#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:10:15 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178711 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/22/4082228.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_4082228
loop_
_publ_author_name
'Saxena, Priya'
'Thirupathi, Natesan'
'Nethaji, Munirathinam'
_publ_contact_author             'Thirupathi N.'
_publ_section_title
;
 Insertion Reactions of Six-Membered
 CyclopalladatedN,N′,N″-Triarylguanidine,
 [Pd{κ2(C,N)-C6H3Me-3(NHC(NHAr)(═NAr))-2}(μ-Br)]2(Ar = 2-MeC6H4)
 with PhC≡C---C(O)OR (R = Me and Et): A Gateway to Second
 Orthopalladation through Novel Rearrangements
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7580
_journal_paper_doi               10.1021/om4010719
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C56 H52 F3 N3 O9 Pd S, C7 H16'
_chemical_formula_sum            'C63 H68 F3 N3 O9 Pd S'
_chemical_formula_weight         1206.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                91.194(2)
_cell_angle_beta                 99.266(3)
_cell_angle_gamma                101.578(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3175(3)
_cell_length_b                   14.3191(5)
_cell_length_c                   20.0908(6)
_cell_measurement_reflns_used    18089
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      3.03
_cell_volume                     2865.48(16)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'OLEX 2-1.2'
_computing_publication_material  'WINGX V1.80.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.3703
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Sapphire-3 CCD detector'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0864
_diffrn_reflns_av_sigmaI/netI    0.0993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37455
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9582
_exptl_absorpt_correction_T_min  0.8818
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       CUBOIDAL
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     692
_refine_ls_number_reflns         11682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0661P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                9001
_reflns_number_total             11682
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om4010719_si_002.cif
_cod_data_source_block           10a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2865.49(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082228
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
S1 S 0.25987(9) -0.03210(7) 0.74071(5) 0.0281(2) Uani 1 1 d .
O1 O -0.1441(2) 0.15746(17) 0.89032(12) 0.0241(5) Uani 1 1 d .
O2 O -0.1718(2) 0.21882(19) 0.78860(12) 0.0294(6) Uani 1 1 d .
O3 O -0.1198(2) 0.29561(17) 1.01292(12) 0.0254(6) Uani 1 1 d .
O4 O -0.0810(2) 0.37874(18) 0.92255(13) 0.0294(6) Uani 1 1 d .
O5 O 0.4250(2) 0.30499(18) 1.11908(12) 0.0272(6) Uani 1 1 d .
O6 O 0.4784(2) 0.19479(17) 1.05344(13) 0.0276(6) Uani 1 1 d .
O7 O 0.1596(2) -0.01933(17) 0.78193(12) 0.0276(6) Uani 1 1 d .
O8 O 0.2338(3) 0.0010(2) 0.67401(13) 0.0351(6) Uani 1 1 d .
O9 O 0.3950(3) -0.0090(2) 0.77470(15) 0.0492(8) Uani 1 1 d .
F1 F 0.0968(2) -0.19008(18) 0.69122(13) 0.0482(6) Uani 1 1 d .
F2 F 0.3056(3) -0.19021(19) 0.69285(14) 0.0582(7) Uani 1 1 d .
F3 F 0.2218(3) -0.20522(18) 0.78454(14) 0.0536(7) Uani 1 1 d .
N1 N 0.0646(3) 0.1629(2) 0.72606(14) 0.0215(6) Uani 1 1 d .
N2 N -0.0448(3) 0.0271(2) 0.65982(14) 0.0242(7) Uani 1 1 d .
H2 H 0.0293 0.0135 0.6495 0.029 Uiso 1 1 calc R
N3 N -0.1422(3) 0.1609(2) 0.65790(14) 0.0247(7) Uani 1 1 d .
H3 H -0.1520 0.2089 0.6834 0.030 Uiso 1 1 calc R
C1 C -0.0405(3) 0.1174(3) 0.68140(16) 0.0214(7) Uani 1 1 d .
C2 C -0.1611(3) -0.0484(3) 0.65249(18) 0.0269(8) Uani 1 1 d .
C3 C -0.2535(4) -0.0476(3) 0.6964(2) 0.0342(9) Uani 1 1 d .
H3A H -0.2405 0.0039 0.7289 0.041 Uiso 1 1 calc R
C4 C -0.3627(4) -0.1212(4) 0.6923(2) 0.0464(11) Uani 1 1 d .
H4 H -0.4264 -0.1202 0.7214 0.056 Uiso 1 1 calc R
C5 C -0.3797(5) -0.1961(4) 0.6464(2) 0.0507(13) Uani 1 1 d .
H5 H -0.4546 -0.2477 0.6441 0.061 Uiso 1 1 calc R
C6 C -0.2885(4) -0.1970(3) 0.6034(2) 0.0428(11) Uani 1 1 d .
H6 H -0.3016 -0.2496 0.5717 0.051 Uiso 1 1 calc R
C7 C -0.1768(4) -0.1223(3) 0.60529(19) 0.0322(9) Uani 1 1 d .
C8 C -0.0838(4) -0.1221(3) 0.5563(2) 0.0436(11) Uani 1 1 d .
