# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_sa1575 _database_code_depnum_ccdc_archive 'CCDC 917449' #TrackingRef '16423_web_deposit_cif_file_0_YudongCai_1356436891.sa1575.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 F6 N2 O4 P2 Pd S2' _chemical_formula_sum 'C48 H36 F6 N2 O4 P2 Pd S2' _chemical_formula_weight 1051.25 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.8039(17) _cell_length_b 14.5782(16) _cell_length_c 22.466(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4521.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15234 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 27.49 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8201 _exptl_absorpt_correction_T_max 0.9208 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28506 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10315 _reflns_number_gt 9817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Olex2 ver 1.1' _computing_publication_material 'SHELX97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+2.9980P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 10315 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.08621(2) 0.379628(17) 0.989537(13) 0.02269(7) Uani 1 1 d . . . S1 S 0.15001(7) 0.40323(6) 0.85300(5) 0.0278(2) Uani 1 1 d . . . S2 S -0.07701(7) 0.51125(6) 1.04444(4) 0.0270(2) Uani 1 1 d . . . P1 P 0.13475(7) 0.23561(7) 0.96903(5) 0.0251(2) Uani 1 1 d . . . P2 P 0.17082(8) 0.35317(7) 1.07526(5) 0.0275(2) Uani 1 1 d . . . F1 F 0.28370(19) 0.49487(19) 0.79685(14) 0.0534(8) Uani 1 1 d . . . F2 F 0.1456(2) 0.56358(18) 0.79859(14) 0.0524(8) Uani 1 1 d . . . F3 F 0.2347(2) 0.56081(17) 0.87740(14) 0.0489(7) Uani 1 1 d . . . F4 F -0.1300(2) 0.5617(2) 1.15188(13) 0.0567(8) Uani 1 1 d . . . F5 F 0.0211(2) 0.5331(2) 1.14432(13) 0.0574(8) Uani 1 1 d . . . F6 F -0.0365(3) 0.65735(19) 1.10820(15) 0.0662(10) Uani 1 1 d . . . O1 O 0.22929(19) 0.35967(18) 0.88282(13) 0.0313(6) Uani 1 1 d . . . O2 O 0.1169(2) 0.3679(2) 0.79697(13) 0.0393(7) Uani 1 1 d . . . O3 O -0.1511(2) 0.5682(2) 1.01907(14) 0.0400(7) Uani 1 1 d . . . O4 O -0.1023(2) 0.41961(18) 1.06216(13) 0.0337(7) Uani 1 1 d . . . N1 N 0.0681(2) 0.4236(2) 0.89916(14) 0.0231(7) Uani 1 1 d . . . N2 N 0.0207(2) 0.50921(18) 1.01073(15) 0.0235(6) Uani 1 1 d . . . C1 C 0.2559(3) 0.2579(3) 1.0598(2) 0.0325(9) Uani 1 1 d . . . H1B H 0.3216 0.2759 1.0731 0.039 Uiso 1 1 calc R . . H1A H 0.2360 0.2035 1.0832 0.039 Uiso 1 1 calc R . . C2 C 0.2598(3) 0.2320(3) 0.99394(19) 0.0290(8) Uani 1 1 d . . . H2B H 0.2873 0.1698 0.9887 0.035 Uiso 1 1 calc R . . H2A H 0.2999 0.2763 0.9714 0.035 Uiso 1 1 calc R . . C3 C 0.1201(3) 0.1835(3) 0.89694(19) 0.0273(9) Uani 1 1 d . . . C4 C 0.0268(3) 0.1601(3) 0.8796(2) 0.0344(10) Uani 1 1 d . . . H4 H -0.0264 0.1755 0.9045 0.041 Uiso 1 1 calc R . . C5 C 0.0103(3) 0.1146(3) 0.8263(2) 0.0395(10) Uani 1 1 d . . . H5 H -0.0539 0.1002 0.8142 0.047 Uiso 1 1 calc R . . C6 C 0.0885(4) 0.0904(3) 0.79091(19) 0.0404(10) Uani 1 1 d . . . H6 H 0.0781 0.0587 0.7545 0.048 Uiso 1 1 calc R . . C7 C 0.1812(3) 0.1122(3) 0.8084(2) 0.0411(11) Uani 1 1 d . . . H7 H 0.2344 0.0946 0.7841 0.049 Uiso 1 1 calc R . . C8 C 0.1980(3) 0.1594(3) 0.8609(2) 0.0349(10) Uani 1 1 d . . . H8 H 0.2622 0.1751 0.8722 0.042 Uiso 1 1 calc R . . C9 C 0.0760(3) 0.1508(2) 1.01605(18) 0.0287(8) Uani 1 1 d . . . C10 C 0.1128(3) 0.0610(3) 1.0147(2) 0.0368(10) Uani 1 1 d . . . H10 H 0.1649 0.0453 0.9890 0.044 Uiso 1 1 calc R . . C11 C 0.0714(4) -0.0044(3) 1.0517(2) 0.0440(11) Uani 1 1 d . . . H11 H 0.0959 -0.0653 1.0513 0.053 Uiso 1 1 calc R . . C12 C -0.0040(4) 0.0166(3) 1.0889(2) 0.0471(12) Uani 1 1 d . . . H12 H -0.0305 -0.0289 1.1143 0.057 Uiso 1 1 calc R . . C13 C -0.0412(3) 0.1049(3) 1.0891(2) 0.0437(12) Uani 1 1 d . . . H13 H -0.0942 0.1197 1.1143 0.052 Uiso 1 1 calc R . . C14 C -0.0013(3) 0.1718(3) 1.0525(2) 0.0339(9) Uani 1 1 d . . . H14 H -0.0273 0.2322 1.0525 0.041 Uiso 1 1 calc R . . C15 C 0.1273(3) 0.3244(3) 1.1487(2) 0.0344(10) Uani 1 1 d . . . C16 C 0.0290(4) 0.3214(3) 1.1618(2) 0.0447(12) Uani 1 1 d . . . H16 H -0.0169 0.3386 1.1323 0.054 Uiso 1 1 calc R . . C17 C -0.0026(5) 0.2938(4) 1.2169(3) 0.0712(19) Uani 1 1 d . . . H17 H -0.0700 0.2920 1.2253 0.085 Uiso 1 1 calc R . . C18 C 0.0633(5) 0.2688(4) 1.2602(2) 0.073(2) Uani 1 1 d . . . H18 H 0.0411 0.2484 1.2980 0.088 Uiso 1 1 calc R . . C19 C 0.1619(4) 0.2734(3) 1.2484(2) 0.0574(15) Uani 1 1 d . . . H19 H 0.2077 0.2582 1.2784 0.069 Uiso 1 1 calc R . . C20 C 0.1930(4) 0.3003(3) 1.1924(2) 0.0415(11) Uani 1 1 d . . . H20 H 0.2604 0.3021 1.1839 0.050 Uiso 1 1 calc R . . C21 C 0.2484(3) 0.4533(3) 1.0843(2) 0.0309(9) Uani 1 1 d . . . C22 C 0.2564(3) 0.5007(3) 1.1383(2) 0.0398(11) Uani 1 1 d . . . H22 H 0.2176 0.4838 1.1714 0.048 Uiso 1 1 calc R . . C23 C 0.3213(4) 0.5719(3) 1.1427(3) 0.0498(14) Uani 1 1 d . . . H23 H 0.3274 0.6039 1.1794 0.060 Uiso 1 1 calc R . . C24 C 0.3769(4) 0.5975(3) 1.0955(3) 0.0504(14) Uani 1 1 d . . . H24 H 0.4228 0.6455 1.0999 0.061 Uiso 1 1 calc R . . C25 C 0.3668(3) 0.5534(3) 1.0403(3) 0.0485(13) Uani 1 1 d . . . H25 H 0.4035 0.5728 1.0068 0.058 Uiso 1 1 calc R . . C26 C 0.3022(3) 0.4807(3) 1.0357(2) 0.0430(11) Uani 1 1 d . . . H26 H 0.2950 0.4496 0.9988 0.052 Uiso 1 1 calc R . . C27 C -0.0235(3) 0.4565(3) 0.87917(17) 0.0247(8) Uani 1 1 d . . . C28 C -0.0860(3) 0.3958(2) 0.84799(17) 0.0297(8) Uani 1 1 d . . . H28 H -0.0653 0.3349 0.8398 0.036 Uiso 1 1 calc R . . C29 C -0.1753(3) 0.4241(3) 0.82978(19) 0.0302(9) Uani 1 1 d . . . H29 H -0.2150 0.3834 0.8076 0.036 Uiso 1 1 calc R . . C30 C -0.2098(3) 0.5133(3) 0.84352(18) 0.0273(8) Uani 1 1 d . . . C31 C -0.3024(3) 0.5436(3) 0.8249(2) 0.0363(10) Uani 1 1 d . . . H31 H -0.3427 0.5032 0.8028 0.044 Uiso 1 1 calc R . . C32 C -0.3351(3) 0.6295(4) 0.8382(2) 0.0425(11) Uani 1 1 d . . . H32 H -0.3971 0.6491 0.8250 0.051 Uiso 1 1 calc R . . C33 C -0.2760(3) 0.6887(3) 0.8715(2) 0.0378(10) Uani 1 1 d . . . H33 H -0.2983 0.7488 0.8804 0.045 Uiso 1 1 calc R . . C34 C -0.1868(3) 0.6613(3) 0.8912(2) 0.0331(9) Uani 1 1 d . . . H34 H -0.1495 0.7013 0.9154 0.040 Uiso 1 1 calc R . . C35 C -0.1493(3) 0.5736(3) 0.87583(18) 0.0253(8) Uani 1 1 d . . . C36 C -0.0530(3) 0.5456(3) 0.89297(18) 0.0234(8) Uani 1 1 d . . . C37 C 0.0157(3) 0.6101(2) 0.92245(17) 0.0239(8) Uani 1 1 d . . . C38 C 0.0503(3) 0.6911(3) 0.89270(19) 0.0263(8) Uani 1 1 d . . . C39 C 0.0187(3) 0.7167(3) 0.83518(18) 0.0297(9) Uani 1 1 d . . . H39 H -0.0275 0.6796 0.8152 0.036 Uiso 1 1 calc R . . C40 C 0.0531(3) 0.7936(3) 0.8077(2) 0.0371(10) Uani 1 1 d . . . H40 H 0.0304 0.8093 0.7691 0.045 Uiso 1 1 calc R . . C41 C 0.1222(3) 0.8501(3) 0.8364(2) 0.0389(11) Uani 1 1 d . . . H41 H 0.1465 0.9032 0.8170 0.047 Uiso 1 1 calc R . . C42 C 0.1539(3) 0.8278(3) 0.8922(2) 0.0368(10) Uani 1 1 d . . . H42 H 0.1995 0.8663 0.9115 0.044 Uiso 1 1 calc R . . C43 C 0.1200(3) 0.7484(3) 0.92162(19) 0.0298(9) Uani 1 1 d . . . C44 C 0.1547(3) 0.7236(3) 0.9782(2) 0.0342(10) Uani 1 1 d . . . H44 H 0.2022 0.7608 0.9971 0.041 Uiso 1 1 calc R . . C45 C 0.1215(3) 0.6471(2) 1.0066(2) 0.0320(9) Uani 1 1 d . . . H45 H 0.1455 0.6316 1.0449 0.038 Uiso 1 1 calc R . . C46 C 0.0510(3) 0.5905(2) 0.97868(18) 0.0250(8) Uani 1 1 d . . . C47 C 0.2058(3) 0.5125(3) 0.8303(2) 0.0376(10) Uani 1 1 d . . . C48 C -0.0545(3) 0.5682(3) 1.1161(2) 0.0373(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02503(13) 0.02339(12) 0.01964(13) -0.00146(11) 0.00036(12) 0.00157(11) S1 0.0291(5) 0.0311(5) 0.0233(5) -0.0010(4) 0.0021(4) 0.0015(4) S2 0.0277(5) 0.0303(5) 0.0229(5) -0.0024(4) 0.0010(4) 0.0018(4) P1 0.0262(5) 0.0258(5) 0.0232(5) -0.0036(4) 0.0005(4) 0.0041(4) P2 0.0323(5) 0.0269(5) 0.0232(5) -0.0011(4) -0.0027(4) 0.0017(4) F1 0.0459(16) 0.0518(16) 0.062(2) 0.0124(15) 0.0277(15) 0.0055(13) F2 0.0592(18) 0.0480(16) 0.0500(19) 0.0200(14) 0.0119(15) 0.0185(13) F3 0.0507(17) 0.0374(14) 0.059(2) -0.0062(13) 0.0071(15) -0.0112(12) F4 0.0545(18) 0.082(2) 0.0336(16) -0.0125(15) 0.0182(15) 0.0026(16) F5 0.0551(18) 0.079(2) 0.0384(17) -0.0184(16) -0.0164(15) 0.0099(16) F6 0.113(3) 0.0385(15) 0.0471(19) -0.0174(14) 0.018(2) -0.0104(16) O1 0.0257(14) 0.0366(16) 0.0316(16) 0.0039(12) 0.0026(12) 0.0060(11) O2 0.0411(17) 0.0521(18) 0.0246(15) -0.0122(14) 0.0017(13) 0.0024(14) O3 0.0335(15) 0.0541(18) 0.0325(18) 0.0059(15) 0.0026(14) 0.0149(13) O4 0.0366(17) 0.0345(14) 0.0302(16) -0.0002(12) 0.0082(14) -0.0077(12) N1 0.0256(17) 0.0270(15) 0.0169(15) -0.0007(12) 0.0001(13) 0.0032(12) N2 0.0287(15) 0.0191(13) 0.0227(15) -0.0015(13) 0.0049(15) 0.0016(11) C1 0.030(2) 0.034(2) 0.033(2) 0.0014(18) -0.0067(19) 0.0025(17) C2 0.0268(18) 0.0331(19) 0.027(2) -0.0042(17) 0.0006(17) 0.0065(15) C3 0.030(2) 0.0246(19) 0.027(2) 0.0002(16) -0.0012(17) 0.0048(15) C4 0.032(2) 0.040(2) 0.031(2) -0.0028(19) -0.0030(19) 0.0001(18) C5 0.041(2) 0.038(2) 0.039(3) -0.007(2) -0.009(2) -0.003(2) C6 0.068(3) 0.0257(19) 0.027(2) -0.0016(16) -0.010(3) 0.004(2) C7 0.047(3) 0.044(2) 0.032(2) -0.003(2) 0.009(2) 0.009(2) C8 0.034(2) 0.039(2) 0.032(2) -0.0070(19) 0.0054(19) 0.0024(18) C9 0.0277(19) 0.0321(18) 0.026(2) -0.0005(16) -0.0019(18) -0.0005(15) C10 0.039(2) 0.034(2) 0.037(2) 0.005(2) -0.002(2) 0.0048(17) C11 0.048(3) 0.041(2) 0.044(3) 0.010(2) -0.007(2) 0.000(2) C12 0.051(3) 0.049(3) 0.042(3) 0.019(2) -0.006(2) -0.013(2) C13 0.028(2) 0.062(3) 0.042(3) 0.010(2) 0.003(2) -0.007(2) C14 0.026(2) 0.039(2) 0.036(2) 0.0002(19) -0.0008(18) -0.0016(17) C15 0.048(3) 0.031(2) 0.024(2) -0.0009(18) -0.005(2) 0.0065(19) C16 0.054(3) 0.049(3) 0.031(3) 0.009(2) 0.006(2) 0.011(2) C17 0.075(4) 0.086(4) 0.052(4) 0.026(3) 0.029(3) 0.023(3) C18 0.103(5) 0.083(4) 0.034(3) 0.027(3) 0.021(3) 0.043(4) C19 0.089(4) 0.053(3) 0.030(3) 0.008(2) -0.004(3) 0.031(3) C20 0.058(3) 0.037(2) 0.030(3) 0.006(2) -0.003(2) 0.012(2) C21 0.030(2) 0.030(2) 0.033(2) -0.0052(18) -0.0036(18) 0.0049(17) C22 0.050(3) 0.034(2) 0.036(3) -0.005(2) -0.008(2) 0.007(2) C23 0.057(3) 0.038(3) 0.054(3) -0.014(2) -0.022(3) -0.002(2) C24 0.040(3) 0.035(3) 0.076(4) -0.009(2) -0.015(3) -0.005(2) C25 0.040(3) 0.044(3) 0.062(4) -0.004(2) 0.007(3) -0.009(2) C26 0.045(3) 0.039(2) 0.045(3) -0.009(2) 0.003(2) -0.004(2) C27 0.0267(19) 0.0295(19) 0.0180(18) 0.0021(15) -0.0010(15) -0.0004(15) C28 0.035(2) 0.0266(19) 0.027(2) -0.0008(15) -0.0007(19) -0.0069(18) C29 0.033(2) 0.033(2) 0.024(2) 0.0016(17) -0.0012(17) -0.0107(17) C30 0.0272(19) 0.034(2) 0.021(2) 0.0037(16) 0.0022(16) -0.0019(16) C31 0.026(2) 0.054(3) 0.029(2) 0.006(2) -0.0022(18) -0.0035(19) C32 0.031(2) 0.062(3) 0.034(3) 0.013(2) -0.0017(18) 0.009(2) C33 0.034(2) 0.040(2) 0.040(3) 0.007(2) 0.007(2) 0.0136(18) C34 0.034(2) 0.034(2) 0.031(2) 0.0001(18) -0.0002(19) 0.0067(18) C35 0.0254(19) 0.031(2) 0.0193(19) 0.0020(16) -0.0040(16) 0.0019(15) C36 0.0231(18) 0.0264(19) 0.020(2) 0.0035(15) -0.0012(15) -0.0007(15) C37 0.0256(18) 0.0216(17) 0.0246(19) 0.0001(16) -0.0009(15) -0.0025(15) C38 0.0275(19) 0.0242(18) 0.027(2) -0.0007(16) 0.0043(17) 0.0029(15) C39 0.033(2) 0.030(2) 0.026(2) 0.0020(16) -0.0014(17) 0.0013(17) C40 0.044(3) 0.036(2) 0.032(2) 0.0039(19) 0.003(2) 0.0021(19) C41 0.049(3) 0.030(2) 0.038(3) 0.0047(18) 0.006(2) -0.0031(19) C42 0.048(3) 0.026(2) 0.036(3) -0.0035(18) 0.001(2) -0.0033(19) C43 0.031(2) 0.027(2) 0.032(2) -0.0038(17) -0.0014(18) -0.0023(15) C44 0.039(2) 0.030(2) 0.033(3) -0.0059(17) -0.0041(19) -0.0090(17) C45 0.036(2) 0.0318(19) 0.028(2) -0.0022(17) -0.0042(18) -0.0012(15) C46 0.0288(18) 0.0210(16) 0.025(2) -0.0001(15) -0.0011(16) 0.0005(14) C47 0.039(2) 0.039(2) 0.035(3) 0.006(2) 0.013(2) 0.0042(19) C48 0.041(3) 0.038(2) 0.032(3) -0.004(2) 0.005(2) 0.0045(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N1 2.144(3) . ? Pd1 N2 2.148(3) . ? Pd1 P1 2.2515(10) . ? Pd1 P2 2.2850(11) . ? S1 O1 1.432(3) . ? S1 O2 1.435(3) . ? S1 N1 1.562(3) . ? S1 C47 1.841(5) . ? S2 O3 1.435(3) . ? S2 O4 1.437(3) . ? S2 N2 1.547(3) . ? S2 C48 1.838(5) . ? P1 C3 1.800(4) . ? P1 C2 1.816(4) . ? P1 C9 1.817(4) . ? P2 C15 1.804(5) . ? P2 C21 1.822(4) . ? P2 C1 1.852(4) . ? F1 C47 1.338(5) . ? F2 C47 1.325(5) . ? F3 C47 1.332(5) . ? F4 C48 1.320(5) . ? F5 C48 1.324(5) . ? F6 C48 1.335(5) . ? N1 C27 1.426(5) . ? N2 C46 1.449(4) . ? C1 C2 1.528(6) . ? C1 H1B 0.9900 . ? C1 H1A 0.9900 . ? C2 H2B 0.9900 . ? C2 H2A 0.9900 . ? C3 C4 1.388(6) . ? C3 C8 1.391(6) . ? C4 C5 1.387(6) . ? C4 H4 0.9500 . ? C5 C6 1.388(6) . ? C5 H5 0.9500 . ? C6 C7 1.375(7) . ? C6 H6 0.9500 . ? C7 C8 1.386(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.379(6) . ? C9 C10 1.405(5) . ? C10 C11 1.388(6) . ? C10 H10 0.9500 . ? C11 C12 1.368(7) . ? C11 H11 0.9500 . ? C12 C13 1.385(7) . ? C12 H12 0.9500 . ? C13 C14 1.390(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.382(6) . ? C15 C16 1.390(6) . ? C16 C17 1.374(7) . ? C16 H16 0.9500 . ? C17 C18 1.380(8) . ? C17 H17 0.9500 . ? C18 C19 1.389(8) . ? C18 H18 0.9500 . ? C19 C20 1.386(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.379(6) . ? C21 C22 1.401(6) . ? C22 C23 1.375(6) . ? C22 H22 0.9500 . ? C23 C24 1.361(8) . ? C23 H23 0.9500 . ? C24 C25 1.404(7) . ? C24 H24 0.9500 . ? C25 C26 1.389(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C36 1.395(5) . ? C27 C28 1.420(5) . ? C28 C29 1.363(6) . ? C28 H28 0.9500 . ? C29 C30 1.420(6) . ? C29 H29 0.9500 . ? C30 C35 1.413(5) . ? C30 C31 1.415(5) . ? C31 C32 1.364(6) . ? C31 H31 0.9500 . ? C32 C33 1.403(7) . ? C32 H32 0.9500 . ? C33 C34 1.369(6) . ? C33 H33 0.9500 . ? C34 C35 1.421(5) . ? C34 H34 0.9500 . ? C35 C36 1.443(5) . ? C36 C37 1.491(5) . ? C37 C46 1.384(5) . ? C37 C38 1.438(5) . ? C38 C39 1.414(5) . ? C38 C43 1.431(5) . ? C39 C40 1.364(6) . ? C39 H39 0.9500 . ? C40 C41 1.416(6) . ? C40 H40 0.9500 . ? C41 C42 1.366(6) . ? C41 H41 0.9500 . ? C42 C43 1.412(6) . ? C42 H42 0.9500 . ? C43 C44 1.407(6) . ? C44 C45 1.364(5) . ? C44 H44 0.9500 . ? C45 C46 1.421(5) . ? C45 H45 0.9500 . ? 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 N1 Pd1 N2 84.13(12) . . ? N1 Pd1 P1 96.88(8) . . ? N2 Pd1 P1 172.23(8) . . ? N1 Pd1 P2 155.26(9) . . ? N2 Pd1 P2 100.19(10) . . ? P1 Pd1 P2 82.13(4) . . ? O1 S1 O2 119.63(18) . . ? O1 S1 N1 109.07(17) . . ? O2 S1 N1 114.86(17) . . ? O1 S1 C47 101.16(19) . . ? O2 S1 C47 101.6(2) . . ? N1 S1 C47 108.75(18) . . ? O3 S2 O4 118.30(19) . . ? O3 S2 N2 115.99(18) . . ? O4 S2 N2 109.24(16) . . ? O3 S2 C48 102.0(2) . . ? O4 S2 C48 102.62(19) . . ? N2 S2 C48 106.9(2) . . ? C3 P1 C2 111.83(18) . . ? C3 P1 C9 100.71(18) . . ? C2 P1 C9 103.03(18) . . ? C3 P1 Pd1 122.98(13) . . ? C2 P1 Pd1 104.28(13) . . ? C9 P1 Pd1 112.50(13) . . ? C15 P2 C21 106.3(2) . . ? C15 P2 C1 102.0(2) . . ? C21 P2 C1 104.40(19) . . ? C15 P2 Pd1 129.75(16) . . ? C21 P2 Pd1 105.00(14) . . ? C1 P2 Pd1 107.02(14) . . ? C27 N1 S1 119.8(3) . . ? C27 N1 Pd1 120.2(2) . . ? S1 N1 Pd1 119.17(17) . . ? C46 N2 S2 118.6(2) . . ? C46 N2 Pd1 119.2(2) . . ? S2 N2 Pd1 119.51(15) . . ? C2 C1 P2 112.9(3) . . ? C2 C1 H1B 109.0 . . ? P2 C1 H1B 109.0 . . ? C2 C1 H1A 109.0 . . ? P2 C1 H1A 109.0 . . ? H1B C1 H1A 107.8 . . ? C1 C2 P1 104.9(3) . . ? C1 C2 H2B 110.8 . . ? P1 C2 H2B 110.8 . . ? C1 C2 H2A 110.8 . . ? P1 C2 H2A 110.8 . . ? H2B C2 H2A 108.8 . . ? C4 C3 C8 119.4(4) . . ? C4 C3 P1 117.4(3) . . ? C8 C3 P1 122.9(3) . . ? C5 C4 C3 120.9(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.2(4) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C7 C6 C5 120.1(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.9(4) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C7 C8 C3 119.4(4) . . ? C7 C8 H8 120.3 . . ? C3 C8 H8 120.3 . . ? C14 C9 C10 119.9(4) . . ? C14 C9 P1 122.6(3) . . ? C10 C9 P1 117.5(3) . . ? C11 C10 C9 118.6(4) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C12 C11 C10 121.6(4) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 119.5(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C9 C14 C13 120.1(4) . . ? C9 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C20 C15 C16 118.8(5) . . ? C20 C15 P2 119.4(4) . . ? C16 C15 P2 121.7(4) . . ? C17 C16 C15 120.7(5) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.3(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 119.9(5) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 119.4(5) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C15 C20 C19 120.9(5) . . ? C15 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C26 C21 C22 120.1(4) . . ? C26 C21 P2 117.4(3) . . ? C22 C21 P2 122.5(4) . . ? C23 C22 C21 119.1(5) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C22 121.2(5) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.4(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 118.7(5) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C21 C26 C25 120.4(5) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C36 C27 C28 120.9(4) . . ? C36 C27 N1 120.1(3) . . ? C28 C27 N1 118.9(3) . . ? C29 C28 C27 120.5(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 121.0(4) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C35 C30 C31 119.4(4) . . ? C35 C30 C29 118.9(4) . . ? C31 C30 C29 121.7(4) . . ? C32 C31 C30 121.4(4) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 119.3(4) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 121.0(4) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 120.8(4) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C30 C35 C34 118.0(4) . . ? C30 C35 C36 120.4(4) . . ? C34 C35 C36 121.7(4) . . ? C27 C36 C35 118.2(4) . . ? C27 C36 C37 120.0(3) . . ? C35 C36 C37 121.7(3) . . ? C46 C37 C38 118.5(3) . . ? C46 C37 C36 120.0(3) . . ? C38 C37 C36 121.5(3) . . ? C39 C38 C43 117.8(4) . . ? C39 C38 C37 122.7(4) . . ? C43 C38 C37 119.5(4) . . ? C40 C39 C38 121.6(4) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C39 C40 C41 120.4(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 119.6(4) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 121.3(4) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 121.4(4) . . ? C44 C43 C38 119.3(4) . . ? C42 C43 C38 119.3(4) . . ? C45 C44 C43 121.2(4) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C46 119.9(4) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C37 C46 C45 121.6(4) . . ? C37 C46 N2 121.4(3) . . ? C45 C46 N2 117.0(4) . . ? F2 C47 F3 108.6(4) . . ? F2 C47 F1 108.0(4) . . ? F3 C47 F1 107.9(4) . . ? F2 C47 S1 111.9(3) . . ? F3 C47 S1 111.3(3) . . ? F1 C47 S1 109.0(3) . . ? F4 C48 F5 107.7(4) . . ? F4 C48 F6 107.3(4) . . ? F5 C48 F6 107.0(4) . . ? F4 C48 S2 111.6(3) . . ? F5 C48 S2 112.2(3) . . ? F6 C48 S2 110.8(3) . . ? 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 N1 Pd1 P1 C3 -15.13(18) . . . . ? N2 Pd1 P1 C3 81.9(7) . . . . ? P2 Pd1 P1 C3 -170.20(17) . . . . ? N1 Pd1 P1 C2 113.38(17) . . . . ? N2 Pd1 P1 C2 -149.6(7) . . . . ? P2 Pd1 P1 C2 -41.69(15) . . . . ? N1 Pd1 P1 C9 -135.69(16) . . . . ? N2 Pd1 P1 C9 -38.7(7) . . . . ? P2 Pd1 P1 C9 69.24(14) . . . . ? N1 Pd1 P2 C15 168.7(3) . . . . ? N2 Pd1 P2 C15 70.6(2) . . . . ? P1 Pd1 P2 C15 -101.91(18) . . . . ? N1 Pd1 P2 C21 41.8(2) . . . . ? N2 Pd1 P2 C21 -56.31(16) . . . . ? P1 Pd1 P2 C21 131.20(14) . . . . ? N1 Pd1 P2 C1 -68.7(2) . . . . ? N2 Pd1 P2 C1 -166.88(16) . . . . ? P1 Pd1 P2 C1 20.63(15) . . . . ? O1 S1 N1 C27 -172.2(3) . . . . ? O2 S1 N1 C27 -34.8(3) . . . . ? C47 S1 N1 C27 78.3(3) . . . . ? O1 S1 N1 Pd1 -2.9(2) . . . . ? O2 S1 N1 Pd1 134.52(19) . . . . ? C47 S1 N1 Pd1 -112.4(2) . . . . ? N2 Pd1 N1 C27 -50.4(3) . . . . ? P1 Pd1 N1 C27 121.9(3) . . . . ? P2 Pd1 N1 C27 -152.0(2) . . . . ? N2 Pd1 N1 S1 140.36(19) . . . . ? P1 Pd1 N1 S1 -47.40(18) . . . . ? P2 Pd1 N1 S1 38.7(3) . . . . ? O3 S2 N2 C46 31.3(4) . . . . ? O4 S2 N2 C46 168.0(3) . . . . ? C48 S2 N2 C46 -81.6(3) . . . . ? O3 S2 N2 Pd1 -130.2(2) . . . . ? O4 S2 N2 Pd1 6.6(3) . . . . ? C48 S2 N2 Pd1 116.9(2) . . . . ? N1 Pd1 N2 C46 -43.3(3) . . . . ? P1 Pd1 N2 C46 -141.2(6) . . . . ? P2 Pd1 N2 C46 112.1(3) . . . . ? N1 Pd1 N2 S2 118.0(2) . . . . ? P1 Pd1 N2 S2 20.1(9) . . . . ? P2 Pd1 N2 S2 -86.6(2) . . . . ? C15 P2 C1 C2 147.3(3) . . . . ? C21 P2 C1 C2 -102.1(3) . . . . ? Pd1 P2 C1 C2 8.8(3) . . . . ? P2 C1 C2 P1 -41.4(3) . . . . ? C3 P1 C2 C1 -167.5(3) . . . . ? C9 P1 C2 C1 -60.1(3) . . . . ? Pd1 P1 C2 C1 57.5(3) . . . . ? C2 P1 C3 C4 163.6(3) . . . . ? C9 P1 C3 C4 54.8(4) . . . . ? Pd1 P1 C3 C4 -71.2(4) . . . . ? C2 P1 C3 C8 -11.0(4) . . . . ? C9 P1 C3 C8 -119.8(4) . . . . ? Pd1 P1 C3 C8 114.2(3) . . . . ? C8 C3 C4 C5 -1.2(7) . . . . ? P1 C3 C4 C5 -176.0(3) . . . . ? C3 C4 C5 C6 1.6(7) . . . . ? C4 C5 C6 C7 -0.6(7) . . . . ? C5 C6 C7 C8 -0.8(7) . . . . ? C6 C7 C8 C3 1.2(7) . . . . ? C4 C3 C8 C7 -0.2(6) . . . . ? P1 C3 C8 C7 174.3(3) . . . . ? C3 P1 C9 C14 -122.1(4) . . . . ? C2 P1 C9 C14 122.2(4) . . . . ? Pd1 P1 C9 C14 10.5(4) . . . . ? C3 P1 C9 C10 58.3(4) . . . . ? C2 P1 C9 C10 -57.3(4) . . . . ? Pd1 P1 C9 C10 -169.0(3) . . . . ? C14 C9 C10 C11 -1.7(6) . . . . ? P1 C9 C10 C11 177.8(3) . . . . ? C9 C10 C11 C12 0.3(7) . . . . ? C10 C11 C12 C13 1.1(7) . . . . ? C11 C12 C13 C14 -1.0(7) . . . . ? C10 C9 C14 C13 1.7(6) . . . . ? P1 C9 C14 C13 -177.7(3) . . . . ? C12 C13 C14 C9 -0.4(7) . . . . ? C21 P2 C15 C20 -61.6(4) . . . . ? C1 P2 C15 C20 47.5(4) . . . . ? Pd1 P2 C15 C20 172.0(3) . . . . ? C21 P2 C15 C16 121.7(4) . . . . ? C1 P2 C15 C16 -129.2(4) . . . . ? Pd1 P2 C15 C16 -4.7(5) . . . . ? C20 C15 C16 C17 -0.8(8) . . . . ? P2 C15 C16 C17 175.9(4) . . . . ? C15 C16 C17 C18 0.1(9) . . . . ? C16 C17 C18 C19 1.4(10) . . . . ? C17 C18 C19 C20 -2.1(9) . . . . ? C16 C15 C20 C19 0.0(7) . . . . ? P2 C15 C20 C19 -176.8(4) . . . . ? C18 C19 C20 C15 1.4(8) . . . . ? C15 P2 C21 C26 170.6(3) . . . . ? C1 P2 C21 C26 63.2(4) . . . . ? Pd1 P2 C21 C26 -49.2(4) . . . . ? C15 P2 C21 C22 -7.9(4) . . . . ? C1 P2 C21 C22 -115.3(4) . . . . ? Pd1 P2 C21 C22 132.3(3) . . . . ? C26 C21 C22 C23 -2.7(7) . . . . ? P2 C21 C22 C23 175.8(3) . . . . ? C21 C22 C23 C24 0.6(7) . . . . ? C22 C23 C24 C25 2.2(8) . . . . ? C23 C24 C25 C26 -2.8(8) . . . . ? C22 C21 C26 C25 2.0(7) . . . . ? P2 C21 C26 C25 -176.5(4) . . . . ? C24 C25 C26 C21 0.7(7) . . . . ? S1 N1 C27 C36 -112.4(4) . . . . ? Pd1 N1 C27 C36 78.4(4) . . . . ? S1 N1 C27 C28 71.0(4) . . . . ? Pd1 N1 C27 C28 -98.2(4) . . . . ? C36 C27 C28 C29 1.4(6) . . . . ? N1 C27 C28 C29 178.0(4) . . . . ? C27 C28 C29 C30 -2.6(6) . . . . ? C28 C29 C30 C35 0.9(6) . . . . ? C28 C29 C30 C31 -179.9(4) . . . . ? C35 C30 C31 C32 -0.7(6) . . . . ? C29 C30 C31 C32 -179.8(4) . . . . ? C30 C31 C32 C33 -0.7(7) . . . . ? C31 C32 C33 C34 -0.5(7) . . . . ? C32 C33 C34 C35 3.3(7) . . . . ? C31 C30 C35 C34 3.4(6) . . . . ? C29 C30 C35 C34 -177.5(4) . . . . ? C31 C30 C35 C36 -177.3(4) . . . . ? C29 C30 C35 C36 1.8(6) . . . . ? C33 C34 C35 C30 -4.7(6) . . . . ? C33 C34 C35 C36 176.0(4) . . . . ? C28 C27 C36 C35 1.3(6) . . . . ? N1 C27 C36 C35 -175.3(3) . . . . ? C28 C27 C36 C37 -176.3(4) . . . . ? N1 C27 C36 C37 7.2(6) . . . . ? C30 C35 C36 C27 -2.9(6) . . . . ? C34 C35 C36 C27 176.4(4) . . . . ? C30 C35 C36 C37 174.6(4) . . . . ? C34 C35 C36 C37 -6.1(6) . . . . ? C27 C36 C37 C46 -62.9(5) . . . . ? C35 C36 C37 C46 119.6(4) . . . . ? C27 C36 C37 C38 114.2(4) . . . . ? C35 C36 C37 C38 -63.3(5) . . . . ? C46 C37 C38 C39 179.9(4) . . . . ? C36 C37 C38 C39 2.7(6) . . . . ? C46 C37 C38 C43 0.3(5) . . . . ? C36 C37 C38 C43 -176.8(3) . . . . ? C43 C38 C39 C40 0.0(6) . . . . ? C37 C38 C39 C40 -179.6(4) . . . . ? C38 C39 C40 C41 0.2(6) . . . . ? C39 C40 C41 C42 -0.7(7) . . . . ? C40 C41 C42 C43 0.9(7) . . . . ? C41 C42 C43 C44 177.9(4) . . . . ? C41 C42 C43 C38 -0.8(6) . . . . ? C39 C38 C43 C44 -178.4(4) . . . . ? C37 C38 C43 C44 1.2(6) . . . . ? C39 C38 C43 C42 0.3(6) . . . . ? C37 C38 C43 C42 179.9(4) . . . . ? C42 C43 C44 C45 179.8(4) . . . . ? C38 C43 C44 C45 -1.5(6) . . . . ? C43 C44 C45 C46 0.4(6) . . . . ? C38 C37 C46 C45 -1.5(6) . . . . ? C36 C37 C46 C45 175.7(3) . . . . ? C38 C37 C46 N2 -178.8(3) . . . . ? C36 C37 C46 N2 -1.6(5) . . . . ? C44 C45 C46 C37 1.1(6) . . . . ? C44 C45 C46 N2 178.6(3) . . . . ? S2 N2 C46 C37 -81.3(4) . . . . ? Pd1 N2 C46 C37 80.2(4) . . . . ? S2 N2 C46 C45 101.2(4) . . . . ? Pd1 N2 C46 C45 -97.3(4) . . . . ? O1 S1 C47 F2 176.8(3) . . . . ? O2 S1 C47 F2 53.1(4) . . . . ? N1 S1 C47 F2 -68.4(4) . . . . ? O1 S1 C47 F3 -61.5(3) . . . . ? O2 S1 C47 F3 174.8(3) . . . . ? N1 S1 C47 F3 53.3(4) . . . . ? O1 S1 C47 F1 57.4(4) . . . . ? O2 S1 C47 F1 -66.3(4) . . . . ? N1 S1 C47 F1 172.2(3) . . . . ? O3 S2 C48 F4 67.0(4) . . . . ? O4 S2 C48 F4 -56.0(4) . . . . ? N2 S2 C48 F4 -170.9(3) . . . . ? O3 S2 C48 F5 -172.1(3) . . . . ? O4 S2 C48 F5 64.9(4) . . . . ? N2 S2 C48 F5 -50.0(4) . . . . ? O3 S2 C48 F6 -52.5(4) . . . . ? O4 S2 C48 F6 -175.5(3) . . . . ? N2 S2 C48 F6 69.