#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:05:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178801 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/55/4105581.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_4105581
loop_
_publ_author_name
'Bin Xiao'
'Tian-Jun Gong'
'Jun Xu'
'Zhao-Jing Liu'
'Lei Liu'
_publ_section_title
;
 Palladium-Catalyzed Intermolecular directed C-H Amidation of Aromatic
 Ketones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1466
_journal_page_last               1474
_journal_paper_doi               10.1021/ja108450m
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C66 H86 Cl8 F6 N8 O22 Pd2 S10'
_chemical_formula_weight         2274.43
_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                96.267(4)
_cell_angle_beta                 99.984(4)
_cell_angle_gamma                98.252(5)
_cell_formula_units_Z            1
_cell_length_a                   11.0983(6)
_cell_length_b                   13.4473(8)
_cell_length_c                   15.9684(6)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1318
_cell_measurement_theta_min      2.8379
_cell_volume                     2300.7(2)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Gemini S Ultra, Oxford Diffraction'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0929
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22170
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.7672
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         4.869
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         9389
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.1054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1474P)²+53.4245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3295
_refine_ls_wR_factor_ref         0.3411
_reflns_number_gt                6256
_reflns_number_total             9389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108450m_si_005.cif
_cod_data_source_block           100422
_cod_database_code               4105581
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
Pd1 Pd 0.45250(8) 0.53325(7) 0.41102(5) 0.0209(3) Uani 1 1 d .
S1 S 0.7150(3) 0.6375(2) 0.52329(19) 0.0262(6) Uani 1 1 d .
S2 S 0.4249(3) 0.3796(3) 0.24533(19) 0.0318(7) Uani 1 1 d .
S3 S 0.3959(3) 0.7552(2) 0.4036(2) 0.0314(7) Uani 1 1 d .
O1 O 0.7154(8) 0.7067(7) 0.4612(5) 0.0303(19) Uani 1 1 d .
O2 O 0.7771(8) 0.6777(7) 0.6095(5) 0.0303(19) Uani 1 1 d .
O4 O 0.5210(8) 0.4438(8) 0.2205(6) 0.042(2) Uani 1 1 d .
O3 O 0.4532(9) 0.3112(7) 0.3051(6) 0.038(2) Uani 1 1 d .
O5 O 0.2705(9) 0.7197(7) 0.3645(7) 0.043(2) Uani 1 1 d .
O6 O 0.4339(10) 0.7630(7) 0.4947(6) 0.042(2) Uani 1 1 d .
N1 N 0.5663(8) 0.5937(8) 0.5269(6) 0.024(2) Uani 1 1 d .
H1 H 0.5329 0.6435 0.5533 0.028 Uiso 1 1 calc R
N2 N 0.3442(9) 0.4614(8) 0.2951(6) 0.026(2) Uani 1 1 d .
H2A H 0.2734 0.4265 0.3045 0.031 Uiso 1 1 calc R
H2B H 0.3243 0.5079 0.2610 0.031 Uiso 1 1 calc R
N3 N 0.4768(9) 0.6699(8) 0.3610(6) 0.026(2) Uani 1 1 d .
H3B H 0.5580 0.6965 0.3721 0.031 Uiso 1 1 calc R
H3A H 0.4513 0.6581 0.3036 0.031 Uiso 1 1 calc R
C1 C 0.7728(10) 0.5299(9) 0.4881(7) 0.023(2) Uani 1 1 d .
C2 C 0.7505(13) 0.4966(10) 0.4034(8) 0.032(3) Uani 1 1 d U
H2 H 0.7092 0.5329 0.3645 0.039 Uiso 1 1 calc R
C3 C 0.7907(12) 0.4052(10) 0.3736(8) 0.033(3) Uani 1 1 d .
H3 H 0.7692 0.3773 0.3161 0.039 Uiso 1 1 calc R
C4 C 0.8638(12) 0.3584(10) 0.4337(9) 0.034(3) Uani 1 1 d .
