#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:44:41 +0100 (vie 25 de mar de 2016) $
#$Revision: 179732 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/28/7002875.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_7002875
loop_
_publ_author_name
'Maldonado, Carmen R.'
'Quirós, Miguel'
'Salas, Juan M.'
'Rodríguez-Diéguez, Antonio'
_publ_section_title
;
 Versatile binding behaviour of
 4,6-dimethyl-1,2,3-triazolo[4,5-d]-pyrimidin-5,7-dionato in the
 presence of bipyrimidine. Supramolecular H-bond architectures
;
_journal_issue                   46
_journal_name_full               'Dalton Transactions'
_journal_page_first              10311
_journal_page_last               10317
_journal_paper_doi               10.1039/b913541c
_journal_year                    2009
_chemical_formula_moiety         'C32 H34 N24 O10 Zn2, 2(H2 O)'
_chemical_formula_sum            'C32 H38 N24 O12 Zn2'
_chemical_formula_weight         1081.60
_chemical_name_systematic
;
?
;
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.483(1)
_cell_angle_beta                 100.866(1)
_cell_angle_gamma                112.462(1)
_cell_formula_units_Z            1
_cell_length_a                   10.3170(9)
_cell_length_b                   10.3555(9)
_cell_length_c                   11.0667(9)
_cell_measurement_reflns_used    2899
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.4
_cell_volume                     1046.06(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      298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.920
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12383
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0.1
_diffrn_standards_number         108
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4771
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0423
_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+0.0400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                3798
_reflns_number_total             4771
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b913541c.txt
_cod_data_source_block           znaxbpir
_cod_database_code               7002875
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.48665(3) 0.32123(3) 0.26900(3) 0.03037(11) Uani 1 1 d . . .
N1A N 0.2044(2) 0.2867(2) 0.1366(2) 0.0323(5) Uani 1 1 d . . .
N2A N 0.2715(2) 0.2162(2) 0.1941(2) 0.0315(5) Uani 1 1 d . . .
N3A N 0.1785(2) 0.0890(2) 0.2102(2) 0.0323(5) Uani 1 1 d . . .
C3AA C 0.0485(3) 0.0818(3) 0.1590(2) 0.0279(5) Uani 1 1 d . . .
N4A N -0.0858(2) -0.0261(2) 0.1499(2) 0.0330(5) Uani 1 1 d . . .
C4A C -0.0969(3) -0.1534(3) 0.1991(3) 0.0470(8) Uani 1 1 d . . .
H41A H -0.1547 -0.1650 0.2588 0.056 Uiso 1 1 d R . .
H42A H -0.0014 -0.1427 0.2399 0.056 Uiso 1 1 d R . .
H43A H -0.1415 -0.2362 0.1304 0.056 Uiso 1 1 d R . .
C5A C -0.2083(3) -0.0152(3) 0.0913(2) 0.0338(6) Uani 1 1 d . . .
O5A O -0.3295(2) -0.1091(2) 0.08140(19) 0.0434(5) Uani 1 1 d . . .
N6A N -0.1932(2) 0.1065(2) 0.0437(2) 0.0340(5) Uani 1 1 d . . .
C6A C -0.3275(3) 0.1095(3) -0.0261(3) 0.0550(9) Uani 1 1 d . . .
H61A H -0.3785 0.1310 0.0322 0.066 Uiso 1 1 d R . .
H62A H -0.3879 0.0177 -0.0818 0.066 Uiso 1 1 d R . .
H63A H -0.3041 0.1818 -0.0745 0.066 Uiso 1 1 d R . .
C7A C -0.0624(3) 0.2244(3) 0.0534(3) 0.0336(6) Uani 1 1 d . . .
O7A O -0.0605(2) 0.3291(2) 0.0140(2) 0.0521(6) Uani 1 1 d . . .
C7AA C 0.0615(3) 0.2027(3) 0.1140(2) 0.0280(5) Uani 1 1 d . . .
N1B N 0.6405(2) 0.2507(2) 0.3053(2) 0.0341(5) Uani 1 1 d . . .
