454(13) . ?
C11 C11 1.586(15) 2_566 ?