C5 C 0.8903(12) 0.3991(10) 0.5190(8) 0.030(3) Uani 1 1 d U
H5 H 0.9395 0.3675 0.5576 0.036 Uiso 1 1 calc R
C6 C 0.8483(12) 0.4831(9) 0.5494(9) 0.032(3) Uani 1 1 d U
H6 H 0.8675 0.5091 0.6074 0.038 Uiso 1 1 calc R
C7 C 0.9149(14) 0.2659(11) 0.4034(10) 0.043(3) Uani 1 1 d .
H7A H 0.8877 0.2485 0.3425 0.065 Uiso 1 1 calc R
H7B H 0.8858 0.2103 0.4317 0.065 Uiso 1 1 calc R
H7C H 1.0039 0.2801 0.4169 0.065 Uiso 1 1 calc R
C8 C 0.3181(12) 0.3173(10) 0.1573(8) 0.030(3) Uani 1 1 d .
C9 C 0.2311(13) 0.2344(11) 0.1666(8) 0.038(3) Uani 1 1 d .
H9 H 0.2340 0.2114 0.2197 0.045 Uiso 1 1 calc R
C10 C 0.1411(14) 0.1866(11) 0.0971(9) 0.042(4) Uani 1 1 d .
H10 H 0.0845 0.1312 0.1036 0.050 Uiso 1 1 calc R
C11 C 0.1346(13) 0.2210(11) 0.0173(9) 0.037(3) Uani 1 1 d .
C12 C 0.2236(13) 0.3029(10) 0.0097(8) 0.034(3) Uani 1 1 d .
H12 H 0.2225 0.3251 -0.0435 0.040 Uiso 1 1 calc R
C13 C 0.3113(12) 0.3508(11) 0.0774(8) 0.033(3) Uani 1 1 d .
H13 H 0.3673 0.4064 0.0705 0.040 Uiso 1 1 calc R
C14 C 0.0359(16) 0.1716(13) -0.0575(10) 0.054(4) Uani 1 1 d .
H14A H -0.0159 0.1170 -0.0405 0.080 Uiso 1 1 calc R
H14B H 0.0736 0.1456 -0.1032 0.080 Uiso 1 1 calc R
H14C H -0.0136 0.2206 -0.0771 0.080 Uiso 1 1 calc R
C15 C 0.4527(12) 0.8667(10) 0.3677(9) 0.033(3) Uani 1 1 d .
C20 C 0.3943(16) 0.8879(12) 0.2897(11) 0.053(4) Uani 1 1 d .
H20 H 0.3231 0.8462 0.2582 0.063 Uiso 1 1 calc R
C19 C 0.4480(17) 0.9761(13) 0.2598(11) 0.055(4) Uani 1 1 d .
H19 H 0.4130 0.9911 0.2064 0.066 Uiso 1 1 calc R
C18 C 0.5489(14) 1.0392(11) 0.3072(11) 0.046(4) Uani 1 1 d .
C17 C 0.6022(16) 1.0157(11) 0.3847(11) 0.051(4) Uani 1 1 d .
H17 H 0.6721 1.0585 0.4168 0.061 Uiso 1 1 calc R
C16 C 0.5563(17) 0.9323(11) 0.4161(10) 0.050(4) Uani 1 1 d .
H16 H 0.5933 0.9186 0.4695 0.060 Uiso 1 1 calc R
C21 C 0.5987(18) 1.1330(13) 0.2719(14) 0.066(5) Uani 1 1 d .
H21A H 0.5485 1.1357 0.2171 0.099 Uiso 1 1 calc R
H21B H 0.6827 1.1307 0.2653 0.099 Uiso 1 1 calc R
H21C H 0.5967 1.1921 0.3108 0.099 Uiso 1 1 calc R
S4 S 0.9657(3) 0.4229(3) 0.18133(19) 0.0305(7) Uani 1 1 d D
N4 N 0.9969(11) 0.4183(10) 0.0869(7) 0.038(3) Uani 1 1 d D
O8 O 0.8663(8) 0.3411(7) 0.1793(6) 0.036(2) Uani 1 1 d .
O7 O 1.0820(9) 0.4273(8) 0.2388(6) 0.039(2) Uani 1 1 d U
C22 C 0.9109(12) 0.5377(10) 0.2065(8) 0.030(3) Uani 1 1 d .
