Supplementary Material (ESI) for Journal of Materials Chemistry
This journal is © The Royal Society of Chemistry 2002

data_global 

_audit_creation_method            'SHELXL-97 plus manual editing' 

_journal_coden_Cambridge      1145

_publ_requested_journal       'Journal of Materials Chemistry'


loop_
_publ_author_name
'Benevelli, Francesca'
'Bond, Andrew'
'Jones, W.'

_publ_contact_author_name         'Andrew Bond'
_publ_contact_author_address
;
Department of Chemistry
University of Cambridge
Lensfield Road
Cambridge
CB2 1EW
UK
;
_publ_contact_author_email       'adb29@cam.ac.uk'
_publ_contact_author_fax          '(01223) 336362'
_publ_contact_author_phone        '(01223) 336352'

_publ_section_title		
;
Modification of the Solid-State Structure of
Bis(1-Hydroxy-2(1H)-Pyridinethiolato-S2,O)Zinc(II):  Synthesis and
Characterization of a Molecular Solid Solution Incorporating
3-Hydroxy-4-Methyl-2(3H)-Thiazolethione
;

data_wj9916 

_database_code_CSD	168321


_chemical_name_systematic 
; 
(1-hydroxy-2(1H)-pyridinethiolato-S2,O)
(3-hydroxy-4-methyl-2(3H)-thiazolethiolate-S2,O)zinc(II) hydrate 
; 
_chemical_name_common             'Zn(PT)1.2(MTT)0.8(H2O)' 
_chemical_melting_point           484-485
_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             'C9.20 H10 N2 O3 S2.80 Zn' 
_chemical_formula_weight          351.73 

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' 

_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    P2(1)2(1)2(1)

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' 

_cell_length_a                    7.1353(5) 
_cell_length_b                    11.6238(5) 
_cell_length_c                    15.9011(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1318.83(15) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     5887 
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       25.03

_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.771 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              712 
_exptl_absorpt_coefficient_mu     2.305 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.700
_exptl_absorpt_correction_T_max   0.758 
_exptl_absorpt_process_details    'Sortav Blessing (1995)'

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius Kappa CCD' 
_diffrn_measurement_method        'thin-slice \w and \f scans'
_diffrn_standards_number          0
_diffrn_reflns_number             5887 
_diffrn_reflns_av_R_equivalents   0.0374 
_diffrn_reflns_av_sigmaI/netI     0.0441 
_diffrn_reflns_limit_h_min        -6 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          3.10 
_diffrn_reflns_theta_max          24.95 
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              24.95 
_diffrn_measured_fraction_theta_full   0.998 
_reflns_number_total              2313 
_reflns_number_gt                 2176 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Collect (Nonius B.V. 1998)'
_computing_cell_refinement        'HKL Scalepack (Otwinowski & Minor 1997)' 
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution     'SHELXS-97 (Sheldrick 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick 1997)' 
_computing_publication_material   'SHELXL-97 (Sheldrick 1997)' 

