#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/97/2239751.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_2239751
loop_
_publ_author_name
'Reyes-Martínez, Reyna'
'Carballo, Rubén M.'
'Mena-Rejón, Gonzalo J.'
'Hernández-Ortega, Simón'
'Cáceres-Castillo, David'
_publ_section_title
;
 Bis(2-amino-4-phenyl-1,3-thiazol-3-ium) tetrachloridopalladate(II)
;
_journal_coeditor_code           PJ2013
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m295
_journal_paper_doi               10.1107/S1600536814015360
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C9 H9 N2 S)2 [Pd Cl4]'
_chemical_formula_moiety         '2(C9 H9 N2 S +), Cl4 Pd 2-'
_chemical_formula_sum            'C18 H18 Cl4 N4 Pd S2'
_chemical_formula_weight         602.68
_chemical_name_systematic
;
Bis(2-amino-4-phenyl-1,3-thiazol-3-ium) tetrachloridopalladate(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                66.2580(10)
_cell_angle_beta                 73.7780(10)
_cell_angle_gamma                84.4680(10)
_cell_formula_units_Z            1
_cell_length_a                   7.2880(2)
_cell_length_b                   8.9214(3)
_cell_length_c                   9.8192(3)
_cell_measurement_reflns_used    4506
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.35
_cell_volume                     561.04(3)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg,
2006)
;
_computing_publication_material
'SHELXTL  (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.388
_diffrn_reflns_theta_min         2.349
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  0.8417
_exptl_absorpt_correction_T_min  0.6584
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2012)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       Prism
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.463
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.205
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.300
_refine_ls_extinction_coef       0.015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2060
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0270P)²+0.0969P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0508
_reflns_number_gt                1982
_reflns_number_total             2060
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pj2013sup1.cf
_cod_data_source_block           I
_cod_database_code               2239751
_cod_database_fobs_code          2239751
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.543
_shelx_estimated_absorpt_t_max   0.748
_shelxl_version_number           20.13
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
Pd Pd 0.5000 0.0000 1.0000 0.03103(10) Uani d 1
Cl Cl1 0.54163(7) 0.23160(6) 0.77534(6) 0.04971(15) Uani d 1
Cl Cl2 0.78000(7) -0.10267(6) 0.89335(6) 0.04577(14) Uani d 1
N N1 0.9774(2) 0.2276(2) 0.56952(19) 0.0382(4) Uani d 1
