(Dimethyl sulfoxide-κ<i>O</i>)bis(thiosemicarbazide-κ^2^<i>N</i>^1^,<i>S</i>)zinc dipicrate dimethyl sulfoxide solvate monohydrate
Shanthakumari, R.; Hema, Ramu; Ramamurthy, K.; Sridar, Balasubramnian; Stoeckli-Evans, Helen; Acta Crystallographica Section E 67 (2011) m133–m134; doi:10.1107/S160053681005378X

data_2229076
_publ_section_title
;
 (Dimethyl
 sulfoxide-\k<i>O</i>)bis(thiosemicarbazide-\k^2^<i>N</i>^1^,<i>S</i>)zinc
 dipicrate dimethyl sulfoxide solvate monohydrate
;
_journal_coeditor_code           HG2775
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m133
_journal_page_last               m134
_journal_paper_doi               10.1107/S160053681005378X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Zn (C H5 N3 S)2 (C2 H6 O S)] (C6 H2 N3 O7)2, C2 H6 O S, H2 O'
_chemical_formula_moiety
'C4 H16 N6 O S3 Zn 2+, 2(C6 H2 N3 O7 -), C2 H6 O S, H2 O'
_chemical_formula_sum            'C18 H28 N12 O17 S4 Zn'
_chemical_formula_weight         878.13
_chemical_melting_point          469
_chemical_name_systematic
;
(Dimethyl
sulfoxide-\k<i>O</i>)bis(thiosemicarbazide-\k^2^<i>N</i>^1^,<i>S</i>)zinc
dipicrate dimethyl sulfoxide solvate monohydrate
;
_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           SHELXL-97
_cell_angle_alpha                81.124(2)
_cell_angle_beta                 77.063(2)
_cell_angle_gamma                81.168(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8762(11)
_cell_length_b                   11.2559(12)
_cell_length_c                   14.4859(15)
_cell_measurement_reflns_used    5926
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.9
_cell_volume                     1694.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18781
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         7719
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0338
_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/[\s^2^(Fo^2^)+(0.0559P)^2^+0.4578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                6573
_reflns_number_total             7719
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2775.cif
_cod_data_source_block           I
_cod_database_code               2229076
_cod_database_fobs_code          2229076