Design, Synthesis, and Crystal Structure of a cis-Configuration N2S2-Coordinated Palladium(II) Complex: Role of the Intra- and Intermolecular Aromatic-Ring Stacking Interaction
Ze-Hua Liu; Chun-Ying Duan; Jun Hu; Xiao-Zeng You; Inorganic Chemistry 38 (1999) 1719–1724; doi:10.1021/ic9711731

data_4321898
_publ_section_title
;
 Design, Synthesis, and Crystal Structure of a cis-Configuration
 N2S2-Coordinated Palladium(II) Complex: Role of the Intra- and
 Intermolecular Aromatic-Ring Stacking Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1719
_journal_page_last               1724
_journal_paper_doi               10.1021/ic9711731
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_moiety         (C11H6N2)CNNHCSNH2
_chemical_formula_sum            'C12 H9 N5 S'
_chemical_formula_weight         255.30
_chemical_name_systematic
; 
4,5-DIAZAFLUORENE 9-ONE THIOSEMICARBAZONE 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
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_cell_length_b                   15.427(3)
_cell_length_c                   17.387(3)
_cell_measurement_reflns_used    264
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55
_cell_measurement_theta_min      3
_cell_volume                     2272.7(8)
_computing_cell_refinement       biotex
_computing_data_collection       biotex
_computing_data_reduction        biotex
_computing_molecular_graphics    'SHELXTL 5.0(Siemens, 1995)'
_computing_publication_material  'SHELXTL 5.0(Siemens, 1995)'
_computing_structure_refinement  'SHELXTL 5.0(Siemens, 1995)'
_computing_structure_solution    'SHELXTL 5.0(Siemens, 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Regaku Raxis II'
_diffrn_measurement_method       'Take oscillation photos'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.041
_refine_ls_goodness_of_fit_all   0.792
_refine_ls_goodness_of_fit_obs   0.775
_refine_ls_hydrogen_treatment    'refined isotropically'
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_refine_ls_number_reflns         2353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      0.775
_refine_ls_R_factor_all          0.1443
_refine_ls_R_factor_obs          0.0413
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1782
_refine_ls_wR_factor_obs         0.0859
_reflns_number_observed          1111
_reflns_number_total             2354
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9711731_1.cif
_cod_data_source_block           Free_ligand_HL
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthromobic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0500P] 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^)+(0.0300P)^2^+0.0500P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321898