#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/28/2212852.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2212852
loop_
_publ_author_name
'Dorazco-Gonzalez, Alejandro'
'Hernández-Ortega, Simón'
'Valdés-Martínez, Jesús'
_publ_section_title
;
 cis-Bis(thiosemicarbazide-κ²N¹,S)palladium(II)
 dinitrate
;
_journal_coeditor_code           DN2141
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1120
_journal_page_last               m1121
_journal_paper_doi               10.1107/S160053680701224X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Pd (C H5 N3 S)] (N O3)2'
_chemical_formula_moiety         'C2 H10 N6 Pd S2 , 2N O3'
_chemical_formula_sum            'C2 H10 N8 O6 Pd S2'
_chemical_formula_weight         412.70
_chemical_name_systematic
;
cis-Bis(thiosemicarbazide-κ²N¹,S)palladium(II) dinitrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0540(5)
_cell_length_b                   8.8997(5)
_cell_length_c                   15.0991(9)
_cell_measurement_reflns_used    8014
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.29
_cell_volume                     1211.78(12)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9854
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_T_max  0.6357
_exptl_absorpt_correction_T_min  0.5454
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Sheldrick, 2000)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.467
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0221P)²+0.4048P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0456
_reflns_number_gt                2094
_reflns_number_total             2215
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2141.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212852
_cod_database_fobs_code          2212852
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Pd Pd1 0.749137(16) 0.489779(16) 0.511140(10) 0.02227(7) Uani d . 1
S S1 0.62827(6) 0.42910(6) 0.37817(3) 0.02786(13) Uani d . 1
S S2 0.87784(6) 0.68175(6) 0.45651(3) 0.02746(13) Uani d . 1
N N1 0.62789(19) 0.31931(19) 0.56212(11) 0.0270(4) Uani d . 1
H H1A 0.6910 0.2484 0.5852 0.032 Uiso calc R 1
H H1B 0.5796 0.3566 0.6069 0.032 Uiso calc R 1
N N2 0.52323(19) 0.2507(2) 0.49940(10) 0.0281(4) Uani d . 1
H H2 0.4645 0.1828 0.5166 0.034 Uiso calc R 1
N N3 0.4166(2) 0.2243(2) 0.35833(12) 0.0331(4) Uani d . 1
H H3A 0.3585 0.1565 0.3764 0.040 Uiso calc R 1
H H3B 0.4104 0.2493 0.3031 0.040 Uiso calc R 1
N N4 0.86491(19) 0.5395(2) 0.63200(11) 0.0272(4) Uani d . 1
H H4A 0.7995 0.5561 0.6724 0.033 Uiso calc R 1
H H4B 0.9199 0.4591 0.6502 0.033 Uiso calc R 1
N N5 0.9592(2) 0.6660(2) 0.62972(11) 0.0311(4) Uani d . 1
H H5 1.0052 0.6985 0.6783 0.037 Uiso calc R 1
N N6 1.0739(2) 0.8456(2) 0.55428(13) 0.0342(4) Uani d . 1
