# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Catherine S. J. Cazin' _publ_contact_author_email cc111@st-andrews.ac.uk loop_ _publ_author_name 'Vaclav Jurcik' 'Thibault Schmid' 'Quentin Dumont' 'Alexandra Slawin' 'Catherine Cazin' data_2c _database_code_depnum_ccdc_archive 'CCDC 799172' #TrackingRef '- 2c.cif' # start Validation Reply Form _vrf_PLAT216_2c ; PROBLEM: Disordered C56 (An/Solv) ADP max/min Ratio 13.20 RESPONSE: half-weight pentane solvent atom. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H71 N2 O2 P Pd, C H2 Cl2, C6 H6, 0.5(C5 H12)' _chemical_formula_sum 'C54.50 H85 Cl2 N2 O2 P Pd' _chemical_formula_weight 1008.52 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.578(7) _cell_length_b 26.279(12) _cell_length_c 16.698(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.148(4) _cell_angle_gamma 90.00 _cell_volume 5557(5) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 10511 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.206 _exptl_crystal_size_mid 0.197 _exptl_crystal_size_min 0.151 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 ccd _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48593 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.40 _reflns_number_total 10183 _reflns_number_gt 8149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Some ISOR and DFIX restaints were used on the hydrocarbon solvent moieties. ; _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^)+(0.0737P)^2^+22.8400P] 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 10183 _refine_ls_number_parameters 575 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1759 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.174 _refine_ls_shift/su_mean 0.002 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 0.65545(3) 0.194417(14) 0.99397(2) 0.01994(11) Uani 1 1 d . . . O1 O 0.6129(3) 0.19078(13) 1.0970(2) 0.0285(8) Uani 1 1 d . . . O2 O 0.5707(3) 0.23618(14) 1.0473(2) 0.0302(8) Uani 1 1 d . . . C1 C 0.6536(4) 0.23099(18) 0.8868(3) 0.0195(10) Uani 1 1 d . . . N2 N 0.5641(3) 0.23941(16) 0.8183(3) 0.0231(9) Uani 1 1 d . . . C3 C 0.5829(4) 0.2664(2) 0.7472(3) 0.0300(12) Uani 1 1 d . . . H3A H 0.5320 0.2945 0.7245 0.036 Uiso 1 1 calc R . . H3B H 0.5787 0.2428 0.6998 0.036 Uiso 1 1 calc R . . C4 C 0.6944(4) 0.2863(2) 0.7915(3) 0.0280(12) Uani 1 1 d . . . H4A H 0.7377 0.2812 0.7555 0.034 Uiso 1 1 calc R . . H4B H 0.6942 0.3229 0.8055 0.034 Uiso 1 1 calc R . . N5 N 0.7337(3) 0.25485(16) 0.8705(3) 0.0240(9) Uani 1 1 d . . . C6 C 0.4558(4) 0.2340(2) 0.8134(3) 0.0250(10) Uani 1 1 d U . . C7 C 0.4001(4) 0.1893(2) 0.7790(3) 0.0273(12) Uani 1 1 d . . . C8 C 0.2933(4) 0.1875(2) 0.7682(4) 0.0334(13) Uani 1 1 d . . . H8A H 0.2538 0.1576 0.7458 0.040 Uiso 1 1 calc R . . C9 C 0.2442(4) 0.2288(2) 0.7895(4) 0.0375(14) Uani 1 1 d . . . H9A H 0.1713 0.2269 0.7813 0.045 Uiso 1 1 calc R . . C10 C 0.2997(4) 0.2723(2) 0.8222(4) 0.0348(13) Uani 1 1 d . . . H10A H 0.2647 0.3002 0.8365 0.042 Uiso 1 1 calc R . . C11 C 0.4067(4) 0.2762(2) 0.8349(3) 0.0277(12) Uani 1 1 d . . . C12 C 0.4494(4) 0.1452(2) 0.7487(3) 0.0307(12) Uani 1 1 d . . . H12A H 0.5279 0.1485 0.7758 0.037 Uiso 1 1 calc R . . C13 C 0.4181(5) 0.0937(2) 0.7750(4) 0.0419(15) Uani 1 1 d . . . H13A H 0.4384 0.0925 0.8376 0.063 Uiso 1 1 calc R . . H13B H 0.4543 0.0664 0.7565 0.063 Uiso 1 1 calc R . . H13C H 0.3416 0.0891 0.7478 0.063 Uiso 1 1 calc R . . C14 C 0.4191(5) 0.1482(3) 0.6513(4) 0.0464(16) Uani 1 1 d . . . H14A H 0.4405 0.1813 0.6360 0.070 Uiso 1 1 calc R . . H14B H 0.3425 0.1442 0.6233 0.070 Uiso 1 1 calc R . . H14C H 0.4550 0.1210 0.6323 0.070 Uiso 1 1 calc R . . C15 C 0.4637(5) 0.3259(2) 0.8670(3) 0.0333(13) Uani 1 1 d . . . H15A H 0.5392 0.3217 0.8730 0.040 Uiso 1 1 calc R . . C16 C 0.4157(5) 0.3698(2) 0.8030(4) 0.0403(15) Uani 1 1 d . . . H16A H 0.4182 0.3610 0.7467 0.060 Uiso 1 1 calc R . . H16B H 0.4563 0.4010 0.8241 0.060 Uiso 1 1 calc R . . H16C H 0.3421 0.3753 0.7976 0.060 Uiso 1 1 calc R . . C17 C 0.4606(5) 0.3395(2) 0.9565(4) 0.0410(15) Uani 1 1 d . . . H17A H 0.4916 0.3116 0.9967 0.061 Uiso 1 1 calc R . . H17B H 0.3872 0.3447 0.9517 0.061 Uiso 1 1 calc R . . H17C H 0.5010 0.3707 0.9776 0.061 Uiso 1 1 calc R . . C18 C 0.8357(4) 0.2667(2) 0.9334(3) 0.0242(11) Uani 1 1 d . . . C19 C 0.8445(4) 0.29796(19) 1.0054(3) 0.0266(11) Uani 1 1 d . . . C20 C 0.9460(4) 0.3105(2) 1.0614(4) 0.0326(13) Uani 1 1 d . . . H20A H 0.9535 0.3305 1.1107 0.039 Uiso 1 1 calc R . . C21 C 1.0357(5) 0.2948(2) 1.0476(4) 0.0364(14) Uani 1 1 d . . . H21A H 1.1037 0.3032 1.0877 0.044 Uiso 1 1 calc R . . C22 C 1.0258(4) 0.2668(2) 0.9750(4) 0.0349(13) Uani 1 1 d . . . H22A H 1.0875 0.2574 0.9644 0.042 Uiso 1 1 calc R . . C23 C 0.9269(4) 0.2520(2) 0.9169(3) 0.0270(11) Uani 1 1 d . . . C24 C 0.7513(4) 0.3215(2) 1.0203(4) 0.0303(12) Uani 1 1 d . . . H24A H 0.6860 0.3039 0.9820 0.036 Uiso 1 1 calc R . . C25 C 0.7429(5) 0.3783(2) 0.9944(5) 0.0464(16) Uani 1 1 d . . . H25A H 0.7400 0.3813 0.9351 0.070 Uiso 1 1 calc R . . H25B H 0.8047 0.3967 1.0328 0.070 Uiso 1 1 calc R . . H25C H 0.6786 0.3928 0.9989 0.070 Uiso 1 1 calc R . . C26 C 0.7563(5) 0.3158(2) 1.1128(4) 0.0380(14) Uani 1 1 d . . . H26A H 0.7614 0.2796 1.1282 0.057 Uiso 1 1 calc R . . H26B H 0.6923 0.3302 1.1180 0.057 Uiso 1 1 calc R . . H26C H 0.8184 0.3338 1.1515 0.057 Uiso 1 1 calc R . . C27 C 0.9223(4) 0.2246(2) 0.8355(3) 0.0295(12) Uani 1 1 d . . . H27A H 0.8483 0.2127 0.8048 0.035 Uiso 1 1 calc R . . C28 C 0.9508(5) 0.2631(2) 0.7771(4) 0.0351(13) Uani 1 1 d . . . H28A H 0.9035 0.2925 0.7665 0.053 Uiso 1 1 calc R . . H28B H 0.9429 0.2467 0.7224 0.053 Uiso 1 1 calc R . . H28C H 1.0240 0.2743 0.8055 0.053 Uiso 1 1 calc R . . C29 C 0.9963(4) 0.1785(2) 0.8514(4) 0.0356(13) Uani 1 1 d . . . H29A H 0.9784 0.1540 0.8882 0.053 Uiso 1 1 calc R . . H29B H 1.0695 0.1897 0.8797 0.053 Uiso 1 1 calc R . . H29C H 0.9881 0.1624 0.7964 0.053 Uiso 1 1 calc R . . P1 P 0.74673(10) 0.11948(5) 0.99903(8) 0.0215(3) Uani 1 1 d . . . C30 C 0.7202(4) 0.07699(19) 1.0779(3) 0.0254(11) Uani 1 1 d . . . H30A H 0.7529 0.0431 1.0762 0.030 Uiso 1 1 calc R . . C31 C 0.7663(4) 0.0972(2) 1.1709(3) 0.0288(12) Uani 1 1 d . . . H31A H 0.8443 0.0984 1.1897 0.035 Uiso 1 1 calc