#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:21:20 +0100 (vie 25 de mar de 2016) $
#$Revision: 179748 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/44/7004403.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_7004403
loop_
_publ_author_name
'Chitanda, Jackson M.'
'Prokopchuk, Demyan E.'
'Quail, J. Wilson'
'Foley, Stephen R.'
_publ_section_title
;
 Synthesis of palladacycles employing iminoisoindolines as monoanionic
 bidentate ligands
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              6023
_journal_page_last               6029
_journal_paper_doi               10.1039/b806544f
_journal_year                    2008
_chemical_formula_moiety         'C48 H44 N4 O4 Pd2, C H Cl3'
_chemical_formula_sum            'C49 H45 Cl3 N4 O4 Pd2'
_chemical_formula_weight         1073.04
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.026(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.1864(3)
_cell_length_b                   9.6437(1)
_cell_length_c                   20.2415(2)
_cell_measurement_reflns_used    11780
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.700
_cell_measurement_theta_min      0.998
_cell_volume                     4371.30(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1998)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON. (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            77979
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Shelxtl 6.10 (Bruker-AXS, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         11273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0279P)²+7.6740P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                8852
_reflns_number_total             11273
_reflns_threshold_expression     >/2(I)
_cod_data_source_file            b806544f.txt
_cod_data_source_block           1176
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7004403
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Pd1 Pd 0.196278(10) 0.15406(2) 0.136423(11) 0.02188(6) Uani 1 1 d . . .
Pd2 Pd 0.235276(10) 0.38922(2) 0.060686(11) 0.02093(6) Uani 1 1 d . . .
O1 O 0.11961(10) 0.1999(3) 0.05960(11) 0.0334(5) Uani 1 1 d . . .
O2 O 0.15667(10) 0.3213(2) -0.01380(11) 0.0308(5) Uani 1 1 d . . .
O3 O 0.22669(10) 0.0614(2) 0.05436(11) 0.0286(5) Uani 1 1 d . . .
O4 O 0.27823(10) 0.2314(2) 0.02235(11) 0.0306(5) Uani 1 1 d . . .
N1 N 0.22437(12) 0.1098(3) 0.30495(13) 0.0262(5) Uani 1 1 d . . .
N2 N 0.26318(11) 0.0722(3) 0.21036(12) 0.0234(5) Uani 1 1 d . . .
N31 N 0.25010(11) 0.5499(3) 0.20299(12) 0.0217(5) Uani 1 1 d . . .
N32 N 0.19601(11) 0.5581(3) 0.08826(12) 0.0215(5) Uani 1 1 d . . .
C1 C 0.26419(13) 0.0516(3) 0.27420(15) 0.0226(6) Uani 1 1 d . . .
C2 C 0.30432(14) -0.0391(3) 0.32602(15) 0.0256(6) Uani 1 1 d . . .
C3 C 0.35319(14) -0.1234(3) 0.32415(16) 0.0290(7) Uani 1 1 d . . .
H3 H 0.3679 -0.1274 0.2846 0.035 Uiso 1 1 calc R . .
C4 C 0.37938(15) -0.2011(4) 0.38214(17) 0.0326(7) Uani 1 1 d . . .
H4 H 0.4125 -0.2588 0.3818 0.039 Uiso 1 1 calc R . .
C5 C 0.35854(16) -0.1966(4) 0.44018(18) 0.0372(8) Uani 1 1 d . . .
H5 H 0.3767 -0.2527 0.4785 0.045 Uiso 1 1 calc R . .
C6 C 0.31104(16) -0.1105(4) 0.44283(17) 0.0370(8) Uani 1 1 d . . .
H6 H 0.2970 -0.1052 0.4829 0.044 Uiso 1 1 calc R . .
C7 C 0.28495(14) -0.0330(3) 0.38559(16) 0.0281(7) Uani 1 1 d . . .
C8 C 0.23457(15) 0.0668(4) 0.37685(15) 0.0305(7) Uani 1 1 d . . .
H8A H 0.1987 0.0215 0.3850 0.037 Uiso 1 1 calc R . .
H8B H 0.2457 0.1469 0.4082 0.037 Uiso 1 1 calc R . .
C9 C 0.17986(14) 0.2088(3) 0.27625(15) 0.0260(6) Uani 1 1 d . . .
C10 C 0.16303(13) 0.2406(3) 0.20662(15) 0.0245(6) Uani 1 1 d . . .