H H6A 1.1233 0.8721 0.6031 0.041 Uiso calc R 1
H H6B 1.0873 0.8916 0.5055 0.041 Uiso calc R 1
C C1 0.5150(2) 0.2899(2) 0.41538(14) 0.0252(4) Uani d . 1
C C2 0.9776(2) 0.7344(2) 0.55420(13) 0.0259(4) Uani d . 1
N N7 0.6510(2) 0.5695(2) 0.84624(12) 0.0300(4) Uani d . 1
O O1 0.64373(19) 0.52488(17) 0.92373(11) 0.0352(4) Uani d . 1
O O2 0.7310(2) 0.50128(19) 0.79659(13) 0.0499(5) Uani d . 1
O O3 0.5803(2) 0.6835(2) 0.81967(10) 0.0462(4) Uani d . 1
N N8 0.8466(2) 0.0635(2) 0.68309(12) 0.0296(4) Uani d . 1
O O4 0.8780(2) 0.19709(18) 0.70365(11) 0.0437(4) Uani d . 1
O O5 0.8831(2) -0.04067(19) 0.73405(12) 0.0464(5) Uani d . 1
O O6 0.77488(19) 0.03800(19) 0.60922(11) 0.0383(4) Uani d . 1
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
N1 Pd1 N4 94.17(7)
N1 Pd1 S1 85.66(5)
N4 Pd1 S1 178.02(5)
N1 Pd1 S2 178.40(5)
N4 Pd1 S2 85.60(5)
S1 Pd1 S2 94.622(19)
C1 S1 Pd1 97.82(7)
C2 S2 Pd1 98.07(7)
N2 N1 Pd1 114.46(12)
N2 N1 H1A 108.6
Pd1 N1 H1A 108.6
N2 N1 H1B 108.6
Pd1 N1 H1B 108.6
H1A N1 H1B 107.6
C1 N2 N1 120.60(17)
C1 N2 H2 119.7
N1 N2 H2 119.7
C1 N3 H3A 120.0
C1 N3 H3B 120.0
H3A N3 H3B 120.0
N5 N4 Pd1 114.07(12)
N5 N4 H4A 108.7
Pd1 N4 H4A 108.7
N5 N4 H4B 108.7
Pd1 N4 H4B 108.7
H4A N4 H4B 107.6
C2 N5 N4 120.80(17)
C2 N5 H5 119.6
N4 N5 H5 119.6
C2 N6 H6A 120.0
C2 N6 H6B 120.0
H6A N6 H6B 120.0
N2 C1 N3 119.40(19)
N2 C1 S1 121.29(16)
N3 C1 S1 119.30(16)
N5 C2 N6 118.75(19)
N5 C2 S2 121.24(16)
N6 C2 S2 120.01(16)
O1 N7 O2 119.54(19)
O1 N7 O3 119.63(18)
O2 N7 O3 120.82(18)
O5 N8 O4 121.12(18)
O5 N8 O6 120.37(19)
O4 N8 O6 118.50(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 N1 2.0616(17)
Pd1 N4 2.0695(17)
Pd1 S1 2.2644(5)
Pd1 S2 2.2647(5)
S1 C1 1.734(2)
S2 C2 1.724(2)
N1 N2 1.417(2)
N1 H1A 0.9000
N1 H1B 0.9000
N2 C1 1.311(2)
N2 H2 0.8600
N3 C1 1.319(3)
N3 H3A 0.8600
N3 H3B 0.8600
N4 N5 1.415(2)
N4 H4A 0.9000
N4 H4B 0.9000
N5 C2 1.316(3)
N5 H5 0.8600
N6 C2 1.319(3)
N6 H6A 0.8600
N6 H6B 0.8600
N7 O1 1.243(2)
N7 O2 1.246(2)
N7 O3 1.246(2)
N8 O5 1.231(2)
N8 O4 1.255(2)
N8 O6 1.260(2)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A O6 . 0.90 2.04 2.894(2) 157.7
N1 H1A O4 . 0.90 2.39 3.164(2) 143.5
N1 H1B O3 2_646 0.90 2.45 2.967(2) 117.1
N1 H1B S1 3_666 0.90 2.70 3.4027(19) 135.3
N2 H2 O1 2_646 0.86 1.98 2.826(2) 169.2
N2 H2 O3 2_646 0.86 2.54 3.026(2) 116.7
N3 H3A O6 3_656 0.86 2.13 2.974(3) 165.7
N3 H3B O3 3_666 0.86 1.96 2.813(2) 173.3
N4 H4A O2 . 0.90 2.08 2.881(2) 147.0
N4 H4B O5 2_756 0.90 2.38 2.996(3) 125.4
N4 H4B O4 . 0.90 2.51 3.232(2) 137.9
N4 H4B S2 3_766 0.90 2.84 3.4124(19) 123.1
N5 H5 O4 2_756 0.86 1.99 2.813(2) 159.9
N6 H6A O2 2_756 0.86 2.24 3.066(3) 162.1
N6 H6A O1 2_756 0.86 2.57 3.007(2) 112.4
N6 H6B O6 3_766 0.86 2.31 3.106(3) 153.8
