data_General _publ_contact_author_name 'Dr Kei Goto' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, The University of Tokyo 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan ; _publ_contact_author_email 'goto@chem.s.u-tokyo.ac.jp' _publ_contact_author_fax '+81-3-5800-6899' _publ_contact_author_phone '+81-3-5800-6899' _publ_requested_journal ; Journal of the American Chemical Society ; _publ_section_title ; Fixation of Both O2 and CO2 from Air by a Crystalline Palladium Complex Bearing N-Heterocyclic Carbene Ligands ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'FIRST AUTHORS NAME' 'FIRST AUTHORS FOOTNOTES' 'FIRST AUTHORS ADDRESS' _publ_section_synopsis 'Synopsis' _publ_section_abstract 'Abstract' _publ_section_comment 'text' _publ_section_acknowledgements 'acknowledgement' _publ_section_references 'references' _publ_section_figure_captions 'captions' _publ_section_exptl_prep 'preparation details' _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C107 H110 N4 Pd' _chemical_formula_weight 1558.39 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' '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 'P21/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.310(5) _cell_length_b 19.927(6) _cell_length_c 28.867(9) _cell_angle_alpha 90.0000(17) _cell_angle_beta 94.6626(18) _cell_angle_gamma 90.0000(17) _cell_volume 8778(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'red' _exptl_crystal_colour 'block' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9496 _exptl_absorpt_correction_T_max 0.9496 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU MercuryCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54068 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15293 _reflns_number_gt 14945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0541P)^2^+66.4350P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15293 _refine_ls_number_parameters 1138 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2292 _refine_ls_wR_factor_gt 0.2259 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 2.363 _refine_ls_shift/su_mean 0.021 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.63556(3) 0.01428(2) 0.238281(15) 0.02211(14) Uani 1 1 d . B . N1 N 0.5075(3) 0.1104(2) 0.27916(15) 0.0231(10) Uani 1 1 d . B . C1 C 0.7311(4) -0.0554(3) 0.2421(2) 0.0269(12) Uani 1 1 d . . . C2 C 0.5423(4) 0.0961(3) 0.32576(19) 0.0247(12) Uani 1 1 d . . . C3 C 0.4948(4) 0.0992(3) 0.15620(19) 0.0244(12) Uani 1 1 d . . . N2 N 0.4873(3) 0.1118(2) 0.20510(15) 0.0231(10) Uani 1 1 d . B . C4 C 0.5867(4) 0.1341(3) 0.4028(2) 0.0305(13) Uani 1 1 d . . . C5 C 0.5394(4) 0.0834(3) 0.23976(18) 0.0216(11) Uani 1 1 d . . . C6 C 0.5701(4) 0.0323(3) 0.33714(19) 0.0255(12) Uani 1 1 d . . . H1 H 0.5621 -0.0027 0.3149 0.031 Uiso 1 1 calc R . . C7 C 0.8592(10) 0.0160(8) 0.2400(6) 0.019(5) Uiso 0.49 1 d P A 2 C8 C 0.6099(4) 0.0187(3) 0.3810(2) 0.0297(13) Uani 1 1 d . . . C9 C 0.6473(4) -0.0498(3) 0.3908(2) 0.0317(13) Uani 1 1 d . . . C10 C 0.8578(13) 0.1319(11) 0.2226(7) 0.022(6) Uiso 0.49 1 d P A 2 C11 C 0.5499(4) 0.1477(3) 0.35824(19) 0.0278(12) Uani 1 1 d . . . H2 H 0.5301 0.1917 0.3501 0.033 Uiso 1 1 calc R . . N3 N 0.8207(8) -0.0450(6) 0.2496(5) 0.021(3) Uiso 0.51 1 d P B 1 C12 C 0.5581(12) -0.3025(10) 0.3173(7) 0.018(6) Uiso 0.51 1 d P B 1 C13 C 0.4948(13) -0.2337(10) 0.2523(7) 0.019(5) Uiso 0.49 1 d P A 2 H57 H 0.4440 -0.2608 0.2538 0.023 Uiso 0.49 1 calc PR A 2 C14 C 0.4377(4) 0.1543(3) 0.2679(2) 0.0319(14) Uani 1 1 d . . . H3 H 0.4057 0.1790 0.2890 0.038 Uiso 1 1 calc R B . C15 C 0.5991(5) -0.0992(3) 0.4116(2) 0.0393(15) Uani 1 1 d . . . C16 C 0.6173(4) 0.0701(3) 0.4135(2) 0.0321(13) Uani 1 1 d . . . H4 H 0.6439 0.0611 0.4438 0.039 Uiso 1 1 calc R . . C17 C 0.8203(15) 0.0692(11) 0.2193(8) 0.021(7) Uiso 0.49 1 d P A 2 H58 H 0.7654 0.0637 0.2018 0.025 Uiso 0.49 1 calc PR A 2 C18 C 0.4249(4) 0.1548(3) 0.2218(2) 0.0326(14) Uani 1 1 d . B . H5 H 0.3816 0.1796 0.2037 0.039 Uiso 1 1 calc R . . C19 C 0.4928(15) -0.1794(11) 0.2184(8) 0.027(7) Uiso 0.49 1 d P A 2 C20 C 0.7306(4) -0.0633(3) 0.3772(2) 0.0387(15) Uani 1 1 d . . . N4 N 0.7256(7) -0.1218(5) 0.2521(4) 0.018(3) Uiso 0.51 1 d P B 1 C21 C 0.5041(4) 0.0751(3) 0.0627(2) 0.0336(14) Uiso 1 1 d . . . H215 H 0.5107 0.0679 0.0307 0.040 Uiso 0.46 1 calc PR C 1 H216 H 0.5098 0.0645 0.0310 0.040 Uiso 0.54 1 calc PR C 2 C22 C 0.5037(13) -0.2993(10) 0.3512(7) 0.027(6) Uiso 0.51 1 d P B 1 C23 C 0.8013(11) 0.1936(8) 0.2069(6) 0.024(5) Uiso 0.51 1 d P B 1 C24 C 0.5351(10) 0.2086(7) 0.4639(5) 0.034(4) Uiso 0.63 1 d P D 1 C25 C 0.6050(9) 0.1896(6) 0.4379(4) 0.025(4) Uiso 0.63 1 d P D 1 C26 C 0.8150(12) 0.2120(9) 0.1593(6) 0.027(5) Uiso 0.51 1 d P B 1 C27 C 0.3623(11) -0.1126(10) 0.1968(6) 0.033(5) Uiso 0.49 1 d P A 2 C28 C 0.4132(11) -0.1695(9) 0.1893(6) 0.027(5) Uiso 0.49 1 d P A 2 C29 C 0.5503(16) -0.4117(14) 0.3783(9) 0.040(8) Uiso 0.51 1 d P B 1 H59 H 0.5497 -0.4470 0.4004 0.048 Uiso 0.51 1 calc PR B 1 C30 C 0.6181(16) -0.3640(12) 0.3116(9) 0.027(7) Uiso 0.51 1 d P B 1 C31 C 0.7606(11) 0.2645(8) 0.1390(6) 0.030(4) Uiso 0.51 1 d P B 1 H60 H 0.7677 0.2795 0.1083 0.036 Uiso 0.51 1 calc PR B 1 C32 C 1.1482(8) 0.0776(6) 0.2710(6) 0.024(3) Uiso 0.49 1 d P A 2 C33 C 0.4465(14) -0.2408(11) 0.3589(8) 0.027(5) Uiso 0.51 1 d P B 1 H61 H 0.4780 -0.1993 0.3531 0.041 Uiso 0.51 1 calc PR B 1 H62 H 0.4304 -0.2411 0.3911 0.041 Uiso 0.51 1 calc PR B 1 H63 H 0.3933 -0.2435 0.3376 0.041 Uiso 0.51 1 calc PR B 1 C34 C 1.0730(9) 0.0929(7) 0.2945(5) 0.022(3) Uiso 0.49 1 d P A 2 C35 C 0.5993(17) -0.4158(14) 0.3405(10) 0.052(9) Uiso 0.51 1 d P B 1 H64 H 0.6223 -0.4586 0.3338 0.062 Uiso 0.51 1 calc PR B 1 C36 C 0.6347(5) -0.1631(4) 0.4174(3) 0.0486(18) Uani 1 1 d . D . H6 H 0.6025 -0.1972 0.4314 0.058 Uiso 1 1 calc R . . C37 C 0.6842(10) 0.2189(7) 0.4463(5) 0.036(4) Uiso 0.63 1 d P D 1 C38 C 0.5070(12) -0.0970(10) 0.0772(7) 0.049(6) Uiso 0.54 1 d P E 2 H17 H 0.5054 -0.1009 0.1110 0.073 Uiso 0.54 1 calc PR E 2 H18 H 0.5511 -0.0637 0.0701 0.073 Uiso 0.54 1 calc PR E 2 H19 H 0.5222 -0.1406 0.0643 0.073 Uiso 0.54 1 calc PR E 2 C39 C 0.6974(11) 0.2934(8) 0.1646(6) 0.038(4) Uiso 0.51 1 d P B 1 H65 H 0.6608 0.3279 0.1511 0.046 Uiso 0.51 1 calc PR B 1 C40 C 0.7352(12) 0.2257(9) 0.2293(6) 0.030(5) Uiso 0.51 1 d P B 1 C41 C 0.5660(11) -0.1464(8) 0.2130(6) 0.029(5) Uiso 0.49 1 d P A 2 H66 H 0.5671 -0.1137 0.1891 0.035 Uiso 0.49 1 calc PR A 2 C42 C 0.5090(6) -0.0846(4) 0.4265(3) 0.061(2) Uani 1 1 d . D . H7 H 0.4822 -0.1263 0.4363 0.092 Uiso 1 1 calc R . . H8 H 0.4726 -0.0651 0.4004 0.092 Uiso 1 1 calc R . . H9 H 0.5136 -0.0528 0.4525 0.092 Uiso 1 1 calc R . . C43 C 0.7853(5) -0.0094(4) 0.3569(3) 0.0490(18) Uani 1 1 d . D . H10 H 0.8430 -0.0276 0.3515 0.074 Uiso 1 1 calc R . . H11 H 0.7923 0.0284 0.3786 0.074 Uiso 1 1 calc R . . H12 H 0.7560 0.0061 0.3273 0.074 Uiso 1 1 calc R . . C44 C 0.5441(11) 0.2590(7) 0.4962(5) 0.034(4) Uiso 0.63 1 d P D 1 H145 H 0.4955 0.2731 0.5123 0.040 Uiso 0.63 1 calc PR D 1 C45 C 0.5177(7) 0.0364(5) 0.1439(4) 0.018(2) Uani 0.46 1 d P F 1 H20 H 0.5285 0.0030 0.1671 0.022 Uiso 0.46 1 calc PR F 1 C46 C 0.7209(14) 0.2045(11) 0.2742(7) 0.036(6) Uiso 0.51 1 d P B 1 H67 H 0.7045 0.1569 0.2735 0.054 Uiso 0.51 1 calc PR B 1 H68 H 0.6736 0.2311 0.2859 0.054 Uiso 0.51 1 calc PR B 1 H69 H 0.7746 0.2106 0.2946 0.054 Uiso 0.51 1 calc PR B 1 C47 C 0.3953(11) 0.2791(8) -0.0259(5) 0.048(4) Uani 0.46 1 d P F 1 H21 H 0.3770 0.3111 -0.0491 0.058 Uiso 0.46 1 calc PR F 1 C48 C 0.6836(12) -0.3661(8) 0.2749(6) 0.035(4) Uiso 0.51 1 d P B 1 H70 H 0.7365 -0.3414 0.2860 0.053 Uiso 0.51 1 calc PR B 1 H71 H 0.6576 -0.3455 0.2462 0.053 Uiso 0.51 1 calc PR B 1 H72 H 0.6989 -0.4128 0.2688 0.053 Uiso 0.51 1 calc PR B 1 C49 C 0.5008(12) -0.3525(10) 0.3828(7) 0.032(6) Uiso 0.51 1 d P B 1 H73 H 0.4647 -0.3487 0.4080 0.038 Uiso 0.51 1 calc PR B 1 C50 C 0.6873(15) 0.2728(11) 0.2089(8) 0.053(7) Uiso 0.51 1 d P B 1 H74 H 0.6437 0.2937 0.2255 0.064 Uiso 0.51 1 calc PR B 1 C51 C 0.4183(12) -0.0753(8) 0.0559(5) 0.035(4) Uiso 0.54 1 d P E 2 C52 C 0.6231(9) 0.2884(7) 0.5048(4) 0.035(3) Uiso 0.63 1 d P D 1 H146 H 0.6309 0.3231 0.5274 0.043 Uiso 0.63 1 calc PR D 1 C53 C 0.5890(14) 0.2463(9) 0.0579(6) 0.039(4) Uani 0.46 1 d P F 1 H22 H 0.5805 0.2647 0.0887 0.059 Uiso 0.46 1 calc PR F 1 H23 H 0.6251 0.2773 0.0412 0.059 Uiso 0.46 1 calc PR F 1 H24 H 0.6185 0.2028 0.0614 0.059 Uiso 0.46 1 calc PR F 1 C54 C 1.0803(11) 0.1133(8) 0.3428(6) 0.035(4) Uiso 0.49 1 d P A 2 C55 C 0.8665(8) -0.1051(6) 0.2573(5) 0.023(3) Uiso 0.51 1 d P B 1 H75 H 0.9283 -0.1109 0.2608 0.027 Uiso 0.51 1 calc PR B 1 C56 C 0.4411(13) 0.1586(11) 0.4596(7) 0.026(5) Uiso 0.37 1 d P D 2 H147 H 0.4144 0.1608 0.4276 0.040 Uiso 0.37 1 calc PR D 2 H148 H 0.3983 0.1728 0.4811 0.040 Uiso 0.37 1 calc PR D 2 H149 H 0.4597 0.1125 0.4668 0.040 Uiso 0.37 1 calc PR D 2 C57 C 0.3893(16) -0.2159(12) 0.1535(8) 0.053(7) Uiso 0.49 1 d P A 2 C58 C 0.8951(14) 0.1780(11) 0.1353(8) 0.056(6) Uiso 0.51 1 d P B 1 H76 H 0.9503 0.1892 0.1533 0.083 Uiso 0.51 1 calc PR B 1 H77 H 0.8964 0.1950 0.1035 0.083 Uiso 0.51 1 calc PR B 1 H78 H 0.8874 0.1292 0.1346 0.083 Uiso 0.51 1 calc PR B 1 C59 C 0.2822(12) -0.1032(10) 0.1694(7) 0.043(5) Uiso 0.49 1 d P A 2 H79 H 0.2464 -0.0651 0.1736 0.051 Uiso 0.49 1 calc PR A 2 C60 C 0.4393(8) 0.0533(6) 0.1323(4) 0.031(2) Uani 0.54 1 d P E 2 H25 H 0.3978 0.0290 0.1484 0.037 Uiso 0.54 1 calc PR E 2 C61 C 0.7636(5) -0.1284(4) 0.3829(3) 0.0503(19) Uani 1 1 d . D . H13 H 0.8197 -0.1388 0.3729 0.060 Uiso 1 1 calc R . . C62 C 0.7159(6) -0.1776(4) 0.4029(3) 0.0507(19) Uani 1 1 d . . . H14 H 0.7391 -0.2216 0.4067 0.061 Uiso 1 1 calc R D . C63 C 