C11 C 0.11864(14) 0.3408(3) 0.18518(16) 0.0256(6) Uani 1 1 d . . .
H11 H 0.1075 0.3649 0.1381 0.031 Uiso 1 1 calc R . .
C12 C 0.08969(15) 0.4076(3) 0.22859(17) 0.0303(7) Uani 1 1 d . . .
C13 C 0.10772(18) 0.3731(4) 0.29694(19) 0.0411(9) Uani 1 1 d . . .
H13 H 0.0894 0.4176 0.3281 0.049 Uiso 1 1 calc R . .
C14 C 0.15168(17) 0.2754(4) 0.32132(18) 0.0386(8) Uani 1 1 d . . .
H14 H 0.1629 0.2531 0.3686 0.046 Uiso 1 1 calc R . .
C15 C 0.31101(13) 0.0119(3) 0.18619(15) 0.0224(6) Uani 1 1 d . . .
C16 C 0.36357(14) 0.0843(3) 0.19261(16) 0.0264(6) Uani 1 1 d . . .
H16 H 0.3677 0.1757 0.2107 0.032 Uiso 1 1 calc R . .
C17 C 0.41016(14) 0.0222(3) 0.17243(17) 0.0293(7) Uani 1 1 d . . .
H17 H 0.4462 0.0725 0.1766 0.035 Uiso 1 1 calc R . .
C18 C 0.40550(14) -0.1123(4) 0.14612(16) 0.0286(7) Uani 1 1 d . . .
C19 C 0.35144(15) -0.1806(3) 0.13814(16) 0.0287(7) Uani 1 1 d . . .
H19 H 0.3467 -0.2711 0.1190 0.034 Uiso 1 1 calc R . .
C20 C 0.30441(14) -0.1200(3) 0.15740(16) 0.0264(6) Uani 1 1 d . . .
H20 H 0.2676 -0.1682 0.1510 0.032 Uiso 1 1 calc R . .
C21 C 0.04056(16) 0.5104(4) 0.2017(2) 0.0389(8) Uani 1 1 d . . .
H21A H 0.0019 0.4673 0.1999 0.058 Uiso 1 1 calc R . .
H21B H 0.0415 0.5399 0.1557 0.058 Uiso 1 1 calc R . .
H21C H 0.0462 0.5913 0.2320 0.058 Uiso 1 1 calc R . .
C22 C 0.45762(16) -0.1821(4) 0.1282(2) 0.0401(9) Uani 1 1 d . . .
H22A H 0.4855 -0.2166 0.1700 0.060 Uiso 1 1 calc R . .
H22B H 0.4781 -0.1153 0.1057 0.060 Uiso 1 1 calc R . .
H22C H 0.4431 -0.2599 0.0972 0.060 Uiso 1 1 calc R . .
C31 C 0.20400(13) 0.5992(3) 0.15105(15) 0.0218(6) Uani 1 1 d . . .
C32 C 0.16868(13) 0.6958(3) 0.18207(16) 0.0240(6) Uani 1 1 d . . .
C33 C 0.12339(15) 0.7904(4) 0.15401(18) 0.0325(7) Uani 1 1 d . . .
H33 H 0.1089 0.8006 0.1059 0.039 Uiso 1 1 calc R . .
C34 C 0.10004(16) 0.8694(4) 0.1984(2) 0.0392(8) Uani 1 1 d . . .
H34 H 0.0699 0.9360 0.1804 0.047 Uiso 1 1 calc R . .
C35 C 0.12024(16) 0.8523(4) 0.2687(2) 0.0432(9) Uani 1 1 d . . .
H35 H 0.1026 0.9048 0.2980 0.052 Uiso 1 1 calc R . .
C36 C 0.16565(15) 0.7602(4) 0.29684(18) 0.0351(8) Uani 1 1 d . . .
H36 H 0.1795 0.7491 0.3450 0.042 Uiso 1 1 calc R . .
C37 C 0.19027(14) 0.6846(3) 0.25278(17) 0.0275(7) Uani 1 1 d . . .
C38 C 0.24255(14) 0.5878(3) 0.27040(16) 0.0279(7) Uani 1 1 d . . .
H38A H 0.2786 0.6347 0.2985 0.033 Uiso 1 1 calc R . .
H38B H 0.2338 0.5053 0.2953 0.033 Uiso 1 1 calc R . .
C39 C 0.30475(13) 0.5007(3) 0.19264(15) 0.0210(6) Uani 1 1 d . . .