H8A H -0.0767 -0.0628 0.5325 0.065 Uiso 1 1 calc R
H8B H -0.1182 -0.1768 0.5236 0.065 Uiso 1 1 calc R
H8C H 0.0049 -0.1268 0.5804 0.065 Uiso 1 1 calc R
C9 C -0.2356(4) 0.1375(3) 0.59625(18) 0.0289(8) Uani 1 1 d .
C10 C -0.1937(4) 0.1108(3) 0.53839(19) 0.0340(9) Uani 1 1 d .
H10 H -0.1031 0.1052 0.5400 0.041 Uiso 1 1 calc R
C11 C -0.2824(5) 0.0921(3) 0.4779(2) 0.0448(11) Uani 1 1 d .
H11 H -0.2541 0.0721 0.4382 0.054 Uiso 1 1 calc R
C12 C -0.4134(5) 0.1031(4) 0.4763(2) 0.0576(14) Uani 1 1 d .
H12 H -0.4750 0.0920 0.4349 0.069 Uiso 1 1 calc R
C13 C -0.4541(5) 0.1299(4) 0.5341(2) 0.0600(15) Uani 1 1 d .
H13 H -0.5443 0.1368 0.5318 0.072 Uiso 1 1 calc R
C14 C -0.3688(4) 0.1472(3) 0.5957(2) 0.0425(11) Uani 1 1 d .
C15 C -0.4185(5) 0.1717(4) 0.6589(2) 0.0620(15) Uani 1 1 d .
H15A H -0.5151 0.1701 0.6484 0.093 Uiso 1 1 calc R
H15B H -0.3711 0.2358 0.6768 0.093 Uiso 1 1 calc R
H15C H -0.4018 0.1252 0.6927 0.093 Uiso 1 1 calc R
C16 C 0.0931(3) 0.2636(2) 0.73370(17) 0.0215(7) Uani 1 1 d .
C17 C 0.0965(3) 0.3026(2) 0.79795(17) 0.0202(7) Uani 1 1 d .
C18 C 0.1301(3) 0.3990(2) 0.81158(18) 0.0229(8) Uani 1 1 d .
H18 H 0.1311 0.4249 0.8556 0.028 Uiso 1 1 calc R
C19 C 0.1627(4) 0.4587(3) 0.7609(2) 0.0317(9) Uani 1 1 d .
H19 H 0.1848 0.5260 0.7697 0.038 Uiso 1 1 calc R
C20 C 0.1627(4) 0.4197(3) 0.6975(2) 0.0357(9) Uani 1 1 d .
H20 H 0.1864 0.4612 0.6632 0.043 Uiso 1 1 calc R
C21 C 0.1295(4) 0.3224(3) 0.68212(19) 0.0312(9) Uani 1 1 d .
C22 C 0.1350(5) 0.2805(3) 0.6132(2) 0.0444(11) Uani 1 1 d .
H22A H 0.1744 0.2237 0.6183 0.067 Uiso 1 1 calc R
H22B H 0.1902 0.3279 0.5893 0.067 Uiso 1 1 calc R
H22C H 0.0440 0.2627 0.5872 0.067 Uiso 1 1 calc R
C23 C 0.0535(3) 0.2313(2) 0.84896(16) 0.0179(7) Uani 1 1 d .
C24 C -0.0997(3) 0.2033(2) 0.83870(17) 0.0195(7) Uani 1 1 d .
C25 C -0.2873(3) 0.1126(3) 0.8822(2) 0.0309(9) Uani 1 1 d .
H25A H -0.3351 0.1290 0.8386 0.037 Uiso 1 1 calc R
H25B H -0.3274 0.1364 0.9190 0.037 Uiso 1 1 calc R
C26 C -0.3013(4) 0.0072(3) 0.8839(2) 0.0344(9) Uani 1 1 d .
H26A H -0.2620 -0.0159 0.8471 0.052 Uiso 1 1 calc R
H26B H -0.3966 -0.0233 0.8784 0.052 Uiso 1 1 calc R
H26C H -0.2546 -0.0086 0.9273 0.052 Uiso 1 1 calc R
C27 C 0.1221(3) 0.2559(2) 0.92028(16) 0.0165(7) Uani 1 1 d .
C28 C 0.0805(3) 0.2929(2) 0.97299(17) 0.0169(7) Uani 1 1 d .
C29 C -0.0471(3) 0.3283(2) 0.96683(18) 0.0200(7) Uani 1 1 d .
C30 C -0.2503(3) 0.3235(3) 1.0099(2) 0.0296(9) Uani 1 1 d .
H30A H -0.3143 0.2722 1.0270 0.036 Uiso 1 1 calc R
H30B H -0.2875 0.3329 0.9625 0.036 Uiso 1 1 calc R
C31 C -0.2327(4) 0.4133(3) 1.0516(2) 0.0362(10) Uani 1 1 d .
H31A H -0.1928 0.4043 1.0981 0.054 Uiso 1 1 calc R
H31B H -0.3202 0.4303 1.0513 0.054 Uiso 1 1 calc R
H31C H -0.1734 0.4647 1.0329 0.054 Uiso 1 1 calc R
C32 C 0.1751(3) 0.2888(2) 1.03589(16) 0.0159(7) Uani 1 1 d .
