#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/56/4085680.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_4085680
loop_
_publ_author_name
'Garrido, Roberto'
'Hernández-Montes, Paulo S.'
'Gordillo, Álvaro'
'Gómez-Sal, Pilar'
'López-Mardomingo, Carmen'
'de Jesús, Ernesto'
_publ_section_title
;
 Water-Soluble Palladium(II) Complexes with Sulfonated N-Heterocyclic
 Carbenes in Suzuki Cross-Coupling and Hydrodehalogenation Reactions
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1855
_journal_paper_doi               10.1021/om501295b
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C49 H100 Cl3 N2 Na3 O17 Pd1 S13'
_chemical_formula_sum            'C49 H100 Cl3 N2 Na3 O17 Pd S13'
_chemical_formula_weight         1687.81
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-07-14T19:14:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                105.246(10)
_cell_angle_beta                 98.497(10)
_cell_angle_gamma                108.882(10)
_cell_formula_units_Z            2
_cell_length_a                   13.207(3)
_cell_length_b                   17.168(2)
_cell_length_c                   19.774(2)
_cell_measurement_reflns_used    265
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.23
_cell_measurement_theta_min      3.34
_cell_measurement_wavelength     0.71073
_cell_volume                     3957.5(12)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1006
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            89916
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.205
_refine_diff_density_min         -1.871
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         17936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0395P)²+31.2411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.164
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                12580
_reflns_number_total             17936
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om501295b_si_002.cif
_cod_data_source_block           import
_cod_depositor_comments          'Adding full bibliography for 4085680.cif.'
_cod_original_cell_volume        3957.5(11)
_cod_original_formula_sum        'C49 H100 Cl3 N2 Na3 O17 Pd1 S13'
_cod_database_code               4085680
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5539(4) 0.2700(3) 0.2518(3) 0.0249(11) Uani 1 1 d . . .
C2 C 0.6615(4) 0.3319(4) 0.1861(3) 0.0334(13) Uani 1 1 d . . .
H2 H 0.6825 0.3555 0.1507 0.04 Uiso 1 1 calc R . .
C3 C 0.7280(5) 0.3228(4) 0.2386(3) 0.0330(13) Uani 1 1 d . . .
H3 H 0.8042 0.3388 0.2468 0.04 Uiso 1 1 calc R . .
C4 C 0.7060(4) 0.2606(4) 0.3381(3) 0.0290(12) Uani 1 1 d . . .
C5 C 0.7512(5) 0.3237(4) 0.4066(3) 0.0335(13) Uani 1 1 d . . .
C6 C 0.8007(5) 0.3004(4) 0.4611(3) 0.0359(13) Uani 1 1 d . . .
H6 H 0.8312 0.3408 0.5077 0.043 Uiso 1 1 calc R . .
C7 C 0.8056(4) 0.2190(4) 0.4480(3) 0.0312(12) Uani 1 1 d . . .
C8 C 0.7608(5) 0.1581(4) 0.3790(3) 0.0317(12) Uani 1 1 d . . .
H8 H 0.7639 0.1031 0.3706 0.038 Uiso 1 1 calc R . .
C9 C 0.7115(4) 0.1773(4) 0.3222(3) 0.0309(12) Uani 1 1 d . . .
C10 C 0.6720(5) 0.1124(4) 0.2452(4) 0.0411(15) Uani 1 1 d . . .
H10 H 0.6178 0.1268 0.2168 0.049 Uiso 1 1 calc R . .
C11 C 0.7681(7) 0.1205(6) 0.2106(4) 0.063(2) Uani 1 1 d . . .
H11A H 0.7425 0.0796 0.1622 0.095 Uiso 1 1 calc R . .
H11B H 0.8235 0.1086 0.2386 0.095 Uiso 1 1 calc R . .
H11C H 0.7994 0.1787 0.209 0.095 Uiso 1 1 calc R . .
C12 C 0.6168(7) 0.0188(5) 0.2428(5) 0.064(2) Uani 1 1 d . . .
H12A H 0.5556 0.0138 0.2644 0.095 Uiso 1 1 calc R . .
H12B H 0.6694 0.0027 0.269 0.095 Uiso 1 1 calc R . .
H12C H 0.5906 -0.0193 0.1933 0.095 Uiso 1 1 calc R . .
C13 C 0.7557(6) 0.4166(4) 0.4217(4) 0.0484(18) Uani 1 1 d . . .
H13 H 0.6996 0.416 0.3829 0.058 Uiso 1 1 calc R . .
C14 C 0.8676(8) 0.4764(5) 0.4196(5) 0.074(3) Uani 1 1 d . . .