C27 C 0.7843(12) 0.5397(10) 0.1907(8) 0.031(3) Uani 1 1 d .
H27 H 0.7281 0.4815 0.1660 0.037 Uiso 1 1 calc R
C26 C 0.7430(13) 0.6297(11) 0.2122(8) 0.036(3) Uani 1 1 d .
H26 H 0.6584 0.6318 0.2005 0.044 Uiso 1 1 calc R
C25 C 0.8245(14) 0.7163(11) 0.2505(9) 0.040(3) Uani 1 1 d .
C24 C 0.9509(13) 0.7129(11) 0.2652(9) 0.040(3) Uani 1 1 d .
H24 H 1.0075 0.7711 0.2894 0.048 Uiso 1 1 calc R
C23 C 0.9929(12) 0.6230(11) 0.2441(9) 0.034(3) Uani 1 1 d .
H23 H 1.0774 0.6208 0.2556 0.041 Uiso 1 1 calc R
C28 C 0.7784(16) 0.8137(11) 0.2722(11) 0.049(4) Uani 1 1 d .
H28C H 0.8474 0.8655 0.2988 0.074 Uiso 1 1 calc R
H28A H 0.7221 0.8040 0.3111 0.074 Uiso 1 1 calc R
H28B H 0.7363 0.8339 0.2207 0.074 Uiso 1 1 calc R
S5 S 0.2920(3) 0.6503(3) 0.1083(2) 0.0348(8) Uani 1 1 d .
F1 F 0.4749(9) 0.5859(8) 0.0471(7) 0.063(3) Uani 1 1 d .
F2 F 0.5090(9) 0.7441(8) 0.0965(7) 0.066(3) Uani 1 1 d .
F3 F 0.3863(10) 0.6921(9) -0.0243(7) 0.073(3) Uani 1 1 d .
O12 O 0.3493(9) 0.6224(8) 0.1902(6) 0.041(2) Uani 1 1 d .
O11 O 0.2070(9) 0.5681(8) 0.0546(6) 0.040(2) Uani 1 1 d .
O9 O 0.2504(10) 0.7459(8) 0.1134(7) 0.050(3) Uani 1 1 d .
C29 C 0.4237(14) 0.6690(13) 0.0531(10) 0.048(4) Uani 1 1 d .
Cl3 Cl 0.1129(5) -0.0086(4) 0.2492(3) 0.0659(12) Uani 1 1 d .
Cl4 Cl 0.1187(6) -0.0671(4) 0.4463(3) 0.0814(17) Uani 1 1 d .
C32 C 0.182(4) 0.067(3) 0.351(2) 0.146(13) Uani 1 1 d U
H32B H 0.2655 0.0525 0.3682 0.175 Uiso 1 1 calc R
H32A H 0.1905 0.1380 0.3431 0.175 Uiso 1 1 calc R
C33 C 0.123(3) 0.0554(15) 0.4173(16) 0.102(9) Uani 1 1 d .
H33A H 0.0391 0.0685 0.4014 0.122 Uiso 1 1 calc R
H33B H 0.1651 0.1047 0.4664 0.122 Uiso 1 1 calc R
Cl1 Cl 0.6147(6) -0.0778(4) -0.0152(6) 0.109(2) Uani 1 1 d .
Cl2 Cl 0.8414(6) 0.0530(5) 0.1436(5) 0.098(2) Uani 1 1 d .
C31 C 0.702(2) 0.0450(17) -0.0122(18) 0.093(7) Uani 1 1 d .
H31B H 0.7715 0.0374 -0.0407 0.112 Uiso 1 1 calc R
H31A H 0.6502 0.0847 -0.0452 0.112 Uiso 1 1 calc R
C30 C 0.749(3) 0.100(2) 0.0685(14) 0.104(9) Uani 1 1 d .