0.6915(10) 0.2683(7) 0.4811(5) 0.043(3) Uiso 0.63 1 d P D 1 H150 H 0.7470 0.2886 0.4883 0.051 Uiso 0.63 1 calc PR D 1 C64 C 0.3894(13) -0.0596(9) 0.2358(7) 0.035(5) Uiso 0.49 1 d P A 2 H80 H 0.3882 -0.0808 0.2664 0.052 Uiso 0.49 1 calc PR A 2 H81 H 0.3481 -0.0219 0.2335 0.052 Uiso 0.49 1 calc PR A 2 H82 H 0.4487 -0.0431 0.2319 0.052 Uiso 0.49 1 calc PR A 2 C65 C 0.8059(7) -0.1527(6) 0.2588(5) 0.022(2) Uiso 0.51 1 d P B 1 H83 H 0.8162 -0.1993 0.2636 0.026 Uiso 0.51 1 calc PR B 1 C66 C 1.2342(10) 0.1052(8) 0.3459(6) 0.037(3) Uiso 0.49 1 d P A 2 H84 H 1.2901 0.1095 0.3625 0.044 Uiso 0.49 1 calc PR A 2 C67 C 0.5517(8) -0.0492(6) 0.0854(4) 0.024(3) Uani 0.46 1 d P F 1 C68 C 1.1401(10) 0.0558(8) 0.2217(6) 0.037(4) Uiso 0.49 1 d P A 2 H85 H 1.1975 0.0584 0.2090 0.056 Uiso 0.49 1 calc PR A 2 H86 H 1.0987 0.0852 0.2037 0.056 Uiso 0.49 1 calc PR A 2 H87 H 1.1186 0.0095 0.2197 0.056 Uiso 0.49 1 calc PR A 2 C69 C 0.5552(8) 0.1348(6) 0.1336(4) 0.033(3) Uani 0.54 1 d P F 2 H26 H 0.5930 0.1656 0.1505 0.040 Uiso 0.54 1 calc PR F 2 C70 C 0.5257(8) 0.0202(6) 0.0969(4) 0.024(2) Uani 0.46 1 d P F 1 C71 C 0.6250(8) 0.1624(7) 0.0581(4) 0.039(3) Uani 0.54 1 d P F 2 C72 C 0.6409(9) -0.0677(6) 0.0938(4) 0.030(3) Uani 0.46 1 d P F 1 C73 C 0.7586(9) 0.1980(8) 0.4209(5) 0.049(4) Uiso 0.63 1 d P D 1 H151 H 0.7691 0.1499 0.4257 0.073 Uiso 0.63 1 calc PR D 1 H152 H 0.8109 0.2232 0.4324 0.073 Uiso 0.63 1 calc PR D 1 H153 H 0.7455 0.2069 0.3877 0.073 Uiso 0.63 1 calc PR D 1 C74 C 0.499(2) 0.2373(15) 0.0301(9) 0.045(6) Uani 0.46 1 d P F 1 C75 C 0.3865(8) -0.0065(6) 0.0585(4) 0.034(3) Uani 0.54 1 d P E 2 C76 C 0.4717(8) 0.1478(6) 0.1246(4) 0.025(3) Uani 0.46 1 d P F 1 H27 H 0.4533 0.1906 0.1345 0.030 Uiso 0.46 1 calc PR F 1 C77 C 0.4444(8) 0.0427(6) 0.0845(4) 0.035(3) Uani 0.54 1 d P E 2 C78 C 0.4756(8) 0.1340(6) 0.0771(4) 0.026(3) Uani 0.46 1 d P F 1 C79 C 0.4484(8) 0.1854(6) 0.0411(4) 0.025(3) Uani 0.46 1 d P F 1 C80 C 1.2283(9) 0.0842(7) 0.2974(5) 0.031(3) Uiso 0.49 1 d P A 2 H88 H 1.2808 0.0746 0.2832 0.037 Uiso 0.49 1 calc PR A 2 C81 C 0.2584(14) -0.1502(12) 0.1369(7) 0.053(5) Uiso 0.49 1 d P A 2 H89 H 0.2042 -0.1448 0.1188 0.063 Uiso 0.49 1 calc PR A 2 C82 C 1.1586(13) 0.1191(8) 0.3684(6) 0.039(3) Uiso 0.49 1 d P A 2 H90 H 1.1619 0.1320 0.4001 0.046 Uiso 0.49 1 calc PR A 2 C83 C 0.4335(13) -0.2708(10) 0.1440(8) 0.046(5) Uiso 0.49 1 d P A 2 H91 H 0.4957 -0.2597 0.1428 0.069 Uiso 0.49 1 calc PR A 2 H92 H 0.4105 -0.2889 0.1140 0.069 Uiso 0.49 1 calc PR A 2 H93 H 0.4272 -0.3044 0.1684 0.069 Uiso 0.49 1 calc PR A 2 C84 C 0.3644(10) 0.1795(7) 0.0173(4) 0.035(3) Uani 0.46 1 d P F 1 C85 C 1.0019(13) 0.1271(10) 0.3691(7) 0.056(5) Uiso 0.49 1 d P A 2 H94 H 1.0210 0.1444 0.4000 0.083 Uiso 0.49 1 calc PR A 2 H95 H 0.9688 0.0855 0.3722 0.083 Uiso 0.49 1 calc PR A 2 H96 H 0.9644 0.1604 0.3523 0.083 Uiso 0.49 1 calc PR A 2 C86 C 0.5135(12) -0.1612(7) 0.0635(5) 0.041(4) Uani 0.46 1 d P F 1 H28 H 0.4704 -0.1936 0.0537 0.049 Uiso 0.46 1 calc PR F 1 C87 C 0.3648(11) -0.1189(7) 0.0285(5) 0.055(4) Uani 0.54 1 d P E 2 H29 H 0.3834 -0.1638 0.0244 0.066 Uiso 0.54 1 calc PR E 2 C88 C 0.3065(14) -0.2031(11) 0.1291(7) 0.049(6) Uiso 0.49 1 d P A 2 H97 H 0.2849 -0.2343 0.1061 0.059 Uiso 0.49 1 calc PR A 2 C89 C 0.5988(12) -0.1815(7) 0.0718(5) 0.048(4) Uani 0.46 1 d P F 1 H30 H 0.6148 -0.2271 0.0678 0.058 Uiso 0.46 1 calc PR F 1 C90 C 0.3406(10) 0.2276(7) -0.0163(4) 0.035(3) Uani 0.46 1 d P F 1 H31 H 0.2848 0.2245 -0.0331 0.042 Uiso 0.46 1 calc PR F 1 C91 C 0.5617(8) 0.1260(6) 0.0846(4) 0.033(3) Uani 0.54 1 d P F 2 C92 C 0.2572(10) -0.0351(8) 0.0111(5) 0.056(4) Uani 0.54 1 d P E 2 H32 H 0.2022 -0.0226 -0.0041 0.067 Uiso 0.54 1 calc PR E 2 C93 C 0.3042(10) 0.1228(8) 0.0265(5) 0.037(3) Uani 0.46 1 d P F 1 H33 H 0.2495 0.1276 0.0066 0.056 Uiso 0.46 1 calc PR F 1 H34 H 0.2914 0.1236 0.0592 0.056 Uiso 0.46 1 calc PR F 1 H35 H 0.3322 0.0801 0.0196 0.056 Uiso 0.46 1 calc PR F 1 C94 C 0.2836(11) -0.0975(8) 0.0068(5) 0.053(4) Uani 0.54 1 d P . 2 H36 H 0.2477 -0.1285 -0.0111 0.063 Uiso 0.54 1 calc PR . 2 C95 C 0.7449(12) 0.2292(10) 0.0073(5) 0.068(5) Uani 0.54 1 d P F 2 H37 H 0.7851 0.2521 -0.0105 0.082 Uiso 0.54 1 calc PR F 2 C96 C 0.6606(11) -0.1344(8) 0.0861(5) 0.045(4) Uani 0.46 1 d P F 1 H38 H 0.7200 -0.1482 0.0910 0.054 Uiso 0.46 1 calc PR F 1 C97 C 0.3059(9) 0.0140(7) 0.0369(4) 0.041(3) Uani 0.54 1 d P E 2 C98 C 0.7309(10) 0.0656(8) 0.0746(7) 0.067(5) Uani 0.54 1 d P G 2 H39 H 0.6892 0.0542 0.0974 0.100 Uiso 0.54 1 calc PR G 2 H40 H 0.7902 0.0681 0.0902 0.100 Uiso 0.54 1 calc PR G 2 H41 H 0.7291 0.0311 0.0504 0.100 Uiso 0.54 1 calc PR G 2 C99 C 0.4753(12) 0.2850(7) -0.0026(5) 0.044(4) Uani 0.46 1 d P F 1 H42 H 0.5136 0.3209 -0.0087 0.052 Uiso 0.46 1 calc PR F 1 C100 C 0.7090(10) -0.0182(8) 0.1099(5) 0.043(4) Uani 0.46 1 d P F 1 H43 H 0.7125 -0.0153 0.1439 0.065 Uiso 0.46 1 calc PR F 1 H44 H 0.6938 0.0259 0.0965 0.065 Uiso 0.46 1 calc PR F 1 H45 H 0.7658 -0.0324 0.1000 0.065 Uiso 0.46 1 calc PR F 1 C101 C 0.6654(11) 0.2572(9) 0.0141(5) 0.059(4) Uani 0.54 1 d P F 2 H46 H 0.6509 0.2995 0.0004 0.070 Uiso 0.54 1 calc PR F 2 C102 C 0.7665(10) 0.1666(9) 0.0267(6) 0.063(4) Uani 0.54 1 d P . 2 H47 H 0.8217 0.1470 0.0222 0.075 Uiso 0.54 1 calc PR . 2 C103 C 0.7069(9) 0.1319(8) 0.0531(5) 0.048(3) Uani 0.54 1 d P . 2 C104 C 0.2782(12) 0.0841(9) 0.0382(7) 0.066(5) Uani 0.54 1 d P E 2 H48 H 0.2824 0.0998 0.0705 0.100 Uiso 0.54 1 calc PR E 2 H49 H 0.2175 0.0879 0.0249 0.100 Uiso 0.54 1 calc PR E 2 H50 H 0.3163 0.1115 0.0201 0.100 Uiso 0.54 1 calc PR E 2 C105 C 0.5178(16) 0.2540(13) 0.0438(8) 0.045(5) Uani 0.54 1 d P F 2 H51 H 0.5049 0.2869 0.0190 0.068 Uiso 0.54 1 calc PR F 2 H52 H 0.5157 0.2760 0.0741 0.068 Uiso 0.54 1 calc PR F 2 H53 H 0.4743 0.2179 0.0409 0.068 Uiso 0.54 1 calc PR F 2 C106 C 0.4870(12) -0.0939(8) 0.0690(6) 0.023(4) Uiso 0.46 1 d P F 1 C107 C 0.6054(12) 0.2259(9) 0.0400(6) 0.041(4) Uani 0.54 1 d P F 2 C108 C 1.1346(15) 0.1386(13) 0.3754(8) 0.076(7) Uiso 0.51 1 d P B 1 H98 H 1.1338 0.1587 0.4052 0.091 Uiso 0.51 1 calc PR B 1 C109 C 0.8026(8) -0.1572(7) 0.2399(5) 0.028(3) Uiso 0.49 1 d P A 2 H99 H 0.8125 -0.2043 0.2409 0.034 Uiso 0.49 1 calc PR A 2 C110 C 0.3928(13) -0.0715(9) 0.0574(7) 0.038(5) Uiso 0.46 1 d P F 1 H54 H 0.3703 -0.0511 0.0850 0.056 Uiso 0.46 1 calc PR F 1 H55 H 0.3566 -0.1103 0.0477 0.056 Uiso 0.46 1 calc PR F 1 H56 H 0.3907 -0.0384 0.0322 0.056 Uiso 0.46 1 calc PR F 1 C111 C 1.1449(10) 0.0590(8) 0.2386(7) 0.039(4) Uiso 0.51 1 d P B 1 H100 H 1.1209 0.0134 0.2368 0.058 Uiso 0.51 1 calc PR B 1 H101 H 1.2062 0.0581 0.2311 0.058 Uiso 0.51 1 calc PR B 1 H102 H 1.1109 0.0878 0.2163 0.058 Uiso 0.51 1 calc PR B 1 C112 C 1.2212(11) 0.0945(9) 0.3169(8) 0.050(4) Uiso 0.51 1 d P B 1 H103 H 1.2772 0.0836 0.3071 0.060 Uiso 0.51 1 calc PR B 1 C113 C 0.8631(9) -0.1095(7) 0.2400(6) 0.030(3) Uiso 0.49 1 d P A 2 H104 H 0.9247 -0.1160 0.2412 0.036 Uiso 0.49 1 calc PR A 2 C114 C 1.1398(9) 0.0864(7) 0.2876(6) 0.031(3) Uiso 0.51 1 d P B 1 N5 N 0.7207(7) -0.1243(6) 0.2380(5) 0.022(3) Uiso 0.49 1 d P A 2 C115 C 1.0608(10) 0.1049(8) 0.3055(6) 0.032(4) Uiso 0.51 1 d P B 1 C116 C 1.2081(18) 0.1196(11) 0.3605(8) 0.070(5) Uiso 0.51 1 d P B 1 H105 H 1.2586 0.1232 0.3818 0.084 Uiso 0.51 1 calc PR B 1 C117 C 0.9744(13) 0.1467(11) 0.3677(7) 0.059(5) Uiso 0.51 1 d P B 1 H106 H 0.9478 0.1853 0.3509 0.089 Uiso 0.51 1 calc PR B 1 H107 H 0.9849 0.1578 0.4008 0.089 Uiso 0.51 1 calc PR B 1 H108 H 0.9346 0.1082 0.3641 0.089 Uiso 0.51 1 calc PR B 1 C118 C 1.0591(12) 0.1297(9) 0.3486(6) 0.046(4) Uiso 0.51 1 d P B 1 N6 N 0.8193(8) -0.0482(6) 0.2381(5) 0.020(4) Uiso 0.49 1 d P A 2 C119 C 0.5153(14) 0.2019(9) 0.4643(6) 0.015(5) Uiso 0.37 1 d P D 2 C120 C 0.5943(17) 0.2916(12) 0.5021(8) 0.039(6) Uiso 0.37 1 d P D 2 H154 H 0.5955 0.3271 0.5241 0.046 Uiso 0.37 1 calc PR D 2 C121 C 0.6669(15) 0.2822(11) 0.4766(7) 0.037(5) Uiso 0.37 1 d P D 2 H155 H 0.7172 0.3101 0.4810 0.045 Uiso 0.37 1 calc PR D 2 C122 C 0.5221(17) 0.2522(11) 0.4967(8) 0.033(7) Uiso 0.37 1 d P D 2 H156 H 0.4752 0.2597 0.5157 0.039 Uiso 0.37 1 calc PR D 2 C123 C 0.7424(13) 0.2180(10) 0.4122(7) 0.033(4) Uiso 0.37 1 d P D 2 H157 H 0.7960 0.2358 0.4286 0.050 Uiso 0.37 1 calc PR D 2 H158 H 0.7307 0.2417 0.3826 0.050 Uiso 0.37 1 calc PR D 2 H159 H 0.7499 0.1700 0.4062 0.050 Uiso 0.37 1 calc PR D 2 C124 C 0.5822(15) 0.1885(10) 0.4384(7) 0.021(5) Uiso 0.37 1 d P D 2 C125 C 0.6625(15) 0.2284(11) 0.4432(7) 0.029(6) Uiso 0.37 1 d P D 2 C126 C 0.4419(11) 0.1771(8) 0.4534(6) 0.053(5) Uiso 0.63 1 d P D 1 H160 H 0.4169 0.1922 0.4228 0.079 Uiso 0.63 1 calc PR D 1 H161 H 0.4038 0.1912 0.4773 0.079 Uiso 0.63 1 calc PR D 1 H162 H 0.4466 0.1280 0.4535 0.079 Uiso 0.63 1 calc PR D 1 C127 C 0.4528(16) -0.2562(13) 0.1413(10) 0.070(7) Uiso 0.51 1 d P B 1 H109 H 0.4284 -0.3009 0.1460 0.105 Uiso 0.51 1 calc PR B 1 H110 H 0.5083 -0.2514 0.1604 0.105 Uiso 0.51 1 calc PR B 1 H111 H 0.4631 -0.2505 0.1085 0.105 Uiso 0.51 1 calc PR B 1 C128 C 0.4099(11) -0.1548(10) 0.1947(6) 0.030(5) Uiso 0.51 1 d P B 1 C129 C 0.3838(12) -0.1993(10) 0.1562(6) 0.034(5) Uiso 0.51 1 d P B 1 C130 C 0.3625(10) -0.0991(9) 0.2055(6) 0.029(4) Uiso 0.51 1 d P B 1 C131 C 0.3909(15) -0.0599(11) 0.2483(8) 0.050(6) Uiso 0.51 1 d P B 1 H112 H 0.3886 -0.0887 0.2756 0.075 Uiso 0.51 1 calc PR B 1 H113 H 0.3517 -0.0215 0.2509 0.075 Uiso 0.51 1 calc PR B 1 H114 H 0.4510 -0.0439 0.2463 0.075 Uiso 0.51 1 calc PR B 1 C132 C 0.9423(11) 0.1402(9) 0.2464(6) 0.026(5) Uiso 0.49 1 d P A 2 H115 H 0.9698 0.1829 0.2479 0.031 Uiso 0.49 1 calc PR A 2 C133 C 0.9437(10) 0.0234(8) 0.2657(6) 0.019(4) Uiso 0.49 1 d P A 2 H116 H 0.9712 -0.0141 0.2811 0.023 Uiso 0.49 1 calc PR A 2 C134 C 