#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:18:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179321 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/18/4321899.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4321899
loop_
_publ_author_name
'Ze-Hua Liu'
'Chun-Ying Duan'
'Jun Hu'
'Xiao-Zeng You'
_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       '2θ/ω 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/[σ²(Fo²)+(0.0700P)²+0.1500P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd1 Pd 0.417962(12) 0.209518(14) 0.077033(12) 0.02894(4) Uani 1 d . .
S1 S 0.58495(5) 0.18320(6) 0.02161(3) 0.0440(2) Uani 1 d . .
S2 S 0.58459(5) 0.40263(6) 0.13253(3) 0.0437(2) Uani 1 d . .
N1 N 0.5323(2) -0.0756(2) -0.01702(11) 0.0501(7) Uani 1 d . .
H1A H 0.4810(2) -0.1649(2) -0.02755(11) 0.060 Uiso 1 calc R .
H1B H 0.6245(2) -0.0344(2) -0.01804(11) 0.060 Uiso 1 calc R .
N2 N 0.3255(2) -0.0638(2) 0.00272(9) 0.0341(6) Uani 1 d . .
N3 N 0.28187(15) 0.03281(14) 0.01622(8) 0.0290(5) Uani 1 d . .
N4 N -0.2324(2) -0.2643(2) -0.01712(9) 0.0414(6) Uani 1 d . .
N5 N -0.1513(2) 0.0562(2) -0.00972(10) 0.0432(6) Uani 1 d . .
N6 N 0.5286(2) 0.6037(2) 0.17149(11) 0.0483(7) Uani 1 d . .
H6A H 0.4744(2) 0.6375(2) 0.18347(11) 0.058 Uiso 1 calc R .
H6B H 0.6205(2) 0.6576(2) 0.17277(11) 0.058 Uiso 1 calc R .
N7 N 0.32898(14) 0.3943(2) 0.15076(9) 0.0347(6) Uani 1 d . .
N8 N 0.28059(15) 0.25043(15) 0.13783(9) 0.0304(5) Uani 1 d . .
N9 N -0.2302(2) 0.0311(2) 0.17161(9) 0.0387(6) Uani 1 d . .
N10 N -0.1503(2) -0.2063(2) 0.16283(10) 0.0388(6) Uani 1 d . .
C1 C 0.4674(2) 0.0007(2) 0.00133(12) 0.0413(7) Uani 1 d . .
C2 C 0.1486(2) -0.0081(2) 0.00039(10) 0.0283(6) Uani 1 d . .
C3 C -0.2385(2) -0.3901(2) -0.02559(11) 0.0445(8) Uani 1 d . .
H3A H -0.3275(2) -0.4712(2) -0.03324(11) 0.053 Uiso 1 calc R .
C4 C -0.1178(2) -0.4055(2) -0.02349(13) 0.0462(8) Uani 1 d . .
H4A H -0.1288(2) -0.4969(2) -0.02569(13) 0.055 Uiso 1 calc R .
C5 C 0.0167(2) -0.2889(2) -0.01827(12) 0.0439(7) Uani 1 d . .
H5A H 0.0982(2) -0.2983(2) -0.01867(12) 0.053 Uiso 1 calc R .
C6 C 0.0264(2) -0.1570(2) -0.01239(10) 0.0306(6) Uani 1 d . .
C7 C -0.1027(2) -0.1506(2) -0.01246(10) 0.0286(6) Uani 1 d . .
C8 C -0.0611(2) 0.0039(2) -0.00504(10) 0.0264(6) Uani 1 d . .
C9 C 0.0902(2) 0.0853(2) -0.00060(10) 0.0252(6) Uani 1 d . .
C10 C 0.1523(2) 0.2352(2) -0.00137(11) 0.0405(7) Uani 1 d . .
H10A H 0.2514(2) 0.2942(2) 0.00105(11) 0.049 Uiso 1 calc R .
C11 C 0.0636(2) 0.2939(2) -0.00580(11) 0.0399(7) Uani 1 d . .
H11A H 0.1015(2) 0.3928(2) -0.00805(11) 0.048 Uiso 1 calc R .
C12 C -0.0867(2) 0.1983(2) -0.00680(11) 0.0386(7) Uani 1 d . .
H12A H -0.1454(2) 0.2388(2) -0.00527(11) 0.046 Uiso 1 calc R .