R . . H31B H 0.7407 0.1323 1.1725 0.035 Uiso 1 1 calc R . . C32 C 0.7351(5) 0.0638(2) 1.2332(4) 0.0385(14) Uani 1 1 d . . . H32A H 0.7682 0.0299 1.2371 0.046 Uiso 1 1 calc R . . H32B H 0.7620 0.0794 1.2910 0.046 Uiso 1 1 calc R . . C33 C 0.6153(5) 0.0576(3) 1.2042(4) 0.0456(16) Uani 1 1 d . . . H33A H 0.5979 0.0347 1.2443 0.055 Uiso 1 1 calc R . . H33B H 0.5821 0.0911 1.2049 0.055 Uiso 1 1 calc R . . C34 C 0.5721(5) 0.0355(2) 1.1141(4) 0.0422(15) Uani 1 1 d . . . H34A H 0.4944 0.0322 1.0954 0.051 Uiso 1 1 calc R . . H34B H 0.6020 0.0011 1.1144 0.051 Uiso 1 1 calc R . . C35 C 0.5999(4) 0.0695(2) 1.0510(4) 0.0299(12) Uani 1 1 d . . . H35A H 0.5656 0.1031 1.0478 0.036 Uiso 1 1 calc R . . H35B H 0.5720 0.0539 0.9931 0.036 Uiso 1 1 calc R . . C36 C 0.8927(4) 0.1236(2) 1.0321(3) 0.0274(12) Uani 1 1 d . . . H36A H 0.9063 0.1350 0.9799 0.033 Uiso 1 1 calc R . . C37 C 0.9422(4) 0.1644(2) 1.1008(3) 0.0299(12) Uani 1 1 d . . . H37A H 0.9084 0.1977 1.0800 0.036 Uiso 1 1 calc R . . H37B H 0.9292 0.1556 1.1538 0.036 Uiso 1 1 calc R . . C38 C 1.0610(4) 0.1687(2) 1.1212(4) 0.0366(14) Uani 1 1 d . . . H38A H 1.0736 0.1809 1.0696 0.044 Uiso 1 1 calc R . . H38B H 1.0912 0.1941 1.1674 0.044 Uiso 1 1 calc R . . C39 C 1.1166(5) 0.1181(3) 1.1493(4) 0.0455(16) Uani 1 1 d . . . H39A H 1.1929 0.1220 1.1605 0.055 Uiso 1 1 calc R . . H39B H 1.1084 0.1068 1.2031 0.055 Uiso 1 1 calc R . . C40 C 1.0698(5) 0.0785(3) 1.0797(4) 0.0450(16) Uani 1 1 d . . . H40A H 1.1047 0.0453 1.0993 0.054 Uiso 1 1 calc R . . H40B H 1.0831 0.0886 1.0274 0.054 Uiso 1 1 calc R . . C41 C 0.9515(4) 0.0730(2) 1.0584(4) 0.0366(14) Uani 1 1 d . . . H41A H 0.9390 0.0594 1.1091 0.044 Uiso 1 1 calc R . . H41B H 0.9228 0.0482 1.0110 0.044 Uiso 1 1 calc R . . C42 C 0.7011(4) 0.0805(2) 0.8977(3) 0.0257(11) Uani 1 1 d . . . H42A H 0.6234 0.0866 0.8708 0.031 Uiso 1 1 calc R . . C43 C 0.7140(4) 0.02208(19) 0.9069(3) 0.0287(12) Uani 1 1 d . . . H43A H 0.7900 0.0135 0.9323 0.034 Uiso 1 1 calc R . . H43B H 0.6796 0.0096 0.9463 0.034 Uiso 1 1 calc R . . C44 C 0.6650(5) -0.0045(2) 0.8201(4) 0.0338(13) Uani 1 1 d . . . H44A H 0.6769 -0.0416 0.8278 0.041 Uiso 1 1 calc R . . H44B H 0.5879 0.0016 0.7971 0.041 Uiso 1 1 calc R . . C45 C 0.7127(6) 0.0150(2) 0.7564(4) 0.0429(15) Uani 1 1 d . . . H45A H 0.6779 -0.0019 0.7002 0.051 Uiso 1 1 calc R . . H45B H 0.7888 0.0064 0.7771 0.051 Uiso 1 1 calc R . . C46 C 0.6987(5) 0.0733(2) 0.7453(4) 0.0380(14) Uani 1 1 d . . . H46A H 0.7327 0.0855 0.7054 0.046 Uiso 1 1 calc R . . H46B H 0.6225 0.0816 0.7200 0.046 Uiso 1 1 calc R . . C47 C 0.7481(5) 0.1006(2) 0.8322(3) 0.0312(12) Uani 1 1 d . . . H47A H 0.7349 0.1376 0.8241 0.037 Uiso 1 1 calc R . . H47B H 0.8255 0.0951 0.8548 0.037 Uiso 1 1 calc R . . C48 C 0.3645(5) 0.3234(3) 0.5114(4) 0.0489(17) Uani 1 1 d . . . H48A H 0.4421 0.3246 0.5410 0.059 Uiso 1 1 calc R . . H48B H 0.3492 0.3083 0.4539 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.30813(14) 0.28461(9) 0.57124(14) 0.0696(6) Uani 1 1 d . . . Cl2 Cl 0.31365(19) 0.38518(9) 0.50022(19) 0.0863(7) Uani 1 1 d . . . C49 C 0.1042(8) 0.4287(3) 0.1992(6) 0.110(2) Uani 1 1 d GU . . H49A H 0.1415 0.4156 0.1653 0.132 Uiso 1 1 calc R . . C50 C 0.1492(7) 0.4267(4) 0.2883(7) 0.172(2) Uani 1 1 d GU . . H50A H 0.2173 0.4121 0.3153 0.206 Uiso 1 1 calc R . . C51 C 0.0946(10) 0.4459(4) 0.3379(6) 0.153(2) Uani 1 1 d GU . . H51A H 0.1254 0.4445 0.3987 0.184 Uiso 1 1 calc R . . C52 C -0.0049(10) 0.4672(4) 0.2984(9) 0.169(2) Uani 1 1 d GU . . H52A H -0.0422 0.4803 0.3323 0.203 Uiso 1 1 calc R . . C53 C -0.0499(7) 0.4692(4) 0.2093(9) 0.267(3) Uani 1 1 d GU . . H53A H -0.1180 0.4838 0.1824 0.320 Uiso 1 1 calc R . . C54 C 0.0046(8) 0.4500(4) 0.1598(6) 0.177(2) Uani 1 1 d GU . . H54A H -0.0262 0.4514 0.0989 0.212 Uiso 1 1 calc R . . C55 C 0.4088(12) 0.4961(7) 0.0617(11) 0.067(2) Uani 0.50 1 d PDU . . H55A H 0.4339 0.5181 0.1125 0.101 Uiso 0.50 1 calc PR . . H55B H 0.4140 0.5143 0.0122 0.101 Uiso 0.50 1 calc PR . . H55C H 0.4521 0.4652 0.0722 0.101 Uiso 0.50 1 calc PR . . C56 C 0.2929(14) 0.4814(5) 0.0432(10) 0.099(8) Uani 0.50 1 d PD . . H56A H 0.2552 0.5143 0.0376 0.119 Uiso 0.50 1 calc PR . . H56B H 0.2928 0.4660 0.0973 0.119 Uiso 0.50 1 calc PR . . C57 C 0.2152(16) 0.4463(10) -0.0313(15) 0.123(3) Uani 0.50 1 d PDU . . H57A H 0.2106 0.4624 -0.0862 0.148 Uiso 0.50 1 calc PR . . H57B H 0.2528 0.4136 -0.0282 0.148 Uiso 0.50 1 calc PR . . C58 C 0.0993(18) 0.4320(10) -0.0415(17) 0.134(3) Uani 0.50 1 d PDU . . H58A H 0.0967 0.4173 0.0123 0.161 Uiso 0.50 1 calc PR . . H58B H 0.0525 0.4621 -0.0574 0.161 Uiso 0.50 1 calc PR . . C59 C 0.069(2) 0.3940(10) -0.1110(16) 0.126(3) Uani 0.50 1 d PDU . . H59A H -0.0036 0.3826 -0.1221 0.189 Uiso 0.50 1 calc PR . . H59B H 0.1169 0.3649 -0.0941 0.189 Uiso 0.50 1 calc PR . . H59C H 0.0729 0.4094 -0.1633 0.189 Uiso 0.50 1 calc PR . . 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 0.0213(2) 0.0217(2) 0.01780(19) 0.00084(15) 0.00818(14) 0.00196(15) O1 0.037(2) 0.0279(19) 0.0238(18) 0.0055(15) 0.0144(16) 0.0079(16) O2 0.038(2) 0.0263(19) 0.032(2) 0.0041(16) 0.0198(17) 0.0082(16) C1 0.021(2) 0.019(2) 0.019(2) -0.0005(19) 0.0080(19) 0.0033(19) N2 0.023(2) 0.029(2) 0.019(2) 0.0069(17) 0.0109(17) 0.0046(18) C3 0.029(3) 0.042(3) 0.020(3) 0.010(2) 0.010(2) 0.000(2) C4 0.029(3) 0.035(3) 0.022(3) 0.010(2) 0.011(2) 0.001(2) N5 0.023(2) 0.032(2) 0.017(2) 0.0040(18) 0.0062(17) 0.0019(18) C6 0.0249(12) 0.0265(13) 0.0243(13) 0.0013(9) 0.0098(9) 0.0001(9) C7 0.027(3) 0.034(3) 0.021(3) 0.009(2) 0.009(2) 0.004(2) C8 0.025(3) 0.040(3) 0.031(3) 0.005(2) 0.006(2) -0.003(2) C9 0.020(3) 0.049(4) 0.045(3) 0.006(3) 0.014(2) 0.003(3) C10 0.029(3) 0.046(3) 0.033(3) 0.005(3) 0.016(2) 0.010(3) C11 0.025(3) 0.037(3) 0.021(3) 0.004(2) 0.007(2) 0.006(2) C12 0.028(3) 0.034(3) 0.028(3) -0.001(2) 0.007(2) 0.005(2) C13 0.036(3) 0.037(3) 0.046(4) 0.002(3) 0.006(3) -0.002(3) C14 0.054(4) 0.049(4) 0.035(3) -0.001(3) 0.014(3) 0.008(3) C15 0.034(3) 0.039(3) 0.028(3) -0.001(2) 0.012(2) 0.005(3) C16 0.044(3) 0.039(3) 0.037(3) 0.006(3) 0.014(3) 0.006(3) C17 0.049(4) 0.044(3) 0.031(3) 0.003(3) 0.015(3) 0.016(3) C18 0.023(3) 0.027(3) 0.022(3) 0.004(2) 0.008(2) -0.002(2) C19 0.031(3) 0.025(3) 0.023(3) 0.001(2) 