C40 C 0.30764(13) 0.4416(3) 0.13021(15) 0.0219(6) Uani 1 1 d . . .
C41 C 0.36444(14) 0.4117(3) 0.12141(16) 0.0267(6) Uani 1 1 d . . .
H41 H 0.3670 0.3744 0.0789 0.032 Uiso 1 1 calc R . .
C42 C 0.41707(13) 0.4341(3) 0.17189(17) 0.0280(7) Uani 1 1 d . . .
C43 C 0.41203(14) 0.4883(3) 0.23390(17) 0.0297(7) Uani 1 1 d . . .
H43 H 0.4471 0.5031 0.2697 0.036 Uiso 1 1 calc R . .
C44 C 0.35716(14) 0.5208(3) 0.24434(16) 0.0266(6) Uani 1 1 d . . .
H44 H 0.3550 0.5574 0.2872 0.032 Uiso 1 1 calc R . .
C45 C 0.15181(13) 0.6292(3) 0.03597(15) 0.0225(6) Uani 1 1 d . . .
C46 C 0.09371(13) 0.5787(3) 0.01444(16) 0.0273(7) Uani 1 1 d . . .
H46 H 0.0830 0.4956 0.0335 0.033 Uiso 1 1 calc R . .
C47 C 0.05176(14) 0.6496(4) -0.03461(17) 0.0303(7) Uani 1 1 d . . .
H47 H 0.0123 0.6138 -0.0491 0.036 Uiso 1 1 calc R . .
C48 C 0.06540(14) 0.7718(4) -0.06348(17) 0.0313(7) Uani 1 1 d . . .
C49 C 0.12377(14) 0.8212(4) -0.04112(18) 0.0324(7) Uani 1 1 d . . .
H49 H 0.1343 0.9053 -0.0596 0.039 Uiso 1 1 calc R . .
C50 C 0.16698(14) 0.7498(3) 0.00769(16) 0.0282(7) Uani 1 1 d . . .
H50 H 0.2067 0.7840 0.0215 0.034 Uiso 1 1 calc R . .
C51 C 0.47727(15) 0.3995(4) 0.1605(2) 0.0394(8) Uani 1 1 d . . .
H51A H 0.4724 0.3292 0.1245 0.059 Uiso 1 1 calc R . .
H51B H 0.5035 0.3635 0.2030 0.059 Uiso 1 1 calc R . .
H51C H 0.4950 0.4833 0.1466 0.059 Uiso 1 1 calc R . .
C52 C 0.01818(17) 0.8475(4) -0.1161(2) 0.0492(11) Uani 1 1 d . . .
H52A H 0.0118 0.8006 -0.1604 0.074 Uiso 1 1 calc R . .
H52B H 0.0312 0.9431 -0.1203 0.074 Uiso 1 1 calc R . .
H52C H -0.0192 0.8482 -0.1021 0.074 Uiso 1 1 calc R . .
C61 C 0.11686(15) 0.2520(4) 0.00205(16) 0.0306(7) Uani 1 1 d . . .
C62 C 0.05866(16) 0.2320(5) -0.05193(19) 0.0451(10) Uani 1 1 d . . .
H62A H 0.0293 0.2995 -0.0448 0.068 Uiso 1 1 calc R . .
H62B H 0.0437 0.1379 -0.0486 0.068 Uiso 1 1 calc R . .
H62C H 0.0653 0.2455 -0.0974 0.068 Uiso 1 1 calc R . .
C63 C 0.25859(14) 0.1093(3) 0.02021(16) 0.0280(7) Uani 1 1 d . . .
C64 C 0.27751(19) 0.0122(4) -0.0296(2) 0.0452(9) Uani 1 1 d . . .
H64A H 0.2475 -0.0608 -0.0440 0.068 Uiso 1 1 calc R . .
H64B H 0.3161 -0.0299 -0.0072 0.068 Uiso 1 1 calc R . .
H64C H 0.2812 0.0648 -0.0698 0.068 Uiso 1 1 calc R . .
Cl1 Cl 0.37055(5) 0.30044(12) 0.36929(5) 0.0539(3) Uani 1 1 d . . .
Cl2 Cl 0.43874(6) 0.39457(13) 0.50153(7) 0.0658(3) Uani 1 1 d . . .
Cl3 Cl 0.44435(5) 0.10954(11) 0.46294(6) 0.0559(3) Uani 1 1 d . . .