N2B N 0.6166(2) 0.1267(2) 0.3416(2) 0.0412(6) Uani 1 1 d . . .
N3B N 0.7432(3) 0.1168(2) 0.3828(2) 0.0419(6) Uani 1 1 d . . .
C3AB C 0.8466(3) 0.2377(3) 0.3709(2) 0.0305(6) Uani 1 1 d . . .
N4B N 0.9949(2) 0.2787(2) 0.4039(2) 0.0355(5) Uani 1 1 d . . .
C4B C 1.0587(3) 0.1940(3) 0.4679(3) 0.0461(8) Uani 1 1 d . . .
H41B H 1.1141 0.1655 0.4182 0.055 Uiso 1 1 d R . .
H42B H 0.9828 0.1103 0.4786 0.055 Uiso 1 1 d R . .
H43B H 1.1212 0.2507 0.5490 0.055 Uiso 1 1 d R . .
C5B C 1.0848(3) 0.4074(3) 0.3863(2) 0.0360(6) Uani 1 1 d . . .
O5B O 1.2160(2) 0.4487(2) 0.4162(2) 0.0527(6) Uani 1 1 d . . .
N6B N 1.0202(2) 0.4898(2) 0.3320(2) 0.0346(5) Uani 1 1 d . . .
C6B C 1.1185(3) 0.6208(3) 0.3031(3) 0.0510(8) Uani 1 1 d . . .
H61B H 1.0655 0.6460 0.2362 0.061 Uiso 1 1 d R . .
H62B H 1.1957 0.6046 0.2773 0.061 Uiso 1 1 d R . .
H63B H 1.1584 0.6977 0.3769 0.061 Uiso 1 1 d R . .
C7B C 0.8709(3) 0.4594(3) 0.3025(2) 0.0316(6) Uani 1 1 d . . .
O7B O 0.8260(2) 0.5438(2) 0.2650(2) 0.0445(5) Uani 1 1 d . . .
C7AB C 0.7863(3) 0.3221(3) 0.3230(2) 0.0295(6) Uani 1 1 d . . .
N1P N 0.5229(2) 0.5294(2) 0.34710(19) 0.0274(5) Uani 1 1 d . . .
C2P C 0.5166(2) 0.5592(2) 0.4661(2) 0.0258(5) Uani 1 1 d . . .
N3P N 0.5375(2) 0.6865(2) 0.5296(2) 0.0287(5) Uani 1 1 d . . .
C4P C 0.5635(3) 0.7919(3) 0.4675(3) 0.0368(6) Uani 1 1 d . . .
H4P H 0.5795 0.8827 0.5093 0.044 Uiso 1 1 d R . .
C5P C 0.5679(3) 0.7706(3) 0.3435(3) 0.0388(7) Uani 1 1 d . . .
H5P H 0.5833 0.8439 0.3000 0.047 Uiso 1 1 d R . .
C6P C 0.5481(3) 0.6360(3) 0.2859(3) 0.0341(6) Uani 1 1 d . . .
H6P H 0.5521 0.6188 0.2024 0.041 Uiso 1 1 d R . .
O1W O 0.5107(2) 0.3656(2) 0.09202(19) 0.0391(5) Uani 1 1 d D . .
H11W H 0.583(2) 0.405(3) 0.065(3) 0.047 Uiso 1 1 d D . .
H12W H 0.457(3) 0.293(2) 0.036(2) 0.047 Uiso 1 1 d D . .
O2W O 0.2812(2) 0.5468(3) 0.0357(2) 0.0516(6) Uani 1 1 d D . .
H21W H 0.204(2) 0.555(4) 0.012(3) 0.062 Uiso 1 1 d D . .
H22W H 0.259(4) 0.469(2) 0.060(3) 0.062 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
_geom_angle_publ_flag
N1B Zn N2A 131.33(9) . . ?
N1B Zn N1P 121.54(8) . . ?
N2A Zn N1P 105.76(8) . . ?
N1B Zn O1W 98.00(9) . . ?
N2A Zn O1W 89.23(8) . . ?