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.674 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.072 data_a _database_code_depnum_ccdc_archive 'CCDC 917452' #TrackingRef 'web_deposit_cif_file_0_YudongCai_1356445690.a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H32 N2 O4 Pd' _chemical_formula_sum 'C29 H32 N2 O4 Pd' _chemical_formula_weight 578.97 _chemical_absolute_configuration ad 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5931(19) _cell_length_b 12.862(3) _cell_length_c 11.787(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.40(3) _cell_angle_gamma 90.00 _cell_volume 1334.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4647 _cell_measurement_theta_min 1.5833 _cell_measurement_theta_max 27.4851 _exptl_crystal_description plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7825 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9952 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5613 _reflns_number_gt 5166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.9913P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 5613 _refine_ls_number_parameters 330 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.60693(4) 0.09787(4) 0.15102(3) 0.03053(10) Uani 1 1 d . . . O1 O 0.6725(4) 0.0208(3) 0.3171(3) 0.0310(8) Uani 1 1 d . . . O2 O 0.6276(4) 0.1597(3) 0.4103(4) 0.0307(9) Uani 1 1 d . . . O3 O 0.6340(3) 0.2280(3) 0.6156(3) 0.0321(8) Uani 1 1 d . . . H3 H 0.6356 0.2185 0.5456 0.038 Uiso 1 1 d R . . O4 O 0.7896(5) 0.3051(4) 0.7844(4) 0.0455(12) Uani 1 1 d . . . N1 N 0.8341(5) 0.1623(3) 0.1948(4) 0.0339(10) Uani 1 1 d . . . N2 N 0.5527(6) 0.1708(5) -0.0191(4) 0.0518(14) Uani 1 1 d . . . C1 C 0.9554(6) 0.0849(7) 0.2462(5) 0.0508(17) Uani 1 1 d . . . H1B H 0.9609 0.0621 0.3272 0.076 Uiso 1 1 calc R . . H1C H 1.0526 0.1159 0.2553 0.076 Uiso 1 1 calc R . . H1A H 0.9336 0.0250 0.1904 0.076 Uiso 1 1 calc R . . C2 C 0.8658(7) 0.2477(4) 0.2844(6) 0.0492(15) Uani 1 1 d . . . H2A H 0.7883 0.3019 0.2508 0.074 Uiso 1 1 calc R . . H2C H 0.9661 0.2771 0.3005 0.074 Uiso 1 1 calc R . . H2B H 0.8640 0.2212 0.3618 0.074 Uiso 1 1 calc R . . C3 C 0.8276(7) 0.1992(5) 0.0753(6) 0.0507(16) Uani 1 1 d . . . H3A H 0.8451 0.1402 0.0287 0.061 Uiso 1 1 calc R . . H3B H 0.9087 0.2512 0.0888 0.061 Uiso 1 1 calc R . . C4 C 0.6790(8) 0.2464(5) 0.0030(6) 0.0587(18) Uani 1 1 d . . . H4B H 0.6769 0.2707 -0.0774 0.070 Uiso 1 1 calc R . . H4A H 0.6640 0.3076 0.0478 0.070 Uiso 1 1 calc R . . C5 C 0.5530(7) 0.0922(10) -0.1111(5) 0.074(2) Uani 1 1 d . . . H5A H 0.4756 0.0394 -0.1204 0.111 Uiso 1 1 calc R . . H5C H 0.6531 0.0591 -0.0829 0.111 Uiso 1 1 calc R . . H5B H 0.5304 0.1262 -0.1909 0.111 Uiso 1 1 calc R . . C6 C 0.4087(7) 0.2288(6) -0.0679(6) 0.070(2) Uani 1 1 d . . . H6A H 0.3237 0.1804 -0.0857 0.106 Uiso 1 1 calc R . . H6C H 0.3987 0.2649 -0.1440 0.106 Uiso 1 1 calc R . . H6B H 0.4078 0.2799 -0.0064 0.106 Uiso 1 1 calc R . . C7 C 0.3953(6) 0.0405(5) 0.1054(6) 0.0558(18) Uani 1 1 d . . . H7A H 0.3303 0.0943 0.1177 0.084 Uiso 1 1 calc R . . H7C H 0.3996 -0.0195 0.1579 0.084 Uiso 1 1 calc R . . H7B H 0.3533 0.0189 0.0185 0.084 Uiso 1 1 calc R . . C8 C 0.6664(5) 0.0671(4) 0.4095(5) 0.0246(13) Uani 1 1 d . . . C9 C 0.7076(5) 0.0046(3) 0.5251(4) 0.0216(10) Uani 1 1 d . . . C10 C 0.6154(5) -0.0835(4) 0.5221(5) 0.0286(11) Uani 1 1 d . . . H10 H 0.5386 -0.1054 0.4459 0.034 Uiso 1 1 calc R . . C11 C 0.6374(5) -0.1363(4) 0.6282(5) 0.0271(11) Uani 1 1 d . . . H11 H 0.5743 -0.1941 0.6251 0.033 Uiso 1 1 calc R . . C12 C 0.7519(6) -0.1068(4) 0.7424(5) 0.0249(12) Uani 1 1 d . . . C13 C 0.7752(6) -0.1594(4) 0.8535(5) 0.0323(11) Uani 1 1 d . . . H13 H 0.7092 -0.2148 0.8525 0.039 Uiso 1 1 calc R . . C14 C 0.8892(6) -0.1329(4) 0.9611(5) 0.0381(13) Uani 1 1 d . . . H14 H 0.9024 -0.1694 1.0348 0.046 Uiso 1 1 calc R . . C15 C 0.9893(6) -0.0510(4) 0.9645(5) 0.0334(12) Uani 1 1 d . . . H15 H 1.0712 -0.0342 1.0402 0.040 Uiso 1 1 calc R . . C16 C 0.9693(5) 0.0039(4) 0.8607(4) 0.0276(11) Uani 1 1 d . . . H16 H 1.0356 0.0601 0.8654 0.033 Uiso 1 1 calc R . . C17 C 0.8509(5) -0.0214(4) 0.7455(5) 0.0243(10) Uani 1 1 d . . . C18 C 0.8244(5) 0.0343(3) 0.6345(4) 0.0224(10) Uani 1 1 d . . . C19 C 0.7722(6) 0.2546(4) 0.6946(5) 0.0283(11) Uani 1 1 d . . . C20 C 0.9035(5) 0.2226(4) 0.6631(4) 0.0238(10) Uani 1 1 d . . . C21 C 0.9263(5) 0.1228(3) 0.6346(4) 0.0218(11) Uani 1 1 d . . . C22 C 1.0582(4) 0.1022(6) 0.6085(3) 0.0228(8) Uani 1 1 d . . . C23 C 1.0961(6) -0.0017(4) 0.5843(5) 0.0300(13) Uani 1 1 d . . . H23 H 1.0328 -0.0583 0.5848 0.036 Uiso 1 1 calc R . . C24 C 1.2218(6) -0.0190(5) 0.5609(5) 0.0363(13) Uani 1 1 d . . . H24 H 1.2483 -0.0881 0.5489 0.044 Uiso 1 1 calc R . . C25 C 1.3118(6) 0.0633(5) 0.5544(6) 0.0406(17) Uani 1 1 d . . . H25 H 1.3953 0.0501 0.5323 0.049 Uiso 1 1 calc R . . C26 C 1.2833(6) 0.1608(5) 0.5786(5) 0.0353(14) Uani 1 1 d . . . H26 H 1.3493 0.2155 0.5775 0.042 Uiso 1 1 calc R . . C27 C 1.1547(5) 0.1830(4) 0.6059(5) 0.0251(12) Uani 1 1 d . . . C28 C 1.1248(5) 0.2846(4) 0.6368(4) 0.0298(11) Uani 1 1 d . . . H28 H 1.1902 0.3402 0.6371 0.036 Uiso 1 1 calc R . . C29 C 1.0034(5) 0.3035(4) 0.6660(4) 0.0266(10) Uani 1 1 d . . . H29 H 0.9862 0.3717 0.6886 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03491(17) 0.03245(18) 0.02349(17) -0.0002(2) 0.01082(13) -0.0006(2) O1 0.0362(19) 0.0287(18) 0.029(2) -0.0012(16) 0.0139(15) -0.0002(15) O2 0.039(2) 0.0240(19) 0.028(2) 0.0044(17) 0.0113(17) 0.0059(16) O3 0.0250(17) 0.037(2) 0.037(2) -0.0062(17) 0.0151(15) 0.0038(15) O4 0.040(2) 0.057(3) 0.042(3) -0.015(2) 0.019(2) -0.001(2) N1 0.040(2) 0.031(2) 0.038(3) 0.004(2) 0.022(2) -0.0025(19) N2 0.057(3) 0.069(4) 0.031(3) 0.007(3) 0.020(2) 0.021(3) C1 0.040(3) 0.058(5) 0.055(3) 0.019(4) 0.020(2) 0.018(4) C2 0.054(4) 0.037(3) 0.062(4) -0.009(3) 0.029(3) -0.007(3) C3 0.056(4) 0.049(4) 0.059(4) 0.018(3) 0.036(3) 0.006(3) C4 0.078(5) 0.057(4) 0.061(4) 0.024(4) 0.050(4) 0.016(4) C5 0.100(5) 0.083(5) 0.039(3) -0.003(6) 0.028(3) 0.022(7) C6 0.061(4) 0.102(6) 0.045(4) 0.035(4) 0.018(3) 0.042(4) C7 0.040(3) 0.060(4) 0.060(4) -0.013(3) 0.012(3) -0.007(3) C8 0.017(2) 0.028(3) 0.027(3) -0.001(2) 0.0065(19) -0.0025(18) C9 0.022(2) 0.018(2) 0.027(3) 0.0019(19) 0.0120(19) 0.0011(17) C10 0.029(2) 0.027(3) 0.031(3) -0.006(2) 0.014(2) -0.003(2) C11 0.026(2) 0.025(3) 0.036(3) 0.000(2) 0.018(2) -0.0021(19) C12 0.022(2) 0.025(3) 0.029(3) 0.001(2) 0.011(2) -0.002(2) C13 0.038(3) 0.031(3) 0.035(3) 0.005(2) 0.023(2) -0.003(2) C14 0.049(3) 0.036(3) 0.034(3) 0.013(3) 0.022(3) 0.005(3) C15 0.038(3) 0.037(3) 0.027(3) 0.003(2) 0.015(2) 0.004(2) C16 0.029(2) 0.029(3) 0.029(3) 0.000(2) 0.016(2) 0.000(2) C17 0.028(2) 0.018(2) 0.030(3) -0.001(2) 0.015(2) 0.0004(19) C18 0.018(2) 0.020(2) 0.030(3) 0.002(2) 0.0093(19) 0.0007(18) C19 0.032(3) 0.023(3) 0.035(3) 0.001(2) 0.019(2) -0.003(2) C20 0.023(2) 0.027(3) 0.020(2) 0.001(2) 0.0080(19) 0.0033(19) C21 0.025(2) 0.022(3) 0.017(2) 0.0024(17) 0.0060(16) -0.0026(17) C22 0.0214(17) 0.025(2) 0.0218(19) 0.009(3) 0.0081(14) 0.009(3) C23 0.027(3) 0.030(3) 0.033(3) -0.002(2) 0.012(2) -0.001(2) C24 0.031(3) 0.038(3) 0.042(3) 0.003(3) 0.016(3) 0.011(2) C25 0.027(3) 0.056(4) 0.045(4) 0.005(3) 0.020(2) 0.002(2) C26 0.030(3) 0.041(4) 0.040(3) 0.000(3) 0.019(3) -0.008(3) C27 0.022(3) 0.027(3) 0.022(3) 0.000(2) 0.004(2) -0.003(2) C28 0.026(2) 0.025(3) 0.034(3) 0.007(2) 0.007(2) -0.0080(19) C29 0.032(2) 0.015(2) 0.030(3) 0.000(2) 0.009(2) -0.0003(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C7 2.022(6) . ? Pd1 O1 2.057(3) . ? Pd1 N2 2.084(5) . ? Pd1 N1 2.193(4) . ? O1 C8 1.262(6) . ? O2 C8 1.249(6) . ? O3 C19 1.327(6) . ? O3 H3 0.8400 . ? O4 C19 1.195(6) . ? N1 C3 1.464(7) . ? N1 C1 1.467(7) . ? N1 C2 1.470(7) . ? N2 C6 1.471(7) . ? N2 C5 1.483(10) . ? N2 C4 1.494(8) . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1A 0.9800 . ? C2 H2A 0.9800 . ? C2 H2C 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.470(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 H5A 0.9800 . ? C5 H5C 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9800 . ? C6 H6C 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7C 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.494(7) . ? C9 C18 1.384(6) . ? C9 C10 1.430(6) . ? C10 C11 1.364(7) . ? C10 H10 0.9500 . ? C11 C12 1.410(7) . ? C11 H11 0.9500 . ? C12 C13 1.410(8) . ? C12 C17 1.444(7) . ? C13 C14 1.349(7) . ? C13 H13 0.9500 . ? C14 C15 1.415(7) . ? C14 H14 0.9500 . ? C15 C16 1.359(7) . ? C15 H15 0.9500 . ? C16 C17 1.420(7) . ? C16 H16 0.9500 . ? C17 C18 1.423(7) . ? C18 C21 1.500(6) . ? C19 C20 1.505(6) . ? C20 C21 1.366(6) . ? C20 C29 1.406(6) . ? C21 C22 1.440(5) . ? C22 C27 1.400(8) . ? C22 C23 1.443(9) . ? C23 C24 1.357(7) . ? C23 H23 0.9500 . ? C24 C25 1.387(7) . ? C24 H24 0.9500 . ? C25 C26 1.339(8) . ? C25 H25 0.9500 . ? C26 C27 1.422(7) . ? C26 H26 0.9500 . ? C27 C28 1.417(7) . ? C28 C29 1.361(7) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? 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 C7 Pd1 O1 88.4(2) . . ? C7 Pd1 N2 93.9(2) . . ? O1 Pd1 N2 176.06(18) . . ? C7 Pd1 N1 178.2(2) . . ? O1 Pd1 N1 93.37(15) . . ? N2 Pd1 N1 84.33(19) . . ? C8 O1 Pd1 119.5(3) . . ? C19 O3 H3 108.9 . . ? C3 N1 C1 110.0(4) . . ? C3 N1 C2 111.5(5) . . ? C1 N1 C2 107.8(5) . . ? C3 N1 Pd1 103.7(3) . . ? C1 N1 Pd1 113.1(4) . . ? C2 N1 Pd1 110.7(3) . . ? C6 N2 C5 109.5(5) . . ? C6 N2 C4 107.9(6) . . ? C5 N2 C4 109.5(5) . . ? C6 N2 Pd1 116.2(4) . . ? C5 N2 Pd1 108.9(5) . . ? C4 N2 Pd1 104.5(4) . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? H2C C2 H2B 109.5 . . ? N1 C3 C4 110.7(5) . . ? N1 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 N2 111.4(5) . . ? C3 C4 H4B 109.4 . . ? N2 C4 H4B 109.4 . . ? C3 C4 H4A 109.4 . . ? N2 C4 H4A 109.4 . . ? H4B C4 H4A 108.0 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? Pd1 C7 H7A 109.5 . . ? Pd1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? Pd1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? H7C C7 H7B 109.5 . . ? O2 C8 O1 124.9(6) . . ? O2 C8 C9 118.5(6) . . ? O1 C8 C9 116.6(4) . . ? C18 C9 C10 120.4(4) . . ? C18 C9 C8 121.6(4) . . ? C10 C9 C8 117.8(4) . . ? C11 C10 C9 120.2(5) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 121.3(5) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 122.3(5) . . ? C11 C12 C17 118.9(5) . . ? C13 C12 C17 118.8(5) . . ? C14 C13 C12 121.5(5) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.6(5) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 121.1(5) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C18 123.2(4) . . ? C16 C17 C12 117.8(4) . . ? C18 C17 C12 119.0(4) . . ? C9 C18 C17 120.0(4) . . ? C9 C18 C21 119.8(4) . . ? C17 C18 C21 120.2(4) . . ? O4 C19 O3 120.8(5) . . ? O4 C19 C20 122.0(5) . . ? O3 C19 C20 117.2(4) . . ? C21 C20 C29 121.8(4) . . ? C21 C20 C19 123.3(4) . . ? C29 C20 C19 114.9(4) . . ? C20 C21 C22 117.8(5) . . ? C20 C21 C18 123.0(4) . . ? C22 C21 C18 119.2(4) . . ? C27 C22 C21 120.8(6) . . ? C27 C22 C23 117.5(4) . . ? C21 C22 C23 121.6(5) . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.5(6) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 121.3(5) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 120.3(5) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C22 C27 C28 118.4(5) . . ? C22 C27 C26 119.8(5) . . ? C28 C27 C26 121.7(5) . . ? C29 C28 C27 120.7(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C20 120.4(4) . . ? C28 C29 H29 119.8 . . ? C20 C29 H29 119.8 . . ? 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 C7 Pd1 O1 C8 -92.0(4) . . . . ? N2 Pd1 O1 C8 142(3) . . . . ? N1 Pd1 O1 C8 88.1(3) . . . . ? C7 Pd1 N1 C3 -12(8) . . . . ? O1 Pd1 N1 C3 165.3(3) . . . . ? N2 Pd1 N1 C3 -11.5(4) . . . . ? C7 Pd1 N1 C1 -131(7) . . . . ? O1 Pd1 N1 C1 46.2(4) . . . . ? N2 Pd1 N1 C1 -130.6(4) . . . . ? C7 Pd1 N1 C2 108(8) . . . . ? O1 Pd1 N1 C2 -74.9(4) . . . . ? N2 Pd1 N1 C2 108.3(4) . . . . ? C7 Pd1 N2 C6 44.7(6) . . . . ? O1 Pd1 N2 C6 170(3) . . . . ? N1 Pd1 N2 C6 -135.3(5) . . . . ? C7 Pd1 N2 C5 -79.5(4) . . . . ? O1 Pd1 N2 C5 46(3) . . . . ? N1 Pd1 N2 C5 100.5(4) . . . . ? C7 Pd1 N2 C4 163.5(4) . . . . ? O1 Pd1 N2 C4 -71(3) . . . . ? N1 Pd1 N2 C4 -16.5(4) . . . . ? C1 N1 C3 C4 160.0(6) . . . . ? C2 N1 C3 C4 -80.4(6) . . . . ? Pd1 N1 C3 C4 38.8(6) . . . . ? N1 C3 C4 N2 -58.9(7) . . . . ? C6 N2 C4 C3 168.2(5) . . . . ? C5 N2 C4 C3 -72.6(7) . . . . ? Pd1 N2 C4 C3 44.0(6) . . . . ? Pd1 O1 C8 O2 -2.5(7) . . . . ? Pd1 O1 C8 C9 176.8(3) . . . . ? O2 C8 C9 C18 -58.9(7) . . . . ? O1 C8 C9 C18 121.8(5) . . . . ? O2 C8 C9 C10 116.8(5) . . . . ? O1 C8 C9 C10 -62.5(6) . . . . ? C18 C9 C10 C11 3.1(7) . . . . ? C8 C9 C10 C11 -172.7(4) . . . . ? C9 C10 C11 C12 -1.0(7) . . . . ? C10 C11 C12 C13 179.2(5) . . . . ? C10 C11 C12 C17 -2.3(7) . . . . ? C11 C12 C13 C14 177.2(5) . . . . ? C17 C12 C13 C14 -1.3(8) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C13 C14 C15 C16 2.0(8) . . . . ? C14 C15 C16 C17 -2.0(8) . . . . ? C15 C16 C17 C18 179.4(5) . . . . ? C15 C16 C17 C12 0.4(7) . . . . ? C11 C12 C17 C16 -177.4(5) . . . . ? C13 C12 C17 C16 1.2(7) . . . . ? C11 C12 C17 C18 3.6(7) . . . . ? C13 C12 C17 C18 -177.8(5) . . . . ? C10 C9 C18 C17 -1.7(7) . . . . ? C8 C9 C18 C17 173.9(4) . . . . ? C10 C9 C18 C21 176.2(4) . . . . ? C8 C9 C18 C21 -8.2(7) . . . . ? C16 C17 C18 C9 179.4(4) . . . . ? C12 C17 C18 C9 -1.7(7) . . . . ? C16 C17 C18 C21 1.6(7) . . . . ? C12 C17 C18 C21 -179.5(4) . . . . ? O4 C19 C20 C21 130.1(6) . . . . ? O3 C19 C20 C21 -52.4(7) . . . . ? O4 C19 C20 C29 -49.4(7) . . . . ? O3 C19 C20 C29 128.1(5) . . . . ? C29 C20 C21 C22 0.6(7) . . . . ? C19 C20 C21 C22 -178.9(4) . . . . ? C29 C20 C21 C18 178.1(4) . . . . ? C19 C20 C21 C18 -1.4(7) . . . . ? C9 C18 C21 C20 95.3(5) . . . . ? C17 C18 C21 C20 -86.9(6) . . . . ? C9 C18 C21 C22 -87.2(5) . . . . ? C17 C18 C21 C22 90.6(5) . . . . ? C20 C21 C22 C27 -3.4(6) . . . . ? C18 C21 C22 C27 179.0(4) . . . . ? C20 C21 C22 C23 176.5(4) . . . . ? C18 C21 C22 C23 -1.1(6) . . . . ? C27 C22 C23 C24 0.4(7) . . . . ? C21 C22 C23 C24 -179.5(5) . . . . ? C22 C23 C24 C25 -2.9(9) . . . . ? C23 C24 C25 C26 4.3(10) . . . . ? C24 C25 C26 C27 -3.1(11) . . . . ? C21 C22 C27 C28 3.7(7) . . . . ? C23 C22 C27 C28 -176.2(5) . . . . ? C21 C22 C27 C26 -179.3(5) . . . . ? C23 C22 C27 C26 0.7(7) . . . . ? C25 C26 C27 C22 0.6(9) . . . . ? C25 C26 C27 C28 177.4(6) . . . . ? C22 C27 C28 C29 -1.2(7) . . . . ? C26 C27 C28 C29 -178.1(5) . . . . ? C27 C28 C29 C20 -1.6(8) . . . . ? C21 C20 C29 C28 1.9(7) . . . . ? C19 C20 C29 C28 -178.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.84 1.74 2.552(5) 162.2 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.650 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.080 data_a _database_code_depnum_ccdc_archive 'CCDC 917453' #TrackingRef 'web_deposit_cif_file_0_YudongCai_1356446052.a1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H50 Cl2 Fe O4 P2 Pd Si' _chemical_formula_weight 978.03 _chemical_absolute_configuration ad 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.5186(13) _cell_length_b 17.3401(18) _cell_length_c 20.879(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4532.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18116 _cell_measurement_theta_min 1.5266 _cell_measurement_theta_max 27.4816 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6506 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20337 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10348 _reflns_number_gt 9856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.7826P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(17) _refine_ls_number_reflns 10348 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.59035(2) 0.388609(14) 0.787443(11) 0.02162(7) Uani 1 1 d . . . Fe1 Fe 0.81210(4) 0.28625(3) 0.55556(2) 0.02780(12) Uani 1 1 d . . . Cl1 Cl 0.1200(2) 0.42029(17) 0.62746(19) 0.1845(16) Uani 1 1 d . . . Cl2 Cl 0.2185(2) 0.47203(17) 0.51237(10) 0.1337(10) Uani 1 1 d . . . P1 P 0.61790(8) 0.51273(5) 0.74694(4) 0.0262(2) Uani 1 1 d . . . P2 P 0.45120(8) 0.40362(5) 0.85060(4) 0.02529(19) Uani 1 1 d . . . Si1 Si 0.72041(9) 0.25695(6) 0.86617(5) 0.0315(2) Uani 1 1 d . . . O1 O 0.5976(2) 0.28590(16) 0.67433(11) 0.0305(5) Uani 1 1 d . . . O2 O 0.7194(2) 0.35334(15) 0.72779(11) 0.0270(5) Uani 1 1 d . . . O3 O 0.8888(3) 0.18818(18) 0.40270(15) 0.0491(8) Uani 1 1 d . . . O4 O 0.9986(2) 0.28999(17) 0.41037(13) 0.0369(6) Uani 1 1 d . . . H4 H 1.0310 0.2562 0.3890 0.044 Uiso 1 1 d R . . C1 C 0.6011(3) 0.5258(2) 0.66097(17) 0.0299(8) Uani 1 1 d . . . C2 C 0.5404(3) 0.4732(2) 0.62703(18) 0.0305(8) Uani 1 1 d . . . H2 H 0.5136 0.4285 0.6479 0.037 Uiso 1 1 calc R . . C3 C 0.5182(3) 0.4853(3) 0.56246(19) 0.0373(9) Uani 1 1 d . . . H3 H 0.4754 0.4494 0.5396 0.045 Uiso 1 1 calc R . . C4 C 0.5584(4) 0.5491(3) 0.5318(2) 0.0452(11) Uani 1 1 d . . . H4A H 0.5428 0.5573 0.4878 0.054 Uiso 1 1 calc R . . C5 C 0.6213(4) 0.6014(3) 0.5645(2) 0.0515(12) Uani 1 1 d . . . H5 H 0.6504 0.6446 0.5426 0.062 Uiso 1 1 calc R . . C6 C 0.6420(4) 0.5908(2) 0.6293(2) 0.0423(10) Uani 1 1 d . . . H6 H 0.6837 0.6275 0.6521 0.051 Uiso 1 1 calc R . . C7 C 0.7561(3) 0.5377(2) 0.76422(19) 0.0326(8) Uani 1 1 d . . . C8 C 0.8375(3) 0.5237(3) 0.7215(2) 0.0454(11) Uani 1 1 d . . . H8 H 0.8213 0.5018 0.6809 0.055 Uiso 1 1 calc R . . C9 C 0.9437(4) 0.5409(4) 0.7367(3) 0.0653(16) Uani 1 1 d . . . H9 H 0.9988 0.5316 0.7064 0.078 Uiso 1 1 calc R . . C10 C 0.9679(4) 0.5713(3) 0.7957(3) 0.0647(15) Uani 1 1 d . . . H10 H 1.0396 0.5838 0.8062 0.078 Uiso 1 1 calc R . . C11 C 0.8872(4) 0.5835(3) 0.8398(2) 0.0574(13) Uani 1 1 d . . . H11 H 0.9041 0.6034 0.8809 0.069 Uiso 1 1 calc R . . C12 C 0.7822(4) 0.5670(3) 0.8246(2) 0.0433(10) Uani 1 1 d . . . H12 H 0.7275 0.5755 0.8553 0.052 Uiso 1 1 calc R . . C13 C 0.5450(3) 0.5966(2) 0.77792(19) 0.0351(9) Uani 1 1 d . . . H13B H 0.5538 0.5984 0.8250 0.042 Uiso 1 1 calc R . . H13A H 0.5778 0.6440 0.7601 0.042 Uiso 1 1 calc R . . C14 C 0.4253(3) 0.5975(2) 0.76246(19) 0.0360(9) Uani 1 1 d . . . H14B H 0.3926 0.6425 0.7841 0.043 Uiso 1 1 calc R . . H14A H 0.4166 0.6050 0.7157 0.043 Uiso 1 1 calc R . . C15 C 0.3636(3) 0.5256(2) 0.7819(2) 0.0352(8) Uani 1 1 d . . . H15A H 0.3817 0.4833 0.7519 0.042 Uiso 1 1 calc R . . H15B H 0.2862 0.5361 0.7776 0.042 Uiso 1 1 calc R . . C16 C 0.3865(3) 0.4986(2) 0.85065(18) 0.0331(8) Uani 1 1 d . . . H16A H 0.3186 0.4957 0.8749 0.040 Uiso 1 1 calc R . . H16B H 0.4334 0.5365 0.8722 0.040 Uiso 1 1 calc R . . C17 C 0.4807(3) 0.3867(2) 0.93489(16) 0.0289(7) Uani 1 1 d . . . C18 C 0.5491(4) 0.4388(3) 0.96459(19) 0.0401(10) Uani 1 1 d . . . H18 H 0.5745 0.4822 0.9414 0.048 Uiso 1 1 calc R . . C19 C 0.5807(4) 0.4282(3) 1.0275(2) 0.0501(12) Uani 1 1 d . . . H19 H 0.6263 0.4647 1.0475 0.060 Uiso 1 1 calc R . . C20 C 0.5465(4) 0.3653(3) 1.0608(2) 0.0465(11) Uani 1 1 d . . . H20 H 0.5682 0.3580 1.1039 0.056 Uiso 1 1 calc R . . C21 C 0.4806(4) 0.3126(3) 1.0318(2) 0.0512(13) Uani 1 1 d . . . H21 H 0.4577 0.2684 1.0550 0.061 Uiso 1 1 calc R . . C22 C 0.4467(4) 0.3231(3) 0.96872(19) 0.0395(10) Uani 1 1 d . . . H22 H 0.4005 0.2866 0.9492 0.047 Uiso 1 1 calc R . . C23 C 0.3384(3) 0.3437(2) 0.82738(18) 0.0306(8) Uani 1 1 d . . . C24 C 0.2452(3) 0.3406(3) 0.8646(2) 0.0446(11) Uani 1 1 d . . . H24 H 0.2429 0.3655 0.9051 0.054 