Coordinative trends of a tridentate thiosemicarbazone ligand: synthesis, characterization, luminescence studies and desulfurization processes
Pedrido, Rosa; Romero, María J.; Bermejo, Manuel R.; Martínez-Calvo, Miguel; González-Noya, Ana M.; Zaragoza, Guillermo; Dalton Transactions  (2009) 8329–8340; doi:10.1039/b908782f

data_7002392
_publ_section_title
;
 Coordinative trends of a tridentate thiosemicarbazone ligand:
 synthesis, characterization, luminescence studies and desulfurization
 processes
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              8329
_journal_page_last               8340
_journal_paper_doi               10.1039/b908782f
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C9 H12 N4 S1'
_chemical_formula_sum            'C9 H12 N4 S'
_chemical_formula_weight         208.29
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-02-25T17:10:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.8982(6)
_cell_length_b                   13.8982(6)
_cell_length_c                   22.2966(11)
_cell_measurement_reflns_used    1949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.6
_cell_measurement_theta_min      0.99
_cell_measurement_wavelength     1.5418
_cell_volume                     4306.8(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_detector_area_resol_mean 14
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '135mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD2000
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_UB_11      0.0602719
_diffrn_orient_matrix_UB_12      0.0373552
_diffrn_orient_matrix_UB_13      -0.0076075
_diffrn_orient_matrix_UB_21      0.0040867
_diffrn_orient_matrix_UB_22      -0.0281821
_diffrn_orient_matrix_UB_23      -0.0411877
_diffrn_orient_matrix_UB_31      -0.0390853
_diffrn_orient_matrix_UB_32      0.0546573
_diffrn_orient_matrix_UB_33      -0.0160377
_diffrn_radiation_monochromator  'graded mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11934
_diffrn_reflns_theta_full        66.65
_diffrn_reflns_theta_max         66.65
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    2.407
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.128
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+2.4318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                1611
_reflns_number_total             1909
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b908782f.txt
_cod_data_source_block           2004be15
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7002392