C65 C 0.39860(17) 0.2560(4) 0.45533(18) 0.0378(8) Uani 1 1 d . . .
H65 H 0.3643 0.2337 0.4749 0.045 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
C10 Pd1 N2 90.00(11) . . ?
C10 Pd1 O1 91.77(11) . . ?
N2 Pd1 O1 168.66(10) . . ?
C10 Pd1 O3 175.96(11) . . ?
N2 Pd1 O3 93.85(9) . . ?
O1 Pd1 O3 84.22(9) . . ?
C10 Pd1 Pd2 105.92(9) . . ?
N2 Pd1 Pd2 113.50(7) . . ?
O1 Pd1 Pd2 76.74(7) . . ?
O3 Pd1 Pd2 73.65(6) . . ?
C40 Pd2 N32 87.52(11) . . ?
C40 Pd2 O4 93.05(11) . . ?
N32 Pd2 O4 172.48(10) . . ?
C40 Pd2 O2 177.13(11) . . ?
N32 Pd2 O2 94.54(9) . . ?
O4 Pd2 O2 85.17(9) . . ?
C40 Pd2 Pd1 98.24(9) . . ?
N32 Pd2 Pd1 104.57(7) . . ?
O4 Pd2 Pd1 82.78(6) . . ?
O2 Pd2 Pd1 79.33(6) . . ?
C61 O1 Pd1 127.3(2) . . ?
C61 O2 Pd2 122.3(2) . . ?
C63 O3 Pd1 130.0(2) . . ?
C63 O4 Pd2 119.6(2) . . ?
C1 N1 C9 126.8(3) . . ?
C1 N1 C8 112.5(3) . . ?
C9 N1 C8 120.6(2) . . ?
C1 N2 C15 117.2(3) . . ?
C1 N2 Pd1 127.5(2) . . ?
C15 N2 Pd1 114.62(18) . . ?
C31 N31 C39 123.3(2) . . ?
C31 N31 C38 111.6(2) . . ?
C39 N31 C38 123.2(2) . . ?
C31 N32 C45 117.9(2) . . ?
C31 N32 Pd2 123.9(2) . . ?
C45 N32 Pd2 117.87(18) . . ?
N2 C1 N1 123.5(3) . . ?
N2 C1 C2 129.4(3) . . ?
N1 C1 C2 107.1(2) . . ?
C7 C2 C3 119.4(3) . . ?
C7 C2 C1 107.6(3) . . ?
C3 C2 C1 133.0(3) . . ?
C4 C3 C2 117.9(3) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
C5 C4 C3 121.8(3) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 118.0(3) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
C6 C7 C2 122.3(3) . . ?
C6 C7 C8 127.6(3) . . ?
C2 C7 C8 110.1(3) . . ?
N1 C8 C7 102.7(2) . . ?
N1 C8 H8A 111.2 . . ?
C7 C8 H8A 111.2 . . ?
N1 C8 H8B 111.2 . . ?
C7 C8 H8B 111.2 . . ?
H8A C8 H8B 109.1 . . ?
C10 C9 C14 120.0(3) . . ?
C10 C9 N1 123.1(3) . . ?
C14 C9 N1 117.0(3) . . ?
C9 C10 C11 117.1(3) . . ?
C9 C10 Pd1 125.2(2) . . ?
C11 C10 Pd1 117.6(2) . . ?
C12 C11 C10 124.1(3) . . ?
C12 C11 H11 118.0 . . ?
C10 C11 H11 118.0 . . ?
C13 C12 C11 116.8(3) . . ?
C13 C12 C21 121.8(3) . . ?
C11 C12 C21 121.4(3) . . ?
C12 C13 C14 121.8(3) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C13 C14 C9 120.2(3) . . ?
C13 C14 H14 119.9 . . ?
C9 C14 H14 119.9 . . ?
C16 C15 C20 120.0(3) . . ?
C16 C15 N2 120.0(3) . . ?
C20 C15 N2 119.9(3) . . ?
C15 C16 C17 119.4(3) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 121.6(3) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C19 C18 C17 117.6(3) . . ?
C19 C18 C22 121.1(3) . . ?
C17 C18 C22 121.3(3) . . ?
C20 C19 C18 121.5(3) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C15 119.8(3) . . ?
C19 C20 H20 120.1 . . ?
C15 C20 H20 120.1 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N32 C31 N31 121.9(3) . . ?
N32 C31 C32 130.7(3) . . ?
