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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/1/50/92/1509257.cif $
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#
# 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_1509257
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 H26 N12 O6 Zn, C12 H10 N2'
_chemical_formula_sum            'C36 H36 N14 O6 Zn'
_chemical_formula_weight         826.16
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.884(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.686(6)
_cell_length_b                   11.464(3)
_cell_length_c                   13.894(3)
_cell_measurement_reflns_used    1821
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.3
_cell_volume                     3547.8(15)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.903
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10946
_diffrn_reflns_theta_full        26.60
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0.1
_diffrn_standards_number         116
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.147
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.565
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3990
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.565
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0991
_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          0.2436
_refine_ls_wR_factor_ref         0.2527
_reflns_number_gt                3135
_reflns_number_total             3990
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            znaxt2py.cif
_cod_data_source_block           znaxt2py
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1509257
_cod_database_fobs_code          1509257
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 0.2500 0.2500 0.5000 0.0114(3) Uani 1 2 d S
N1 N 0.34499(19) 0.0610(4) 0.5537(3) 0.0183(10) Uani 1 1 d .
N2 N 0.34068(19) 0.1769(4) 0.5549(3) 0.0169(9) Uani 1 1 d .
N3 N 0.39505(19) 0.2308(4) 0.5813(3) 0.0163(9) Uani 1 1 d .
C3A C 0.4345(2) 0.1431(4) 0.5978(4) 0.0137(10) Uani 1 1 d .
N4 N 0.49625(18) 0.1504(4) 0.6256(3) 0.0166(9) Uani 1 1 d .
C4 C 0.5276(3) 0.2628(5) 0.6394(5) 0.0234(12) Uani 1 1 d .
H41 H 0.5557 0.2694 0.7097 0.028 Uiso 1 1 d R
H42 H 0.4982 0.3263 0.6257 0.028 Uiso 1 1 d R
H43 H 0.5497 0.2679 0.5914 0.028 Uiso 1 1 d R
C5 C 0.5293(2) 0.0494(5) 0.6391(4) 0.0186(11) Uani 1 1 d .
O5 O 0.58396(17) 0.0505(4) 0.6636(3) 0.0255(9) Uani 1 1 d .
N6 N 0.49793(19) -0.0567(4) 0.6234(3) 0.0176(10) Uani 1 1 d .
C6 C 0.5351(2) -0.1631(5) 0.6425(4) 0.0226(12) Uani 1 1 d .
H61 H 0.5637 -0.1588 0.6056 0.027 Uiso 1 1 d R
H62 H 0.5091 -0.2313 0.6190 0.027 Uiso 1 1 d R
H63 H 0.5572 -0.1703 0.7161 0.027 Uiso 1 1 d R
C7 C 0.4352(2) -0.0722(5) 0.5924(4) 0.0164(11) Uani 1 1 d .
O7 O 0.41277(17) -0.1698(3) 0.5798(3) 0.0265(9) Uani 1 1 d .
C7A C 0.4042(2) 0.0376(4) 0.5805(4) 0.0157(11) Uani 1 1 d .
N1P N 0.25001(18) 0.2630(3) 0.6614(3) 0.0113(8) Uiso 1 1 d .
C2P C 0.2928(3) 0.2107(5) 0.7373(4) 0.0240(12) Uiso 1 1 d .
H2P H 0.3245 0.1721 0.7228 0.029 Uiso 1 1 d R
C3P C 0.2914(3) 0.2123(6) 0.8380(5) 0.0366(16) Uiso 1 1 d .
H3P H 0.3222 0.1742 0.8911 0.044 Uiso 1 1 d R
C4P C 0.2456(3) 0.2682(6) 0.8583(6) 0.0414(17) Uiso 1 1 d .
C5P C 0.2030(3) 0.3244(6) 0.7801(5) 0.0359(15) Uiso 1 1 d .
H5P H 0.1720 0.3670 0.7931 0.043 Uiso 1 1 d R
C6P C 0.2066(3) 0.3203(5) 0.6840(4) 0.0248(12) Uiso 1 1 d .
H6P H 0.1758 0.3586 0.6310 0.030 Uiso 1 1 d R
C7P C 0.2323(4) 0.2740(7) 0.9617(6) 0.051(2) Uiso 1 1 d .
