#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/75/2207536.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2207536
loop_
_publ_author_name
'Xu, Hong Xia'
'Ma, Jian Ping'
'Huang, Ru Qi'
'Dong, Yu Bin'
_publ_section_title
;Tetraaquabis[5-(4-pyridyl)-1,3,4-oxadiazole-2-thiolato-κN⁴]zinc(II)
 dihydrate
;
_journal_coeditor_code           FL6202
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2462
_journal_page_last               m2463
_journal_paper_doi               10.1107/S1600536805034987
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Zn (C7 H4 N3 O S)2 (H2 O)4] , 2H2 O'
_chemical_formula_moiety         'C14 H16 N6 O6 S2 Zn , 2H2 O1'
_chemical_formula_sum            'C14 H20 N6 O8 S2 Zn'
_chemical_formula_weight         529.85
_chemical_name_systematic
;
Tetraaquabis[5-(4-pyridyl)-1,3,4-oxadiazole-2-thiolato-\kN⁴]zinc(II)
dihydrate
;
_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           SHELXL97
_cell_angle_alpha                90.414(8)
_cell_angle_beta                 90.672(7)
_cell_angle_gamma                105.677(7)
_cell_formula_units_Z            1
_cell_length_a                   7.028(4)
_cell_length_b                   7.981(5)
_cell_length_c                   9.690(6)
_cell_measurement_reflns_used    2297
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.827
_cell_measurement_theta_min      2.651
_cell_volume                     523.2(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2684
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.7830
_exptl_absorpt_correction_T_min  0.5657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1823
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0261
_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)+(0.0342P)²+0.1713P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                1764
_reflns_number_total             1823
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fl6202.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P1 '
_cod_database_code               2207536
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
O4 0.9929(2) 0.42182(18) 0.23317(14) 0.0383(4) Uani d D 1 O
Zn1 0.5000 0.5000 0.5000 0.02811(12) Uani d S 1 Zn
N1 0.1523(3) -0.2494(2) 1.12497(17) 0.0326(4) Uani d . 1 N
N2 0.2026(3) -0.1919(2) 0.99133(17) 0.0331(4) Uani d . 1 N
N3 0.4279(2) 0.3291(2) 0.66924(16) 0.0275(4) Uani d . 1 N
C1 0.1679(3) -0.1120(2) 1.20341(19) 0.0268(4) Uani d . 1 C
C2 0.2477(3) -0.0245(3) 0.99679(19) 0.0275(4) Uani d . 1 C
C3 0.3118(3) 0.0985(3) 0.88519(19) 0.0261(4) Uani d . 1 C
C4 0.3472(3) 0.0396(3) 0.7559(2) 0.0295(4) Uani d . 1 C
H4 0.3331 -0.0781 0.7395 0.035 Uiso calc R 1 H
C5 0.4037(3) 0.1586(3) 0.65196(19) 0.0285(4) Uani d . 1 C
H5 0.4263 0.1181 0.5651 0.034 Uiso calc R 1 H
C6 0.3957(3) 0.3858(3) 0.7951(2) 0.0315(4) Uani d . 1 C
H6 0.4137 0.5045 0.8090 0.038 Uiso calc R 1 H
C7 0.3371(3) 0.2759(3) 0.9048(2) 0.0314(4) Uani d . 1 C
H7 0.3148 0.3197 0.9905 0.038 Uiso calc R 1 H
O1 0.2306(2) 0.03728(17) 1.12512(13) 0.0299(3) Uani d . 1 O
O2 0.3018(2) 0.32482(18) 0.36495(16) 0.0402(4) Uani d D 1 O
O3 0.7278(2) 0.3774(2) 0.44836(16) 0.0438(4) Uani d D 1 O
S1 0.12129(8) -0.09489(7) 1.37225(5) 0.03284(15) Uani d . 1 S
H1O2 0.2074 0.3618 0.3317 0.050 Uiso d RD 1 H
H2O2 0.2677 0.2165 0.3778 0.050 Uiso d RD 1 H
H1O3 0.7747 0.3180 0.5039 0.050 Uiso d RD 1 H
H2O3 0.8065 0.4192 0.3828 0.050 Uiso d RD 1 H
H1O4 0.9327 0.3518 0.1695 0.050 Uiso d RD 1 H
H2O4 1.0436 0.5224 0.1996 0.050 Uiso d RD 1 H
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'
S S 0.1246 0.1234 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
H1O4 O4 H2O4 . . 110.0 ?
N3 Zn1 N3 . 2_666 180 y
N3 Zn1 O2 . 2_666 87.25(7) y
N3 Zn1 O2 2_666 2_666 92.75(7) ?
N3 Zn1 O2 . . 92.75(7) y
N3 Zn1 O2 2_666 . 87.25(7) ?
O2 Zn1 O2 2_666 . 180 y
N3 Zn1 O3 . . 88.34(7) y
N3 Zn1 O3 2_666 . 91.66(7) y
O2 Zn1 O3 2_666 . 90.39(8) ?
O2 Zn1 O3 . . 89.61(8) y
N3 Zn1 O3 . 2_666 91.66(7) ?
N3 Zn1 O3 2_666 2_666 88.34(7) ?
