Diorganotin(IV) complexes of imidazole-2-carbaldehyde thiosemicarbazone (H2ImTSC). The crystal and molecular structures of the “free” ligand and of [SnMe2(ImTSC)]
Casas, José S.; Castiñeiras, Alfonso; Rodríguez-Argüelles, María C.; Sánchez, Agustín; Sordo, José; Vázquez-López, Antonia; Vázquez-López, Ezequiel M.; Journal of the Chemical Society, Dalton Transactions  (2000) 2267–; doi:10.1039/b002286l

data_7009604
_publ_section_title
;
 Diorganotin(IV) complexes of imidazole-2-carbaldehyde
 thiosemicarbazone (H2ImTSC). The crystal and molecular structures of
 the &#x201C;free&#x201D; ligand and of [SnMe2(ImTSC)]
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2267
_journal_paper_doi               10.1039/b002286l
_journal_year                    2000
_chemical_formula_sum            'C5 H8 N5 O0.5 S'
_chemical_formula_weight         178.22
_chemical_name_systematic
; 
 2-forylimidazole thiosemicarbazone 
;
_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   direct
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.828(9)
_cell_angle_beta                 89.140(10)
_cell_angle_gamma                61.146(9)
_cell_formula_units_Z            4
_cell_length_a                   7.7676(9)
_cell_length_b                   7.8401(9)
_cell_length_c                   15.873(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      9
_cell_volume                     836.44(19)
_computing_cell_refinement       'CAD4-Express (Enraf-Nonius, 1995)'
_computing_data_collection       'CAD4-Express (Enraf-Nonius, 1995)'
_computing_data_reduction        'HELENA (Spek, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CAD4 Enraf-Nonius '
_diffrn_measurement_method       omega/2theta
_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  0.0798
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3637
_diffrn_reflns_theta_full        67.51
_diffrn_reflns_theta_max         67.51
_diffrn_reflns_theta_min         5.64
_exptl_absorpt_coefficient_mu    3.081
_exptl_absorpt_correction_T_max  0.8612
_exptl_absorpt_correction_T_min  0.2594
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0190(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         2968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0925P)^2^+0.2192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                2870
_reflns_number_total             2968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002286l.txt
_cod_data_source_block           imh
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0925P)^2^+0.2192P] 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^)+(0.0925P)^2^+0.2192P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        836.44(17)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C5 H8 N5 O0.50 S'
_cod_database_code               7009604