H30A H 0.6777 0.1143 0.0928 0.125 Uiso 1 1 calc R
H30B H 0.7933 0.1640 0.0602 0.125 Uiso 1 1 calc R
H4B H 1.061(12) 0.459(15) 0.081(7) 0.125 Uiso 1 1 d D
H4A H 0.936(7) 0.419(18) 0.046(7) 0.125 Uiso 1 1 d 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'
Cl Cl 0.1484 0.1585 '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'
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'
Pd Pd -0.9988 1.0072 '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'
H H 0.0000 0.0000 '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_1
_geom_angle_site_symmetry_3
N1 Pd1 N1 81.6(4) . 2_666
N1 Pd1 N2 175.2(4) . .
N1 Pd1 N2 94.8(4) 2_666 .
N1 Pd1 N3 93.0(4) . .
N1 Pd1 N3 174.1(4) 2_666 .
N2 Pd1 N3 90.8(4) . .
N1 Pd1 Pd1 40.9(3) . 2_666
N1 Pd1 Pd1 40.7(3) 2_666 2_666
N2 Pd1 Pd1 135.4(3) . 2_666
N3 Pd1 Pd1 133.8(3) . 2_666
O1 S1 O2 116.4(5) . .
O1 S1 N1 108.0(5) . .
O2 S1 N1 107.3(5) . .
O1 S1 C1 110.1(5) . .
O2 S1 C1 110.0(5) . .
N1 S1 C1 104.3(5) . .
O4 S2 O3 120.5(6) . .
O4 S2 C8 111.2(6) . .
O3 S2 C8 110.2(6) . .
O4 S2 N2 104.6(6) . .
O3 S2 N2 104.9(5) . .
C8 S2 N2 103.8(6) . .
O5 S3 O6 120.1(7) . .
O5 S3 N3 105.0(6) . .
O6 S3 N3 105.7(5) . .
O5 S3 C15 111.3(6) . .
O6 S3 C15 110.2(6) . .
N3 S3 C15 102.6(6) . .
S1 N1 Pd1 116.1(5) . .
S1 N1 Pd1 112.7(5) . 2_666
Pd1 N1 Pd1 98.4(4) . 2_666
S1 N1 H1 109.7 . .
Pd1 N1 H1 109.7 . .
Pd1 N1 H1 109.7 2_666 .
S2 N2 Pd1 109.7(5) . .
S2 N2 H2A 109.7 . .
Pd1 N2 H2A 109.7 . .
S2 N2 H2B 109.7 . .
Pd1 N2 H2B 109.7 . .
H2A N2 H2B 108.2 . .
S3 N3 Pd1 111.7(5) . .
S3 N3 H3B 109.3 . .
Pd1 N3 H3B 109.3 . .
S3 N3 H3A 109.3 . .
Pd1 N3 H3A 109.3 . .
H3B N3 H3A 107.9 . .
C2 C1 C6 122.1(12) . .
C2 C1 S1 118.6(10) . .
C6 C1 S1 119.2(9) . .
C1 C2 C3 119.5(12) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C4 C3 C2 118.3(12) . .
C4 C3 H3 120.9 . .
C2 C3 H3 120.9 . .
C5 C4 C3 119.7(12) . .
C5 C4 C7 120.7(13) . .
C3 C4 C7 119.6(13) . .
C6 C5 C4 123.1(13) . .
C6 C5 H5 118.4 . .
C4 C5 H5 118.4 . .
C5 C6 C1 117.0(12) . .
C5 C6 H6 121.5 . .
C1 C6 H6 121.5 . .
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C13 C8 C9 118.8(12) . .
C13 C8 S2 121.3(10) . .
C9 C8 S2 119.8(10) . .
C10 C9 C8 120.3(12) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
C9 C10 C11 120.5(12) . .
C9 C10 H10 119.8 . .
C11 C10 H10 119.8 . .
C10 C11 C12 117.9(12) . .
C10 C11 C14 120.9(13) . .
C12 C11 C14 121.3(13) . .
C13 C12 C11 122.2(12) . .
C13 C12 H12 118.9 . .
C11 C12 H12 118.9 . .
C12 C13 C8 120.3(12) . .
C12 C13 H13 119.8 . .
C8 C13 H13 119.8 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C20 C15 C16 121.0(13) . .
C20 C15 S3 118.4(11) . .
C16 C15 S3 120.6(11) . .
C15 C20 C19 116.8(14) . .
C15 C20 H20 121.6 . .
