#------------------------------------------------------------------------------
#$Date: 2025-08-19 22:21:09 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301810 $
#$URL: file:///home/coder/svn-repositories/cod/cif/3/00/00/3000006.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_3000006
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quiros'
'Juan M. Salas'
_publ_section_title
;
 H-bond superstructures built by aquacomplexes and an azapurine
 derivative: A case of molecular recognition
;
_journal_name_full               'Dalton Transactions'
_journal_page_first              10390
_journal_page_last               10395
_journal_paper_doi               10.1039/c2dt30992k
_journal_year                    2012
_chemical_formula_moiety         'C10 H8 N2, H12 O6 Zn 2+, 2(C6 H6 N5 O2 1-)'
_chemical_formula_sum            'C22 H32 N12 O10 Zn'
_chemical_formula_weight         689.97
_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                109.345(1)
_cell_angle_beta                 107.577(1)
_cell_angle_gamma                101.978(1)
_cell_formula_units_Z            1
_cell_length_a                   8.4575(7)
_cell_length_b                   8.9798(11)
_cell_length_c                   10.8612(8)
_cell_measurement_reflns_used    3253
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.2
_cell_volume                     697.24(12)
_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 0.980
_diffrn_measured_fraction_theta_max 0.862
_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  0.0107
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4421
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0.2
_diffrn_standards_number         218
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2992
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0303
_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)+(0.0500P)²+0.4000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                2921
_reflns_number_total             2992
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            znax44.cif
_cod_data_source_block           znax44
_cod_depositor_comments
;Extending hold period by 9 months (from 2011-12-03 to 2012-09-03)
 Also
 changing journal name to Dalton Transactions

 Releasing structure 3000006 into public domain as published material.
;
_cod_database_code               3000006
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
Zn Zn 0.5000 0.5000 0.5000 0.01169(9) Uani 1 2 d S
O1W O 0.38378(15) 0.24507(15) 0.35005(12) 0.0153(2) Uani 1 1 d D
H11W H 0.314(2) 0.229(3) 0.2703(14) 0.021(5) Uiso 1 1 d D
H12W H 0.457(3) 0.203(3) 0.330(3) 0.036(7) Uiso 1 1 d D
O2W O 0.57401(16) 0.42449(16) 0.66574(13) 0.0174(2) Uani 1 1 d D
H21W H 0.521(3) 0.410(3) 0.717(2) 0.036(7) Uiso 1 1 d D
H22W H 0.673(2) 0.416(4) 0.701(3) 0.055(9) Uiso 1 1 d D
O3W O 0.26128(15) 0.48944(16) 0.51272(13) 0.0170(2) Uani 1 1 d D
H31W H 0.182(2) 0.511(3) 0.460(2) 0.034(7) Uiso 1 1 d D
H32W H 0.229(3) 0.474(3) 0.5746(19) 0.031(6) Uiso 1 1 d D
N1 N 0.13862(18) 0.43603(18) 0.70940(14) 0.0152(3) Uani 1 1 d .
N2 N -0.02244(18) 0.44126(18) 0.68012(15) 0.0162(3) Uani 1 1 d .
N3 N -0.10230(18) 0.37891(18) 0.75335(15) 0.0153(3) Uani 1 1 d .
C3A C 0.0181(2) 0.33386(19) 0.83121(16) 0.0126(3) Uani 1 1 d .
N4 N 0.00421(17) 0.26603(17) 0.92563(14) 0.0132(3) Uani 1 1 d .
C4 C -0.1568(2) 0.2311(2) 0.95194(18) 0.0176(3) Uani 1 1 d .
H41 H -0.2191 0.1095 0.9074 0.021 Uiso 1 1 d R
H42 H -0.2332 0.2858 0.9110 0.021 Uiso 1 1 d R
H43 H -0.1257 0.2746 1.0548 0.021 Uiso 1 1 d R
C5 C 0.1458(2) 0.23333(19) 0.99956(16) 0.0127(3) Uani 1 1 d .