O2 Zn1 O3 2_666 2_666 89.61(8) ?
O2 Zn1 O3 . 2_666 90.39(8) y
O3 Zn1 O3 . 2_666 180 y
C1 N1 N2 . . 107.65(17) ?
C2 N2 N1 . . 106.41(16) ?
C5 N3 C6 . . 117.63(17) ?
C5 N3 Zn1 . . 120.53(13) ?
C6 N3 Zn1 . . 121.76(14) ?
N1 C1 O1 . . 109.59(17) ?
N1 C1 S1 . . 130.68(15) ?
O1 C1 S1 . . 119.72(15) ?
N2 C2 O1 . . 112.64(16) ?
N2 C2 C3 . . 128.34(18) ?
O1 C2 C3 . . 119.02(17) ?
C4 C3 C7 . . 118.45(17) ?
C4 C3 C2 . . 120.12(18) ?
C7 C3 C2 . . 121.43(18) ?
C5 C4 C3 . . 118.70(19) ?
C5 C4 H4 . . 120.6 ?
C3 C4 H4 . . 120.6 ?
N3 C5 C4 . . 123.44(18) ?
N3 C5 H5 . . 118.3 ?
C4 C5 H5 . . 118.3 ?
N3 C6 C7 . . 122.89(19) ?
N3 C6 H6 . . 118.6 ?
C7 C6 H6 . . 118.6 ?
C6 C7 C3 . . 118.87(18) ?
C6 C7 H7 . . 120.6 ?
C3 C7 H7 . . 120.6 ?
C2 O1 C1 . . 103.70(15) ?
Zn1 O2 H1O2 . . 115.4 ?
Zn1 O2 H2O2 . . 122.3 ?
H1O2 O2 H2O2 . . 112.4 ?
Zn1 O3 H1O3 . . 123.9 ?
Zn1 O3 H2O3 . . 118.9 ?
H1O3 O3 H2O3 . . 113.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O4 H1O4 . 0.8564 ?
O4 H2O4 . 0.8541 ?
Zn1 N3 . 2.1179(18) y
Zn1 N3 2_666 2.1179(18) ?
Zn1 O2 2_666 2.1181(16) ?
Zn1 O2 . 2.1181(16) y
Zn1 O3 . 2.1515(18) y
Zn1 O3 2_666 2.1515(18) ?
N1 C1 . 1.309(3) ?
N1 N2 . 1.394(3) ?
N2 C2 . 1.287(3) ?
N3 C5 . 1.334(3) ?
N3 C6 . 1.341(3) ?
C1 O1 . 1.388(2) ?
C1 S1 . 1.684(2) ?
C2 O1 . 1.353(2) ?
C2 C3 . 1.457(3) ?
C3 C4 . 1.384(3) ?
C3 C7 . 1.390(3) ?
C4 C5 . 1.376(3) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C6 C7 . 1.377(3) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
O2 H1O2 . 0.8561 ?
O2 H2O2 . 0.8431 ?
O3 H1O3 . 0.8405 ?
O3 H2O3 . 0.8558 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H1O3 S1 2_657 0.84 2.42 3.246(2) 167
O2 H2O2 S1 1_554 0.84 2.42 3.247(2) 167
O2 H1O2 O4 1_455 0.86 1.94 2.793(2) 171
O4 H2O4 N1 1_664 0.85 1.92 2.778(3) 179
O4 H1O4 N2 2_656 0.86 2.06 2.915(2) 177
O3 H2O3 O4 . 0.86 1.96 2.773(2) 158
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
C1 N1 N2 C2 . 0.8(2)
O2 Zn1 N3 C5 2_666 -138.85(16)
O2 Zn1 N3 C5 . 41.15(16)
O3 Zn1 N3 C5 . -48.38(15)
O3 Zn1 N3 C5 2_666 131.62(15)
O2 Zn1 N3 C6 2_666 44.37(16)
O2 Zn1 N3 C6 . -135.63(16)
O3 Zn1 N3 C6 . 134.84(16)
O3 Zn1 N3 C6 2_666 -45.16(16)
N2 N1 C1 O1 . -0.8(2)
N2 N1 C1 S1 . 177.93(15)
N1 N2 C2 O1 . -0.4(2)
N1 N2 C2 C3 . 179.54(19)
N2 C2 C3 C4 . -5.6(3)
O1 C2 C3 C4 . 174.32(17)
N2 C2 C3 C7 . 173.7(2)
O1 C2 C3 C7 . -6.3(3)
C7 C3 C4 C5 . -0.7(3)
C2 C3 C4 C5 . 178.69(18)
C6 N3 C5 C4 . 0.3(3)
Zn1 N3 C5 C4 . -176.63(15)
C3 C4 C5 N3 . 0.5(3)
C5 N3 C6 C7 . -0.9(3)
Zn1 N3 C6 C7 . 175.99(16)
N3 C6 C7 C3 . 0.7(3)
C4 C3 C7 C6 . 0.1(3)
C2 C3 C7 C6 . -179.24(18)
N2 C2 O1 C1 . -0.1(2)
C3 C2 O1 C1 . 179.97(16)
N1 C1 O1 C2 . 0.6(2)
S1 C1 O1 C2 . -178.34(14)