Uiso 1 1 calc R . . C25 C 0.1571(4) 0.3014(3) 0.8422(3) 0.0600(14) Uani 1 1 d . . . H25 H 0.0945 0.2992 0.8679 0.072 Uiso 1 1 calc R . . C26 C 0.1576(4) 0.2658(3) 0.7839(3) 0.0577(13) Uani 1 1 d . . . H26 H 0.0961 0.2390 0.7694 0.069 Uiso 1 1 calc R . . C27 C 0.2489(4) 0.2689(3) 0.7460(2) 0.0480(11) Uani 1 1 d . . . H27 H 0.2498 0.2446 0.7052 0.058 Uiso 1 1 calc R . . C28 C 0.3388(3) 0.3078(2) 0.76821(19) 0.0338(9) Uani 1 1 d . . . H28 H 0.4013 0.3097 0.7424 0.041 Uiso 1 1 calc R . . C29 C 0.5905(3) 0.27702(19) 0.82647(15) 0.0257(7) Uani 1 1 d . . . H29B H 0.5319 0.2722 0.8581 0.031 Uiso 1 1 calc R . . H29A H 0.5781 0.2388 0.7921 0.031 Uiso 1 1 calc R . . C30 C 0.6913(4) 0.2002(4) 0.9399(3) 0.077(2) Uani 1 1 d . . . H30C H 0.7579 0.1787 0.9569 0.115 Uiso 1 1 calc R . . H30A H 0.6419 0.1582 0.9296 0.115 Uiso 1 1 calc R . . H30B H 0.6588 0.2339 0.9721 0.115 Uiso 1 1 calc R . . C31 C 0.8111(4) 0.1984(3) 0.8144(2) 0.0459(11) Uani 1 1 d . . . H31B H 0.8342 0.2295 0.7777 0.069 Uiso 1 1 calc R . . H31A H 0.7730 0.1527 0.7990 0.069 Uiso 1 1 calc R . . H31C H 0.8737 0.1824 0.8392 0.069 Uiso 1 1 calc R . . C32 C 0.7937(4) 0.3460(3) 0.8884(3) 0.0593(15) Uani 1 1 d . . . H32A H 0.8061 0.3773 0.8500 0.089 Uiso 1 1 calc R . . H32C H 0.8625 0.3322 0.9077 0.089 Uiso 1 1 calc R . . H32B H 0.7514 0.3756 0.9193 0.089 Uiso 1 1 calc R . . C33 C 0.6926(3) 0.3040(2) 0.68586(15) 0.0234(7) Uani 1 1 d . . . C34 C 0.7807(3) 0.2661(2) 0.64977(16) 0.0283(8) Uani 1 1 d . . . C35 C 0.8862(3) 0.2951(3) 0.64314(19) 0.0398(10) Uani 1 1 d . . . H35 H 0.9135 0.3408 0.6622 0.048 Uiso 1 1 calc R . . C36 C 0.9431(4) 0.2440(3) 0.6033(2) 0.0459(12) Uani 1 1 d . . . H36 H 1.0157 0.2493 0.5908 0.055 Uiso 1 1 calc R . . C37 C 0.8739(4) 0.1835(3) 0.58500(19) 0.0420(11) Uani 1 1 d . . . H37 H 0.8921 0.1411 0.5583 0.050 Uiso 1 1 calc R . . C38 C 0.7734(4) 0.1968(2) 0.61324(18) 0.0346(9) Uani 1 1 d . . . H38 H 0.7118 0.1652 0.6088 0.042 Uiso 1 1 calc R . . C39 C 0.9085(3) 0.2529(2) 0.42167(17) 0.0318(8) Uani 1 1 d . . . C40 C 0.8326(3) 0.2987(2) 0.45964(16) 0.0308(8) Uani 1 1 d . . . C41 C 0.8522(3) 0.3696(2) 0.49152(19) 0.0355(9) Uani 1 1 d . . . H41 H 0.9174 0.3976 0.4912 0.043 Uiso 1 1 calc R . . C42 C 0.7570(3) 0.3910(2) 0.5240(2) 0.0373(9) Uani 1 1 d . . . H42 H 0.7472 0.4363 0.5489 0.045 Uiso 1 1 calc R . . C43 C 0.6787(3) 0.3329(2) 0.51265(19) 0.0361(9) Uani 1 1 d . . . H43 H 0.6077 0.3327 0.5286 0.043 Uiso 1 1 calc R . . C44 C 0.7253(3) 0.2759(2) 0.47356(18) 0.0338(9) Uani 1 1 d . . . H44 H 0.6914 0.2302 0.4590 0.041 Uiso 1 1 calc R . . C45 C 0.2326(5) 0.4586(4) 0.5937(3) 0.0773(18) Uani 1 1 d . . . H45A H 0.2937 0.4236 0.6017 0.093 Uiso 1 1 calc R . . H45B H 0.2486 0.5087 0.6142 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02627(12) 0.01939(11) 0.01921(11) -0.00146(10) 0.00215(10) -0.00031(11) Fe1 0.0302(3) 0.0282(3) 0.0250(2) -0.0002(2) 0.0054(2) 0.0056(2) Cl1 0.134(2) 0.127(2) 0.293(4) 0.058(2) 0.130(3) 0.0348(17) Cl2 0.150(2) 0.165(2) 0.0863(13) 0.0115(14) -0.0333(14) 0.0589(19) P1 0.0349(5) 0.0200(4) 0.0238(4) -0.0007(3) 0.0056(4) -0.0038(4) P2 0.0306(4) 0.0226(5) 0.0227(4) 0.0008(3) 0.0059(4) 0.0002(4) Si1 0.0353(6) 0.0325(6) 0.0267(5) 0.0024(4) -0.0020(4) 0.0057(5) O1 0.0290(13) 0.0389(14) 0.0237(11) -0.0075(11) -0.0004(11) -0.0029(13) O2 0.0291(12) 0.0291(13) 0.0226(12) -0.0049(10) 0.0036(10) -0.0014(11) O3 0.055(2) 0.0405(17) 0.0513(18) -0.0157(14) 0.0189(16) -0.0086(15) O4 0.0399(15) 0.0365(15) 0.0343(14) -0.0097(12) 0.0091(13) 0.0038(13) C1 0.038(2) 0.0240(17) 0.0279(17) 0.0016(14) 0.0032(17) 0.0017(17) C2 0.0352(19) 0.0252(18) 0.0311(19) 0.0026(15) 0.0053(16) 0.0000(16) C3 0.038(2) 0.043(2) 0.031(2) -0.0018(18) -0.0018(17) 0.0050(19) C4 0.060(3) 0.050(3) 0.0253(19) 0.0052(18) -0.0015(19) 0.014(2) C5 0.079(3) 0.037(2) 0.039(2) 0.013(2) 0.014(2) 0.005(2) C6 0.060(3) 0.031(2) 0.037(2) 0.0009(17) 0.012(2) -0.007(2) C7 0.035(2) 0.0277(19) 0.035(2) -0.0026(16) 0.0025(16) -0.0035(16) C8 0.043(2) 0.051(3) 0.042(2) -0.012(2) 0.005(2) -0.010(2) C9 0.041(3) 0.085(4) 0.069(4) -0.013(3) 0.007(2) -0.008(3) C10 0.038(2) 0.076(4) 0.080(4) -0.013(3) -0.012(3) -0.010(3) C11 0.057(3) 0.063(3) 0.052(3) -0.016(2) -0.012(2) -0.013(3) C12 0.048(3) 0.046(3) 0.037(2) -0.007(2) 0.000(2) -0.008(2) C13 0.049(2) 0.0226(18) 0.033(2) 0.0022(15) 0.0083(18) -0.0022(16) C14 0.050(2) 0.0225(18) 0.0351(19) 0.0062(15) 0.0072(18) 0.0074(17) C15 0.037(2) 0.0256(18) 0.043(2) 0.0036(18) 0.0026(19) 0.0065(16) C16 0.038(2) 0.0308(19) 0.0302(18) 0.0053(16) 0.0097(16) 0.0041(16) C17 0.0392(19) 0.0264(17) 0.0212(16) -0.0021(15) 0.0101(14) -0.0013(17) C18 0.057(3) 0.032(2) 0.031(2) -0.0005(17) -0.0019(19) -0.009(2) C19 0.071(3) 0.042(2) 0.037(2) -0.0032(19) -0.010(2) -0.017(3) C20 0.060(3) 0.052(3) 0.0266(19) 0.0045(19) -0.003(2) -0.003(2) C21 0.065(3) 0.058(3) 0.031(2) 0.018(2) 0.000(2) -0.016(3) C22 0.046(2) 0.042(2) 0.030(2) 0.0072(18) -0.0005(18) -0.0146(19) C23 0.0328(19) 0.0281(19) 0.0308(19) 0.0069(15) 0.0040(16) 0.0031(16) C24 0.033(2) 0.058(3) 0.042(2) 0.002(2) 0.0062(19) -0.004(2) C25 0.039(3) 0.067(4) 0.075(4) 0.007(3) 0.009(3) -0.009(2) C26 0.041(2) 0.058(3) 0.075(3) 0.004(3) -0.013(3) -0.015(2) C27 0.049(3) 0.041(2) 0.054(3) -0.004(2) -0.014(2) -0.006(2) C28 0.0309(19) 0.031(2) 0.040(2) 0.0028(16) -0.0042(16) 0.0011(16) C29 0.0369(18) 0.0186(15) 0.0217(15) -0.0007(12) -0.0018(16) 0.0001(16) C30 0.051(3) 0.119(5) 0.060(3) 0.056(4) 0.002(3) 0.013(3) C31 0.039(2) 0.055(3) 0.044(2) -0.007(2) -0.009(2) 0.015(2) C32 0.060(3) 0.046(3) 0.072(3) -0.017(3) -0.038(3) 0.009(2) C33 0.0303(18) 0.0238(17) 0.0160(14) -0.0011(13) 0.0014(14) 0.0023(15) C34 0.0346(19) 0.0318(19) 0.0185(16) -0.0005(14) 0.0026(15) 0.0055(16) C35 0.033(2) 0.055(3) 0.032(2) -0.0073(19) -0.0038(17) 0.0033(19) C36 0.036(2) 0.070(3) 0.032(2) 0.000(2) 0.0035(18) 0.019(2) C37 0.055(3) 0.042(2) 0.029(2) 0.0040(18) 0.0104(19) 0.027(2) C38 0.049(2) 0.028(2) 0.0268(18) 0.0028(15) 0.0091(18) 0.0074(18) C39 0.037(2) 0.0340(19) 0.0244(17) 0.0031(15) -0.0012(17) -0.0009(19) C40 0.040(2) 0.032(2) 0.0206(17) 0.0061(15) 0.0055(15) 0.0059(17) C41 0.043(2) 0.0225(18) 0.041(2) 0.0048(16) 0.0127(18) 0.0025(16) C42 0.045(2) 0.0236(18) 0.043(2) 0.0008(18) 0.0117(18) 0.0078(19) C43 0.032(2) 0.039(2) 0.037(2) 0.0086(18) 0.0026(17) 0.0100(18) C44 0.0296(19) 0.040(2) 0.0323(19) 0.0037(17) -0.0011(16) 0.0044(17) C45 0.069(4) 0.076(4) 0.086(4) 0.002(4) 0.000(4) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C29 2.100(3) . ? Pd1 O2 2.129(2) . ? Pd1 P2 2.2003(9) . ? Pd1 P1 2.3381(10) . ? Fe1 C38 2.023(4) . ? Fe1 C40 2.031(3) . ? Fe1 C41 2.031(4) . ? Fe1 C44 2.035(4) . ? Fe1 C34 2.036(3) . ? Fe1 C37 2.038(4) . ? Fe1 C42 2.052(4) . ? Fe1 C36 2.055(4) . ? Fe1 C35 2.056(4) . ? Fe1 C43 2.060(4) . ? Cl1 C45 1.711(7) . ? Cl2 C45 1.723(7) . ? P1 C7 1.820(4) . ? P1 C1 1.821(4) . ? P1 C13 1.835(4) . ? P2 C23 1.820(4) . ? P2 C17 1.822(4) . ? P2 C16 1.836(4) . ? Si1 C32 1.856(5) . ? Si1 C29 1.858(4) . ? Si1 C30 1.864(5) . ? Si1 C31 1.868(4) . ? O1 C33 1.253(4) . ? O2 C33 1.269(4) . ? O3 C39 1.216(5) . ? O4 C39 1.319(5) . ? O4 H4 0.8399 . ? C1 C2 1.384(5) . ? C1 C6 1.403(5) . ? C2 C3 1.392(5) . ? C2 H2 0.9500 . ? C3 C4 1.374(6) . ? C3 H3 0.9500 . ? C4 C5 1.381(7) . ? C4 H4A 0.9500 . ? C5 C6 1.391(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.376(6) . ? C7 C12 1.397(6) . ? C8 C9 1.399(7) . ? C8 H8 0.9500 . ? C9 C10 1.374(8) . ? C9 H9 0.9500 . ? C10 C11 1.381(8) . ? C10 H10 0.9500 . ? C11 C12 1.383(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.533(6) . ? C13 H13B 0.9900 . ? C13 H13A 0.9900 . ? C14 C15 1.522(5) . ? C14 H14B 0.9900 . ? C14 H14A 0.9900 . ? C15 C16 1.537(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.378(5) . ? C17 C18 1.390(6) . ? C18 C19 1.384(6) . ? C18 H18 0.9500 . ? C19 C20 1.362(6) . ? C19 H19 0.9500 . ? C20 C21 1.371(7) . ? C20 H20 0.9500 . ? C21 C22 1.396(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.383(5) . ? C23 C24 1.402(6) . ? C24 C25 1.378(7) . ? C24 H24 0.9500 . ? C25 C26 1.365(8) . ? C25 H25 0.9500 . ? C26 C27 1.391(7) . ? C26 H26 0.9500 . ? C27 C28 1.392(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29B 0.9900 . ? C29 H29A 0.9900 . ? C30 H30C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 H31B 0.9800 . ? C31 H31A 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32C 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.489(5) . ? C34 C35 1.419(6) . ? C34 C38 1.427(5) . ? C35 C36 1.410(6) . ? C35 H35 0.9500 . ? C36 C37 1.413(7) . ? C36 H36 0.9500 . ? C37 C38 1.409(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.470(5) . ? C40 C41 1.419(5) . ? C40 C44 1.430(5) . ? C41 C42 1.421(5) . ? C41 H41 0.9500 . ? C42 C43 1.425(6) . ? C42 H42 0.9500 . ? C43 C44 1.408(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? 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 C29 Pd1 O2 87.80(12) . . ? C29 Pd1 P2 82.95(11) . . ? O2 Pd1 P2 170.09(7) . . ? C29 Pd1 P1 171.35(11) . . ? O2 Pd1 P1 86.61(7) . . ? P2 Pd1 P1 102.98(3) . . ? C38 Fe1 C40 134.35(16) . . ? C38 Fe1 C41 175.16(16) . . ? C40 Fe1 C41 40.88(16) . . ? C38 Fe1 C44 107.78(17) . . ? C40 Fe1 C44 41.17(16) . . ? C41 Fe1 C44 68.96(17) . . ? C38 Fe1 C34 41.17(15) . . ? C40 Fe1 C34 174.55(17) . . ? C41 Fe1 C34 143.65(16) . . ? C44 Fe1 C34 134.00(16) . . ? C38 Fe1 C37 40.60(17) . . ? C40 Fe1 C37 110.04(16) . . ? C41 Fe1 C37 136.59(17) . . ? C44 Fe1 C37 112.29(18) . . ? C34 Fe1 C37 68.41(15) . . ? C38 Fe1 C42 142.17(16) . . ? C40 Fe1 C42 68.36(16) . . ? C41 Fe1 C42 40.72(15) . . ? C44 Fe1 C42 68.18(17) . . ? C34 Fe1 C42 113.41(15) . . ? C37 Fe1 C42 177.19(18) . . ? C38 Fe1 C36 68.21(19) . . ? C40 Fe1 C36 114.54(16) . . ? C41 Fe1 C36 112.06(19) . . ? C44 Fe1 C36 143.37(17) . . ? C34 Fe1 C36 67.93(16) . . ? C37 Fe1 C36 40.39(19) . . ? C42 Fe1 C36 137.8(2) . . ? C38 Fe1 C35 68.63(18) . . ? C40 Fe1 C35 144.32(17) . . ? C41 Fe1 C35 114.89(19) . . ? C44 Fe1 C35 174.46(16) . . ? C34 Fe1 C35 40.57(16) . . ? C37 Fe1 C35 68.01(19) . . ? C42 Fe1 C35 111.81(18) . . ? C36 Fe1 C35 40.11(17) . . ? C38 Fe1 C43 111.46(18) . . ? C40 Fe1 C43 68.39(16) . . ? C41 Fe1 C43 68.60(17) . . ? C44 Fe1 C43 40.21(16) . . ? C34 Fe1 C43 109.34(16) . . ? C37 Fe1 C43 141.47(19) . . ? C42 Fe1 C43 40.56(17) . . ? C36 Fe1 C43 176.42(18) . . ? C35 Fe1 C43 136.31(17) . . ? C7 P1 C1 105.97(19) . . ? C7 P1 C13 102.36(19) . . ? C1 P1 C13 101.03(18) . . ? C7 P1 Pd1 106.73(13) . . ? C1 P1 Pd1 117.01(12) . . ? C13 P1 Pd1 121.93(13) . . ? C23 P2 C17 108.85(17) . . ? C23 P2 C16 99.79(19) . . ? C17 P2 C16 103.48(17) . . ? C23 P2 Pd1 112.79(13) . . ? C17 P2 Pd1 113.54(13) . . ? C16 P2 Pd1 117.13(12) . . ? C32 Si1 C29 112.88(19) . . ? C32 Si1 C30 109.2(3) . . ? C29 Si1 C30 107.2(2) . . ? C32 Si1 C31 107.2(2) . . ? C29 Si1 C31 112.05(18) . . ? C30 Si1 C31 108.1(3) . . ? C33 O2 Pd1 113.4(2) . . ? C39 O4 H4 99.7 . . ? C2 C1 C6 119.3(4) . . ? C2 C1 P1 119.1(3) . . ? C6 C1 P1 121.5(3) . . ? C1 C2 C3 120.4(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 119.7(4) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C8 C7 C12 118.4(4) . . ? C8 C7 P1 122.2(3) . . ? C12 C7 P1 119.2(3) . . ? C7 C8 C9 121.2(4) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 119.7(5) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 119.6(5) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 120.7(5) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 120.3(4) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 P1 114.8(3) . . ? C14 C13 H13B 108.6 . . ? P1 C13 H13B 108.6 . . ? C14 C13 H13A 108.6 . . ? P1 C13 H13A 108.6 . . ? H13B C13 H13A 107.5 . . ? C15 C14 C13 115.6(3) . . ? C15 C14 H14B 108.4 . . ? C13 C14 H14B 108.4 . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14A 108.4 . . ? H14B C14 H14A 107.4 . . ? C14 C15 C16 113.8(3) . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C15 C16 P2 110.8(3) . . ? C15 C16 H16A 109.5 . . ? P2 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? P2 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C22 C17 C18 118.8(4) . . ? C22 C17 P2 124.2(3) . . ? C18 C17 P2 116.9(3) . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.1(4) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 119.9(4) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 120.7(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C17 C22 C21 119.7(4) . . ? C17 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C28 C23 C24 118.8(4) . . ? C28 C23 P2 119.5(3) . . ? C24 C23 P2 121.3(3) . . ? C25 C24 C23 119.8(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 121.4(5) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 119.6(4) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 119.6(5) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C23 C28 C27 120.8(4) . . ? C23 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? Si1 C29 Pd1 110.28(18) . . ? Si1 C29 H29B 109.6 . . ? Pd1 C29 H29B 109.6 . . ? Si1 C29 H29A 109.6 . . ? Pd1 C29 H29A 109.6 . . ? H29B C29 H29A 108.1 . . ? Si1 C30 H30C 109.5 . . ? Si1 C30 H30A 109.5 . . ? H30C C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C31 H31B 109.5 . . ? Si1 C31 H31A 109.5 . . ? H31B C31 H31A 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? O1 C33 O2 123.5(3) . . ? O1 C33 C34 119.7(3) . . ? O2 C33 C34 116.8(3) . . ? C35 C34 C38 107.8(3) . . ? C35 C34 C33 125.7(4) . . ? C38 C34 C33 126.5(4) . . ? C35 C34 Fe1 70.5(2) . . ? C38 C34 Fe1 68.9(2) . . ? C33 C34 Fe1 123.8(2) . . ? C36 C35 C34 107.8(4) . . ? C36 C35 Fe1 69.9(2) . . ? C34 C35 Fe1 69.0(2) . . ? C36 C35 H35 126.1 . . ? C34 C35 H35 126.1 . . ? Fe1 C35 H35 126.6 . . ? C35 C36 C37 108.4(4) . . ? C35 C36 Fe1 70.0(2) . . ? C37 C36 Fe1 69.2(2) . . ? C35 C36 H36 125.8 . . ? C37 C36 H36 125.8 . . ? Fe1 C36 H36 126.6 . . ? C38 C37 C36 108.3(4) . . ? C38 C37 Fe1 69.1(2) . . ? C36 C37 Fe1 70.4(3) . . ? C38 C37 H37 125.9 . . ? C36 C37 H37 125.9 . . ? Fe1 C37 H37 126.1 . . ? C37 C38 C34 107.7(4) . . ? C37 C38 Fe1 70.3(2) . . ? C34 C38 Fe1 69.9(2) . . ? C37 C38 H38 126.1 . . ? C34 C38 H38 126.1 . . ? Fe1 C38 H38 125.3 . . ? O3 C39 O4 124.4(4) . . ? O3 C39 C40 122.9(4) . . ? O4 C39 C40 112.7(3) . . ? C41 C40 C44 107.9(3) . . ? C41 C40 C39 127.5(4) . . ? C44 C40 C39 124.6(4) . . ? C41 C40 Fe1 69.6(2) . . ? C44 C40 Fe1 69.6(2) . . ? C39 C40 Fe1 123.8(3) . . ? C40 C41 C42 107.8(4) . . ? C40 C41 Fe1 69.5(2) . . ? C42 C41 Fe1 70.4(2) . . ? C40 C41 H41 126.1 . . ? C42 C41 H41 126.1 . . ? Fe1 C41 H41 125.5 . . ? C41 C42 C43 108.2(4) . . ? C41 C42 Fe1 68.9(2) . . ? C43 C42 Fe1 70.0(2) . . ? C41 C42 H42 125.9 . . ? C43 C42 H42 125.9 . . ? Fe1 C42 H42 126.8 . . ? C44 C43 C42 107.9(4) . . ? C44 C43 Fe1 68.9(2) . . ? C42 C43 Fe1 69.4(2) . . ? C44 C43 H43 126.1 . . ? C42 C43 H43 126.1 . . ? Fe1 C43 H43 127.2 . . ? C43 C44 C40 108.2(4) . . ? C43 C44 Fe1 70.8(2) . . ? C40 C44 Fe1 69.2(2) . . ? C43 C44 H44 125.9 . . ? C40 C44 H44 125.9 . . ? Fe1 C44 H44 125.6 . . ? Cl1 C45 Cl2 112.0(4) . . ? Cl1 C45 H45A 109.2 . . ? Cl2 C45 H45A 109.2 . . ? Cl1 C45 H45B 109.2 . . ? Cl2 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? 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 C29 Pd1 P1 C7 -7.2(6) . . . . ? O2 Pd1 P1 C7 -57.07(15) . . . . ? P2 Pd1 P1 C7 125.44(13) . . . . ? C29 Pd1 P1 C1 111.2(6) . . . . ? O2 Pd1 P1 C1 61.34(17) . . . . ? P2 Pd1 P1 C1 -116.16(15) . . . . ? C29 Pd1 P1 C13 -124.0(6) . . . . ? O2 Pd1 P1 C13 -173.86(18) . . . . ? P2 Pd1 P1 C13 8.64(17) . . . . ? C29 Pd1 P2 C23 -65.82(16) . . . . ? O2 Pd1 P2 C23 -44.7(4) . . . . ? P1 Pd1 P2 C23 120.58(13) . . . . ? C29 Pd1 P2 C17 58.59(17) . . . . ? O2 Pd1 P2 C17 79.7(4) . . . . ? P1 Pd1 P2 C17 -115.01(14) . . . . ? C29 Pd1 P2 C16 179.18(18) . . . . ? O2 Pd1 P2 C16 -159.7(4) . . . . ? P1 Pd1 P2 C16 5.58(16) . . . . ? C29 Pd1 O2 C33 68.4(2) . . . . ? P2 Pd1 O2 C33 47.4(5) . . . . ? P1 Pd1 O2 C33 -118.2(2) . . . . ? C7 P1 C1 C2 140.4(3) . . . . ? C13 P1 C1 C2 -113.1(3) . . . . ? Pd1 P1 C1 C2 21.6(4) . . . . ? C7 P1 C1 C6 -44.1(4) . . . . ? C13 P1 C1 C6 62.3(4) . . . . ? Pd1 P1 C1 C6 -162.9(3) . . . . ? C6 C1 C2 C3 -1.2(6) . . . . ? P1 C1 C2 C3 174.3(3) . . . . ? C1 C2 C3 C4 1.1(6) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? C3 C4 C5 C6 -1.8(7) . . . . ? C4 C5 C6 C1 1.7(7) . . . . ? C2 C1 C6 C5 -0.2(6) . . . . ? P1 C1 C6 C5 -175.6(4) . . . . ? C1 P1 C7 C8 -33.5(4) . . . . ? C13 P1 C7 C8 -139.0(4) . . . . ? Pd1 P1 C7 C8 91.9(4) . . . . ? C1 P1 C7 C12 151.3(3) . . . . ? C13 P1 C7 C12 45.9(4) . . . . ? Pd1 P1 C7 C12 -83.3(3) . . . . ? C12 C7 C8 C9 -2.6(7) . . . . ? P1 C7 C8 C9 -177.7(4) . . . . ? C7 C8 C9 C10 1.1(9) . . . . ? C8 C9 C10 C11 0.9(10) . . . . ? C9 C10 C11 C12 -1.4(9) . . . . ? C10 C11 C12 C7 -0.1(8) . . . . ? C8 C7 C12 C11 2.1(7) . . . . ? P1 C7 C12 C11 177.4(4) . . . . ? C7 P1 C13 C14 172.5(3) . . . . ? C1 P1 C13 C14 63.2(3) . . . . ? Pd1 P1 C13 C14 -68.6(3) . . . . ? P1 C13 C14 C15 53.7(4) . . . . ? C13 C14 C15 C16 47.6(5) . . . . ? C14 C15 C16 P2 -115.5(3) . . . . ? C23 P2 C16 C15 -72.3(3) . . . . ? C17 P2 C16 C15 175.5(3) . . . . ? Pd1 P2 C16 C15 49.7(3) . . . . ? C23 P2 C17 C22 18.6(4) . . . . ? C16 P2 C17 C22 124.1(4) . . . . ? Pd1 P2 C17 C22 -107.9(3) . . . . ? C23 P2 C17 C18 -166.8(3) . . . . ? C16 P2 C17 C18 -61.3(4) . . . . ? Pd1 P2 C17 C18 66.7(3) . . . . ? C22 C17 C18 C19 -1.5(7) . . . . ? P2 C17 C18 C19 -176.4(4) . . . . ? C17 C18 C19 C20 1.3(8) . . . . ? C18 C19 C20 C21 0.0(8) . . . . ? C19 C20 C21 C22 -0.9(8) . . . . ? C18 C17 C22 C21 0.6(7) . . . . ? P2 C17 C22 C21 175.0(4) . . . . ? C20 C21 C22 C17 0.7(8) . . . . ? C17 P2 C23 C28 -139.9(3) . . . . ? C16 P2 C23 C28 112.1(3) . . . . ? Pd1 P2 C23 C28 -13.0(3) . . . . ? C17 P2 C23 C24 48.1(4) . . . . ? C16 P2 C23 C24 -59.9(4) . . . . ? Pd1 P2 C23 C24 175.0(3) . . . . ? C28 C23 C24 C25 0.9(7) . . . . ? P2 C23 C24 C25 172.9(4) . . . . ? C23 C24 C25 C26 -0.7(8) . . . . ? C24 C25 C26 C27 -0.1(9) . . . . ? C25 C26 C27 C28 0.5(8) . . . . ? C24 C23 C28 C27 -0.4(6) . . . . ? P2 C23 C28 C27 -172.6(3) . . . . ? C26 C27 C28 C23 -0.3(7) . . . . ? C32 Si1 C29 Pd1 21.5(3) . . . . ? C30 Si1 C29 Pd1 141.8(3) . . . . ? C31 Si1 C29 Pd1 -99.7(2) . . . . ? O2 Pd1 C29 Si1 61.77(16) . . . . ? P2 Pd1 C29 Si1 -121.78(16) . . . . ? P1 Pd1 C29 Si1 12.0(7) . . . . ? Pd1 O2 C33 O1 9.7(4) . . . . ? Pd1 O2 C33 C34 -169.7(2) . . . . ? O1 C33 C34 C35 160.1(4) . . . . ? O2 C33 C34 C35 -20.5(5) . . . . ? O1 C33 C34 C38 -16.6(5) . . . . ? O2 C33 C34 C38 162.8(3) . . . . ? O1 C33 C34 Fe1 71.0(4) . . . . ? O2 C33 C34 Fe1 -109.6(3) . . . . ? C38 Fe1 C34 C35 119.0(3) . . . . ? C40 Fe1 C34 C35 155.4(16) . . . . ? C41 Fe1 C34 C35 -60.3(4) . . . . ? C44 Fe1 C34 C35 -178.4(3) . . . . ? C37 Fe1 C34 C35 81.0(3) . . . . ? C42 Fe1 C34 C35 -96.7(3) . . . . ? C36 Fe1 C34 C35 37.3(3) . . . . ? C43 Fe1 C34 C35 -140.2(3) . . . . ? C40 Fe1 C34 C38 36.4(17) . . . . ? C41 Fe1 C34 C38 -179.3(3) . . . . ? C44 Fe1 C34 C38 62.7(3) . . . . ? C37 Fe1 C34 C38 -38.0(3) . . . . ? C42 Fe1 C34 C38 144.3(3) . . . . ? C36 Fe1 C34 C38 -81.7(3) . . . . ? C35 Fe1 C34 C38 -119.0(3) . . . . ? C43 Fe1 C34 C38 100.8(3) . . . . ? C38 Fe1 C34 C33 -120.6(4) . . . . ? C40 Fe1 C34 C33 -84.1(17) . . . . ? C41 Fe1 C34 C33 60.1(4) . . . . ? C44 Fe1 C34 C33 -57.9(4) . . . . ? C37 Fe1 C34 C33 -158.6(4) . . . . ? C42 Fe1 C34 C33 23.8(4) . . . . ? C36 Fe1 C34 C33 157.8(4) . . . . ? C35 Fe1 C34 C33 120.5(4) . . . . ? C43 Fe1 C34 C33 -19.7(4) . . . . ? C38 C34 C35 C36 -0.3(4) . . . . ? C33 C34 C35 C36 -177.5(4) . . . . ? Fe1 C34 C35 C36 -59.3(3) . . . . ? C38 C34 C35 Fe1 59.0(3) . . . . ? C33 C34 C35 Fe1 -118.2(4) . . . . ? C38 Fe1 C35 C36 81.1(3) . . . . ? C40 Fe1 C35 C36 -56.8(4) . . . . ? C41 Fe1 C35 C36 -95.3(3) . . . . ? C44 Fe1 C35 C36 131.5(18) . . . . ? C34 Fe1 C35 C36 119.3(4) . . . . ? C37 Fe1 C35 C36 37.3(3) . . . . ? C42 Fe1 C35 C36 -139.7(3) . . . . ? C43 Fe1 C35 C36 -179.7(3) . . . . ? C38 Fe1 C35 C34 -38.2(2) . . . . ? C40 Fe1 C35 C34 -176.1(3) . . . . ? C41 Fe1 C35 C34 145.4(2) . . . . ? C44 Fe1 C35 C34 12(2) . . . . ? C37 Fe1 C35 C34 -82.0(3) . . . . ? C42 Fe1 C35 C34 101.0(3) . . . . ? C36 Fe1 C35 C34 -119.3(4) . . . . ? C43 Fe1 C35 C34 61.0(3) . . . . ? C34 C35 C36 C37 0.1(5) . . . . ? Fe1 C35 C36 C37 -58.7(3) . . . . ? C34 C35 C36 Fe1 58.7(3) . . . . ? C38 Fe1 C36 C35 -82.3(3) . . . . ? C40 Fe1 C36 C35 147.6(3) . . . . ? C41 Fe1 C36 C35 102.9(3) . . . . ? C44 Fe1 C36 C35 -173.0(3) . . . . ? C34 Fe1 C36 C35 -37.7(3) . . . . ? C37 Fe1 C36 C35 -119.9(4) . . . . ? C42 Fe1 C36 C35 63.3(4) . . . . ? C43 Fe1 C36 C35 3(3) . . . . ? C38 Fe1 C36 C37 37.6(2) . . . . ? C40 Fe1 C36 C37 -92.5(3) . . . . ? C41 Fe1 C36 C37 -137.2(2) . . . . ? C44 Fe1 C36 C37 -53.2(4) . . . . ? C34 Fe1 C36 C37 82.2(3) . . . . ? C42 Fe1 C36 C37 -176.8(2) . . . . ? C35 Fe1 C36 C37 119.9(4) . . . . ? C43 Fe1 C36 C37 123(3) . . . . ? C35 C36 C37 C38 0.2(5) . . . . ? Fe1 C36 C37 C38 -59.0(3) . . . . ? C35 C36 C37 Fe1 59.2(3) . . . . ? C40 Fe1 C37 C38 -135.9(3) . . . . ? C41 Fe1 C37 C38 -174.1(3) . . . . ? C44 Fe1 C37 C38 -91.6(3) . . . . ? C34 Fe1 C37 C38 38.5(2) . . . . ? C42 Fe1 C37 C38 169(4) . . . . ? C36 Fe1 C37 C38 119.4(4) . . . . ? C35 Fe1 C37 C38 82.4(3) . . . . ? C43 Fe1 C37 C38 -55.8(4) . . . . ? C38 Fe1 C37 C36 -119.4(4) . . . . ? C40 Fe1 C37 C36 104.7(3) . . . . ? C41 Fe1 C37 C36 66.5(3) . . . . ? C44 Fe1 C37 C36 148.9(2) . . . . ? C34 Fe1 C37 C36 -80.9(3) . . . . ? C42 Fe1 C37 C36 50(4) . . . . ? C35 Fe1 C37 C36 -37.0(2) . . . . ? C43 Fe1 C37 C36 -175.2(3) . . . . ? C36 C37 C38 C34 -0.4(5) . . . . ? Fe1 C37 C38 C34 -60.1(3) . . . . ? C36 C37 C38 Fe1 59.8(3) . . . . ? C35 C34 C38 C37 0.4(4) . . . . ? C33 C34 C38 C37 177.6(3) . . . . ? Fe1 C34 C38 C37 60.4(3) . . . . ? C35 C34 C38 Fe1 -60.0(3) . . . . ? C33 C34 C38 Fe1 117.2(4) . . . . ? C40 Fe1 C38 C37 66.1(4) . . . . ? C41 Fe1 C38 C37 57(2) . . . . ? C44 Fe1 C38 C37 103.8(3) . . . . ? C34 Fe1 C38 C37 -118.4(4) . . . . ? C42 Fe1 C38 C37 -179.1(3) . . . . ? C36 Fe1 C38 C37 -37.4(3) . . . . ? C35 Fe1 C38 C37 -80.7(3) . . . . ? C43 Fe1 C38 C37 146.4(3) . . . . ? C40 Fe1 C38 C34 -175.5(2) . . . . ? C41 Fe1 C38 C34 175(2) . . . . ? C44 Fe1 C38 C34 -137.9(2) . . . . ? C37 Fe1 C38 C34 118.4(4) . . . . ? C42 Fe1 C38 C34 -60.8(4) . . . . ? C36 Fe1 C38 C34 80.9(3) . . . . ? C35 Fe1 C38 C34 37.7(2) . . . . ? C43 Fe1 C38 C34 -95.2(3) . . . . ? O3 C39 C40 C41 170.5(4) . . . . ? O4 C39 C40 C41 -10.0(5) . . . . ? O3 C39 C40 C44 -5.8(6) . . . . ? O4 C39 C40 C44 173.7(3) . . . . ? O3 C39 C40 Fe1 81.4(5) . . . . ? O4 C39 C40 Fe1 -99.1(4) . . . . ? C38 Fe1 C40 C41 -178.8(3) . . . . ? C44 Fe1 C40 C41 119.2(3) . . . . ? C34 Fe1 C40 C41 148.1(16) . . . . ? C37 Fe1 C40 C41 -139.5(3) . . . . ? C42 Fe1 C40 C41 38.0(2) . . . . ? C36 Fe1 C40 C41 -95.9(3) . . . . ? C35 Fe1 C40 C41 -59.6(4) . . . . ? C43 Fe1 C40 C41 81.8(3) . . . . ? C38 Fe1 C40 C44 62.0(3) . . . . ? C41 Fe1 C40 C44 -119.2(3) . . . . ? C34 Fe1 C40 C44 28.9(17) . . . . ? C37 Fe1 C40 C44 101.3(3) . . . . ? C42 Fe1 C40 C44 -81.1(3) . . . . ? C36 Fe1 C40 C44 144.9(3) . . . . ? C35 Fe1 C40 C44 -178.8(3) . . . . ? C43 Fe1 C40 C44 -37.4(2) . . . . ? C38 Fe1 C40 C39 -56.6(4) . . . . ? C41 Fe1 C40 C39 122.2(5) . . . . ? C44 Fe1 C40 C39 -118.6(4) . . . . ? C34 Fe1 C40 C39 -89.7(17) . . . . ? C37 Fe1 C40 C39 -17.3(4) . . . . ? C42 Fe1 C40 C39 160.2(4) . . . . ? C36 Fe1 C40 C39 26.2(4) . . . . ? C35 Fe1 C40 C39 62.6(5) . . . . ? C43 Fe1 C40 C39 -156.0(4) . . . . ? C44 C40 C41 C42 -1.0(4) . . . . ? C39 C40 C41 C42 -177.8(4) . . . . ? Fe1 C40 C41 C42 -60.3(3) . . . . ? C44 C40 C41 Fe1 59.3(3) . . . . ? C39 C40 C41 Fe1 -117.5(4) . . . . ? C38 Fe1 C41 C40 10(2) . . . . ? C44 Fe1 C41 C40 -38.0(2) . . . . ? C34 Fe1 C41 C40 -175.1(3) . . . . ? C37 Fe1 C41 C40 62.7(4) . . . . ? C42 Fe1 C41 C40 -118.6(4) . . . . ? C36 Fe1 C41 C40 102.5(3) . . . . ? C35 Fe1 C41 C40 146.3(2) . . . . ? C43 Fe1 C41 C40 -81.3(3) . . . . ? C38 Fe1 C41 C42 129(2) . . . . ? C40 Fe1 C41 C42 118.6(4) . . . . ? C44 Fe1 C41 C42 80.6(3) . . . . ? C34 Fe1 C41 C42 -56.6(4) . . . . ? C37 Fe1 C41 C42 -178.8(3) . . . . ? C36 Fe1 C41 C42 -138.9(3) . . . . ? C35 Fe1 C41 C42 -95.1(3) . . . . ? C43 Fe1 C41 C42 37.3(2) . . . . ? C40 C41 C42 C43 0.6(5) . . . . ? Fe1 C41 C42 C43 -59.2(3) . . . . ? C40 C41 C42 Fe1 59.7(3) . . . . ? C38 Fe1 C42 C41 -173.9(3) . . . . ? C40 Fe1 C42 C41 -38.2(2) . . . . ? C44 Fe1 C42 C41 -82.7(3) . . . . ? C34 Fe1 C42 C41 147.4(2) . . . . ? C37 Fe1 C42 C41 18(4) . . . . ? C36 Fe1 C42 C41 65.0(3) . . . . ? C35 Fe1 C42 C41 103.3(3) . . . . ? C43 Fe1 C42 C41 -119.8(4) . . . . ? C38 Fe1 C42 C43 -54.0(4) . . . . ? C40 Fe1 C42 C43 81.6(3) . . . . ? C41 Fe1 C42 C43 119.8(4) . . . . ? C44 Fe1 C42 C43 37.1(2) . . . . ? C34 Fe1 C42 C43 -92.8(3) . . . . ? C37 Fe1 C42 C43 137(4) . . . . ? C36 Fe1 C42 C43 -175.2(3) . . . . ? C35 Fe1 C42 C43 -136.9(2) . . . . ? C41 C42 C43 C44 0.1(5) . . . . ? Fe1 C42 C43 C44 -58.3(3) . . . . ? C41 C42 C43 Fe1 58.4(3) . . . . ? C38 Fe1 C43 C44 -92.5(3) . . . . ? C40 Fe1 C43 C44 38.2(2) . . . . ? C41 Fe1 C43 C44 82.3(3) . . . . ? C34 Fe1 C43 C44 -136.5(2) . . . . ? C37 Fe1 C43 C44 -57.2(4) . . . . ? C42 Fe1 C43 C44 119.8(3) . . . . ? C36 Fe1 C43 C44 -176(3) . . . . ? C35 Fe1 C43 C44 -173.5(3) . . . . ? C38 Fe1 C43 C42 147.8(2) . . . . ? C40 Fe1 C43 C42 -81.5(2) . . . . ? C41 Fe1 C43 C42 -37.4(2) . . . . ? C44 Fe1 C43 C42 -119.8(3) . . . . ? C34 Fe1 C43 C42 103.7(2) . . . . ? C37 Fe1 C43 C42 -176.9(3) . . . . ? C36 Fe1 C43 C42 64(3) . . . . ? C35 Fe1 C43 C42 66.7(3) . . . . ? C42 C43 C44 C40 -0.7(4) . . . . ? Fe1 C43 C44 C40 -59.4(3) . . . . ? C42 C43 C44 Fe1 58.6(3) . . . . ? C41 C40 C44 C43 1.1(4) . . . . ? C39 C40 C44 C43 178.0(3) . . . . ? Fe1 C40 C44 C43 60.4(3) . . . . ? C41 C40 C44 Fe1 -59.3(3) . . . . ? C39 C40 C44 Fe1 117.6(4) . . . . ? C38 Fe1 C44 C43 102.5(3) . . . . ? C40 Fe1 C44 C43 -119.1(3) . . . . ? C41 Fe1 C44 C43 -81.3(3) . . . . ? C34 Fe1 C44 C43 64.6(3) . . . . ? C37 Fe1 C44 C43 145.5(2) . . . . ? C42 Fe1 C44 C43 -37.4(2) . . . . ? C36 Fe1 C44 C43 179.6(3) . . . . ? C35 Fe1 C44 C43 54(2) . . . . ? C38 Fe1 C44 C40 -138.5(2) . . . . ? C41 Fe1 C44 C40 37.7(2) . . . . ? C34 Fe1 C44 C40 -176.3(2) . . . . ? C37 Fe1 C44 C40 -95.4(3) . . . . ? C42 Fe1 C44 C40 81.6(2) . . . . ? C36 Fe1 C44 C40 -61.3(4) . . . . ? C35 Fe1 C44 C40 172.6(18) . . . . ? C43 Fe1 C44 C40 119.1(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O1 0.84 1.73 2.529(4) 159.2 4_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.778 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.081 data_sa1599-b _database_code_depnum_ccdc_archive 'CCDC 917454' #TrackingRef 'web_deposit_cif_file_0_YudongCai_1356446266.sa1599-b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H42 Fe O4 P2 Pd, C H2 Cl2' _chemical_formula_sum 'C50 H44 Cl2 Fe O4 P2 Pd' _chemical_formula_weight 1003.94 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' Fe Fe 0.3463 0.8444 '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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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' _cell_length_a 17.696(3) _cell_length_b 13.606(3) _cell_length_c 18.782(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.300(4) _cell_angle_gamma 90.00 _cell_volume 4474.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11808 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8020 _exptl_absorpt_correction_T_max 0.8933 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23010 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.36 _reflns_number_total 8138 _reflns_number_gt 6468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELX97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0052P)^2^+28.1036P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8138 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1629 _refine_ls_R_factor_gt 0.1347 _refine_ls_wR_factor_ref 0.1985 _refine_ls_wR_factor_gt 0.1872 _refine_ls_goodness_of_fit_ref 1.297 _refine_ls_restrained_S_all 1.297 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.20148(5) 0.97779(5) 0.77832(4) 0.0411(2) Uani 1 1 d . . . Fe1 Fe 0.51269(9) 0.99161(11) 0.72960(9) 0.0506(4) Uani 1 1 d . . . Cl1 Cl 0.2069(2) 0.6553(3) 0.7790(3) 0.1107(15) Uani 1 1 d . . . Cl2 Cl 0.1193(4) 0.4796(5) 0.7627(4) 0.208(4) Uani 1 1 d . . . P1 P 0.13404(16) 0.97115(19) 0.66369(14) 0.0433(7) Uani 1 1 d . . . P2 P 0.25870(17) 0.98832(19) 0.89820(15) 0.0451(7) Uani 1 1 d . . . O1 O 0.3082(4) 0.9578(5) 0.7417(3) 0.0463(18) Uani 1 1 d . . . O2 O 0.3161(4) 1.1120(5) 0.7028(4) 0.0494(18) Uani 1 1 d . . . O3 O 0.6065(4) 0.7741(5) 0.8075(5) 0.061(2) Uani 1 1 d . . . H3 H 0.6361 0.7263 0.8049 0.092 Uiso 1 1 calc R . . O4 O 0.7096(5) 0.8599(6) 0.7880(5) 0.069(2) Uani 1 1 d . . . C1 C 0.4061(6) 0.9931(7) 0.6751(6) 0.045(3) Uani 1 1 d . . . C2 C 0.4545(6) 1.0514(8) 0.6383(6) 0.058(3) Uani 1 1 d . . . H2 H 0.4482 1.1194 0.6277 0.070 Uiso 1 1 calc R . . C3 C 0.5131(7) 0.9912(8) 0.6204(6) 0.057(3) Uani 1 1 d . . . H3A H 0.5536 1.0119 0.5958 0.069 Uiso 1 1 calc R . . C4 C 0.5024(6) 0.8958(8) 0.6444(6) 0.058(3) Uani 1 1 d . . . H4 H 0.5339 0.8406 0.6392 0.070 Uiso 1 1 calc R . . C5 C 0.4364(6) 0.8968(8) 0.6776(5) 0.049(3) Uani 1 1 d . . . H5 H 0.4154 0.8415 0.6986 0.058 Uiso 1 1 calc R . . C6 C 0.3393(6) 1.0253(8) 0.7091(5) 0.047(3) Uani 1 1 d . . . C7 C 0.5972(6) 0.9454(8) 0.8068(6) 0.051(3) Uani 1 1 d . . . C8 C 0.6136(7) 1.0414(8) 0.7831(7) 0.069(4) Uani 1 1 d . . . H8 H 0.6572 1.0602 0.7623 0.083 Uiso 1 1 calc R . . C9 C 0.5532(8) 1.1035(9) 0.7963(7) 0.068(4) Uani 1 1 d . . . H9 H 0.5491 1.1718 0.7859 0.082 Uiso 1 1 calc R . . C10 C 0.4996(7) 1.0465(9) 0.8278(7) 0.069(4) Uani 1 1 d . . . H10 H 0.4536 1.0701 0.8422 0.083 Uiso 1 1 calc R . . C11 C 0.5259(6) 0.9502(8) 0.8342(6) 0.054(3) Uani 1 1 d . . . H11 H 0.5008 0.8968 0.8534 0.064 Uiso 1 1 calc R . . C12 C 0.6435(7) 0.8573(9) 0.7999(6) 0.054(3) Uani 1 1 d . . . C13 C 0.1903(6) 0.9480(8) 0.5912(6) 0.050(3) Uani 1 1 d . . . C14 C 0.2430(6) 0.8742(8) 0.5971(6) 0.055(3) Uani 1 1 d . . . H14 H 0.2509 0.8354 0.6396 0.066 Uiso 1 1 calc R . . C15 C 0.2854(7) 0.8549(9) 0.5421(8) 0.068(4) Uani 1 1 d . . . H15 H 0.3245 0.8066 0.5482 0.081 Uiso 1 1 calc R . . C16 C 0.2703(9) 0.9067(11) 0.4784(8) 0.084(5) Uani 1 1 d . . . H16 H 0.2983 0.8920 0.4402 0.101 Uiso 1 1 calc R . . C17 C 0.2161(9) 0.9780(10) 0.4692(7) 0.082(4) Uani 1 1 d . . . H17 H 0.2054 1.0127 0.4250 0.099 Uiso 1 1 calc R . . C18 C 0.1769(7) 0.9989(8) 0.5258(6) 0.063(3) Uani 1 1 d . . . H18 H 0.1395 1.0495 0.5203 0.076 Uiso 1 1 calc R . . C19 C 0.0563(6) 0.8821(7) 0.6455(5) 0.041(2) Uani 1 1 d . . . C20 C 0.0145(6) 0.8732(8) 0.5765(6) 0.051(3) Uani 1 1 d . . . H20 H 0.0288 0.9107 0.5380 0.061 Uiso 1 1 calc R . . C21 C -0.0463(7) 0.8115(7) 0.5642(6) 0.054(3) Uani 1 1 d . . . H21 H -0.0739 0.8065 0.5171 0.065 Uiso 1 1 calc R . . C22 C -0.0682(7) 0.7569(8) 0.6179(7) 0.060(3) Uani 1 1 d . . . H22 H -0.1128 0.7174 0.6092 0.072 Uiso 1 1 calc R . . C23 C -0.0247(7) 0.7592(8) 0.6863(6) 0.063(3) Uani 1 1 d . . . H23 H -0.0374 0.7180 0.7237 0.075 Uiso 1 1 calc R . . C24 C 0.0364(6) 0.8219(8) 0.6984(5) 0.050(3) Uani 1 1 d . . . H24 H 0.0659 0.8237 0.7449 0.060 Uiso 1 1 calc R . . C25 C 0.0879(6) 1.0896(7) 0.6439(5) 0.040(2) Uani 1 1 d . . . C26 C 0.0089(6) 1.1046(8) 0.6286(5) 0.044(3) Uani 1 1 d . . . H26 H -0.0248 1.0499 0.6252 0.053 Uiso 1 1 calc R . . C27 C -0.0198(7) 1.1977(8) 0.6186(5) 0.049(3) Uani 1 1 d . . . H27 H -0.0734 1.2073 0.6081 0.058 Uiso 1 1 calc R . . C28 C 0.0283(7) 1.2775(8) 0.6235(5) 0.052(3) Uani 1 1 d . . . H28 H 0.0074 1.3417 0.6171 0.062 Uiso 1 1 calc R . . C29 C 0.1056(7) 1.2656(7) 0.6373(5) 0.048(3) Uani 1 1 d . . . H29 H 0.1383 1.3212 0.6399 0.057 Uiso 1 1 calc R . . C30 C 0.1362(6) 1.1720(7) 0.6476(5) 0.047(3) Uani 1 1 d . . . H30 H 0.1900 1.1635 0.6572 0.057 Uiso 1 1 calc R . . C31 C 0.3389(6) 0.9045(8) 0.9193(6) 0.050(3) Uani 1 1 d . . . C32 C 0.3930(7) 0.9127(9) 0.9808(6) 0.061(3) Uani 1 1 d . . . H32 H 0.3910 0.9673 1.0120 0.073 Uiso 1 1 calc R . . C33 C 0.4491(7) 0.8430(10) 0.9969(6) 0.071(4) Uani 1 1 d . . . H33 H 0.4860 0.8502 1.0387 0.085 Uiso 1 1 calc R . . C34 C 0.4519(7) 0.7626(9) 0.9525(6) 0.060(3) Uani 1 1 d . . . H34 H 0.4900 0.7137 0.9642 0.071 Uiso 1 1 calc R . . C35 C 0.3995(6) 0.7534(8) 0.8915(6) 0.051(3) Uani 1 1 d . . . H35 H 0.4011 0.6981 0.8609 0.061 Uiso 1 1 calc R . . C36 C 0.3444(6) 0.8247(7) 0.8748(5) 0.049(3) Uani 1 1 d . . . H36 H 0.3093 0.8189 0.8317 0.058 Uiso 1 1 calc R . . C37 C 0.2921(6) 1.1130(7) 0.9236(5) 0.042(3) Uani 1 1 d . . . C38 C 0.2916(6) 1.1814(7) 0.8688(6) 0.047(3) Uani 1 1 d . . . H38 H 0.2786 1.1629 0.8198 0.056 Uiso 1 1 calc R . . C39 C 0.3106(7) 1.2768(8) 0.8877(7) 0.060(3) Uani 1 1 d . . . H39 H 0.3100 1.3244 0.8506 0.072 Uiso 1 1 calc R . . C40 C 0.3303(7) 1.3063(8) 0.9569(7) 0.067(4) Uani 1 1 d . . . H40 H 0.3451 1.3724 0.9676 0.081 Uiso 1 1 calc R . . C41 C 0.3286(8) 1.2397(8) 1.0110(7) 0.075(4) Uani 1 1 d . . . H41 H 0.3412 1.2603 1.0596 0.090 Uiso 1 1 calc R . . C42 C 0.3089(7) 1.1436(8) 0.9964(6) 0.067(4) Uani 1 1 d . . . H42 H 0.3065 1.0981 1.0344 0.081 Uiso 1 1 calc R . . C43 C 0.1970(6) 0.9544(7) 0.9644(5) 0.042(2) Uani 1 1 d . . . C44 C 0.1871(6) 0.8560(8) 0.9792(6) 0.047(3) Uani 1 1 d . . . H44 H 0.2176 0.8083 0.9598 0.057 Uiso 1 1 calc R . . C45 C 0.1338(7) 0.8257(9) 1.0215(6) 0.060(3) Uani 1 1 d . . . H45 H 0.1282 0.7579 1.0315 0.073 Uiso 1 1 calc R . . C46 C 0.0890(7) 0.8945(9) 1.0490(6) 0.063(3) Uani 1 1 d . . . H46 H 0.0516 0.8738 1.0774 0.076 Uiso 1 1 calc R . . C47 C 0.0977(7) 0.9911(9) 1.0362(6) 0.059(3) Uani 1 1 d . . . H47 H 0.0676 1.0385 1.0565 0.071 Uiso 1 1 calc R . . C48 C 0.1510(6) 1.0208(8) 0.9930(5) 0.053(3) Uani 1 1 d . . . H48 H 0.1558 1.0888 0.9830 0.063 Uiso 1 1 calc R . . C49 C 0.1708(9) 0.5533(13) 0.7292(9) 0.122(6) Uani 1 1 d . . . H49A H 0.1415 0.5778 0.6838 0.146 Uiso 1 1 calc R . . H49B H 0.2149 0.5161 0.7161 0.146 Uiso 1 1 calc R . . C C 0.0990(6) 0.9996(8) 0.8135(6) 0.060(3) Uani 1 1 d . . . HA H 0.0581 0.9999 0.7722 0.090 Uiso 1 1 calc R . . HC H 0.0997 1.0628 0.8386 0.090 Uiso 1 1 calc R . . HB H 0.0899 0.9466 0.8465 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0480(5) 0.0361(4) 0.0366(4) -0.0003(4) -0.0024(3) -0.0022(4) Fe1 0.0514(10) 0.0405(9) 0.0588(10) -0.0030(8) 0.0047(8) -0.0026(8) Cl1 0.085(3) 0.106(3) 0.142(4) -0.036(3) 0.018(3) -0.011(3) Cl2 0.183(6) 0.209(6) 0.266(8) -0.161(6) 0.152(6) -0.111(5) P1 0.0513(17) 0.0375(14) 0.0393(15) -0.0010(12) 0.0010(13) -0.0004(14) P2 0.0537(18) 0.0354(14) 0.0432(15) -0.0001(12) -0.0028(13) 0.0008(14) O1 0.051(5) 0.048(4) 0.040(4) 0.004(3) 0.008(4) -0.001(4) O2 0.046(5) 0.044(4) 0.057(5) 0.001(4) 0.006(4) 0.008(4) O3 0.064(6) 0.044(4) 0.076(6) 0.009(4) 0.013(5) 0.004(4) O4 0.053(5) 0.065(5) 0.085(7) 0.001(5) 0.003(5) -0.001(5) C1 0.044(6) 0.033(5) 0.056(7) -0.003(5) -0.002(5) -0.003(5) C2 0.061(8) 0.043(6) 0.073(9) 0.001(6) 0.021(7) 0.004(6) C3 0.066(8) 0.051(7) 0.055(7) 0.006(6) 0.010(6) 0.004(6) C4 0.052(8) 0.055(7) 0.069(8) -0.020(6) 0.015(6) 0.015(6) C5 0.050(7) 0.050(6) 0.045(6) -0.008(5) 0.003(5) -0.009(6) C6 0.055(7) 0.046(6) 0.037(6) -0.005(5) -0.006(5) 0.005(6) C7 0.051(7) 0.051(7) 0.048(7) -0.009(5) 0.001(6) -0.012(6) C8 0.059(8) 0.057(8) 0.091(10) -0.005(7) 0.007(7) -0.010(7) C9 0.078(10) 0.047(7) 0.073(9) -0.026(6) -0.010(7) -0.009(7) C10 0.066(9) 0.056(8) 0.084(10) -0.014(7) 0.001(7) 0.005(7) C11 0.055(7) 0.052(7) 0.052(7) 0.001(5) 0.001(6) -0.002(6) C12 0.059(8) 0.066(8) 0.035(6) 0.000(6) -0.001(6) -0.001(7) C13 0.053(7) 0.044(6) 0.054(7) -0.004(5) 0.009(6) -0.015(6) C14 0.046(7) 0.054(7) 0.063(8) -0.013(6) -0.002(6) 0.000(6) C15 0.047(8) 0.068(8) 0.088(10) -0.036(8) 0.010(7) 0.004(7) C16 0.090(12) 0.090(11) 0.080(11) -0.029(9) 0.037(9) -0.023(9) C17 0.116(12) 0.070(9) 0.073(9) 0.002(8) 0.053(9) -0.009(9) C18 0.086(10) 0.042(7) 0.067(8) -0.004(6) 0.026(7) 0.000(6) C19 0.043(6) 0.045(6) 0.033(6) -0.007(5) -0.001(5) 0.010(5) C20 0.063(8) 0.049(6) 0.037(6) 0.005(5) -0.003(6) -0.005(6) C21 0.064(8) 0.034(6) 0.057(7) -0.004(5) -0.016(6) -0.003(6) C22 0.055(8) 0.048(7) 0.075(9) -0.001(6) 0.003(7) -0.023(6) C23 0.082(9) 0.065(8) 0.039(7) -0.003(6) 0.000(6) -0.023(7) C24 0.063(8) 0.055(7) 0.027(6) 0.008(5) -0.007(5) -0.005(6) C25 0.061(7) 0.036(5) 0.024(5) 0.000(4) 0.007(5) -0.011(5) C26 0.046(7) 0.057(7) 0.028(5) 0.001(5) -0.002(5) -0.005(6) C27 0.060(7) 0.053(7) 0.033(6) 0.012(5) 0.005(5) 0.015(6) C28 0.069(8) 0.046(6) 0.038(6) 0.004(5) 0.002(6) 0.013(6) C29 0.067(8) 0.038(6) 0.039(6) 0.004(5) 0.008(6) 0.001(6) C30 0.058(7) 0.044(6) 0.038(6) 0.006(5) -0.002(5) 0.009(6) C31 0.041(7) 0.053(7) 0.052(7) 0.002(6) -0.003(5) 0.000(6) C32 0.056(8) 0.068(8) 0.055(8) -0.013(6) -0.002(6) 0.017(7) C33 0.065(9) 0.095(10) 0.046(7) -0.003(7) -0.012(6) 0.014(8) C34 0.054(8) 0.063(8) 0.061(8) 0.016(7) 0.005(7) 0.012(6) C35 0.058(8) 0.045(6) 0.046(7) 0.004(5) 0.000(6) -0.008(6) C36 0.066(8) 0.047(6) 0.030(6) 0.007(5) -0.002(5) 0.001(6) C37 0.049(7) 0.038(6) 0.038(6) 0.002(5) -0.001(5) 0.003(5) C38 0.050(7) 0.040(6) 0.049(7) -0.002(5) 0.005(5) 0.007(5) C39 0.081(9) 0.037(6) 0.062(8) 0.000(6) 0.010(7) -0.006(6) C40 0.091(10) 0.033(6) 0.074(9) -0.011(6) -0.001(8) -0.013(6) C41 0.100(11) 0.046(7) 0.069(9) -0.009(7) -0.025(8) -0.012(7) C42 0.098(10) 0.055(7) 0.042(7) 0.000(6) -0.015(7) 0.000(7) C43 0.042(6) 0.040(6) 0.039(6) -0.001(5) -0.012(5) 0.006(5) C44 0.038(6) 0.052(7) 0.051(7) 0.001(5) 0.001(5) 0.001(5) C45 0.052(8) 0.060(8) 0.067(8) 0.011(6) 0.001(7) 0.001(6) C46 0.061(8) 0.079(9) 0.049(7) 0.008(7) 0.008(6) -0.007(7) C47 0.082(9) 0.058(7) 0.042(6) -0.011(6) 0.019(6) 0.000(7) C48 0.065(8) 0.046(6) 0.044(6) -0.008(5) -0.004(6) -0.010(6) C49 0.095(12) 0.163(17) 0.101(13) -0.047(12) -0.009(10) -0.057(12) C 0.071(8) 0.060(7) 0.049(7) 0.005(6) 0.009(6) 0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C 2.040(10) . ? Pd1 O1 2.120(7) . ? Pd1 P1 2.308(3) . ? Pd1 P2 2.336(3) . ? Fe1 C1 2.012(10) . ? Fe1 C5 2.014(10) . ? Fe1 C11 2.024(11) . ? Fe1 C7 2.027(11) . ? Fe1 C10 2.034(13) . ? Fe1 C8 2.035(12) . ? Fe1 C9 2.035(11) . ? Fe1 C2 2.038(12) . ? Fe1 C4 2.051(11) . ? Fe1 C3 2.052(11) . ? Cl1 C49 1.744(14) . ? Cl2 C49 1.550(16) . ? P1 C25 1.821(10) . ? P1 C19 1.827(10) . ? P1 C13 1.827(11) . ? P2 C31 1.820(11) . ? P2 C43 1.828(11) . ? P2 C37 1.837(10) . ? O1 C6 1.271(12) . ? O2 C6 1.249(11) . ? O3 C12 1.326(13) . ? O3 H3 0.8400 . ? O4 C12 1.222(13) . ? C1 C5 1.414(13) . ? C1 C2 1.418(13) . ? C1 C6 1.487(14) . ? C2 C3 1.400(14) . ? C2 H2 0.9500 . ? C3 C4 1.396(14) . ? C3 H3A 0.9500 . ? C4 C5 1.400(14) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 C8 1.423(15) . ? C7 C11 1.431(14) . ? C7 C12 1.468(15) . ? C8 C9 1.413(16) . ? C8 H8 0.9500 . ? C9 C10 1.418(16) . ? C9 H9 0.9500 . ? C10 C11 1.389(14) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C14 1.364(14) . ? C13 C18 1.400(15) . ? C14 C15 1.386(15) . ? C14 H14 0.9500 . ? C15 C16 1.382(18) . ? C15 H15 0.9500 . ? C16 C17 1.358(18) . ? C16 H16 0.9500 . ? C17 C18 1.380(15) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.373(13) . ? C19 C20 1.402(13) . ? C20 C21 1.358(14) . ? C20 H20 0.9500 . ? C21 C22 1.353(14) . ? C21 H21 0.9500 . ? C22 C23 1.399(15) . ? C22 H22 0.9500 . ? C23 C24 1.370(14) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.401(13) . ? C25 C30 1.404(13) . ? C26 C27 1.368(13) . ? C26 H26 0.9500 . ? C27 C28 1.373(14) . ? C27 H27 0.9500 . ? C28 C29 1.365(14) . ? C28 H28 0.9500 . ? C29 C30 1.387(13) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.382(14) . ? C31 C32 1.393(14) . ? C32 C33 1.375(15) . ? C32 H32 0.9500 . ? C33 C34 1.381(15) . ? C33 H33 0.9500 . ? C34 C35 1.372(14) . ? C34 H34 0.9500 . ? C35 C36 1.380(14) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.387(13) . ? C37 C42 1.418(14) . ? C38 C39 1.376(13) . ? C38 H38 0.9500 . ? C39 C40 1.356(15) . ? C39 H39 0.9500 . ? C40 C41 1.365(16) . ? C40 H40 0.9500 . ? C41 C42 1.372(14) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.377(13) . ? C43 C44 1.383(13) . ? C44 C45 1.381(14) . ? C44 H44 0.9500 . ? C45 C46 1.376(15) . ? C45 H45 0.9500 . ? C46 C47 1.349(15) . ? C46 H46 0.9500 . ? C47 C48 1.389(14) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C HA 0.9800 . ? C HC 0.9800 . ? C HB 0.9800 . ? 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 C Pd1 O1 179.0(4) . . ? C Pd1 P1 86.8(3) . . ? O1 Pd1 P1 93.27(19) . . ? C Pd1 P2 87.8(3) . . ? O1 Pd1 P2 92.2(2) . . ? P1 Pd1 P2 174.51(11) . . ? C1 Fe1 C5 41.1(4) . . ? C1 Fe1 C11 117.7(4) . . ? C5 Fe1 C11 105.5(4) . . ? C1 Fe1 C7 155.2(4) . . ? C5 Fe1 C7 121.4(4) . . ? C11 Fe1 C7 41.4(4) . . ? C1 Fe1 C10 103.7(5) . . ? C5 Fe1 C10 121.2(5) . . ? C11 Fe1 C10 40.0(4) . . ? C7 Fe1 C10 68.5(5) . . ? C1 Fe1 C8 160.0(4) . . ? C5 Fe1 C8 158.6(5) . . ? C11 Fe1 C8 69.1(5) . . ? C7 Fe1 C8 41.0(4) . . ? C10 Fe1 C8 68.7(5) . . ? C1 Fe1 C9 121.8(5) . . ? C5 Fe1 C9 158.3(5) . . ? C11 Fe1 C9 68.3(5) . . ? C7 Fe1 C9 68.5(5) . . ? C10 Fe1 C9 40.8(5) . . ? C8 Fe1 C9 40.6(4) . . ? C1 Fe1 C2 41.0(4) . . ? C5 Fe1 C2 68.0(4) . . ? C11 Fe1 C2 154.3(5) . . ? C7 Fe1 C2 163.1(4) . . ? C10 Fe1 C2 120.4(5) . . ? C8 Fe1 C2 125.7(5) . . ? C9 Fe1 C2 108.1(5) . . ? C1 Fe1 C4 68.8(4) . . ? C5 Fe1 C4 40.3(4) . . ? C11 Fe1 C4 124.4(5) . . ? C7 Fe1 C4 109.5(5) . . ? C10 Fe1 C4 158.7(5) . . ? C8 Fe1 C4 124.7(5) . . ? C9 Fe1 C4 159.9(5) . . ? C2 Fe1 C4 67.7(4) . . ? C1 Fe1 C3 68.3(4) . . ? C5 Fe1 C3 67.2(4) . . ? C11 Fe1 C3 162.3(4) . . ? C7 Fe1 C3 127.3(5) . . ? C10 Fe1 C3 157.6(5) . . ? C8 Fe1 C3 111.4(5) . . ? C9 Fe1 C3 124.5(5) . . ? C2 Fe1 C3 40.0(4) . . ? C4 Fe1 C3 39.8(4) . . ? C25 P1 C19 104.2(5) . . ? C25 P1 C13 106.1(5) . . ? C19 P1 C13 102.9(5) . . ? C25 P1 Pd1 108.2(3) . . ? C19 P1 Pd1 118.3(3) . . ? C13 P1 Pd1 116.0(4) . . ? C31 P2 C43 102.5(5) . . ? C31 P2 C37 108.1(5) . . ? C43 P2 C37 104.9(5) . . ? C31 P2 Pd1 112.8(4) . . ? C43 P2 Pd1 115.0(3) . . ? C37 P2 Pd1 112.7(3) . . ? C6 O1 Pd1 122.1(6) . . ? C12 O3 H3 109.5 . . ? C5 C1 C2 106.3(9) . . ? C5 C1 C6 125.5(10) . . ? C2 C1 C6 128.1(9) . . ? C5 C1 Fe1 69.5(6) . . ? C2 C1 Fe1 70.5(6) . . ? C6 C1 Fe1 122.0(7) . . ? C3 C2 C1 108.1(9) . . ? C3 C2 Fe1 70.6(7) . . ? C1 C2 Fe1 68.5(6) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe1 C2 H2 126.5 . . ? C4 C3 C2 109.0(10) . . ? C4 C3 Fe1 70.1(6) . . ? C2 C3 Fe1 69.4(7) . . ? C4 C3 H3A 125.5 . . ? C2 C3 H3A 125.5 . . ? Fe1 C3 H3A 126.6 . . ? C3 C4 C5 107.2(10) . . ? C3 C4 Fe1 70.2(6) . . ? C5 C4 Fe1 68.4(6) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? Fe1 C4 H4 126.6 . . ? C4 C5 C1 109.3(10) . . ? C4 C5 Fe1 71.3(6) . . ? C1 C5 Fe1 69.4(6) . . ? C4 C5 H5 125.3 . . ? C1 C5 H5 125.3 . . ? Fe1 C5 H5 125.6 . . ? O2 C6 O1 124.6(10) . . ? O2 C6 C1 120.6(10) . . ? O1 C6 C1 114.8(9) . . ? C8 C7 C11 107.5(10) . . ? C8 C7 C12 125.4(11) . . ? C11 C7 C12 127.0(10) . . ? C8 C7 Fe1 69.8(7) . . ? C11 C7 Fe1 69.2(6) . . ? C12 C7 Fe1 123.6(8) . . ? C9 C8 C7 107.5(11) . . ? C9 C8 Fe1 69.7(7) . . ? C7 C8 Fe1 69.2(7) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? Fe1 C8 H8 126.4 . . ? C8 C9 C10 108.3(11) . . ? C8 C9 Fe1 69.7(7) . . ? C10 C9 Fe1 69.6(7) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? Fe1 C9 H9 126.5 . . ? C11 C10 C9 108.4(11) . . ? C11 C10 Fe1 69.6(7) . . ? C9 C10 Fe1 69.6(7) . . ? C11 C10 H10 125.8 . . ? C9 C10 H10 125.8 . . ? Fe1 C10 H10 126.6 . . ? C10 C11 C7 108.3(11) . . ? C10 C11 Fe1 70.4(7) . . ? C7 C11 Fe1 69.4(6) . . ? C10 C11 H11 125.8 . . ? C7 C11 H11 125.8 . . ? Fe1 C11 H11 125.9 . . ? O4 C12 O3 123.0(11) . . ? O4 C12 C7 123.6(11) . . ? O3 C12 C7 113.4(10) . . ? C14 C13 C18 117.6(11) . . ? C14 C13 P1 120.4(9) . . ? C18 C13 P1 121.7(9) . . ? C13 C14 C15 121.0(12) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 119.5(13) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 121.2(13) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 118.3(14) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C17 C18 C13 122.1(12) . . ? C17 C18 H18 118.9 . . ? C13 C18 H18 118.9 . . ? C24 C19 C20 117.4(10) . . ? C24 C19 P1 121.7(8) . . ? C20 C19 P1 120.9(8) . . ? C21 C20 C19 120.7(10) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 121.1(11) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 119.6(11) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 118.8(11) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C19 122.1(10) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? C26 C25 C30 118.4(9) . . ? C26 C25 P1 125.1(8) . . ? C30 C25 P1 116.4(8) . . ? C27 C26 C25 120.1(10) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.6(11) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C29 C28 C27 120.8(10) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 119.7(11) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C25 120.2(10) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C36 C31 C32 117.7(10) . . ? C36 C31 P2 118.7(9) . . ? C32 C31 P2 123.4(9) . . ? C33 C32 C31 121.0(11) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 120.0(12) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 119.9(11) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 119.7(11) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C31 121.6(10) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? C38 C37 C42 119.8(10) . . ? C38 C37 P2 117.3(8) . . ? C42 C37 P2 122.4(8) . . ? C39 C38 C37 117.8(10) . . ? C39 C38 H38 121.1 . . ? C37 C38 H38 121.1 . . ? C40 C39 C38 123.1(11) . . ? C40 C39 H39 118.5 . . ? C38 C39 H39 118.5 . . ? C39 C40 C41 119.2(11) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C40 C41 C42 121.1(12) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C41 C42 C37 119.0(11) . . ? C41 C42 H42 120.5 . . ? C37 C42 H42 120.5 . . ? C48 C43 C44 117.2(10) . . ? C48 C43 P2 123.0(8) . . ? C44 C43 P2 119.1(8) . . ? C45 C44 C43 121.4(10) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C46 C45 C44 119.5(11) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C47 C46 C45 120.6(11) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 C47 C48 119.5(11) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C43 C48 C47 121.7(10) . . ? C43 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? Cl2 C49 Cl1 119.2(10) . . ? Cl2 C49 H49A 107.5 . . ? Cl1 C49 H49A 107.5 . . ? Cl2 C49 H49B 107.5 . . ? Cl1 C49 H49B 107.5 . . ? H49A C49 H49B 107.0 . . ? Pd1 C HA 109.5 . . ? Pd1 C HC 109.5 . . ? HA C HC 109.5 . . ? Pd1 C HB 109.5 . . ? HA C HB 109.5 . . ? HC C HB 109.5 . . ? 