H14A H 0.8692 0.5346 0.4289 0.111 Uiso 1 1 calc R . .
H14B H 0.88 0.4561 0.3726 0.111 Uiso 1 1 calc R . .
H14C H 0.9246 0.4763 0.4559 0.111 Uiso 1 1 calc R . .
C15 C 0.7282(9) 0.4497(6) 0.4932(5) 0.078(3) Uani 1 1 d . . .
H15A H 0.7318 0.5083 0.5011 0.117 Uiso 1 1 calc R . .
H15B H 0.7805 0.449 0.532 0.117 Uiso 1 1 calc R . .
H15C H 0.6549 0.4128 0.4915 0.117 Uiso 1 1 calc R . .
C16 C 0.4570(4) 0.2922(4) 0.1448(3) 0.0258(11) Uani 1 1 d . . .
C17 C 0.4075(4) 0.2174(4) 0.0822(3) 0.0271(11) Uani 1 1 d . . .
C18 C 0.3112(4) 0.2108(4) 0.0367(3) 0.0289(12) Uani 1 1 d . . .
H18 H 0.2751 0.162 -0.0048 0.035 Uiso 1 1 calc R . .
C19 C 0.2688(4) 0.2747(4) 0.0519(3) 0.0264(11) Uani 1 1 d . . .
C20 C 0.3223(5) 0.3494(4) 0.1109(3) 0.0303(12) Uani 1 1 d . . .
H20 H 0.2933 0.3926 0.1194 0.036 Uiso 1 1 calc R . .
C21 C 0.4207(4) 0.3612(4) 0.1586(3) 0.0271(11) Uani 1 1 d . . .
C22 C 0.4575(5) 0.1492(4) 0.0615(3) 0.0353(13) Uani 1 1 d . . .
H22 H 0.5038 0.1512 0.106 0.042 Uiso 1 1 calc R . .
C23 C 0.3715(6) 0.0569(4) 0.0261(4) 0.0482(17) Uani 1 1 d . . .
H23A H 0.408 0.0169 0.0145 0.072 Uiso 1 1 calc R . .
H23B H 0.3245 0.0533 -0.0175 0.072 Uiso 1 1 calc R . .
H23C H 0.3277 0.0422 0.0589 0.072 Uiso 1 1 calc R . .
C24 C 0.5322(6) 0.1721(5) 0.0118(5) 0.0531(19) Uani 1 1 d . . .
H24A H 0.564 0.129 -0.001 0.08 Uiso 1 1 calc R . .
H24B H 0.5902 0.2284 0.0366 0.08 Uiso 1 1 calc R . .
H24C H 0.4893 0.1733 -0.0313 0.08 Uiso 1 1 calc R . .
C25 C 0.4856(5) 0.4476(4) 0.2185(3) 0.0354(13) Uani 1 1 d . . .
H25 H 0.5306 0.4369 0.2564 0.042 Uiso 1 1 calc R . .
C26 C 0.4148(6) 0.4914(5) 0.2527(4) 0.0511(18) Uani 1 1 d . . .
H26A H 0.4615 0.5455 0.29 0.077 Uiso 1 1 calc R . .
H26B H 0.3678 0.4539 0.2734 0.077 Uiso 1 1 calc R . .
H26C H 0.3702 0.5027 0.2164 0.077 Uiso 1 1 calc R . .
C27 C 0.5643(6) 0.5083(5) 0.1879(4) 0.0545(19) Uani 1 1 d . . .
H27A H 0.6062 0.5634 0.2254 0.082 Uiso 1 1 calc R . .
H27B H 0.5221 0.5172 0.1488 0.082 Uiso 1 1 calc R . .
H27C H 0.6138 0.4824 0.1703 0.082 Uiso 1 1 calc R . .
C28 C 0.3331(7) 0.0482(6) 0.4837(4) 0.064(2) Uani 1 1 d . . .
H28A H 0.2738 0.0044 0.4916 0.097 Uiso 1 1 calc R . .
H28B H 0.3039 0.0826 0.4616 0.097 Uiso 1 1 calc R . .
H28C H 0.3853 0.0851 0.5292 0.097 Uiso 1 1 calc R . .
C29 C 0.5003(7) 0.0929(7) 0.4226(5) 0.078(3) Uani 1 1 d . . .
H29A H 0.5462 0.0772 0.3925 0.117 Uiso 1 1 calc R . .
H29B H 0.5453 0.1282 0.4707 0.117 Uiso 1 1 calc R . .
H29C H 0.464 0.1253 0.4028 0.117 Uiso 1 1 calc R . .
C30 C 0.3980(7) -0.2213(7) 0.3559(5) 0.078(3) Uani 1 1 d . . .
