#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/19/4321990.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_4321990
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            'C18.5 H13 Cd Cl N11 O6'
_chemical_formula_weight         633.25
_chemical_name_common            {[Cd2(mu-3,3'-pytz)3(NO3)4](CH2Cl2)}n
_chemical_name_systematic
; 
 3,6-bis(pyrid-3-yl)-1,2,4,5-tetrazine Cadmium 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                94.12(15)
_cell_angle_beta                 102.35(13)
_cell_angle_gamma                88.12(15)
_cell_formula_units_Z            2
_cell_length_a                   8.981(16)
_cell_length_b                   9.93(2)
_cell_length_c                   13.19(2)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      12
_cell_volume                     1146(4)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1516
_diffrn_reflns_av_sigmaI/netI    0.0489
_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       -5
_diffrn_reflns_number            4084
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        '+- 11.3'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Pink-Red
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Sphenoid
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.463
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0005(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4031
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0563
_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)+(0.0410P)²+10.9459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                3494
_reflns_number_total             4031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980898h_3.cif
_cod_data_source_block           cdpytz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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^)+(0.0410P)^2^+10.9459P] 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^)+(0.0410P)^2^+10.9459P] 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        'C18.50 H13 Cd Cl N11 O6'
_cod_database_code               4321990
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
Cd Cd 1.00019(5) -0.08661(5) 0.73868(4) 0.02262(18) Uani 1 d . . .
N1 N 0.5753(6) 0.3144(5) 0.6753(4) 0.0278(12) Uani 1 d . . .
N2 N 0.5297(7) 0.4368(6) 0.6478(5) 0.0300(13) Uani 1 d . . .
C3 C 0.4102(7) 0.4904(6) 0.6821(5) 0.0244(14) Uani 1 d . . .
N4 N 0.3268(6) 0.4272(6) 0.7362(5) 0.0293(13) Uani 1 d . . .
N5 N 0.3716(6) 0.3048(6) 0.7640(5) 0.0292(13) Uani 1 d . . .
C6 C 0.4988(7) 0.2541(6) 0.7353(5) 0.0232(13) Uani 1 d . . .
N10 N 1.1285(7) -0.1600(6) 0.9404(4) 0.0315(13) Uani 1 d . . .
O11 O 1.0549(6) -0.2417(5) 0.8699(4) 0.0314(11) Uani 1 d . . .
O12 O 1.1502(7) -0.0448(5) 0.9148(4) 0.0419(13) Uani 1 d . . .
O13 O 1.1727(7) -0.1936(6) 1.0292(4) 0.0532(16) Uani 1 d . . .
N20 N 0.8097(6) -0.2031(6) 0.5546(4) 0.0282(13) Uani 1 d . . .
O21 O 0.8548(5) -0.0822(5) 0.5646(3) 0.0302(11) Uani 1 d . . .
O22 O 0.7201(6) -0.2437(6) 0.4749(4) 0.0480(15) Uani 1 d . . .
O23 O 0.8600(6) -0.2772(5) 0.6275(4) 0.0348(12) Uani 1 d . . .
N31 N 0.7629(6) -0.0400(5) 0.7816(4) 0.0250(12) Uani 1 d D . .
C32 C 0.6920(7) 0.0733(6) 0.7468(4) 0.0232(13) Uani 1 d D . .
H32 H 0.7363 0.1229 0.7021 0.028 Uiso 1 calc R . .
C33 C 0.5572(7) 0.1226(6) 0.7722(4) 0.0216(13) Uani 1 d D . .
C34 C 0.4938(8) 0.0491(7) 0.8376(5) 0.0296(15) Uani 1 d D . .
H34 H 0.4022 0.0797 0.8576 0.036 Uiso 1 calc R . .
C35 C 0.5647(8) -0.0679(7) 0.8730(5) 0.0343(17) Uani 1 d D . .
H35 H 0.5217 -0.1202 0.9167 0.041 Uiso 1 calc R . .
C36 C 0.6987(8) -0.1089(7) 0.8447(5) 0.0286(15) Uani 1 d D . .
H36 H 0.7480 -0.1892 0.8709 0.034 Uiso 1 calc R . .
N61 N 1.2064(6) -0.1753(5) 0.6766(4) 0.0243(12) Uani 1 d D . .
C62 C 1.2492(7) -0.3045(6) 0.6944(4) 0.0252(14) Uani 1 d D . .
H62 H 1.1959 -0.3530 0.7346 0.030 Uiso 1 calc R . .
C63 C 1.3666(7) -0.3693(6) 0.6574(4) 0.0246(14) Uani 1 d D . .
C64 C 1.4453(7) -0.2974(7) 0.5983(5) 0.0275(15) Uani 1 d D . .