0.008(2) 0.001(2) C20 0.032(3) 0.036(3) 0.026(3) -0.004(2) 0.006(2) -0.008(2) C21 0.028(3) 0.044(3) 0.032(3) 0.002(3) 0.004(2) -0.008(3) C22 0.029(3) 0.041(3) 0.035(3) 0.003(3) 0.012(2) -0.001(2) C23 0.029(3) 0.031(3) 0.023(3) 0.003(2) 0.011(2) 0.000(2) C24 0.035(3) 0.025(3) 0.030(3) -0.001(2) 0.010(2) 0.003(2) C25 0.050(4) 0.031(3) 0.059(4) 0.000(3) 0.021(3) 0.006(3) C26 0.034(3) 0.047(4) 0.033(3) -0.010(3) 0.012(3) 0.000(3) C27 0.026(3) 0.038(3) 0.028(3) 0.001(2) 0.015(2) 0.001(2) C28 0.032(3) 0.043(3) 0.036(3) 0.007(3) 0.020(2) 0.002(3) C29 0.030(3) 0.042(3) 0.039(3) 0.003(3) 0.018(3) 0.003(3) P1 0.0233(6) 0.0211(6) 0.0208(6) 0.0001(5) 0.0090(5) 0.0016(5) C30 0.031(3) 0.022(3) 0.028(3) 0.002(2) 0.016(2) 0.003(2) C31 0.035(3) 0.028(3) 0.024(3) 0.001(2) 0.011(2) -0.005(2) C32 0.056(4) 0.035(3) 0.026(3) 0.005(2) 0.016(3) 0.000(3) C33 0.060(4) 0.050(4) 0.036(3) 0.002(3) 0.029(3) -0.015(3) C34 0.050(4) 0.040(3) 0.043(4) 0.000(3) 0.025(3) -0.016(3) C35 0.032(3) 0.028(3) 0.033(3) 0.001(2) 0.016(2) -0.002(2) C36 0.022(3) 0.034(3) 0.027(3) 0.001(2) 0.009(2) 0.002(2) C37 0.030(3) 0.030(3) 0.027(3) 0.002(2) 0.007(2) 0.004(2) C38 0.028(3) 0.037(3) 0.040(3) -0.003(3) 0.007(2) -0.001(3) C39 0.024(3) 0.057(4) 0.046(4) 0.003(3) 0.001(3) 0.005(3) C40 0.033(3) 0.050(4) 0.049(4) -0.005(3) 0.010(3) 0.011(3) C41 0.029(3) 0.032(3) 0.044(3) -0.004(3) 0.008(3) 0.009(2) C42 0.028(3) 0.026(3) 0.023(3) -0.001(2) 0.009(2) -0.002(2) C43 0.039(3) 0.021(3) 0.026(3) 0.000(2) 0.012(2) 0.001(2) C44 0.045(3) 0.020(3) 0.037(3) -0.006(2) 0.016(3) 0.003(2) C45 0.064(4) 0.036(3) 0.035(3) -0.013(3) 0.025(3) -0.004(3) C46 0.055(4) 0.036(3) 0.030(3) -0.004(2) 0.022(3) -0.002(3) C47 0.041(3) 0.029(3) 0.024(3) -0.004(2) 0.013(2) -0.004(2) C48 0.042(4) 0.060(4) 0.046(4) -0.008(3) 0.017(3) 0.006(3) Cl1 0.0361(9) 0.0912(15) 0.0786(14) 0.0121(12) 0.0173(9) -0.0045(10) Cl2 0.0718(14) 0.0613(13) 0.135(2) -0.0022(13) 0.0481(14) 0.0156(11) C49 0.110(2) 0.109(2) 0.110(2) -0.0001(10) 0.0393(11) 0.0005(10) C50 0.172(3) 0.172(3) 0.171(3) -0.0002(10) 0.0622(12) 0.0001(10) C51 0.153(2) 0.153(2) 0.153(3) -0.0001(10) 0.0552(12) -0.0001(10) C52 0.169(2) 0.169(3) 0.169(3) -0.0002(10) 0.0609(12) 0.0001(10) C53 0.267(3) 0.267(3) 0.266(3) -0.0003(10) 0.0962(12) 0.0000(10) C54 0.176(3) 0.177(3) 0.177(3) -0.0002(10) 0.0636(12) 0.0000(10) C55 0.067(2) 0.067(2) 0.067(2) 0.0004(10) 0.0242(11) 0.0002(10) C56 0.20(2) 0.021(7) 0.059(10) 0.021(7) 0.027(12) 0.057(10) C57 0.123(3) 0.123(3) 0.123(3) 0.0002(10) 0.0445(12) 0.0001(10) C58 0.134(3) 0.134(3) 0.134(3) 0.0003(10) 0.0485(12) -0.0001(10) C59 0.126(3) 0.126(3) 0.126(3) 0.0004(10) 0.0454(12) -0.0005(10) _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 O1 2.004(4) . ? Pd1 O2 2.015(4) . ? Pd1 C1 2.024(5) . ? Pd1 P1 2.3121(16) . ? O1 O2 1.448(5) . ? C1 N2 1.353(6) . ? C1 N5 1.365(6) . ? N2 C6 1.450(6) . ? N2 C3 1.481(6) . ? C3 C4 1.518(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.483(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N5 C18 1.438(6) . ? C6 C7 1.403(7) . ? C6 C11 1.406(7) . ? C7 C8 1.395(8) . ? C7 C12 1.514(8) . ? C8 C9 1.385(8) . ? C8 H8A 0.9500 . ? C9 C10 1.369(9) . ? C9 H9A 0.9500 . ? C10 C11 1.395(8) . ? C10 H10A 0.9500 . ? C11 C15 1.515(8) . ? C12 C14 1.529(8) . ? C12 C13 1.529(8) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.548(8) . ? C15 C17 1.551(8) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.415(7) . ? C18 C19 1.425(7) . ? C19 C20 1.397(8) . ? C19 C24 1.508(8) . ? C20 C21 1.382(9) . ? C20 H20A 0.9500 . ? C21 C22 1.382(8) . ? C21 H21A 0.9500 . ? C22 C23 1.398(8) . ? C22 H22A 0.9500 . ? C23 C27 1.521(7) . ? C24 C26 1.528(8) . ? C24 C25 1.546(8) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.534(8) . ? C27 C28 1.546(8) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 C30 1.859(5) . ? P1 C36 1.859(5) . ? P1 C42 1.882(5) . ? C30 C35 1.542(7) . ? C30 C31 1.544(7) . ? C30 H30A 1.0000 . ? C31 C32 1.532(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.529(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.518(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.529(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C41 1.530(7) . ? C36 C37 1.538(7) . ? C36 H36A 1.0000 . ? C37 C38 1.528(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.517(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.517(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.522(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C47 1.544(7) . ? C42 C43 1.546(7) . ? C42 H42A 1.0000 . ? C43 C44 1.528(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.520(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.548(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.538(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 Cl2 1.747(7) . ? C48 Cl1 1.782(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C49 H49A 0.9500 . ? C50 C51 1.3900 . ? C50 H50A 0.9500 . ? C51 C52 1.3900 . ? C51 H51A 0.9500 . ? C52 C53 1.3900 . ? C52 H52A 0.9500 . ? C53 C54 1.3900 . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C55 C56 1.539(16) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.602(17) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.567(17) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.473(17) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 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 O1 Pd1 O2 42.23(14) . . ? O1 Pd1 C1 150.01(17) . . ? O2 Pd1 C1 107.78(17) . . ? O1 Pd1 P1 104.16(11) . . ? O2 Pd1 P1 146.28(11) . . ? C1 Pd1 P1 105.80(14) . . ? O2 O1 Pd1 69.3(2) . . ? O1 O2 Pd1 68.5(2) . . ? N2 C1 N5 107.1(4) . . ? N2 C1 Pd1 123.1(3) . . ? N5 C1 Pd1 129.6(3) . . ? C1 N2 C6 127.9(4) . . ? C1 N2 C3 113.2(4) . . ? C6 N2 C3 117.8(4) . . ? N2 C3 C4 101.8(4) . . ? N2 C3 H3A 111.4 . . ? C4 C3 H3A 111.4 . . ? N2 C3 H3B 111.4 . . ? C4 C3 H3B 111.4 . . ? H3A C3 H3B 109.3 . . ? N5 C4 C3 102.5(4) . . ? N5 C4 H4A 111.3 . . ? C3 C4 H4A 111.3 . . ? N5 C4 H4B 111.3 . . ? C3 C4 H4B 111.3 . . ? H4A C4 H4B 109.2 . . ? C1 N5 C18 125.5(4) . . ? C1 N5 C4 112.1(4) . . ? C18 N5 C4 118.1(4) . . ? C7 C6 C11 121.9(5) . . ? C7 C6 N2 119.5(5) . . ? C11 C6 N2 118.2(5) . . ? C8 C7 C6 117.6(5) . . ? C8 C7 C12 119.7(5) . . ? C6 