_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
'calc w=1/[\s^2^(Fo^2^)+0.4630P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.001(14) 
_refine_ls_number_reflns          2313 
_refine_ls_number_parameters      227 
_refine_ls_number_restraints      27 
_refine_ls_R_factor_all           0.0305 
_refine_ls_R_factor_gt            0.0273 
_refine_ls_wR_factor_ref          0.0566 
_refine_ls_wR_factor_gt           0.0553 
_refine_ls_goodness_of_fit_ref    1.088 
_refine_ls_restrained_S_all       1.114 
_refine_ls_shift/su_max           0.018 
_refine_ls_shift/su_mean          0.002 
_refine_diff_density_max          0.331 
_refine_diff_density_min          -0.359 
_refine_diff_density_rms          0.055 
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_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Zn1 0.0325(2) 0.02905(18) 0.03341(18) 0.00001(17) -0.00123(19) 0.00372(17) 
O1 0.0378(16) 0.0534(14) 0.0365(12) -0.0029(12) 0.0001(12) -0.0055(11) 
O2 0.0365(16) 0.0413(13) 0.0611(17) -0.0132(13) 0.0079(13) -0.0045(11) 
O3 0.0333(15) 0.0596(17) 0.0549(16) -0.0229(13) 0.0120(16) -0.0140(15) 
S1 0.0699(8) 0.0674(7) 0.0515(6) 0.0113(5) -0.0291(6) 0.0008(6) 
S2 0.0796(9) 0.0500(6) 0.0990(10) 0.0359(6) 0.0422(8) 0.0326(6) 
N1 0.065(2) 0.0342(15) 0.0489(19) -0.0094(15) 0.028(2) -0.0055(17) 
C1 0.093(4) 0.036(2) 0.036(2) 0.0073(16) 0.012(2) 0.014(2) 
C2 0.045(5) 0.061(5) 0.035(4) 0.001(4) -0.019(3) 0.019(4) 
C3 0.054(3) 0.050(2) 0.041(2) 0.0060(18) 0.009(2) 0.010(2) 
C4 0.047(4) 0.040(4) 0.036(4) 0.007(3) 0.023(4) -0.005(3) 
C5 0.040(5) 0.033(4) 0.028(3) -0.005(3) 0.005(3) 0.001(3) 
N2 0.063(2) 0.0483(19) 0.0377(17) -0.0149(16) 0.0130(17) -0.0263(17) 
C6 0.083(4) 0.0333(19) 0.046(2) 0.0077(18) 0.016(2) -0.001(2) 
C7 0.062(7) 0.043(7) 0.071(7) -0.013(6) 0.002(5) 0.017(5) 
C8 0.110(5) 0.050(3) 0.040(3) 0.007(2) -0.003(3) -0.031(3) 
C9 0.080(7) 0.078(7) 0.044(5) 0.012(5) -0.001(5) -0.038(6) 
C10 0.055(7) 0.060(6) 0.035(5) 0.002(4) 0.005(5) -0.024(5) 
S3 0.062(2) 0.0425(13) 0.0447(18) 0.0159(13) 0.0008(16) 0.0108(16) 
N1A 0.065(2) 0.0342(15) 0.0489(19) -0.0094(15) 0.028(2) -0.0055(17) 
C1A 0.093(4) 0.036(2) 0.036(2) 0.0073(16) 0.012(2) 0.014(2) 
C3A 0.054(3) 0.050(2) 0.041(2) 0.0060(18) 0.009(2) 0.010(2) 
C11 0.053(8) 0.047(7) 0.026(6) 0.007(5) 0.023(6) 0.009(6) 
C12 0.050(7) 0.054(6) 0.056(7) 0.000(5) 0.021(7) 0.000(6) 
S4 0.089(3) 0.0343(19) 0.0497(18) 0.0140(15) 0.009(2) 0.0173(18) 
N2A 0.063(2) 0.0483(19) 0.0377(17) -0.0149(16) 0.0130(17) -0.0263(17) 
C6A 0.083(4) 0.0333(19) 0.046(2) 0.0077(18) 0.016(2) -0.001(2) 
C8A 0.110(5) 0.050(3) 0.040(3) 0.007(2) -0.003(3) -0.031(3) 
C13 0.058(10) 0.036(7) 0.028(7) -0.002(5) -0.002(6) -0.018(6) 
C14 0.058(7) 0.054(6) 0.042(5) 0.010(5) -0.001(7) -0.031(6) 

_geom_special_details 
; 
All esds (except the esd in the dihedral angle between two l.s. planes) 
are estimated using the full covariance matrix.  The cell esds are taken 
into account individually in the estimation of esds in distances, angles 
and torsion angles; correlations between esds in cell parameters are only 
used when they are defined by crystal symmetry.  An approximate (isotropic) 
treatment of cell esds is used for estimating esds involving l.s. planes. 
; 

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) . ? 

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) . . ?