C33 C 0.1530(3) 0.3194(2) 1.10300(17) 0.0199(7) Uani 1 1 d .
C34 C 0.1301(3) 0.4097(3) 1.11468(18) 0.0268(8) Uani 1 1 d .
H34 H 0.1286 0.4524 1.0791 0.032 Uiso 1 1 calc R
C35 C 0.1095(4) 0.4385(3) 1.1774(2) 0.0344(9) Uani 1 1 d .
H35 H 0.0962 0.5013 1.1854 0.041 Uiso 1 1 calc R
C36 C 0.1082(4) 0.3758(3) 1.2284(2) 0.0413(11) Uani 1 1 d .
H36 H 0.0923 0.3952 1.2713 0.050 Uiso 1 1 calc R
C37 C 0.1301(4) 0.2835(3) 1.21758(19) 0.0337(9) Uani 1 1 d .
H37 H 0.1294 0.2404 1.2529 0.040 Uiso 1 1 calc R
C38 C 0.1528(3) 0.2563(2) 1.15448(17) 0.0214(7) Uani 1 1 d .
H38 H 0.1683 0.1942 1.1465 0.026 Uiso 1 1 calc R
C39 C 0.2783(3) 0.2519(2) 1.01955(16) 0.0160(7) Uani 1 1 d .
C40 C 0.4033(3) 0.2454(2) 1.06444(17) 0.0178(7) Uani 1 1 d .
C41 C 0.5334(3) 0.2954(3) 1.17254(18) 0.0311(9) Uani 1 1 d .
H41A H 0.6210 0.3133 1.1570 0.037 Uiso 1 1 calc R
H41B H 0.5220 0.2286 1.1863 0.037 Uiso 1 1 calc R
C42 C 0.5278(4) 0.3612(3) 1.2307(2) 0.0380(10) Uani 1 1 d .
H42A H 0.5435 0.4273 1.2170 0.057 Uiso 1 1 calc R
H42B H 0.5971 0.3547 1.2688 0.057 Uiso 1 1 calc R
H42C H 0.4393 0.3446 1.2442 0.057 Uiso 1 1 calc R
C43 C 0.2556(3) 0.2256(2) 0.94428(16) 0.0155(7) Uani 1 1 d .
C44 C 0.3650(3) 0.2840(2) 0.90889(16) 0.0165(7) Uani 1 1 d .
C45 C 0.4176(3) 0.3795(2) 0.93155(17) 0.0199(7) Uani 1 1 d .
H45 H 0.3898 0.4046 0.9698 0.024 Uiso 1 1 calc R
C46 C 0.5085(3) 0.4374(3) 0.89946(19) 0.0261(8) Uani 1 1 d .
H46 H 0.5419 0.5022 0.9152 0.031 Uiso 1 1 calc R
C47 C 0.5516(4) 0.4016(3) 0.84406(19) 0.0298(9) Uani 1 1 d .
H47 H 0.6158 0.4410 0.8223 0.036 Uiso 1 1 calc R
C48 C 0.5005(4) 0.3087(3) 0.82129(19) 0.0298(9) Uani 1 1 d .
H48 H 0.5284 0.2839 0.7830 0.036 Uiso 1 1 calc R
C49 C 0.4082(3) 0.2502(2) 0.85372(17) 0.0205(7) Uani 1 1 d .
H49 H 0.3744 0.1857 0.8374 0.025 Uiso 1 1 calc R
C50 C 0.2327(3) 0.1169(2) 0.93051(15) 0.0148(6) Uani 1 1 d .
C51 C 0.1023(3) 0.0599(2) 0.92813(15) 0.0173(7) Uani 1 1 d .
H51 H 0.0276 0.0894 0.9279 0.021 Uiso 1 1 calc R
C52 C 0.0836(4) -0.0402(2) 0.92613(17) 0.0240(8) Uani 1 1 d .
H52 H -0.0039 -0.0779 0.9245 0.029 Uiso 1 1 calc R
C53 C 0.1893(4) -0.0836(2) 0.92653(18) 0.0268(8) Uani 1 1 d .
H53 H 0.1751 -0.1513 0.9238 0.032 Uiso 1 1 calc R
C54 C 0.3196(4) -0.0283(2) 0.93105(17) 0.0246(8) Uani 1 1 d .
H54 H 0.3937 -0.0589 0.9328 0.030 Uiso 1 1 calc R
C55 C 0.3406(3) 0.0685(2) 0.93292(17) 0.0214(7) Uani 1 1 d .
H55 H 0.4295 0.1047 0.9359 0.026 Uiso 1 1 calc R
C56 C 0.2198(4) -0.1608(3) 0.7267(2) 0.0375(10) Uani 1 1 d .
C1A C 0.0925(14) 0.6391(9) 0.5701(7) 0.198(5) Uiso 1 1 d .
C2A C -0.303(3) 0.4447(15) 0.5691(11) 0.305(9) Uiso 1 1 d .
C3A C -0.4448(16) 0.4563(12) 0.6463(9) 0.244(7) Uiso 1 1 d .
C4A C 0.191(3) 0.6117(16) 0.5273(13) 0.312(10) Uiso 1 1 d .