N31 C31 C32 107.4(2) . . ?
C37 C32 C33 120.0(3) . . ?
C37 C32 C31 107.2(3) . . ?
C33 C32 C31 132.7(3) . . ?
C34 C33 C32 118.2(3) . . ?
C34 C33 H33 120.9 . . ?
C32 C33 H33 120.9 . . ?
C35 C34 C33 120.9(3) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C36 C35 C34 121.2(3) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C35 C36 C37 118.0(3) . . ?
C35 C36 H36 121.0 . . ?
C37 C36 H36 121.0 . . ?
C36 C37 C32 121.5(3) . . ?
C36 C37 C38 128.2(3) . . ?
C32 C37 C38 110.2(3) . . ?
N31 C38 C37 102.6(2) . . ?
N31 C38 H38A 111.2 . . ?
C37 C38 H38A 111.2 . . ?
N31 C38 H38B 111.2 . . ?
C37 C38 H38B 111.2 . . ?
H38A C38 H38B 109.2 . . ?
C44 C39 C40 119.7(3) . . ?
C44 C39 N31 118.7(3) . . ?
C40 C39 N31 121.5(3) . . ?
C39 C40 C41 117.6(3) . . ?
C39 C40 Pd2 121.3(2) . . ?
C41 C40 Pd2 120.9(2) . . ?
C42 C41 C40 123.3(3) . . ?
C42 C41 H41 118.4 . . ?
C40 C41 H41 118.4 . . ?
C41 C42 C43 117.3(3) . . ?
C41 C42 C51 121.6(3) . . ?
C43 C42 C51 121.2(3) . . ?
C44 C43 C42 121.3(3) . . ?
C44 C43 H43 119.3 . . ?
C42 C43 H43 119.3 . . ?
C43 C44 C39 120.8(3) . . ?
C43 C44 H44 119.6 . . ?
C39 C44 H44 119.6 . . ?
C50 C45 C46 119.6(3) . . ?
C50 C45 N32 119.7(3) . . ?
C46 C45 N32 120.7(3) . . ?
C47 C46 C45 119.8(3) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C46 C47 C48 122.0(3) . . ?
C46 C47 H47 119.0 . . ?
C48 C47 H47 119.0 . . ?
C47 C48 C49 117.5(3) . . ?
C47 C48 C52 120.5(3) . . ?
C49 C48 C52 122.1(3) . . ?
C50 C49 C48 121.3(3) . . ?
C50 C49 H49 119.3 . . ?
C48 C49 H49 119.3 . . ?
C45 C50 C49 119.8(3) . . ?
C45 C50 H50 120.1 . . ?
C49 C50 H50 120.1 . . ?
C42 C51 H51A 109.5 . . ?
C42 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C42 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C48 C52 H52A 109.5 . . ?
C48 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C48 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O2 C61 O1 126.2(3) . . ?
O2 C61 C62 117.6(3) . . ?
O1 C61 C62 116.1(3) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O3 C63 O4 126.8(3) . . ?
O3 C63 C64 117.5(3) . . ?
O4 C63 C64 115.7(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
Cl1 C65 Cl3 110.3(2) . . ?
Cl1 C65 Cl2 110.7(2) . . ?
Cl3 C65 Cl2 110.0(2) . . ?
Cl1 C65 H65 108.6 . . ?
Cl3 C65 H65 108.6 . . ?
Cl2 C65 H65 108.6 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C10 1.969(3) . ?
Pd1 N2 2.016(3) . ?
Pd1 O1 2.083(2) . ?
Pd1 O3 2.159(2) . ?
Pd1 Pd2 3.0049(3) . ?
Pd2 C40 1.956(3) . ?
Pd2 N32 2.014(2) . ?
Pd2 O4 2.077(2) . ?
Pd2 O2 2.145(2) . ?
O1 C61 1.255(4) . ?
O2 C61 1.247(4) . ?
O3 C63 1.226(4) . ?
O4 C63 1.259(4) . ?
N1 C1 1.361(4) . ?
N1 C9 1.416(4) . ?
N1 C8 1.472(4) . ?
N2 C1 1.302(4) . ?
N2 C15 1.445(4) . ?
N31 C31 1.375(4) . ?
N31 C39 1.418(4) . ?
N31 C38 1.466(4) . ?
N32 C31 1.298(4) . ?
N32 C45 1.441(4) . ?
C1 C2 1.492(4) . ?
C2 C7 1.393(4) . ?
