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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/92/1509258.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_1509258
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quirós'
'Juan M. Salas'
_publ_contact_author_address
;
Departamento de Química Inorgánica, Facultad de Ciencias,
c/ Severo Ochoa s/n, 18071 Granada, Spain
;
_publ_contact_author_email       jsalas@ugr.es
_publ_contact_author_fax         '34 958 248526'
_publ_contact_author_name        'Juan M. Salas'
_publ_contact_author_phone       '34 958 248525'
_publ_section_title
;
 One-dimensional zinc(II) polymers with 4,6-dimethyl-1,2,3-triazolo[4,5-d]
 pyrimidin-5,7-dionato built by bipyridyl-based ligands acting as spacers
 both in the first and in the second sphere
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              371
_journal_page_last               376
_journal_paper_doi               10.1016/j.ica.2010.09.048
_journal_volume                  365
_journal_year                    2011
_chemical_formula_moiety         'C24 H24 N12 O4 Zn'
_chemical_formula_sum            'C24 H24 N12 O4 Zn'
_chemical_formula_weight         609.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.511(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.684(6)
_cell_length_b                   16.797(5)
_cell_length_c                   16.731(5)
_cell_measurement_reflns_used    3183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.4
_cell_volume                     5246(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'φ and ω 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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16414
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0.1
_diffrn_standards_number         212
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+6.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                4423
_reflns_number_total             5928
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            znbpeax.cif
_cod_data_source_block           znbpeax
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1509258
_cod_database_fobs_code          1509258
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Zn Zn 0.255942(18) 0.51533(2) 0.29854(2) 0.02031(11) Uani 1 1 d .
N1A N 0.15464(13) 0.41720(15) 0.32931(16) 0.0227(6) Uani 1 1 d .
N2A N 0.17232(13) 0.49150(15) 0.32171(16) 0.0229(6) Uani 1 1 d .
N3A N 0.12982(13) 0.54754(15) 0.33495(16) 0.0234(6) Uani 1 1 d .
C3AA C 0.08362(16) 0.50311(17) 0.35187(18) 0.0212(7) Uani 1 1 d .
N4A N 0.02827(13) 0.53067(15) 0.37026(17) 0.0232(6) Uani 1 1 d .
C4A C 0.01531(18) 0.61572(19) 0.3736(2) 0.0336(8) Uani 1 1 d .
H41A H -0.0216 0.6329 0.3161 0.040 Uiso 1 1 d R
H42A H 0.0596 0.6454 0.3872 0.040 Uiso 1 1 d R
H43A H -0.0010 0.6259 0.4197 0.040 Uiso 1 1 d R
C5A C -0.01542(16) 0.47673(19) 0.3846(2) 0.0248(7) Uani 1 1 d .
O5A O -0.06570(12) 0.49813(14) 0.39916(16) 0.0322(6) Uani 1 1 d .
N6A N 0.00040(13) 0.39526(15) 0.38193(16) 0.0228(6) Uani 1 1 d .
C6A C -0.04750(17) 0.3374(2) 0.3936(2) 0.0326(8) Uani 1 1 d .
H61A H -0.0737 0.3083 0.3382 0.039 Uiso 1 1 d R
H62A H -0.0816 0.3655 0.4099 0.039 Uiso 1 1 d R
H63A H -0.0195 0.2999 0.4407 0.039 Uiso 1 1 d R
C7A C 0.05594(16) 0.36301(19) 0.36490(19) 0.0227(7) Uani 1 1 d .
O7A O 0.06421(12) 0.29119(13) 0.36490(15) 0.0309(5) Uani 1 1 d .
C7AA C 0.09741(15) 0.42397(17) 0.34886(18) 0.0201(6) Uani 1 1 d .
N1B N 0.36826(14) 0.59718(16) 0.43979(16) 0.0267(6) Uani 1 1 d .
N2B N 0.34283(14) 0.52570(15) 0.40978(16) 0.0254(6) Uani 1 1 d .
N3B N 0.37879(14) 0.46414(16) 0.46530(17) 0.0266(6) Uani 1 1 d .
C3AB C 0.42904(16) 0.50233(18) 0.53308(19) 0.0237(7) Uani 1 1 d .
N4B N 0.48143(13) 0.46753(15) 0.60848(16) 0.0247(6) Uani 1 1 d .