H30A H 0.4305 -0.1771 0.3357 0.118 Uiso 1 1 calc R . .
H30B H 0.4551 -0.2346 0.3807 0.118 Uiso 1 1 calc R . .
H30C H 0.3595 -0.2006 0.3896 0.118 Uiso 1 1 calc R . .
C31 C 0.2631(11) -0.3799(8) 0.3420(6) 0.092(4) Uani 1 1 d . . .
H31A H 0.2098 -0.4367 0.3125 0.138 Uiso 1 1 calc R . .
H31B H 0.2308 -0.3518 0.3763 0.138 Uiso 1 1 calc R . .
H31C H 0.3266 -0.3856 0.3675 0.138 Uiso 1 1 calc R . .
C32 C -0.0621(9) -0.4061(6) 0.2723(5) 0.075(3) Uani 1 1 d . . .
H32A H -0.0887 -0.3961 0.3152 0.112 Uiso 1 1 calc R . .
H32B H 0.0173 -0.3823 0.2856 0.112 Uiso 1 1 calc R . .
H32C H -0.0885 -0.4678 0.2471 0.112 Uiso 1 1 calc R . .
C33 C -0.0473(8) -0.3868(6) 0.1437(5) 0.067(2) Uani 1 1 d . . .
H33A H -0.0654 -0.3643 0.106 0.1 Uiso 1 1 calc R . .
H33B H -0.0741 -0.4493 0.1243 0.1 Uiso 1 1 calc R . .
H33C H 0.0316 -0.3637 0.1627 0.1 Uiso 1 1 calc R . .
C34 C -0.3983(8) -0.2024(7) 0.2412(5) 0.072(3) Uani 1 1 d . . .
H34A H -0.3975 -0.1482 0.2713 0.108 Uiso 1 1 calc R . .
H34B H -0.3645 -0.2282 0.2708 0.108 Uiso 1 1 calc R . .
H34C H -0.4733 -0.2414 0.217 0.108 Uiso 1 1 calc R . .
C35 C -0.3416(8) -0.2928(6) 0.1324(7) 0.085(3) Uani 1 1 d . . .
H35A H -0.3052 -0.2952 0.0938 0.127 Uiso 1 1 calc R . .
H35B H -0.4191 -0.328 0.113 0.127 Uiso 1 1 calc R . .
H35C H -0.3101 -0.3146 0.1667 0.127 Uiso 1 1 calc R . .
C38 C 0.1938(6) -0.1362(6) 0.0781(4) 0.058(2) Uani 1 1 d . . .
H38A H 0.1197 -0.1469 0.0538 0.087 Uiso 1 1 calc R . .
H38B H 0.2315 -0.1551 0.0431 0.087 Uiso 1 1 calc R . .
H38C H 0.2325 -0.0749 0.104 0.087 Uiso 1 1 calc R . .
C39 C 0.3354(6) -0.1601(6) 0.1732(5) 0.061(2) Uani 1 1 d . . .
H39A H 0.3505 -0.1862 0.2088 0.092 Uiso 1 1 calc R . .
H39B H 0.3675 -0.0977 0.1948 0.092 Uiso 1 1 calc R . .
H39C H 0.3667 -0.1777 0.1338 0.092 Uiso 1 1 calc R . .
C40 C -0.0771(6) -0.0809(6) 0.3992(4) 0.0518(18) Uani 1 1 d . . .
H40A H -0.0583 -0.12 0.4208 0.078 Uiso 1 1 calc R . .
H40B H -0.13 -0.1139 0.3532 0.078 Uiso 1 1 calc R . .
H40C H -0.1085 -0.0478 0.4305 0.078 Uiso 1 1 calc R . .
C41 C -0.0179(6) 0.0522(5) 0.3475(4) 0.0463(16) Uani 1 1 d . . .
H41A H 0.038 0.0958 0.3368 0.07 Uiso 1 1 calc R . .
H41B H -0.0515 0.08 0.381 0.07 Uiso 1 1 calc R . .
H41C H -0.0732 0.0139 0.3036 0.07 Uiso 1 1 calc R . .
C44 C 0.6097(13) 0.6364(11) 0.4716(8) 0.134(6) Uani 1 1 d . . .
H44A H 0.5647 0.6565 0.5001 0.201 Uiso 1 1 calc R . .
H44B H 0.662 0.6231 0.501 0.201 Uiso 1 1 calc R . .
H44C H 0.5635 0.5849 0.4315 0.201 Uiso 1 1 calc R . .
C45 C 0.730(3) 0.6625(11) 0.3928(9) 0.293(19) Uani 1 1 d . . .