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 C Pd1 P1 C25 62.5(5) . . . . ? O1 Pd1 P1 C25 -116.5(4) . . . . ? P2 Pd1 P1 C25 57.5(11) . . . . ? C Pd1 P1 C19 -55.6(5) . . . . ? O1 Pd1 P1 C19 125.4(4) . . . . ? P2 Pd1 P1 C19 -60.5(11) . . . . ? C Pd1 P1 C13 -178.5(5) . . . . ? O1 Pd1 P1 C13 2.5(4) . . . . ? P2 Pd1 P1 C13 176.5(10) . . . . ? C Pd1 P2 C31 143.2(5) . . . . ? O1 Pd1 P2 C31 -37.8(4) . . . . ? P1 Pd1 P2 C31 148.2(10) . . . . ? C Pd1 P2 C43 26.1(5) . . . . ? O1 Pd1 P2 C43 -154.9(4) . . . . ? P1 Pd1 P2 C43 31.1(12) . . . . ? C Pd1 P2 C37 -94.0(5) . . . . ? O1 Pd1 P2 C37 85.0(4) . . . . ? P1 Pd1 P2 C37 -89.1(11) . . . . ? C Pd1 O1 C6 -19(21) . . . . ? P1 Pd1 O1 C6 72.8(7) . . . . ? P2 Pd1 O1 C6 -106.6(7) . . . . ? C11 Fe1 C1 C5 -81.9(7) . . . . ? C7 Fe1 C1 C5 -54.0(12) . . . . ? C10 Fe1 C1 C5 -122.2(7) . . . . ? C8 Fe1 C1 C5 173.0(13) . . . . ? C9 Fe1 C1 C5 -162.2(7) . . . . ? C2 Fe1 C1 C5 116.8(9) . . . . ? C4 Fe1 C1 C5 36.9(6) . . . . ? C3 Fe1 C1 C5 79.8(7) . . . . ? C5 Fe1 C1 C2 -116.8(9) . . . . ? C11 Fe1 C1 C2 161.3(6) . . . . ? C7 Fe1 C1 C2 -170.8(9) . . . . ? C10 Fe1 C1 C2 121.0(7) . . . . ? C8 Fe1 C1 C2 56.2(16) . . . . ? C9 Fe1 C1 C2 81.0(8) . . . . ? C4 Fe1 C1 C2 -79.9(7) . . . . ? C3 Fe1 C1 C2 -37.0(6) . . . . ? C5 Fe1 C1 C6 119.8(11) . . . . ? C11 Fe1 C1 C6 38.0(10) . . . . ? C7 Fe1 C1 C6 65.8(13) . . . . ? C10 Fe1 C1 C6 -2.4(9) . . . . ? C8 Fe1 C1 C6 -67.2(17) . . . . ? C9 Fe1 C1 C6 -42.4(10) . . . . ? C2 Fe1 C1 C6 -123.4(11) . . . . ? C4 Fe1 C1 C6 156.7(10) . . . . ? C3 Fe1 C1 C6 -160.4(9) . . . . ? C5 C1 C2 C3 -0.9(12) . . . . ? C6 C1 C2 C3 175.6(10) . . . . ? Fe1 C1 C2 C3 59.7(8) . . . . ? C5 C1 C2 Fe1 -60.6(7) . . . . ? C6 C1 C2 Fe1 115.9(11) . . . . ? C1 Fe1 C2 C3 -119.5(9) . . . . ? C5 Fe1 C2 C3 -80.2(7) . . . . ? C11 Fe1 C2 C3 -160.3(9) . . . . ? C7 Fe1 C2 C3 47.2(17) . . . . ? C10 Fe1 C2 C3 165.4(7) . . . . ? C8 Fe1 C2 C3 81.0(8) . . . . ? C9 Fe1 C2 C3 122.5(7) . . . . ? C4 Fe1 C2 C3 -36.6(7) . . . . ? C5 Fe1 C2 C1 39.3(6) . . . . ? C11 Fe1 C2 C1 -40.8(13) . . . . ? C7 Fe1 C2 C1 166.7(13) . . . . ? C10 Fe1 C2 C1 -75.0(7) . . . . ? C8 Fe1 C2 C1 -159.5(6) . . . . ? C9 Fe1 C2 C1 -118.0(7) . . . . ? C4 Fe1 C2 C1 82.9(6) . . . . ? C3 Fe1 C2 C1 119.5(9) . . . . ? C1 C2 C3 C4 0.6(13) . . . . ? Fe1 C2 C3 C4 59.0(8) . . . . ? C1 C2 C3 Fe1 -58.4(8) . . . . ? C1 Fe1 C3 C4 -82.5(7) . . . . ? C5 Fe1 C3 C4 -37.9(7) . . . . ? C11 Fe1 C3 C4 30.8(18) . . . . ? C7 Fe1 C3 C4 75.1(8) . . . . ? C10 Fe1 C3 C4 -155.1(12) . . . . ? C8 Fe1 C3 C4 119.0(7) . . . . ? C9 Fe1 C3 C4 163.0(7) . . . . ? C2 Fe1 C3 C4 -120.4(10) . . . . ? C1 Fe1 C3 C2 37.9(6) . . . . ? C5 Fe1 C3 C2 82.5(7) . . . . ? C11 Fe1 C3 C2 151.3(14) . . . . ? C7 Fe1 C3 C2 -164.5(6) . . . . ? C10 Fe1 C3 C2 -34.7(16) . . . . ? C8 Fe1 C3 C2 -120.5(7) . . . . ? C9 Fe1 C3 C2 -76.5(8) . . . . ? C4 Fe1 C3 C2 120.4(10) . . . . ? C2 C3 C4 C5 0.0(14) . . . . ? Fe1 C3 C4 C5 58.6(8) . . . . ? C2 C3 C4 Fe1 -58.6(8) . . . . ? C1 Fe1 C4 C3 81.1(7) . . . . ? C5 Fe1 C4 C3 118.7(10) . . . . ? C11 Fe1 C4 C3 -169.1(7) . . . . ? C7 Fe1 C4 C3 -125.3(7) . . . . ? C10 Fe1 C4 C3 153.9(12) . . . . ? C8 Fe1 C4 C3 -82.1(9) . . . . ? C9 Fe1 C4 C3 -44.6(17) . . . . ? C2 Fe1 C4 C3 36.8(7) . . . . ? C1 Fe1 C4 C5 -37.6(6) . . . . ? C11 Fe1 C4 C5 72.1(8) . . . . ? C7 Fe1 C4 C5 115.9(7) . . . . ? C10 Fe1 C4 C5 35.1(16) . . . . ? C8 Fe1 C4 C5 159.2(7) . . . . ? C9 Fe1 C4 C5 -163.4(13) . . . . ? C2 Fe1 C4 C5 -81.9(7) . . . . ? C3 Fe1 C4 C5 -118.7(10) . . . . ? C3 C4 C5 C1 -0.6(13) . . . . ? Fe1 C4 C5 C1 59.1(7) . . . . ? C3 C4 C5 Fe1 -59.7(8) . . . . ? C2 C1 C5 C4 0.9(12) . . . . ? C6 C1 C5 C4 -175.7(10) . . . . ? Fe1 C1 C5 C4 -60.3(8) . . . . ? C2 C1 C5 Fe1 61.2(7) . . . . ? C6 C1 C5 Fe1 -115.4(10) . . . . ? C1 Fe1 C5 C4 120.1(10) . . . . ? C11 Fe1 C5 C4 -125.4(7) . . . . ? C7 Fe1 C5 C4 -83.4(8) . . . . ? C10 Fe1 C5 C4 -165.9(7) . . . . ? C8 Fe1 C5 C4 -53.3(16) . . . . ? C9 Fe1 C5 C4 164.6(12) . . . . ? C2 Fe1 C5 C4 80.9(7) . . . . ? C3 Fe1 C5 C4 37.5(7) . . . . ? C11 Fe1 C5 C1 114.5(7) . . . . ? C7 Fe1 C5 C1 156.5(6) . . . . ? C10 Fe1 C5 C1 74.1(8) . . . . ? C8 Fe1 C5 C1 -173.4(12) . . . . ? C9 Fe1 C5 C1 44.5(16) . . . . ? C2 Fe1 C5 C1 -39.2(6) . . . . ? C4 Fe1 C5 C1 -120.1(10) . . . . ? C3 Fe1 C5 C1 -82.6(7) . . . . ? Pd1 O1 C6 O2 9.0(14) . . . . ? Pd1 O1 C6 C1 -168.9(6) . . . . ? C5 C1 C6 O2 -178.9(10) . . . . ? C2 C1 C6 O2 5.2(17) . . . . ? Fe1 C1 C6 O2 94.6(11) . . . . ? C5 C1 C6 O1 -0.9(15) . . . . ? C2 C1 C6 O1 -176.8(10) . . . . ? Fe1 C1 C6 O1 -87.4(10) . . . . ? C1 Fe1 C7 C8 -157.6(10) . . . . ? C5 Fe1 C7 C8 163.8(7) . . . . ? C11 Fe1 C7 C8 -118.9(10) . . . . ? C10 Fe1 C7 C8 -81.8(8) . . . . ? C9 Fe1 C7 C8 -37.8(7) . . . . ? C2 Fe1 C7 C8 43.5(17) . . . . ? C4 Fe1 C7 C8 120.9(7) . . . . ? C3 Fe1 C7 C8 79.9(8) . . . . ? C1 Fe1 C7 C11 -38.7(13) . . . . ? C5 Fe1 C7 C11 -77.3(7) . . . . ? C10 Fe1 C7 C11 37.1(6) . . . . ? C8 Fe1 C7 C11 118.9(10) . . . . ? C9 Fe1 C7 C11 81.1(7) . . . . ? C2 Fe1 C7 C11 162.4(13) . . . . ? C4 Fe1 C7 C11 -120.3(7) . . . . ? C3 Fe1 C7 C11 -161.3(6) . . . . ? C1 Fe1 C7 C12 82.7(14) . . . . ? C5 Fe1 C7 C12 44.1(11) . . . . ? C11 Fe1 C7 C12 121.4(12) . . . . ? C10 Fe1 C7 C12 158.4(11) . . . . ? C8 Fe1 C7 C12 -119.8(13) . . . . ? C9 Fe1 C7 C12 -157.6(11) . . . . ? C2 Fe1 C7 C12 -76.3(18) . . . . ? C4 Fe1 C7 C12 1.1(11) . . . . ? C3 Fe1 C7 C12 -39.9(12) . . . . ? C11 C7 C8 C9 0.3(13) . . . . ? C12 C7 C8 C9 177.0(10) . . . . ? Fe1 C7 C8 C9 59.4(8) . . . . ? C11 C7 C8 Fe1 -59.1(8) . . . . ? C12 C7 C8 Fe1 117.5(11) . . . . ? C1 Fe1 C8 C9 33.2(18) . . . . ? C5 Fe1 C8 C9 -159.6(12) . . . . ? C11 Fe1 C8 C9 -80.6(8) . . . . ? C7 Fe1 C8 C9 -118.9(11) . . . . ? C10 Fe1 C8 C9 -37.5(7) . . . . ? C2 Fe1 C8 C9 75.4(9) . . . . ? C4 Fe1 C8 C9 161.3(8) . . . . ? C3 Fe1 C8 C9 118.4(8) . . . . ? C1 Fe1 C8 C7 152.1(12) . . . . ? C5 Fe1 C8 C7 -40.7(16) . . . . ? C11 Fe1 C8 C7 38.3(7) . . . . ? C10 Fe1 C8 C7 81.3(7) . . . . ? C9 Fe1 C8 C7 118.9(11) . . . . ? C2 Fe1 C8 C7 -165.8(6) . . . . ? C4 Fe1 C8 C7 -79.8(8) . . . . ? C3 Fe1 C8 C7 -122.7(7) . . . . ? C7 C8 C9 C10 -0.1(14) . . . . ? Fe1 C8 C9 C10 59.0(9) . . . . ? C7 C8 C9 Fe1 -59.1(8) . . . . ? C1 Fe1 C9 C8 -167.3(7) . . . . ? C5 Fe1 C9 C8 159.9(12) . . . . ? C11 Fe1 C9 C8 82.8(8) . . . . ? C7 Fe1 C9 C8 38.1(7) . . . . ? C10 Fe1 C9 C8 119.7(11) . . . . ? C2 Fe1 C9 C8 -124.3(8) . . . . ? C4 Fe1 C9 C8 -50.1(18) . . . . ? C3 Fe1 C9 C8 -83.2(9) . . . . ? C1 Fe1 C9 C10 73.0(9) . . . . ? C5 Fe1 C9 C10 40.2(17) . . . . ? C11 Fe1 C9 C10 -36.9(7) . . . . ? C7 Fe1 C9 C10 -81.6(8) . . . . ? C8 Fe1 C9 C10 -119.7(11) . . . . ? C2 Fe1 C9 C10 116.0(7) . . . . ? C4 Fe1 C9 C10 -169.9(13) . . . . ? C3 Fe1 C9 C10 157.1(7) . . . . ? C8 C9 C10 C11 -0.1(14) . . . . ? Fe1 C9 C10 C11 58.9(9) . . . . ? C8 C9 C10 Fe1 -59.1(9) . . . . ? C1 Fe1 C10 C11 117.0(7) . . . . ? C5 Fe1 C10 C11 76.4(8) . . . . ? C7 Fe1 C10 C11 -38.3(7) . . . . ? C8 Fe1 C10 C11 -82.5(8) . . . . ? C9 Fe1 C10 C11 -119.8(11) . . . . ? C2 Fe1 C10 C11 157.7(7) . . . . ? C4 Fe1 C10 C11 50.6(16) . . . . ? C3 Fe1 C10 C11 -177.2(11) . . . . ? C1 Fe1 C10 C9 -123.2(7) . . . . ? C5 Fe1 C10 C9 -163.8(7) . . . . ? C11 Fe1 C10 C9 119.8(11) . . . . ? C7 Fe1 C10 C9 81.6(8) . . . . ? C8 Fe1 C10 C9 37.4(7) . . . . ? C2 Fe1 C10 C9 -82.5(8) . . . . ? C4 Fe1 C10 C9 170.4(12) . . . . ? C3 Fe1 C10 C9 -57.3(16) . . . . ? C9 C10 C11 C7 0.3(14) . . . . ? Fe1 C10 C11 C7 59.3(8) . . . . ? C9 C10 C11 Fe1 -59.0(9) . . . . ? C8 C7 C11 C10 -0.4(13) . . . . ? C12 C7 C11 C10 -177.0(11) . . . . ? Fe1 C7 C11 C10 -59.9(8) . . . . ? C8 C7 C11 Fe1 59.5(8) . . . . ? C12 C7 C11 Fe1 -117.1(11) . . . . ? C1 Fe1 C11 C10 -77.9(8) . . . . ? C5 Fe1 C11 C10 -120.4(8) . . . . ? C7 Fe1 C11 C10 119.3(10) . . . . ? C8 Fe1 C11 C10 81.4(8) . . . . ? C9 Fe1 C11 C10 37.6(7) . . . . ? C2 Fe1 C11 C10 -49.0(13) . . . . ? C4 Fe1 C11 C10 -160.1(7) . . . . ? C3 Fe1 C11 C10 176.5(14) . . . . ? C1 Fe1 C11 C7 162.7(6) . . . . ? C5 Fe1 C11 C7 120.2(6) . . . . ? C10 Fe1 C11 C7 -119.3(10) . . . . ? C8 Fe1 C11 C7 -38.0(6) . . . . ? C9 Fe1 C11 C7 -81.7(7) . . . . ? C2 Fe1 C11 C7 -168.3(9) . . . . ? C4 Fe1 C11 C7 80.6(8) . . . . ? C3 Fe1 C11 C7 57.2(17) . . . . ? C8 C7 C12 O4 17.1(18) . . . . ? C11 C7 C12 O4 -166.9(11) . . . . ? Fe1 C7 C12 O4 105.0(12) . . . . ? C8 C7 C12 O3 -162.5(11) . . . . ? C11 C7 C12 O3 13.5(16) . . . . ? Fe1 C7 C12 O3 -74.6(12) . . . . ? C25 P1 C13 C14 167.5(9) . . . . ? C19 P1 C13 C14 -83.3(9) . . . . ? Pd1 P1 C13 C14 47.4(10) . . . . ? C25 P1 C13 C18 -17.9(10) . . . . ? C19 P1 C13 C18 91.3(10) . . . . ? Pd1 P1 C13 C18 -138.0(8) . . . . ? C18 C13 C14 C15 4.3(16) . . . . ? P1 C13 C14 C15 179.1(9) . . . . ? C13 C14 C15 C16 -4.6(18) . . . . ? C14 C15 C16 C17 2(2) . . . . ? C15 C16 C17 C18 1(2) . . . . ? C16 C17 C18 C13 -1(2) . . . . ? C14 C13 C18 C17 -1.5(18) . . . . ? P1 C13 C18 C17 -176.2(10) . . . . ? C25 P1 C19 C24 -118.5(9) . . . . ? C13 P1 C19 C24 131.0(9) . . . . ? Pd1 P1 C19 C24 1.7(10) . . . . ? C25 P1 C19 C20 61.3(9) . . . . ? C13 P1 C19 C20 -49.3(9) . . . . ? Pd1 P1 C19 C20 -178.5(7) . . . . ? C24 C19 C20 C21 4.0(15) . . . . ? P1 C19 C20 C21 -175.8(8) . . . . ? C19 C20 C21 C22 0.0(17) . . . . ? C20 C21 C22 C23 -4.2(18) . . . . ? C21 C22 C23 C24 4.3(18) . . . . ? C22 C23 C24 C19 -0.2(18) . . . . ? C20 C19 C24 C23 -3.8(16) . . . . ? P1 C19 C24 C23 176.0(9) . . . . ? C19 P1 C25 C26 8.1(9) . . . . ? C13 P1 C25 C26 116.3(9) . . . . ? Pd1 P1 C25 C26 -118.6(8) . . . . ? C19 P1 C25 C30 -174.9(7) . . . . ? C13 P1 C25 C30 -66.6(8) . . . . ? Pd1 P1 C25 C30 58.4(8) . . . . ? C30 C25 C26 C27 -0.8(14) . . . . ? P1 C25 C26 C27 176.2(7) . . . . ? C25 C26 C27 C28 -0.2(15) . . . . ? C26 C27 C28 C29 1.0(15) . . . . ? C27 C28 C29 C30 -0.9(16) . . . . ? C28 C29 C30 C25 -0.1(15) . . . . ? C26 C25 C30 C29 0.9(14) . . . . ? P1 C25 C30 C29 -176.3(7) . . . . ? C43 P2 C31 C36 104.2(9) . . . . ? C37 P2 C31 C36 -145.3(8) . . . . ? Pd1 P2 C31 C36 -20.0(10) . . . . ? C43 P2 C31 C32 -71.6(11) . . . . ? C37 P2 C31 C32 38.9(11) . . . . ? Pd1 P2 C31 C32 164.2(9) . . . . ? C36 C31 C32 C33 -0.9(18) . . . . ? P2 C31 C32 C33 175.0(9) . . . . ? C31 C32 C33 C34 -1.0(19) . . . . ? C32 C33 C34 C35 1.3(19) . . . . ? C33 C34 C35 C36 0.1(17) . . . . ? C34 C35 C36 C31 -2.1(16) . . . . ? C32 C31 C36 C35 2.4(16) . . . . ? P2 C31 C36 C35 -173.7(8) . . . . ? C31 P2 C37 C38 115.3(9) . . . . ? C43 P2 C37 C38 -135.9(8) . . . . ? Pd1 P2 C37 C38 -10.1(9) . . . . ? C31 P2 C37 C42 -72.5(10) . . . . ? C43 P2 C37 C42 36.4(11) . . . . ? Pd1 P2 C37 C42 162.1(9) . . . . ? C42 C37 C38 C39 2.4(16) . . . . ? P2 C37 C38 C39 174.9(8) . . . . ? C37 C38 C39 C40 0.7(18) . . . . ? C38 C39 C40 C41 -3(2) . . . . ? C39 C40 C41 C42 1(2) . . . . ? C40 C41 C42 C37 2(2) . . . . ? C38 C37 C42 C41 -3.6(18) . . . . ? P2 C37 C42 C41 -175.6(10) . . . . ? C31 P2 C43 C48 148.1(9) . . . . ? C37 P2 C43 C48 35.2(10) . . . . ? Pd1 P2 C43 C48 -89.1(9) . . . . ? C31 P2 C43 C44 -41.6(9) . . . . ? C37 P2 C43 C44 -154.4(8) . . . . ? Pd1 P2 C43 C44 81.2(8) . . . . ? C48 C43 C44 C45 -0.7(15) . . . . ? P2 C43 C44 C45 -171.6(9) . . . . ? C43 C44 C45 C46 0.7(17) . . . . ? C44 C45 C46 C47 -1.3(18) . . . . ? C45 C46 C47 C48 1.8(18) . . . . ? C44 C43 C48 C47 1.3(15) . . . . ? P2 C43 C48 C47 171.8(8) . . . . ? C46 C47 C48 C43 -1.9(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.84 1.79 2.617(10) 169.8 2_646 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.639 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.099 data_a _database_code_depnum_ccdc_archive 'CCDC 917455' #TrackingRef 'web_deposit_cif_file_0_YudongCai_1356446440.a2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 Cl2 N2 O2 Pd' _chemical_formula_weight 607.87 _chemical_absolute_configuration ad 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.754(2) _cell_length_b 11.776(2) _cell_length_c 12.101(2) _cell_angle_alpha 66.21(3) _cell_angle_beta 77.67(3) _cell_angle_gamma 89.24(3) _cell_volume 1365.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5406 _cell_measurement_theta_min 1.8888 _cell_measurement_theta_max 27.4812 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6389 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17486 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11389 _reflns_number_gt 11057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.2526P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.030(19) _refine_ls_number_reflns 11389 _refine_ls_number_parameters 641 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.67633(2) 0.976358(19) 0.805646(19) 0.02178(7) Uani 1 1 d . . . Pd2 Pd 0.23607(2) 0.98485(2) 0.55102(2) 0.02174(7) Uani 1 1 d . . . Cl1 Cl 0.96166(15) 0.99919(15) -0.00077(13) 0.0611(4) Uani 1 1 d . . . Cl2 Cl 1.19842(16) 0.95822(15) 0.08449(12) 0.0630(4) Uani 1 1 d . . . Cl3 Cl 0.61446(15) 0.98129(15) 0.30798(17) 0.0676(4) Uani 1 1 d . . . Cl4 Cl 0.88493(14) 0.97626(13) 0.30792(11) 0.0494(3) Uani 1 1 d . . . O1 O 0.7365(3) 0.8287(2) 0.7647(2) 0.0266(6) Uani 1 1 d . . . O2 O 0.7464(3) 0.7219(3) 0.6135(3) 0.0283(7) Uani 1 1 d . . . H2 H 0.7529 0.7755 0.6417 0.034 Uiso 1 1 d R . . O3 O 0.2771(3) 1.1357(2) 0.5849(2) 0.0264(6) Uani 1 1 d . . . O4 O 0.2193(3) 1.2362(3) 0.7385(3) 0.0287(7) Uani 1 1 d . . . H4 H 0.2474 1.1888 0.7041 0.034 Uiso 1 1 d R . . N1 N 0.8045(3) 1.1139(3) 0.6386(3) 0.0263(7) Uani 1 1 d . . . N2 N 0.6105(3) 1.1317(3) 0.8339(3) 0.0257(7) Uani 1 1 d . . . N3 N 0.1849(3) 0.8263(3) 0.5313(3) 0.0242(7) Uani 1 1 d . . . N4 N 0.2936(3) 0.8537(3) 0.7167(3) 0.0250(7) Uani 1 1 d . . . C1 C 0.7846(3) 0.7344(3) 0.8469(3) 0.0217(7) Uani 1 1 d . . . C2 C 0.8740(4) 0.7614(4) 0.9055(4) 0.0268(8) Uani 1 1 d . . . H2A H 0.8936 0.8455 0.8906 0.032 Uiso 1 1 calc R . . C3 C 0.9328(4) 0.6694(4) 0.9830(4) 0.0251(8) Uani 1 1 d . . . H3 H 0.9913 0.6899 1.0221 0.030 Uiso 1 1 calc R . . C4 C 0.9068(3) 0.5439(4) 1.0053(3) 0.0227(8) Uani 1 1 d . . . C5 C 0.9678(4) 0.4474(4) 1.0829(4) 0.0285(9) Uani 1 1 d . . . H5 H 1.0311 0.4678 1.1175 0.034 Uiso 1 1 calc R . . C6 C 0.9382(4) 0.3252(4) 1.1097(4) 0.0307(9) Uani 1 1 d . . . H6 H 0.9773 0.2614 1.1657 0.037 Uiso 1 1 calc R . . C7 C 0.8499(4) 0.2950(4) 1.0541(4) 0.0286(9) Uani 1 1 d . . . H7 H 0.8313 0.2103 1.0703 0.034 Uiso 1 1 calc R . . C8 C 0.7902(4) 0.3859(4) 0.9768(4) 0.0248(8) Uani 1 1 d . . . H8 H 0.7318 0.3631 0.9390 0.030 Uiso 1 1 calc R . . C9 C 0.8128(3) 0.5141(4) 0.9509(3) 0.0206(7) Uani 1 1 d . . . C10 C 0.7486(3) 0.6108(3) 0.8739(3) 0.0203(7) Uani 1 1 d . . . C11 C 0.6461(4) 0.5801(4) 0.8222(4) 0.0198(8) Uani 1 1 d . . . C12 C 0.6553(4) 0.6296(4) 0.6950(3) 0.0230(8) Uani 1 1 d . . . C13 C 0.5694(4) 0.5860(4) 0.6432(4) 0.0260(8) Uani 1 1 d . . . H13 H 0.5822 0.6162 0.5557 0.031 Uiso 1 1 calc R . . C14 C 0.4699(4) 0.5019(4) 0.7173(4) 0.0272(8) Uani 1 1 d . . . H14 H 0.4155 0.4709 0.6816 0.033 Uiso 1 1 calc R . . C15 C 0.4464(4) 0.4600(4) 0.8477(4) 0.0246(8) Uani 1 1 d . . . C16 C 0.3357(4) 0.3802(4) 0.9271(4) 0.0313(9) Uani 1 1 d . . . H16 H 0.2773 0.3532 0.8921 0.038 Uiso 1 1 calc R . . C17 C 0.3127(4) 0.3419(4) 1.0532(4) 0.0340(10) Uani 1 1 d . . . H17 H 0.2381 0.2897 1.1052 0.041 Uiso 1 1 calc R . . C18 C 0.4002(4) 0.3805(4) 1.1051(4) 0.0313(9) Uani 1 1 d . . . H18 H 0.3849 0.3524 1.1927 0.038 Uiso 1 1 calc R . . C19 C 0.5062(4) 0.4573(4) 1.0320(4) 0.0275(8) Uani 1 1 d . . . H19 H 0.5625 0.4838 1.0693 0.033 Uiso 1 1 calc R . . C20 C 0.5346(4) 0.4989(3) 0.9004(4) 0.0210(7) Uani 1 1 d . . . C21 C 0.5581(4) 0.8552(4) 0.9635(4) 0.0368(10) Uani 1 1 d . . . H21A H 0.5552 0.7727 0.9620 0.055 Uiso 1 1 calc R . . H21B H 0.4722 0.8842 0.9695 0.055 Uiso 1 1 calc R . . H21C H 0.5900 0.8501 1.0353 0.055 Uiso 1 1 calc R . . C22 C 0.9359(4) 1.1129(4) 0.6557(4) 0.0355(10) Uani 1 1 d . . . H22A H 0.9690 1.0327 0.6636 0.053 Uiso 1 1 calc R . . H22C H 0.9365 1.1252 0.7310 0.053 Uiso 1 1 calc R . . H22B H 0.9900 1.1801 0.5839 0.053 Uiso 1 1 calc R . . C23 C 0.8040(5) 1.0917(4) 0.5271(4) 0.0352(10) Uani 1 1 d . . . H23B H 0.8321 1.0089 0.5393 0.053 Uiso 1 1 calc R . . H23C H 0.8621 1.1549 0.4551 0.053 Uiso 1 1 calc R . . H23A H 0.7174 1.0966 0.5128 0.053 Uiso 1 1 calc R . . C24 C 0.7522(4) 1.2349(4) 0.6250(4) 0.0311(9) Uani 1 1 d . . . H24A H 0.6795 1.2466 0.5842 0.037 Uiso 1 1 calc R . . H24B H 0.8188 1.3038 0.5724 0.037 Uiso 1 1 calc R . . C25 C 0.7082(4) 1.2368(4) 0.7513(4) 0.0313(10) Uani 1 1 d . . . H25B H 0.7823 1.2306 0.7893 0.038 Uiso 1 1 calc R . . H25A H 0.6714 1.3167 0.7422 0.038 Uiso 1 1 calc R . . C26 C 0.4861(4) 1.1570(4) 0.7970(4) 0.0334(9) Uani 1 1 d . . . H26A H 0.4947 1.1591 0.7139 0.050 Uiso 1 1 calc R . . H26C H 0.4609 1.2374 0.7964 0.050 Uiso 1 1 calc R . . H26B H 0.4208 1.0910 0.8563 0.050 Uiso 1 1 calc R . . C27 C 0.5919(4) 1.1219(4) 0.9624(4) 0.0354(10) Uani 1 1 d . . . H27A H 0.5274 1.0535 1.0179 0.053 Uiso 1 1 calc R . . H27C H 0.5633 1.2001 0.9655 0.053 Uiso 1 1 calc R . . H27B H 0.6728 1.1056 0.9888 0.053 Uiso 1 1 calc R . . C28 C 0.3634(4) 1.2274(4) 0.5021(3) 0.0237(8) Uani 1 1 d . . . C29 C 0.4786(4) 1.1986(4) 0.4388(4) 0.0290(9) Uani 1 1 d . . . H29 H 0.4897 1.1146 0.4510 0.035 Uiso 1 1 calc R . . C30 C 0.5730(4) 1.2882(4) 0.3616(4) 0.0296(9) Uani 1 1 d . . . H30 H 0.6475 1.2669 0.3182 0.036 Uiso 1 1 calc R . . C31 C 0.5606(3) 1.4131(4) 0.3456(3) 0.0224(8) Uani 1 1 d . . . C32 C 0.6608(4) 1.5074(4) 0.2698(4) 0.0311(9) Uani 1 1 d . . . H32 H 0.7383 1.4852 0.2318 0.037 Uiso 1 1 calc R . . C33 C 0.6482(4) 1.6282(4) 0.2508(4) 0.0341(10) Uani 1 1 d . . . H33 H 0.7147 1.6905 0.1971 0.041 Uiso 1 1 calc R . . C34 C 0.5356(4) 1.6602(4) 0.3113(4) 0.0332(9) Uani 1 1 d . . . H34 H 0.5274 1.7444 0.2996 0.040 Uiso 1 1 calc R . . C35 C 0.4376(4) 1.5721(4) 0.3869(3) 0.0240(8) Uani 1 1 d . . . H35 H 0.3633 1.5959 0.4282 0.029 Uiso 1 1 calc R . . C36 C 0.4455(3) 1.4454(3) 0.4043(3) 0.0193(7) Uani 1 1 d . . . C37 C 0.3431(3) 1.3508(3) 0.4799(3) 0.0204(7) Uani 1 1 d . . . C38 C 0.2168(4) 1.3849(3) 0.5334(3) 0.0190(8) Uani 1 1 d . . . C39 C 0.1645(4) 1.3306(3) 0.6605(4) 0.0224(8) Uani 1 1 d . . . C40 C 0.0534(4) 1.3713(4) 0.7131(4) 0.0288(9) Uani 1 1 d . . . H40 H 0.0238 1.3374 0.8007 0.035 Uiso 1 1 calc R . . C41 C -0.0127(4) 1.4585(4) 0.6405(4) 0.0278(9) Uani 1 1 d . . . H41 H -0.0868 1.4862 0.6778 0.033 Uiso 1 1 calc R . . C42 C 0.0285(4) 1.5085(4) 0.5091(4) 0.0251(8) Uani 1 1 d . . . C43 C -0.0427(4) 1.5934(4) 0.4319(4) 0.0325(9) Uani 1 1 d . . . H43 H -0.1208 1.6165 0.4680 0.039 Uiso 1 1 calc R . . C44 C -0.0007(5) 1.6430(4) 0.3054(4) 0.0355(10) Uani 1 1 d . . . H44 H -0.0482 1.7015 0.2541 0.043 Uiso 1 1 calc R . . C45 C 0.1132(4) 1.6066(4) 0.2523(4) 0.0327(9) Uani 1 1 d . . . H45 H 0.1420 1.6409 0.1646 0.039 Uiso 1 1 calc R . . C46 C 0.1827(4) 1.5240(4) 0.3229(4) 0.0256(8) Uani 1 1 d . . . H46 H 0.2586 1.5002 0.2840 0.031 Uiso 1 1 calc R . . C47 C 0.1442(4) 1.4715(3) 0.4555(3) 0.0223(8) Uani 1 1 d . . . C48 C 0.1876(4) 1.1017(4) 0.3937(4) 0.0339(10) Uani 1 1 d . . . H48B H 0.2545 1.1080 0.3219 0.051 Uiso 1 1 calc R . . H48C H 0.1783 1.1842 0.3945 0.051 Uiso 1 1 calc R . . H48A H 0.1066 1.0694 0.3883 0.051 Uiso 1 1 calc R . . C49 C 0.2215(4) 0.8318(4) 0.4037(4) 0.0339(10) Uani 1 1 d . . . H49A H 0.1922 0.7532 0.4041 0.051 Uiso 1 1 calc R . . H49C H 0.3146 0.8453 0.3745 0.051 Uiso 1 1 calc R . . H49B H 0.1820 0.9006 0.3484 0.051 Uiso 1 1 calc R . . C50 C 0.0437(4) 0.7992(4) 0.5762(4) 0.0315(9) Uani 1 1 d . . . H50B H 0.0014 0.8657 0.5215 0.047 Uiso 1 1 calc R . . H50C H 0.0181 0.7945 0.6608 0.047 Uiso 1 1 calc R . . H50A H 0.0190 0.7195 0.5759 0.047 Uiso 1 1 calc R . . C51 C 0.2501(4) 