C4B C 0.48110(17) 0.38183(19) 0.6221(2) 0.0302(7) Uani 1 1 d .
H41B H 0.4900 0.3542 0.5762 0.036 Uiso 1 1 d R
H42B H 0.4344 0.3656 0.6185 0.036 Uiso 1 1 d R
H43B H 0.5187 0.3680 0.6805 0.036 Uiso 1 1 d R
C5B C 0.53011(16) 0.51541(19) 0.6720(2) 0.0239(7) Uani 1 1 d .
O5B O 0.57743(11) 0.48855(13) 0.73925(15) 0.0302(5) Uani 1 1 d .
N6B N 0.52364(13) 0.59843(15) 0.65664(17) 0.0249(6) Uani 1 1 d .
C6B C 0.57754(17) 0.6490(2) 0.7237(2) 0.0316(8) Uani 1 1 d .
H61B H 0.6137 0.6648 0.7036 0.038 Uiso 1 1 d R
H62B H 0.6006 0.6192 0.7792 0.038 Uiso 1 1 d R
H63B H 0.5546 0.6967 0.7335 0.038 Uiso 1 1 d R
C7B C 0.47334(17) 0.6376(2) 0.5815(2) 0.0278(7) Uani 1 1 d .
O7B O 0.47453(13) 0.71009(14) 0.57473(16) 0.0397(6) Uani 1 1 d .
C7AB C 0.42467(16) 0.58338(18) 0.52007(19) 0.0223(6) Uani 1 1 d .
N1P N 0.24593(13) 0.61884(14) 0.23417(16) 0.0196(5) Uani 1 1 d .
C2P C 0.30530(15) 0.65398(17) 0.23573(19) 0.0199(6) Uani 1 1 d .
H2P H 0.3505 0.6416 0.2827 0.024 Uiso 1 1 d R
C3P C 0.30267(16) 0.70684(17) 0.17196(18) 0.0203(6) Uani 1 1 d .
H3P H 0.3454 0.7306 0.1751 0.024 Uiso 1 1 d R
C4P C 0.23699(16) 0.72538(17) 0.10264(19) 0.0195(6) Uani 1 1 d .
C5P C 0.17590(16) 0.69216(19) 0.1035(2) 0.0254(7) Uani 1 1 d .
H5P H 0.1300 0.7059 0.0589 0.031 Uiso 1 1 d R
C6P C 0.18204(16) 0.63923(19) 0.1693(2) 0.0246(7) Uani 1 1 d .
H6P H 0.1399 0.6164 0.1688 0.030 Uiso 1 1 d R
C7P C 0.23449(17) 0.77447(18) 0.02663(19) 0.0235(7) Uani 1 1 d .
H71P H 0.2628 0.8237 0.0491 0.028 Uiso 1 1 d R
H72P H 0.1844 0.7897 -0.0120 0.028 Uiso 1 1 d R
N1Q N 0.25294(12) 0.43824(15) 0.20333(16) 0.0203(5) Uani 1 1 d .
C2Q C 0.23209(15) 0.36199(19) 0.2031(2) 0.0243(7) Uani 1 1 d .
H2Q H 0.2246 0.3435 0.2522 0.029 Uiso 1 1 d R
C3Q C 0.22126(17) 0.31039(19) 0.1353(2) 0.0272(7) Uani 1 1 d .
H3Q H 0.2073 0.2570 0.1383 0.033 Uiso 1 1 d R
C4Q C 0.23076(15) 0.33572(18) 0.06176(19) 0.0215(6) Uani 1 1 d .
C5Q C 0.25294(16) 0.41354(19) 0.0631(2) 0.0262(7) Uani 1 1 d .
H5Q H 0.2609 0.4334 0.0150 0.031 Uiso 1 1 d R
C6Q C 0.26356(16) 0.46233(19) 0.13376(19) 0.0240(7) Uani 1 1 d .
H6Q H 0.2792 0.5154 0.1331 0.029 Uiso 1 1 d R
C7Q C 0.21880(16) 0.27965(18) -0.0130(2) 0.0249(7) Uani 1 1 d .
H71Q H 0.2145 0.3104 -0.0656 0.030 Uiso 1 1 d R
H72Q H 0.1735 0.2501 -0.0289 0.030 Uiso 1 1 d 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'
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
N2B Zn N2A 110.79(11) . .