H45A H 0.7776 0.6933 0.3683 0.44 Uiso 1 1 calc R . .
H45B H 0.6697 0.6131 0.3577 0.44 Uiso 1 1 calc R . .
H45C H 0.7709 0.6427 0.424 0.44 Uiso 1 1 calc R . .
C46 C 0.8154(9) 0.4395(7) 0.9427(7) 0.094(3) Uani 1 1 d . . .
H46A H 0.8357 0.414 0.9001 0.142 Uiso 1 1 calc R . .
H46B H 0.8279 0.4124 0.9781 0.142 Uiso 1 1 calc R . .
H46C H 0.8595 0.5009 0.9624 0.142 Uiso 1 1 calc R . .
C47 C 0.6669(10) 0.4766(9) 1.0075(7) 0.115(5) Uani 1 1 d . . .
H47A H 0.5929 0.4744 1.0053 0.172 Uiso 1 1 calc R . .
H47B H 0.7176 0.5364 1.0245 0.172 Uiso 1 1 calc R . .
H47C H 0.6855 0.4478 1.0402 0.172 Uiso 1 1 calc R . .
C48 C 0.8915(9) 0.2645(7) 0.1100(5) 0.081(3) Uani 1 1 d . . .
H48A H 0.822 0.2221 0.0784 0.122 Uiso 1 1 calc R . .
H48B H 0.887 0.2758 0.1594 0.122 Uiso 1 1 calc R . .
H48C H 0.9488 0.2424 0.1034 0.122 Uiso 1 1 calc R . .
C49 C 1.0518(9) 0.4229(8) 0.1553(7) 0.098(4) Uani 1 1 d . . .
H49A H 1.0815 0.4802 0.1517 0.147 Uiso 1 1 calc R . .
H49B H 1.1024 0.3942 0.1466 0.147 Uiso 1 1 calc R . .
H49C H 1.0411 0.4276 0.203 0.147 Uiso 1 1 calc R . .
N1 N 0.6618(4) 0.2848(3) 0.2787(2) 0.0266(10) Uani 1 1 d . . .
N2 N 0.5545(4) 0.2992(3) 0.1945(2) 0.0257(9) Uani 1 1 d . . .
O12 O 0.0653(4) -0.0069(3) 0.1881(3) 0.0443(11) Uani 1 1 d . . .
O13 O -0.2055(4) -0.1331(4) 0.2167(3) 0.0557(14) Uani 1 1 d . . .
O14 O -0.1306(4) -0.2139(5) 0.0742(3) 0.0686(18) Uani 1 1 d . . .
O15 O -0.1349(5) -0.3431(4) -0.0100(4) 0.088(2) Uani 1 1 d . . .
O16 O -0.0590(4) -0.2053(5) -0.0264(4) 0.088(2) Uani 1 1 d . . .
O1 O 0.8430(6) 0.4009(5) 0.1147(5) 0.088(2) Uani 1 1 d . . .
O23 O -0.0474(4) -0.2593(3) 0.2509(3) 0.0474(12) Uani 1 1 d . . .
O2 O 0.5950(8) 0.7156(7) 0.3787(5) 0.119(3) Uani 1 1 d . . .
O31 O 0.3199(4) -0.0461(3) 0.3515(2) 0.0432(11) Uani 1 1 d . . .
O32 O 0.2066(4) -0.2947(3) 0.2603(3) 0.0475(12) Uani 1 1 d . . .
O33 O 0.1906(5) -0.1948(4) 0.4282(3) 0.0622(16) Uani 1 1 d . . .
O34 O 0.0178(5) -0.2643(5) 0.4528(4) 0.092(2) Uani 1 1 d . . .
O35 O 0.1237(6) -0.1100(4) 0.5134(3) 0.0727(19) Uani 1 1 d . . .
O5 O 0.6140(8) 0.3301(6) 0.9051(6) 0.129(4) Uani 1 1 d . . .
O3 O -0.0108(6) 0.3579(6) 0.2935(5) 0.114(3) Uani 1 1 d . . .
O123 O 0.1506(3) -0.1485(3) 0.2005(2) 0.0327(9) Uani 1 1 d . . .
O456 O 0.0737(3) -0.0637(3) 0.3253(2) 0.0345(9) Uani 1 1 d . . .
Na1 Na 0.21862(18) 0.00174(15) 0.27343(12) 0.0313(5) Uani 1 1 d . A .
Na2 Na -0.03775(18) -0.14477(15) 0.19883(12) 0.0317(5) Uani 1 1 d . A .
Na3 Na 0.14634(19) -0.17876(16) 0.31438(12) 0.0335(5) Uani 1 1 d . A .