0.9838(12) 0.0846(9) 0.2676(7) 0.030(5) Uiso 0.49 1 d P A 2 C135 C 0.5589(16) -0.2458(13) 0.2791(9) 0.041(9) Uiso 0.51 1 d P A 2 C136 C 0.2574(10) -0.1261(9) 0.1403(6) 0.037(4) Uiso 0.51 1 d P B 1 H117 H 0.2036 -0.1166 0.1227 0.044 Uiso 0.51 1 calc PR B 1 C137 C 0.3078(13) -0.1818(11) 0.1296(7) 0.048(5) Uiso 0.51 1 d P B 1 H118 H 0.2893 -0.2084 0.1033 0.058 Uiso 0.51 1 calc PR B 1 C138 C 0.6382(12) -0.2093(10) 0.2742(7) 0.031(6) Uiso 0.49 1 d P A 2 H119 H 0.6894 -0.2198 0.2936 0.038 Uiso 0.49 1 calc PR A 2 C139 C 0.6409(9) -0.1588(7) 0.2416(6) 0.022(4) Uiso 0.49 1 d P A 2 C140 C 0.2876(10) -0.0845(9) 0.1775(6) 0.034(4) Uiso 0.51 1 d P B 1 H120 H 0.2554 -0.0452 0.1835 0.040 Uiso 0.51 1 calc PR B 1 C141 C 0.5604(18) -0.4180(14) 0.3729(10) 0.045(9) Uiso 0.49 1 d P A 2 H121 H 0.5561 -0.4576 0.3909 0.054 Uiso 0.49 1 calc PR A 2 C142 C 0.5115(14) -0.3657(12) 0.3822(7) 0.036(6) Uiso 0.49 1 d P A 2 H122 H 0.4769 -0.3670 0.4081 0.043 Uiso 0.49 1 calc PR A 2 C143 C 0.6080(19) -0.3606(16) 0.3072(10) 0.040(10) Uiso 0.49 1 d P A 2 C144 C 0.6613(13) -0.3675(10) 0.2660(7) 0.045(5) Uiso 0.49 1 d P A 2 H123 H 0.6245 -0.3573 0.2375 0.068 Uiso 0.49 1 calc PR A 2 H124 H 0.6833 -0.4136 0.2644 0.068 Uiso 0.49 1 calc PR A 2 H125 H 0.7108 -0.3363 0.2692 0.068 Uiso 0.49 1 calc PR A 2 C145 C 0.6159(15) -0.4175(10) 0.3391(7) 0.027(6) Uiso 0.49 1 d P A 2 H126 H 0.6578 -0.4521 0.3362 0.032 Uiso 0.49 1 calc PR A 2 C146 C 0.5108(15) -0.3106(12) 0.3549(8) 0.035(7) Uiso 0.49 1 d P A 2 C147 C 0.5677(15) -0.3098(12) 0.3146(8) 0.032(8) Uiso 0.49 1 d P A 2 C148 C 0.452(2) -0.2508(14) 0.3624(11) 0.055(10) Uiso 0.49 1 d P A 2 H127 H 0.3978 -0.2551 0.3425 0.082 Uiso 0.49 1 calc PR A 2 H128 H 0.4826 -0.2095 0.3545 0.082 Uiso 0.49 1 calc PR A 2 H129 H 0.4391 -0.2492 0.3950 0.082 Uiso 0.49 1 calc PR A 2 C149 C 0.9411(11) 0.0310(9) 0.2753(6) 0.032(5) Uiso 0.51 1 d P B 1 H130 H 0.9697 -0.0044 0.2925 0.038 Uiso 0.51 1 calc PR B 1 C150 C 0.9780(10) 0.0931(8) 0.2762(6) 0.024(4) Uiso 0.51 1 d P B 1 C151 C 0.9326(11) 0.1475(9) 0.2545(6) 0.029(5) Uiso 0.51 1 d P B 1 H131 H 0.9561 0.1915 0.2579 0.035 Uiso 0.51 1 calc PR B 1 C152 C 0.8563(14) 0.1376(11) 0.2292(8) 0.029(7) Uiso 0.51 1 d P B 1 C153 C 0.8189(16) 0.0733(13) 0.2255(8) 0.031(8) Uiso 0.51 1 d P B 1 H132 H 0.7653 0.0658 0.2073 0.037 Uiso 0.51 1 calc PR B 1 C154 C 0.8641(12) 0.0191(9) 0.2500(7) 0.029(5) Uiso 0.51 1 d P B 1 C155 C 0.7016(12) 0.2779(8) 0.2010(6) 0.028(4) Uiso 0.49 1 d P A 2 H163 H 0.6581 0.3016 0.2161 0.033 Uiso 0.49 1 calc PR A 2 C156 C 0.7201(10) 0.2931(7) 0.1548(5) 0.024(3) Uiso 0.49 1 d P A 2 H133 H 0.6895 0.3291 0.1391 0.029 Uiso 0.49 1 calc PR A 2 C157 C 0.7814(10) 0.2574(7) 0.1312(5) 0.024(4) Uiso 0.49 1 d P A 2 H134 H 0.7920 0.2694 0.1003 0.029 Uiso 0.49 1 calc PR A 2 C158 C 0.8268(13) 0.2041(10) 0.1531(7) 0.036(6) Uiso 0.49 1 d P A 2 C159 C 0.8128(11) 0.1891(8) 0.1985(6) 0.022(5) Uiso 0.49 1 d P A 2 C160 C 0.7532(13) 0.2237(9) 0.2243(6) 0.027(5) Uiso 0.49 1 d P A 2 C161 C 0.5680(12) -0.2487(9) 0.2855(6) 0.015(5) Uiso 0.51 1 d P B 1 C162 C 0.6426(10) -0.2113(8) 0.2845(6) 0.020(4) Uiso 0.51 1 d P B 1 H136 H 0.6924 -0.2217 0.3051 0.024 Uiso 0.51 1 calc PR B 1 C163 C 0.6460(9) -0.1595(7) 0.2543(5) 0.019(4) Uiso 0.51 1 d P B 1 C164 C 0.5738(10) -0.1403(8) 0.2240(6) 0.024(4) Uiso 0.51 1 d P B 1 H137 H 0.5779 -0.1041 0.2029 0.029 Uiso 0.51 1 calc PR B 1 C165 C 0.4944(15) -0.1770(12) 0.2262(8) 0.033(8) Uiso 0.51 1 d P B 1 C166 C 0.4888(17) -0.2261(12) 0.2570(8) 0.038(8) Uiso 0.51 1 d P B 1 H138 H 0.4339 -0.2467 0.2606 0.046 Uiso 0.51 1 calc PR B 1 C167 C 0.8809(12) 0.1667(10) 0.1259(7) 0.040(5) Uiso 0.49 1 d P A 2 H139 H 0.8814 0.1874 0.0951 0.060 Uiso 0.49 1 calc PR A 2 H140 H 0.8586 0.1207 0.1227 0.060 Uiso 0.49 1 calc PR A 2 H141 H 0.9406 0.1660 0.1410 0.060 Uiso 0.49 1 calc PR A 2 C168 C 0.7387(18) 0.2059(15) 0.2775(9) 0.052(8) Uiso 0.49 1 d P A 2 H142 H 0.7139 0.1607 0.2791 0.079 Uiso 0.49 1 calc PR A 2 H143 H 0.6983 0.2385 0.2895 0.079 Uiso 0.49 1 calc PR A 2 H144 H 0.7950 0.2076 0.2961 0.079 Uiso 0.49 1 calc PR A 2 C169 C 0.7290(13) -0.1262(13) 0.1262(9) 0.097(8) Uiso 0.48 1 d PD H 3 H164 H 0.7484 -0.1620 0.1479 0.145 Uiso 0.48 1 calc PR H 3 H165 H 0.6806 -0.1426 0.1049 0.145 Uiso 0.48 1 calc PR H 3 H166 H 0.7092 -0.0877 0.1436 0.145 Uiso 0.48 1 calc PR H 3 C170 C 0.8066(13) -0.1045(14) 0.0979(8) 0.214(11) Uiso 0.48 1 d PD H 3 H167 H 0.7848 -0.0739 0.0725 0.257 Uiso 0.48 1 calc PR H 3 H168 H 0.8320 -0.1445 0.0837 0.257 Uiso 0.48 1 calc PR H 3 C171 C 0.8789(13) -0.0681(13) 0.1302(8) 0.222(11) Uiso 0.48 1 d PD H 3 H169 H 0.8535 -0.0287 0.1450 0.266 Uiso 0.48 1 calc PR H 3 H170 H 0.9026 -0.0990 0.1549 0.266 Uiso 0.48 1 calc PR H 3 C172 C 0.9531(11) -0.0455(11) 0.1004(7) 0.073(5) Uiso 0.48 1 d PD H 3 H171 H 0.9297 -0.0141 0.0759 0.088 Uiso 0.48 1 calc PR H 3 H172 H 0.9783 -0.0848 0.0854 0.088 Uiso 0.48 1 calc PR H 3 C173 C 1.0254(13) -0.0098(12) 0.1331(7) 0.084(6) Uiso 0.48 1 d PD H 3 H173 H 0.9984 0.0248 0.1520 0.101 Uiso 0.48 1 calc PR H 3 H174 H 1.0555 -0.0429 0.1544 0.101 Uiso 0.48 1 calc PR H 3 C174 C 1.0919(15) 0.0231(15) 0.1025(11) 0.102(9) Uiso 0.48 1 d PD H 3 H175 H 1.1231 -0.0119 0.0866 0.153 Uiso 0.48 1 calc PR H 3 H176 H 1.1341 0.0497 0.1221 0.153 Uiso 0.48 1 calc PR H 3 H177 H 1.0607 0.0524 0.0794 0.153 Uiso 0.48 1 calc PR H 3 C175 C 0.9728(16) -0.0313(15) 0.1374(8) 0.124(10) Uiso 0.34 1 d PD I 4 H178 H 0.9702 0.0073 0.1588 0.149 Uiso 0.34 1 calc PR I 4 H179 H 1.0184 -0.0629 0.1503 0.149 Uiso 0.34 1 calc PR I 4 C176 C 0.993(2) -0.0073(15) 0.0881(10) 0.22(2) Uiso 0.34 1 d PD I 4 H180 H 0.9795 -0.0444 0.0658 0.262 Uiso 0.34 1 calc PR I 4 H181 H 0.9533 0.0305 0.0788 0.262 Uiso 0.34 1 calc PR I 4 C177 C 0.988(3) -0.0680(17) 0.0541(10) 0.049(10) Uiso 0.18 1 d PD J 5 H182 H 1.0217 -0.1062 0.0684 0.059 Uiso 0.18 1 calc PR J 5 H183 H 0.9263 -0.0823 0.0476 0.059 Uiso 0.18 1 calc PR J 5 C178 C 1.026(4) -0.047(3) 0.0085(12) 0.072(16) Uiso 0.18 1 d PD J 5 H184 H 0.9825 -0.0216 -0.0108 0.108 Uiso 0.18 1 calc PR J 5 H185 H 1.0427 -0.0874 -0.0083 0.108 Uiso 0.18 1 calc PR J 5 H186 H 1.0785 -0.0192 0.0156 0.108 Uiso 0.18 1 calc PR J 5 C179 C 1.087(3) 0.015(4) 0.0847(17) 0.28(6) Uiso 0.34 1 d PD I 4 H187 H 1.1241 -0.0015 0.1121 0.340 Uiso 0.34 1 calc PR I 4 H188 H 1.0899 0.0647 0.0847 0.340 Uiso 0.34 1 calc PR I 4 C180 C 1.123(4) -0.013(4) 0.039(2) 0.24(4) Uiso 0.34 1 d PD I 4 H189 H 1.1432 0.0250 0.0210 0.367 Uiso 0.34 1 calc PR I 4 H190 H 1.0770 -0.0371 0.0212 0.367 Uiso 0.34 1 calc PR I 4 H191 H 1.1728 -0.0427 0.0476 0.367 Uiso 0.34 1 calc PR I 4 C181 C 0.8066(13) -0.1045(14) 0.0979(8) 0.214(11) Uiso 0.34 1 d P I 4 H192 H 0.7510 -0.0802 0.0985 0.321 Uiso 0.34 1 calc PR I 4 H193 H 0.7992 -0.1505 0.1089 0.321 Uiso 0.34 1 calc PR I 4 H194 H 0.8242 -0.1055 0.0660 0.321 Uiso 0.34 1 calc PR I 4 C182 C 0.8789(13) -0.0681(13) 0.1302(8) 0.222(11) Uiso 0.34 1 d PD I 4 H195 H 0.8871 -0.1021 0.1551 0.266 Uiso 0.34 1 calc PR I 4 H196 H 0.8423 -0.0332 0.1434 0.266 Uiso 0.34 1 calc PR I 4 C183 C 0.8066(13) -0.1045(14) 0.0979(8) 0.214(11) Uiso 0.18 1 d P J 5 H197 H 0.8171 -0.1530 0.0987 0.321 Uiso 0.18 1 calc PR J 5 H198 H 0.8084 -0.0882 0.0659 0.321 Uiso 0.18 1 calc PR J 5 H199 H 0.7488 -0.0950 0.1087 0.321 Uiso 0.18 1 calc PR J 5 C184 C 0.8789(13) -0.0681(13) 0.1302(8) 0.222(11) Uiso 0.18 1 d P J 5 H200 H 0.8871 -0.1021 0.1551 0.266 Uiso 0.18 1 calc PR J 5 H201 H 0.8423 -0.0332 0.1434 0.266 Uiso 0.18 1 calc PR J 5 C185 C 0.9728(16) -0.0313(15) 0.1374(8) 0.124(10) Uiso 0.18 1 d PD J 5 H202 H 0.9702 0.0073 0.1588 0.149 Uiso 0.18 1 calc PR J 5 H203 H 1.0184 -0.0629 0.1503 0.149 Uiso 0.18 1 calc PR J 5 C186 C 0.993(2) -0.0073(15) 0.0881(10) 0.22(2) Uiso 0.18 1 d PD J 5 H204 H 0.9497 0.0272 0.0769 0.262 Uiso 0.18 1 calc PR J 5 H205 H 1.0520 0.0129 0.0895 0.262 Uiso 0.18 1 calc PR J 5 C187 C 0.724(3) 0.1281(14) 0.5753(13) 0.067(11) Uiso 0.32 1 d PD K 2 H206 H 0.7734 0.1570 0.5853 0.101 Uiso 0.32 1 calc PR K 2 H207 H 0.7029 0.1052 0.6023 0.101 Uiso 0.32 1 calc PR K 2 H208 H 0.6763 0.1555 0.5603 0.101 Uiso 0.32 1 calc PR K 2 C188 C 0.730(3) 0.1294(18) 0.5620(15) 0.091(12) Uiso 0.40 1 d P L 1 H209 H 0.6869 0.1544 0.5418 0.136 Uiso 0.40 1 calc PR L 1 H210 H 0.7722 0.1608 0.5775 0.136 Uiso 0.40 1 calc PR L 1 H211 H 0.7002 0.1047 0.5854 0.136 Uiso 0.40 1 calc PR L 1 C189 C 0.7763(10) 0.0823(6) 0.5340(5) 0.032(4) Uiso 0.40 1 d PG L 1 C190 C 0.7459(10) 0.0167(7) 0.5303(6) 0.060(6) Uiso 0.40 1 d PG L 1 H220 H 0.6969 0.0033 0.5463 0.072 Uiso 0.40 1 calc PR L 1 C191 C 0.7871(13) -0.0294(6) 0.5033(7) 0.060(6) Uiso 0.40 1 d PG L 1 H221 H 0.7663 -0.0743 0.5008 0.072 Uiso 0.40 1 calc PR L 1 C192 C 0.8589(13) -0.0099(8) 0.4800(7) 0.077(7) Uiso 0.40 1 d PG L 1 H222 H 0.8871 -0.0414 0.4615 0.092 Uiso 0.40 1 calc PR L 1 C193 C 0.8893(13) 0.0557(9) 0.4836(7) 0.100(10) Uiso 0.40 1 d PG L 1 H223 H 0.9383 0.0691 0.4676 0.120 Uiso 0.40 1 calc PR L 1 C194 C 0.8481(12) 0.1019(7) 0.5106(7) 0.076(8) Uiso 0.40 1 d PG L 1 H224 H 0.8689 0.1467 0.5131 0.091 Uiso 0.40 1 calc PR L 1 C195 C 0.934(3) 0.012(4) 0.475(2) 0.20(3) Uiso 0.28 1 d PG M 3 H225 H 0.9846 0.0033 0.4588 0.234 Uiso 0.28 1 calc PR M 3 C196 C 0.904(5) 0.077(4) 0.480(3) 0.44(12) Uiso 0.28 1 d PG M 3 H226 H 0.9330 0.1130 0.4661 0.522 Uiso 0.28 1 calc PR M 3 C197 C 0.830(5) 0.089(2) 0.503(2) 0.27(6) Uiso 0.28 1 d PGD M 3 H227 H 0.8091 0.1334 0.5064 0.318 Uiso 0.28 1 calc PR M 3 C198 C 0.787(3) 0.036(2) 0.5230(17) 0.13(2) Uiso 0.28 1 d PGD M 3 C199 C 0.818(4) -0.029(2) 0.519(2) 0.27(6) Uiso 0.28 1 d PGD M 3 H228 H 0.7884 -0.0657 0.5321 0.329 Uiso 0.28 1 calc PR M 3 C200 C 0.891(5) -0.042(3) 0.495(3) 0.41(10) Uiso 0.28 1 d PG M 3 H229 H 0.9123 -0.0861 