H64 H 1.5274 -0.3385 0.5719 0.033 Uiso 1 calc R . .
C65 C 1.4010(8) -0.1659(7) 0.5794(5) 0.0308(15) Uani 1 d D . .
H65 H 1.4517 -0.1154 0.5389 0.037 Uiso 1 calc R . .
C66 C 1.2823(7) -0.1077(7) 0.6197(5) 0.0261(14) Uani 1 d D . .
H66 H 1.2534 -0.0166 0.6066 0.031 Uiso 1 calc R . .
N101 N 0.8881(7) 0.5293(6) 0.9164(5) 0.0374(15) Uani 1 d . . .
N102 N 0.8929(8) 0.5979(6) 1.0068(5) 0.0371(15) Uani 1 d . . .
C106 C 0.9981(8) 0.4328(6) 0.9127(6) 0.0322(16) Uani 1 d . . .
N131 N 1.0323(6) 0.1446(5) 0.7246(4) 0.0245(12) Uani 1 d . . .
C132 C 1.0344(8) 0.2257(7) 0.8114(5) 0.0287(15) Uani 1 d . . .
H13A H 1.0678 0.1869 0.8763 0.034 Uiso 1 calc R . .
C133 C 0.9923(9) 0.3593(6) 0.8134(6) 0.0325(16) Uani 1 d . . .
C134 C 0.9403(9) 0.4149(7) 0.7184(6) 0.0356(17) Uani 1 d . . .
H13B H 0.9053 0.5061 0.7159 0.043 Uiso 1 calc R . .
C135 C 0.9400(9) 0.3361(7) 0.6274(6) 0.0357(17) Uani 1 d . . .
H135 H 0.9091 0.3733 0.5616 0.043 Uiso 1 calc R . .
C136 C 0.9857(8) 0.2022(7) 0.6341(5) 0.0279(15) Uani 1 d . . .
H13E H 0.9839 0.1482 0.5715 0.033 Uiso 1 calc R . .
C1 C 0.565(3) -0.484(2) 0.9946(19) 0.075(6) Uiso 0.50 d P . .
Cl1 Cl 0.4160(9) -0.3793(8) 0.9821(6) 0.099(2) Uiso 0.50 d P . 1
Cl2 Cl 0.4975(10) -0.3728(8) 0.9435(7) 0.107(2) Uiso 0.50 d P . 2
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'
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
N61 Cd N31 166.99(18) . . y
N61 Cd N131 100.2(2) . . y
N31 Cd N131 90.2(2) . . y
N61 Cd O11 88.3(2) . . y
N31 Cd O11 89.3(2) . . y
N131 Cd O11 137.5(2) . . y
N61 Cd O21 90.0(2) . . y
N31 Cd O21 83.2(2) . . y
N131 Cd O21 84.6(2) . . y
O11 Cd O21 137.37(19) . . ?
N61 Cd O12 93.0(2) . . ?
N31 Cd O12 95.7(2) . . ?
N131 Cd O12 84.5(2) . . ?
O11 Cd O12 53.3(2) . . ?
O21 Cd O12 169.12(17) . . ?
N61 Cd O23 83.9(2) . . ?
N31 Cd O23 83.2(2) . . ?
N131 Cd O23 136.8(2) . . ?
O11 Cd O23 85.3(2) . . ?
O21 Cd O23 52.2(2) . . ?
O12 Cd O23 138.5(2) . . ?
N2 N1 C6 117.7(5) . . ?
N1 N2 C3 117.2(6) . . ?
N2 C3 N4 125.4(6) . . ?
N2 C3 C63 116.9(6) . 1_465 ?
N4 C3 C63 117.7(6) . 1_465 ?
N5 N4 C3 117.7(5) . . ?
N4 N5 C6 116.8(6) . . ?
N1 C6 N5 124.9(6) . . ?
N1 C6 C33 117.4(6) . . ?
N5 C6 C33 117.7(6) . . ?
O13 N10 O12 122.2(6) . . ?
O13 N10 O11 120.6(6) . . ?
O12 N10 O11 117.1(6) . . ?
N10 O11 Cd 96.2(4) . . ?
N10 O12 Cd 93.3(4) . . ?
O22 N20 O23 122.4(6) . . ?
O22 N20 O21 119.9(6) . . ?
O23 N20 O21 117.7(6) . . ?
N20 O21 Cd 97.5(4) . . ?
N20 O23 Cd 92.4(4) . . ?
C32 N31 C36 117.4(6) . . ?
C32 N31 Cd 115.9(4) . . ?
C36 N31 Cd 126.5(4) . . ?