O5 O 0.14213(15) 0.18016(15) 1.08861(12) 0.0158(2) Uani 1 1 d .
N6 N 0.29492(17) 0.26211(17) 0.96685(14) 0.0127(3) Uani 1 1 d .
C6 C 0.4406(2) 0.2172(2) 1.04165(18) 0.0172(3) Uani 1 1 d .
H61 H 0.5146 0.1997 0.9878 0.021 Uiso 1 1 d R
H62 H 0.3924 0.1137 1.0501 0.021 Uiso 1 1 d R
H63 H 0.5118 0.3082 1.1369 0.021 Uiso 1 1 d R
C7 C 0.3196(2) 0.33226(19) 0.87352(16) 0.0125(3) Uani 1 1 d .
O7 O 0.45875(15) 0.35604(15) 0.85680(12) 0.0156(2) Uani 1 1 d .
C7A C 0.1682(2) 0.36781(19) 0.80540(16) 0.0129(3) Uani 1 1 d .
N1P N 0.6307(2) 0.08720(18) 0.31354(16) 0.0200(3) Uani 1 1 d .
C2P C 0.6178(2) -0.0054(2) 0.38704(19) 0.0199(3) Uani 1 1 d .
H2P H 0.5059 -0.0483 0.3881 0.024 Uiso 1 1 d R
C3P C 0.7577(2) -0.0416(2) 0.46210(18) 0.0183(3) Uani 1 1 d .
H3P H 0.7412 -0.1059 0.5141 0.022 Uiso 1 1 d R
C4P C 0.9228(2) 0.01736(19) 0.45994(17) 0.0148(3) Uani 1 1 d .
C5P C 0.9356(2) 0.1088(2) 0.37961(19) 0.0187(3) Uani 1 1 d .
H5P H 1.0441 0.1483 0.3721 0.022 Uiso 1 1 d R
C6P C 0.7891(2) 0.1416(2) 0.31066(19) 0.0205(4) Uani 1 1 d .
H6P H 0.8016 0.2067 0.2585 0.025 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
O3W Zn O3W 180.0 . 2_666
O3W Zn O2W 90.85(5) . .
O3W Zn O2W 89.15(5) 2_666 .
O3W Zn O2W 89.15(5) . 2_666
O3W Zn O2W 90.85(5) 2_666 2_666
O2W Zn O2W 180.0 . 2_666
O3W Zn O1W 88.69(5) . .
O3W Zn O1W 91.31(5) 2_666 .
O2W Zn O1W 89.92(5) . .
O2W Zn O1W 90.08(5) 2_666 .
O3W Zn O1W 91.31(5) . 2_666
O3W Zn O1W 88.69(5) 2_666 2_666
O2W Zn O1W 90.08(5) . 2_666
O2W Zn O1W 89.92(5) 2_666 2_666
O1W Zn O1W 180.0 . 2_666
Zn O1W H11W 114.4(15) . .
Zn O1W H12W 113.4(18) . .
H11W O1W H12W 102(2) . .
Zn O2W H21W 128.8(18) . .
Zn O2W H22W 125(2) . .
H21W O2W H22W 106(3) . .
Zn O3W H31W 124.5(17) . .
Zn O3W H32W 127.6(16) . .
H31W O3W H32W 108(2) . .
N2 N1 C7A 106.34(13) . .
N1 N2 N3 112.23(13) . .
C3A N3 N2 104.70(13) . .
N3 C3A C7A 109.46(14) . .
N3 C3A N4 128.03(14) . .
C7A C3A N4 122.51(14) . .
C5 N4 C3A 119.30(13) . .
C5 N4 C4 118.98(13) . .
C3A N4 C4 121.71(13) . .
N4 C4 H41 109.5 . .
N4 C4 H42 109.3 . .