0.4918 0.494 Uiso 0.28 1 calc PR M 3 C201 C 0.7490(16) 0.0826(8) 0.5451(8) 0.059(7) Uiso 0.32 1 d PGD K 2 C202 C 0.8160(16) 0.0974(8) 0.5170(8) 0.068(8) Uiso 0.32 1 d PGD K 2 H230 H 0.8389 0.1417 0.5163 0.081 Uiso 0.32 1 calc PR K 2 C203 C 0.8496(16) 0.0475(11) 0.4899(8) 0.098(12) Uiso 0.32 1 d PG K 2 H231 H 0.8954 0.0577 0.4707 0.117 Uiso 0.32 1 calc PR K 2 C204 C 0.8161(16) -0.0173(9) 0.4908(8) 0.066(8) Uiso 0.32 1 d PG K 2 H232 H 0.8390 -0.0514 0.4723 0.080 Uiso 0.32 1 calc PR K 2 C205 C 0.7491(16) -0.0321(8) 0.5189(8) 0.066(8) Uiso 0.32 1 d PG K 2 H233 H 0.7262 -0.0764 0.5195 0.079 Uiso 0.32 1 calc PR K 2 C206 C 0.7156(15) 0.0178(10) 0.5460(8) 0.089(11) Uiso 0.32 1 d PGD K 2 H234 H 0.6698 0.0077 0.5652 0.107 Uiso 0.32 1 calc PR K 2 C207 C 0.734(4) 0.049(3) 0.556(2) 0.17(3) Uiso 0.28 1 d PD M 3 H217 H 0.6791 0.0237 0.5501 0.253 Uiso 0.28 1 calc PR M 3 H218 H 0.7208 0.0970 0.5565 0.253 Uiso 0.28 1 calc PR M 3 H219 H 0.7622 0.0356 0.5865 0.253 Uiso 0.28 1 calc PR M 3 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 0.0224(2) 0.0206(2) 0.0231(2) -0.00153(17) 0.00069(16) 0.00331(17) N1 0.030(2) 0.022(2) 0.017(2) -0.0021(18) -0.0013(19) 0.0048(19) C1 0.029(3) 0.019(3) 0.034(3) 0.001(2) 0.008(2) -0.001(2) C2 0.025(3) 0.031(3) 0.018(3) -0.002(2) 0.003(2) 0.003(2) C3 0.028(3) 0.027(3) 0.018(3) -0.001(2) -0.001(2) 0.002(2) N2 0.027(2) 0.024(2) 0.018(2) -0.0005(18) 0.0006(18) 0.0053(19) C4 0.046(4) 0.028(3) 0.017(3) 0.000(2) 0.004(2) -0.001(3) C5 0.026(3) 0.025(3) 0.013(3) -0.001(2) 0.001(2) 0.000(2) C6 0.029(3) 0.027(3) 0.021(3) -0.001(2) 0.001(2) 0.001(2) C8 0.036(3) 0.032(3) 0.022(3) 0.003(2) 0.003(2) 0.001(3) C9 0.043(4) 0.031(3) 0.020(3) 0.003(2) -0.006(3) 0.003(3) C11 0.037(3) 0.026(3) 0.020(3) 0.001(2) 0.001(2) 0.006(2) C14 0.036(3) 0.035(3) 0.025(3) 0.000(3) 0.001(2) 0.015(3) C15 0.055(4) 0.035(4) 0.027(3) 0.007(3) 0.000(3) 0.004(3) C16 0.043(4) 0.036(3) 0.017(3) 0.004(2) 0.000(2) 0.004(3) C18 0.034(3) 0.038(3) 0.026(3) -0.001(3) -0.001(2) 0.016(3) C20 0.042(4) 0.041(4) 0.031(3) 0.001(3) -0.007(3) 0.011(3) C36 0.065(5) 0.036(4) 0.043(4) 0.012(3) -0.003(4) -0.001(3) C42 0.066(5) 0.048(5) 0.073(6) 0.021(4) 0.026(4) 0.003(4) C43 0.038(4) 0.060(5) 0.048(4) 0.011(4) 0.003(3) 0.006(3) C45 0.022(6) 0.014(5) 0.018(6) 0.000(4) 0.001(4) 0.005(4) C47 0.067(11) 0.047(9) 0.028(8) 0.006(7) -0.009(7) 0.017(8) C53 0.059(13) 0.026(9) 0.032(11) -0.005(7) 0.003(9) -0.009(8) C60 0.044(7) 0.028(6) 0.022(6) 0.002(4) 0.006(5) -0.003(5) C61 0.055(5) 0.049(4) 0.045(4) 0.001(3) -0.007(3) 0.019(4) C62 0.069(5) 0.031(4) 0.050(4) 0.001(3) -0.011(4) 0.016(4) C67 0.039(7) 0.023(6) 0.011(5) -0.002(4) 0.004(5) 0.009(5) C69 0.039(7) 0.036(6) 0.023(6) -0.001(5) 0.000(5) 0.000(5) C70 0.029(6) 0.025(6) 0.015(6) 0.002(5) -0.003(5) 0.005(5) C71 0.042(7) 0.048(8) 0.028(6) -0.005(5) 0.010(5) -0.012(6) C72 0.039(7) 0.029(7) 0.024(6) 0.002(5) 0.006(5) 0.011(6) C74 0.066(17) 0.036(13) 0.030(13) -0.009(8) -0.011(10) 0.004(10) C75 0.039(7) 0.038(7) 0.026(6) -0.002(5) 0.004(5) -0.009(5) C76 0.035(7) 0.017(6) 0.022(6) -0.004(5) -0.003(5) 0.007(5) C77 0.042(7) 0.028(6) 0.033(6) -0.004(5) 0.000(5) -0.002(5) C78 0.030(7) 0.029(6) 0.018(6) 0.001(5) -0.003(5) 0.006(5) C79 0.038(7) 0.022(6) 0.015(6) 0.000(5) -0.004(5) 0.008(5) C84 0.045(8) 0.039(8) 0.020(6) -0.008(5) -0.008(6) 0.015(6) C86 0.072(11) 0.025(7) 0.026(7) -0.001(6) 0.006(7) -0.005(7) C87 0.082(11) 0.037(7) 0.051(9) -0.020(6) 0.030(8) -0.026(7) C89 0.085(13) 0.020(7) 0.044(9) -0.005(6) 0.026(8) 0.011(7) C90 0.049(8) 0.039(8) 0.016(6) 0.001(5) -0.009(6) 0.019(7) C91 0.045(7) 0.030(6) 0.025(6) 0.000(5) 0.003(5) -0.004(5) C92 0.055(9) 0.068(11) 0.044(8) -0.005(7) -0.002(7) -0.028(8) C93 0.042(9) 0.046(9) 0.023(7) 0.002(7) -0.008(6) 0.009(7) C94 0.067(10) 0.063(10) 0.029(7) -0.010(6) 0.015(7) -0.032(8) C95 0.071(11) 0.098(14) 0.036(8) -0.001(8) 0.007(8) -0.045(10) C96 0.057(10) 0.040(9) 0.040(8) 0.001(7) 0.014(7) 0.024(7) C97 0.045(7) 0.049(8) 0.028(6) 0.000(5) -0.005(5) -0.003(6) C98 0.036(8) 0.060(10) 0.103(14) 0.000(9) 0.001(8) 0.007(7) C99 0.077(11) 0.033(8) 0.021(7) 0.005(6) 0.003(7) 0.005(7) C100 0.038(8) 0.052(9) 0.040(8) -0.009(7) 0.005(6) 0.016(7) C101 0.070(11) 0.066(10) 0.040(8) 0.008(7) 0.007(7) -0.024(8) C102 0.042(8) 0.080(12) 0.068(11) -0.019(9) 0.016(7) -0.016(8) C103 0.040(7) 0.068(10) 0.037(7) -0.006(7) 0.003(6) -0.014(7) C104 0.063(11) 0.059(11) 0.073(13) 0.003(9) -0.021(9) 0.002(9) C105 0.047(14) 0.048(15) 0.041(14) 0.013(10) 0.006(11) 0.007(10) C107 0.059(10) 0.037(9) 0.028(9) -0.004(6) 0.007(7) -0.014(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 C1 2.013(6) . ? Pd1 C5 2.020(5) . ? N1 C5 1.382(7) . ? N1 C14 1.399(7) . ? N1 C2 1.435(7) . ? C1 N4 1.360(12) . ? C1 N6 1.371(14) . ? C1 N3 1.386(13) . ? C1 N5 1.387(13) . ? C2 C6 1.372(8) . ? C2 C11 1.391(8) . ? C3 C45 1.354(12) . ? C3 C76 1.359(13) . ? C3 C69 1.372(13) . ? C3 C60 1.393(13) . ? C3 N2 1.448(7) . ? N2 C5 1.352(7) . ? N2 C18 1.398(7) . ? C4 C16 1.387(9) . ? C4 C11 1.388(8) . ? C4 C124 1.50(2) . ? C4 C25 1.510(13) . ? C6 C8 1.386(8) . ? C6 H1 0.9500 . ? C7 C17 1.34(3) . ? C7 N6 1.42(2) . ? C7 C133 1.45(2) . ? C8 C16 1.389(9) . ? C8 C9 1.498(8) . ? C9 C20 1.391(9) . ? C9 C15 1.396(9) . ? C10 C17 1.37(3) . ? C10 C132 1.42(3) . ? C10 C159 1.48(3) . ? C11 H2 0.9500 . ? N3 C55 1.398(17) . ? N3 C154 1.44(2) . ? C12 C22 1.34(3) . ? C12 C161 1.43(3) . ? C12 C30 1.55(3) . ? C13 C135 1.22(3) . ? C13 C19 1.46(3) . ? C13 H57 0.9500 . ? C14 C18 1.327(8) . ? C14 H3 0.9500 . ? C15 C36 1.390(10) . ? C15 C42 1.505(11) . ? C16 H4 0.9500 . ? C17 H58 0.9500 . ? C18 H5 0.9500 . ? C19 C41 1.32(3) . ? C19 C28 1.44(3) . ? C20 C61 1.397(10) . ? C20 C43 1.510(10) . ? N4 C65 1.374(15) . ? N4 C163 1.437(17) . ? C21 C77 1.318(14) . ? C21 C78 1.331(14) . ? C21 C91 1.454(13) . ? C21 C70 1.493(13) . ? C21 H215 0.9500 . ? C21 H216 0.9500 . ? C22 C49 1.40(3) . ? C22 C33 1.49(3) . ? C23 C40 1.40(2) . ? C23 C26 1.45(2) . ? C23 C152 1.51(3) . ? C24 C44 1.37(2) . ? C24 C25 1.407(19) . ? C24 C126 1.57(2) . ? C25 C37 1.35(2) . ? C26 C31 1.43(2) . ? C26 C58 1.61(3) . ? C27 C28 1.40(3) . ? C27 C59 1.42(3) . ? C27 C64 1.58(3) . ? C28 C57 1.41(3) . ? C29 C35 1.38(4) . ? C29 C49 1.41(3) . ? C29 H59 0.9500 . ? C30 C35 1.37(4) . ? C30 C48 1.52(3) . ? C31 C39 1.39(2) . ? C31 H60 0.9500 . ? C32 C80 1.396(19) . ? C32 C34 1.42(2) . ? C32 C68 1.49(2) . ? C33 H61 0.9800 . ? C33 H62 0.9800 . ? C33 H63 0.9800 . ? C34 C54 1.45(2) . ? C34 C134 1.52(2) . ? C35 H64 0.9500 . ? C36 C62 1.373(11) . ? C36 H6 0.9500 . ? C37 C63 1.402(19) . ? C37 C73 1.46(2) . ? C38 C51 1.51(2) . ? C38 H17 0.9800 . ? C38 H18 0.9800 . ? C38 H19 0.9800 . ? C39 C50 1.36(3) . ? C39 H65 0.9500 . ? C40 C50 1.30(3) . ? C40 C46 1.40(3) . ? C41 C139 1.38(2) . ? C41 H66 0.9500 . ? C42 H7 0.9800 . ? C42 H8 0.9800 . ? C42 H9 0.9800 . ? C43 H10 0.9800 . ? C43 H11 0.9800 . ? C43 H12 0.9800 . ? C44 C52 1.35(2) . ? C44 H145 0.9500 . ? C45 C70 1.408(16) . ? C45 H20 0.9500 . ? C46 H67 0.9800 . ? C46 H68 0.9800 . ? C46 H69 0.9800 . ? C47 C99 1.35(2) . ? C47 C90 1.37(2) . ? C47 H21 0.9500 . ? C48 H70 0.9800 . ? C48 H71 0.9800 . ? C48 H72 0.9800 . ? C49 H73 0.9500 . ? C50 H74 0.9500 . ? C51 C87 1.39(2) . ? C51 C75 1.46(2) . ? C52 C63 1.36(2) . ? C52 H146 0.9500 . ? C53 C74 1.55(3) . ? C53 H22 0.9800 . ? C53 H23 0.9800 . ? C53 H24 0.9800 . ? C54 C82 1.36(2) . ? C54 C85 1.50(2) . ? C55 C65 1.330(17) . ? C55 H75 0.9500 . ? C56 C119 1.42(3) . ? C56 H147 0.9800 . ? C56 H148 0.9800 . ? C56 H149 0.9800 . ? C57 C83 1.33(3) . ? C57 C88 1.42(3) . ? C58 H76 0.9800 . ? C58 H77 0.9800 . ? C58 H78 0.9800 . ? C59 C81 1.35(3) . ? C59 H79 0.9500 . ? C60 C77 1.404(16) . ? C60 H25 0.9500 . ? C61 C62 1.378(12) . ? C61 H13 0.9500 . ? C62 H14 0.9500 . ? C63 H150 0.9500 . ? C64 H80 0.9800 . ? C64 H81 0.9800 . ? C64 H82 0.9800 . ? C65 H83 0.9500 . ? C66 C82 1.40(2) . ? C66 C80 1.46(2) . ? C66 H84 0.9500 . ? C67 C106 1.39(2) . ? C67 C72 1.416(18) . ? C67 C70 1.485(16) . ? C68 H85 0.9800 . ? C68 H86 0.9800 . ? C68 H87 0.9800 . ? C69 C91 1.438(16) . ? C69 H26 0.9500 . ? C71 C107 1.39(2) . ? C71 C103 1.412(19) . ? C71 C91 1.474(16) . ? C72 C96 1.38(2) . ? C72 C100 1.48(2) . ? C73 H151 0.9800 . ? C73 H152 0.9800 . ? C73 H153 0.9800 . ? C74 C79 1.34(4) . ? C74 C99 1.37(4) . ? C75 C97 1.398(18) . ? C75 C77 1.484(16) . ? C76 C78 1.405(17) . ? C76 H27 0.9500 . ? C78 C79 1.493(16) . ? C79 C84 1.413(18) . ? C80 H88 0.9500 . ? C81 C88 1.32(3) . ? C81 H89 0.9500 . ? C82 H90 0.9500 . ? C83 H91 0.9800 . ? C83 H92 0.9800 . ? C83 H93 0.9800 . ? C84 C90 1.392(18) . ? C84 C93 1.49(2) . ? C85 H94 0.9800 . ? C85 H95 0.9800 . ? C85 H96 0.9800 . ? C86 C89 1.37(2) . ? C86 C106 1.41(2) . ? C86 H28 0.9500 . ? C87 C94 1.41(2) . ? C87 H29 0.9500 . ? C88 H97 0.9500 . ? C89 C96 1.37(2) . ? C89 H30 0.9500 . ? C90 H31 0.9500 . ? C92 C94 1.32(2) . ? C92 C97 1.408(19) . ? C92 H32 0.9500 . ? C93 H33 0.9800 . ? C93 H34 0.9800 . ? C93 H35 0.9800 . ? C94 C102 1.81(2) 3_655 ? C94 C103 1.876(19) 3_655 ? C94 H36 0.9500 . ? C95 C101 1.37(3) . ? C95 C102 1.40(3) . ? C95 H37 0.9500 . ? C96 H38 0.9500 . ? C97 C104 1.46(2) . ? C98 C103 1.49(2) . ? C98 H39 0.9800 . ? C98 H40 0.9800 . ? C98 H41 0.9800 . ? C99 H42 0.9500 . ? C100 H43 0.9800 . ? C100 H44 0.9800 . ? C100 H45 0.9800 . ? C101 C107 1.38(2) . ? C101 H46 0.9500 . ? C102 C103 1.42(2) . ? C102 C94 1.81(2) 3_655 ? C102 H47 0.9500 . ? C103 C94 1.876(19) 3_655 ? C104 H48 0.9800 . ? C104 H49 0.9800 . ? C104 H50 0.9800 . ? C105 C107 1.46(3) . ? C105 H51 0.9800 . ? C105 H52 0.9800 . ? C105 H53 0.9800 . ? C106 C110 1.52(2) . ? C108 C116 1.29(3) . ? C108 C118 1.35(3) . ? C108 H98 0.9500 . ? C109 C113 