N31 C32 C33 123.6(6) . . ?
C34 C33 C32 117.6(6) . . ?
C34 C33 C6 124.5(6) . . ?
C32 C33 C6 117.7(6) . . ?
C35 C34 C33 119.3(6) . . ?
C34 C35 C36 119.4(6) . . ?
N31 C36 C35 122.7(6) . . ?
C66 N61 C62 117.9(6) . . ?
C66 N61 Cd 123.7(4) . . ?
C62 N61 Cd 118.3(4) . . ?
N61 C62 C63 123.2(6) . . ?
C62 C63 C64 118.3(6) . . ?
C62 C63 C3 120.4(6) . 1_645 ?
C64 C63 C3 121.3(6) . 1_645 ?
C65 C64 C63 118.6(6) . . ?
C64 C65 C66 119.7(6) . . ?
N61 C66 C65 122.3(6) . . ?
N102 N101 C106 116.9(7) . . ?
N101 N102 C106 118.4(6) . 2_767 ?
N102 C106 N101 124.6(7) 2_767 . ?
N102 C106 C133 119.0(6) 2_767 . ?
N101 C106 C133 116.4(7) . . ?
C136 N131 C132 116.1(6) . . ?
C136 N131 Cd 121.6(5) . . ?
C132 N131 Cd 116.3(5) . . ?
N131 C132 C133 125.3(7) . . ?
C132 C133 C134 117.2(7) . . ?
C132 C133 C106 118.9(7) . . ?
C134 C133 C106 123.8(7) . . ?
C135 C134 C133 119.4(7) . . ?
C136 C135 C134 118.6(7) . . ?
N131 C136 C135 123.4(7) . . ?
C1 C1 Cl2 88(2) 2_647 . ?
C1 C1 Cl1 77(2) 2_647 2_647 ?
Cl2 C1 Cl1 157(2) . 2_647 ?
C1 C1 Cl1 55.8(18) 2_647 . ?
Cl2 C1 Cl1 36.4(7) . . ?
Cl1 C1 Cl1 132.4(15) 2_647 . ?
C1 C1 Cl2 48.8(18) 2_647 2_647 ?
Cl2 C1 Cl2 137.1(15) . 2_647 ?
Cl1 C1 Cl2 31.7(6) 2_647 2_647 ?
Cl1 C1 Cl2 102.9(12) . 2_647 ?
C1 Cl1 C1 47.6(15) 2_647 . ?
C1 Cl2 C1 42.9(15) . 2_647 ?
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
Cd N61 2.305(7) . y
Cd N31 2.343(7) . y
Cd N131 2.348(7) . y
Cd O11 2.362(6) . y
Cd O21 2.389(6) . y
Cd O12 2.438(7) . y
Cd O23 2.507(7) . y
N1 N2 1.320(8) . ?
N1 C6 1.336(9) . ?
N2 C3 1.331(9) . ?
C3 N4 1.338(9) . ?
C3 C63 1.475(9) 1_465 ?
N4 N5 1.320(8) . ?
N5 C6 1.349(9) . ?
C6 C33 1.468(9) . ?
N10 O13 1.220(8) . ?
N10 O12 1.248(8) . ?
N10 O11 1.275(8) . ?
N20 O22 1.230(8) . ?
N20 O23 1.251(8) . ?
N20 O21 1.269(8) . ?
N31 C32 1.336(8) . ?
N31 C36 1.344(9) . ?
C32 C33 1.389(9) . ?
C33 C34 1.389(9) . ?
C34 C35 1.369(10) . ?
C35 C36 1.375(10) . ?
N61 C66 1.342(9) . ?
N61 C62 1.349(8) . ?
C62 C63 1.377(9) . ?
C63 C64 1.402(9) . ?
C63 C3 1.475(9) 1_645 ?
C64 C65 1.377(10) . ?
C65 C66 1.382(10) . ?
N101 N102 1.323(9) . ?
N101 C106 1.360(9) . ?
N102 C106 1.327(10) 2_767 ?
C106 N102 1.327(10) 2_767 ?
C106 C133 1.445(10) . ?
N131 C136 1.339(9) . ?
N131 C132 1.349(8) . ?
C132 C133 1.368(10) . ?
C133 C134 1.387(11) . ?
C134 C135 1.385(11) . ?
C135 C136 1.382(10) . ?
C1 C1 1.26(4) 2_647 ?
C1 Cl2 1.39(2) . ?
C1 Cl1 1.41(2) 2_647 ?
C1 Cl1 1.66(3) . ?
C1 Cl2 1.85(3) 2_647 ?
Cl1 C1 1.41(2) 2_647 ?
Cl2 C1 1.85(3) 2_647 ?