C7 C12 122.6(5) . . ? C9 C8 C7 121.0(5) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C10 C9 C8 120.6(5) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C11 121.0(5) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? C10 C11 C6 117.9(5) . . ? C10 C11 C15 119.2(5) . . ? C6 C11 C15 122.8(5) . . ? C7 C12 C14 109.5(5) . . ? C7 C12 C13 112.3(5) . . ? C14 C12 C13 110.8(5) . . ? C7 C12 H12A 108.0 . . ? C14 C12 H12A 108.0 . . ? C13 C12 H12A 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 111.4(5) . . ? C11 C15 C17 110.6(5) . . ? C16 C15 C17 110.1(5) . . ? C11 C15 H15A 108.2 . . ? C16 C15 H15A 108.2 . . ? C17 C15 H15A 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.5(5) . . ? C23 C18 N5 118.6(5) . . ? C19 C18 N5 120.4(5) . . ? C20 C19 C18 117.6(5) . . ? C20 C19 C24 118.4(5) . . ? C18 C19 C24 123.8(5) . . ? C21 C20 C19 122.2(5) . . ? C21 C20 H20A 118.9 . . ? C19 C20 H20A 118.9 . . ? C20 C21 C22 119.5(5) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 121.5(5) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C22 C23 C18 118.5(5) . . ? C22 C23 C27 118.1(5) . . ? C18 C23 C27 123.1(5) . . ? C19 C24 C26 113.2(5) . . ? C19 C24 C25 109.3(5) . . ? C26 C24 C25 110.5(5) . . ? C19 C24 H24A 107.9 . . ? C26 C24 H24A 107.9 . . ? C25 C24 H24A 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 114.0(5) . . ? C23 C27 C28 108.4(5) . . ? C29 C27 C28 109.2(4) . . ? C23 C27 H27A 108.4 . . ? C29 C27 H27A 108.4 . . ? C28 C27 H27A 108.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C30 P1 C36 106.4(2) . . ? C30 P1 C42 103.0(2) . . ? C36 P1 C42 105.6(2) . . ? C30 P1 Pd1 107.40(17) . . ? C36 P1 Pd1 117.51(18) . . ? C42 P1 Pd1 115.64(17) . . ? C35 C30 C31 109.9(4) . . ? C35 C30 P1 109.0(3) . . ? C31 C30 P1 113.2(4) . . ? C35 C30 H30A 108.2 . . ? C31 C30 H30A 108.2 . . ? P1 C30 H30A 108.2 . . ? C32 C31 C30 112.0(4) . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C33 C32 C31 111.7(5) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 109.9(5) . . ? C34 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? C34 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C33 C34 C35 110.9(5) . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C30 111.9(5) . . ? C34 C35 H35A 109.2 . . ? C30 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? C30 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C41 C36 C37 110.5(4) . . ? C41 C36 P1 115.2(4) . . ? C37 C36 P1 113.2(4) . . ? C41 C36 H36A 105.7 . . ? C37 C36 H36A 105.7 . . ? P1 C36 H36A 105.7 . . ? C38 C37 C36 111.1(5) . . ? C38 C37 H37A 109.4 . . ? C36 C37 H37A 109.4 . . ? C38 C37 H37B 109.4 . . ? C36 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C39 C38 C37 111.8(5) . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38B 109.2 . . ? C37 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C38 109.9(5) . . ? C40 C39 H39A 109.7 . . ? C38 C39 H39A 109.7 . . ? C40 C39 H39B 109.7 . . ? C38 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C39 C40 C41 111.0(5) . . ? C39 C40 H40A 109.4 . . ? C41 C40 H40A 109.4 . . ? C39 C40 H40B 109.4 . . ? C41 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C40 C41 C36 112.5(5) . . ? C40 C41 H41A 109.1 . . ? C36 C41 H41A 109.1 . . ? C40 C41 H41B 109.1 . . ? C36 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C47 C42 C43 110.5(4) . . ? C47 C42 P1 111.4(4) . . ? C43 C42 P1 117.5(4) . . ? C47 C42 H42A 105.5 . . ? C43 C42 H42A 105.5 . . ? P1 C42 H42A 105.5 . . ? C44 C43 C42 111.3(4) . . ? C44 C43 H43A 109.4 . . ? C42 C43 H43A 109.4 . . ? C44 C43 H43B 109.4 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C45 C44 C43 111.1(5) . . ? 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 110.6(5) . . ? C44 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C47 C46 C45 110.9(5) . . ? C47 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C46 C47 C42 110.9(5) . . ? C46 C47 H47A 109.5 . . ? C42 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 108.0 . . ? Cl2 C48 Cl1 111.0(4) . . ? Cl2 C48 H48A 109.4 . . ? Cl1 C48 H48A 109.4 . . ? Cl2 C48 H48B 109.4 . . ? Cl1 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C50 C49 C54 120.0 . . ? C50 C49 H49A 120.0 . . ? C54 C49 H49A 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 H50A 120.0 . . ? C51 C50 H50A 120.0 . . ? C52 C51 C50 120.0 . . ? C52 C51 H51A 120.0 . . ? C50 C51 H51A 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 H54A 120.0 . . ? C49 C54 H54A 120.0 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C55 C56 C57 129.7(16) . . ? C55 C56 H56A 104.9 . . ? C57 C56 H56A 104.9 . . ? C55 C56 H56B 104.9 . . ? C57 C56 H56B 104.9 . . ? H56A C56 H56B 105.8 . . ? C58 C57 C56 125.2(19) . . ? C58 C57 H57A 106.0 . . ? C56 C57 H57A 106.0 . . ? C58 C57 H57B 106.0 . . ? C56 C57 H57B 106.0 . . ? H57A C57 H57B 106.3 . . ? C59 C58 C57 103.5(19) . . ? C59 C58 H58A 111.1 . . ? C57 C58 H58A 111.1 . . ? C59 C58 H58B 111.1 . . ? C57 C58 H58B 111.1 . . ? H58A C58 H58B 109.0 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 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 C1 Pd1 O1 O2 0.5(4) . . . . ? P1 Pd1 O1 O2 -176.69(19) . . . . ? C1 Pd1 O2 O1 -179.7(2) . . . . ? P1 Pd1 O2 O1 5.8(3) . . . . ? O1 Pd1 C1 N2 -63.2(6) . . . . ? O2 Pd1 C1 N2 -62.8(4) . . . . ? P1 Pd1 C1 N2 114.0(4) . . . . ? O1 Pd1 C1 N5 110.9(5) . . . . ? O2 Pd1 C1 N5 111.3(4) . . . . ? P1 Pd1 C1 N5 -71.9(4) . . . . ? N5 C1 N2 C6 -162.3(5) . . . . ? Pd1 C1 N2 C6 13.0(7) . . . . ? N5 C1 N2 C3 5.4(6) . . . . ? Pd1 C1 N2 C3 -179.4(4) . . . . ? C1 N2 C3 C4 -14.9(6) . . . . ? C6 N2 C3 C4 154.1(4) . . . . ? N2 C3 C4 N5 17.2(5) . . . . ? N2 C1 N5 C18 163.4(5) . . . . ? Pd1 C1 N5 C18 -11.4(7) . . . . ? N2 C1 N5 C4 7.3(6) . . . . ? Pd1 C1 N5 C4 -167.6(4) . . . . ? C3 C4 N5 C1 -16.1(6) . . . . ? C3 C4 N5 C18 -174.2(4) . . . . ? C1 N2 C6 C7 -97.9(6) . . . . ? C3 N2 C6 C7 95.0(6) . . . . ? C1 N2 C6 C11 88.9(6) . . . . ? C3 N2 C6 C11 -78.3(6) . . . . ? C11 C6 C7 C8 -1.2(8) . . . . ? N2 C6 C7 C8 -174.2(5) . . . . ? C11 C6 C7 C12 174.9(5) . . . . ? N2 C6 C7 C12 1.8(7) . . . . ? C6 C7 C8 C9 0.9(8) . . . . ? C12 C7 C8 C9 -175.3(5) . . . . ? C7 C8 C9 C10 -0.4(9) . . . . ? C8 C9 C10 C11 0.0(9) . . . . ? C9 C10 C11 C6 -0.3(8) . . . . ? C9 