1.327(19) . ? C109 N5 1.413(17) . ? C109 H99 0.9500 . ? C110 H54 0.9800 . ? C110 H55 0.9800 . ? C110 H56 0.9800 . ? C111 C114 1.52(2) . ? C111 H100 0.9800 . ? C111 H101 0.9800 . ? C111 H102 0.9800 . ? C112 C116 1.38(3) . ? C112 C114 1.46(2) . ? C112 H103 0.9500 . ? C113 N6 1.394(19) . ? C113 H104 0.9500 . ? C114 C115 1.40(2) . ? N5 C139 1.413(18) . ? C115 C118 1.34(2) . ? C115 C150 1.48(2) . ? C116 H105 0.9500 . ? C117 C118 1.49(3) . ? C117 H106 0.9800 . ? C117 H107 0.9800 . ? C117 H108 0.9800 . ? C119 C124 1.34(3) . ? C119 C122 1.37(3) . ? C120 C122 1.35(3) . ? C120 C121 1.40(3) . ? C120 H154 0.9500 . ? C121 C125 1.44(3) . ? C121 H155 0.9500 . ? C122 H156 0.9500 . ? C123 C125 1.59(3) . ? C123 H157 0.9800 . ? C123 H158 0.9800 . ? C123 H159 0.9800 . ? C124 C125 1.46(3) . ? C126 H160 0.9800 . ? C126 H161 0.9800 . ? C126 H162 0.9800 . ? C127 C129 1.63(3) . ? C127 H109 0.9800 . ? C127 H110 0.9800 . ? C127 H111 0.9800 . ? C128 C130 1.38(3) . ? C128 C129 1.45(3) . ? C128 C165 1.58(3) . ? C129 C137 1.39(3) . ? C130 C140 1.38(2) . ? C130 C131 1.49(3) . ? C131 H112 0.9800 . ? C131 H113 0.9800 . ? C131 H114 0.9800 . ? C132 C134 1.39(2) . ? C132 H115 0.9500 . ? C133 C134 1.36(2) . ? C133 H116 0.9500 . ? C135 C138 1.43(3) . ? C135 C147 1.63(3) . ? C136 C140 1.40(2) . ? C136 C137 1.40(3) . ? C136 H117 0.9500 . ? C137 H118 0.9500 . ? C138 C139 1.38(3) . ? C138 H119 0.9500 . ? C140 H120 0.9500 . ? C141 C142 1.32(4) . ? C141 C145 1.35(4) . ? C141 H121 0.9500 . ? C142 C146 1.35(3) . ? C142 H122 0.9500 . ? C143 C147 1.21(3) . ? C143 C145 1.46(3) . ? C143 C144 1.50(4) . ? C144 H123 0.9800 . ? C144 H124 0.9800 . ? C144 H125 0.9800 . ? C145 H126 0.9500 . ? C146 C148 1.51(3) . ? C146 C147 1.51(3) . ? C148 H127 0.9800 . ? C148 H128 0.9800 . ? C148 H129 0.9800 . ? C149 C154 1.36(3) . ? C149 C150 1.36(2) . ? C149 H130 0.9500 . ? C150 C151 1.41(2) . ? C151 C152 1.34(3) . ? C151 H131 0.9500 . ? C152 C153 1.40(3) . ? C153 C154 1.44(3) . ? C153 H132 0.9500 . ? C155 C156 1.42(2) . ? C155 C160 1.47(2) . ? C155 H163 0.9500 . ? C156 C157 1.40(2) . ? C156 H133 0.9500 . ? C157 C158 1.39(2) . ? C157 H134 0.9500 . ? C158 C159 1.38(3) . ? C158 C167 1.40(3) . ? C159 C160 1.40(2) . ? C160 C168 1.61(3) . ? C161 C162 1.37(2) . ? C161 C166 1.48(3) . ? C162 C163 1.36(2) . ? C162 H136 0.9500 . ? C163 C164 1.40(2) . ? C164 C165 1.43(3) . ? C164 H137 0.9500 . ? C165 C166 1.33(3) . ? C166 H138 0.9500 . ? C167 H139 0.9800 . ? C167 H140 0.9800 . ? C167 H141 0.9800 . ? C168 H142 0.9800 . ? C168 H143 0.9800 . ? C168 H144 0.9800 . ? C169 C170 1.557(17) . ? C169 H164 0.9800 . ? C169 H165 0.9800 . ? C169 H166 0.9800 . ? C170 C171 1.567(17) . ? C170 H167 0.9900 . ? C170 H168 0.9900 . ? C171 C172 1.545(16) . ? C171 H169 0.9900 . ? C171 H170 0.9900 . ? C172 C173 1.564(16) . ? C172 H171 0.9900 . ? C172 H172 0.9900 . ? C173 C174 1.547(17) . ? C173 H173 0.9900 . ? C173 H174 0.9900 . ? C174 H175 0.9800 . ? C174 H176 0.9800 . ? C174 H177 0.9800 . ? C175 C176 1.554(18) . ? C175 H178 0.9900 . ? C175 H179 0.9900 . ? C176 C179 1.52(2) . ? C176 H180 0.9900 . ? C176 H181 0.9900 . ? C177 C178 1.54(2) . ? C177 H182 0.9900 . ? C177 H183 0.9900 . ? C178 H184 0.9824 . ? C178 H185 0.9823 . ? C178 H186 0.9825 . ? C179 C180 1.56(2) . ? C179 H187 0.9900 . ? C179 H188 0.9900 . ? C180 H189 1.1227 . ? C180 H190 1.1074 . ? C180 H191 1.1125 . ? C187 C201 1.337(13) . ? C187 H206 0.9810 . ? C187 H207 0.9809 . ? C187 H208 0.9808 . ? C188 C189 1.46(4) . ? C188 H209 0.9824 . ? C188 H210 0.9821 . ? C188 H211 0.9822 . ? C189 C190 1.3900 . ? C189 C194 1.3900 . ? C190 C191 1.3900 . ? C190 H220 0.9500 . ? C191 C192 1.3900 . ? C191 H221 0.9500 . ? C192 C193 1.3900 . ? C192 H222 0.9500 . ? C193 C194 1.3900 . ? C193 H223 0.9500 . ? C194 H224 0.9500 . ? C195 C196 1.3900 . ? C195 C200 1.3900 . ? C195 H225 0.9500 . ? C196 C197 1.3900 . ? C196 H226 0.9500 . ? C197 C198 1.3900 . ? C197 H227 0.9500 . ? C198 C207 1.335(15) . ? C198 C199 1.3900 . ? C199 C200 1.3900 . ? C199 H228 0.9500 . ? C200 H229 0.9500 . ? C201 C202 1.3900 . ? C201 C206 1.3900 . ? C202 C203 1.3900 . ? C202 H230 0.9500 . ? C203 C204 1.3900 . ? C203 H231 0.9500 . ? C204 C205 1.3900 . ? C204 H232 0.9500 . ? C205 C206 1.3900 . ? C205 H233 0.9500 . ? C206 H234 0.9500 . ? C207 H217 0.9998 . ? C207 H218 1.0001 . ? C207 H219 0.9998 . ? 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 C1 Pd1 C5 175.6(2) . . ? C5 N1 C14 111.5(4) . . ? C5 N1 C2 124.4(4) . . ? C14 N1 C2 124.1(5) . . ? N4 C1 N6 101.5(8) . . ? N4 C1 N3 101.0(8) . . ? N6 C1 N3 14.0(8) . . ? N4 C1 N5 17.2(6) . . ? N6 C1 N5 101.8(8) . . ? N3 C1 N5 105.5(8) . . ? N4 C1 Pd1 128.7(6) . . ? N6 C1 Pd1 129.7(6) . . ? N3 C1 Pd1 127.6(6) . . ? N5 C1 Pd1 126.9(6) . . ? C6 C2 C11 121.1(5) . . ? C6 C2 N1 119.5(5) . . ? C11 C2 N1 119.3(5) . . ? C45 C3 C76 122.8(8) . . ? C45 C3 C69 98.9(8) . . ? C76 C3 C69 57.3(8) . . ? C45 C3 C60 54.8(7) . . ? C76 C3 C60 91.2(7) . . ? C69 C3 C60 120.8(8) . . ? C45 C3 N2 117.4(6) . . ? C76 C3 N2 119.6(7) . . ? C69 C3 N2 118.9(7) . . ? C60 C3 N2 120.3(6) . . ? C5 N2 C18 112.3(5) . . ? C5 N2 C3 124.1(5) . . ? C18 N2 C3 123.7(5) . . ? C16 C4 C11 119.5(5) . . ? C16 C4 C124 123.1(9) . . ? C11 C4 C124 117.1(9) . . ? C16 C4 C25 118.8(7) . . ? C11 C4 C25 121.2(7) . . ? C124 C4 C25 13.4(9) . . ? N2 C5 N1 102.7(4) . . ? N2 C5 Pd1 131.1(4) . . ? N1 C5 Pd1 126.1(4) . . ? C2 C6 C8 120.4(5) . . ? C2 C6 H1 119.8 . . ? C8 C6 H1 119.8 . . ? C17 C7 N6 121.6(16) . . ? C17 C7 C133 119.8(16) . . ? N6 C7 C133 118.5(14) . . ? C6 C8 C16 118.6(6) . . ? C6 C8 C9 119.0(5) . . ? C16 C8 C9 122.3(5) . . ? C20 C9 C15 121.0(6) . . ? C20 C9 C8 117.8(6) . . ? C15 C9 C8 121.1(6) . . ? C17 C10 C132 119.8(19) . . ? C17 C10 C159 119.5(18) . . ? C132 C10 C159 120.6(17) . . ? C4 C11 C2 119.0(5) . . ? C4 C11 H2 120.5 . . ? C2 C11 H2 120.5 . . ? C1 N3 C55 112.0(10) . . ? C1 N3 C154 125.8(11) . . ? C55 N3 C154 122.3(12) . . ? C22 C12 C161 122.7(19) . . ? C22 C12 C30 121.7(18) . . ? C161 C12 C30 115.5(17) . . ? C135 C13 C19 123(2) . . ? C135 C13 H57 118.6 . . ? C19 C13 H57 118.6 . . ? C18 C14 N1 106.5(5) . . ? C18 C14 H3 126.7 . . ? N1 C14 H3 126.7 . . ? C36 C15 C9 118.7(7) . . ? C36 C15 C42 120.2(7) . . ? C9 C15 C42 121.0(6) . . ? C4 C16 C8 121.3(5) . . ? C4 C16 H4 119.3 . . ? C8 C16 H4 119.3 . . ? C7 C17 C10 121(2) . . ? C7 C17 H58 119.3 . . ? C10 C17 H58 119.3 . . ? C14 C18 N2 107.0(5) . . ? C14 C18 H5 126.5 . . ? N2 C18 H5 126.5 . . ? C41 C19 C13 118.5(19) . . ? C41 C19 C28 123(2) . . ? C13 C19 C28 117.7(19) . . ? C9 C20 C61 118.5(7) . . ? C9 C20 C43 121.5(6) . . ? C61 C20 C43 120.0(7) . . ? C1 N4 C65 113.3(9) . . ? C1 N4 C163 125.8(10) . . ? C65 N4 C163 120.8(10) . . ? C77 C21 C78 91.4(9) . . ? C77 C21 C91 123.6(9) . . ? C78 C21 C91 56.8(8) . . ? C77 C21 C70 56.8(8) . . ? C78 C21 C70 120.1(8) . . ? C91 C21 C70 97.5(8) . . ? C77 C21 H215 121.6 . . ? C78 C21 H215 119.9 . . ? C91 C21 H215 114.7 . . ? C70 C21 H215 119.9 . . ? C77 C21 H216 118.2 . . ? C78 C21 H216 123.6 . . ? C91 C21 H216 118.2 . . ? C70 C21 H216 116.3 . . ? H215 C21 H216 4.2 . . ? C12 C22 C49 119.8(19) . . ? C12 C22 C33 123.8(18) . . ? C49 C22 C33 116.4(18) . . ? C40 C23 C26 119.2(15) . . ? C40 C23 C152 122.6(16) . . ? C26 C23 C152 118.2(17) . . ? C44 C24 C25 121.4(14) . . ? C44 C24 C126 117.7(14) . . ? C25 C24 C126 120.6(13) . . ? C37 C25 C24 119.8(12) . . ? C37 C25 C4 123.5(11) . . ? C24 C25 C4 116.6(11) . . ? C31 C26 C23 116.6(16) . . ? C31 C26 C58 124.8(16) . . ? C23 C26 C58 118.3(16) . . ? C28 C27 C59 119.2(18) . . ? C28 C27 C64 122.3(16) . . ? C59 C27 C64 118.4(17) . . ? C27 C28 C57 121.8(18) . . ? C27 C28 C19 118.5(18) . . ? C57 C28 C19 119.7(18) . . ? C35 C29 C49 117(2) . . ? C35 C29 H59 121.5 . . ? C49 C29 H59 121.5 . . ? C35 C30 C48 126(2) . . ? C35 C30 C12 112(2) . . ? C48 C30 C12 121.9(18) . . ? C39 C31 C26 119.5(15) . . ? C39 C31 H60 120.3 . . ? C26 C31 H60 120.3 . . ? C80 C32 C34 115.6(15) . . ? C80 C32 C68 123.5(14) . . ? C34 C32 C68 120.9(12) . . ? C32 C34 C54 121.2(13) . . ? C32 C34 C134 117.6(14) . . ? C54 C34 C134 121.1(14) . . ? C30 C35 C29 126(2) . . ? C30 C35 H64 116.8 . . ? C29 C35 H64 116.8 . . ? C62 C36 C15 120.8(7) . . ? C62 C36 H6 119.6 . . ? C15 C36 H6 119.6 . . ? C25 C37 C63 116.8(13) . . ? C25 C37 C73 120.7(12) . . ? C63 C37 C73 122.5(13) . . ? C51 C38 H17 109.5 . . ? C51 C38 H18 109.5 . . ? H17 C38 H18 109.5 . . ? C51 C38 H19 109.5 . . ? H17 C38 H19 109.5 . . ? H18 C38 H19 109.5 . . ? C50 C39 C31 120.8(17) . . ? C50 C39 H65 119.6 . . ? C31 C39 H65 119.6 . . ? C50 C40 C23 121.4(18) . . ? C50 C40 C46 121(2) . . ? C23 C40 C46 117.8(17) . . ? C19 C41 C139 120.9(17) . . ? C19 C41 H66 119.6 . . ? C139 C41 H66 119.6 . . ? C15 C42 H7 109.5 . . ? C15 C42 H8 109.5 . . ? H7 C42 H8 109.5 . . ? C15 C42 H9 109.5 . . ? H7 C42 H9 109.5 . . ? H8 C42 H9 109.5 . . ? C20 C43 H10 109.5 . . ? C20 C43 H11 109.5 . . ? H10 C43 H11 109.5 . . ? C20 C43 H12 109.5 . . ? H10 C43 H12 109.5 . . ? H11 C43 H12 109.5 . . ? C52 C44 C24 118.9(14) . . ? C52 C44 H145 120.6 . . ? C24 C44 H145 120.6 . . ? C3 C45 C70 120.7(10) . . ? C3 C45 H20 119.7 . . ? C70 C45 H20 119.7 . . ? C99 C47 C90 120.5(14) . . ? C99 C47 H21 119.7 . . ? C90 C47 H21 119.8 . . ? C22 C49 C29 121.6(19) . . ? C22 C49 H73 119.2 . . ? C29 C49 H73 119.2 . . ? C40 C50 C39 123(2) . . ? C40 C50 H74 118.7 . . ? C39 C50 H74 118.7 . . ? C87 C51 C75 115.6(15) . . ? C87 C51 C38 121.4(16) . . ? C75 C51 C38 122.7(14) . . ? C44 C52 C63 119.7(13) . . ? C44 C52 H146 120.2 . . ? C63 C52 H146 120.2 . . ? C82 C54 C34 122.8(16) . . ? C82 C54 C85 114.7(16) . . ? C34 C54 C85 122.4(15) . . ? C65 C55 N3 105.9(11) . . ? C65 C55 H75 127.0 . . ? N3 C55 H75 127.0 . . ? C119 C56 H147 