C19 C20 H20 121.6 . .
C18 C19 C20 121.7(15) . .
C18 C19 H19 119.1 . .
C20 C19 H19 119.1 . .
C19 C18 C17 119.1(15) . .
C19 C18 C21 118.6(17) . .
C17 C18 C21 122.3(16) . .
C16 C17 C18 121.9(15) . .
C16 C17 H17 119.1 . .
C18 C17 H17 119.1 . .
C17 C16 C15 119.4(15) . .
C17 C16 H16 120.3 . .
C15 C16 H16 120.3 . .
C18 C21 H21A 109.5 . .
C18 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C18 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
O8 S4 O7 119.4(6) . .
O8 S4 N4 107.4(6) . .
O7 S4 N4 106.0(6) . .
O8 S4 C22 107.5(6) . .
O7 S4 C22 107.3(6) . .
N4 S4 C22 108.9(6) . .
S4 N4 H4B 117(9) . .
S4 N4 H4A 117(9) . .
H4B N4 H4A 110(7) . .
C23 C22 C27 120.3(12) . .
C23 C22 S4 119.9(10) . .
C27 C22 S4 119.8(10) . .
C26 C27 C22 119.0(13) . .
C26 C27 H27 120.5 . .
C22 C27 H27 120.5 . .
C25 C26 C27 121.5(13) . .
C25 C26 H26 119.3 . .
C27 C26 H26 119.3 . .
C26 C25 C24 118.6(13) . .
C26 C25 C28 120.8(14) . .
C24 C25 C28 120.5(14) . .
C23 C24 C25 120.2(13) . .
C23 C24 H24 119.9 . .
C25 C24 H24 119.9 . .
C22 C23 C24 120.4(12) . .
C22 C23 H23 119.8 . .
C24 C23 H23 119.8 . .
C25 C28 H28C 109.5 . .
C25 C28 H28A 109.5 . .
H28C C28 H28A 109.5 . .
C25 C28 H28B 109.5 . .
H28C C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
O9 S5 O11 115.4(6) . .
O9 S5 O12 115.5(6) . .
O11 S5 O12 113.1(6) . .
O9 S5 C29 104.3(7) . .
O11 S5 C29 104.1(7) . .
O12 S5 C29 102.2(6) . .
F3 C29 F2 108.5(13) . .
F3 C29 F1 109.6(15) . .
F2 C29 F1 108.1(13) . .
F3 C29 S5 110.0(11) . .
F2 C29 S5 110.0(12) . .
F1 C29 S5 110.6(10) . .
C33 C32 Cl3 117(3) . .
C33 C32 H32B 107.9 . .
Cl3 C32 H32B 107.9 . .
C33 C32 H32A 107.9 . .
Cl3 C32 H32A 107.9 . .
H32B C32 H32A 107.2 . .
C32 C33 Cl4 112(2) . .
C32 C33 H33A 109.2 . .
Cl4 C33 H33A 109.2 . .
C32 C33 H33B 109.2 . .
Cl4 C33 H33B 109.2 . .
H33A C33 H33B 107.9 . .
C30 C31 Cl1 116(2) . .
C30 C31 H31B 108.3 . .
Cl1 C31 H31B 108.3 . .
C30 C31 H31A 108.3 . .
Cl1 C31 H31A 108.3 . .
H31B C31 H31A 107.4 . .
C31 C30 Cl2 121(2) . .
C31 C30 H30A 107.0 . .
Cl2 C30 H30A 107.0 . .
C31 C30 H30B 107.0 . .
Cl2 C30 H30B 107.0 . .
H30A C30 H30B 106.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.061(9) .
Pd1 N1 2.069(10) 2_666
Pd1 N2 2.076(10) .
Pd1 N3 2.083(10) .
Pd1 Pd1 3.1262(17) 2_666
S1 O1 1.432(9) .
S1 O2 1.437(8) .
S1 N1 1.684(10) .
S1 C1 1.742(13) .
S2 O4 1.414(10) .
S2 O3 1.424(10) .
S2 C8 1.722(13) .
S2 N2 1.727(10) .
S3 O5 1.413(10) .
S3 O6 1.430(10) .