C5A C -0.170(2) 0.4107(16) 0.5674(12) 0.345(10) Uiso 1 1 d .
C6A C 0.306(3) 0.6010(16) 0.5318(12) 0.339(12) Uiso 1 1 d .
C7A C -0.423(4) 0.421(2) 0.5827(17) 0.481(19) Uiso 1 1 d .
Pd1 Pd 0.10586(2) 0.108529(18) 0.819290(12) 0.01654(7) Uani 1 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'
F F 0.0171 0.0103 '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_3
O9 S1 O8 116.73(18) .
O9 S1 O7 115.06(16) .
O8 S1 O7 113.25(15) .
O9 S1 C56 105.72(19) .
O8 S1 C56 103.26(18) .
O7 S1 C56 100.20(17) .
C24 O1 C25 118.1(3) .
C29 O3 C30 117.1(3) .
C40 O5 C41 116.8(3) .
S1 O7 Pd1 131.38(15) .
C1 N1 C16 120.0(3) .
C1 N1 Pd1 119.4(2) .
C16 N1 Pd1 108.9(2) .
C1 N2 C2 124.7(3) .
C1 N2 H2 117.6 .
C2 N2 H2 117.6 .
C1 N3 C9 127.2(3) .
C1 N3 H3 116.4 .
C9 N3 H3 116.4 .
N1 C1 N2 119.3(3) .
N1 C1 N3 120.8(3) .
N2 C1 N3 119.8(3) .
C7 C2 C3 121.3(4) .
C7 C2 N2 119.8(3) .
C3 C2 N2 118.8(3) .
C4 C3 C2 119.9(4) .
C4 C3 H3A 120.1 .
C2 C3 H3A 120.1 .
C5 C4 C3 120.0(4) .
C5 C4 H4 120.0 .
C3 C4 H4 120.0 .
C4 C5 C6 120.1(4) .
C4 C5 H5 120.0 .
C6 C5 H5 120.0 .
C5 C6 C7 121.7(4) .
C5 C6 H6 119.2 .
C7 C6 H6 119.2 .
C2 C7 C6 117.1(4) .
C2 C7 C8 122.0(4) .
C6 C7 C8 120.8(4) .
C7 C8 H8A 109.5 .
C7 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C7 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C10 C9 C14 121.2(4) .
C10 C9 N3 120.3(3) .
C14 C9 N3 118.4(3) .
C9 C10 C11 120.6(4) .
C9 C10 H10 119.7 .
C11 C10 H10 119.7 .
C10 C11 C12 118.8(4) .
C10 C11 H11 120.6 .
C12 C11 H11 120.6 .
C13 C12 C11 120.2(4) .
C13 C12 H12 119.9 .
C11 C12 H12 119.9 .
C12 C13 C14 122.5(4) .
C12 C13 H13 118.7 .
C14 C13 H13 118.7 .
C13 C14 C9 116.7(4) .
C13 C14 C15 121.2(4) .
C9 C14 C15 122.1(4) .
C14 C15 H15A 109.5 .
C14 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
C14 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
C17 C16 C21 120.4(3) .
C17 C16 N1 116.3(3) .
C21 C16 N1 123.0(3) .
C18 C17 C16 121.0(3) .
C18 C17 C23 123.8(3) .
C16 C17 C23 115.2(3) .
C17 C18 C19 119.6(3) .
C17 C18 H18 120.2 .
C19 C18 H18 120.2 .
C20 C19 C18 119.3(4) .
C20 C19 H19 120.3 .
C18 C19 H19 120.3 .
C19 C20 C21 122.5(4) .
C19 C20 H20 118.8 .
C21 C20 H20 118.8 .
C20 C21 C16 117.1(4) .
C20 C21 C22 121.8(3) .
C16 C21 C22 121.0(4) .
C21 C22 H22A 109.5 .
C21 C22 H22B 109.5 .
H22A C22 H22B 109.5 .
C21 C22 H22C 109.5 .
H22A C22 H22C 109.5 .
H22B C22 H22C 109.5 .
C27 C23 C17 115.6(3) .
C27 C23 C24 115.5(3) .
C17 C23 C24 109.9(3) .
C27 C23 Pd1 106.8(2) .
C17 C23 Pd1 104.8(2) .
C24 C23 Pd1 102.7(2) .
O2 C24 O1 123.9(3) .
O2 C24 C23 123.5(3) .
O1 C24 C23 112.6(3) .
O1 C25 C26 109.0(3) .
O1 C25 H25A 109.9 .
C26 C25 H25A 109.9 .
O1 C25 H25B 109.9 .
C26 C25 H25B 109.9 .
H25A C25 H25B 108.3 .
C25 C26 H26A 109.5 .
C25 C26 H26B 109.5 .
H26A C26 H26B 109.5 .
C25 C26 H26C 109.5 .
H26A C26 H26C 109.5 .
H26B C26 H26C 109.5 .
C28 C27 C23 130.8(3) .
C28 C27 C43 109.6(3) .
C23 C27 C43 119.1(3) .
C27 C28 C32 110.3(3) .
C27 C28 C29 123.1(3) .