109.5 . . ? C119 C56 H148 109.5 . . ? H147 C56 H148 109.5 . . ? C119 C56 H149 109.5 . . ? H147 C56 H149 109.5 . . ? H148 C56 H149 109.5 . . ? C83 C57 C28 126(2) . . ? C83 C57 C88 120(2) . . ? C28 C57 C88 114(2) . . ? C81 C59 C27 117.9(18) . . ? C81 C59 H79 121.1 . . ? C27 C59 H79 121.1 . . ? C3 C60 C77 120.3(10) . . ? C3 C60 H25 119.9 . . ? C77 C60 H25 119.8 . . ? C62 C61 C20 120.7(7) . . ? C62 C61 H13 119.7 . . ? C20 C61 H13 119.6 . . ? C36 C62 C61 120.2(7) . . ? C36 C62 H14 119.9 . . ? C61 C62 H14 119.9 . . ? C52 C63 C37 123.3(13) . . ? C52 C63 H150 118.4 . . ? C37 C63 H150 118.4 . . ? C27 C64 H80 109.5 . . ? C27 C64 H81 109.5 . . ? H80 C64 H81 109.5 . . ? C27 C64 H82 109.5 . . ? H80 C64 H82 109.5 . . ? H81 C64 H82 109.5 . . ? C55 C65 N4 107.1(10) . . ? C55 C65 H83 126.4 . . ? N4 C65 H83 126.4 . . ? C82 C66 C80 120.9(14) . . ? C82 C66 H84 119.5 . . ? C80 C66 H84 119.6 . . ? C106 C67 C72 123.0(13) . . ? C106 C67 C70 118.5(12) . . ? C72 C67 C70 118.4(11) . . ? C32 C68 H85 109.5 . . ? C32 C68 H86 109.5 . . ? H85 C68 H86 109.5 . . ? C32 C68 H87 109.5 . . ? H85 C68 H87 109.5 . . ? H86 C68 H87 109.5 . . ? C3 C69 C91 120.5(10) . . ? C3 C69 H26 119.8 . . ? C91 C69 H26 119.8 . . ? C45 C70 C67 118.4(10) . . ? C45 C70 C21 115.8(10) . . ? C67 C70 C21 125.7(9) . . ? C107 C71 C103 121.3(13) . . ? C107 C71 C91 120.8(13) . . ? C103 C71 C91 117.9(12) . . ? C96 C72 C67 116.2(13) . . ? C96 C72 C100 122.1(13) . . ? C67 C72 C100 121.7(11) . . ? C79 C74 C99 125(2) . . ? C79 C74 C53 118(2) . . ? C99 C74 C53 117(2) . . ? C97 C75 C51 122.4(12) . . ? C97 C75 C77 120.2(11) . . ? C51 C75 C77 117.4(12) . . ? C3 C76 C78 119.1(10) . . ? C3 C76 H27 120.4 . . ? C78 C76 H27 120.4 . . ? C21 C77 C60 119.4(10) . . ? C21 C77 C75 119.4(10) . . ? C60 C77 C75 121.1(11) . . ? C21 C78 C76 121.2(10) . . ? C21 C78 C79 117.9(10) . . ? C76 C78 C79 120.9(11) . . ? C74 C79 C84 117.8(18) . . ? C74 C79 C78 124.0(17) . . ? C84 C79 C78 118.2(12) . . ? C32 C80 C66 122.2(14) . . ? C32 C80 H88 118.9 . . ? C66 C80 H88 118.9 . . ? C88 C81 C59 123(2) . . ? C88 C81 H89 118.4 . . ? C59 C81 H89 118.4 . . ? C54 C82 C66 117.2(16) . . ? C54 C82 H90 121.4 . . ? C66 C82 H90 121.4 . . ? C57 C83 H91 109.5 . . ? C57 C83 H92 109.5 . . ? H91 C83 H92 109.5 . . ? C57 C83 H93 109.5 . . ? H91 C83 H93 109.5 . . ? H92 C83 H93 109.5 . . ? C90 C84 C79 117.3(14) . . ? C90 C84 C93 120.9(13) . . ? C79 C84 C93 121.8(12) . . ? C54 C85 H94 109.5 . . ? C54 C85 H95 109.5 . . ? H94 C85 H95 109.5 . . ? C54 C85 H96 109.4 . . ? H94 C85 H96 109.5 . . ? H95 C85 H96 109.5 . . ? C89 C86 C106 122.7(15) . . ? C89 C86 H28 118.7 . . ? C106 C86 H28 118.7 . . ? C51 C87 C94 121.3(15) . . ? C51 C87 H29 119.4 . . ? C94 C87 H29 119.3 . . ? C81 C88 C57 123(2) . . ? C81 C88 H97 118.4 . . ? C57 C88 H97 118.4 . . ? C86 C89 C96 118.3(13) . . ? C86 C89 H30 120.8 . . ? C96 C89 H30 120.9 . . ? C47 C90 C84 121.9(14) . . ? C47 C90 H31 119.0 . . ? C84 C90 H31 119.0 . . ? C69 C91 C21 115.2(10) . . ? C69 C91 C71 123.4(11) . . ? C21 C91 C71 121.3(10) . . ? C94 C92 C97 123.6(15) . . ? C94 C92 H32 118.2 . . ? C97 C92 H32 118.2 . . ? C92 C94 C87 120.6(13) . . ? C92 C94 C102 130.3(15) . 3_655 ? C87 C94 C102 109.1(13) . 3_655 ? C92 C94 C103 118.6(13) . 3_655 ? C87 C94 C103 99.7(11) . 3_655 ? C102 C94 C103 45.1(7) 3_655 3_655 ? C92 C94 H36 119.7 . . ? C87 C94 H36 119.7 . . ? C102 C94 H36 10.9 3_655 . ? C103 C94 H36 49.1 3_655 . ? C101 C95 C102 119.4(14) . . ? C101 C95 H37 120.3 . . ? C102 C95 H37 120.3 . . ? C89 C96 C72 123.4(15) . . ? C89 C96 H38 118.3 . . ? C72 C96 H38 118.3 . . ? C75 C97 C92 116.4(13) . . ? C75 C97 C104 121.0(12) . . ? C92 C97 C104 122.4(14) . . ? C103 C98 H39 109.5 . . ? C103 C98 H40 109.5 . . ? H39 C98 H40 109.5 . . ? C103 C98 H41 109.5 . . ? H39 C98 H41 109.5 . . ? H40 C98 H41 109.5 . . ? C47 C99 C74 117.4(19) . . ? C47 C99 H42 121.3 . . ? C74 C99 H42 121.3 . . ? C95 C101 C107 122.2(17) . . ? C95 C101 H46 118.9 . . ? C107 C101 H46 118.9 . . ? C95 C102 C103 120.7(15) . . ? C95 C102 C94 112.8(14) . 3_655 ? C103 C102 C94 69.8(10) . 3_655 ? C95 C102 H47 119.6 . . ? C103 C102 H47 119.6 . . ? C94 C102 H47 87.6 3_655 . ? C71 C103 C102 117.4(15) . . ? C71 C103 C98 122.0(13) . . ? C102 C103 C98 120.6(14) . . ? C71 C103 C94 112.8(11) . 3_655 ? C102 C103 C94 65.2(9) . 3_655 ? C98 C103 C94 91.5(12) . 3_655 ? C97 C104 H48 109.5 . . ? C97 C104 H49 109.6 . . ? H48 C104 H49 109.5 . . ? C97 C104 H50 109.3 . . ? H48 C104 H50 109.5 . . ? H49 C104 H50 109.5 . . ? C107 C105 H51 109.5 . . ? C107 C105 H52 109.4 . . ? H51 C105 H52 109.5 . . ? C107 C105 H53 109.5 . . ? H51 C105 H53 109.5 . . ? H52 C105 H53 109.5 . . ? C67 C106 C86 116.3(16) . . ? C67 C106 C110 121.6(14) . . ? C86 C106 C110 122.1(15) . . ? C101 C107 C71 118.8(16) . . ? C101 C107 C105 121.4(18) . . ? C71 C107 C105 119.3(16) . . ? C116 C108 C118 120(2) . . ? C116 C108 H98 120.0 . . ? C118 C108 H98 120.0 . . ? C113 C109 N5 106.5(12) . . ? C113 C109 H99 126.7 . . ? N5 C109 H99 126.7 . . ? C116 C112 C114 112.9(17) . . ? C116 C112 H103 123.6 . . ? C114 C112 H103 123.6 . . ? C109 C113 N6 107.2(12) . . ? C109 C113 H104 126.4 . . ? N6 C113 H104 126.4 . . ? C115 C114 C112 118.6(16) . . ? C115 C114 C111 123.2(13) . . ? C112 C114 C111 118.2(15) . . ? C1 N5 C139 124.8(10) . . ? C1 N5 C109 111.2(10) . . ? C139 N5 C109 122.8(11) . . ? C118 C115 C114 121.4(15) . . ? C118 C115 C150 120.5(15) . . ? C114 C115 C150 118.1(15) . . ? C108 C116 C112 127(2) . . ? C108 C116 H105 116.5 . . ? C112 C116 H105 116.5 . . ? C115 C118 C108 120(2) . . ? C115 C118 C117 120.8(16) . . ? C108 C118 C117 119(2) . . ? C1 N6 C113 112.2(11) . . ? C1 N6 C7 121.1(11) . . ? C113 N6 C7 125.9(12) . . ? C124 C119 C122 121(2) . . ? C124 C119 C56 117.6(17) . . ? C122 C119 C56 122(2) . . ? C122 C120 C121 123(2) . . ? C122 C120 H154 118.7 . . ? C121 C120 H154 118.7 . . ? C120 C121 C125 117(2) . . ? C120 C121 H155 121.3 . . ? C125 C121 H155 121.3 . . ? C120 C122 C119 121(2) . . ? C120 C122 H156 119.4 . . ? C119 C122 H156 119.4 . . ? C125 C123 H157 109.5 . . ? C125 C123 H158 109.5 . . ? H157 C123 H158 109.5 . . ? C125 C123 H159 109.5 . . ? H157 C123 H159 109.5 . . ? H158 C123 H159 109.5 . . ? C119 C124 C125 120.8(19) . . ? C119 C124 C4 127.3(17) . . ? C125 C124 C4 111.9(17) . . ? C121 C125 C124 117.5(19) . . ? C121 C125 C123 118.6(18) . . ? C124 C125 C123 123.8(18) . . ? C130 C128 C129 123.4(17) . . ? C130 C128 C165 121.0(16) . . ? C129 C128 C165 115.5(17) . . ? C137 C129 C128 115.9(18) . . ? C137 C129 C127 124.1(19) . . ? C128 C129 C127 118.9(17) . . ? C140 C130 C128 117.6(17) . . ? C140 C130 C131 123.2(17) . . ? C128 C130 C131 119.1(16) . . ? C134 C132 C10 118.9(17) . . ? C134 C132 H115 120.5 . . ? C10 C132 H115 120.5 . . ? C134 C133 C7 119.5(15) . . ? C134 C133 H116 120.2 . . ? C7 C133 H116 120.2 . . ? C133 C134 C132 120.3(16) . . ? C133 C134 C34 120.0(15) . . ? C132 C134 C34 119.6(15) . . ? C13 C135 C138 119(2) . . ? C13 C135 C147 125(2) . . ? C138 C135 C147 115.5(19) . . ? C140 C136 C137 118.9(16) . . ? C140 C136 H117 120.6 . . ? C137 C136 H117 120.6 . . ? C129 C137 C136 122.0(18) . . ? C129 C137 H118 119.0 . . ? C136 C137 H118 119.0 . . ? C139 C138 C135 120.6(18) . . ? C139 C138 H119 119.7 . . ? C135 C138 H119 119.7 . . ? C41 C139 C138 118.0(15) . . ? C41 C139 N5 123.4(14) . . ? C138 C139 N5 118.5(15) . . ? C130 C140 C136 122.1(16) . . ? C130 C140 H120 118.9 . . ? C136 C140 H120 119.0 . . ? C142 C141 C145 123(3) . . ? C142 C141 H121 118.6 . . ? C145 C141 H121 118.6 . . ? C141 C142 C146 120(2) . . ? C141 C142 H122 119.9 . . ? C146 C142 H122 120.0 . . ? C147 C143 C145 124(3) . . ? C147 C143 C144 122(3) . . ? C145 C143 C144 114(2) . . ? C143 C144 H123 109.5 . . ? C143 C144 H124 109.5 . . ? H123 C144 H124 109.5 . . ? C143 C144 H125 109.5 . . ? H123 C144 H125 109.5 . . ? H124 C144 H125 109.5 . . ? C141 C145 C143 116(2) . . ? C141 C145 H126 122.0 . . ? C143 C145 H126 122.0 . . ? C142 C146 C148 122(2) . . ? C142 C146 C147 119(2) . . ? C148 C146 C147 119(2) . . ? C143 C147 C146 117(2) . . ? C143 C147 C135 124(2) . . ? C146 C147 C135 118(2) . . ? C146 C148 H127 109.5 . . ? C146 C148 H128 109.5 . . ? H127 C148 H128 109.5 . . ? C146 C148 H129 109.5 . . ? H127 C148 H129 109.5 . . ? H128 C148 H129 109.5 . . ? C154 C149 C150 120.8(17) . . ? C154 C149 H130 119.6 . . ? C150 C149 H130 119.6 . . ? C149 C150 C151 120.2(15) . . ? C149 C150 C115 119.3(15) . . ? C151 C150 C115 120.0(14) . . ? C152 C151 C150 120.4(17) . . ? C152 C151 H131 119.8 . . ? C150 C151 H131 119.8 . . ? C151 C152 C153 120(2) . . ? C151 C152 C23 123.7(19) . . ? C153 C152 C23 115.6(19) . . ? C152 C153 C154 118(2) . . ? C152 C153 H132 120.9 . . ? C154 C153 H132 120.9 . . ? C149 C154 N3 122.8(16) . . ? C149 C154 C153 119.6(18) . . ? N3 C154 C153 117.4(17) . . ? C156 C155 C160 116.4(16) . . ? C156 C155 H163 121.8 . . ? C160 C155 H163 121.8 . . ? C157 C156 C155 122.8(14) . . ? C157 C156 H133 118.6 . . ? C155 C156 H133 118.6 . . ? C158 C157 C156 119.9(15) . . ? C158 C157 H134 120.1 . . ? C156 C157 H134 120.1 . . ? C159 C158 C157 119.1(18) . . ? C159 C158 C167 124.2(18) . . ? C157 C158 C167 116.6(18) . . ? C158 C159 C160 123.7(16) . . ? C158 C159 C10 120.8(17) . . ? C160 C159 C10 115.5(16) . . ? C159 C160 C155 118.0(16) . . ? C159 C160 C168 122.9(18) . . ? C155 C160 C168 119.1(19) . . ? C162 C161 C12 123.8(17) . . ? C162 C161 C166 118.1(17) . . ? C12 C161 C166 117.5(17) . . ? C163 C162 C161 120.3(16) . . ? C163 C162 H136 119.9 . . ? C161 C162 H136 119.9 . . ? C162 C163 C164 122.6(14) . . ? C162 C163 N4 120.1(13) . . ? C164 C163 N4 117.2(13) . . ? C163 C164 C165 117.6(15) . . ? C163 C164 H137 121.2 . . ? C165 C164 H137 121.2 . . ? C166 C165 C164 