C2 C3 1.404(5) . ?
C3 C4 1.392(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.380(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.488(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.395(4) . ?
C9 C14 1.407(4) . ?
C10 C11 1.397(4) . ?
C11 C12 1.394(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.378(5) . ?
C12 C21 1.502(5) . ?
C13 C14 1.381(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.381(4) . ?
C15 C20 1.391(4) . ?
C16 C17 1.386(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.396(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(5) . ?
C18 C22 1.508(5) . ?
C19 C20 1.380(4) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C31 C32 1.483(4) . ?
C32 C37 1.393(5) . ?
C32 C33 1.396(4) . ?
C33 C34 1.391(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.382(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.384(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.498(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C44 1.397(4) . ?
C39 C40 1.403(4) . ?
C40 C41 1.404(4) . ?
C41 C42 1.390(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.392(5) . ?
C42 C51 1.510(4) . ?
C43 C44 1.379(4) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C50 1.382(4) . ?
C45 C46 1.392(4) . ?
C46 C47 1.378(4) . ?
C46 H46 0.9500 . ?
C47 C48 1.388(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.395(4) . ?
C48 C52 1.504(5) . ?
C49 C50 1.393(4) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 C62 1.513(5) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C64 1.522(5) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
Cl1 C65 1.747(4) . ?
Cl2 C65 1.754(4) . ?
Cl3 C65 1.749(4) . ?
C65 H65 1.0000 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 Pd1 Pd2 C40 75.11(13) . . . . ?
N2 Pd1 Pd2 C40 -22.02(12) . . . . ?
O1 Pd1 Pd2 C40 163.14(11) . . . . ?
O3 Pd1 Pd2 C40 -109.08(11) . . . . ?
C10 Pd1 Pd2 N32 -14.46(12) . . . . ?
N2 Pd1 Pd2 N32 -111.59(10) . . . . ?
O1 Pd1 Pd2 N32 73.57(10) . . . . ?
O3 Pd1 Pd2 N32 161.35(9) . . . . ?
C10 Pd1 Pd2 O4 167.16(11) . . . . ?
N2 Pd1 Pd2 O4 70.03(10) . . . . ?
O1 Pd1 Pd2 O4 -104.81(9) . . . . ?
O3 Pd1 Pd2 O4 -17.03(9) . . . . ?
C10 Pd1 Pd2 O2 -106.43(11) . . . . ?
N2 Pd1 Pd2 O2 156.45(10) . . . . ?
O1 Pd1 Pd2 O2 -18.39(9) . . . . ?
O3 Pd1 Pd2 O2 69.39(9) . . . . ?
C10 Pd1 O1 C61 133.4(3) . . . . ?
N2 Pd1 O1 C61 -127.8(5) . . . . ?
O3 Pd1 O1 C61 -47.1(3) . . . . ?
Pd2 Pd1 O1 C61 27.4(3) . . . . ?
N32 Pd2 O2 C61 -83.3(3) . . . . ?
O4 Pd2 O2 C61 104.2(3) . . . . ?
Pd1 Pd2 O2 C61 20.7(2) . . . . ?
N2 Pd1 O3 C63 -94.7(3) . . . . ?
O1 Pd1 O3 C63 96.5(3) . . . . ?
Pd2 Pd1 O3 C63 18.7(3) . . . . ?
C40 Pd2 O4 C63 123.2(2) . . . . ?
O2 Pd2 O4 C63 -54.6(2) . . . . ?
Pd1 Pd2 O4 C63 25.3(2) . . . . ?
C10 Pd1 N2 C1 20.7(3) . . . . ?
O1 Pd1 N2 C1 -78.4(6) . . . . ?
O3 Pd1 N2 C1 -158.1(3) . . . . ?
Pd2 Pd1 N2 C1 128.1(2) . . . . ?
C10 Pd1 N2 C15 -169.2(2) . . . . ?
O1 Pd1 N2 C15 91.8(5) . . . . ?
O3 Pd1 N2 C15 12.0(2) . . . . ?
Pd2 Pd1 N2 C15 -61.8(2) . . . . ?
C40 Pd2 N32 C31 -39.8(2) . . . . ?
O2 Pd2 N32 C31 138.2(2) . . . . ?
Pd1 Pd2 N32 C31 58.1(2) . . . . ?
C40 Pd2 N32 C45 146.9(2) . . . . ?
O2 Pd2 N32 C45 -35.1(2) . . . . ?