C10 C11 C15 176.9(5) . . . . ? C7 C6 C11 C10 0.9(8) . . . . ? N2 C6 C11 C10 174.0(5) . . . . ? C7 C6 C11 C15 -176.2(5) . . . . ? N2 C6 C11 C15 -3.1(7) . . . . ? C8 C7 C12 C14 78.1(6) . . . . ? C6 C7 C12 C14 -97.9(6) . . . . ? C8 C7 C12 C13 -45.5(7) . . . . ? C6 C7 C12 C13 138.5(5) . . . . ? C10 C11 C15 C16 -61.8(7) . . . . ? C6 C11 C15 C16 115.3(6) . . . . ? C10 C11 C15 C17 60.9(6) . . . . ? C6 C11 C15 C17 -122.0(6) . . . . ? C1 N5 C18 C23 129.2(5) . . . . ? C4 N5 C18 C23 -76.0(6) . . . . ? C1 N5 C18 C19 -58.5(7) . . . . ? C4 N5 C18 C19 96.3(6) . . . . ? C23 C18 C19 C20 -4.1(7) . . . . ? N5 C18 C19 C20 -176.3(5) . . . . ? C23 C18 C19 C24 170.8(5) . . . . ? N5 C18 C19 C24 -1.4(8) . . . . ? C18 C19 C20 C21 1.8(8) . . . . ? C24 C19 C20 C21 -173.4(5) . . . . ? C19 C20 C21 C22 1.7(9) . . . . ? C20 C21 C22 C23 -2.9(9) . . . . ? C21 C22 C23 C18 0.5(8) . . . . ? C21 C22 C23 C27 175.7(5) . . . . ? C19 C18 C23 C22 3.0(8) . . . . ? N5 C18 C23 C22 175.4(5) . . . . ? C19 C18 C23 C27 -171.9(5) . . . . ? N5 C18 C23 C27 0.5(8) . . . . ? C20 C19 C24 C26 -50.6(7) . . . . ? C18 C19 C24 C26 134.6(5) . . . . ? C20 C19 C24 C25 73.0(6) . . . . ? C18 C19 C24 C25 -101.8(6) . . . . ? C22 C23 C27 C29 52.0(7) . . . . ? C18 C23 C27 C29 -133.1(5) . . . . ? C22 C23 C27 C28 -69.8(6) . . . . ? C18 C23 C27 C28 105.1(6) . . . . ? O1 Pd1 P1 C30 13.5(2) . . . . ? O2 Pd1 P1 C30 9.5(3) . . . . ? C1 Pd1 P1 C30 -165.0(2) . . . . ? O1 Pd1 P1 C36 -106.3(2) . . . . ? O2 Pd1 P1 C36 -110.3(3) . . . . ? C1 Pd1 P1 C36 75.2(2) . . . . ? O1 Pd1 P1 C42 127.9(2) . . . . ? O2 Pd1 P1 C42 123.9(3) . . . . ? C1 Pd1 P1 C42 -50.7(2) . . . . ? C36 P1 C30 C35 -176.7(4) . . . . ? C42 P1 C30 C35 -65.9(4) . . . . ? Pd1 P1 C30 C35 56.6(4) . . . . ? C36 P1 C30 C31 60.6(4) . . . . ? C42 P1 C30 C31 171.4(4) . . . . ? Pd1 P1 C30 C31 -66.0(4) . . . . ? C35 C30 C31 C32 52.9(6) . . . . ? P1 C30 C31 C32 175.1(4) . . . . ? C30 C31 C32 C33 -55.1(7) . . . . ? C31 C32 C33 C34 56.9(7) . . . . ? C32 C33 C34 C35 -58.0(7) . . . . ? C33 C34 C35 C30 57.9(7) . . . . ? C31 C30 C35 C34 -54.4(6) . . . . ? P1 C30 C35 C34 -179.0(4) . . . . ? C30 P1 C36 C41 43.4(5) . . . . ? C42 P1 C36 C41 -65.6(5) . . . . ? Pd1 P1 C36 C41 163.8(3) . . . . ? C30 P1 C36 C37 -85.0(4) . . . . ? C42 P1 C36 C37 165.9(4) . . . . ? Pd1 P1 C36 C37 35.3(4) . . . . ? C41 C36 C37 C38 53.0(6) . . . . ? P1 C36 C37 C38 -176.1(4) . . . . ? C36 C37 C38 C39 -56.3(7) . . . . ? C37 C38 C39 C40 57.9(7) . . . . ? C38 C39 C40 C41 -57.1(7) . . . . ? C39 C40 C41 C36 56.1(7) . . . . ? C37 C36 C41 C40 -53.5(7) . . . . ? P1 C36 C41 C40 176.7(4) . . . . ? C30 P1 C42 C47 -161.5(4) . . . . ? C36 P1 C42 C47 -50.1(4) . . . . ? Pd1 P1 C42 C47 81.6(4) . . . . ? C30 P1 C42 C43 -32.7(5) . . . . ? C36 P1 C42 C43 78.8(4) . . . . ? Pd1 P1 C42 C43 -149.5(3) . . . . ? C47 C42 C43 C44 -55.6(6) . . . . ? P1 C42 C43 C44 175.1(4) . . . . ? C42 C43 C44 C45 57.0(6) . . . . ? C43 C44 C45 C46 -57.2(7) . . . . ? C44 C45 C46 C47 56.9(7) . . . . ? C45 C46 C47 C42 -56.1(7) . . . . ? C43 C42 C47 C46 55.3(6) . . . . ? P1 C42 C47 C46 -172.2(4) . . . . ? C54 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C52 0.0 . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C49 0.0 . . . . ? C50 C49 C54 C53 0.0 . . . . ? C55 C56 C57 C58 177(2) . . . . ? C56 C57 C58 C59 -172(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.002 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.128 # Attachment '- 2d.cif' data_2d _database_code_depnum_ccdc_archive 'CCDC 799173' #TrackingRef '- 2d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety 'C45 H53 N2 O2 P Pd,C H2 Cl2' _chemical_formula_sum 'C46 H55 Cl2 N2 O2 P Pd' _chemical_formula_weight 876.19 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.800(10) _cell_length_b 16.619(11) _cell_length_c 11.950(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.790(14) _cell_angle_gamma 90.00 _cell_volume 2161(3) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 6934 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.0 _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22385 _diffrn_reflns_av_R_equivalents 0.1032 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.39 _reflns_number_total 7292 _reflns_number_gt 6595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0622P)^2^+4.3244P] 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(4) _refine_ls_number_reflns 7292 _refine_ls_number_parameters 488 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.005 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 0.05093(4) 0.75516(4) 0.06024(4) 0.02665(15) Uani 1 1 d . . . O1 O 0.0296(5) 0.8088(5) 0.2011(6) 0.064(2) Uani 1 1 d . . . O2 O 0.0905(6) 0.8689(4) 0.1331(6) 0.069(2) Uani 1 1 d . . . C1 C -0.0182(7) 0.6425(4) 0.0444(7) 0.0285(17) Uani 1 1 d . . . N2 N 0.0400(5) 0.5816(4) 0.1194(6) 0.0265(13) Uani 1 1 d . . . C3 C -0.0300(7) 0.5038(5) 0.0791(7) 0.0294(17) Uani 1 1 d . . . H3A H 0.0098 0.4683 0.0386 0.035 Uiso 1 1 calc R . . H3B H -0.0371 0.4748 0.1484 0.035 Uiso 1 1 calc R . . C4 C -0.1531(7) 0.5321(5) -0.0082(7) 0.0317(17) Uani 1 1 d . . . H4A H -0.2144 0.5314 0.0295 0.038 Uiso 1 1 calc R . . H4B H -0.1832 0.4985 -0.0824 0.038 Uiso 1 1 calc R . . N5 N -0.1273(5) 0.6164(4) -0.0364(6) 0.0274(14) Uani 1 1 d . . . C6 C 0.1378(6) 0.5861(4) 0.2344(7) 0.0257(16) Uani 1 1 d . . . C7 C 0.2622(6) 0.5774(5) 0.2491(7) 0.0296(17) Uani 1 1 d . . . C8 C 0.3519(7) 0.5774(5) 0.3651(8) 0.0363(19) Uani 1 1 d . . . H8A H 0.4356 0.5727 0.3756 0.044 Uiso 1 1 calc R . . C9 C 0.3232(7) 0.5840(5) 0.4663(7) 0.0352(19) Uani 1 1 d . . . H9A H 0.3865 0.5833 0.5453 0.042 Uiso 1 1 calc R . . C10 C 0.1995(7) 0.5918(5) 0.4513(7) 0.0347(18) Uani 1 1 d . . . H10A H 0.1798 0.5978 0.5207 0.042 Uiso 1 1 calc R . . C11 C 0.1046(7) 0.5908(5) 0.3352(7) 0.0307(17) Uani 1 1 d . . . C12 C 0.2932(7) 0.5652(5) 0.1395(7) 0.0325(18) Uani 1 1 d . . . H12A H 0.2233 0.5869 0.0676 0.039 Uiso 1 1 calc R . . C13 C 0.3060(8) 0.4769(6) 0.1167(8) 0.043(2) Uani 1 1 d . . . H13A H 0.2308 0.4484 0.1096 0.064 Uiso 1 1 calc R . . H13B H 0.3761 0.4543 0.1844 0.064 Uiso 1 1 calc R . . H13C H 0.3196 0.4706 0.0412 0.064 Uiso 1 1 calc R . . C14 C 0.4087(8) 0.6103(5) 0.1484(8) 0.040(2) Uani 1 1 d . . . H14A