S1 S 0.9220(2) 0.3610(2) 0.08952(15) 0.0791(7) Uani 1 1 d . . .
S2 S 0.6846(3) 0.7223(3) 0.4371(2) 0.1094(11) Uani 1 1 d . . .
S13 S -0.32399(14) -0.18319(12) 0.17641(10) 0.0445(4) Uani 1 1 d . . .
S14 S -0.13734(12) -0.25835(10) 0.00142(8) 0.0338(3) Uani 1 1 d . . .
S23 S -0.11088(15) -0.35523(13) 0.21522(13) 0.0578(5) Uani 1 1 d . . .
S4 S 0.6756(2) 0.4237(2) 0.92000(15) 0.0828(8) Uani 1 1 d . . .
S31 S 0.39983(13) -0.00266(12) 0.42578(9) 0.0438(4) Uani 1 1 d . . .
S32 S 0.30414(18) -0.31621(15) 0.28590(11) 0.0561(5) Uani 1 1 d . . .
S33 S 0.12499(13) -0.19476(12) 0.48060(9) 0.0395(4) Uani 1 1 d . . .
S123 S 0.18960(14) -0.19461(11) 0.13999(10) 0.0439(4) Uani 1 1 d . . .
S456 S 0.04354(12) -0.00903(12) 0.38655(8) 0.0384(4) Uani 1 1 d . . .
Cl1 Cl 0.46896(16) 0.36712(11) 0.36341(10) 0.0489(4) Uani 1 1 d . . .
Cl2 Cl 0.28017(14) 0.17552(11) 0.34533(9) 0.0433(4) Uani 1 1 d . . .
Cl3 Cl 0.38860(13) 0.08559(10) 0.21693(9) 0.0403(3) Uani 1 1 d . . .
Pd01 Pd 0.42944(3) 0.22629(3) 0.29230(2) 0.02691(11) Uani 1 1 d . . .
S3 S 0.0455(2) 0.2920(2) 0.31023(19) 0.0496(12) Uani 0.564(7) 1 d P B .
C36 C -0.0701(8) 0.0131(7) 0.0902(5) 0.076(3) Uani 1 1 d . A 1
H36A H -0.1344 -0.0278 0.0965 0.114 Uiso 1 1 calc R A 1
H36B H -0.0444 -0.0167 0.0524 0.114 Uiso 1 1 calc R A 1
H36C H -0.0886 0.0578 0.0773 0.114 Uiso 1 1 calc R A 1
C37 C 0.1371(9) 0.1288(11) 0.1483(10) 0.165(9) Uani 1 1 d . A 1
H37A H 0.2004 0.1593 0.1892 0.247 Uiso 1 1 calc R A 1
H37B H 0.1123 0.1702 0.1339 0.247 Uiso 1 1 calc R A 1
H37C H 0.1569 0.0959 0.1089 0.247 Uiso 1 1 calc R A 1
S03 S 0.1001(6) 0.3729(5) 0.3238(4) 0.087(2) Uiso 0.436(7) 1 d P B 2
S12 S 0.0343(2) 0.0604(2) 0.17123(17) 0.0359(9) Uani 0.524(5) 1 d P A .
C42 C 0.0634(11) 0.3044(8) 0.3932(8) 0.111(4) Uani 1 1 d . B 1
H42A H -0.0069 0.2806 0.4033 0.166 Uiso 1 1 calc R B 1
H42B H 0.0984 0.3655 0.4208 0.166 Uiso 1 1 calc R B 1
H42C H 0.1096 0.2747 0.4062 0.166 Uiso 1 1 calc R B 1
C43 C 0.1714(14) 0.3342(13) 0.2959(14) 0.221(13) Uani 1 1 d . B 1
H43A H 0.1636 0.3281 0.2455 0.332 Uiso 1 1 calc R B 1
H43B H 0.2161 0.3036 0.3093 0.332 Uiso 1 1 calc R B 1
H43C H 0.2063 0.3949 0.3246 0.332 Uiso 1 1 calc R B 1
S012 S 0.0780(3) 0.0338(2) 0.12540(18) 0.0357(10) Uiso 0.476(5) 1 d P A 2
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-13 14 -5 0.186
1 1 -3 0.185
5 -8 6 0.126
-3 -2 7 0.149
1 -7 -3 0.127
-1 3 1 0.188
6 -1 2 0.184
-8 2 -3 0.131
-3 5 1 0.154
4 -1 9 0.172
-3 1 -5 0.187
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_3
N2 C1 N1 104.3(5) .
N2 C1 Pd01 128.2(4) .