N2B Zn N1P 105.83(10) . .
N2A Zn N1P 112.64(10) . .
N2B Zn N1Q 120.44(10) . .
N2A Zn N1Q 106.97(10) . .
N1P Zn N1Q 99.78(10) . .
N2A N1A C7AA 104.4(2) . .
N1A N2A N3A 114.2(2) . .
N1A N2A Zn 120.89(19) . .
N3A N2A Zn 124.85(19) . .
C3AA N3A N2A 102.6(2) . .
N3A C3AA C7AA 110.9(3) . .
N3A C3AA N4A 126.5(3) . .
C7AA C3AA N4A 122.6(3) . .
C5A N4A C3AA 119.2(3) . .
C5A N4A C4A 119.6(3) . .
C3AA N4A C4A 121.2(3) . .
N4A C4A H41A 109.2 . .
N4A C4A H42A 109.8 . .
H41A C4A H42A 109.5 . .
N4A C4A H43A 109.5 . .
H41A C4A H43A 109.5 . .
H42A C4A H43A 109.5 . .
O5A C5A N4A 121.5(3) . .
O5A C5A N6A 121.4(3) . .
N4A C5A N6A 117.1(3) . .
C7A N6A C5A 126.9(3) . .
C7A N6A C6A 115.6(3) . .
C5A N6A C6A 117.4(2) . .
N6A C6A H61A 109.6 . .
N6A C6A H62A 109.2 . .
H61A C6A H62A 109.5 . .
N6A C6A H63A 109.7 . .
H61A C6A H63A 109.5 . .
H62A C6A H63A 109.5 . .
O7A C7A N6A 120.6(3) . .
O7A C7A C7AA 127.7(3) . .
N6A C7A C7AA 111.7(3) . .
N1A C7AA C3AA 107.9(3) . .
N1A C7AA C7A 129.6(3) . .
C3AA C7AA C7A 122.5(3) . .
N2B N1B C7AB 104.5(2) . .
N1B N2B N3B 114.6(2) . .
N1B N2B Zn 119.6(2) . .
N3B N2B Zn 125.6(2) . .
C3AB N3B N2B 102.1(2) . .
N3B C3AB C7AB 111.7(3) . .
N3B C3AB N4B 126.2(3) . .
C7AB C3AB N4B 122.2(3) . .
C5B N4B C3AB 118.9(3) . .
C5B N4B C4B 120.7(3) . .
C3AB N4B C4B 120.2(3) . .
N4B C4B H41B 109.3 . .
N4B C4B H42B 109.6 . .
H41B C4B H42B 109.5 . .
N4B C4B H43B 109.5 . .
H41B C4B H43B 109.5 . .
H42B C4B H43B 109.5 . .
O5B C5B N4B 122.1(3) . .
O5B C5B N6B 120.6(3) . .
N4B C5B N6B 117.3(3) . .
C7B N6B C5B 127.0(3) . .
C7B N6B C6B 116.1(3) . .
C5B N6B C6B 116.9(2) . .
N6B C6B H61B 109.5 . .
N6B C6B H62B 109.1 . .
H61B C6B H62B 109.5 . .
N6B C6B H63B 109.8 . .
H61B C6B H63B 109.5 . .
H62B C6B H63B 109.5 . .
O7B C7B N6B 120.8(3) . .
O7B C7B C7AB 127.5(3) . .
N6B C7B C7AB 111.6(3) . .
N1B C7AB C3AB 107.1(3) . .
N1B C7AB C7B 130.0(3) . .
C3AB C7AB C7B 123.0(3) . .
C6P N1P C2P 118.3(2) . .
C6P N1P Zn 119.5(2) . .
C2P N1P Zn 118.97(19) . .
N1P C2P C3P 122.4(3) . .
N1P C2P H2P 118.8 . .
C3P C2P H2P 118.8 . .
C2P C3P C4P 119.4(3) . .
C2P C3P H3P 120.3 . .
C4P C3P H3P 120.2 . .
C5P C4P C3P 117.9(3) . .
C5P C4P C7P 122.1(3) . .
C3P C4P C7P 119.7(3) . .
C6P C5P C4P 119.8(3) . .
C6P C5P H5P 120.1 . .
C4P C5P H5P 120.1 . .
N1P C6P C5P 122.0(3) . .
N1P C6P H6P 119.0 . .