C32 C28 C29 126.5(3) .
O4 C29 O3 124.4(3) .
O4 C29 C28 122.9(3) .
O3 C29 C28 112.7(3) .
O3 C30 C31 109.5(3) .
O3 C30 H30A 109.8 .
C31 C30 H30A 109.8 .
O3 C30 H30B 109.8 .
C31 C30 H30B 109.8 .
H30A C30 H30B 108.2 .
C30 C31 H31A 109.5 .
C30 C31 H31B 109.5 .
H31A C31 H31B 109.5 .
C30 C31 H31C 109.5 .
H31A C31 H31C 109.5 .
H31B C31 H31C 109.5 .
C39 C32 C33 128.9(3) .
C39 C32 C28 108.0(3) .
C33 C32 C28 123.2(3) .
C34 C33 C38 119.7(3) .
C34 C33 C32 120.6(3) .
C38 C33 C32 119.6(3) .
C35 C34 C33 120.7(4) .
C35 C34 H34 119.6 .
C33 C34 H34 119.6 .
C36 C35 C34 119.6(4) .
C36 C35 H35 120.2 .
C34 C35 H35 120.2 .
C35 C36 C37 120.8(4) .
C35 C36 H36 119.6 .
C37 C36 H36 119.6 .
C38 C37 C36 118.8(4) .
C38 C37 H37 120.6 .
C36 C37 H37 120.6 .
C33 C38 C37 120.3(3) .
C33 C38 H38 119.8 .
C37 C38 H38 119.8 .
C32 C39 C40 127.1(3) .
C32 C39 C43 110.6(3) .
C40 C39 C43 122.0(3) .
O6 C40 O5 123.8(3) .
O6 C40 C39 125.0(3) .
O5 C40 C39 111.1(3) .
O5 C41 C42 106.8(3) .
O5 C41 H41A 110.4 .
C42 C41 H41A 110.4 .
O5 C41 H41B 110.4 .
C42 C41 H41B 110.4 .
H41A C41 H41B 108.6 .
C41 C42 H42A 109.5 .
C41 C42 H42B 109.5 .
H42A C42 H42B 109.5 .
C41 C42 H42C 109.5 .
H42A C42 H42C 109.5 .
H42B C42 H42C 109.5 .
C39 C43 C27 101.4(2) .
C39 C43 C50 111.3(3) .
C27 C43 C50 107.7(2) .
C39 C43 C44 112.3(3) .
C27 C43 C44 109.0(2) .
C50 C43 C44 114.2(3) .
C49 C44 C45 117.7(3) .
C49 C44 C43 124.0(3) .
C45 C44 C43 118.2(3) .
C46 C45 C44 121.3(3) .
C46 C45 H45 119.4 .
C44 C45 H45 119.4 .
C45 C46 C47 120.1(3) .
C45 C46 H46 119.9 .
C47 C46 H46 119.9 .
C48 C47 C46 119.1(3) .
C48 C47 H47 120.4 .
C46 C47 H47 120.4 .
C47 C48 C49 120.7(3) .
C47 C48 H48 119.7 .
C49 C48 H48 119.7 .
C44 C49 C48 121.1(3) .
C44 C49 H49 119.4 .
C48 C49 H49 119.4 .
C51 C50 C55 117.1(3) .
C51 C50 C43 119.5(3) .
C55 C50 C43 122.3(3) .
C51 C50 Pd1 69.53(17) .
C55 C50 Pd1 111.8(2) .
C43 C50 Pd1 97.56(18) .
C52 C51 C50 120.1(3) .
C52 C51 Pd1 108.1(2) .
C50 C51 Pd1 75.37(18) .
C52 C51 H51 119.9 .
C50 C51 H51 119.9 .
Pd1 C51 H51 86.6 .
C53 C52 C51 120.8(3) .
C53 C52 H52 119.6 .
C51 C52 H52 119.6 .
C52 C53 C54 119.9(3) .
C52 C53 H53 120.0 .
C54 C53 H53 120.0 .
C55 C54 C53 120.5(3) .
C55 C54 H54 119.7 .
C53 C54 H54 119.7 .
C54 C55 C50 121.5(3) .
C54 C55 H55 119.3 .
C50 C55 H55 119.3 .
F2 C56 F1 107.9(3) .
F2 C56 F3 108.2(3) .
F1 C56 F3 106.5(4) .
F2 C56 S1 111.0(3) .
F1 C56 S1 110.8(3) .
F3 C56 S1 112.1(3) .
C7A C2A C5A 145(3) .
C6A C4A C1A 142(3) .
C6A C4A C5A 89(2) 2_566
C1A C4A C5A 130(2) 2_566
C2A C5A C4A 97.6(17) 2_566
C2A C7A C3A 117(3) .
C23 Pd1 N1 81.08(12) .
C23 Pd1 O7 176.75(11) .
N1 Pd1 O7 95.67(10) .
C23 Pd1 C51 88.07(12) .
N1 Pd1 C51 165.24(11) .
O7 Pd1 C51 95.15(10) .
C23 Pd1 C50 85.61(11) .
N1 Pd1 C50 151.72(11) .
O7 Pd1 C50 97.30(10) .