H7P H 0.1986 0.3150 0.9668 0.061 Uiso 1 1 d R
N1Q N 0.1586(2) 0.0320(4) 0.6197(4) 0.0229(11) Uani 1 1 d .
C2Q C 0.1012(3) 0.0532(4) 0.5681(4) 0.0216(12) Uani 1 1 d .
H2Q H 0.0897 0.0670 0.4966 0.026 Uiso 1 1 d R
C3Q C 0.0574(3) 0.0580(5) 0.6136(4) 0.0214(12) Uani 1 1 d .
H3Q H 0.0168 0.0715 0.5726 0.026 Uiso 1 1 d R
C4Q C 0.0732(2) 0.0431(4) 0.7186(4) 0.0194(12) Uani 1 1 d .
C5Q C 0.1332(2) 0.0206(5) 0.7721(4) 0.0233(12) Uani 1 1 d .
H5Q H 0.1463 0.0077 0.8439 0.028 Uiso 1 1 d R
C6Q C 0.1740(2) 0.0161(5) 0.7212(5) 0.0264(13) Uani 1 1 d .
H6Q H 0.2149 0.0013 0.7593 0.032 Uiso 1 1 d R
C7Q C 0.0299(2) 0.0465(4) 0.7725(4) 0.0195(11) Uani 1 1 d .
H7Q H 0.0452 0.0476 0.8452 0.023 Uiso 1 1 d R
O1W O 0.22260(16) 0.0742(3) 0.4949(3) 0.0170(8) Uani 1 1 d D
H11W H 0.202(2) 0.060(5) 0.532(4) 0.020 Uiso 1 1 d D
H12W H 0.2586(10) 0.052(5) 0.519(4) 0.020 Uiso 1 1 d 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'
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
O1W Zn O1W 180.0 7_556 .
O1W Zn N2 95.72(15) 7_556 .
O1W Zn N2 84.28(15) . .
O1W Zn N2 84.28(15) 7_556 7_556
O1W Zn N2 95.72(15) . 7_556
N2 Zn N2 179.998(1) . 7_556
O1W Zn N1P 89.55(14) 7_556 7_556
O1W Zn N1P 90.45(14) . 7_556
N2 Zn N1P 89.40(15) . 7_556
N2 Zn N1P 90.60(15) 7_556 7_556
O1W Zn N1P 90.45(14) 7_556 .
O1W Zn N1P 89.55(14) . .
N2 Zn N1P 90.61(15) . .
N2 Zn N1P 89.39(15) 7_556 .
N1P Zn N1P 179.997(1) 7_556 .
N2 N1 C7A 105.8(4) . .
N1 N2 N3 112.7(4) . .
N1 N2 Zn 116.6(3) . .
N3 N2 Zn 130.3(3) . .
C3A N3 N2 104.3(4) . .
N3 C3A N4 127.8(5) . .
N3 C3A C7A 109.6(4) . .
N4 C3A C7A 122.6(5) . .
C5 N4 C3A 119.1(4) . .
C5 N4 C4 118.9(4) . .
C3A N4 C4 122.0(4) . .
N4 C4 H41 109.9 . .
N4 C4 H42 109.4 . .
H41 C4 H42 109.5 . .
N4 C4 H43 109.1 . .
H41 C4 H43 109.4 . .
H42 C4 H43 109.5 . .
O5 C5 N4 122.0(5) . .
O5 C5 N6 120.4(5) . .
N4 C5 N6 117.5(4) . .
C5 N6 C7 127.2(4) . .
C5 N6 C6 115.9(4) . .
C7 N6 C6 116.9(4) . .
N6 C6 H61 109.9 . .
N6 C6 H62 109.3 . .
H61 C6 H62 109.5 . .
N6 C6 H63 109.3 . .
H61 C6 H63 109.5 . .
H62 C6 H63 109.5 . .
O7 C7 N6 121.3(5) . .
O7 C7 C7A 127.1(5) . .
N6 C7 C7A 111.6(4) . .
N1 C7A C3A 107.6(4) . .
N1 C7A C7 130.4(5) . .
C3A C7A C7 122.0(5) . .
C2P N1P C6P 118.2(5) . .
C2P N1P Zn 120.2(4) . .
