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_4321899
_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_analytical     'C24H16N10S2Pd H6O3'
_chemical_formula_moiety         (C12H8N5S)2Pd(H2O)3
_chemical_formula_structural     '[(C11H6N2)CNNCS(NH2)]Pd  [H2O]3'
_chemical_formula_sum            'C24 H22 N10 O3 Pd S2'
_chemical_formula_weight         669.04
_chemical_name_systematic
; 
 bis(4,5-diazafluorene-9-one thiosemicarbazone)palladium(II) trihydrate 
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.749(3)
_cell_length_b                   10.749(3)
_cell_length_c                   19.872(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.12
_cell_measurement_theta_min      4.51
_cell_volume                     1988.4(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w 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  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3221
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        6.60
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.5466
_exptl_absorpt_correction_T_min  0.4797
_exptl_absorpt_correction_type   'Semi-emprical from psi-scan'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.090
_refine_ls_goodness_of_fit_obs   1.138
_refine_ls_hydrogen_treatment    'riding with fixed Uiso'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         2536
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_obs          0.0602
_refine_ls_shift/esd_max         -0.100
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1470
_refine_ls_wR_factor_obs         0.1339
_reflns_number_observed          2011
_reflns_number_total             2539
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9711731_2.cif
_cod_data_source_block           for_the_palladium_compex
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.1500P] 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^)+(0.0700P)^2^+0.1500P] 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        1988.3(8)
_cod_database_code               4321899