C51 Pd1 C50 35.10(11) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O9 1.421(3) .
S1 O8 1.433(3) .
S1 O7 1.461(2) .
S1 C56 1.811(4) .
O1 C24 1.333(4) .
O1 C25 1.470(4) .
O2 C24 1.204(4) .
O3 C29 1.319(4) .
O3 C30 1.472(4) .
O4 C29 1.209(4) .
O5 C40 1.337(4) .
O5 C41 1.451(4) .
O6 C40 1.204(4) .
O7 Pd1 2.170(2) .
F1 C56 1.333(5) .
F2 C56 1.325(4) .
F3 C56 1.336(5) .
N1 C1 1.336(4) .
N1 C16 1.413(4) .
N1 Pd1 2.057(3) .
N2 C1 1.345(4) .
N2 C2 1.430(5) .
N2 H2 0.8800 .
N3 C1 1.352(4) .
N3 C9 1.430(4) .
N3 H3 0.8800 .
C2 C7 1.373(5) .
C2 C3 1.400(5) .
C3 C4 1.370(6) .
C3 H3A 0.9500 .
C4 C5 1.364(7) .
C4 H4 0.9500 .
C5 C6 1.378(7) .
C5 H5 0.9500 .
C6 C7 1.401(6) .
C6 H6 0.9500 .
C7 C8 1.481(6) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.377(5) .
C9 C14 1.407(5) .
C10 C11 1.385(5) .
C10 H10 0.9500 .
C11 C12 1.387(6) .
C11 H11 0.9500 .
C12 C13 1.370(7) .
C12 H12 0.9500 .
C13 C14 1.384(6) .
C13 H13 0.9500 .
C14 C15 1.505(6) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C17 1.388(5) .
C16 C21 1.400(5) .
C17 C18 1.364(5) .
C17 C23 1.516(4) .
C18 C19 1.382(5) .
C18 H18 0.9500 .
C19 C20 1.381(6) .
C19 H19 0.9500 .
C20 C21 1.382(5) .
C20 H20 0.9500 .
C21 C22 1.512(5) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 C27 1.493(4) .
C23 C24 1.530(4) .
C23 Pd1 2.044(3) .
C25 C26 1.488(5) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 C28 1.342(4) .
C27 C43 1.533(4) .
C28 C32 1.477(4) .
C28 C29 1.492(4) .
C30 C31 1.484(5) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 C39 1.361(4) .
C32 C33 1.475(5) .
C33 C34 1.382(5) .
C33 C38 1.387(5) .
C34 C35 1.380(5) .
C34 H34 0.9500 .
C35 C36 1.375(6) .
C35 H35 0.9500 .
C36 C37 1.403(6) .
C36 H36 0.9500 .
C37 C38 1.388(5) .
C37 H37 0.9500 .
C38 H38 0.9500 .
C39 C40 1.470(4) .
C39 C43 1.520(4) .
C41 C42 1.501(5) .
C41 H41A 0.9900 .
C41 H41B 0.9900 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 C50 1.539(4) .
C43 C44 1.544(4) .
C44 C49 1.373(4) .
C44 C45 1.403(5) .
C45 C46 1.374(5) .
C45 H45 0.9500 .
C46 C47 1.388(5) .
C46 H46 0.9500 .
C47 C48 1.368(5) .
C47 H47 0.9500 .
C48 C49 1.392(5) .
C48 H48 0.9500 .
C49 H49 0.9500 .
C50 C51 1.419(4) .
C50 C55 1.420(4) .
C50 Pd1 2.388(3) .
C51 C52 1.406(5) .
C51 Pd1 2.312(3) .
C51 H51 0.9500 .
C52 C53 1.358(5) .
C52 H52 0.9500 .
C53 C54 1.405(5) .
C53 H53 0.9500 .
C54 C55 1.359(5) .
C54 H54 0.9500 .
C55 H55 0.9500 .
C1A C4A 1.53(2) .
C2A C7A 1.29(3) .
C2A C5A 1.56(2) .
C3A C7A 1.43(3) .
C4A C6A 1.22(3) .
C4A C5A 1.89(3) 2_566
C5A C4A 1.89(3) 2_566
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
O9 S1 O7 Pd1 73.6(3) .
O8 S1 O7 Pd1 -64.3(2) .
C56 S1 O7 Pd1 -173.6(2) .
C16 N1 C1 N2 160.3(3) .
Pd1 N1 C1 N2 -60.6(4) .
C16 N1 C1 N3 -19.8(5) .
Pd1 N1 C1 N3 119.2(3) .
C2 N2 C1 N1 136.4(3) .
C2 N2 C1 N3 -43.5(5) .
C9 N3 C1 N1 157.3(3) .
C9 N3 C1 N2 -22.8(5) .
C1 N2 C2 C7 151.6(3) .
C1 N2 C2 C3 -31.6(5) .
C7 C2 C3 C4 -0.5(5) .
N2 C2 C3 C4 -177.2(3) .
C2 C3 C4 C5 1.3(6) .
C3 C4 C5 C6 -1.1(7) .
C4 C5 C6 C7 0.0(6) .
C3 C2 C7 C6 -0.5(5) .
N2 C2 C7 C6 176.1(3) .