H 0.3988 0.6677 0.1609 0.060 Uiso 1 1 calc R . . H14B H 0.4221 0.6028 0.0731 0.060 Uiso 1 1 calc R . . H14C H 0.4795 0.5892 0.2169 0.060 Uiso 1 1 calc R . . C15 C -0.0240(7) 0.5995(5) 0.3268(7) 0.0316(18) Uani 1 1 d . . . H15A H -0.0790 0.6021 0.2388 0.038 Uiso 1 1 calc R . . C16 C -0.0440(8) 0.6773(6) 0.3875(9) 0.046(2) Uani 1 1 d . . . H16A H -0.0212 0.7240 0.3506 0.070 Uiso 1 1 calc R . . H16B H 0.0074 0.6758 0.4745 0.070 Uiso 1 1 calc R . . H16C H -0.1306 0.6814 0.3760 0.070 Uiso 1 1 calc R . . C17 C -0.0620(8) 0.5247(5) 0.3818(8) 0.043(2) Uani 1 1 d . . . H17A H -0.0511 0.4760 0.3407 0.064 Uiso 1 1 calc R . . H17B H -0.1485 0.5296 0.3708 0.064 Uiso 1 1 calc R . . H17C H -0.0105 0.5212 0.4686 0.064 Uiso 1 1 calc R . . C18 C -0.2288(6) 0.6655(4) -0.1134(7) 0.0266(16) Uani 1 1 d . . . C19 C -0.2771(7) 0.6490(5) -0.2386(7) 0.0310(17) Uani 1 1 d . . . C20 C -0.3753(7) 0.6958(5) -0.3100(8) 0.039(2) Uani 1 1 d . . . H20A H -0.4072 0.6880 -0.3954 0.047 Uiso 1 1 calc R . . C21 C -0.4306(6) 0.7545(7) -0.2628(7) 0.0415(17) Uani 1 1 d . . . H21A H -0.4973 0.7861 -0.3147 0.050 Uiso 1 1 calc R . . C22 C -0.3847(6) 0.7644(6) -0.1395(7) 0.0337(18) Uani 1 1 d . . . H22A H -0.4226 0.8026 -0.1060 0.040 Uiso 1 1 calc R . . C23 C -0.2846(7) 0.7208(5) -0.0614(7) 0.0312(17) Uani 1 1 d . . . C24 C -0.2288(7) 0.5847(5) -0.2963(7) 0.0342(18) Uani 1 1 d . . . H24A H -0.1521 0.5623 -0.2330 0.041 Uiso 1 1 calc R . . C25 C -0.3237(8) 0.5155(5) -0.3432(8) 0.042(2) Uani 1 1 d . . . H25A H -0.3431 0.4944 -0.2761 0.063 Uiso 1 1 calc R . . H25B H -0.2892 0.4723 -0.3762 0.063 Uiso 1 1 calc R . . H25C H -0.3989 0.5360 -0.4071 0.063 Uiso 1 1 calc R . . C26 C -0.1978(8) 0.6163(6) -0.3996(8) 0.046(2) Uani 1 1 d . . . H26A H -0.1380 0.6602 -0.3702 0.069 Uiso 1 1 calc R . . H26B H -0.2726 0.6364 -0.4644 0.069 Uiso 1 1 calc R . . H26C H -0.1625 0.5728 -0.4314 0.069 Uiso 1 1 calc R . . C27 C -0.2515(7) 0.7292(4) 0.0746(8) 0.032(2) Uani 1 1 d . . . H27A H -0.1673 0.7063 0.1175 0.039 Uiso 1 1 calc R . . C28 C -0.3398(7) 0.6794(6) 0.1087(8) 0.041(2) Uani 1 1 d . . . H28A H -0.3191 0.6839 0.1962 0.061 Uiso 1 1 calc R . . H28B H -0.3341 0.6229 0.0877 0.061 Uiso 1 1 calc R . . H28C H -0.4238 0.6988 0.0645 0.061 Uiso 1 1 calc R . . C29 C -0.2493(7) 0.8165(5) 0.1173(8) 0.038(2) Uani 1 1 d . . . H29A H -0.2271 0.8173 0.2052 0.057 Uiso 1 1 calc R . . H29B H -0.3309 0.8405 0.0763 0.057 Uiso 1 1 calc R . . H29C H -0.1887 0.8473 0.0975 0.057 Uiso 1 1 calc R . . P1 P 0.11496(14) 0.76017(17) -0.09686(15) 0.0268(4) Uani 1 1 d . . . C30 C -0.0036(7) 0.7985(4) -0.2372(7) 0.0309(17) Uani 1 1 d . . . C31 C -0.1098(7) 0.8308(4) -0.2312(7) 0.0324(18) Uani 1 1 d . . . H31A H -0.1207 0.8308 -0.1565 0.039 Uiso 1 1 calc R . . C32 C -0.2009(8) 0.8633(6) -0.3360(8) 0.039(2) Uani 1 1 d . . . H32A H -0.2737 0.8852 -0.3321 0.047 Uiso 1 1 calc R . . C33 C -0.1851(8) 0.8634(5) -0.4437(8) 0.0363(19) Uani 1 1 d . . . H33A H -0.2464 0.8864 -0.5139 0.044 Uiso 1 1 calc R . . C34 C -0.0796(8) 0.8299(5) -0.4509(7) 0.0371(19) Uani 1 1 d . . . H34A H -0.0694 0.8294 -0.5259 0.044 Uiso 1 1 calc R . . C35 C 0.0101(7) 0.7975(5) -0.3476(7) 0.0304(17) Uani 1 1 d . . . H35A H 0.0817 0.7744 -0.3524 0.036 Uiso 1 1 calc R . . C36 C 0.2419(7) 0.8327(5) -0.0591(7) 0.0316(18) Uani 1 1 d . . . C37 C 0.3219(7) 0.8394(5) 0.0620(7) 0.0317(18) Uani 1 1 d . . . H37A H 0.3074 0.8085 0.1221 0.038 Uiso 1 1 calc R . . C38 C 0.4222(7) 0.8903(5) 0.0960(8) 0.037(2) Uani 1 1 d . . . H38A H 0.4773 0.8932 0.1786 0.045 Uiso 1 1 calc R . . C39 C 0.4422(7) 0.9363(5) 0.0110(7) 0.0342(19) Uani 1 1 d . . . H39A H 0.5102 0.9720 0.0341 0.041 Uiso 1 1 calc R . . C40 C 0.3638(8) 0.9305(6) -0.1072(8) 0.041(2) Uani 1 1 d . . . H40A H 0.3779 0.9624 -0.1665 0.049 Uiso 1 1 calc R . . C41 C 0.2649(7) 0.8798(5) -0.1424(8) 0.0368(19) Uani 1 1 d . . . H41A H 0.2114 0.8771 -0.2255 0.044 Uiso 1 1 calc R . . C42 C 0.1725(7) 0.6719(5) -0.1514(7) 0.0308(17) Uani 1 1 d . . . C43 C 0.2881(8) 0.6751(6) -0.1682(7) 0.041(2) Uani 1 1 d . . . H43A H 0.3354 0.7230 -0.1537 0.049 Uiso 1 1 calc R . . C44 C 0.3255(8) 0.6063(6) -0.2056(8) 0.045(2) Uani 1 1 d . . . H44A H 0.4013 0.6066 -0.2160 0.055 Uiso 1 1 calc R . . C45 C 0.2578(9) 0.5365(7) -0.2289(8) 0.051(3) Uani 1 1 d . . . H45A H 0.2866 0.4898 -0.2557 0.061 Uiso 1 1 calc R . . C46 C 0.1460(8) 0.5343(6) -0.2132(8) 0.045(2) Uani 1 1 d . . . H46A H 0.0979 0.4866 -0.2298 0.054 Uiso 1 1 calc R . . C47 C 0.1078(8) 0.6023(5) -0.1733(7) 0.0358(19) Uani 1 1 d . . . H47A H 0.0333 0.6006 -0.1605 0.043 Uiso 1 1 calc R . . C48 C 0.2896(9) 0.7973(7) 0.3846(9) 0.058(3) Uani 1 1 d . . . H48A H 0.2640 0.7405 0.3658 0.070 Uiso 1 1 calc R . . H48B H 0.2406 0.8302 0.3131 0.070 Uiso 1 1 calc R . . Cl1 Cl 0.2573(3) 0.8287(2) 0.5112(3) 0.0691(8) Uani 1 1 d . . . Cl2 Cl 0.4438(2) 0.80605(18) 0.4097(2) 0.0598(7) 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 0.0219(2) 0.0326(3) 0.0281(3) 0.0002(3) 0.01255(19) -0.0004(3) O1 0.019(3) 0.123(6) 0.055(4) -0.026(4) 0.019(3) -0.008(3) O2 0.050(4) 0.053(4) 0.064(5) 0.026(4) -0.023(3) -0.031(3) C1 0.029(4) 0.028(4) 0.037(5) 0.006(3) 0.021(4) 0.003(3) N2 0.020(3) 0.024(3) 0.036(4) 0.003(3) 0.011(3) -0.001(3) C3 0.024(4) 0.032(4) 0.030(4) 0.002(3) 0.008(3) -0.002(3) C4 0.029(4) 0.029(4) 0.036(4) 0.004(3) 0.011(4) -0.003(3) N5 0.017(3) 0.032(3) 0.033(4) -0.004(3) 0.010(3) -0.005(2) C6 0.026(4) 0.026(4) 0.033(4) 0.000(3) 0.019(3) 0.001(3) C7 0.015(3) 0.039(4) 0.032(4) -0.003(4) 0.006(3) 0.000(3) C8 0.023(4) 0.044(5) 0.043(5) -0.001(4) 0.013(4) 0.003(3) C9 0.027(4) 0.050(5) 0.023(4) -0.006(4) 0.003(3) 0.006(4) C10 0.030(4) 0.045(5) 0.030(4) 0.002(4) 0.013(4) 0.001(4) C11 0.028(4) 0.033(4) 0.032(4) 0.001(3) 0.013(3) 0.002(3) C12 0.019(4) 0.044(5) 0.033(5) -0.002(4) 0.008(3) -0.002(3) C13 0.038(5) 0.057(6) 0.045(5) -0.007(4) 0.030(4) -0.009(4) C14 0.037(5) 0.044(5) 0.038(5) 0.005(4) 0.015(4) -0.004(4) C15 0.034(4) 0.040(5) 0.025(4) -0.008(3) 0.016(3) 0.007(3) C16 0.038(5) 0.044(5) 0.067(6) -0.012(5) 0.032(5) 0.001(4) C17 0.035(5) 0.048(5) 0.048(6) 0.008(4) 0.019(4) -0.006(4) C18 0.021(3) 0.022(4) 0.038(5) 0.009(3) 0.013(3) -0.001(3) C19 0.025(4) 0.035(4) 0.035(5) 0.002(4) 0.014(3) -0.003(3) C20 0.026(4) 0.042(5) 