Rhenium(I)-Induced Cyclization of Thiosemicarbazones Derived from β-Keto Esters
Rosa Carballo; José S. Casas; Emilia García-Martínez; Gumersindo Pereiras-Gabián; Agustín Sánchez; José Sordo; Ezequiel M. Vázquez-López; Inorganic Chemistry 42 (2003) 6395–6403; doi:10.1021/ic030154q

data_4314314
_publ_section_title
;
 Rhenium(I)-Induced Cyclization of Thiosemicarbazones Derived from \b-Keto
 Esters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6395
_journal_page_last               6403
_journal_paper_doi               10.1021/ic030154q
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12.5 H16 Br N3 O5.5 Re S'
_chemical_formula_weight         594.45
_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                 105.4270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   14.3705(9)
_cell_length_b                   30.862(2)
_cell_length_c                   17.4628(11)
_cell_measurement_temperature    293(2)
_cell_volume                     7465.7(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.1180
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21637
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    8.792
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.782345
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .05
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8490
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                4546
_reflns_number_total             8490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030154q_1.cif
_cod_data_source_block           1c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C12.50 H16 Br N3 O5.50 Re S'
_cod_database_code               4314314