H H1 0.8651(19) 0.185(3) 0.628(2) 0.046 Uiso d 1
C C2 1.1103(3) 0.2483(2) 0.6301(2) 0.0380(4) Uani d 1
N N2 1.0983(3) 0.1821(2) 0.7791(2) 0.0527(5) Uani d 1
H H2A 1.203(2) 0.195(3) 0.804(3) 0.063 Uiso d 1
H H2B 1.001(3) 0.112(3) 0.837(3) 0.063 Uiso d 1
S S3 1.29130(7) 0.37696(7) 0.49056(6) 0.04726(15) Uani d 1
C C4 1.1739(3) 0.4022(3) 0.3520(2) 0.0459(5) Uani d 1
H H4 1.2196 0.4690 0.2481 0.055 Uiso calc 1
C C5 1.0096(3) 0.3149(2) 0.4107(2) 0.0365(4) Uani d 1
C C6 0.8732(3) 0.3009(2) 0.3309(2) 0.0374(4) Uani d 1
C C7 0.8497(3) 0.4318(3) 0.2005(2) 0.0484(5) Uani d 1
H H7 0.9175 0.5291 0.1660 0.058 Uiso calc 1
C C8 0.7259(4) 0.4194(3) 0.1206(3) 0.0572(6) Uani d 1
H H8 0.7096 0.5087 0.0340 0.069 Uiso calc 1
C C9 0.6278(4) 0.2758(3) 0.1694(3) 0.0585(6) Uani d 1
H H9 0.5474 0.2666 0.1143 0.070 Uiso calc 1
C C10 0.6482(3) 0.1453(3) 0.2995(3) 0.0576(6) Uani d 1
H H10 0.5800 0.0484 0.3328 0.069 Uiso calc 1
C C11 0.7696(3) 0.1563(3) 0.3820(3) 0.0475(5) Uani d 1
H H11 0.7815 0.0678 0.4707 0.057 Uiso calc 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
Cl1 Pd Cl1 . 2_657 180.0
Cl1 Pd Cl2 . 2_657 90.134(19)
Cl1 Pd Cl2 2_657 2_657 89.866(19)
Cl1 Pd Cl2 . . 89.866(19)
Cl1 Pd Cl2 2_657 . 90.134(19)
Cl2 Pd Cl2 2_657 . 180.00(2)
C2 N1 C5 . . 115.25(16)
C2 N1 H1 . . 120.8(15)
C5 N1 H1 . . 121.9(15)
N2 C2 N1 . . 123.49(18)
N2 C2 S3 . . 125.28(16)
N1 C2 S3 . . 111.19(14)
C2 N2 H2A . . 114.7(17)
C2 N2 H2B . . 115.3(18)
H2A N2 H2B . . 128(2)
C2 S3 C4 . . 90.03(10)
C5 C4 S3 . . 112.71(16)
C5 C4 H4 . . 123.6
S3 C4 H4 . . 123.6
C4 C5 N1 . . 110.80(17)
C4 C5 C6 . . 129.09(18)
N1 C5 C6 . . 120.10(17)
C7 C6 C11 . . 119.06(19)
C7 C6 C5 . . 119.70(18)
C11 C6 C5 . . 121.22(19)
C6 C7 C8 . . 120.7(2)
C6 C7 H7 . . 119.7
C8 C7 H7 . . 119.7
C9 C8 C7 . . 120.0(2)
C9 C8 H8 . . 120.0
C7 C8 H8 . . 120.0
C8 C9 C10 . . 120.0(2)
C8 C9 H9 . . 120.0
C10 C9 H9 . . 120.0
C9 C10 C11 . . 120.7(2)
C9 C10 H10 . . 119.6
C11 C10 H10 . . 119.6
C10 C11 C6 . . 119.5(2)
C10 C11 H11 . . 120.2
C6 C11 H11 . . 120.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd Cl1 . 2.3031(5)
Pd Cl1 2_657 2.3031(5)
Pd Cl2 2_657 2.3061(5)
Pd Cl2 . 2.3061(5)
N1 C2 . 1.331(2)
N1 C5 . 1.395(3)
N1 H1 . 0.876(10)
C2 N2 . 1.319(3)
C2 S3 . 1.7179(19)
N2 H2A . 0.894(10)
N2 H2B . 0.887(10)
S3 C4 . 1.733(2)
C4 C5 . 1.343(3)
C4 H4 . 0.9300
C5 C6 . 1.468(3)
C6 C7 . 1.383(3)
C6 C11 . 1.393(3)
C7 C8 . 1.388(3)
C7 H7 . 0.9300
C8 C9 . 1.369(4)
C8 H8 . 0.9300
C9 C10 . 1.373(4)
C9 H9 . 0.9300
C10 C11 . 1.389(3)
C10 H10 . 0.9300
C11 H11 . 0.9300
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
N2 H2B Cl2 . 0.887(10) 2.412(15) 3.237(2) 155(2)
N2 H2A Cl2 2_757 0.894(10) 2.78(2) 3.3572(19) 123(2)
N2 H2A Cl1 1_655 0.894(10) 2.442(14) 3.291(2) 159(2)
N1 H1 Cl2 . 0.876(10) 2.786(19) 3.4028(17) 128.6(18)
N1 H1 Cl1 . 0.876(10) 2.492(15) 3.2593(17) 146.5(19)