C13 C 0.4703(2) 0.4680(2) 0.15095(10) 0.0325(7) Uani 1 d . .
C14 C 0.1485(2) 0.1582(2) 0.15349(9) 0.0268(6) Uani 1 d . .
C15 C -0.2360(2) 0.1534(2) 0.17747(12) 0.0506(8) Uani 1 d . .
H15A H -0.3260(2) 0.1457(2) 0.18005(12) 0.061 Uiso 1 calc R .
C16 C -0.1180(2) 0.2875(2) 0.17982(13) 0.0492(7) Uani 1 d . .
H16A H -0.1302(2) 0.3665(2) 0.18604(13) 0.059 Uiso 1 calc R .
C17 C 0.0185(2) 0.3084(2) 0.17320(11) 0.0434(7) Uani 1 d . .
H17A H 0.0997(2) 0.3994(2) 0.17411(11) 0.052 Uiso 1 calc R .
C18 C 0.0269(2) 0.1842(2) 0.16504(10) 0.0310(6) Uani 1 d . .
C19 C -0.1011(2) 0.0490(2) 0.16579(10) 0.0296(6) Uani 1 d . .
C20 C -0.0606(2) -0.0625(2) 0.16080(10) 0.0322(7) Uani 1 d . .
C21 C 0.0889(2) 0.0004(2) 0.15255(10) 0.0298(6) Uani 1 d . .
C22 C 0.1517(2) -0.0816(2) 0.15553(10) 0.0379(7) Uani 1 d . .
H22A H 0.2511(2) -0.0403(2) 0.15538(10) 0.045 Uiso 1 calc R .
C23 C 0.0639(2) -0.2268(2) 0.15877(11) 0.0381(6) Uani 1 d . .
H23A H 0.1010(2) -0.2886(2) 0.15848(11) 0.046 Uiso 1 calc R .
C24 C -0.0868(2) -0.2804(2) 0.16260(14) 0.0513(9) Uani 1 d . .
H24A H -0.1453(2) -0.3796(2) 0.16522(14) 0.062 Uiso 1 calc R .
O1W O -0.5467(2) -0.3778(2) -0.02369(13) 0.0906(9) Uani 1 d . .
O3W O -0.5451(2) -0.1627(2) 0.17909(13) 0.0893(9) Uani 1 d . .
O2W O -0.7147(2) -0.3550(3) 0.07660(14) 0.1143(12) Uani 1 d . .
H3WA H -0.4734(19) -0.1039(19) 0.1851(11) 0.043(6) Uiso 1 d . .
H3WB H -0.5476(20) -0.1802(20) 0.1441(11) 0.050(7) Uiso 1 d . .
H1WA H -0.4950(22) -0.3553(23) -0.0052(13) 0.065(8) Uiso 1 d . .
H1WB H -0.5650(27) -0.4008(27) -0.0524(15) 0.094(10) Uiso 1 d . .
H2WB H -0.6576(21) -0.3747(22) 0.0445(12) 0.060(7) Uiso 1 d . .
H2WA H -0.7604(26) -0.4141(26) 0.0938(15) 0.092(10) Uiso 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Pd1 N8 105.84(6) . . ?
N3 Pd1 S2 172.82(5) . . ?
N8 Pd1 S2 81.03(4) . . ?
N3 Pd1 S1 80.97(5) . . ?
N8 Pd1 S1 172.93(4) . . ?
S2 Pd1 S1 92.24(2) . . ?
C1 S1 Pd1 94.53(8) . . ?
C13 S2 Pd1 94.55(6) . . ?
C1 N2 N3 110.5(2) . . ?
C2 N3 N2 115.59(14) . . ?
C2 N3 Pd1 126.25(15) . . ?
N2 N3 Pd1 116.88(11) . . ?
C7 N4 C3 116.2(2) . . ?
C12 N5 C8 114.0(2) . . ?
C13 N7 N8 110.4(2) . . ?
C14 N8 N7 117.6(2) . . ?
C14 N8 Pd1 126.00(14) . . ?
N7 N8 Pd1 115.19(10) . . ?
C19 N9 C15 115.24(14) . . ?
C24 N10 C20 114.4(2) . . ?
N2 C1 N1 119.5(2) . . ?
N2 C1 S1 125.0(2) . . ?
N1 C1 S1 115.54(13) . . ?
N3 C2 C9 124.02(15) . . ?
N3 C2 C6 128.8(2) . . ?