S3 N3 1.710(10) .
S3 C15 1.738(13) .
N1 Pd1 2.069(10) 2_666
N1 H1 0.9100 .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
N3 H3B 0.9000 .
N3 H3A 0.9000 .
C1 C2 1.346(16) .
C1 C6 1.435(18) .
C2 C3 1.428(18) .
C2 H2 0.9300 .
C3 C4 1.408(19) .
C3 H3 0.9300 .
C4 C5 1.376(19) .
C4 C7 1.506(18) .
C5 C6 1.356(18) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C13 1.392(17) .
C8 C9 1.405(18) .
C9 C10 1.385(19) .
C9 H9 0.9300 .
C10 C11 1.396(19) .
C10 H10 0.9300 .
C11 C12 1.400(19) .
C11 C14 1.495(19) .
C12 C13 1.354(18) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C20 1.38(2) .
C15 C16 1.40(2) .
C20 C19 1.42(2) .
C20 H20 0.9300 .
C19 C18 1.36(2) .
C19 H19 0.9300 .
C18 C17 1.37(2) .
C18 C21 1.51(2) .
C17 C16 1.35(2) .
C17 H17 0.9300 .
C16 H16 0.9300 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
S4 O8 1.436(10) .
S4 O7 1.438(10) .
S4 N4 1.602(11) .
S4 C22 1.770(14) .
N4 H4B 0.86(4) .
N4 H4A 0.86(4) .
C22 C23 1.366(19) .
C22 C27 1.388(17) .
C27 C26 1.384(19) .
C27 H27 0.9300 .
C26 C25 1.38(2) .
C26 H26 0.9300 .
C25 C24 1.39(2) .
C25 C28 1.50(2) .
C24 C23 1.39(2) .
C24 H24 0.9300 .
C23 H23 0.9300 .
C28 H28C 0.9600 .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
S5 O9 1.426(11) .
S5 O11 1.436(10) .
S5 O12 1.463(9) .
S5 C29 1.834(15) .
F1 C29 1.327(19) .
F2 C29 1.320(19) .
F3 C29 1.319(17) .
Cl3 C32 1.81(4) .
Cl4 C33 1.76(2) .
C32 C33 1.34(4) .
C32 H32B 0.9700 .
C32 H32A 0.9700 .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
Cl1 C31 1.78(2) .
Cl2 C30 1.68(3) .
C31 C30 1.39(3) .
C31 H31B 0.9700 .
C31 H31A 0.9700 .
C30 H30A 0.9700 .
C30 H30B 0.9700 .
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_1
_geom_torsion_site_symmetry_4
O1 S1 N1 Pd1 52.7(7) . .
O2 S1 N1 Pd1 178.9(5) . .
C1 S1 N1 Pd1 -64.4(7) . .
O1 S1 N1 Pd1 165.1(5) . 2_666
O2 S1 N1 Pd1 -68.7(6) . 2_666
C1 S1 N1 Pd1 48.0(6) . 2_666
N1 Pd1 N1 S1 120.4(7) 2_666 .
N2 Pd1 N1 S1 80(5) . .
N3 Pd1 N1 S1 -61.8(6) . .
Pd1 Pd1 N1 S1 120.4(7) 2_666 .
N1 Pd1 N1 Pd1 0.0 2_666 2_666
N2 Pd1 N1 Pd1 -41(5) . 2_666
N3 Pd1 N1 Pd1 177.8(4) . 2_666
O4 S2 N2 Pd1 -69.4(6) . .
O3 S2 N2 Pd1 58.3(6) . .
C8 S2 N2 Pd1 174.0(6) . .
N1 Pd1 N2 S2 -33(5) . .
N1 Pd1 N2 S2 -73.0(5) 2_666 .
N3 Pd1 N2 S2 108.9(5) . .
Pd1 Pd1 N2 S2 -70.1(6) 2_666 .
O5 S3 N3 Pd1 -73.9(6) . .
O6 S3 N3 Pd1 54.1(7) . .
C15 S3 N3 Pd1 169.6(6) . .
N1 Pd1 N3 S3 -74.6(5) . .
N1 Pd1 N3 S3 -53(4) 2_666 .