H41 C4 H42 109.5 . .
N4 C4 H43 109.6 . .
H41 C4 H43 109.5 . .
H42 C4 H43 109.5 . .
O5 C5 N4 121.55(14) . .
O5 C5 N6 121.32(14) . .
N4 C5 N6 117.13(13) . .
C7 N6 C5 126.74(13) . .
C7 N6 C6 117.26(13) . .
C5 N6 C6 115.98(13) . .
N6 C6 H61 109.5 . .
N6 C6 H62 109.5 . .
H61 C6 H62 109.5 . .
N6 C6 H63 109.5 . .
H61 C6 H63 109.5 . .
H62 C6 H63 109.5 . .
O7 C7 N6 120.78(14) . .
O7 C7 C7A 127.12(14) . .
N6 C7 C7A 112.10(13) . .
N1 C7A C3A 107.28(14) . .
N1 C7A C7 130.65(14) . .
C3A C7A C7 122.07(14) . .
C2P N1P C6P 116.35(15) . .
N1P C2P C3P 124.07(16) . .
N1P C2P H2P 117.9 . .
C3P C2P H2P 118.1 . .
C2P C3P C4P 119.18(16) . .
C2P C3P H3P 120.3 . .
C4P C3P H3P 120.5 . .
C5P C4P C3P 117.04(15) . .
C5P C4P C4P 121.96(19) . 2_756
C3P C4P C4P 121.00(18) . 2_756
C6P C5P C4P 119.53(16) . .
C6P C5P H5P 120.2 . .
C4P C5P H5P 120.2 . .
N1P C6P C5P 123.78(16) . .
N1P C6P H6P 118.1 . .
C5P C6P H6P 118.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn O3W 2.0499(11) .
Zn O3W 2.0499(11) 2_666
Zn O2W 2.0967(11) .
Zn O2W 2.0968(11) 2_666
Zn O1W 2.1186(12) .
Zn O1W 2.1186(12) 2_666
O1W H11W 0.831(10) .
O1W H12W 0.832(10) .
O2W H21W 0.838(10) .
O2W H22W 0.843(10) .
O3W H31W 0.840(10) .
O3W H32W 0.839(10) .
N1 N2 1.3167(19) .
N1 C7A 1.362(2) .
N2 N3 1.3656(18) .
N3 C3A 1.339(2) .
C3A C7A 1.376(2) .
C3A N4 1.376(2) .
N4 C5 1.374(2) .
N4 C4 1.467(2) .
C4 H41 0.9800 .
C4 H42 0.9800 .
C4 H43 0.9800 .
C5 O5 1.2176(19) .
C5 N6 1.407(2) .
N6 C7 1.401(2) .
N6 C6 1.4693(19) .
C6 H61 0.9800 .
C6 H62 0.9800 .
C6 H63 0.9800 .
C7 O7 1.230(2) .
C7 C7A 1.429(2) .
N1P C2P 1.340(2) .
N1P C6P 1.341(2) .
C2P C3P 1.387(2) .
C2P H2P 0.9500 .
C3P C4P 1.397(2) .
C3P H3P 0.9500 .
C4P C5P 1.394(2) .
C4P C4P 1.491(3) 2_756
C5P C6P 1.386(2) .
C5P H5P 0.9500 .
C6P H6P 0.9500 .
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 H12W N1P 0.832(10) 1.988(11) 2.8080(19) 169(2) .
O1W H11W O5 0.831(10) 1.906(10) 2.7357(16) 175(2) 1_554
O2W H21W O7 0.838(10) 1.919(12) 2.7299(16) 162(3) .
O2W H22W N3 0.843(10) 1.942(11) 2.7780(18) 171(3) 1_655
O3W H32W N1 0.839(10) 1.933(10) 2.7713(18) 176(2) .
O3W H31W N2 0.840(10) 1.940(11) 2.7721(18) 171(2) 2_566
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168327377