0.7242(4) 0.6110(4) 0.0276(9) Uani 1 1 d . . . H51B H 0.3411 0.7308 0.5688 0.033 Uiso 1 1 calc R . . H51A H 0.2105 0.6430 0.6240 0.033 Uiso 1 1 calc R . . C52 C 0.2410(4) 0.7295(4) 0.7359(4) 0.0276(8) Uani 1 1 d . . . H52A H 0.1506 0.7146 0.7821 0.033 Uiso 1 1 calc R . . H52B H 0.2896 0.6639 0.7856 0.033 Uiso 1 1 calc R . . C53 C 0.4348(4) 0.8595(4) 0.6927(4) 0.0346(10) Uani 1 1 d . . . H53B H 0.4609 0.7985 0.7655 0.052 Uiso 1 1 calc R . . H53C H 0.4682 0.9432 0.6762 0.052 Uiso 1 1 calc R . . H53A H 0.4687 0.8407 0.6207 0.052 Uiso 1 1 calc R . . C54 C 0.2442(4) 0.8772(4) 0.8278(4) 0.0336(9) Uani 1 1 d . . . H54A H 0.1510 0.8773 0.8424 0.050 Uiso 1 1 calc R . . H54C H 0.2810 0.9582 0.8156 0.050 Uiso 1 1 calc R . . H54B H 0.2675 0.8116 0.8997 0.050 Uiso 1 1 calc R . . C55 C 1.0953(5) 1.0673(5) 0.0196(5) 0.0452(12) Uani 1 1 d . . . H55A H 1.1423 1.1298 -0.0618 0.054 Uiso 1 1 calc R . . H55B H 1.0656 1.1110 0.0740 0.054 Uiso 1 1 calc R . . C56 C 0.7468(5) 0.8927(5) 0.3215(5) 0.0477(13) Uani 1 1 d . . . H56B H 0.7276 0.8205 0.4030 0.057 Uiso 1 1 calc R . . H56A H 0.7618 0.8602 0.2564 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02192(15) 0.01960(15) 0.02454(15) -0.00903(12) -0.00687(12) 0.00240(11) Pd2 0.02161(15) 0.01941(15) 0.02381(15) -0.00854(12) -0.00509(12) 0.00293(12) Cl1 0.0707(10) 0.0754(10) 0.0514(7) -0.0397(7) -0.0147(7) 0.0023(8) Cl2 0.0743(11) 0.0725(10) 0.0364(7) -0.0171(7) -0.0120(7) 0.0179(8) Cl3 0.0543(9) 0.0680(10) 0.0965(13) -0.0501(10) -0.0178(8) 0.0162(8) Cl4 0.0542(8) 0.0586(8) 0.0347(6) -0.0193(6) -0.0079(6) -0.0048(6) O1 0.0368(16) 0.0185(13) 0.0264(14) -0.0100(12) -0.0099(12) 0.0050(12) O2 0.0323(16) 0.0276(16) 0.0227(14) -0.0092(12) -0.0033(13) -0.0037(13) O3 0.0295(15) 0.0190(13) 0.0292(14) -0.0118(12) 0.0005(12) -0.0007(11) O4 0.0334(17) 0.0275(15) 0.0229(14) -0.0097(12) -0.0032(13) 0.0071(13) N1 0.0257(17) 0.0228(16) 0.0302(18) -0.0107(14) -0.0064(14) 0.0039(13) N2 0.0242(16) 0.0274(17) 0.0296(17) -0.0143(14) -0.0091(14) 0.0053(14) N3 0.0247(17) 0.0251(17) 0.0260(16) -0.0129(14) -0.0071(13) 0.0038(13) N4 0.0266(17) 0.0225(16) 0.0279(17) -0.0106(14) -0.0094(14) 0.0013(13) C1 0.0206(18) 0.0234(19) 0.0210(18) -0.0098(16) -0.0031(14) 0.0046(15) C2 0.028(2) 0.0235(19) 0.030(2) -0.0123(17) -0.0062(16) -0.0034(16) C3 0.0212(18) 0.031(2) 0.0275(19) -0.0146(17) -0.0086(15) 0.0007(16) C4 0.0203(18) 0.0231(19) 0.0227(18) -0.0087(16) -0.0020(14) 0.0022(15) C5 0.0228(19) 0.034(2) 0.031(2) -0.0142(18) -0.0102(16) 0.0053(17) C6 0.032(2) 0.027(2) 0.033(2) -0.0088(19) -0.0135(18) 0.0094(17) C7 0.029(2) 0.023(2) 0.034(2) -0.0102(18) -0.0104(18) 0.0063(17) C8 0.0206(18) 0.027(2) 0.029(2) -0.0128(17) -0.0074(15) 0.0036(15) C9 0.0148(16) 0.0261(19) 0.0211(17) -0.0111(15) -0.0015(14) 0.0048(14) C10 0.0172(17) 0.0223(18) 0.0184(17) -0.0064(15) -0.0020(14) 0.0003(14) C11 0.0182(19) 0.0191(18) 0.0245(19) -0.0099(16) -0.0081(15) 0.0078(15) C12 0.0216(19) 0.0231(19) 0.0247(19) -0.0109(16) -0.0043(15) 0.0045(15) C13 0.030(2) 0.027(2) 0.0231(19) -0.0106(16) -0.0103(16) 0.0080(16) C14 0.030(2) 0.027(2) 0.034(2) -0.0177(18) -0.0163(17) 0.0073(17) C15 0.0230(19) 0.0216(19) 0.029(2) -0.0098(16) -0.0072(16) 0.0047(15) C16 0.0195(19) 0.031(2) 0.046(2) -0.017(2) -0.0106(18) 0.0014(16) C17 0.027(2) 0.031(2) 0.037(2) -0.009(2) -0.004(2) -0.0039(19) C18 0.028(2) 0.031(2) 0.027(2) -0.0076(18) 0.0016(17) 0.0005(17) C19 0.027(2) 0.028(2) 0.028(2) -0.0120(17) -0.0055(16) 0.0023(17) C20 0.0190(17) 0.0222(18) 0.0236(17) -0.0093(15) -0.0086(14) 0.0043(14) C21 0.032(2) 0.032(2) 0.037(2) -0.008(2) -0.0019(19) 0.0024(18) C22 0.029(2) 0.033(2) 0.039(2) -0.011(2) -0.0044(18) 0.0027(18) C23 0.046(3) 0.032(2) 0.030(2) -0.0140(19) -0.0109(19) 0.005(2) C24 0.038(2) 0.021(2) 0.030(2) -0.0068(17) -0.0073(19) 0.0009(18) C25 0.029(2) 0.026(2) 0.041(2) -0.018(2) -0.004(2) -0.0014(19) C26 0.028(2) 0.032(2) 0.047(3) -0.019(2) -0.0160(19) 0.0078(18) C27 0.035(2) 0.045(3) 0.035(2) -0.028(2) -0.0041(19) 0.003(2) C28 0.0265(19) 0.0232(19) 0.0234(18) -0.0107(16) -0.0077(15) 0.0021(15) C29 0.031(2) 0.025(2) 0.029(2) -0.0094(17) -0.0070(17) 0.0091(17) C30 0.0238(19) 0.040(2) 0.028(2) -0.0180(18) -0.0023(16) 0.0057(17) C31 0.0211(18) 0.029(2) 0.0178(17) -0.0104(16) -0.0056(14) 0.0035(15) C32 0.023(2) 0.041(2) 0.028(2) -0.0154(19) 0.0006(16) -0.0001(18) C33 0.028(2) 0.040(3) 0.027(2) -0.009(2) -0.0001(18) -0.0108(19) C34 0.038(2) 0.029(2) 0.029(2) -0.0077(18) -0.0093(19) -0.0041(19) C35 0.0213(18) 0.027(2) 0.0232(18) -0.0102(16) -0.0038(15) -0.0008(15) C36 0.0203(18) 0.0242(19) 0.0156(16) -0.0093(15) -0.0060(14) 0.0004(15) C37 0.0208(18) 0.0231(19) 0.0175(16) -0.0085(15) -0.0049(14) 0.0028(15) C38 0.0203(19) 0.0169(18) 0.0205(18) -0.0089(15) -0.0037(15) 0.0016(15) C39 0.0236(19) 0.0213(18) 0.0269(19) -0.0136(16) -0.0077(15) 0.0014(15) C40 0.028(2) 0.030(2) 0.027(2) -0.0132(18) 0.0013(16) -0.0046(17) C41 0.0169(17) 0.026(2) 0.042(2) -0.0190(19) 0.0012(16) 0.0005(15) C42 0.0229(19) 0.0197(19) 0.036(2) -0.0140(17) -0.0078(16) 0.0015(15) C43 0.024(2) 0.033(2) 0.048(3) -0.023(2) -0.0116(18) 0.0097(17) C44 0.043(3) 0.034(2) 0.038(2) -0.017(2) -0.024(2) 0.015(2) C45 0.037(2) 0.036(2) 0.028(2) -0.0111(19) -0.0160(18) 0.0046(19) C46 0.028(2) 0.027(2) 0.0257(19) -0.0135(17) -0.0105(16) 0.0055(16) C47 0.0227(18) 0.0219(19) 0.0270(19) -0.0139(16) -0.0071(15) 0.0016(15) C48 0.038(2) 0.029(2) 0.029(2) -0.0044(18) -0.0123(18) 0.0052(19) C49 0.037(2) 0.038(2) 0.031(2) -0.019(2) -0.0063(18) 0.0060(19) C50 0.0217(19) 0.034(2) 0.041(2) -0.017(2) -0.0068(17) 0.0018(17) C51 0.032(2) 0.021(2) 0.033(2) -0.0134(18) -0.0093(19) 0.0078(18) C52 0.035(2) 0.0182(19) 0.029(2) -0.0088(16) -0.0085(18) 0.0061(17) C53 0.027(2) 0.040(2) 0.042(2) -0.018(2) -0.0159(19) 0.0101(19) C54 0.038(2) 0.035(2) 0.029(2) -0.0148(19) -0.0065(18) -0.0016(19) C55 0.059(3) 0.035(3) 0.039(3) -0.016(2) -0.004(2) -0.002(3) C56 0.056(3) 0.034(3) 0.048(3) -0.014(2) -0.010(3) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C21 2.028(4) . ? Pd1 O1 2.054(3) . ? Pd1 N2 2.081(3) . ? Pd1 N1 2.200(3) . ? Pd2 C48 2.020(4) . ? Pd2 O3 2.050(3) . ? Pd2 N3 2.071(3) . ? Pd2 N4 2.190(3) . ? Cl1 C55 1.764(6) . ? Cl2 C55 1.736(6) . ? Cl3 C56 1.750(6) . ? Cl4 C56 1.734(5) . ? O1 C1 1.343(4) . ? O2 C12 1.365(5) . ? O2 H2 0.8399 . ? O3 C28 1.337(5) . ? O4 C39 1.359(5) . ? O4 H4 0.8401 . ? N1 C22 1.471(5) . ? N1 C23 1.475(5) . ? N1 C24 1.484(5) . ? N2 C27 1.480(5) . ? N2 C26 1.489(5) . ? N2 C25 1.491(5) . ? N3 C51 1.483(5) . ? N3 C49 1.484(5) . ? N3 C50 1.491(5) . ? N4 C54 1.470(5) . ? N4 C53 1.481(5) . ? N4 C52 1.484(5) . ? C1 C10 1.397(5) . ? C1 C2 1.418(5) . ? C2 C3 1.367(6) . ? C2 H2A 0.9500 . ? C3 C4 1.411(5) . ? C3 H3 0.9500 . ? C4 C5 1.410(5) . ? C4 C9 1.434(5) . ? C5 C6 1.367(6) . ? C5 H5 0.9500 . ? C6 C7 1.399(6) . ? C6 H6 0.9500 . ? C7 C8 1.366(6) . ? C7 H7 0.9500 . ? C8 C9 1.425(5) . ? C8 H8 0.9500 . ? C9 C10 1.428(5) . ? C10 C11 1.492(5) . ? C11 C12 1.389(5) . ? C11 C20 1.436(5) . ? C12 C13 1.425(5) . ? C13 C14 1.353(6) . ? C13 H13 0.9500 . ? C14 C15 1.415(6) . ? C14 H14 0.9500 . ? C15 C20 1.422(5) . ? C15 C16 1.427(5) . ? C16 C17 1.371(6) . ? C16 H16 0.9500 . ? C17 C18 1.408(6) . ? C17 H17 0.9500 . ? C18 C19 1.362(5) . ? C18 H18 0.9500 . ? C19 C20 1.427(5) . ? C19 H19 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23A 0.9800 . ? C24 C25 1.509(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25B 0.9900 . ? C25 H25A 0.9900 . ? C26 H26A 0.9800 . ? C26 H26C 0.9800 . ? C26 H26B 0.9800 . ? C27 H27A 0.9800 . ? C27 H27C 0.9800 . ? C27 H27B 0.9800 . ? C28 C37 1.390(5) . ? C28 C29 1.424(5) . ? C29 C30 1.358(6) . ? C29 H29 0.9500 . ? C30 C31 1.413(6) . ? C30 H30 0.9500 . ? C31 C36 1.417(5) . ? C31 C32 1.422(5) . ? C32 C33 1.357(6) . ? C32 H32 0.9500 . ? C33 C34 1.405(6) . ? C33 H33 0.9500 . ? C34 C35 1.370(6) . ? C34 H34 0.9500 . ? C35 C36 1.425(5) . ? C35 H35 0.9500 . ? C36 C37 1.439(5) . ? C37 C38 1.498(5) . ? C38 C39 1.392(5) . ? C38 C47 1.435(5) . ? C39 C40 1.403(5) . ? C40 C41 1.360(6) . ? C40 H40 0.9500 . ? C41 C42 1.422(6) . ? C41 H41 0.9500 . ? C42 C43 1.411(6) . ? C42 C47 1.424(5) . ? C43 C44 1.371(6) . ? C43 H43 0.9500 . ? C44 C45 1.403(6) . ? C44 H44 0.9500 . ? C45 C46 1.348(6) . ? C45 H45 0.9500 . ? C46 C47 1.432(5) . ? C46 H46 0.9500 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C48 H48A 0.9800 . ? C49 H49A 0.9800 . ? C49 H49C 0.9800 . ? C49 H49B 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C50 H50A 0.9800 . ? C51 C52 1.521(6) . ? C51 H51B 0.9900 . ? C51 H51A 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C53 H53A 0.9800 . ? C54 H54A 0.9800 . ? C54 H54C 0.9800 . ? C54 H54B 0.9800 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56B 0.9900 . ? C56 H56A 0.9900 . ? 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 C21 Pd1 O1 88.99(15) . . ? C21 Pd1 N2 93.30(16) . . ? O1 Pd1 N2 175.43(12) . . ? C21 Pd1 N1 177.30(16) . . ? O1 Pd1 N1 93.46(12) . . ? N2 Pd1 N1 84.33(13) . . ? C48 Pd2 O3 89.07(15) . . ? C48 Pd2 N3 93.73(16) . . ? O3 Pd2 N3 175.30(12) . . ? C48 Pd2 N4 177.32(16) . . ? O3 Pd2 N4 92.80(12) . . ? N3 Pd2 N4 84.52(12) . . ? C1 O1 Pd1 119.5(2) . . ? C12 O2 H2 109.4 . . ? C28 O3 Pd2 120.6(2) . . ? C39 O4 H4 109.5 . . ? C22 N1 C23 109.2(3) . . ? C22 N1 C24 110.8(3) . . ? C23 N1 C24 109.8(3) . . ? C22 N1 Pd1 110.6(3) . . ? C23 N1 Pd1 112.2(3) . . ? C24 N1 Pd1 104.3(2) . . ? C27 N2 C26 107.9(3) . . ? C27 N2 C25 108.4(3) . . ? C26 N2 C25 110.2(3) . . ? C27 N2 Pd1 115.8(3) . . ? C26 N2 Pd1 108.5(2) . . ? C25 N2 Pd1 106.0(2) . . ? C51 N3 C49 107.8(3) . . ? C51 N3 C50 109.9(3) . . ? C49 N3 C50 108.5(3) . . ? C51 N3 Pd2 106.3(2) . . ? C49 N3 Pd2 115.8(3) . . ? C50 N3 Pd2 108.4(2) . . ? C54 N4 C53 108.8(3) . . ? C54 N4 C52 109.8(3) . . ? C53 N4 C52 110.5(3) . . ? C54 N4 Pd2 113.6(3) . . ? C53 N4 Pd2 109.3(3) . . ? C52 N4 Pd2 104.9(2) . . ? O1 C1 C10 120.8(3) . . ? O1 C1 C2 119.3(3) . . ? C10 C1 C2 120.0(3) . . ? C3 C2 C1 121.6(4) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 121.5(4) . . ? C5 C4 C9 119.5(3) . . ? C3 C4 C9 119.0(3) . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 119.5(4) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 120.6(4) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 122.1(4) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C8 C9 C10 123.3(3) . . ? C8 C9 C4 116.6(3) . . ? C10 C9 C4 120.1(3) . . ? C1 C10 C9 118.8(3) . . ? C1 C10 C11 120.7(3) . . ? C9 C10 C11 120.4(3) . . ? C12 C11 C20 117.2(3) . . ? C12 C11 C10 120.8(3) . . ? C20 C11 C10 122.0(3) . . ? O2 C12 C11 122.1(3) . . ? O2 C12 C13 116.6(3) . . ? C11 C12 C13 121.3(4) . . ? C14 C13 C12 120.7(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C20 119.2(4) . . ? C14 C15 C16 121.3(4) . . ? C20 C15 C16 119.5(4) . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 119.6(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 121.1(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 121.3(4) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C15 C20 C19 117.7(4) . . ? C15 C20 C11 120.4(3) . . ? C19 C20 C11 121.9(3) . . ? Pd1 C21 H21A 109.5 . . ? Pd1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Pd1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? N1 C23 H23B 109.5 . . ? N1 C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? N1 C24 C25 109.5(3) . . ? N1 C24 H24A 109.8 . . ? C25 C24 H24A 109.8 . . ? N1 C24 H24B 109.8 . . ? C25 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? N2 C25 C24 111.0(3) . . ? N2 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? N2 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? H25B C25 H25A 108.0 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? O3 C28 C37 120.4(3) . . ? O3 C28 C29 119.9(3) . . ? C37 C28 C29 119.7(3) . . ? C30 C29 C28 121.7(4) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C31 120.1(4) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C36 119.4(3) . . ? C30 C31 C32 121.0(4) . . ? C36 C31 C32 119.5(4) . . ? C33 C32 C31 121.5(4) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 119.2(4) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 121.3(4) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 120.8(4) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C31 C36 C35 117.6(3) . . ? C31 C36 C37 119.9(3) . . ? C35 C36 C37 122.5(3) . . ? C28 C37 C36 118.8(3) . . ? C28 C37 C38 120.7(3) . . ? C36 C37 C38 120.5(3) . . ? C39 C38 C47 117.8(3) . . ? C39 C38 C37 120.9(3) . . ? C47 C38 C37 121.3(3) . . ? O4 C39 C38 121.3(3) . . ? O4 C39 C40 117.4(3) . . ? C38 C39 C40 121.3(4) . . ? C41 C40 C39 121.0(4) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C42 120.3(4) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 121.3(4) . . ? C43 C42 C47 119.9(4) . . ? C41 C42 C47 118.8(4) . . ? C44 C43 C42 120.8(4) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 119.4(4) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C46 C45 C44 121.5(4) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C45 C46 C47 121.2(4) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C42 C47 C46 117.2(4) . . ? C42 C47 C38 120.2(3) . . ? C46 C47 C38 122.7(3) . . ? Pd2 C48 H48B 109.5 . . ? Pd2 C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Pd2 C48 H48A 109.5 . . ? H48B C48 H48A 109.5 . . ? H48C C48 H48A 109.5 . . ? N3 C49 H49A 109.5 . . ? N3 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? N3 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? H49C C49 H49B 109.5 . . ? N3 C50 H50B 109.5 . . ? N3 C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N3 C50 H50A 109.5 . . ? H50B C50 H50A 109.5 . . ? H50C C50 H50A 109.5 . . ? N3 C51 C52 111.1(3) . . ? N3 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? N3 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? H51B C51 H51A 108.0 . . ? N4 C52 C51 109.6(3) . . ? N4 C52 H52A 109.8 . . ? C51 C52 H52A 109.8 . . ? N4 C52 H52B 109.8 . . ? C51 C52 H52B 109.8 . . ? H52A C52 H52B 108.2 . . ? N4 C53 H53B 109.5 . . ? N4 C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N4 C53 H53A 109.5 . . ? H53B C53 H53A 109.5 . . ? H53C C53 H53A 109.5 . . ? N4 C54 H54A 109.5 . . ? N4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? N4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? H54C C54 H54B 109.5 . . ? Cl2 C55 Cl1 112.5(3) . . ? Cl2 C55 H55A 109.1 . . ? Cl1 C55 H55A 109.1 . . ? Cl2 C55 H55B 109.1 . . ? Cl1 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? Cl4 C56 Cl3 113.2(3) . . ? Cl4 C56 H56B 108.9 . . ? Cl3 C56 H56B 108.9 . . ? Cl4 C56 H56A 108.9 . . ? Cl3 C56 H56A 108.9 . . ? H56B C56 H56A 107.8 . . ? 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 C21 Pd1 O1 C1 -56.0(3) . . . . ? N2 Pd1 O1 C1 -176.2(15) . . . . ? N1 Pd1 O1 C1 122.9(3) . . . . ? C48 Pd2 O3 C28 -57.6(3) . . . . ? N3 Pd2 O3 C28 175.7(15) . . . . ? N4 Pd2 O3 C28 120.5(3) . . . . ? C21 Pd1 N1 C22 77(4) . . . . ? O1 Pd1 N1 C22 -77.7(3) . . . . ? N2 Pd1 N1 C22 106.3(3) . . . . ? C21 Pd1 N1 C23 -160(3) . . . . ? O1 Pd1 N1 C23 44.4(3) . . . . ? N2 Pd1 N1 C23 -131.6(3) . . . . ? C21 Pd1 N1 C24 -42(4) . . . . ? O1 Pd1 N1 C24 163.2(3) . . . . ? N2 Pd1 N1 C24 -12.8(3) . . . . ? C21 Pd1 N2 C27 42.8(3) . . . . ? O1 Pd1 N2 C27 162.8(15) . . . . ? N1 Pd1 N2 C27 -135.9(3) . . . . ? C21 Pd1 N2 C26 -78.7(3) . . . . ? O1 Pd1 N2 C26 41.3(17) . . . . ? N1 Pd1 N2 C26 102.6(3) . . . . ? C21 Pd1 N2 C25 163.0(3) . . . . ? O1 Pd1 N2 C25 -77.0(16) . . . . ? N1 Pd1 N2 C25 -15.7(3) . . . . ? C48 Pd2 N3 C51 161.1(3) . . . . ? O3 Pd2 N3 C51 -72.4(16) . . . . ? N4 Pd2 N3 C51 -16.9(2) . . . . ? C48 Pd2 N3 C49 41.4(3) . . . . ? O3 Pd2 N3 C49 167.9(15) . . . . ? N4 Pd2 N3 C49 -136.6(3) . . . . ? C48 Pd2 N3 C50 -80.8(3) . . . . ? O3 Pd2 N3 C50 45.8(17) . . . . ? N4 Pd2 N3 C50 101.3(3) . . . . ? C48 Pd2 N4 C54 180(100) . . . . ? O3 Pd2 N4 C54 45.1(3) . . . . ? N3 Pd2 N4 C54 -131.0(3) . . . . ? C48 Pd2 N4 C53 58(3) . . . . ? O3 Pd2 N4 C53 -76.5(3) . . . . ? N3 Pd2 N4 C53 107.4(3) . . . . ? C48 Pd2 N4 C52 -61(3) . . . . ? O3 Pd2 N4 C52 165.0(2) . . . . ? N3 Pd2 N4 C52 -11.1(2) . . . . ? Pd1 O1 C1 C10 135.9(3) . . . . ? Pd1 O1 C1 C2 -44.8(4) . . . . ? O1 C1 C2 C3 -175.2(3) . . . . ? C10 C1 C2 C3 4.0(6) . . . . ? C1 C2 C3 C4 1.0(6) . . . . ? C2 C3 C4 C5 178.8(4) . . . . ? C2 C3 C4 C9 -3.4(5) . . . . ? C3 C4 C5 C6 176.6(4) . . . . ? C9 C4 C5 C6 -1.2(6) . . . . ? C4 C5 C6 C7 3.3(6) . . . . ? C5 C6 C7 C8 -2.2(6) . . . . ? C6 C7 C8 C9 -1.1(6) . . . . ? C7 C8 C9 C10 -177.8(4) . . . . ? C7 C8 C9 C4 3.1(5) . . . . ? C5 C4 C9 C8 -2.0(5) . . . . ? C3 C4 C9 C8 -179.8(3) . . . . ? C5 C4 C9 C10 178.9(3) . . . . ? C3 C4 C9 C10 1.0(5) . . . . ? O1 C1 C10 C9 172.9(3) . . . . ? C2 C1 C10 C9 -6.3(5) . . . . ? O1 C1 C10 C11 -6.3(5) . . . . ? C2 C1 C10 C11 174.4(3) . . . . ? C8 C9 C10 C1 -175.3(3) . . . . ? C4 C9 C10 C1 3.8(5) . . . . ? C8 C9 C10 C11 4.0(5) . . . . ? C4 C9 C10 C11 -176.9(3) . . . . ? C1 C10 C11 C12 56.6(5) . . . . ? C9 C10 C11 C12 -122.6(4) . . . . ? C1 C10 C11 C20 -123.4(4) . . . . ? C9 C10 C11 C20 57.3(5) . . . . ? C20 C11 C12 O2 169.9(3) . . . . ? C10 C11 C12 O2 -10.2(6) . . . . ? C20 C11 C12 C13 -10.2(6) . . . . ? C10 C11 C12 C13 169.7(3) . . . . ? O2 C12 C13 C14 -174.7(4) . . . . ? C11 C12 C13 C14 5.4(6) . . . . ? C12 C13 C14 C15 2.7(6) . . . . ? C13 C14 C15 C20 -5.3(6) . . . . ? C13 C14 C15 C16 174.3(4) . . . . ? C14 C15 C16 C17 -178.8(4) . . . . ? C20 C15 C16 C17 0.8(6) . . . . ? C15 C16 C17 C18 -0.8(7) . . . . ? C16 C17 C18 C19 1.3(7) . . . . ? C17 C18 C19 C20 -1.7(6) . . . . ? C14 C15 C20 C19 178.5(4) . . . . ? C16 C15 C20 C19 -1.1(5) . . . . ? C14 C15 C20 C11 0.1(5) . . . . ? C16 C15 C20 C11 -179.5(4) . . . . ? C18 C19 C20 C15 1.6(6) . . . . ? C18 C19 C20 C11 179.9(4) . . . . ? C12 C11 C20 C15 7.5(5) . . . . ? C10 C11 C20 C15 -172.5(3) . . . . ? C12 C11 C20 C19 -170.8(3) . . . . ? C10 C11 C20 C19 9.2(6) . . . . ? C22 N1 C24 C25 -79.8(4) . . . . ? C23 N1 C24 C25 159.5(4) . . . . ? Pd1 N1 C24 C25 39.1(4) . . . . ? C27 N2 C25 C24 167.9(4) . . . . ? C26 N2 C25 C24 -74.2(4) . . . . ? Pd1 N2 C25 C24 42.9(4) . . . . ? N1 C24 C25 N2 -57.7(5) . . . . ? Pd2 O3 C28 C37 141.1(3) . . . . ? Pd2 O3 C28 C29 -40.7(5) . . . . ? O3 C28 C29 C30 -174.7(4) . . . . ? C37 C28 C29 C30 3.5(6) . . . . ? C28 C29 C30 C31 2.3(6) . . . . ? C29 C30 C31 C36 -4.1(6) . . . . ? C29 C30 C31 C32 176.9(4) . . . . ? C30 C31 C32 C33 177.9(4) . . . . ? C36 C31 C32 C33 -1.0(6) . . . . ? C31 C32 C33 C34 2.7(7) . . . . ? C32 C33 C34 C35 -1.4(7) . . . . ? C33 C34 C35 C36 -1.4(6) . . . . ? C30 C31 C36 C35 179.3(3) . . . . ? C32 C31 C36 C35 -1.8(5) . . . . ? C30 C31 C36 C37 0.3(5) . . . . ? C32 C31 C36 C37 179.2(3) . . . . ? C34 C35 C36 C31 3.0(5) . . . . ? C34 C35 C36 C37 -178.1(4) . . . . ? O3 C28 C37 C36 171.0(3) . . . . ? C29 C28 C37 C36 -7.2(5) . . . . ? O3 C28 C37 C38 -9.0(5) . . . . ? C29 C28 C37 C38 172.7(3) . . . . ? C31 C36 C37 C28 5.4(5) . . . . ? C35 C36 C37 C28 -173.6(3) . . . . ? C31 C36 C37 C38 -174.6(3) . . . . ? C35 C36 C37 C38 6.5(5) . . . . ? C28 C37 C38 C39 55.7(5) . . . . ? C36 C37 C38 C39 -124.3(4) . . . . ? C28 C37 C38 C47 -122.4(4) . . . . ? C36 C37 C38 C47 57.6(5) . . . . ? C47 C38 C39 O4 171.4(3) . . . . ? C37 C38 C39 O4 -6.8(6) . . . . ? C47 C38 C39 C40 -8.7(6) . . . . ? C37 C38 C39 C40 173.1(3) . . . . ? O4 C39 C40 C41 -174.8(3) . . . . ? C38 C39 C40 C41 5.2(6) . . . . ? C39 C40 C41 C42 1.3(6) . . . . ? C40 C41 C42 C43 176.2(4) . . . . ? C40 C41 C42 C47 -3.9(6) . . . . ? C41 C42 C43 C44 178.6(4) . . . . ? C47 C42 C43 C44 -1.3(6) . . . . ? C42 C43 C44 C45 1.4(7) . . . . ? C43 C44 C45 C46 -0.2(7) . . . . ? C44 C45 C46 C47 -1.0(6) . . . . ? C43 C42 C47 C46 0.1(5) . . . . ? C41 C42 C47 C46 -179.8(4) . . . . ? C43 C42 C47 C38 -179.8(3) . . . . ? C41 C42 C47 C38 0.3(5) . . . . ? C45 C46 C47 C42 1.1(6) . . . . ? C45 C46 C47 C38 -179.0(4) . . . . ? C39 C38 C47 C42 5.9(5) . . . . ? C37 C38 C47 C42 -175.9(3) . . . . ? C39 C38 C47 C46 -174.0(4) . . . . ? C37 C38 C47 C46 4.2(6) . . . . ? C49 N3 C51 C52 167.9(3) . . . . ? C50 N3 C51 C52 -74.1(4) . . . . ? Pd2 N3 C51 C52 43.1(4) . . . . ? C54 N4 C52 C51 159.2(3) . . . . ? C53 N4 C52 C51 -80.9(4) . . . . ? Pd2 N4 C52 C51 36.8(4) . . . . ? N3 C51 C52 N4 -55.9(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.84 1.81 2.591(4) 153.9 . O4 H4 O3 0.84 1.76 2.551(4) 155.8 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.024 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.074 data_a _database_code_depnum_ccdc_archive 'CCDC 917456' #TrackingRef 'web_deposit_cif_file_0_YudongCai_1356446564.a3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H40 N2 O2 Pd, C H2 Cl2' _chemical_formula_sum 'C28 H42 Cl2 N2 O2 Pd' _chemical_formula_weight 615.94 _chemical_absolute_configuration ad 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.839(2) _cell_length_b 12.056(2) _cell_length_c 12.660(3) _cell_angle_alpha 62.30(3) _cell_angle_beta 78.85(3) _cell_angle_gamma 89.82(3) _cell_volume 1430.