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
Bond, Andrew D.; Benevelli, Francesca; Jones, William; Journal of Materials Chemistry 12 (2002) 324–332; doi:10.1039/b106734f

data_7204224
_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 \w and \f 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/[\s^2^(Fo^2^)+0.4630P] where P=(Fo^2^+2Fc^2^)/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