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#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/19/2001906.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_2001906
loop_
_publ_author_name
'Román, P.'
'Beitia, J. I.'
'Luque, A.'
_publ_section_title
;
 Structures of 2-amino-3-methylpyridinium
 bis(1,2--dithiooxalato-S,S')metallates(II) (M =
 Ni, Pd and Pt)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              584
_journal_page_last               587
_journal_paper_doi               10.1107/S0108270192010503
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety         'C12 H18 N4 2+,C4 O4 Pd S4 2-'
_chemical_formula_sum            'C16 H18 N4 O4 Pd S4'
_chemical_formula_weight         565.0
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.
_cell_angle_beta                 102.230(10)
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   5.750(4)
_cell_length_b                   16.229(4)
_cell_length_c                   11.728(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     1069.6(9)
_diffrn_measurement_device       CAD-4
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6543
_diffrn_reflns_theta_max         40
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  1.174
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   'empirical (DIFABS: Walker & Stuart, 1983)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_meas      1.760(10)
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.85
_refine_diff_density_min         -0.71
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     169
_refine_ls_number_reflns         4257
_refine_ls_R_factor_obs          0.050
_refine_ls_shift/esd_max         0.11
_refine_ls_structure_factor_coef F
_refine_ls_wR_factor_obs         0.064
_reflns_number_observed          4257
_reflns_number_total             6543
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            mu1013.cif
_cod_data_source_block           mu1013_structure-1_of_1
_cod_original_cell_volume        1070.0(10)
_cod_database_code               2001906
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Pd 0 0 0 .0361(2)
S(1) .34296(8) .05021(6) .11979(6) .0458(3)
S(2) .03191(8) .09769(6) -.13777(6) .0476(3)
C(1) .4403(3) .1274(2) .0413(2) .0407(7)
C(2) .2943(3) .1496(2) -.0817(2) .0402(6)
O(1) .6208(3) .1685(2) .0775(2) .0573(8)
O(2) .3732(3) .2055(2) -.1330(2) .0561(7)
N(11) -.1694(3) .2937(2) -.0433(2) .0428(6)
C(12) .0289(3) .3077(2) .0402(2) .0391(7)
C(13) .1868(4) .3723(2) .0228(3) .0485(9)
C(14) .1248(4) .4164(2) -.0790(3) .0630(11)
C(15) -.0821(5) .3999(2) -.1640(3) .0635(12)
C(16) -.2279(5) .3381(2) -.1439(3) .0547(10)
N(17) .0693(3) .2588(2) .1335(2) .0489(7)
C(18) .4105(6) .3878(3) .1139(4) .0692(12)
H(11) -.272(5) .254(3) -.031(4) .034(9)
H(14) .251(7) .457(4) -.095(6) .068(14)
H(15) -.124(8) .433(4) -.233(5) .055(11)
H(16) -.376(5) .321(3) -.195(4) .032(10)
H(171) .170(6) .271(3) .188(4) .030(10)
H(172) -.039(5) .223(3) .142(3) .022(8)
H(181) .543(9) .418(4) .081(6) .070(16)
H(182) .497(7) .334(4) .145(5) .051(14)
H(183) .375(8) .415(4) .187(6) .066(16)
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
S(1) Pd S(2) 89.96(3) yes
Pd S(1) C(1) 105.32(9) yes
Pd S(2) C(2) 105.15(9) yes
S(1) C(1) O(1) 123.9(2) yes
S(1) C(1) C(2) 119.6(2) yes
C(2) C(1) O(1) 116.4(2) yes
S(2) C(2) C(1) 119.8(2) yes
C(1) C(2) O(2) 116.4(2) yes
S(2) C(2) O(2) 123.8(2) yes
C(12) N(11) C(16) 123.6(2) yes
N(11) C(12) N(17) 118.0(2) yes
N(11) C(12) C(13) 118.8(2) yes
C(13) C(12) N(17) 123.3(2) yes
C(12) C(13) C(18) 119.5(3) yes
C(12) C(13) C(14) 116.8(2) yes
C(14) C(13) C(18) 123.7(3) yes
C(14) C(15) C(16) 118.5(3) yes
C(16) N(11) H(11) 118(2) yes
C(12) N(11) H(11) 119(3) yes
C(13) C(14) H(14) 116(3) yes
C(15) C(14) H(14) 121(4) yes
C(14) C(15) H(15) 121(3) yes
C(16) C(15) H(15) 120(3) yes
N(11) C(16) C(15) 119(3) yes
C(15) C(16) H(16) 127(3) yes
N(11) C(16) H(16) 114(2) yes
C(12) N(17) H(172) 119(2) yes
C(12) N(17) H(171) 119(3) yes
H(171) N(17) H(172) 119(4) yes
C(13) C(18) H(183) 112(3) yes
C(13) C(18) H(182) 113(3) yes
C(13) C(18) H(181) 113(4) yes
H(182) C(18) H(183) 103(5) yes
H(181) C(18) H(182) 101(4) yes
H(181) C(18) H(183) 114(5) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd S(1) 2.3140(10) yes
Pd S(2) 2.2990(10) yes
S(1) C(1) 1.717(3) yes
S(2) C(2) 1.731(2) yes
C(1) C(2) 1.550(3) yes
C(1) O(1) 1.232(3) yes
C(2) O(2) 1.229(4) yes
N(11) C(12) 1.355(2) yes
N(11) C(16) 1.362(3) yes
C(12) C(13) 1.431(3) yes
C(12) N(17) 1.331(3) yes
C(13) C(14) 1.372(4) yes
C(13) C(18) 1.509(4) yes
C(14) C(15) 1.407(4) yes
C(15) C(16) 1.359(5) yes
N(11) H(11) 0.91(4) yes
C(14) H(14) 1.03(6) yes
C(15) H(15) 0.96(6) yes
C(16) H(16) 0.98(3) yes
N(17) H(171) 0.80(4) yes
N(17) H(172) 0.87(4) yes
C(18) H(181) 1.05(7) yes
C(18) H(182) 1.03(6) yes
C(18) H(183) 1.02(8) yes