C9 C2 C6 106.8(2) . . ?
N4 C3 C4 122.9(2) . . ?
C5 C4 C3 121.2(2) . . ?
C4 C5 C6 116.9(2) . . ?
C5 C6 C7 118.5(2) . . ?
C5 C6 C2 133.6(2) . . ?
C7 C6 C2 107.7(2) . . ?
N4 C7 C6 124.0(2) . . ?
N4 C7 C8 128.7(2) . . ?
C6 C7 C8 107.26(13) . . ?
N5 C8 C9 126.3(2) . . ?
N5 C8 C7 125.45(14) . . ?
C9 C8 C7 107.8(2) . . ?
C10 C9 C8 116.7(2) . . ?
C10 C9 C2 133.3(2) . . ?
C8 C9 C2 109.93(15) . . ?
C11 C10 C9 119.0(2) . . ?
C10 C11 C12 117.7(2) . . ?
N5 C12 C11 126.0(2) . . ?
N7 C13 N6 115.5(2) . . ?
N7 C13 S2 126.5(2) . . ?
N6 C13 S2 117.91(14) . . ?
N8 C14 C21 123.5(2) . . ?
N8 C14 C18 128.5(2) . . ?
C21 C14 C18 107.43(13) . . ?
N9 C15 C16 124.1(2) . . ?
C15 C16 C17 121.5(2) . . ?
C16 C17 C18 115.5(2) . . ?
C17 C18 C19 119.2(2) . . ?
C17 C18 C14 133.17(14) . . ?
C19 C18 C14 107.7(2) . . ?
N9 C19 C18 124.5(2) . . ?
N9 C19 C20 127.75(15) . . ?
C18 C19 C20 107.7(2) . . ?
N10 C20 C21 122.9(2) . . ?
N10 C20 C19 126.7(2) . . ?
C21 C20 C19 110.5(2) . . ?
C22 C21 C20 120.3(2) . . ?
C22 C21 C14 132.3(2) . . ?
C20 C21 C14 106.5(2) . . ?
C21 C22 C23 117.5(2) . . ?
C22 C23 C24 117.5(2) . . ?
N10 C24 C23 126.9(2) . . ?
H1WA O1W H1WB 140.3(38) . . ?
H3WA O3W H3WB 105.9(21) . . ?
H2WB O2W H2WA 111.6(31) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N3 2.1046(14) . ?
Pd1 N8 2.117(2) . ?
Pd1 S2 2.2394(7) . ?
Pd1 S1 2.2410(8) . ?
S1 C1 1.768(2) . ?
S2 C13 1.732(3) . ?
N1 C1 1.366(3) . ?
N2 C1 1.323(2) . ?
N2 N3 1.362(3) . ?
N3 C2 1.309(2) . ?
N4 C7 1.320(2) . ?
N4 C3 1.331(3) . ?
N5 C12 1.325(3) . ?
N5 C8 1.345(3) . ?
N6 C13 1.331(3) . ?
N7 C13 1.316(2) . ?
N7 N8 1.387(2) . ?
N8 C14 1.299(2) . ?
N9 C19 1.307(3) . ?
N9 C15 1.352(3) . ?
N10 C24 1.282(4) . ?
N10 C20 1.353(2) . ?
C2 C9 1.426(3) . ?
C2 C6 1.500(2) . ?
C3 C4 1.388(4) . ?
C4 C5 1.363(2) . ?
C5 C6 1.374(3) . ?
C6 C7 1.423(3) . ?
C7 C8 1.496(3) . ?
C8 C9 1.413(2) . ?
C9 C10 1.402(3) . ?
C10 C11 1.384(4) . ?
C11 C12 1.416(2) . ?
C14 C21 1.484(3) . ?
C14 C18 1.485(3) . ?
C15 C16 1.363(2) . ?
C16 C17 1.375(3) . ?
C17 C18 1.392(3) . ?
C18 C19 1.417(2) . ?
C19 C20 1.469(3) . ?
C20 C21 1.407(3) . ?
C21 C22 1.353(4) . ?
C22 C23 1.364(2) . ?
C23 C24 1.424(3) . ?
O1W H1WA 0.61(2) . ?
O1W H1WB 0.61(3) . ?
O3W H3WA 0.72(2) . ?
O3W H3WB 0.72(2) . ?
O2W H2WB 0.98(3) . ?
O2W H2WA 0.67(2) . ?
