#------------------------------------------------------------------------------
#$Date: 2025-01-08 17:11:48 +0200 (Wed, 08 Jan 2025) $
#$Revision: 297228 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/42/7204224.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_7204224
loop_
_publ_author_name
'Bond, Andrew D.'
'Benevelli, Francesca'
'Jones, William'
_publ_section_title
;
 Modification of the solid-state structure of
 bis(1-hydroxy-2(1H)-pyridinethiolato-S2,O)zinc(II): synthesis and
 characterisation of a molecular solid solution incorporating
 3-hydroxy-4-methyl-2(3H)-thiazolethione
;
_journal_coden_ASTM              JMACEP
_journal_issue                   2
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              324
_journal_page_last               332
_journal_paper_doi               10.1039/b106734f
_journal_volume                  12
_journal_year                    2002
_chemical_formula_moiety
;
(C5 H4 N O S 1-)1.2, (C4 H4 N O S2 1-)0.8, (Zn 2+), (H2 O)
;
_chemical_formula_sum            'C9.2 H10 N2 O3 S2.8 Zn'
_chemical_formula_weight         351.73
_chemical_melting_point          484.5(5)
_chemical_name_common            Zn(PT)1.2(MTT)0.8(H2O)
_chemical_name_systematic
; 
(1-hydroxy-2(1H)-pyridinethiolato-S2,O)
(3-hydroxy-4-methyl-2(3H)-thiazolethiolate-S2,O)zinc(II) hydrate 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1353(5)
_cell_length_b                   11.6238(5)
_cell_length_c                   15.9011(12)
_cell_measurement_reflns_used    5887
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.91
_cell_volume                     1318.83(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'thin-slice ω and φ 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5887
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         3.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.305
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2313
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+0.4630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                2176
_reflns_number_total             2313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106734f.txt
_cod_data_source_block           wj9916
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '484-485' was changed to '484.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        'C9.20 H10 N2 O3 S2.80 Zn'
_cod_database_code               7204224
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
Zn1 Zn 0.14318(5) 0.14711(3) 0.91155(2) 0.03164(11) Uani 1 1 d . A .
O1 O 0.3934(3) 0.2219(2) 0.86668(15) 0.0425(6) Uani 1 1 d . . .
O2 O -0.1049(3) 0.0755(2) 0.96083(16) 0.0463(6) Uani 1 1 d . . .
O3 O 0.1409(4) 0.2616(2) 1.00651(18) 0.0493(6) Uani 1 1 d D . .
H100 H 0.218(4) 0.313(2) 1.007(2) 0.051(13) Uiso 1 1 d D . .
H101 H 0.058(4) 0.260(3) 1.0411(19) 0.054(13) Uiso 1 1 d D . .
S1 S 0.02150(18) 0.21636(10) 0.78661(7) 0.0629(3) Uani 1 1 d . . .
S2 S 0.27069(19) -0.02988(10) 0.94463(9) 0.0762(4) Uani 1 1 d . . .
N1 N 0.3656(5) 0.3044(2) 0.8105(2) 0.0494(8) Uani 0.60 1 d PD A 1
C1 C 0.2014(7) 0.3118(3) 0.7692(2) 0.0548(12) Uani 0.60 1 d PD A 1
C2 C 0.2221(11) 0.4086(7) 0.7169(5) 0.047(2) Uani 0.60 1 d PD A 1
H2 H 0.1149 0.4282 0.6845 0.056 Uiso 0.60 1 calc PR A 1
C3 C 0.3638(6) 0.4737(3) 0.7067(2) 0.0485(9) Uani 0.60 1 d PD A 1
H3 H 0.3564 0.5330 0.6657 0.058 Uiso 0.60 1 calc PR A 1
C4 C 0.5252(10) 0.4625(6) 0.7515(4) 0.0411(17) Uani 0.60 1 d PD A 1
H4 H 0.6279 0.5138 0.7448 0.049 Uiso 0.60 1 calc PR A 1