Pd1 Pd2 N32 C45 -115.25(19) . . . . ?
C15 N2 C1 N1 175.5(3) . . . . ?
Pd1 N2 C1 N1 -14.6(4) . . . . ?
C15 N2 C1 C2 -7.4(5) . . . . ?
Pd1 N2 C1 C2 162.5(2) . . . . ?
C9 N1 C1 N2 -5.9(5) . . . . ?
C8 N1 C1 N2 178.6(3) . . . . ?
C9 N1 C1 C2 176.4(3) . . . . ?
C8 N1 C1 C2 0.9(3) . . . . ?
N2 C1 C2 C7 -175.9(3) . . . . ?
N1 C1 C2 C7 1.6(3) . . . . ?
N2 C1 C2 C3 2.9(6) . . . . ?
N1 C1 C2 C3 -179.6(3) . . . . ?
C7 C2 C3 C4 1.7(5) . . . . ?
C1 C2 C3 C4 -176.9(3) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C3 C4 C5 C6 -1.6(6) . . . . ?
C4 C5 C6 C7 1.4(5) . . . . ?
C5 C6 C7 C2 0.3(5) . . . . ?
C5 C6 C7 C8 -179.1(3) . . . . ?
C3 C2 C7 C6 -1.9(5) . . . . ?
C1 C2 C7 C6 177.1(3) . . . . ?
C3 C2 C7 C8 177.6(3) . . . . ?
C1 C2 C7 C8 -3.4(4) . . . . ?
C1 N1 C8 C7 -2.8(4) . . . . ?
C9 N1 C8 C7 -178.6(3) . . . . ?
C6 C7 C8 N1 -176.7(3) . . . . ?
C2 C7 C8 N1 3.8(4) . . . . ?
C1 N1 C9 C10 13.2(5) . . . . ?
C8 N1 C9 C10 -171.6(3) . . . . ?
C1 N1 C9 C14 -167.5(3) . . . . ?
C8 N1 C9 C14 7.6(5) . . . . ?
C14 C9 C10 C11 1.0(5) . . . . ?
N1 C9 C10 C11 -179.8(3) . . . . ?
C14 C9 C10 Pd1 -178.4(3) . . . . ?
N1 C9 C10 Pd1 0.9(5) . . . . ?
N2 Pd1 C10 C9 -13.2(3) . . . . ?
O1 Pd1 C10 C9 155.6(3) . . . . ?
Pd2 Pd1 C10 C9 -127.7(3) . . . . ?
N2 Pd1 C10 C11 167.5(2) . . . . ?
O1 Pd1 C10 C11 -23.7(2) . . . . ?
Pd2 Pd1 C10 C11 53.0(2) . . . . ?
C9 C10 C11 C12 -1.5(5) . . . . ?
Pd1 C10 C11 C12 177.9(3) . . . . ?
C10 C11 C12 C13 1.5(5) . . . . ?
C10 C11 C12 C21 -177.5(3) . . . . ?
C11 C12 C13 C14 -1.0(6) . . . . ?
C21 C12 C13 C14 178.0(4) . . . . ?
C12 C13 C14 C9 0.6(6) . . . . ?
C10 C9 C14 C13 -0.6(6) . . . . ?
N1 C9 C14 C13 -179.9(3) . . . . ?
C1 N2 C15 C16 -87.5(4) . . . . ?
Pd1 N2 C15 C16 101.3(3) . . . . ?
C1 N2 C15 C20 91.5(3) . . . . ?
Pd1 N2 C15 C20 -79.7(3) . . . . ?
C20 C15 C16 C17 -2.3(4) . . . . ?
N2 C15 C16 C17 176.7(3) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
C16 C17 C18 C19 2.5(5) . . . . ?
C16 C17 C18 C22 -176.4(3) . . . . ?
C17 C18 C19 C20 -2.0(5) . . . . ?
C22 C18 C19 C20 176.9(3) . . . . ?
C18 C19 C20 C15 -0.7(5) . . . . ?
C16 C15 C20 C19 2.9(4) . . . . ?
N2 C15 C20 C19 -176.1(3) . . . . ?
C45 N32 C31 N31 -171.6(3) . . . . ?
Pd2 N32 C31 N31 15.1(4) . . . . ?
C45 N32 C31 C32 10.8(5) . . . . ?
Pd2 N32 C31 C32 -162.6(2) . . . . ?
C39 N31 C31 N32 27.1(4) . . . . ?