N1P Zn O1W 93.71(8) . . ?
N1B Zn N3P 88.67(8) . 2_666 ?
N2A Zn N3P 92.20(8) . 2_666 ?
N1P Zn N3P 76.13(8) . 2_666 ?
O1W Zn N3P 169.75(8) . 2_666 ?
N2A N1A C7AA 105.2(2) . . ?
N1A N2A N3A 113.19(19) . . ?
N1A N2A Zn 117.22(16) . . ?
N3A N2A Zn 128.74(16) . . ?
C3AA N3A N2A 103.8(2) . . ?
N3A C3AA C7AA 110.3(2) . . ?
N3A C3AA N4A 128.1(2) . . ?
C7AA C3AA N4A 121.6(2) . . ?
C5A N4A C3AA 119.4(2) . . ?
C5A N4A C4A 119.9(2) . . ?
C3AA N4A C4A 120.6(2) . . ?
N4A C4A H41A 109.9 . . ?
N4A C4A H42A 109.4 . . ?
H41A C4A H42A 109.5 . . ?
N4A C4A H43A 109.2 . . ?
H41A C4A H43A 109.5 . . ?
H42A C4A H43A 109.5 . . ?
O5A C5A N4A 121.2(3) . . ?
O5A C5A N6A 120.6(3) . . ?
N4A C5A N6A 118.2(2) . . ?
C5A N6A C7A 126.6(2) . . ?
C5A N6A C6A 116.4(2) . . ?
C7A N6A C6A 117.0(2) . . ?
N6A C6A H61A 109.6 . . ?
N6A C6A H62A 109.4 . . ?
H61A C6A H62A 109.5 . . ?
N6A C6A H63A 109.4 . . ?
H61A C6A H63A 109.5 . . ?
H62A C6A H63A 109.5 . . ?
O7A C7A N6A 121.8(2) . . ?
O7A C7A C7AA 126.7(2) . . ?
N6A C7A C7AA 111.6(2) . . ?
N1A C7AA C3AA 107.6(2) . . ?
N1A C7AA C7A 129.9(2) . . ?
C3AA C7AA C7A 122.6(2) . . ?
N2B N1B C7AB 107.4(2) . . ?
N2B N1B Zn 122.29(17) . . ?
C7AB N1B Zn 129.21(18) . . ?
N1B N2B N3B 110.4(2) . . ?
C3AB N3B N2B 105.6(2) . . ?
N3B C3AB C7AB 110.4(2) . . ?
N3B C3AB N4B 127.3(2) . . ?
C7AB C3AB N4B 122.2(2) . . ?
C5B N4B C3AB 119.3(2) . . ?
C5B N4B C4B 119.0(2) . . ?
C3AB N4B C4B 121.5(2) . . ?
N4B C4B H41B 109.5 . . ?
N4B C4B H42B 109.6 . . ?
H41B C4B H42B 109.5 . . ?
N4B C4B H43B 109.4 . . ?
H41B C4B H43B 109.5 . . ?
H42B C4B H43B 109.5 . . ?
O5B C5B N4B 121.4(3) . . ?
O5B C5B N6B 121.1(3) . . ?
N4B C5B N6B 117.5(2) . . ?
C5B N6B C7B 126.5(2) . . ?
C5B N6B C6B 116.2(2) . . ?
C7B N6B C6B 117.3(2) . . ?
N6B C6B H61B 109.4 . . ?
N6B C6B H62B 109.4 . . ?
H61B C6B H62B 109.5 . . ?
N6B C6B H63B 109.6 . . ?
H61B C6B H63B 109.5 . . ?
H62B C6B H63B 109.5 . . ?
O7B C7B N6B 121.7(2) . . ?
O7B C7B C7AB 126.9(2) . . ?
N6B C7B C7AB 111.4(2) . . ?
C3AB C7AB N1B 106.3(2) . . ?
C3AB C7AB C7B 122.8(2) . . ?
N1B C7AB C7B 130.9(2) . . ?
C2P N1P C6P 116.9(2) . . ?
C2P N1P Zn 118.06(16) . . ?