N1 C1 Pd01 127.3(4) .
C3 C2 N2 106.8(5) .
C2 C3 N1 107.0(5) .
C5 C4 C9 123.1(5) .
C5 C4 N1 118.4(5) .
C9 C4 N1 118.2(5) .
C4 C5 C6 116.9(5) .
C4 C5 C13 122.7(5) .
C6 C5 C13 120.2(5) .
C7 C6 C5 121.8(6) .
C6 C7 C8 119.8(5) .
C6 C7 S33 119.6(5) 2_656
C8 C7 S33 120.6(4) 2_656
C9 C8 C7 121.4(5) .
C8 C9 C4 117.0(5) .
C8 C9 C10 120.5(5) .
C4 C9 C10 122.3(5) .
C11 C10 C12 109.8(7) .
C11 C10 C9 110.1(5) .
C12 C10 C9 112.5(6) .
C14 C13 C15 111.6(7) .
C14 C13 C5 110.3(6) .
C15 C13 C5 111.5(7) .
C21 C16 C17 123.2(5) .
C21 C16 N2 118.9(5) .
C17 C16 N2 117.7(5) .
C18 C17 C16 116.5(5) .
C18 C17 C22 120.4(5) .
C16 C17 C22 123.0(5) .
C19 C18 C17 121.4(5) .
C18 C19 C20 121.0(5) .
C18 C19 S14 120.1(4) 2
C20 C19 S14 118.8(4) 2
C19 C20 C21 120.8(5) .
C16 C21 C20 116.7(5) .
C16 C21 C25 122.9(5) .
C20 C21 C25 120.3(5) .
C17 C22 C23 113.4(5) .
C17 C22 C24 109.6(5) .
C23 C22 C24 110.3(6) .
C26 C25 C21 114.2(5) .
C26 C25 C27 109.9(6) .
C21 C25 C27 108.6(5) .
C1 N1 C3 111.0(4) .
C1 N1 C4 126.9(5) .
C3 N1 C4 122.1(4) .
C1 N2 C2 110.9(4) .
C1 N2 C16 125.1(4) .
C2 N2 C16 123.8(5) .
S12 O12 S012 47.0(2) .
S12 O12 Na1 131.2(3) .
S012 O12 Na1 123.1(3) .
S12 O12 Na2 133.4(3) .
S012 O12 Na2 137.0(3) .
Na1 O12 Na2 88.16(16) .
S13 O13 Na2 134.0(3) .
S14 O14 Na2 153.0(3) .
S23 O23 Na3 130.4(3) .
S23 O23 Na2 127.6(3) .
Na3 O23 Na2 88.46(17) .
S31 O31 Na1 134.4(3) .
S31 O31 Na3 126.3(3) .
Na1 O31 Na3 84.97(15) .
S32 O32 Na3 132.0(3) .
S33 O33 Na3 126.5(3) .
S03 O3 S3 49.2(4) .
S123 O123 Na1 130.6(2) .
S123 O123 Na3 125.0(2) .
Na1 O123 Na3 85.71(15) .
S123 O123 Na2 128.8(2) .
Na1 O123 Na2 85.47(15) .
Na3 O123 Na2 86.26(15) .
S456 O456 Na1 121.4(2) .
S456 O456 Na3 133.6(3) .
Na1 O456 Na3 85.57(15) .
S456 O456 Na2 128.0(2) .
Na1 O456 Na2 85.88(15) .
Na3 O456 Na2 87.15(16) .
O31 Na1 O12 156.90(19) .
O31 Na1 O123 81.93(17) .
O12 Na1 O123 79.36(16) .
O31 Na1 O456 81.58(17) .
O12 Na1 O456 81.34(17) .
O123 Na1 O456 77.81(15) .
O31 Na1 Cl2 104.46(14) .
O12 Na1 Cl2 94.32(14) .
O123 Na1 Cl2 173.59(14) .
O456 Na1 Cl2 102.43(13) .
O31 Na1 Cl3 99.09(14) .
O12 Na1 Cl3 98.69(14) .
O123 Na1 Cl3 104.79(13) .
O456 Na1 Cl3 177.37(15) .
Cl2 Na1 Cl3 74.95(7) .
O31 Na1 Na3 49.12(13) .
O12 Na1 Na3 107.82(14) .
O123 Na1 Na3 47.88(11) .
O456 Na1 Na3 47.66(11) .
Cl2 Na1 Na3 136.52(10) .
Cl3 Na1 Na3 134.49(10) .
O31 Na1 Na2 110.72(14) .
O12 Na1 Na2 46.25(12) .
O123 Na1 Na2 48.75(11) .
O456 Na1 Na2 47.94(11) .
