Metal-Induced Cyclization of Thiosemicarbazones Derived from β-Keto Amides and β-Keto Esters: Open-Chain and Cyclized Ligands in Zinc(II) Complexes
José S. Casas; María V. Castaño; Eduardo E. Castellano; Javier Ellena; María S. García-Tasende; Ángeles Gato; Agustín Sánchez; Luisa M. Sanjuán; José Sordo; Inorganic Chemistry 41 (2002) 1550–1557; doi:10.1021/ic0111942

data_4317745
_publ_section_title
;
 Metal-Induced Cyclization of Thiosemicarbazones Derived from \b-Keto
 Amides and \b-Keto Esters: Open-Chain and Cyclized Ligands in Zinc(II)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1550
_journal_page_last               1557
_journal_paper_doi               10.1021/ic0111942
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C26 H36 N8 O5 S3 Zn'
_chemical_formula_weight         702.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.00(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.781(3)
_cell_length_b                   12.311(3)
_cell_length_c                   21.147(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      17
_cell_volume                     3325.4(12)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.471
_diffrn_measured_fraction_theta_max 0.471
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3079
_diffrn_reflns_theta_full        66.91
_diffrn_reflns_theta_max         66.91
_diffrn_reflns_theta_min         4.18
_diffrn_standards_decay_%        13
_diffrn_standards_interval_count 42
_diffrn_standards_interval_time  30
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    3.183
_exptl_absorpt_correction_T_max  0.6670
_exptl_absorpt_correction_T_min  0.3675
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+2.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                2436
_reflns_number_total             2936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0111942_1.cif
_cod_data_source_block           '[Zn(TSC3)2].DMSO'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+2.4300P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+2.4300P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C26 H36 N8 O5 S3 Zn1'
_cod_database_code               4317745