C5 C 0.5292(11) 0.3724(5) 0.8067(4) 0.0336(14) Uani 0.60 1 d PD A 1
H5 H 0.6358 0.3565 0.8406 0.040 Uiso 0.60 1 calc PR A 1
N2 N -0.0766(5) -0.0182(3) 1.00856(18) 0.0497(9) Uani 0.60 1 d PD A 2
C6 C 0.0897(6) -0.0738(3) 1.0067(2) 0.0540(11) Uani 0.60 1 d PD A 2
C7 C 0.0738(17) -0.1669(9) 1.0635(8) 0.058(3) Uani 0.60 1 d PD A 2
H7 H 0.1783 -0.2164 1.0713 0.070 Uiso 0.60 1 calc PR A 2
C8 C -0.0841(9) -0.1874(4) 1.1065(3) 0.0669(15) Uani 0.60 1 d PD A 2
H8 H -0.0824 -0.2509 1.1441 0.080 Uiso 0.60 1 calc PR A 2
C9 C -0.2342(14) -0.1311(8) 1.1022(5) 0.068(3) Uani 0.60 1 d PD A 2
H9 H -0.3406 -0.1526 1.1346 0.081 Uiso 0.60 1 calc PR A 2
C10 C -0.2401(14) -0.0393(8) 1.0505(5) 0.050(2) Uani 0.60 1 d PD A 2
H10 H -0.3490 0.0069 1.0438 0.060 Uiso 0.60 1 calc PR A 2
S3 S 0.1384(5) 0.4106(2) 0.6896(2) 0.0496(7) Uani 0.40 1 d PD A 3
N1A N 0.3656(5) 0.3044(2) 0.8105(2) 0.0494(8) Uani 0.40 1 d PD A 3
C1A C 0.2014(7) 0.3118(3) 0.7692(2) 0.0548(12) Uani 0.40 1 d PD A 3
C3A C 0.3638(6) 0.4737(3) 0.7067(2) 0.0485(9) Uani 0.40 1 d PD A 3
H3A H 0.4146 0.5397 0.6798 0.058 Uiso 0.40 1 calc PR A 3
C11 C 0.4521(16) 0.4031(10) 0.7700(7) 0.042(3) Uani 0.40 1 d PD A 3
C12 C 0.6390(15) 0.4154(10) 0.8029(7) 0.053(3) Uani 0.40 1 d PD A 3
H12A H 0.6330 0.4281 0.8637 0.064 Uiso 0.40 1 calc PR A 3
H12B H 0.7004 0.4812 0.7759 0.064 Uiso 0.40 1 calc PR A 3
H12C H 0.7108 0.3453 0.7913 0.064 Uiso 0.40 1 calc PR A 3
S4 S 0.1281(8) -0.1996(4) 1.0691(3) 0.0577(11) Uani 0.40 1 d PD A 4
N2A N -0.0766(5) -0.0182(3) 1.00856(18) 0.0497(9) Uani 0.40 1 d PD A 4
C6A C 0.0897(6) -0.0738(3) 1.0067(2) 0.0540(11) Uani 0.40 1 d PD A 4
C8A C -0.0841(9) -0.1874(4) 1.1065(3) 0.0669(15) Uani 0.40 1 d PD A 4
H8A H -0.1386 -0.2387 1.1461 0.080 Uiso 0.40 1 calc PR A 4
C13 C -0.1798(18) -0.0864(11) 1.0709(8) 0.041(3) Uani 0.40 1 d PD A 4
C14 C -0.3698(15) -0.0394(8) 1.0837(7) 0.052(2) Uani 0.40 1 d PD A 4
H14A H -0.3616 0.0434 1.0945 0.062 Uiso 0.40 1 calc PR A 4
H14B H -0.4285 -0.0776 1.1319 0.062 Uiso 0.40 1 calc PR A 4
H14C H -0.4454 -0.0530 1.0332 0.062 Uiso 0.40 1 calc PR A 4
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 O2 88.60(11) . . ?
O3 Zn1 O1 89.32(10) . . ?
O2 Zn1 O1 177.82(10) . . ?
O3 Zn1 S2 114.92(10) . . ?
O2 Zn1 S2 83.92(7) . . ?
O1 Zn1 S2 96.35(7) . . ?
O3 Zn1 S1 114.27(9) . . ?
O2 Zn1 S1 98.15(8) . . ?
O1 Zn1 S1 83.32(7) . . ?
S2 Zn1 S1 130.80(5) . . ?
N1 O1 Zn1 113.6(2) . . ?
N2 O2 Zn1 113.9(2) . . ?
C1 S1 Zn1 94.75(14) . . ?
C6 S2 Zn1 95.73(14) . . ?
O1 N1 C1 120.3(3) . . ?
O1 N1 C5 108.1(4) . . ?
C1 N1 C5 131.6(4) . . ?
N1 C1 C2 104.4(5) . . ?
N1 C1 S1 122.0(3) . . ?
C2 C1 S1 133.6(5) . . ?
C3 C2 C1 129.3(6) . . ?
C2 C3 C4 123.3(5) . . ?
C3 C4 C5 115.3(7) . . ?
C4 C5 N1 116.0(8) . . ?
O2 N2 C6 120.5(3) . . ?
O2 N2 C10 107.0(5) . . ?
C6 N2 C10 132.4(5) . . ?
N2 C6 C7 106.3(5) . . ?
N2 C6 S2 122.4(3) . . ?
C7 C6 S2 131.3(5) . . ?
C8 C7 C6 122.0(7) . . ?
C9 C8 C7 126.6(6) . . ?
C8 C9 C10 118.2(9) . . ?
C9 C10 N2 114.4(9) . . ?
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
Zn1 O3 2.013(3) . ?
Zn1 O2 2.107(2) . ?
Zn1 O1 2.110(2) . ?
Zn1 S2 2.3101(10) . ?
Zn1 S1 2.3128(11) . ?
O1 N1 1.326(4) . ?
O2 N2 1.342(4) . ?
S1 C1 1.719(4) . ?
S2 C6 1.703(4) . ?
N1 C1 1.346(5) . ?
N1 C5 1.411(8) . ?
C1 C2 1.407(8) . ?
C2 C3 1.273(9) . ?
C3 C4 1.360(8) . ?
C4 C5 1.368(9) . ?
N2 C6 1.351(5) . ?
N2 C10 1.366(9) . ?
C6 C7 1.414(11) . ?
C7 C8 1.340(12) . ?
C8 C9 1.257(10) . ?
C9 C10 1.348(11) . ?
C11 C12 1.440(15) . ?
C13 C14 1.475(15) . ?