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5540 _cell_measurement_theta_min 1.8610 _cell_measurement_theta_max 27.4839 _exptl_crystal_description rod _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5278 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18592 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.45 _reflns_number_total 11701 _reflns_number_gt 11340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 11701 _refine_ls_number_parameters 643 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0847 _refine_ls_wR_factor_ref 0.2143 _refine_ls_wR_factor_gt 0.2123 _refine_ls_goodness_of_fit_ref 1.435 _refine_ls_restrained_S_all 1.435 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 0.59345(4) 0.73436(4) 0.70243(4) 0.02040(15) Uani 1 1 d . . . Pd2 Pd 0.14510(4) 0.72296(4) 0.47596(4) 0.02093(15) Uani 1 1 d . . . Cl1 Cl 0.1391(4) 0.7249(3) 0.9921(3) 0.0667(9) Uani 1 1 d . . . Cl2 Cl -0.1026(4) 0.7292(4) 0.9207(3) 0.0689(10) Uani 1 1 d . . . Cl3 Cl 0.5443(4) 0.7273(5) 0.2353(6) 0.0926(15) Uani 1 1 d . . . Cl4 Cl 0.8152(3) 0.7248(3) 0.2197(2) 0.0486(6) Uani 1 1 d . . . O1 O 0.6387(6) 0.5797(5) 0.6814(5) 0.0258(11) Uani 1 1 d . . . O2 O 0.6657(6) 0.4804(6) 0.5344(5) 0.0296(12) Uani 1 1 d . . . H2 H 0.6761 0.5275 0.5649 0.044 Uiso 1 1 calc R . . O3 O 0.1827(6) 0.8765(5) 0.4957(5) 0.0278(12) Uani 1 1 d . . . O4 O 0.1410(6) 0.9722(6) 0.6445(5) 0.0286(12) Uani 1 1 d . . . H4 H 0.1728 0.9306 0.6099 0.043 Uiso 1 1 calc R . . N1 N 0.7251(6) 0.8643(6) 0.5324(6) 0.0241(13) Uani 1 1 d . . . N2 N 0.5417(6) 0.8986(7) 0.7100(7) 0.0270(14) Uani 1 1 d . . . N3 N 0.2032(6) 0.5949(6) 0.6462(6) 0.0223(12) Uani 1 1 d . . . N4 N 0.0962(6) 0.5591(6) 0.4719(6) 0.0258(14) Uani 1 1 d . . . C1 C 0.6875(7) 0.4863(7) 0.7665(6) 0.0215(14) Uani 1 1 d . . . C2 C 0.7736(8) 0.5115(8) 0.8250(7) 0.0266(16) Uani 1 1 d . . . H2A H 0.7907 0.5947 0.8120 0.032 Uiso 1 1 calc R . . C3 C 0.8327(8) 0.4139(8) 0.9015(8) 0.0286(17) Uani 1 1 d . . . H3 H 0.8885 0.4318 0.9422 0.034 Uiso 1 1 calc R . . C4 C 0.8148(7) 0.2918(7) 0.9219(7) 0.0226(14) Uani 1 1 d . . . C5 C 0.8879(8) 0.1926(8) 1.0026(8) 0.0304(17) Uani 1 1 d . . . H5A H 0.8520 0.1706 1.0888 0.037 Uiso 1 1 calc R . . H5B H 0.9767 0.2280 0.9823 0.037 Uiso 1 1 calc R . . C6 C 0.8859(12) 0.0735(10) 0.9899(14) 0.063(4) Uani 1 1 d . . . H6A H 0.9522 0.0866 0.9182 0.075 Uiso 1 1 calc R . . H6B H 0.9082 0.0043 1.0631 0.075 Uiso 1 1 calc R . . C7 C 0.7662(12) 0.0340(10) 0.9758(11) 0.050(3) Uani 1 1 d . . . H7B H 0.7027 0.0074 1.0528 0.060 Uiso 1 1 calc R . . H7A H 0.7770 -0.0400 0.9617 0.060 Uiso 1 1 calc R . . C8 C 0.7172(7) 0.1341(7) 0.8731(7) 0.0229(14) Uani 1 1 d . . . H8A H 0.6270 0.1093 0.8831 0.027 Uiso 1 1 calc R . . H8B H 0.7637 0.1394 0.7952 0.027 Uiso 1 1 calc R . . C9 C 0.7292(7) 0.2644(7) 0.8648(7) 0.0193(13) Uani 1 1 d . . . C10 C 0.6616(7) 0.3614(7) 0.7904(6) 0.0191(13) Uani 1 1 d . . . C11 C 0.5608(6) 0.3301(6) 0.7399(7) 0.0157(14) Uani 1 1 d . . . C12 C 0.5733(7) 0.3850(7) 0.6127(7) 0.0209(14) Uani 1 1 d . . . C13 C 0.4922(8) 0.3424(7) 0.5633(7) 0.0259(15) Uani 1 1 d . . . H13 H 0.5056 0.3746 0.4773 0.031 Uiso 1 1 calc R . . C14 C 0.3929(8) 0.2535(8) 0.6398(7) 0.0237(16) Uani 1 1 d . . . H14 H 0.3399 0.2221 0.6060 0.028 Uiso 1 1 calc R . . C15 C 0.3680(7) 0.2079(7) 0.7666(7) 0.0209(14) Uani 1 1 d . . . C16 C 0.2508(8) 0.1167(8) 0.8457(8) 0.0304(17) Uani 1 1 d . . . H16B H 0.1751 0.1627 0.8292 0.037 Uiso 1 1 calc R . . H16A H 0.2469 0.0502 0.8211 0.037 Uiso 1 1 calc R . . C17 C 0.2456(11) 0.0566(11) 0.9776(9) 0.046(3) Uani 1 1 d . . . H17B H 0.2998 -0.0137 0.9995 0.055 Uiso 1 1 calc R . . H17A H 0.1578 0.0210 1.0225 0.055 Uiso 1 1 calc R . . C18 C 0.2894(11) 0.1487(11) 1.0166(9) 0.049(3) Uani 1 1 d . . . H18A H 0.2315 0.2158 0.9996 0.059 Uiso 1 1 calc R . . H18B H 0.2843 0.1040 1.1058 0.059 Uiso 1 1 calc R . . C19 C 0.4222(8) 0.2082(8) 0.9522(7) 0.0287(17) Uani 1 1 d . . . H19A H 0.4818 0.1478 0.9916 0.034 Uiso 1 1 calc R . . H19B H 0.4363 0.2832 0.9628 0.034 Uiso 1 1 calc R . . C20 C 0.4523(7) 0.2477(7) 0.8162(7) 0.0213(14) Uani 1 1 d . . . C21 C 0.4777(9) 0.6189(9) 0.8642(8) 0.0357(19) Uani 1 1 d . . . H21A H 0.4719 0.5333 0.8742 0.054 Uiso 1 1 calc R . . H21B H 0.3934 0.6486 0.8662 0.054 Uiso 1 1 calc R . . H21C H 0.5115 0.6187 0.9307 0.054 Uiso 1 1 calc R . . C22 C 0.7221(9) 0.8379(8) 0.4311(8) 0.0334(18) Uani 1 1 d . . . H22A H 0.7098 0.7466 0.4622 0.050 Uiso 1 1 calc R . . H22C H 0.8022 0.8719 0.3708 0.050 Uiso 1 1 calc R . . H22B H 0.6524 0.8773 0.3926 0.050 Uiso 1 1 calc R . . C23 C 0.8536(7) 0.8576(9) 0.5559(9) 0.0353(19) Uani 1 1 d . . . H23A H 0.8783 0.7724 0.5792 0.053 Uiso 1 1 calc R . . H23C H 0.8550 0.8777 0.6222 0.053 Uiso 1 1 calc R . . H23B H 0.9129 0.9181 0.4817 0.053 Uiso 1 1 calc R . . C24 C 0.6826(8) 0.9914(8) 0.5055(8) 0.0322(18) Uani 1 1 d . . . H24A H 0.6111 1.0062 0.4639 0.039 Uiso 1 1 calc R . . H24B H 0.7527 1.0574 0.4504 0.039 Uiso 1 1 calc R . . C25 C 0.6420(9) 0.9984(9) 0.6233(10) 0.037(2) Uani 1 1 d . . . H25B H 0.7157 0.9905 0.6610 0.044 Uiso 1 1 calc R . . H25A H 0.6113 1.0814 0.6051 0.044 Uiso 1 1 calc R . . C26 C 0.5277(10) 0.8906(10) 0.8340(10) 0.041(2) Uani 1 1 d . . . H26A H 0.4619 0.8232 0.8929 0.061 Uiso 1 1 calc R . . H26C H 0.5041 0.9709 0.8297 0.061 Uiso 1 1 calc R . . H26B H 0.6081 0.8726 0.8602 0.061 Uiso 1 1 calc R . . C27 C 0.4194(8) 0.9262(8) 0.6722(10) 0.036(2) Uani 1 1 d . . . H27A H 0.4221 0.9169 0.5990 0.053 Uiso 1 1 calc R . . H27C H 0.4037 1.0127 0.6543 0.053 Uiso 1 1 calc R . . H27B H 0.3513 0.8675 0.7384 0.053 Uiso 1 1 calc R . . C28 C 0.2700(7) 0.9700(7) 0.4108(6) 0.0219(14) Uani 1 1 d . . . C29 C 0.3800(8) 0.9466(8) 0.3501(7) 0.0273(16) Uani 1 1 d . . . H29 H 0.3908 0.8639 0.3613 0.033 Uiso 1 1 calc R . . C30 C 0.4747(8) 1.0450(8) 0.2725(8) 0.0293(17) Uani 1 1 d . . . H30 H 0.5482 1.0289 0.2291 0.035 Uiso 1 1 calc R . . C31 C 0.4630(7) 1.1659(8) 0.2579(7) 0.0260(16) Uani 1 1 d . . . C32 C 0.5709(8) 1.2685(9) 0.1747(8) 0.0327(18) Uani 1 1 d . . . H32B H 0.6518 1.2336 0.1919 0.039 Uiso 1 1 calc R . . H32A H 0.5708 1.2912 0.0889 0.039 Uiso 1 1 calc R . . C33 C 0.5658(9) 1.3864(10) 0.1873(10) 0.041(2) Uani 1 1 d . . . H33A H 0.6213 1.4559 0.1149 0.049 Uiso 1 1 calc R . . H33B H 0.5965 1.3728 0.2607 0.049 Uiso 1 1 calc R . . C34 C 0.4324(10) 1.4209(10) 0.1981(9) 0.043(2) Uani 1 1 d . . . H34B H 0.4310 1.5003 0.2033 0.052 Uiso 1 1 calc R . . H34A H 0.4038 1.4365 0.1231 0.052 Uiso 1 1 calc R . . C35 C 0.3414(8) 1.3224(7) 0.3065(7) 0.0265(16) Uani 1 1 d . . . H35A H 0.2543 1.3453 0.3009 0.032 Uiso 1 1 calc R . . H35B H 0.3582 1.3197 0.3818 0.032 Uiso 1 1 calc R . . C36 C 0.3519(7) 1.1916(7) 0.3151(6) 0.0205(14) Uani 1 1 d . . . C37 C 0.2521(7) 1.0945(7) 0.3870(7) 0.0209(14) Uani 1 1 d . . . C38 C 0.1279(7) 1.1257(7) 0.4393(6) 0.0169(14) Uani 1 1 d . . . C39 C 0.0851(7) 1.0690(7) 0.5666(6) 0.0200(14) Uani 1 1 d . . . C40 C -0.0215(8) 1.1079(8) 0.6178(7) 0.0269(16) Uani 1 1 d . . . H40 H -0.0497 1.0707 0.7040 0.032 Uiso 1 1 calc R . . C41 C -0.0856(8) 1.2014(8) 0.5413(8) 0.0263(16) Uani 1 1 d . . . H41 H -0.1532 1.2334 0.5753 0.032 Uiso 1 1 calc R . . C42 C -0.0511(7) 1.2490(7) 0.4140(7) 0.0222(15) Uani 1 1 d . . . C43 C -0.1309(8) 1.3449(8) 0.3374(8) 0.0281(16) Uani 1 1 d . . . H43B H -0.1144 1.4251 0.3384 0.034 Uiso 1 1 calc R . . H43A H -0.2213 1.3147 0.3752 0.034 Uiso 1 1 calc R . . C44 C -0.1055(9) 1.3696(10) 0.2056(8) 0.038(2) Uani 1 1 d . . . H44A H -0.1497 1.3007 0.2012 0.045 Uiso 1 1 calc R . . H44B H -0.1392 1.4492 0.1552 0.045 Uiso 1 1 calc R . . C45 C 0.0342(10) 1.3785(9) 0.1553(9) 0.041(2) Uani 1 1 d . . . H45B H 0.0784 1.4475 0.1598 0.049 Uiso 1 1 calc R . . H45A H 0.0486 1.3987 0.0683 0.049 Uiso 1 1 calc R . . C46 C 0.0884(7) 1.2555(7) 0.2267(7) 0.0248(15) Uani 1 1 d . . . H46B H 0.1815 1.2673 0.1987 0.030 Uiso 1 1 calc R . . H46A H 0.0554 1.1900 0.2101 0.030 Uiso 1 1 calc R . . C47 C 0.0544(7) 1.2110(7) 0.3641(6) 0.0200(14) Uani 1 1 d . . . C48 C 0.0976(8) 0.8357(8) 0.3145(7) 0.0320(18) Uani 1 1 d . . . H48B H 0.1607 0.8357 0.2476 0.048 Uiso 1 1 calc R . . H48C H 0.0949 0.9216 0.3034 0.048 Uiso 1 1 calc R . . H48A H 0.0144 0.8042 0.3145 0.048 Uiso 1 1 calc R . . C49 C 0.3423(9) 0.6037(10) 0.6221(11) 0.042(2) Uani 1 1 d . . . H49B H 0.3694 0.5484 0.6976 0.064 Uiso 1 1 calc R . . H49C H 0.3758 0.6908 0.5928 0.064 Uiso 1 1 calc R . . H49A H 0.3741 0.5778 0.5599 0.064 Uiso 1 1 calc R . . C50 C 0.1544(10) 0.6208(8) 0.7473(8) 0.037(2) Uani 1 1 d . . . H50A H 0.0680 0.5803 0.7865 0.055 Uiso 1 1 calc R . . H50C H 0.1544 0.7119 0.7164 0.055 Uiso 1 1 calc R . . H50B H 0.2082 0.5875 0.8072 0.055 Uiso 1 1 calc R . . C51 C 0.1504(9) 0.4700(8) 0.6753(9) 0.0348(19) Uani 1 1 d . . . H51A H 0.0604 0.4558 0.7173 0.042 Uiso 1 1 calc R . . H51B H 0.1963 0.4048 0.7310 0.042 Uiso 1 1 calc R . . C52 C 0.1621(9) 0.4596(8) 0.5576(10) 0.036(2) Uani 1 1 d . . . H52B H 0.2525 0.4687 0.5183 0.043 Uiso 1 1 calc R . . H52A H 0.1245 0.3756 0.5775 0.043 Uiso 1 1 calc R . . C53 C 0.1351(9) 0.5618(10) 0.3513(9) 0.038(2) Uani 1 1 d . . . H53A H 0.1176 0.4775 0.3610 0.057 Uiso 1 1 calc R . . H53C H 0.2258 0.5887 0.3193 0.057 Uiso 1 1 calc R . . H53B H 0.0876 0.6211 0.2942 0.057 Uiso 1 1 calc R . . C54 C -0.0427(7) 0.5291(8) 0.5129(9) 0.0302(17) Uani 1 1 d . . . H54B H -0.0840 0.5981 0.4575 0.045 Uiso 1 1 calc R . . H54C H -0.0691 0.5185 0.5959 0.045 Uiso 1 1 calc R . . H54A H -0.0668 0.4511 0.5125 0.045 Uiso 1 1 calc R . . C55 C 0.0208(11) 0.8194(10) 0.9264(10) 0.045(3) Uani 1 1 d . . . H55B H -0.0139 0.8614 0.9753 0.054 Uiso 1 1 calc R . . H55A H 0.0592 0.8856 0.8426 0.054 Uiso 1 1 calc R . . C56 C 0.6752(12) 0.6437(11) 0.2412(11) 0.049(3) Uani 1 1 d . . . H56B H 0.6605 0.5671 0.3217 0.059 Uiso 1 1 calc R . . H56A H 0.6832 0.6160 0.1780 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0197(3) 0.0185(3) 0.0242(3) -0.0109(2) -0.0053(2) 0.0003(2) Pd2 0.0184(3) 0.0196(3) 0.0244(3) -0.0106(2) -0.0034(2) 0.0018(2) Cl1 0.077(2) 0.0472(17) 0.0619(19) -0.0148(14) -0.0134(17) 0.0136(15) Cl2 0.074(2) 0.082(2) 0.0614(19) -0.0483(19) -0.0011(17) -0.0119(18) Cl3 0.058(2) 0.102(3) 0.152(5) -0.083(3) -0.036(3) 0.022(2) Cl4 0.0563(15) 0.0495(15) 0.0344(11) -0.0170(11) -0.0049(11) -0.0071(11) O1 0.033(3) 0.017(3) 0.030(3) -0.011(2) -0.017(2) 0.005(2) O2 0.034(3) 0.028(3) 0.024(3) -0.011(2) -0.002(2) -0.007(2) O3 0.031(3) 0.020(3) 0.033(3) -0.015(2) 0.000(2) 0.000(2) O4 0.035(3) 0.029(3) 0.020(3) -0.010(2) -0.006(2) 0.012(3) N1 0.020(3) 0.018(3) 0.028(3) -0.007(2) -0.004(3) -0.002(2) N2 0.025(3) 0.028(4) 0.039(4) -0.025(3) -0.009(3) 0.002(3) N3 0.021(3) 0.021(3) 0.025(3) -0.011(2) -0.003(2) 0.001(2) N4 0.022(3) 0.029(3) 0.033(3) -0.019(3) -0.008(3) 0.005(3) C1 0.017(3) 0.027(4) 0.019(3) -0.011(3) -0.001(3) 0.002(3) C2 0.028(4) 0.024(4) 0.031(4) -0.014(3) -0.011(3) -0.001(3) C3 0.025(4) 0.031(4) 0.036(4) -0.019(3) -0.012(3) -0.001(3) C4 0.024(3) 0.026(4) 0.023(3) -0.014(3) -0.009(3) 0.004(3) C5 0.025(4) 0.036(4) 0.034(4) -0.017(4) -0.014(3) 0.012(3) C6 0.062(8) 0.034(6) 0.106(11) -0.028(6) -0.063(8) 0.019(5) C7 0.074(8) 0.034(5) 0.056(6) -0.023(5) -0.037(6) 0.033(5) C8 0.023(3) 0.022(4) 0.028(4) -0.014(3) -0.009(3) 0.007(3) C9 0.017(3) 0.021(3) 0.024(3) -0.014(3) -0.005(3) 0.002(3) C10 0.017(3) 0.023(3) 0.019(3) -0.011(3) -0.003(3) 0.002(3) C11 0.011(3) 0.014(3) 0.022(3) -0.008(3) -0.005(3) 0.002(2) C12 0.017(3) 0.020(3) 0.024(3) -0.010(3) -0.002(3) -0.001(3) C13 0.029(4) 0.025(4) 0.022(3) -0.011(3) -0.003(3) 0.000(3) C14 0.023(4) 0.028(4) 0.023(4) -0.013(3) -0.009(3) 0.005(3) C15 0.020(3) 0.019(4) 0.024(4) -0.010(3) -0.004(3) 0.002(3) C16 0.027(4) 0.029(4) 0.031(4) -0.012(3) -0.002(3) -0.005(3) C17 0.035(5) 0.059(7) 0.031(5) -0.015(5) 0.008(4) -0.027(5) C18 0.055(6) 0.057(7) 0.031(5) -0.021(5) 0.003(4) -0.013(5) C19 0.026(4) 0.034(4) 0.024(4) -0.014(3) 0.001(3) -0.004(3) C20 0.022(3) 0.020(3) 0.021(3) -0.010(3) -0.004(3) 0.001(3) C21 0.032(4) 0.035(5) 0.036(4) -0.014(4) -0.004(4) 0.002(4) C22 0.043(5) 0.025(4) 0.031(4) -0.012(3) -0.006(4) -0.003(3) C23 0.016(4) 0.039(5) 0.055(5) -0.029(4) 0.001(4) -0.002(3) C24 0.031(4) 0.023(4) 0.035(4) -0.009(3) -0.003(3) -0.002(3) C25 0.036(5) 0.027(4) 0.054(6) -0.024(4) -0.009(4) -0.003(4) C26 0.037(5) 0.052(6) 0.051(6) -0.041(5) -0.006(4) 0.002(4) C27 0.028(4) 0.027(4) 0.060(6) -0.026(4) -0.012(4) 0.007(3) C28 0.019(3) 0.027(4) 0.018(3) -0.011(3) -0.002(3) -0.001(3) C29 0.027(4) 0.025(4) 0.031(4) -0.013(3) -0.007(3) 0.005(3) C30 0.023(4) 0.043(5) 0.031(4) -0.027(4) 0.000(3) 0.008(3) C31 0.017(3) 0.036(4) 0.027(4) -0.018(3) -0.001(3) -0.003(3) C32 0.017(3) 0.045(5) 0.041(5) -0.028(4) 0.005(3) -0.010(3) C33 0.024(4) 0.044(6) 0.047(5) -0.021(4) 0.007(4) -0.012(4) C34 0.042(6) 0.036(5) 0.037(5) -0.008(4) 0.003(4) -0.012(4) C35 0.026(4) 0.017(3) 0.033(4) -0.011(3) -0.003(3) -0.008(3) C36 0.025(4) 0.020(3) 0.018(3) -0.011(3) -0.004(3) -0.001(3) C37 0.016(3) 0.020(3) 0.022(3) -0.007(3) -0.004(3) 0.000(3) C38 0.014(3) 0.015(3) 0.018(3) -0.006(3) 0.000(3) 0.000(3) C39 0.021(3) 0.018(3) 0.016(3) -0.005(3) -0.001(3) -0.002(3) C40 0.025(4) 0.027(4) 0.028(4) -0.014(3) -0.002(3) 0.001(3) C41 0.024(4) 0.029(4) 0.030(4) -0.019(3) -0.002(3) 0.003(3) C42 0.020(4) 0.020(4) 0.029(4) -0.013(3) -0.008(3) 0.004(3) C43 0.021(3) 0.029(4) 0.037(4) -0.015(3) -0.014(3) 0.009(3) C44 0.030(4) 0.046(5) 0.025(4) -0.007(4) -0.007(4) 0.008(4) C45 0.045(5) 0.039(5) 0.032(4) -0.011(4) -0.009(4) 0.007(4) C46 0.021(3) 0.030(4) 0.020(3) -0.009(3) -0.005(3) -0.003(3) C47 0.022(3) 0.018(3) 0.020(3) -0.009(3) -0.003(3) -0.005(3) C48 0.025(4) 0.032(4) 0.026(4) -0.003(3) -0.005(3) 0.000(3) C49 0.029(4) 0.043(5) 0.069(7) -0.032(5) -0.027(5) 0.008(4) C50 0.053(6) 0.027(4) 0.029(4) -0.012(3) -0.008(4) -0.002(4) C51 0.041(5) 0.022(4) 0.044(5) -0.014(4) -0.019(4) 0.005(3) C52 0.038(5) 0.023(4) 0.055(6) -0.023(4) -0.019(5) 0.010(4) C53 0.032(5) 0.053(6) 0.049(5) -0.041(5) -0.007(4) 0.011(4) C54 0.019(4) 0.031(4) 0.045(5) -0.022(4) -0.005(3) -0.001(3) C55 0.066(7) 0.027(5) 0.040(5) -0.017(4) -0.005(5) 0.016(5) C56 0.059(7) 0.042(6) 0.044(6) -0.018(5) -0.011(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C21 2.018(9) . ? Pd1 O1 2.048(5) . ? Pd1 N2 2.096(7) . ? Pd1 N1 2.194(7) . ? Pd2 C48 2.027(8) . ? Pd2 O3 2.032(6) . ? Pd2 N4 2.074(7) . ? Pd2 N3 2.202(6) . ? Cl1 C55 1.776(11) . ? Cl2 C55 1.760(13) . ? Cl3 C56 1.731(14) . ? Cl4 C56 1.714(12) . ? O1 C1 1.341(9) . ? O2 C12 1.368(9) . ? O2 H2 0.8400 . ? O3 C28 1.345(9) . ? O4 C39 1.364(9) . ? O4 H4 0.8400 . ? N1 C22 1.464(11) . ? N1 C23 1.474(10) . ? N1 C24 1.499(10) . ? N2 C25 1.468(12) . ? N2 C27 1.480(10) . ? N2 C26 1.506(11) . ? N3 C50 1.458(11) . ? N3 C51 1.462(10) . ? N3 C49 1.473(11) . ? N4 C54 1.481(10) . ? N4 C53 1.487(11) . ? N4 C52 1.487(11) . ? C1 C10 1.409(11) . ? C1 C2 1.411(10) . ? C2 C3 1.382(11) . ? C2 H2A 0.9500 . ? C3 C4 1.379(11) . ? C3 H3 0.9500 . ? C4 C9 1.406(9) . ? C4 C5 1.508(10) . ? C5 C6 1.517(14) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.454(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.495(11) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C8 C9 1.529(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.425(9) . ? C10 C11 1.496(9) . ? C11 C12 1.406(10) . ? C11 C20 1.407(10) . ? C12 C13 1.393(10) . ? C13 C14 1.373(11) . ? C13 H13 0.9500 . ? C14 C15 1.402(11) . ? C14 H14 0.9500 . ? C15 C20 1.402(10) . ? C15 C16 1.523(11) . ? C16 C17 1.468(13) . ? C16 H16B 0.9900 . ? C16 H16A 0.9900 . ? C17 C18 1.519(15) . ? C17 H17B 0.9900 . ? C17 H17A 0.9900 . ? C18 C19 1.504(13) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.523(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9800 . ? C23 H23C 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.512(13) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25B 0.9900 . ? C25 H25A 0.9900 . ? C26 H26A 0.9800 . ? C26 H26C 0.9800 . ? C26 H26B 0.9800 . ? C27 H27A 0.9800 . ? C27 H27C 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.391(11) . ? C28 C37 1.408(11) . ? C29 C30 1.401(12) . ? C29 H29 0.9500 . ? C30 C31 1.391(12) . ? C30 H30 0.9500 . ? C31 C36 1.392(11) . ? C31 C32 1.526(11) . ? C32 C33 1.501(13) . ? C32 H32B 0.9900 . ? C32 H32A 0.9900 . ? C33 C34 1.502(15) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.495(12) . ? C34 H34B 0.9900 . ? C34 H34A 0.9900 . ? C35 C36 1.535(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.416(10) . ? C37 C38 1.507(10) . ? C38 C39 1.404(9) . ? C38 C47 1.407(10) . ? C39 C40 1.402(11) . ? C40 C41 1.389(12) . ? C40 H40 0.9500 . ? C41 C42 1.406(12) . ? C41 H41 0.9500 . ? C42 C47 1.379(11) . ? C42 C43 1.516(10) . ? C43 C44 1.520(12) . ? C43 H43B 0.9900 . ? C43 H43A 0.9900 . ? C44 C45 1.508(14) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.522(12) . ? C45 H45B 0.9900 . ? C45 H45A 0.9900 . ? C46 C47 1.528(10) . ? C46 H46B 0.9900 . ? C46 H46A 0.9900 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C48 H48A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C49 H49A 0.9800 . ? C50 H50A 0.9800 . ? C50 H50C 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.534(13) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52B 0.9900 . ? C52 H52A 0.9900 . ? C53 H53A 0.9800 . ? C53 H53C 0.9800 . ? C53 H53B 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C54 H54A 0.9800 . ? C55 H55B 0.9900 . ? C55 H55A 0.9900 . ? C56 H56B 0.9900 . ? C56 H56A 0.9900 . ? 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 C21 Pd1 O1 88.7(3) . . ? C21 Pd1 N2 93.8(3) . . ? O1 Pd1 N2 175.1(2) . . ? C21 Pd1 N1 176.5(3) . . ? O1 Pd1 N1 93.3(2) . . ? N2 Pd1 N1 84.4(3) . . ? C48 Pd2 O3 89.9(3) . . ? C48 Pd2 N4 93.4(3) . . ? O3 Pd2 N4 174.7(3) . . ? C48 Pd2 N3 176.7(3) . . ? O3 Pd2 N3 92.4(2) . . ? N4 Pd2 N3 84.5(2) . . ? C1 O1 Pd1 119.4(5) . . ? C12 O2 H2 109.5 . . ? C28 O3 Pd2 120.3(5) . . ? C39 O4 H4 109.5 . . ? C22 N1 C23 110.1(7) . . ? C22 N1 C24 110.9(6) . . ? C23 N1 C24 110.0(7) . . ? C22 N1 Pd1 113.1(5) . . ? C23 N1 Pd1 108.5(5) . . ? C24 N1 Pd1 104.1(5) . . ? C25 N2 C27 110.9(7) . . ? C25 N2 C26 108.9(7) . . ? C27 N2 C26 108.5(7) . . ? C25 N2 Pd1 106.1(5) . . ? C27 N2 Pd1 107.9(5) . . ? C26 N2 Pd1 114.6(6) . . ? C50 N3 C51 109.6(7) . . ? C50 N3 C49 109.9(7) . . ? C51 N3 C49 110.9(7) . . ? C50 N3 Pd2 113.5(5) . . ? C51 N3 Pd2 104.3(5) . . ? C49 N3 Pd2 108.6(6) . . ? C54 N4 C53 108.3(6) . . ? C54 N4 C52 111.0(7) . . ? C53 N4 C52 107.1(7) . . ? C54 N4 Pd2 108.7(5) . . ? C53 N4 Pd2 115.7(6) . . ? C52 N4 Pd2 105.9(5) . . ? O1 C1 C10 119.5(6) . . ? O1 C1 C2 121.3(7) . . ? C10 C1 C2 119.0(7) . . ? C3 C2 C1 119.2(7) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C4 C3 C2 123.4(7) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C3 C4 C9 118.4(7) . . ? C3 C4 C5 119.6(7) . . ? C9 C4 C5 122.1(7) . . ? C4 C5 C6 113.4(7) . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C5 115.3(9) . . ? C7 C6 H6A 108.5 . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? C5 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C6 C7 C8 113.7(9) . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? H7B C7 H7A 107.7 . . ? C7 C8 C9 114.1(7) . . ? C7 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C4 C9 C10 119.8(7) . . ? C4 C9 C8 120.1(6) . . ? C10 C9 C8 119.9(6) . . ? C1 C10 C9 120.0(6) . . ? C1 C10 C11 120.0(6) . . ? C9 C10 C11 120.0(6) . . ? C12 C11 C20 118.5(6) . . ? C12 C11 C10 119.6(6) . . ? C20 C11 C10 121.9(6) . . ? O2 C12 C13 118.4(7) . . ? O2 C12 C11 121.1(7) . . ? C13 C12 C11 120.5(7) . . ? C14 C13 C12 119.5(7) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 121.5(7) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C20 118.7(7) . . ? C14 C15 C16 119.0(7) . . ? C20 C15 C16 122.3(7) . . ? C17 C16 C15 114.6(7) . . ? C17 C16 H16B 108.6 . . ? C15 C16 H16B 108.6 . . ? C17 C16 H16A 108.6 . . ? C15 C16 H16A 108.6 . . ? H16B C16 H16A 107.6 . . ? C16 C17 C18 112.0(9) . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? H17B C17 H17A 107.9 . . ? C19 C18 C17 112.9(9) . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 114.0(7) . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C15 C20 C11 120.3(7) . . ? C15 C20 C19 119.8(7) . . ? C11 C20 C19 119.7(6) . . ? Pd1 C21 H21A 109.5 . . ? Pd1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Pd1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? N1 C23 H23A 109.5 . . ? N1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? N1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? N1 C24 C25 109.7(7) . . ? N1 C24 H24A 109.7 . . ? C25 C24 H24A 109.7 . . ? N1 C24 H24B 109.7 . . ? C25 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? N2 C25 C24 111.6(7) . . ? N2 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? N2 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? H25B C25 H25A 108.0 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? O3 C28 C29 121.9(7) . . ? O3 C28 C37 118.8(7) . . ? C29 C28 C37 119.2(7) . . ? C28 C29 C30 120.0(7) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 121.0(7) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C36 119.5(7) . . ? C30 C31 C32 118.7(7) . . ? C36 C31 C32 121.8(8) . . ? C33 C32 C31 115.2(7) . . ? C33 C32 H32B 108.5 . . ? C31 C32 H32B 108.5 . . ? C33 C32 H32A 108.5 . . ? C31 C32 H32A 108.5 . . ? H32B C32 H32A 107.5 . . ? C32 C33 C34 109.7(8) . . ? C32 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? C32 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C35 C34 C33 113.7(9) . . ? C35 C34 H34B 108.8 . . ? C33 C34 H34B 108.8 . . ? C35 C34 H34A 108.8 . . ? C33 C34 H34A 108.8 . . ? H34B C34 H34A 107.7 . . ? C34 C35 C36 112.0(8) . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C31 C36 C37 119.7(7) . . ? C31 C36 C35 119.9(7) . . ? C37 C36 C35 120.3(7) . . ? C28 C37 C36 120.0(7) . . ? C28 C37 C38 120.6(6) . . ? C36 C37 C38 119.4(6) . . ? C39 C38 C47 119.0(7) . . ? C39 C38 C37 119.1(6) . . ? C47 C38 C37 121.9(6) . . ? O4 C39 C40 117.6(6) . . ? O4 C39 C38 122.1(7) . . ? C40 C39 C38 120.2(7) . . ? C41 C40 C39 119.4(7) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C40 C41 C42 120.6(8) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C47 C42 C41 119.5(7) . . ? C47 C42 C43 123.1(7) . . ? C41 C42 C43 117.3(7) . . ? C42 C43 C44 113.5(7) . . ? C42 C43 H43B 108.9 . . ? C44 C43 H43B 108.9 . . ? C42 C43 H43A 108.9 . . ? C44 C43 H43A 108.9 . . ? H43B C43 H43A 107.7 . . ? C45 C44 C43 111.0(7) . . ? C45 C44 H44A 109.4 . . ? C43 C44 H44A 109.4 . . ? C45 C44 H44B 109.4 . . ? C43 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 111.1(8) . . ? C44 C45 H45B 109.4 . . ? C46 C45 H45B 109.4 . . ? C44 C45 H45A 109.4 . . ? C46 C45 H45A 109.4 . . ? H45B C45 H45A 108.0 . . ? C45 C46 C47 111.7(7) . . ? C45 C46 H46B 109.3 . . ? C47 C46 H46B 109.3 . . ? C45 C46 H46A 109.3 . . ? C47 C46 H46A 109.3 . . ? H46B C46 H46A 107.9 . . ? C42 C47 C38 120.7(7) . . ? C42 C47 C46 120.2(7) . . ? C38 C47 C46 119.0(7) . . ? Pd2 C48 H48B 109.5 . . ? Pd2 C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Pd2 C48 H48A 109.5 . . ? H48B C48 H48A 109.5 . . ? H48C C48 H48A 109.5 . . ? N3 C49 H49B 109.5 . . ? N3 C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N3 C49 H49A 109.5 . . ? H49B C49 H49A 109.5 . . ? H49C C49 H49A 109.5 . . ? N3 C50 H50A 109.5 . . ? N3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? N3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? H50C C50 H50B 109.5 . . ? N3 C51 C52 109.8(7) . . ? N3 C51 H51A 109.7 . . ? C52 C51 H51A 109.7 . . ? N3 C51 H51B 109.7 . . ? C52 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? N4 C52 C51 110.2(7) . . ? N4 C52 H52B 109.6 . . ? C51 C52 H52B 109.6 . . ? N4 C52 H52A 109.6 . . ? C51 C52 H52A 109.6 . . ? H52B C52 H52A 108.1 . . ? N4 C53 H53A 109.5 . . ? N4 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? N4 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? H53C C53 H53B 109.5 . . ? N4 C54 H54B 109.5 . . ? N4 C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N4 C54 H54A 109.5 . . ? H54B C54 H54A 109.5 . . ? H54C C54 H54A 109.5 . . ? Cl2 C55 Cl1 111.6(6) . . ? Cl2 C55 H55B 109.3 . . ? Cl1 C55 H55B 109.3 . . ? Cl2 C55 H55A 109.3 . . ? Cl1 C55 H55A 109.3 . . ? H55B C55 H55A 108.0 . . ? Cl4 C56 Cl3 115.0(7) . . ? Cl4 C56 H56B 108.5 . . ? Cl3 C56 H56B 108.5 . . ? Cl4 C56 H56A 108.5 . . ? Cl3 C56 H56A 108.5 . . ? H56B C56 H56A 107.5 . . ? 