C6P N1P Zn 124.99(18) . . ?
N3P C2P N1P 125.4(2) . . ?
N3P C2P C2P 116.9(3) . 2_666 ?
N1P C2P C2P 117.6(3) . 2_666 ?
C2P N3P C4P 116.9(2) . . ?
C2P N3P Zn 111.24(16) . 2_666 ?
C4P N3P Zn 131.85(18) . 2_666 ?
N3P C4P C5P 121.9(3) . . ?
N3P C4P H4P 119.2 . . ?
C5P C4P H4P 118.8 . . ?
C4P C5P C6P 117.2(3) . . ?
C4P C5P H5P 121.5 . . ?
C6P C5P H5P 121.2 . . ?
N1P C6P C5P 121.5(3) . . ?
N1P C6P H6P 119.2 . . ?
C5P C6P H6P 119.2 . . ?
Zn O1W H11W 133(2) . . ?
Zn O1W H12W 109(2) . . ?
H11W O1W H12W 105(3) . . ?
H21W O2W H22W 106(3) . . ?
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
Zn N1B 1.984(2) . ?
Zn N2A 2.006(2) . ?
Zn N1P 2.076(2) . ?
Zn O1W 2.107(2) . ?
Zn N3P 2.297(2) 2_666 ?
N1A N2A 1.326(3) . ?
N1A C7AA 1.348(3) . ?
N2A N3A 1.359(3) . ?
N3A C3AA 1.324(3) . ?
C3AA C7AA 1.376(3) . ?
C3AA N4A 1.383(3) . ?
N4A C5A 1.360(3) . ?
N4A C4A 1.464(3) . ?
C4A H41A 0.9600 . ?
C4A H42A 0.9600 . ?
C4A H43A 0.9600 . ?
C5A O5A 1.230(3) . ?
C5A N6A 1.394(3) . ?
N6A C7A 1.405(3) . ?
N6A C6A 1.468(3) . ?
C6A H61A 0.9600 . ?
C6A H62A 0.9600 . ?
C6A H63A 0.9600 . ?
C7A O7A 1.216(3) . ?
C7A C7AA 1.438(3) . ?
N1B N2B 1.342(3) . ?
N1B C7AB 1.360(3) . ?
N2B N3B 1.347(3) . ?
N3B C3AB 1.341(3) . ?
C3AB C7AB 1.357(3) . ?
C3AB N4B 1.381(3) . ?
N4B C5B 1.366(4) . ?
N4B C4B 1.459(3) . ?
C4B H41B 0.9601 . ?
C4B H42B 0.9601 . ?
C4B H43B 0.9601 . ?
C5B O5B 1.215(3) . ?
C5B N6B 1.396(3) . ?
N6B C7B 1.412(3) . ?
N6B C6B 1.468(4) . ?
C6B H61B 0.9601 . ?
C6B H62B 0.9601 . ?
C6B H63B 0.9601 . ?
C7B O7B 1.217(3) . ?
C7B C7AB 1.430(4) . ?
N1P C2P 1.332(3) . ?
N1P C6P 1.337(3) . ?
C2P N3P 1.328(3) . ?
C2P C2P 1.483(5) 2_666 ?
N3P C4P 1.332(3) . ?
N3P Zn 2.297(2) 2_666 ?
C4P C5P 1.374(4) . ?
C4P H4P 0.9300 . ?
C5P C6P 1.375(4) . ?
C5P H5P 0.9300 . ?
C6P H6P 0.9300 . ?
O1W H11W 0.832(10) . ?
O1W H12W 0.829(10) . ?
O2W H21W 0.832(10) . ?
O2W H22W 0.837(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
_geom_hbond_site_symmetry_A
O1W H11W O2W 0.832(10) 1.913(13) 2.724(3) 165(3) 2_665
O1W H12W O5A 0.829(10) 1.959(11) 2.785(3) 174(3) 2
O2W H22W N1A 0.837(10) 2.100(11) 2.934(3) 175(3) .
O2W H21W O7A 0.832(10) 2.234(17) 3.015(3) 156(3) 2_565