N2 Pd1 N3 S3 108.4(5) . .
Pd1 Pd1 N3 S3 -72.6(6) 2_666 .
O1 S1 C1 C2 -33.6(12) . .
O2 S1 C1 C2 -163.2(10) . .
N1 S1 C1 C2 82.1(11) . .
O1 S1 C1 C6 142.9(9) . .
O2 S1 C1 C6 13.4(11) . .
N1 S1 C1 C6 -101.4(9) . .
C6 C1 C2 C3 7.3(19) . .
S1 C1 C2 C3 -176.3(10) . .
C1 C2 C3 C4 -6.3(19) . .
C2 C3 C4 C5 2.4(18) . .
C2 C3 C4 C7 -175.8(12) . .
C3 C4 C5 C6 0.7(19) . .
C7 C4 C5 C6 179.0(12) . .
C4 C5 C6 C1 0.0(18) . .
C2 C1 C6 C5 -4.1(18) . .
S1 C1 C6 C5 179.5(9) . .
O4 S2 C8 C13 -17.4(13) . .
O3 S2 C8 C13 -153.6(11) . .
N2 S2 C8 C13 94.5(12) . .
O4 S2 C8 C9 166.2(11) . .
O3 S2 C8 C9 30.0(13) . .
N2 S2 C8 C9 -81.9(12) . .
C13 C8 C9 C10 1(2) . .
S2 C8 C9 C10 177.0(12) . .
C8 C9 C10 C11 -1(2) . .
C9 C10 C11 C12 2(2) . .
C9 C10 C11 C14 -178.5(14) . .
C10 C11 C12 C13 -2(2) . .
C14 C11 C12 C13 177.8(14) . .
C11 C12 C13 C8 2(2) . .
C9 C8 C13 C12 -1(2) . .
S2 C8 C13 C12 -177.6(11) . .
O5 S3 C15 C20 -22.5(15) . .
O6 S3 C15 C20 -158.4(12) . .
N3 S3 C15 C20 89.3(13) . .
O5 S3 C15 C16 158.5(12) . .
O6 S3 C15 C16 22.7(14) . .
N3 S3 C15 C16 -89.6(13) . .
C16 C15 C20 C19 3(2) . .
S3 C15 C20 C19 -176.0(13) . .
C15 C20 C19 C18 -3(3) . .
C20 C19 C18 C17 2(3) . .
C20 C19 C18 C21 -178.5(16) . .
C19 C18 C17 C16 -1(3) . .
C21 C18 C17 C16 179.4(16) . .
C18 C17 C16 C15 1(3) . .
C20 C15 C16 C17 -2(2) . .
S3 C15 C16 C17 176.7(13) . .
O8 S4 C22 C23 155.1(10) . .
O7 S4 C22 C23 25.5(12) . .
N4 S4 C22 C23 -88.8(11) . .
O8 S4 C22 C27 -22.6(11) . .
O7 S4 C22 C27 -152.1(10) . .
N4 S4 C22 C27 93.5(11) . .
C23 C22 C27 C26 1.2(18) . .
S4 C22 C27 C26 178.8(9) . .
C22 C27 C26 C25 -1.5(19) . .
C27 C26 C25 C24 2(2) . .
C27 C26 C25 C28 179.1(12) . .
C26 C25 C24 C23 -2(2) . .
C28 C25 C24 C23 -179.2(13) . .
C27 C22 C23 C24 -1.4(19) . .
S4 C22 C23 C24 -179.0(10) . .
C25 C24 C23 C22 2(2) . .
O9 S5 C29 F3 -61.2(14) . .
O11 S5 C29 F3 60.2(14) . .
O12 S5 C29 F3 178.1(12) . .
O9 S5 C29 F2 58.2(12) . .
O11 S5 C29 F2 179.6(10) . .
O12 S5 C29 F2 -62.5(12) . .
O9 S5 C29 F1 177.5(11) . .
O11 S5 C29 F1 -61.0(12) . .
O12 S5 C29 F1 56.9(12) . .
Cl3 C32 C33 Cl4 64(4) . .
Cl1 C31 C30 Cl2 57(3) . .