C38 N31 C31 N32 -167.8(3) . . . . ?
C39 N31 C31 C32 -154.7(3) . . . . ?
C38 N31 C31 C32 10.3(3) . . . . ?
N32 C31 C32 C37 169.5(3) . . . . ?
N31 C31 C32 C37 -8.4(3) . . . . ?
N32 C31 C32 C33 -13.3(6) . . . . ?
N31 C31 C32 C33 168.8(3) . . . . ?
C37 C32 C33 C34 -1.5(5) . . . . ?
C31 C32 C33 C34 -178.4(3) . . . . ?
C32 C33 C34 C35 -1.5(5) . . . . ?
C33 C34 C35 C36 2.5(6) . . . . ?
C34 C35 C36 C37 -0.4(6) . . . . ?
C35 C36 C37 C32 -2.7(5) . . . . ?
C35 C36 C37 C38 174.7(3) . . . . ?
C33 C32 C37 C36 3.6(5) . . . . ?
C31 C32 C37 C36 -178.7(3) . . . . ?
C33 C32 C37 C38 -174.2(3) . . . . ?
C31 C32 C37 C38 3.5(3) . . . . ?
C31 N31 C38 C37 -7.9(3) . . . . ?
C39 N31 C38 C37 157.1(3) . . . . ?
C36 C37 C38 N31 -175.3(3) . . . . ?
C32 C37 C38 N31 2.3(3) . . . . ?
C31 N31 C39 C44 146.9(3) . . . . ?
C38 N31 C39 C44 -16.4(4) . . . . ?
C31 N31 C39 C40 -28.6(4) . . . . ?
C38 N31 C39 C40 168.1(3) . . . . ?
C44 C39 C40 C41 -3.3(4) . . . . ?
N31 C39 C40 C41 172.2(3) . . . . ?
C44 C39 C40 Pd2 172.1(2) . . . . ?
N31 C39 C40 Pd2 -12.5(4) . . . . ?
N32 Pd2 C40 C39 36.5(2) . . . . ?
O4 Pd2 C40 C39 -151.0(2) . . . . ?
Pd1 Pd2 C40 C39 -67.9(2) . . . . ?
N32 Pd2 C40 C41 -148.3(3) . . . . ?
O4 Pd2 C40 C41 24.2(3) . . . . ?
Pd1 Pd2 C40 C41 107.3(2) . . . . ?
C39 C40 C41 C42 1.9(5) . . . . ?
Pd2 C40 C41 C42 -173.4(2) . . . . ?
C40 C41 C42 C43 0.3(5) . . . . ?
C40 C41 C42 C51 179.5(3) . . . . ?
C41 C42 C43 C44 -1.2(5) . . . . ?
C51 C42 C43 C44 179.6(3) . . . . ?
C42 C43 C44 C39 -0.2(5) . . . . ?
C40 C39 C44 C43 2.5(5) . . . . ?
N31 C39 C44 C43 -173.1(3) . . . . ?
C31 N32 C45 C50 84.8(4) . . . . ?
Pd2 N32 C45 C50 -101.5(3) . . . . ?
C31 N32 C45 C46 -94.2(4) . . . . ?
Pd2 N32 C45 C46 79.6(3) . . . . ?
C50 C45 C46 C47 -0.3(5) . . . . ?
N32 C45 C46 C47 178.7(3) . . . . ?
C45 C46 C47 C48 -0.4(5) . . . . ?
C46 C47 C48 C49 0.2(5) . . . . ?
C46 C47 C48 C52 -179.1(4) . . . . ?
C47 C48 C49 C50 0.8(5) . . . . ?
C52 C48 C49 C50 -180.0(4) . . . . ?
C46 C45 C50 C49 1.2(5) . . . . ?
N32 C45 C50 C49 -177.8(3) . . . . ?
C48 C49 C50 C45 -1.5(5) . . . . ?
Pd2 O2 C61 O1 -8.7(5) . . . . ?
Pd2 O2 C61 C62 169.1(2) . . . . ?
Pd1 O1 C61 O2 -21.4(5) . . . . ?
Pd1 O1 C61 C62 160.7(2) . . . . ?
Pd1 O3 C63 O4 -5.4(5) . . . . ?
Pd1 O3 C63 C64 173.8(2) . . . . ?
Pd2 O4 C63 O3 -21.5(4) . . . . ?
Pd2 O4 C63 C64 159.3(2) . . . . ?