Cl2 Na1 Na2 126.89(9) .
Cl3 Na1 Na2 133.61(9) .
Na3 Na1 Na2 61.61(7) .
O13 Na2 O14 86.6(2) .
O13 Na2 O12 103.9(2) .
O14 Na2 O12 95.7(2) .
O13 Na2 O23 96.8(2) .
O14 Na2 O23 107.1(2) .
O12 Na2 O23 149.99(18) .
O13 Na2 O456 97.03(18) .
O14 Na2 O456 174.5(2) .
O12 Na2 O456 79.38(16) .
O23 Na2 O456 76.68(17) .
O13 Na2 O123 171.24(19) .
O14 Na2 O123 102.13(18) .
O12 Na2 O123 76.56(16) .
O23 Na2 O123 79.75(16) .
O456 Na2 O123 74.38(14) .
O13 Na2 Na1 128.73(16) .
O14 Na2 Na1 128.38(18) .
O12 Na2 Na1 45.58(11) .
O23 Na2 Na1 104.42(14) .
O456 Na2 Na1 46.18(11) .
O123 Na2 Na1 45.78(11) .
O13 Na2 Na3 126.25(17) .
O14 Na2 Na3 134.16(18) .
O12 Na2 Na3 104.25(13) .
O23 Na2 Na3 45.76(12) .
O456 Na2 Na3 45.99(11) .
O123 Na2 Na3 46.14(11) .
Na1 Na2 Na3 58.71(7) .
O33 Na3 O23 112.9(2) .
O33 Na3 O32 90.21(19) .
O23 Na3 O32 95.21(19) .
O33 Na3 O456 109.73(19) .
O23 Na3 O456 77.36(16) .
O32 Na3 O456 160.06(18) .
O33 Na3 O123 165.6(2) .
O23 Na3 O123 80.96(17) .
O32 Na3 O123 84.54(16) .
O456 Na3 O123 76.08(15) .
O33 Na3 O31 89.8(2) .
O23 Na3 O31 151.22(18) .
O32 Na3 O31 102.43(19) .
O456 Na3 O31 78.42(16) .
O123 Na3 O31 78.31(16) .
O33 Na3 Na1 128.03(19) .
O23 Na3 Na1 105.42(13) .
O32 Na3 Na1 120.32(15) .
O456 Na3 Na1 46.77(11) .
O123 Na3 Na1 46.41(11) .
O31 Na3 Na1 45.91(11) .
O33 Na3 Na2 145.52(16) .
O23 Na3 Na2 45.78(12) .
O32 Na3 Na2 115.31(14) .
O456 Na3 Na2 46.85(11) .
O123 Na3 Na2 47.61(11) .
O31 Na3 Na2 105.60(13) .
Na1 Na3 Na2 59.69(7) .
O1 S1 C48 106.7(5) .
O1 S1 C49 105.9(5) .
C48 S1 C49 98.1(6) .
O2 S2 C45 98.7(9) .
O2 S2 C44 101.1(7) .
C45 S2 C44 91.3(11) .
O13 S13 C34 106.8(4) .
O13 S13 C35 108.5(4) .
C34 S13 C35 97.6(5) .
O14 S14 O16 111.4(4) .
O14 S14 O15 113.6(4) .
O16 S14 O15 113.5(5) .
O14 S14 C19 107.2(3) 2
O16 S14 C19 104.5(3) 2
O15 S14 C19 105.9(3) 2
O23 S23 C32 106.3(4) .
O23 S23 C33 104.8(4) .
C32 S23 C33 97.2(5) .
O5 S4 C46 105.8(6) .
O5 S4 C47 105.4(7) .
C46 S4 C47 97.7(6) .
O31 S31 C28 106.7(3) .
O31 S31 C29 106.3(4) .
C28 S31 C29 97.9(5) .
O32 S32 C30 105.9(4) .
O32 S32 C31 106.1(4) .
C30 S32 C31 96.6(6) .
O35 S33 O34 114.7(5) .
O35 S33 O33 112.2(4) .
O34 S33 O33 112.5(4) .
O35 S33 C7 105.8(3) 2_656
O34 S33 C7 104.9(3) 2_656
O33 S33 C7 105.9(3) 2_656
O123 S123 C38 105.4(3) .
O123 S123 C39 106.1(3) .
C38 S123 C39 96.9(4) .
O456 S456 C40 106.0(3) .
O456 S456 C41 105.3(3) .
C40 S456 C41 98.3(3) .
Pd01 Cl2 Na1 96.94(7) .
Pd01 Cl3 Na1 96.69(7) .
C1 Pd01 Cl1 88.90(16) .