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 C21 Pd1 O1 C1 -57.7(6) . . . . ? N2 Pd1 O1 C1 -179(3) . . . . ? N1 Pd1 O1 C1 119.5(6) . . . . ? C48 Pd2 O3 C28 -58.6(6) . . . . ? N4 Pd2 O3 C28 173(3) . . . . ? N3 Pd2 O3 C28 119.0(6) . . . . ? C21 Pd1 N1 C22 168(5) . . . . ? O1 Pd1 N1 C22 42.9(6) . . . . ? N2 Pd1 N1 C22 -132.8(6) . . . . ? C21 Pd1 N1 C23 45(6) . . . . ? O1 Pd1 N1 C23 -79.7(5) . . . . ? N2 Pd1 N1 C23 104.7(6) . . . . ? C21 Pd1 N1 C24 -72(5) . . . . ? O1 Pd1 N1 C24 163.3(5) . . . . ? N2 Pd1 N1 C24 -12.4(5) . . . . ? C21 Pd1 N2 C25 161.3(6) . . . . ? O1 Pd1 N2 C25 -78(3) . . . . ? N1 Pd1 N2 C25 -15.7(5) . . . . ? C21 Pd1 N2 C27 -79.8(6) . . . . ? O1 Pd1 N2 C27 41(3) . . . . ? N1 Pd1 N2 C27 103.2(6) . . . . ? C21 Pd1 N2 C26 41.1(6) . . . . ? O1 Pd1 N2 C26 162(3) . . . . ? N1 Pd1 N2 C26 -135.9(6) . . . . ? C48 Pd2 N3 C50 178(5) . . . . ? O3 Pd2 N3 C50 44.4(6) . . . . ? N4 Pd2 N3 C50 -131.4(6) . . . . ? C48 Pd2 N3 C51 -63(5) . . . . ? O3 Pd2 N3 C51 163.5(5) . . . . ? N4 Pd2 N3 C51 -12.2(5) . . . . ? C48 Pd2 N3 C49 55(5) . . . . ? O3 Pd2 N3 C49 -78.1(6) . . . . ? N4 Pd2 N3 C49 106.2(6) . . . . ? C48 Pd2 N4 C54 -80.1(6) . . . . ? O3 Pd2 N4 C54 48(3) . . . . ? N3 Pd2 N4 C54 102.4(5) . . . . ? C48 Pd2 N4 C53 42.0(6) . . . . ? O3 Pd2 N4 C53 170(3) . . . . ? N3 Pd2 N4 C53 -135.5(6) . . . . ? C48 Pd2 N4 C52 160.5(6) . . . . ? O3 Pd2 N4 C52 -71(3) . . . . ? N3 Pd2 N4 C52 -17.0(6) . . . . ? Pd1 O1 C1 C10 148.2(6) . . . . ? Pd1 O1 C1 C2 -37.6(9) . . . . ? O1 C1 C2 C3 -172.5(8) . . . . ? C10 C1 C2 C3 1.7(12) . . . . ? C1 C2 C3 C4 1.8(13) . . . . ? C2 C3 C4 C9 -2.0(13) . . . . ? C2 C3 C4 C5 177.3(8) . . . . ? C3 C4 C5 C6 -164.5(10) . . . . ? C9 C4 C5 C6 14.7(13) . . . . ? C4 C5 C6 C7 -38.7(15) . . . . ? C5 C6 C7 C8 54.1(16) . . . . ? C6 C7 C8 C9 -43.2(13) . . . . ? C3 C4 C9 C10 -1.4(11) . . . . ? C5 C4 C9 C10 179.4(7) . . . . ? C3 C4 C9 C8 173.2(7) . . . . ? C5 C4 C9 C8 -6.0(11) . . . . ? C7 C8 C9 C4 19.6(11) . . . . ? C7 C8 C9 C10 -165.8(8) . . . . ? O1 C1 C10 C9 169.4(7) . . . . ? C2 C1 C10 C9 -5.0(11) . . . . ? O1 C1 C10 C11 -12.0(10) . . . . ? C2 C1 C10 C11 173.6(7) . . . . ? C4 C9 C10 C1 4.9(11) . . . . ? C8 C9 C10 C1 -169.7(7) . . . . ? C4 C9 C10 C11 -173.7(7) . . . . ? C8 C9 C10 C11 11.7(10) . . . . ? C1 C10 C11 C12 62.3(10) . . . . ? C9 C10 C11 C12 -119.2(8) . . . . ? C1 C10 C11 C20 -117.1(8) . . . . ? C9 C10 C11 C20 61.4(10) . . . . ? C20 C11 C12 O2 169.6(7) . . . . ? C10 C11 C12 O2 -9.8(11) . . . . ? C20 C11 C12 C13 -11.1(11) . . . . ? C10 C11 C12 C13 169.5(7) . . . . ? O2 C12 C13 C14 -175.1(7) . . . . ? C11 C12 C13 C14 5.5(12) . . . . ? C12 C13 C14 C15 2.6(12) . . . . ? C13 C14 C15 C20 -4.8(12) . . . . ? C13 C14 C15 C16 175.5(7) . . . . ? C14 C15 C16 C17 169.1(9) . . . . ? C20 C15 C16 C17 -10.6(13) . . . . ? C15 C16 C17 C18 41.4(13) . . . . ? C16 C17 C18 C19 -58.6(14) . . . . ? C17 C18 C19 C20 42.4(12) . . . . ? C14 C15 C20 C11 -1.1(11) . . . . ? C16 C15 C20 C11 178.7(7) . . . . ? C14 C15 C20 C19 175.1(7) . . . . ? C16 C15 C20 C19 -5.1(11) . . . . ? C12 C11 C20 C15 8.8(11) . . . . ? C10 C11 C20 C15 -171.8(7) . . . . ? C12 C11 C20 C19 -167.4(7) . . . . ? C10 C11 C20 C19 12.0(11) . . . . ? C18 C19 C20 C15 -11.2(11) . . . . ? C18 C19 C20 C11 165.0(8) . . . . ? C22 N1 C24 C25 160.0(7) . . . . ? C23 N1 C24 C25 -78.0(9) . . . . ? Pd1 N1 C24 C25 38.1(7) . . . . ? C27 N2 C25 C24 -74.3(9) . . . . ? C26 N2 C25 C24 166.4(8) . . . . ? Pd1 N2 C25 C24 42.6(8) . . . . ? N1 C24 C25 N2 -57.0(10) . . . . ? Pd2 O3 C28 C29 -36.2(9) . . . . ? Pd2 O3 C28 C37 146.8(5) . . . . ? O3 C28 C29 C30 -172.9(7) . . . . ? C37 C28 C29 C30 4.0(11) . . . . ? C28 C29 C30 C31 2.3(12) . . . . ? C29 C30 C31 C36 -4.2(12) . . . . ? C29 C30 C31 C32 178.4(7) . . . . ? C30 C31 C32 C33 -165.7(8) . . . . ? C36 C31 C32 C33 16.9(11) . . . . ? C31 C32 C33 C34 -41.9(11) . . . . ? C32 C33 C34 C35 60.5(12) . . . . ? C33 C34 C35 C36 -50.2(11) . . . . ? C30 C31 C36 C37 -0.2(11) . . . . ? C32 C31 C36 C37 177.1(7) . . . . ? C30 C31 C36 C35 176.0(7) . . . . ? C32 C31 C36 C35 -6.7(11) . . . . ? C34 C35 C36 C31 22.7(10) . . . . ? C34 C35 C36 C37 -161.2(7) . . . . ? O3 C28 C37 C36 168.7(6) . . . . ? C29 C28 C37 C36 -8.4(10) . . . . ? O3 C28 C37 C38 -10.3(10) . . . . ? C29 C28 C37 C38 172.6(7) . . . . ? C31 C36 C37 C28 6.5(10) . . . . ? C35 C36 C37 C28 -169.7(6) . . . . ? C31 C36 C37 C38 -174.5(6) . . . . ? C35 C36 C37 C38 9.3(10) . . . . ? C28 C37 C38 C39 60.8(9) . . . . ? C36 C37 C38 C39 -118.2(8) . . . . ? C28 C37 C38 C47 -120.0(8) . . . . ? C36 C37 C38 C47 61.1(9) . . . . ? C47 C38 C39 O4 170.1(7) . . . . ? C37 C38 C39 O4 -10.6(11) . . . . ? C47 C38 C39 C40 -7.3(11) . . . . ? C37 C38 C39 C40 172.0(7) . . . . ? O4 C39 C40 C41 -176.4(7) . . . . ? C38 C39 C40 C41 1.1(11) . . . . ? C39 C40 C41 C42 5.6(12) . . . . ? C40 C41 C42 C47 -6.0(12) . . . . ? C40 C41 C42 C43 176.2(7) . . . . ? C47 C42 C43 C44 14.9(11) . . . . ? C41 C42 C43 C44 -167.4(8) . . . . ? C42 C43 C44 C45 -41.9(11) . . . . ? C43 C44 C45 C46 61.8(11) . . . . ? C44 C45 C46 C47 -51.9(10) . . . . ? C41 C42 C47 C38 -0.3(11) . . . . ? C43 C42 C47 C38 177.3(7) . . . . ? C41 C42 C47 C46 176.2(7) . . . . ? C43 C42 C47 C46 -6.2(11) . . . . ? C39 C38 C47 C42 6.9(11) . . . . ? C37 C38 C47 C42 -172.4(7) . . . . ? C39 C38 C47 C46 -169.7(6) . . . . ? C37 C38 C47 C46 11.1(10) . . . . ? C45 C46 C47 C42 24.4(10) . . . . ? C45 C46 C47 C38 -159.1(7) . . . . ? C50 N3 C51 C52 160.4(7) . . . . ? C49 N3 C51 C52 -78.1(9) . . . . ? Pd2 N3 C51 C52 38.6(7) . . . . ? C54 N4 C52 C51 -74.4(9) . . . . ? C53 N4 C52 C51 167.6(7) . . . . ? Pd2 N4 C52 C51 43.5(8) . . . . ? N3 C51 C52 N4 -58.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 7.143 _refine_diff_density_min -1.254 _refine_diff_density_rms 0.215 data_mx1321 _database_code_depnum_ccdc_archive 'CCDC 917457' #TrackingRef 'web_deposit_cif_file_0_YudongCai_1356446823.mx1321.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 N2 O2 Pd, C H Cl3' _chemical_formula_sum 'C27 H37 Cl3 N2 O2 Pd' _chemical_formula_weight 634.34 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.8418(15) _cell_length_b 11.4447(18) _cell_length_c 24.284(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2735.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7923 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8406 _exptl_absorpt_correction_T_max 0.9425 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17508 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6166 _reflns_number_gt 5607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELX97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+3.7941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 6166 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.05890(3) 0.64788(3) 0.999200(16) 0.02008(8) Uani 1 1 d . . . Cl1 Cl 0.19659(15) 0.17095(13) 1.06082(7) 0.0449(4) Uani 1 1 d . . . Cl2 Cl 0.43480(17) 0.31720(13) 1.05085(7) 0.0522(4) Uani 1 1 d . . . Cl3 Cl 0.33952(19) 0.24415(16) 1.15818(7) 0.0578(4) Uani 1 1 d . . . O1 O 0.1368(3) 0.7526(3) 0.94015(13) 0.0238(7) Uani 1 1 d . . . O2 O 0.0382(3) 0.5063(3) 0.95068(13) 0.0241(7) Uani 1 1 d . . . N1 N -0.0118(4) 0.5513(4) 1.06539(16) 0.0276(10) Uani 1 1 d . . . N2 N 0.0686(5) 0.7857(4) 1.05360(16) 0.0291(9) Uani 1 1 d . . . C1 C 0.0649(5) 0.7508(4) 0.89243(19) 0.0187(9) Uani 1 1 d . . . C2 C -0.0116(5) 0.8492(5) 0.87781(19) 0.0289(11) Uani 1 1 d . . . H2 H -0.0087 0.9177 0.8998 0.035 Uiso 1 1 calc R . . C3 C -0.0916(5) 0.8454(5) 0.8308(2) 0.0299(11) Uani 1 1 d . . . H3 H -0.1419 0.9129 0.8206 0.036 Uiso 1 1 calc R . . C4 C -0.1002(5) 0.7456(5) 0.7980(2) 0.0263(11) Uani 1 1 d . . . C5 C -0.1961(5) 0.7435(5) 0.7493(2) 0.0354(13) Uani 1 1 d . . . H5A H -0.1772 0.8124 0.7259 0.042 Uiso 1 1 calc R . . H5B H -0.2903 0.7510 0.7631 0.042 Uiso 1 1 calc R . . C6 C -0.1871(6) 0.6347(6) 0.7139(2) 0.0413(14) Uani 1 1 d . . . H6A H -0.1106 0.6428 0.6877 0.050 Uiso 1 1 calc R . . H6B H -0.2718 0.6263 0.6923 0.050 Uiso 1 1 calc R . . C7 C -0.1660(5) 0.5263(5) 0.7489(2) 0.0329(12) Uani 1 1 d . . . H7A H -0.1654 0.4560 0.7252 0.039 Uiso 1 1 calc R . . H7B H -0.2412 0.5185 0.7757 0.039 Uiso 1 1 calc R . . C8 C -0.0315(5) 0.5368(5) 0.7791(2) 0.0301(12) Uani 1 1 d . . . H8A H 0.0436 0.5336 0.7521 0.036 Uiso 1 1 calc R . . H8B H -0.0212 0.4696 0.8044 0.036 Uiso 1 1 calc R . . C9 C -0.0207(4) 0.6494(4) 0.81194(17) 0.0214(9) Uani 1 1 d . . . C10 C 0.0679(5) 0.6541(4) 0.85795(17) 0.0209(9) Uani 1 1 d . . . C11 C 0.1640(4) 0.5578(4) 0.86940(17) 0.0191(9) Uani 1 1 d . . . C12 C 0.2761(5) 0.5378(4) 0.83502(17) 0.0188(9) Uani 1 1 d . . . C13 C 0.3032(5) 0.6186(4) 0.78690(18) 0.0266(11) Uani 1 1 d . . . H13B H 0.2994 0.7003 0.8001 0.032 Uiso 1 1 calc R . . H13A H 0.2297 0.6084 0.7595 0.032 Uiso 1 1 calc R . . C14 C 0.4392(5) 0.5989(5) 0.75851(19) 0.0314(11) Uani 1 1 d . . . H14A H 0.4377 0.6366 0.7218 0.038 Uiso 1 1 calc R . . H14B H 0.5120 0.6361 0.7805 0.038 Uiso 1 1 calc R . . C15 C 0.4704(5) 0.4714(5) 0.7518(2) 0.0325(13) Uani 1 1 d . . . H15B H 0.5574 0.4620 0.7318 0.039 Uiso 1 1 calc R . . H15A H 0.3979 0.4335 0.7298 0.039 Uiso 1 1 calc R . . C16 C 0.4801(5) 0.4142(5) 0.8074(2) 0.0305(12) Uani 1 1 d . . . H16B H 0.5647 0.4403 0.8256 0.037 Uiso 1 1 calc R . . H16A H 0.4861 0.3285 0.8023 0.037 Uiso 1 1 calc R . . C17 C 0.3611(5) 0.4413(4) 0.84450(18) 0.0215(10) Uani 1 1 d . . . C18 C 0.3337(5) 0.3677(4) 0.88888(19) 0.0247(10) Uani 1 1 d . . . H18 H 0.3892 0.3010 0.8948 0.030 Uiso 1 1 calc R . . C19 C 0.2275(5) 0.3902(4) 0.92445(19) 0.0248(11) Uani 1 1 d . . . H19 H 0.2119 0.3397 0.9548 0.030 Uiso 1 1 calc R . . C20 C 0.1424(5) 0.4867(4) 0.91618(18) 0.0185(10) Uani 1 1 d . . . C21 C -0.0610(8) 0.6411(6) 1.1051(2) 0.0543(17) Uani 1 1 d . . . H21A H -0.1516 0.6690 1.0933 0.065 Uiso 1 1 calc R . . H21B H -0.0711 0.6049 1.1419 0.065 Uiso 1 1 calc R . . C22 C 0.0285(7) 0.7377(6) 1.1091(3) 0.054(2) Uani 1 1 d . . . H22A H 0.1113 0.7134 1.1292 0.065 Uiso 1 1 calc R . . H22B H -0.0159 0.8003 1.1307 0.065 Uiso 1 1 calc R . . C23 C -0.1270(7) 0.4737(7) 1.0538(3) 0.061(2) Uani 1 1 d . . . H23B H -0.2054 0.5204 1.0422 0.091 Uiso 1 1 calc R . . H23C H -0.1502 0.4296 1.0870 0.091 Uiso 1 1 calc R . . H23A H -0.1022 0.4193 1.0243 0.091 Uiso 1 1 calc R . . C24 C 0.0978(7) 0.4794(6) 1.0863(3) 0.056(2) Uani 1 1 d . . . H24A H 0.1221 0.4204 1.0587 0.084 Uiso 1 1 calc R . . H24C H 0.0686 0.4406 1.1202 0.084 Uiso 1 1 calc R . . H24B H 0.1770 0.5287 1.0940 0.084 Uiso 1 1 calc R . . C25 C 0.2067(5) 0.8342(5) 1.0583(2) 0.0371(13) Uani 1 1 d . . . H25B H 0.2696 0.7725 1.0699 0.056 Uiso 1 1 calc R . . H25C H 0.2071 0.8973 1.0856 0.056 Uiso 1 1 calc R . . H25A H 0.2354 0.8650 1.0225 0.056 Uiso 1 1 calc R . . C26 C -0.0268(6) 0.8767(5) 1.0362(2) 0.0443(15) Uani 1 1 d . . . H26A H -0.0013 0.9051 0.9996 0.066 Uiso 1 1 calc R . . H26C H -0.0242 0.9415 1.0625 0.066 Uiso 1 1 calc R . . H26B H -0.1189 0.8442 1.0349 0.066 Uiso 1 1 calc R . . C27 C 0.3586(6) 0.2045(5) 1.0886(2) 0.0336(13) Uani 1 1 d . . . H27 H 0.4174 0.1334 1.0864 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02056(14) 0.02429(15) 0.01538(13) -0.0019(2) 0.00246(18) 0.00221(14) Cl1 0.0381(8) 0.0375(8) 0.0592(9) -0.0057(7) -0.0048(7) 0.0003(7) Cl2 0.0425(8) 0.0460(9) 0.0682(10) 0.0126(8) 0.0086(8) -0.0030(8) Cl3 0.0627(11) 0.0686(11) 0.0419(9) -0.0050(8) -0.0024(8) 0.0055(10) O1 0.0260(17) 0.0270(19) 0.0183(17) -0.0014(15) 0.0015(14) -0.0031(16) O2 0.0289(19) 0.0219(16) 0.0213(16) -0.0045(14) 0.0064(14) -0.0021(15) N1 0.040(2) 0.027(2) 0.0160(19) 0.0027(18) 0.0033(17) 0.012(2) N2 0.038(2) 0.029(2) 0.020(2) -0.0051(18) 0.005(2) 0.002(2) C1 0.018(2) 0.017(2) 0.022(2) 0.0018(18) 0.010(2) -0.002(2) C2 0.034(3) 0.023(2) 0.030(2) 0.000(2) 0.014(2) -0.001(2) C3 0.027(3) 0.030(3) 0.032(3) 0.016(2) 0.006(2) 0.007(2) C4 0.021(2) 0.033(3) 0.026(2) 0.009(2) 0.0026(19) 0.000(2) C5 0.024(3) 0.045(3) 0.038(3) 0.017(3) -0.007(2) 0.005(3) C6 0.031(3) 0.064(4) 0.029(3) 0.006(3) -0.010(2) -0.004(3) C7 0.025(3) 0.040(3) 0.034(3) -0.004(2) -0.003(2) 0.002(3) C8 0.021(3) 0.038(3) 0.031(3) -0.005(2) -0.006(2) 0.000(2) C9 0.020(2) 0.026(2) 0.018(2) -0.001(2) 0.0032(16) -0.004(2) C10 0.022(2) 0.020(2) 0.022(2) -0.0003(19) 0.0054(18) -0.002(2) C11 0.017(2) 0.024(2) 0.016(2) -0.0011(19) 0.0015(17) -0.003(2) C12 0.022(2) 0.023(2) 0.012(2) -0.0040(18) 0.0000(17) -0.006(2) C13 0.023(2) 0.036(3) 0.021(2) 0.006(2) 0.0063(19) -0.003(2) C14 0.028(3) 0.046(3) 0.020(2) -0.004(2) 0.004(2) -0.011(3) C15 0.022(3) 0.051(3) 0.024(2) -0.011(2) 0.005(2) -0.005(2) C16 0.024(3) 0.036(3) 0.031(3) -0.006(2) 0.007(2) 0.005(2) C17 0.017(2) 0.028(3) 0.020(2) -0.007(2) -0.0036(18) -0.001(2) C18 0.024(2) 0.018(2) 0.033(2) -0.007(2) -0.007(2) 0.003(2) C19 0.032(3) 0.022(2) 0.020(2) -0.0003(19) -0.006(2) -0.004(2) C20 0.022(2) 0.021(2) 0.013(2) -0.0015(19) 0.0053(18) -0.003(2) C21 0.088(5) 0.046(3) 0.028(3) 0.003(3) 0.023(3) 0.009(4) C22 0.065(5) 0.068(5) 0.028(3) -0.018(3) 0.015(3) -0.002(4) C23 0.055(4) 0.092(6) 0.035(3) 0.026(4) -0.003(3) -0.036(4) C24 0.054(4) 0.052(4) 0.061(4) 0.032(4) 0.007(3) 0.022(4) C25 0.036(3) 0.037(3) 0.038(3) -0.006(3) -0.008(2) 0.001(3) C26 0.050(4) 0.044(4) 0.038(3) -0.016(3) -0.002(3) 0.022(3) C27 0.032(3) 0.028(3) 0.041(3) 0.004(2) -0.001(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 2.013(3) . ? Pd1 O1 2.020(3) . ? Pd1 N2 2.060(4) . ? Pd1 N1 2.071(4) . ? Cl1 C27 1.774(6) . ? Cl2 C27 1.752(6) . ? Cl3 C27 1.759(6) . ? O1 C1 1.358(6) . ? O2 C20 1.343(5) . ? N1 C24 1.448(7) . ? N1 C23 1.467(8) . ? N1 C21 1.491(7) . ? N2 C26 1.465(7) . ? N2 C25 1.472(7) . ? N2 C22 1.507(7) . ? C1 C10 1.388(6) . ? C1 C2 1.400(7) . ? C2 C3 1.388(7) . ? C2 H2 0.9500 . ? C3 C4 1.395(7) . ? C3 H3 0.9500 . ? C4 C9 1.392(7) . ? C4 C5 1.513(7) . ? C5 C6 1.515(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.518(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.518(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.418(6) . ? C10 C11 1.479(6) . ? C11 C12 1.403(6) . ? C11 C20 1.414(6) . ? C12 C17 1.404(6) . ? C12 C13 1.514(6) . ? C13 C14 1.523(7) . ? C13 H13B 0.9900 . ? C13 H13A 0.9900 . ? C14 C15 1.500(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.504(7) . ? C15 H15B 0.9900 . ? C15 H15A 0.9900 . ? C16 C17 1.510(6) . ? C16 H16B 0.9900 . ? C16 H16A 0.9900 . ? C17 C18 1.393(7) . ? C18 C19 1.381(7) . ? C18 H18 0.9500 . ? C19 C20 1.401(7) . ? C19 H19 0.9500 . ? C21 C22 1.417(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23A 0.9800 . ? C24 H24A 0.9800 . ? C24 H24C 0.9800 . ? C24 H24B 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25A 0.9800 . ? C26 H26A 0.9800 . ? C26 H26C 0.9800 . ? C26 H26B 0.9800 . ? C27 H27 1.0000 . ? 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 O2 Pd1 O1 95.75(13) . . ? O2 Pd1 N2 174.99(15) . . ? O1 Pd1 N2 89.06(15) . . ? O2 Pd1 N1 89.46(16) . . ? O1 Pd1 N1 174.33(15) . . ? N2 Pd1 N1 85.80(17) . . ? C1 O1 Pd1 113.5(3) . . ? C20 O2 Pd1 115.0(3) . . ? C24 N1 C23 107.4(5) . . ? C24 N1 C21 114.0(5) . . ? C23 N1 C21 106.9(5) . . ? C24 N1 Pd1 108.9(4) . . ? C23 N1 Pd1 115.7(3) . . ? C21 N1 Pd1 104.1(3) . . ? C26 N2 C25 110.3(4) . . ? C26 N2 C22 110.4(5) . . ? C25 N2 C22 108.1(5) . . ? C26 N2 Pd1 109.2(3) . . ? C25 N2 Pd1 112.4(3) . . ? C22 N2 Pd1 106.4(3) . . ? O1 C1 C10 121.0(4) . . ? O1 C1 C2 119.0(4) . . ? C10 C1 C2 120.0(5) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 121.9(5) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C9 C4 C3 118.4(4) . . ? C9 C4 C5 121.9(5) . . ? C3 C4 C5 119.8(5) . . ? C4 C5 C6 114.8(4) . . ? C4 C5 H5A 108.6 . . ? C6 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? C6 C5 H5B 108.6 . . ? H5A C5 H5B 107.5 . . ? C5 C6 C7 111.2(4) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C6 C7 C8 109.0(4) . . ? C6 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? C6 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C7 C8 C9 112.5(4) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C4 C9 C10 120.4(4) . . ? C4 C9 C8 120.3(4) . . ? C10 C9 C8 119.3(4) . . ? C1 C10 C9 119.5(4) . . ? C1 C10 C11 119.6(4) . . ? C9 C10 C11 120.9(4) . . ? C12 C11 C20 120.2(4) . . ? C12 C11 C10 120.9(4) . . ? C20 C11 C10 118.9(4) . . ? C11 C12 C17 120.0(4) . . ? C11 C12 C13 119.9(4) . . ? C17 C12 C13 120.2(4) . . ? C12 C13 C14 114.4(4) . . ? C12 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? H13B C13 H13A 107.6 . . ? C15 C14 C13 111.9(4) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 109.8(4) . . ? C14 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? H15B C15 H15A 108.2 . . ? C15 C16 C17 113.4(4) . . ? C15 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? H16B C16 H16A 107.7 . . ? C18 C17 C12 119.1(4) . . ? C18 C17 C16 119.2(4) . . ? C12 C17 C16 121.7(4) . . ? C19 C18 C17 121.2(4) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 120.7(5) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? O2 C20 C19 119.9(4) . . ? O2 C20 C11 121.4(4) . . ? C19 C20 C11 118.6(4) . . ? C22 C21 N1 112.3(5) . . ? C22 C21 H21A 109.1 . . ? N1 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? N1 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C21 C22 N2 112.7(5) . . ? C21 C22 H22A 109.0 . . ? N2 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? N2 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N1 C23 H23B 109.5 . . ? N1 C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? H24C C24 H24B 109.5 . . ? N2 C25 H25B 109.5 . . ? N2 C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? Cl2 C27 Cl3 111.0(3) . . ? Cl2 C27 Cl1 110.2(3) . . ? Cl3 C27 Cl1 109.0(3) . . ? Cl2 C27 H27 108.9 . . ? Cl3 C27 H27 108.9 . . ? Cl1 C27 H27 108.9 . . ? 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 O2 Pd1 O1 C1 48.5(3) . . . . ? N2 Pd1 O1 C1 -130.0(3) . . . . ? N1 Pd1 O1 C1 -154.8(15) . . . . ? O1 Pd1 O2 C20 41.4(3) . . . . ? N2 Pd1 O2 C20 -155.2(18) . . . . ? N1 Pd1 O2 C20 -136.3(3) . . . . ? O2 Pd1 N1 C24 79.4(4) . . . . ? O1 Pd1 N1 C24 -77.3(17) . . . . ? N2 Pd1 N1 C24 -102.2(4) . . . . ? O2 Pd1 N1 C23 -41.6(5) . . . . ? O1 Pd1 N1 C23 161.6(14) . . . . ? N2 Pd1 N1 C23 136.7(5) . . . . ? O2 Pd1 N1 C21 -158.6(4) . . . . ? O1 Pd1 N1 C21 44.7(17) . . . . ? N2 Pd1 N1 C21 19.8(4) . . . . ? O2 Pd1 N2 C26 -97.0(19) . . . . ? O1 Pd1 N2 C26 66.4(4) . . . . ? N1 Pd1 N2 C26 -115.9(4) . . . . ? O2 Pd1 N2 C25 140.3(18) . . . . ? O1 Pd1 N2 C25 -56.3(4) . . . . ? N1 Pd1 N2 C25 121.3(4) . . . . ? O2 Pd1 N2 C22 22(2) . . . . ? O1 Pd1 N2 C22 -174.4(4) . . . . ? N1 Pd1 N2 C22 3.2(4) . . . . ? Pd1 O1 C1 C10 -72.1(5) . . . . ? Pd1 O1 C1 C2 108.9(4) . . . . ? O1 C1 C2 C3 -176.3(4) . . . . ? C10 C1 C2 C3 4.7(7) . . . . ? C1 C2 C3 C4 1.2(7) . . . . ? C2 C3 C4 C9 -3.1(7) . . . . ? C2 C3 C4 C5 175.9(5) . . . . ? C9 C4 C5 C6 -6.3(7) . . . . ? C3 C4 C5 C6 174.7(5) . . . . ? C4 C5 C6 C7 38.6(6) . . . . ? C5 C6 C7 C8 -62.6(6) . . . . ? C6 C7 C8 C9 53.9(6) . . . . ? C3 C4 C9 C10 -0.8(7) . . . . ? C5 C4 C9 C10 -179.8(4) . . . . ? C3 C4 C9 C8 177.1(4) . . . . ? C5 C4 C9 C8 -1.9(7) . . . . ? C7 C8 C9 C4 -22.5(6) . . . . ? C7 C8 C9 C10 155.4(4) . . . . ? O1 C1 C10 C9 172.5(4) . . . . ? C2 C1 C10 C9 -8.5(7) . . . . ? O1 C1 C10 C11 -7.9(7) . . . . ? C2 C1 C10 C11 171.1(4) . . . . ? C4 C9 C10 C1 6.6(6) . . . . ? C8 C9 C10 C1 -171.3(4) . . . . ? C4 C9 C10 C11 -173.0(4) . . . . ? C8 C9 C10 C11 9.1(6) . . . . ? C1 C10 C11 C12 -109.8(5) . . . . ? C9 C10 C11 C12 69.7(6) . . . . ? C1 C10 C11 C20 69.3(6) . . . . ? C9 C10 C11 C20 -111.1(5) . . . . ? C20 C11 C12 C17 5.1(7) . . . . ? C10 C11 C12 C17 -175.8(4) . . . . ? C20 C11 C12 C13 -176.5(4) . . . . ? C10 C11 C12 C13 2.7(6) . . . . ? C11 C12 C13 C14 170.8(4) . . . . ? C17 C12 C13 C14 -10.7(6) . . . . ? C12 C13 C14 C15 41.9(6) . . . . ? C13 C14 C15 C16 -61.8(6) . . . . ? C14 C15 C16 C17 49.7(6) . . . . ? C11 C12 C17 C18 -1.2(7) . . . . ? C13 C12 C17 C18 -179.6(4) . . . . ? C11 C12 C17 C16 177.9(4) . . . . ? C13 C12 C17 C16 -0.5(7) . . . . ? C15 C16 C17 C18 159.7(4) . . . . ? C15 C16 C17 C12 -19.4(7) . . . . ? C12 C17 C18 C19 -2.0(7) . . . . ? C16 C17 C18 C19 178.9(4) . . . . ? C17 C18 C19 C20 1.2(7) . . . . ? Pd1 O2 C20 C19 110.8(4) . . . . ? Pd1 O2 C20 C11 -72.9(5) . . . . ? C18 C19 C20 O2 179.0(4) . . . . ? C18 C19 C20 C11 2.6(7) . . . . ? C12 C11 C20 O2 177.9(4) . . . . ? C10 C11 C20 O2 -1.2(7) . . . . ? C12 C11 C20 C19 -5.7(7) . . . . ? C10 C11 C20 C19 175.1(4) . . . . ? C24 N1 C21 C22 76.4(7) . . . . ? C23 N1 C21 C22 -165.0(6) . . . . ? Pd1 N1 C21 C22 -42.2(6) . . . . ? N1 C21 C22 N2 49.0(8) . . . . ? C26 N2 C22 C21 90.1(7) . . . . ? C25 N2 C22 C21 -149.2(6) . . . . ? Pd1 N2 C22 C21 -28.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.797 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.093