C5P C6P H6P 119.1 . .
C4P C7P C7P 109.1(3) . 7_565
C4P C7P H71P 109.9 . .
C7P C7P H71P 109.8 7_565 .
C4P C7P H72P 109.9 . .
C7P C7P H72P 109.9 7_565 .
H71P C7P H72P 108.3 . .
C6Q N1Q C2Q 117.2(3) . .
C6Q N1Q Zn 121.9(2) . .
C2Q N1Q Zn 120.5(2) . .
N1Q C2Q C3Q 122.7(3) . .
N1Q C2Q H2Q 118.6 . .
C3Q C2Q H2Q 118.7 . .
C2Q C3Q C4Q 120.3(3) . .
C2Q C3Q H3Q 119.9 . .
C4Q C3Q H3Q 119.8 . .
C5Q C4Q C3Q 116.5(3) . .
C5Q C4Q C7Q 122.8(3) . .
C3Q C4Q C7Q 120.7(3) . .
C6Q C5Q C4Q 120.4(3) . .
C6Q C5Q H5Q 119.8 . .
C4Q C5Q H5Q 119.7 . .
N1Q C6Q C5Q 122.8(3) . .
N1Q C6Q H6Q 118.6 . .
C5Q C6Q H6Q 118.6 . .
C4Q C7Q C7Q 110.7(3) . 7
C4Q C7Q H71Q 109.5 . .
C7Q C7Q H71Q 109.5 7 .
C4Q C7Q H72Q 109.6 . .
C7Q C7Q H72Q 109.5 7 .
H71Q C7Q H72Q 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn N2B 1.960(3) .
Zn N2A 1.970(3) .
Zn N1P 2.008(2) .
Zn N1Q 2.033(2) .
N1A N2A 1.322(3) .
N1A C7AA 1.362(4) .
N2A N3A 1.369(3) .
N3A C3AA 1.335(4) .
C3AA C7AA 1.365(4) .
C3AA N4A 1.387(4) .
N4A C5A 1.372(4) .
N4A C4A 1.459(4) .
C4A H41A 0.9800 .
C4A H42A 0.9800 .
C4A H43A 0.9800 .
C5A O5A 1.219(4) .
C5A N6A 1.412(4) .
N6A C7A 1.406(4) .
N6A C6A 1.460(4) .
C6A H61A 0.9800 .
C6A H62A 0.9800 .
C6A H63A 0.9800 .
C7A O7A 1.218(4) .
C7A C7AA 1.433(4) .
N1B N2B 1.320(4) .
N1B C7AB 1.367(4) .
N2B N3B 1.375(4) .
N3B C3AB 1.328(4) .
C3AB C7AB 1.376(4) .
C3AB N4B 1.389(4) .
N4B C5B 1.367(4) .
N4B C4B 1.458(4) .
C4B H41B 0.9800 .
C4B H42B 0.9800 .
C4B H43B 0.9800 .
C5B O5B 1.216(4) .
C5B N6B 1.414(4) .
N6B C7B 1.404(4) .
N6B C6B 1.466(4) .
C6B H61B 0.9800 .
C6B H62B 0.9800 .
C6B H63B 0.9800 .
C7B O7B 1.223(4) .
C7B C7AB 1.417(4) .
N1P C6P 1.344(4) .
N1P C2P 1.352(4) .
C2P C3P 1.371(4) .
C2P H2P 0.9500 .
C3P C4P 1.389(4) .
C3P H3P 0.9500 .
C4P C5P 1.387(4) .
C4P C7P 1.498(4) .
C5P C6P 1.378(4) .
C5P H5P 0.9500 .
C6P H6P 0.9500 .
C7P C7P 1.541(6) 7_565
C7P H71P 0.9900 .
C7P H72P 0.9900 .
N1Q C6Q 1.337(4) .
N1Q C2Q 1.351(4) .
C2Q C3Q 1.368(4) .
C2Q H2Q 0.9500 .
C3Q C4Q 1.393(4) .
C3Q H3Q 0.9500 .
C4Q C5Q 1.382(4) .
C4Q C7Q 1.499(4) .
C5Q C6Q 1.376(4) .
C5Q H5Q 0.9500 .
C6Q H6Q 0.9500 .
C7Q C7Q 1.537(6) 7
C7Q H71Q 0.9900 .
C7Q H72Q 0.9900 .