121(2) . . ? C166 C165 C128 120(2) . . ? C164 C165 C128 119.5(18) . . ? C165 C166 C161 120(2) . . ? C165 C166 H138 119.9 . . ? C161 C166 H138 119.9 . . ? C158 C167 H139 109.5 . . ? C158 C167 H140 109.5 . . ? H139 C167 H140 109.5 . . ? C158 C167 H141 109.5 . . ? H139 C167 H141 109.5 . . ? H140 C167 H141 109.5 . . ? C160 C168 H142 109.5 . . ? C160 C168 H143 109.5 . . ? H142 C168 H143 109.5 . . ? C160 C168 H144 109.5 . . ? H142 C168 H144 109.5 . . ? H143 C168 H144 109.5 . . ? C169 C170 C171 110.4(15) . . ? C169 C170 H167 109.5 . . ? C171 C170 H167 109.5 . . ? C169 C170 H168 109.6 . . ? C171 C170 H168 109.6 . . ? H167 C170 H168 108.1 . . ? C172 C171 C170 108.7(14) . . ? C172 C171 H169 110.0 . . ? C170 C171 H169 110.0 . . ? C172 C171 H170 109.9 . . ? C170 C171 H170 109.9 . . ? H169 C171 H170 108.3 . . ? C171 C172 C173 108.3(13) . . ? C171 C172 H171 110.0 . . ? C173 C172 H171 110.0 . . ? C171 C172 H172 110.1 . . ? C173 C172 H172 110.0 . . ? H171 C172 H172 108.4 . . ? C174 C173 C172 108.4(15) . . ? C174 C173 H173 110.1 . . ? C172 C173 H173 110.0 . . ? C174 C173 H174 109.9 . . ? C172 C173 H174 110.0 . . ? H173 C173 H174 108.4 . . ? C176 C175 H178 110.6 . . ? C176 C175 H179 110.9 . . ? H178 C175 H179 108.8 . . ? C179 C176 C175 114(2) . . ? C179 C176 H180 108.9 . . ? C175 C176 H180 108.6 . . ? C179 C176 H181 108.5 . . ? C175 C176 H181 108.9 . . ? H180 C176 H181 107.6 . . ? C178 C177 H182 110.1 . . ? C178 C177 H183 109.9 . . ? H182 C177 H183 108.2 . . ? C176 C179 C180 111(2) . . ? C176 C179 H187 109.4 . . ? C180 C179 H187 108.8 . . ? C176 C179 H188 109.7 . . ? C180 C179 H188 109.9 . . ? H187 C179 H188 108.1 . . ? C201 C187 H206 110.0 . . ? C201 C187 H207 109.8 . . ? H206 C187 H207 109.4 . . ? C201 C187 H208 108.9 . . ? H206 C187 H208 109.3 . . ? H207 C187 H208 109.4 . . ? C190 C189 C194 120.0 . . ? C190 C189 C188 118.2(19) . . ? C194 C189 C188 121.8(19) . . ? C191 C190 C189 120.0 . . ? C191 C190 H220 120.0 . . ? C189 C190 H220 120.0 . . ? C190 C191 C192 120.0 . . ? C190 C191 H221 120.0 . . ? C192 C191 H221 120.0 . . ? C193 C192 C191 120.0 . . ? C193 C192 H222 120.0 . . ? C191 C192 H222 120.0 . . ? C192 C193 C194 120.0 . . ? C192 C193 H223 120.0 . . ? C194 C193 H223 120.0 . . ? C193 C194 C189 120.0 . . ? C193 C194 H224 120.0 . . ? C189 C194 H224 120.0 . . ? C196 C195 C200 120.0 . . ? C196 C195 H225 119.9 . . ? C200 C195 H225 120.1 . . ? C195 C196 C197 120.0 . . ? C195 C196 H226 120.0 . . ? C197 C196 H226 120.0 . . ? C198 C197 C196 120.0 . . ? C198 C197 H227 120.0 . . ? C196 C197 H227 120.0 . . ? C207 C198 C197 118.7(14) . . ? C207 C198 C199 118.6(15) . . ? C197 C198 C199 120.0 . . ? C200 C199 C198 120.0 . . ? C200 C199 H228 120.0 . . ? C198 C199 H228 120.0 . . ? C199 C200 C195 120.0 . . ? C199 C200 H229 120.0 . . ? C195 C200 H229 120.0 . . ? C187 C201 C202 120.2(11) . . ? C187 C201 C206 119.4(11) . . ? C202 C201 C206 120.0 . . ? C203 C202 C201 120.0 . . ? C203 C202 H230 120.0 . . ? C201 C202 H230 120.0 . . ? C202 C203 C204 120.0 . . ? C202 C203 H231 120.0 . . ? C204 C203 H231 120.0 . . ? C203 C204 C205 120.0 . . ? C203 C204 H232 120.0 . . ? C205 C204 H232 120.0 . . ? C206 C205 C204 120.0 . . ? C206 C205 H233 120.0 . . ? C204 C205 H233 120.0 . . ? C205 C206 C201 120.0 . . ? C205 C206 H234 120.0 . . ? C201 C206 H234 120.0 . . ? 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 C5 Pd1 C1 N4 68(3) . . . . ? C5 Pd1 C1 N6 -107(3) . . . . ? C5 Pd1 C1 N3 -89(3) . . . . ? C5 Pd1 C1 N5 90(3) . . . . ? C5 N1 C2 C6 -38.0(8) . . . . ? C14 N1 C2 C6 143.1(6) . . . . ? C5 N1 C2 C11 139.9(6) . . . . ? C14 N1 C2 C11 -39.1(8) . . . . ? C45 C3 N2 C5 35.4(9) . . . . ? C76 C3 N2 C5 -150.2(8) . . . . ? C69 C3 N2 C5 -83.6(9) . . . . ? C60 C3 N2 C5 98.7(8) . . . . ? C45 C3 N2 C18 -144.3(7) . . . . ? C76 C3 N2 C18 30.0(10) . . . . ? C69 C3 N2 C18 96.7(8) . . . . ? C60 C3 N2 C18 -81.0(9) . . . . ? C18 N2 C5 N1 -0.2(6) . . . . ? C3 N2 C5 N1 -180.0(5) . . . . ? C18 N2 C5 Pd1 176.2(4) . . . . ? C3 N2 C5 Pd1 -3.6(8) . . . . ? C14 N1 C5 N2 -0.2(6) . . . . ? C2 N1 C5 N2 -179.3(5) . . . . ? C14 N1 C5 Pd1 -176.9(4) . . . . ? C2 N1 C5 Pd1 4.1(8) . . . . ? C1 Pd1 C5 N2 -167(3) . . . . ? C1 Pd1 C5 N1 8(3) . . . . ? C11 C2 C6 C8 -2.7(9) . . . . ? N1 C2 C6 C8 175.1(5) . . . . ? C2 C6 C8 C16 2.8(9) . . . . ? C2 C6 C8 C9 -174.2(5) . . . . ? C6 C8 C9 C20 82.4(8) . . . . ? C16 C8 C9 C20 -94.4(7) . . . . ? C6 C8 C9 C15 -95.6(7) . . . . ? C16 C8 C9 C15 87.5(8) . . . . ? C16 C4 C11 C2 1.8(9) . . . . ? C124 C4 C11 C2 -171.7(11) . . . . ? C25 C4 C11 C2 173.8(8) . . . . ? C6 C2 C11 C4 0.3(9) . . . . ? N1 C2 C11 C4 -177.5(5) . . . . ? N4 C1 N3 C55 8.2(13) . . . . ? N6 C1 N3 C55 -85(4) . . . . ? N5 C1 N3 C55 -8.8(14) . . . . ? Pd1 C1 N3 C55 170.7(8) . . . . ? N4 C1 N3 C154 -171.5(14) . . . . ? N6 C1 N3 C154 95(4) . . . . ? N5 C1 N3 C154 171.5(14) . . . . ? Pd1 C1 N3 C154 -9.0(19) . . . . ? C5 N1 C14 C18 0.5(7) . . . . ? C2 N1 C14 C18 179.6(6) . . . . ? C20 C9 C15 C36 -1.9(10) . . . . ? C8 C9 C15 C36 176.1(6) . . . . ? C20 C9 C15 C42 179.8(7) . . . . ? C8 C9 C15 C42 -2.2(10) . . . . ? C11 C4 C16 C8 -1.6(10) . . . . ? C124 C4 C16 C8 171.5(11) . . . . ? C25 C4 C16 C8 -173.7(8) . . . . ? C6 C8 C16 C4 -0.7(9) . . . . ? C9 C8 C16 C4 176.2(6) . . . . ? N6 C7 C17 C10 177.7(18) . . . . ? C133 C7 C17 C10 -2(3) . . . . ? C132 C10 C17 C7 3(3) . . . . ? C159 C10 C17 C7 179.3(19) . . . . ? N1 C14 C18 N2 -0.6(7) . . . . ? C5 N2 C18 C14 0.5(7) . . . . ? C3 N2 C18 C14 -179.7(5) . . . . ? C135 C13 C19 C41 7(4) . . . . ? C135 C13 C19 C28 -179(2) . . . . ? C15 C9 C20 C61 2.8(10) . . . . ? C8 C9 C20 C61 -175.3(6) . . . . ? C15 C9 C20 C43 -176.8(6) . . . . ? C8 C9 C20 C43 5.2(9) . . . . ? N6 C1 N4 C65 6.0(13) . . . . ? N3 C1 N4 C65 -8.3(13) . . . . ? N5 C1 N4 C65 99(3) . . . . ? Pd1 C1 N4 C65 -170.5(8) . . . . ? N6 C1 N4 C163 -171.7(13) . . . . ? N3 C1 N4 C163 174.0(13) . . . . ? N5 C1 N4 C163 -79(3) . . . . ? Pd1 C1 N4 C163 11.7(17) . . . . ? C161 C12 C22 C49 -176.4(18) . . . . ? C30 C12 C22 C49 1(3) . . . . ? C161 C12 C22 C33 1(3) . . . . ? C30 C12 C22 C33 178.4(19) . . . . ? C44 C24 C25 C37 3(2) . . . . ? C126 C24 C25 C37 177.7(13) . . . . ? C44 C24 C25 C4 -179.0(11) . . . . ? C126 C24 C25 C4 -4.7(18) . . . . ? C16 C4 C25 C37 74.9(14) . . . . ? C11 C4 C25 C37 -97.1(13) . . . . ? C124 C4 C25 C37 -173(5) . . . . ? C16 C4 C25 C24 -102.5(12) . . . . ? C11 C4 C25 C24 85.5(12) . . . . ? C124 C4 C25 C24 10(4) . . . . ? C40 C23 C26 C31 2(2) . . . . ? C152 C23 C26 C31 179.0(15) . . . . ? C40 C23 C26 C58 176.2(16) . . . . ? C152 C23 C26 C58 -7(2) . . . . ? C59 C27 C28 C57 4(3) . . . . ? C64 C27 C28 C57 -178.6(18) . . . . ? C59 C27 C28 C19 -178.0(17) . . . . ? C64 C27 C28 C19 0(3) . . . . ? C41 C19 C28 C27 -77(3) . . . . ? C13 C19 C28 C27 109(2) . . . . ? C41 C19 C28 C57 101(3) . . . . ? C13 C19 C28 C57 -72(3) . . . . ? C22 C12 C30 C35 8(3) . . . . ? C161 C12 C30 C35 -175(2) . . . . ? C22 C12 C30 C48 -176.5(19) . . . . ? C161 C12 C30 C48 1(3) . . . . ? C23 C26 C31 C39 -2(2) . . . . ? C58 C26 C31 C39 -175.2(16) . . . . ? C80 C32 C34 C54 -0.6(19) . . . . ? C68 C32 C34 C54 179.1(13) . . . . ? C80 C32 C34 C134 -178.3(13) . . . . ? C68 C32 C34 C134 1.4(19) . . . . ? C48 C30 C35 C29 170(2) . . . . ? C12 C30 C35 C29 -15(4) . . . . ? C49 C29 C35 C30 13(4) . . . . ? C9 C15 C36 C62 0.1(11) . . . . ? C42 C15 C36 C62 178.4(8) . . . . ? C24 C25 C37 C63 -1(2) . . . . ? C4 C25 C37 C63 -178.1(11) . . . . ? C24 C25 C37 C73 177.6(13) . . . . ? C4 C25 C37 C73 0(2) . . . . ? C26 C31 C39 C50 1(2) . . . . ? C26 C23 C40 C50 -2(3) . . . . ? C152 C23 C40 C50 -178.4(19) . . . . ? C26 C23 C40 C46 176.9(17) . . . . ? C152 C23 C40 C46 0(3) . . . . ? C13 C19 C41 C139 -6(3) . . . . ? C28 C19 C41 C139 -179.0(18) . . . . ? C25 C24 C44 C52 -4(2) . . . . ? C126 C24 C44 C52 -177.9(13) . . . . ? C76 C3 C45 C70 5.4(15) . . . . ? C69 C3 C45 C70 -51.3(12) . . . . ? C60 C3 C45 C70 70.3(11) . . . . ? N2 C3 C45 C70 179.6(9) . . . . ? C12 C22 C49 C29 -4(3) . . . . ? C33 C22 C49 C29 178.1(19) . . . . ? C35 C29 C49 C22 -2(3) . . . . ? C23 C40 C50 C39 1(3) . . . . ? C46 C40 C50 C39 -177.9(19) . . . . ? C31 C39 C50 C40 0(3) . . . . ? C24 C44 C52 C63 1(2) . . . . ? C32 C34 C54 C82 0(2) . . . . ? C134 C34 C54 C82 177.7(15) . . . . ? C32 C34 C54 C85 -177.4(15) . . . . ? C134 C34 C54 C85 0(2) . . . . ? C1 N3 C55 C65 -5.4(16) . . . . ? C154 N3 C55 C65 174.3(14) . . . . ? C27 C28 C57 C83 180(2) . . . . ? C19 C28 C57 C83 2(3) . . . . ? C27 C28 C57 C88 -6(3) . . . . ? C19 C28 C57 C88 176.2(19) . . . . ? C28 C27 C59 C81 0(3) . . . . ? C64 C27 C59 C81 -177.9(17) . . . . ? C45 C3 C60 C77 -78.4(12) . . . . ? C76 C3 C60 C77 51.9(12) . . . . ? C69 C3 C60 C77 0.0(15) . . . . ? N2 C3 C60 C77 177.7(9) . . . . ? C9 C20 C61 C62 -1.9(11) . . . . ? C43 C20 C61 C62 177.7(7) . . . . ? C15 C36 C62 C61 0.7(12) . . . . ? C20 C61 C62 C36 0.2(12) . . . . ? C44 C52 C63 C37 2(2) . . . . ? C25 C37 C63 C52 -2(2) . . . . ? C73 C37 C63 C52 179.7(14) . . . . ? N3 C55 C65 N4 0.1(16) . . . . ? C1 N4 C65 C55 5.5(16) . . . . ? C163 N4 C65 C55 -176.6(13) . . . . ? C45 C3 C69 C91 54.8(12) . . . . ? C76 C3 C69 C91 -68.6(11) . . . . ? C60 C3 C69 C91 0.7(15) . . . . ? N2 C3 C69 C91 -177.0(9) . . . . ? C3 C45 C70 C67 179.5(10) . . . . ? C3 C45 C70 C21 -2.4(15) . . . . ? C106 C67 C70 C45 99.9(14) . . . . ? C72 C67 C70 C45 -77.1(15) . . . . ? C106 C67 C70 C21 -78.0(16) . . . . ? C72 C67 C70 C21 105.0(13) . . . . ? C77 C21 C70 C45 -72.6(11) . . . . ? C78 C21 C70 C45 -2.8(14) . . . . ? C91 C21 C70 C45 53.0(12) . . . . ? C77 C21 C70 C67 105.4(14) . . . . ? C78 C21 C70 C67 175.2(11) . . . . ? C91 C21 C70 C67 -129.1(12) . . . . ? C106 C67 C72 C96 -2.1(19) . . . . ? C70 