C1 Pd01 Cl3 90.08(16) .
Cl1 Pd01 Cl3 177.98(7) .
C1 Pd01 Cl2 178.36(16) .
Cl1 Pd01 Cl2 89.88(6) .
Cl3 Pd01 Cl2 91.17(6) .
S03 S3 C42 91.4(6) .
S03 S3 O3 56.9(5) .
C42 S3 O3 108.2(6) .
S03 S3 C43 55.0(7) .
C42 S3 C43 107.1(10) .
O3 S3 C43 101.9(6) .
S3 S03 O3 73.9(6) .
S012 S12 O12 72.5(3) .
S012 S12 C37 58.0(7) .
O12 S12 C37 111.2(6) .
S012 S12 C36 75.2(4) .
O12 S12 C36 108.9(4) .
C37 S12 C36 101.5(6) .
S12 S012 O12 60.6(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.353(7) .
C1 N1 1.360(6) .
C1 Pd01 1.953(6) .
C2 C3 1.333(8) .
C2 N2 1.394(7) .
C3 N1 1.387(7) .
C4 C5 1.391(8) .
C4 C9 1.409(8) .
C4 N1 1.451(7) .
C5 C6 1.391(8) .
C5 C13 1.524(9) .
C6 C7 1.376(8) .
C7 C8 1.385(8) .
C7 S33 1.783(5) 2_656
C8 C9 1.383(8) .
C9 C10 1.526(9) .
C10 C11 1.513(11) .
C10 C12 1.518(10) .
C13 C14 1.517(12) .
C13 C15 1.522(11) .
C16 C21 1.395(8) .
C16 C17 1.410(8) .
C16 N2 1.450(6) .
C17 C18 1.398(7) .
C17 C22 1.518(8) .
C18 C19 1.372(8) .
C19 C20 1.374(8) .
C19 S14 1.787(5) 2
C20 C21 1.409(7) .
C21 C25 1.512(8) .
C22 C23 1.519(9) .
C22 C24 1.526(9) .
C25 C26 1.508(9) .
C25 C27 1.532(10) .
C28 S31 1.766(9) .
C29 S31 1.769(9) .
C30 S32 1.763(10) .
C31 S32 1.775(10) .
C32 S23 1.767(9) .
C33 S23 1.800(10) .
C34 S13 1.761(9) .
C35 S13 1.775(9) .
C38 S123 1.771(8) .
C39 S123 1.781(8) .
C40 S456 1.769(7) .
C41 S456 1.775(7) .
C44 S2 1.844(15) .
C45 S2 1.50(2) .
C46 S4 1.746(12) .
C47 S4 1.770(11) .
C48 S1 1.744(11) .
C49 S1 1.788(12) .
O12 S12 1.444(5) .
O12 S012 1.581(6) .
O12 Na1 2.373(5) .
O12 Na2 2.400(5) .
O13 S13 1.491(5) .
O13 Na2 2.357(5) .
O14 S14 1.416(5) .
O14 Na2 2.368(5) .
O15 S14 1.424(6) .
O16 S14 1.423(6) .
O1 S1 1.497(7) .
O23 S23 1.494(5) .
O23 Na3 2.425(5) .
O23 Na2 2.426(5) .
O2 S2 1.479(8) .
O31 S31 1.511(4) .
O31 Na1 2.370(5) .
O31 Na3 2.495(5) .
O32 S32 1.506(5) .
O32 Na3 2.428(5) .
O33 S33 1.446(5) .
O33 Na3 2.350(5) .
O34 S33 1.437(6) .
O35 S33 1.436(6) .
O5 S4 1.470(9) .
O3 S03 1.409(9) .
O3 S3 1.617(9) .
O123 S123 1.507(4) .
O123 Na1 2.388(5) .
O123 Na3 2.445(5) .
O123 Na2 2.504(5) .
O456 S456 1.514(4) .
O456 Na1 2.402(5) .
O456 Na3 2.437(5) .
O456 Na2 2.472(5) .
Na1 Cl2 2.728(3) .
Na1 Cl3 2.803(3) .
Na1 Na3 3.287(3) .
Na1 Na2 3.321(3) .
Na2 Na3 3.384(3) .
S14 C19 1.787(5) 2
S33 C7 1.783(5) 2_656
Cl1 Pd01 2.2964(18) .
Cl2 Pd01 2.3927(16) .
Cl3 Pd01 2.3180(17) .
S3 S03 1.274(8) .
S3 C42 1.568(14) .
S3 C43 1.685(13) .
C36 S12 1.751(8) .
C37 S12 1.691(11) .
S12 S012 1.212(5) .