C3 C2 C7 C8 177.0(3) .
N2 C2 C7 C8 -6.4(5) .
C5 C6 C7 C2 0.8(6) .
C5 C6 C7 C8 -176.8(4) .
C1 N3 C9 C10 -38.7(6) .
C1 N3 C9 C14 144.4(4) .
C14 C9 C10 C11 -0.4(6) .
N3 C9 C10 C11 -177.2(4) .
C9 C10 C11 C12 1.6(7) .
C10 C11 C12 C13 -1.5(8) .
C11 C12 C13 C14 0.1(9) .
C12 C13 C14 C9 1.1(8) .
C12 C13 C14 C15 -176.9(5) .
C10 C9 C14 C13 -1.0(7) .
N3 C9 C14 C13 175.9(4) .
C10 C9 C14 C15 177.0(4) .
N3 C9 C14 C15 -6.1(7) .
C1 N1 C16 C17 122.1(3) .
Pd1 N1 C16 C17 -20.8(3) .
C1 N1 C16 C21 -64.2(4) .
Pd1 N1 C16 C21 152.9(3) .
C21 C16 C17 C18 2.7(5) .
N1 C16 C17 C18 176.5(3) .
C21 C16 C17 C23 179.5(3) .
N1 C16 C17 C23 -6.7(4) .
C16 C17 C18 C19 -0.7(5) .
C23 C17 C18 C19 -177.3(3) .
C17 C18 C19 C20 -1.0(5) .
C18 C19 C20 C21 0.9(6) .
C19 C20 C21 C16 1.0(6) .
C19 C20 C21 C22 -177.7(4) .
C17 C16 C21 C20 -2.7(5) .
N1 C16 C21 C20 -176.1(3) .
C17 C16 C21 C22 175.9(4) .
N1 C16 C21 C22 2.5(5) .
C18 C17 C23 C27 -35.8(4) .
C16 C17 C23 C27 147.5(3) .
C18 C17 C23 C24 97.3(4) .
C16 C17 C23 C24 -79.5(3) .
C18 C17 C23 Pd1 -153.0(3) .
C16 C17 C23 Pd1 30.3(3) .
C25 O1 C24 O2 8.1(5) .
C25 O1 C24 C23 -170.0(3) .
C27 C23 C24 O2 148.6(3) .
C17 C23 C24 O2 15.5(5) .
Pd1 C23 C24 O2 -95.6(3) .
C27 C23 C24 O1 -33.4(4) .
C17 C23 C24 O1 -166.5(3) .
Pd1 C23 C24 O1 82.4(3) .
C24 O1 C25 C26 114.7(3) .
C17 C23 C27 C28 101.5(4) .
C24 C23 C27 C28 -28.9(5) .
Pd1 C23 C27 C28 -142.4(3) .
C17 C23 C27 C43 -87.1(4) .
C24 C23 C27 C43 142.5(3) .
Pd1 C23 C27 C43 29.0(3) .
C23 C27 C28 C32 170.3(3) .
C43 C27 C28 C32 -1.8(4) .
C23 C27 C28 C29 -7.4(6) .
C43 C27 C28 C29 -179.4(3) .
C30 O3 C29 O4 -0.5(5) .
C30 O3 C29 C28 -177.8(3) .
C27 C28 C29 O4 -45.5(5) .
C32 C28 C29 O4 137.2(4) .
C27 C28 C29 O3 131.9(3) .
C32 C28 C29 O3 -45.3(4) .
C29 O3 C30 C31 -90.2(4) .
C27 C28 C32 C39 2.5(4) .
C29 C28 C32 C39 180.0(3) .
C27 C28 C32 C33 -176.7(3) .
C29 C28 C32 C33 0.8(5) .
C39 C32 C33 C34 126.7(4) .
C28 C32 C33 C34 -54.4(5) .
C39 C32 C33 C38 -54.5(5) .
C28 C32 C33 C38 124.4(3) .
C38 C33 C34 C35 1.2(5) .
C32 C33 C34 C35 180.0(3) .
C33 C34 C35 C36 -1.7(6) .
C34 C35 C36 C37 1.2(6) .
C35 C36 C37 C38 -0.1(6) .
C34 C33 C38 C37 -0.2(5) .
C32 C33 C38 C37 -179.0(3) .
C36 C37 C38 C33 -0.4(5) .
C33 C32 C39 C40 -8.8(6) .
C28 C32 C39 C40 172.1(3) .
C33 C32 C39 C43 177.0(3) .
C28 C32 C39 C43 -2.1(4) .
C41 O5 C40 O6 -10.6(5) .
C41 O5 C40 C39 170.7(3) .
C32 C39 C40 O6 162.8(3) .
C43 C39 C40 O6 -23.7(5) .
C32 C39 C40 O5 -18.5(5) .
C43 C39 C40 O5 155.0(3) .
C40 O5 C41 C42 -173.7(3) .
C32 C39 C43 C27 1.1(3) .
C40 C39 C43 C27 -173.4(3) .
C32 C39 C43 C50 -113.3(3) .
C40 C39 C43 C50 72.2(4) .
C32 C39 C43 C44 117.3(3) .