0.037(5) 0.011(4) -0.001(4) 0.000(3) C21 0.031(4) 0.043(4) 0.045(4) 0.002(6) 0.009(3) 0.004(6) C22 0.022(3) 0.034(5) 0.042(4) 0.005(4) 0.009(3) 0.002(4) C23 0.024(4) 0.034(4) 0.038(5) 0.004(3) 0.015(4) -0.002(3) C24 0.030(4) 0.040(5) 0.029(4) 0.005(4) 0.007(3) -0.004(3) C25 0.034(5) 0.043(5) 0.043(5) 0.000(4) 0.009(4) -0.002(4) C26 0.034(5) 0.066(7) 0.040(6) 0.003(5) 0.017(4) -0.001(4) C27 0.021(4) 0.035(5) 0.045(5) 0.003(3) 0.018(4) 0.006(3) C28 0.028(4) 0.062(6) 0.037(5) 0.010(4) 0.017(4) 0.006(4) C29 0.027(4) 0.045(5) 0.045(5) 0.003(4) 0.017(4) 0.011(4) P1 0.0214(7) 0.0353(10) 0.0256(8) 0.0022(12) 0.0112(7) 0.0001(11) C30 0.034(4) 0.027(4) 0.031(4) 0.002(3) 0.013(4) 0.003(3) C31 0.042(5) 0.023(4) 0.031(4) 0.000(3) 0.014(4) -0.001(3) C32 0.028(4) 0.046(5) 0.044(5) -0.003(4) 0.014(4) 0.000(4) C33 0.038(5) 0.037(5) 0.031(5) 0.002(4) 0.011(4) 0.011(4) C34 0.046(5) 0.035(5) 0.029(4) 0.000(4) 0.013(4) 0.003(4) C35 0.031(4) 0.031(4) 0.032(4) 0.001(3) 0.015(3) 0.003(3) C36 0.028(4) 0.037(5) 0.038(5) -0.004(4) 0.023(4) 0.003(3) C37 0.025(4) 0.049(5) 0.026(4) 0.001(4) 0.014(3) 0.004(3) C38 0.024(4) 0.043(5) 0.042(5) -0.003(4) 0.008(4) 0.002(4) C39 0.017(3) 0.045(5) 0.044(5) -0.004(4) 0.015(4) 0.001(3) C40 0.033(4) 0.051(5) 0.046(5) 0.002(4) 0.022(4) -0.002(4) C41 0.029(4) 0.049(5) 0.034(5) 0.004(4) 0.014(4) -0.005(4) C42 0.035(4) 0.037(4) 0.023(4) 0.005(3) 0.015(4) 0.010(4) C43 0.045(5) 0.048(6) 0.033(5) 0.008(4) 0.019(4) 0.011(4) C44 0.044(5) 0.057(6) 0.045(5) 0.007(5) 0.027(4) 0.024(5) C45 0.064(6) 0.066(7) 0.027(5) 0.006(4) 0.021(5) 0.032(6) C46 0.036(5) 0.052(6) 0.036(5) -0.009(4) 0.001(4) 0.000(4) C47 0.033(4) 0.038(5) 0.033(5) -0.001(4) 0.010(4) 0.005(4) C48 0.045(5) 0.067(7) 0.055(6) -0.001(5) 0.012(5) 0.002(5) Cl1 0.0603(16) 0.088(2) 0.0573(17) 0.0107(15) 0.0210(14) -0.0012(15) Cl2 0.0595(16) 0.0683(18) 0.0479(14) 0.0136(12) 0.0167(12) 0.0075(13) _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 O1 2.006(6) . ? Pd1 C1 2.022(8) . ? Pd1 O2 2.058(7) . ? Pd1 P1 2.281(2) . ? O1 O2 1.621(9) . ? C1 N5 1.347(10) . ? C1 N2 1.350(9) . ? N2 C6 1.413(9) . ? N2 C3 1.508(9) . ? C3 C4 1.498(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.499(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N5 C18 1.448(9) . ? C6 C11 1.405(10) . ? C6 C7 1.417(9) . ? C7 C8 1.380(11) . ? C7 C12 1.504(10) . ? C8 C9 1.381(11) . ? C8 H8A 0.9500 . ? C9 C10 1.406(11) . ? C9 H9A 0.9500 . ? C10 C11 1.406(11) . ? C10 H10A 0.9500 . ? C11 C15 1.489(10) . ? C12 C13 1.512(12) . ? C12 C14 1.522(11) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.543(11) . ? C15 C17 1.552(11) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.408(10) . ? C18 C19 1.407(11) . ? C19 C20 1.383(11) . ? C19 C24 1.498(11) . ? C20 C21 1.407(13) . ? C20 H20A 0.9500 . ? C21 C22 1.369(10) . ? C21 H21A 0.9500 . ? C22 C23 1.392(11) . ? C22 H22A 0.9500 . ? C23 C27 1.523(11) . ? C24 C26 1.512(11) . ? C24 C25 1.552(11) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.507(10) . ? C27 C29 1.534(12) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 C30 1.833(8) . ? P1 C36 1.837(8) . ? P1 C42 1.840(8) . ? C30 C31 1.390(11) . ? C30 C35 1.390(11) . ? C31 C32 1.404(12) . ? C31 H31A 0.9500 . ? C32 C33 1.370(12) . ? C32 H32A 0.9500 . ? C33 C34 1.397(11) . ? C33 H33A 0.9500 . ? C34 C35 1.386(11) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C41 1.374(11) . ? C36 C37 1.393(11) . ? C37 C38 1.382(11) . ? C37 H37A 0.9500 . ? C38 C39 1.363(12) . ? C38 H38A 0.9500 . ? C39 C40 1.359(12) . ? C39 H39A 0.9500 . ? C40 C41 1.367(12) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C47 1.355(12) . ? C42 C43 1.454(11) . ? C43 C44 1.361(12) . ? C43 H43A 0.9500 . ? C44 C45 1.375(14) . ? C44 H44A 0.9500 . ? C45 C46 1.403(13) . ? C45 H45A 0.9500 . ? C46 C47 1.368(12) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 Cl2 1.733(10) . ? C48 Cl1 1.775(10) . ? C48 H48A 0.9900 . ? C48 H48B 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 O1 Pd1 C1 108.2(3) . . ? O1 Pd1 O2 47.0(3) . . ? C1 Pd1 O2 155.1(3) . . ? O1 Pd1 P1 149.8(2) . . ? C1 Pd1 P1 102.0(2) . . ? O2 Pd1 P1 102.8(2) . . ? O2 O1 Pd1 68.2(4) . . ? O1 O2 Pd1 64.8(3) . . ? N5 C1 N2 109.5(6) . . ? N5 C1 Pd1 127.2(5) . . ? N2 C1 Pd1 123.3(6) . . ? C1 N2 C6 128.3(6) . . ? C1 N2 C3 110.8(6) . . ? C6 N2 C3 119.8(6) . . ? C4 C3 N2 102.5(6) . . ? C4 C3 H3A 111.3 . . ? N2 C3 H3A 111.3 . . ? C4 C3 H3B 111.3 . . ? N2 C3 H3B 111.3 . . ? H3A C3 H3B 109.2 . . ? C3 C4 N5 102.9(6) . . ? C3 C4 H4A 111.2 . . ? N5 C4 H4A 111.2 . . ? C3 C4 H4B 111.2 . . ? N5 C4 H4B 111.2 . . ? H4A C4 H4B 109.1 . . ? C1 N5 C18 126.9(6) . . ? C1 N5 C4 111.1(6) . . ? C18 N5 C4 118.7(6) . . ? C11 C6 C7 121.2(7) . . ? C11 C6 N2 116.2(6) . . ? C7 C6 N2 122.2(6) . . ? C8 C7 C6 118.7(7) . . ? C8 C7 C12 121.6(7) . . ? C6 C7 C12 119.7(6) . . ? C9 C8 C7 121.8(7) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C8 C9 C10 119.3(7) . . ? C8 C9 H9A 120.3 . . ? C10 C9 H9A 120.3 . . ? C9 C10 C11 121.1(7) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? C6 C11 C10 117.8(7) . . ? C6 C11 C15 124.3(7) . . ? C10 C11 C15 117.8(7) . . ? C7 C12 C13 111.3(7) . . ? C7 C12 C14 112.7(7) . . ? C13 C12 C14 109.9(7) . . ? C7 C12 H12A 107.6 . . ? C13 C12 H12A 107.6 . . ? C14 C12 H12A 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 112.7(7) . . ? C11 C15 C17 110.4(7) . . ? C16 C15 C17 110.5(7) . . ? C11 C15 H15A 107.7 . . ? C16 C15 H15A 107.7 . . ? C17 C15 H15A 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 122.1(7) . . ? C23 C18 N5 120.1(7) . . ? C19 C18 N5 117.4(7) . . ? C20 C19 C18 116.4(7) . . ? C20 C19 C24 119.6(8) . . ? C18 C19 C24 124.0(7) . . ? C19 C20 C21 123.4(8) . . ? C19 C20 H20A 118.3 . . ? C21 C20 H20A 118.3 . . ? C22 C21 C20 117.6(8) . . ? C22 C21 H21A 121.2 . . ? C20 C21 H21A 121.2 . . ? C21 C22 C23 122.6(9) . . ? C21 C22 H22A 118.7 . . ? C23 C22 H22A 118.7 . . ? C22 C23 C18 117.6(7) . . ? C22 C23 C27 118.0(7) . . ? C18 C23 C27 124.0(7) . . ? C19 C24 C26 112.6(7) . . ? C19 C24 C25 110.1(7) . . ? C26 C24 C25 109.4(7) . . ? C19 C24 H24A 108.2 . . ? C26 C24 H24A 108.2 . . ? C25 C24 H24A 108.