C6P N1P Zn 121.7(3) . .
N1P C2P C3P 120.7(6) . .
N1P C2P H2P 119.0 . .
C3P C2P H2P 120.3 . .
C4P C3P C2P 119.9(6) . .
C4P C3P H3P 120.6 . .
C2P C3P H3P 119.5 . .
C5P C4P C3P 118.6(7) . .
C5P C4P C7P 112.5(6) . .
C3P C4P C7P 128.8(7) . .
C4P C5P C6P 119.0(7) . .
C4P C5P H5P 120.1 . .
C6P C5P H5P 120.8 . .
N1P C6P C5P 123.5(5) . .
N1P C6P H6P 119.5 . .
C5P C6P H6P 117.0 . .
C7P C7P C4P 118.7(11) 7_557 .
C7P C7P H7P 119.8 7_557 .
C4P C7P H7P 121.6 . .
C2Q N1Q C6Q 117.0(5) . .
N1Q C2Q C3Q 123.3(5) . .
N1Q C2Q H2Q 118.3 . .
C3Q C2Q H2Q 118.4 . .
C2Q C3Q C4Q 119.9(5) . .
C2Q C3Q H3Q 119.8 . .
C4Q C3Q H3Q 120.3 . .
C5Q C4Q C3Q 116.5(5) . .
C5Q C4Q C7Q 120.1(5) . .
C3Q C4Q C7Q 123.4(5) . .
C6Q C5Q C4Q 120.1(5) . .
C6Q C5Q H5Q 119.8 . .
C4Q C5Q H5Q 120.1 . .
N1Q C6Q C5Q 123.1(5) . .
N1Q C6Q H6Q 118.1 . .
C5Q C6Q H6Q 118.8 . .
C7Q C7Q C4Q 125.1(7) 2_556 .
C7Q C7Q H7Q 117.4 2_556 .
C4Q C7Q H7Q 117.5 . .
Zn O1W H11W 114(4) . .
Zn O1W H12W 91(4) . .
H11W O1W H12W 114(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn O1W 2.111(4) 7_556
Zn O1W 2.111(4) .
Zn N2 2.187(4) .
Zn N2 2.187(4) 7_556
Zn N1P 2.248(4) 7_556
Zn N1P 2.248(4) .
N1 N2 1.334(6) .
N1 C7A 1.349(7) .
N2 N3 1.361(6) .
N3 C3A 1.338(6) .
C3A N4 1.383(6) .
C3A C7A 1.385(7) .
N4 C5 1.374(7) .
N4 C4 1.466(6) .
C4 H41 0.9802 .
C4 H42 0.9802 .
C4 H43 0.9802 .
C5 O5 1.222(6) .
C5 N6 1.403(7) .
N6 C7 1.411(7) .
N6 C6 1.476(6) .
C6 H61 0.9801 .
C6 H62 0.9801 .
C6 H63 0.9801 .
C7 O7 1.224(6) .
C7 C7A 1.439(7) .
N1P C2P 1.332(7) .
N1P C6P 1.344(7) .
C2P C3P 1.410(9) .
C2P H2P 0.9500 .
C3P C4P 1.369(10) .
C3P H3P 0.9500 .
C4P C5P 1.366(9) .
C4P C7P 1.574(12) .
C5P C6P 1.367(9) .
C5P H5P 0.9500 .
C6P H6P 0.9500 .
C7P C7P 1.238(16) 7_557
C7P H7P 0.9500 .
N1Q C2Q 1.325(7) .
N1Q C6Q 1.344(7) .
C2Q C3Q 1.386(8) .
C2Q H2Q 0.9500 .
C3Q C4Q 1.389(8) .
C3Q H3Q 0.9500 .
C4Q C5Q 1.386(7) .
C4Q C7Q 1.462(8) .
C5Q C6Q 1.378(8) .
C5Q H5Q 0.9500 .
C6Q H6Q 0.9500 .
C7Q C7Q 1.338(10) 2_556
C7Q H7Q 0.9498 .
O1W H11W 0.841(10) .
O1W H12W 0.842(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H12W N1 0.842(10) 1.94(3) 2.736(6) 157(6)
O1W H11W N1Q 0.841(10) 1.866(12) 2.706(6) 178(6)