C40 C39 C43 C44 -57.2(4) .
C28 C27 C43 C39 0.5(3) .
C23 C27 C43 C39 -172.6(3) .
C28 C27 C43 C50 117.5(3) .
C23 C27 C43 C50 -55.6(4) .
C28 C27 C43 C44 -118.1(3) .
C23 C27 C43 C44 68.8(4) .
C39 C43 C44 C49 148.5(3) .
C27 C43 C44 C49 -99.9(3) .
C50 C43 C44 C49 20.6(4) .
C39 C43 C44 C45 -35.8(4) .
C27 C43 C44 C45 75.8(3) .
C50 C43 C44 C45 -163.7(3) .
C49 C44 C45 C46 0.4(5) .
C43 C44 C45 C46 -175.6(3) .
C44 C45 C46 C47 -0.9(5) .
C45 C46 C47 C48 1.2(5) .
C46 C47 C48 C49 -1.0(5) .
C45 C44 C49 C48 -0.2(5) .
C43 C44 C49 C48 175.5(3) .
C47 C48 C49 C44 0.6(5) .
C39 C43 C50 C51 83.9(3) .
C27 C43 C50 C51 -26.5(4) .
C44 C43 C50 C51 -147.7(3) .
C39 C43 C50 C55 -83.6(4) .
C27 C43 C50 C55 166.0(3) .
C44 C43 C50 C55 44.8(4) .
C39 C43 C50 Pd1 154.6(2) .
C27 C43 C50 Pd1 44.3(2) .
C44 C43 C50 Pd1 -77.0(2) .
C55 C50 C51 C52 -2.0(5) .
C43 C50 C51 C52 -170.1(3) .
Pd1 C50 C51 C52 102.7(3) .
C55 C50 C51 Pd1 -104.7(3) .
C43 C50 C51 Pd1 87.2(3) .
C50 C51 C52 C53 0.1(5) .
Pd1 C51 C52 C53 83.4(3) .
C51 C52 C53 C54 1.9(5) .
C52 C53 C54 C55 -2.1(5) .
C53 C54 C55 C50 0.1(5) .
C51 C50 C55 C54 1.9(5) .
C43 C50 C55 C54 169.7(3) .
Pd1 C50 C55 C54 -75.5(4) .
O9 S1 C56 F2 -56.3(3) .
O8 S1 C56 F2 66.8(3) .
O7 S1 C56 F2 -176.2(3) .
O9 S1 C56 F1 -176.2(3) .
O8 S1 C56 F1 -53.1(3) .
O7 S1 C56 F1 63.9(3) .
O9 S1 C56 F3 64.8(3) .
O8 S1 C56 F3 -172.1(3) .
O7 S1 C56 F3 -55.0(3) .
C7A C2A C5A C4A 105(5) 2_566
C5A C2A C7A C3A 100(5) .
C27 C23 Pd1 N1 -154.7(2) .
C17 C23 Pd1 N1 -31.5(2) .
C24 C23 Pd1 N1 83.4(2) .
C27 C23 Pd1 O7 -153.1(18) .
C17 C23 Pd1 O7 -30(2) .
C24 C23 Pd1 O7 85(2) .
C27 C23 Pd1 C51 35.4(2) .
C17 C23 Pd1 C51 158.5(2) .
C24 C23 Pd1 C51 -86.6(2) .
C27 C23 Pd1 C50 0.3(2) .
C17 C23 Pd1 C50 123.5(2) .
C24 C23 Pd1 C50 -121.7(2) .
C1 N1 Pd1 C23 -113.1(3) .
C16 N1 Pd1 C23 30.0(2) .
C1 N1 Pd1 O7 67.0(3) .
C16 N1 Pd1 O7 -149.9(2) .
C1 N1 Pd1 C51 -70.0(5) .
C16 N1 Pd1 C51 73.2(5) .
C1 N1 Pd1 C50 -176.0(2) .
C16 N1 Pd1 C50 -32.9(3) .
S1 O7 Pd1 C23 55(2) .
S1 O7 Pd1 N1 56.2(2) .
S1 O7 Pd1 C51 -133.9(2) .
S1 O7 Pd1 C50 -98.6(2) .
C52 C51 Pd1 C23 157.5(2) .
C50 C51 Pd1 C23 -85.10(19) .
C52 C51 Pd1 N1 115.0(4) .
C50 C51 Pd1 N1 -127.6(4) .
C52 C51 Pd1 O7 -22.0(2) .
C50 C51 Pd1 O7 95.38(18) .
C52 C51 Pd1 C50 -117.4(3) .
C51 C50 Pd1 C23 92.90(19) .
C55 C50 Pd1 C23 -155.1(3) .
C43 C50 Pd1 C23 -25.80(19) .
C51 C50 Pd1 N1 154.8(2) .
C55 C50 Pd1 N1 -93.2(3) .
C43 C50 Pd1 N1 36.1(3) .
C51 C50 Pd1 O7 -88.57(18) .
C55 C50 Pd1 O7 23.5(2) .
C43 C50 Pd1 O7 152.73(18) .
C55 C50 Pd1 C51 112.0(3) .
C43 C50 Pd1 C51 -118.7(3) .