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C23 108.6(7) . . ? C28 C27 C29 110.7(7) . . ? C23 C27 C29 113.9(6) . . ? C28 C27 H27A 107.8 . . ? C23 C27 H27A 107.8 . . ? C29 C27 H27A 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C30 P1 C36 104.9(4) . . ? C30 P1 C42 102.1(3) . . ? C36 P1 C42 103.4(3) . . ? C30 P1 Pd1 112.8(3) . . ? C36 P1 Pd1 108.7(2) . . ? C42 P1 Pd1 123.3(3) . . ? C31 C30 C35 119.5(7) . . ? C31 C30 P1 118.1(6) . . ? C35 C30 P1 122.4(6) . . ? C30 C31 C32 119.8(7) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C33 C32 C31 120.2(8) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 120.4(8) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C35 C34 C33 119.5(8) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C34 C35 C30 120.7(7) . . ? C34 C35 H35A 119.7 . . ? C30 C35 H35A 119.7 . . ? C41 C36 C37 117.5(7) . . ? C41 C36 P1 124.6(6) . . ? C37 C36 P1 117.9(6) . . ? C38 C37 C36 120.9(8) . . ? C38 C37 H37A 119.6 . . ? C36 C37 H37A 119.6 . . ? C39 C38 C37 120.0(8) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C40 C39 C38 119.4(8) . . ? C40 C39 H39A 120.3 . . ? C38 C39 H39A 120.3 . . ? C39 C40 C41 121.3(8) . . ? C39 C40 H40A 119.4 . . ? C41 C40 H40A 119.4 . . ? C40 C41 C36 120.9(8) . . ? C40 C41 H41A 119.5 . . ? C36 C41 H41A 119.5 . . ? C47 C42 C43 119.5(8) . . ? C47 C42 P1 119.5(6) . . ? C43 C42 P1 121.0(7) . . ? C44 C43 C42 117.1(9) . . ? C44 C43 H43A 121.4 . . ? C42 C43 H43A 121.5 . . ? C43 C44 C45 122.6(9) . . ? C43 C44 H44A 118.7 . . ? C45 C44 H44A 118.7 . . ? C44 C45 C46 119.8(9) . . ? C44 C45 H45A 120.1 . . ? C46 C45 H45A 120.1 . . ? C47 C46 C45 118.7(9) . . ? C47 C46 H46A 120.7 . . ? C45 C46 H46A 120.7 . . ? C42 C47 C46 122.3(8) . . ? C42 C47 H47A 118.8 . . ? C46 C47 H47A 118.8 . . ? Cl2 C48 Cl1 112.7(6) . . ? Cl2 C48 H48A 109.1 . . ? Cl1 C48 H48A 109.1 . . ? Cl2 C48 H48B 109.1 . . ? Cl1 C48 H48B 109.1 . . ? H48A C48 H48B 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 C1 Pd1 O1 O2 -177.7(4) . . . . ? P1 Pd1 O1 O2 0.9(6) . . . . ? C1 Pd1 O2 O1 5.1(8) . . . . ? P1 Pd1 O2 O1 -179.5(3) . . . . ? O1 Pd1 C1 N5 102.2(6) . . . . ? O2 Pd1 C1 N5 98.3(9) . . . . ? P1 Pd1 C1 N5 -77.1(6) . . . . ? O1 Pd1 C1 N2 -75.5(6) . . . . ? O2 Pd1 C1 N2 -79.5(9) . . . . ? P1 Pd1 C1 N2 105.2(6) . . . . ? N5 C1 N2 C6 -161.4(6) . . . . ? Pd1 C1 N2 C6 16.7(10) . . . . ? N5 C1 N2 C3 6.1(8) . . . . ? Pd1 C1 N2 C3 -175.9(5) . . . . ? C1 N2 C3 C4 -15.1(8) . . . . ? C6 N2 C3 C4 153.6(6) . . . . ? N2 C3 C4 N5 16.9(7) . . . . ? N2 C1 N5 C18 164.8(6) . . . . ? Pd1 C1 N5 C18 -13.2(10) . . . . ? N2 C1 N5 C4 5.9(8) . . . . ? Pd1 C1 N5 C4 -172.1(5) . . . . ? C3 C4 N5 C1 -15.0(8) . . . . ? C3 C4 N5 C18 -175.9(6) . . . . ? C1 N2 C6 C11 91.1(9) . . . . ? C3 N2 C6 C11 -75.3(8) . . . . ? C1 N2 C6 C7 -95.6(9) . . . . ? C3 N2 C6 C7 97.9(8) . . . . ? C11 C6 C7 C8 -3.0(12) . . . . ? N2 C6 C7 C8 -175.9(7) . . . . ? C11 C6 C7 C12 174.7(7) . . . . ? N2 C6 C7 C12 1.8(11) . . . . ? C6 C7 C8 C9 1.3(13) . . . . ? C12 C7 C8 C9 -176.3(8) . . . . ? C7 C8 C9 C10 -0.7(13) . . . . ? C8 C9 C10 C11 1.7(13) . . . . ? C7 C6 C11 C10 3.9(11) . . . . ? N2 C6 C11 C10 177.2(7) . . . . ? C7 C6 C11 C15 -179.6(8) . . . . ? N2 C6 C11 C15 -6.3(11) . . . . ? C9 C10 C11 C6 -3.3(12) . . . . ? C9 C10 C11 C15 -179.9(8) . . . . ? C8 C7 C12 C13 82.8(10) . . . . ? C6 C7 C12 C13 -94.9(9) . . . . ? C8 C7 C12 C14 -41.3(11) . . . . ? C6 C7 C12 C14 141.1(8) . . . . ? C6 C11 C15 C16 -119.5(9) . . . . ? C10 C11 C15 C16 56.9(10) . . . . ? C6 C11 C15 C17 116.3(8) . . . . ? C10 C11 C15 C17 -67.2(9) . . . . ? C1 N5 C18 C23 -59.9(10) . . . . ? C4 N5 C18 C23 97.6(8) . . . . ? C1 N5 C18 C19 127.3(8) . . . . ? C4 N5 C18 C19 -75.2(8) . . . . ? C23 C18 C19 C20 6.4(11) . . . . ? N5 C18 C19 C20 179.0(6) . . . . ? C23 C18 C19 C24 -173.5(7) . . . . ? N5 C18 C19 C24 -0.8(10) . . . . ? C18 C19 C20 C21 -3.3(12) . . . . ? C24 C19 C20 C21 176.6(8) . . . . ? C19 C20 C21 C22 -0.8(14) . . . . ? C20 C21 C22 C23 2.0(14) . . . . ? C21 C22 C23 C18 1.0(13) . . . . ? C21 C22 C23 C27 -172.5(8) . . . . ? C19 C18 C23 C22 -5.3(11) . . . . ? N5 C18 C23 C22 -177.8(7) . . . . ? C19 C18 C23 C27 167.7(7) . . . . ? N5 C18 C23 C27 -4.7(11) . . . . ? C20 C19 C24 C26 53.3(10) . . . . ? C18 C19 C24 C26 -126.9(8) . . . . ? C20 C19 C24 C25 -69.1(9) . . . . ? C18 C19 C24 C25 110.7(8) . . . . ? C22 C23 C27 C28 77.7(9) . . . . ? C18 C23 C27 C28 -95.3(9) . . . . ? C22 C23 C27 C29 -46.2(10) . . . . ? C18 C23 C27 C29 140.8(7) . . . . ? O1 Pd1 P1 C30 -87.4(5) . . . . ? C1 Pd1 P1 C30 91.2(4) . . . . ? O2 Pd1 P1 C30 -86.8(3) . . . . ? O1 Pd1 P1 C36 28.4(5) . . . . ? C1 Pd1 P1 C36 -152.9(4) . . . . ? O2 Pd1 P1 C36 29.1(3) . . . . ? O1 Pd1 P1 C42 149.4(5) . . . . ? C1 Pd1 P1 C42 -31.9(4) . . . . ? O2 Pd1 P1 C42 150.1(4) . . . . ? C36 P1 C30 C31 -109.1(6) . . . . ? C42 P1 C30 C31 143.3(6) . . . . ? Pd1 P1 C30 C31 9.0(7) . . . . ? C36 P1 C30 C35 69.9(7) . . . . ? C42 P1 C30 C35 -37.7(7) . . . . ? Pd1 P1 C30 C35 -172.0(6) . . . . ? C35 C30 C31 C32 -1.2(12) . . . . ? P1 C30 C31 C32 177.9(6) . . . . ? C30 C31 C32 C33 -0.2(12) . . . . ? C31 C32 C33 C34 1.2(13) . . . . ? C32 C33 C34 C35 -0.9(13) . . . . ? C33 C34 C35 C30 -0.5(12) . . . . ? C31 C30 C35 C34 1.5(12) . . . . ? P1 C30 C35 C34 -177.5(6) . . . . ? C30 P1 C36 C41 -26.5(8) . . . . ? C42 P1 C36 C41 80.1(7) . . . . ? Pd1 P1 C36 C41 -147.3(6) . . . . ? C30 P1 C36 C37 154.8(6) . . . . ? C42 P1 C36 C37 -98.6(6) . . . . ? Pd1 P1 C36 C37 33.9(6) . . . . ? C41 C36 C37 C38 -1.5(11) . . . . ? P1 C36 C37 C38 177.3(6) . . . . ? C36 C37 C38 C39 1.7(12) . . . . ? C37 C38 C39 C40 -1.1(12) . . . . ? C38 C39 C40 C41 0.3(13) . . . . ? C39 C40 C41 C36 -0.2(13) . . . . ? C37 C36 C41 C40 0.8(12) . . . . ? P1 C36 C41 C40 -178.0(7) . . . . ? C30 P1 C42 C47 -79.5(7) . . . . ? C36 P1 C42 C47 171.8(6) . . . . ? Pd1 P1 C42 C47 48.4(7) . . . . ? C30 P1 C42 C43 102.3(7) . . . . ? C36 P1 C42 C43 -6.5(7) . . . . ? Pd1 P1 C42 C43 -129.9(5) . . . . ? C47 C42 C43 C44 -0.1(12) . . . . ? P1 C42 C43 C44 178.2(6) . . . . ? C42 C43 C44 C45 1.0(13) . . . . ? C43 C44 C45 C46 -0.6(14) . . . . ? C44 C45 C46 C47 -0.7(13) . . . . ? C43 C42 C47 C46 -1.2(13) . . . . ? P1 C42 C47 C46 -179.5(7) . . . . ? C45 C46 C47 C42 1.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.020 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.100