C67 C72 C96 174.7(12) . . . . ? C106 C67 C72 C100 178.0(13) . . . . ? C70 C67 C72 C100 -5.1(18) . . . . ? C87 C51 C75 C97 3(2) . . . . ? C38 C51 C75 C97 177.0(14) . . . . ? C87 C51 C75 C77 -175.7(12) . . . . ? C38 C51 C75 C77 -2(2) . . . . ? C45 C3 C76 C78 -3.1(16) . . . . ? C69 C3 C76 C78 75.6(12) . . . . ? C60 C3 C76 C78 -50.9(12) . . . . ? N2 C3 C76 C78 -177.2(9) . . . . ? C78 C21 C77 C60 -55.3(12) . . . . ? C91 C21 C77 C60 -5.2(16) . . . . ? C70 C21 C77 C60 70.4(12) . . . . ? C78 C21 C77 C75 127.5(12) . . . . ? C91 C21 C77 C75 177.6(10) . . . . ? C70 C21 C77 C75 -106.8(13) . . . . ? C3 C60 C77 C21 2.2(17) . . . . ? C3 C60 C77 C75 179.4(10) . . . . ? C97 C75 C77 C21 -91.4(14) . . . . ? C51 C75 C77 C21 87.2(15) . . . . ? C97 C75 C77 C60 91.4(15) . . . . ? C51 C75 C77 C60 -90.0(15) . . . . ? C77 C21 C78 C76 56.8(13) . . . . ? C91 C21 C78 C76 -73.3(12) . . . . ? C70 C21 C78 C76 5.1(16) . . . . ? C77 C21 C78 C79 -123.7(12) . . . . ? C91 C21 C78 C79 106.1(13) . . . . ? C70 C21 C78 C79 -175.4(10) . . . . ? C3 C76 C78 C21 -2.3(18) . . . . ? C3 C76 C78 C79 178.3(11) . . . . ? C99 C74 C79 C84 0(3) . . . . ? C53 C74 C79 C84 176.7(17) . . . . ? C99 C74 C79 C78 -179.8(19) . . . . ? C53 C74 C79 C78 -3(3) . . . . ? C21 C78 C79 C74 -101(2) . . . . ? C76 C78 C79 C74 79(2) . . . . ? C21 C78 C79 C84 79.9(15) . . . . ? C76 C78 C79 C84 -100.6(15) . . . . ? C34 C32 C80 C66 0.2(19) . . . . ? C68 C32 C80 C66 -179.5(13) . . . . ? C82 C66 C80 C32 1(2) . . . . ? C27 C59 C81 C88 -1(3) . . . . ? C34 C54 C82 C66 1(2) . . . . ? C85 C54 C82 C66 178.5(15) . . . . ? C80 C66 C82 C54 -1(2) . . . . ? C74 C79 C84 C90 1(2) . . . . ? C78 C79 C84 C90 -179.5(11) . . . . ? C74 C79 C84 C93 179.0(18) . . . . ? C78 C79 C84 C93 -1.5(18) . . . . ? C75 C51 C87 C94 -3(2) . . . . ? C38 C51 C87 C94 -177.0(14) . . . . ? C59 C81 C88 C57 -1(3) . . . . ? C83 C57 C88 C81 179(2) . . . . ? C28 C57 C88 C81 4(3) . . . . ? C106 C86 C89 C96 0(2) . . . . ? C99 C47 C90 C84 0(2) . . . . ? C79 C84 C90 C47 -1(2) . . . . ? C93 C84 C90 C47 -178.8(14) . . . . ? C3 C69 C91 C21 -3.2(16) . . . . ? C3 C69 C91 C71 -179.9(11) . . . . ? C77 C21 C91 C69 5.6(15) . . . . ? C78 C21 C91 C69 72.1(11) . . . . ? C70 C21 C91 C69 -49.1(11) . . . . ? C77 C21 C91 C71 -177.6(11) . . . . ? C78 C21 C91 C71 -111.1(14) . . . . ? C70 C21 C91 C71 127.6(12) . . . . ? C107 C71 C91 C69 -85.7(17) . . . . ? C103 C71 C91 C69 92.3(15) . . . . ? C107 C71 C91 C21 97.9(15) . . . . ? C103 C71 C91 C21 -84.2(15) . . . . ? C97 C92 C94 C87 0(2) . . . . ? C97 C92 C94 C102 -176.8(13) . . . 3_655 ? C97 C92 C94 C103 -123.1(15) . . . 3_655 ? C51 C87 C94 C92 1(2) . . . . ? C51 C87 C94 C102 178.8(13) . . . 3_655 ? C51 C87 C94 C103 133.2(14) . . . 3_655 ? C86 C89 C96 C72 2(2) . . . . ? C67 C72 C96 C89 -1(2) . . . . ? C100 C72 C96 C89 179.0(14) . . . . ? C51 C75 C97 C92 -1.6(19) . . . . ? C77 C75 C97 C92 176.9(12) . . . . ? C51 C75 C97 C104 -176.7(15) . . . . ? C77 C75 C97 C104 2(2) . . . . ? C94 C92 C97 C75 0(2) . . . . ? C94 C92 C97 C104 175.2(16) . . . . ? C90 C47 C99 C74 1(3) . . . . ? C79 C74 C99 C47 -1(3) . . . . ? C53 C74 C99 C47 -177.6(18) . . . . ? C102 C95 C101 C107 1(2) . . . . ? C101 C95 C102 C103 0(2) . . . . ? C101 C95 C102 C94 79.5(18) . . . 3_655 ? C107 C71 C103 C102 -4(2) . . . . ? C91 C71 C103 C102 178.5(12) . . . . ? C107 C71 C103 C98 176.4(14) . . . . ? C91 C71 C103 C98 -1(2) . . . . ? C107 C71 C103 C94 -76.4(16) . . . 3_655 ? C91 C71 C103 C94 105.7(13) . . . 3_655 ? C95 C102 C103 C71 1(2) . . . . ? C94 C102 C103 C71 -103.9(13) 3_655 . . . ? C95 C102 C103 C98 -178.8(15) . . . . ? C94 C102 C103 C98 76.1(15) 3_655 . . . ? C95 C102 C103 C94 105.1(17) . . . 3_655 ? C72 C67 C106 C86 4(2) . . . . ? C70 C67 C106 C86 -173.0(12) . . . . ? C72 C67 C106 C110 -176.1(14) . . . . ? C70 C67 C106 C110 7(2) . . . . ? C89 C86 C106 C67 -3(2) . . . . ? C89 C86 C106 C110 177.1(15) . . . . ? C95 C101 C107 C71 -3(2) . . . . ? C95 C101 C107 C105 -174.9(18) . . . . ? C103 C71 C107 C101 4(2) . . . . ? C91 C71 C107 C101 -177.7(13) . . . . ? C103 C71 C107 C105 176.6(16) . . . . ? C91 C71 C107 C105 -6(2) . . . . ? N5 C109 C113 N6 -0.1(17) . . . . ? C116 C112 C114 C115 1(2) . . . . ? C116 C112 C114 C111 -179.8(15) . . . . ? N4 C1 N5 C139 87(3) . . . . ? N6 C1 N5 C139 177.4(14) . . . . ? N3 C1 N5 C139 163.5(14) . . . . ? Pd1 C1 N5 C139 -16.0(18) . . . . ? N4 C1 N5 C109 -81(3) . . . . ? N6 C1 N5 C109 10.2(13) . . . . ? N3 C1 N5 C109 -3.8(14) . . . . ? Pd1 C1 N5 C109 176.7(8) . . . . ? C113 C109 N5 C1 -6.6(17) . . . . ? C113 C109 N5 C139 -174.1(15) . . . . ? C112 C114 C115 C118 0(2) . . . . ? C111 C114 C115 C118 -179.1(15) . . . . ? C112 C114 C115 C150 -176.8(13) . . . . ? C111 C114 C115 C150 4(2) . . . . ? C118 C108 C116 C112 5(4) . . . . ? C114 C112 C116 C108 -4(3) . . . . ? C114 C115 C118 C108 1(3) . . . . ? C150 C115 C118 C108 178.2(18) . . . . ? C114 C115 C118 C117 -177.7(16) . . . . ? C150 C115 C118 C117 -1(3) . . . . ? C116 C108 C118 C115 -4(3) . . . . ? C116 C108 C118 C117 175(2) . . . . ? N4 C1 N6 C113 7.2(14) . . . . ? N3 C1 N6 C113 97(4) . . . . ? N5 C1 N6 C113 -10.4(14) . . . . ? Pd1 C1 N6 C113 -176.4(9) . . . . ? N4 C1 N6 C7 -162.9(13) . . . . ? N3 C1 N6 C7 -74(4) . . . . ? N5 C1 N6 C7 179.5(13) . . . . ? Pd1 C1 N6 C7 13.5(18) . . . . ? C109 C113 N6 C1 6.9(18) . . . . ? C109 C113 N6 C7 176.5(15) . . . . ? C17 C7 N6 C1 -40(2) . . . . ? C133 C7 N6 C1 139.0(14) . . . . ? C17 C7 N6 C113 151.0(18) . . . . ? C133 C7 N6 C113 -30(2) . . . . ? C122 C120 C121 C125 1(3) . . . . ? C121 C120 C122 C119 -2(4) . . . . ? C124 C119 C122 C120 3(3) . . . . ? C56 C119 C122 C120 178(2) . . . . ? C122 C119 C124 C125 -2(3) . . . . ? C56 C119 C124 C125 -176.6(19) . . . . ? C122 C119 C124 C4 177.8(17) . . . . ? C56 C119 C124 C4 3(3) . . . . ? C16 C4 C124 C119 -89(2) . . . . ? C11 C4 C124 C119 84(2) . . . . ? C25 C4 C124 C119 -164(6) . . . . ? C16 C4 C124 C125 90.7(16) . . . . ? C11 C4 C124 C125 -96.1(16) . . . . ? C25 C4 C124 C125 15(4) . . . . ? C120 C121 C125 C124 1(3) . . . . ? C120 C121 C125 C123 178(2) . . . . ? C119 C124 C125 C121 0(3) . . . . ? C4 C124 C125 C121 -179.6(17) . . . . ? C119 C124 C125 C123 -177.0(19) . . . . ? C4 C124 C125 C123 3(3) . . . . ? C130 C128 C129 C137 1(3) . . . . ? C165 C128 C129 C137 177.4(17) . . . . ? C130 C128 C129 C127 169.8(17) . . . . ? C165 C128 C129 C127 -14(2) . . . . ? C129 C128 C130 C140 -1(2) . . . . ? C165 C128 C130 C140 -177.3(16) . . . . ? C129 C128 C130 C131 174.8(17) . . . . ? C165 C128 C130 C131 -1(3) . . . . ? C17 C10 C132 C134 -2(3) . . . . ? C159 C10 C132 C134 -178.3(18) . . . . ? C17 C7 C133 C134 -1(3) . . . . ? N6 C7 C133 C134 179.4(16) . . . . ? C7 C133 C134 C132 2(3) . . . . ? C7 C133 C134 C34 -179.8(15) . . . . ? C10 C132 C134 C133 0(3) . . . . ? C10 C132 C134 C34 -178.3(17) . . . . ? C32 C34 C134 C133 85(2) . . . . ? C54 C34 C134 C133 -92(2) . . . . ? C32 C34 C134 C132 -96.8(19) . . . . ? C54 C34 C134 C132 85(2) . . . . ? C19 C13 C135 C138 -6(4) . . . . ? C19 C13 C135 C147 -174(2) . . . . ? C128 C129 C137 C136 -2(3) . . . . ? C127 C129 C137 C136 -170.4(18) . . . . ? C140 C136 C137 C129 4(3) . . . . ? C13 C135 C138 C139 3(3) . . . . ? C147 C135 C138 C139 173.1(18) . . . . ? C19 C41 C139 C138 4(3) . . . . ? C19 C41 C139 N5 -178.9(17) . . . . ? C135 C138 C139 C41 -2(3) . . . . ? C135 C138 C139 N5 -179.8(17) . . . . ? C1 N5 C139 C41 59(2) . . . . ? C109 N5 C139 C41 -135.5(16) . . . . ? C1 N5 C139 C138 -123.8(16) . . . . ? C109 N5 C139 C138 42(2) . . . . ? C128 C130 C140 C136 3(2) . . . . ? C131 C130 C140 C136 -173.2(17) . . . . ? C137 C136 C140 C130 -4(2) . . . . ? C145 C141 C142 C146 5(4) . . . . ? C142 C141 C145 C143 -11(4) . . . . ? C147 C143 C145 C141 14(4) . . . . ? C144 C143 C145 C141 -171(2) . . . . ? C141 C142 C146 C148 177(2) . . . . ? C141 C142 C146 C147 -1(3) . . . . ? C145 C143 C147 C146 -10(4) . . . . ? C144 C143 C147 C146 175(2) . . . . ? C145 C143 C147 C135 180(2) . . . . ? C144 C143 C147 C135 6(4) . . . . ? C142 C146 C147 C143 4(4) . . . . ? C148 C146 C147 C143 -174(3) . . . . ? C142 C146 C147 C135 174(2) . . . . ? C148 C146 C147 C135 -4(3) . . . . ? C13 C135 C147 C143 101(3) . . . . ? C138 C135 C147 C143 -68(3) . . . . ? C13 C135 C147 C146 -69(3) . . . . ? C138 C135 C147 C146 122(2) . . . . ? C154 C149 C150 C151 6(3) . . . . ? C154 C149 C150 C115 177.9(17) . . . . ? C118 C115 C150 C149 -95(2) . . . . ? C114 C115 C150 C149 82(2) . . . . ? C118 C115 C150 C151 77(2) . . . . ? C114 C115 C150 C151 -106.2(19) . . . . ? C149 C150 C151 C152 -6(3) . . . . ? C115 C150 C151 C152 -177.9(18) . . . . ? C150 C151 C152 C153 3(3) . . . . ? C150 C151 C152 C23 176.8(18) . . . . ? C40 C23 C152 C151 -91(2) . . . . ? C26 C23 C152 C151 92(2) . . . . ? C40 C23 C152 C153 83(2) . . . . ? C26 C23 C152 C153 -93(2) . . . . ? C151 C152 C153 C154 1(3) . . . . ? C23 C152 C153 C154 -173.8(19) . . . . ? C150 C149 C154 N3 -177.2(16) . . . . ? C150 C149 C154 C153 -3(3) . . . . ? C1 N3 C154 C149 151.6(16) . . . . ? C55 N3 C154 C149 -28(3) . . . . ? C1 N3 C154 C153 -23(2) . . . . ? C55 N3 C154 C153 157.3(17) . . . . ? C152 C153 C154 C149 -1(3) . . . . ? C152 C153 C154 N3 174.0(18) . . . . ? C160 C155 C156 C157 2(2) . . . . ? C155 C156 C157 C158 0(2) . . . . ? C156 C157 C158 C159 -3(2) . . . . ? C156 C157 C158 C167 174.2(16) . . . . ? C157 C158 C159 C160 2(3) . . . . ? C167 C158 C159 C160 -174.8(18) . . . . ? C157 C158 C159 C10 178.3(16) . . . . ? C167 C158 C159 C10 2(3) . . . . ? C17 C10 C159 C158 -88(2) . . . . ? C132 C10 C159 C158 88(2) . . . . ? C17 C10 C159 C160 89(2) . . . . ? C132 C10 C159 C160 -95(2) . . . . ? C158 C159 C160 C155 1(3) . . . . ? C10 C159 C160 C155 -175.6(16) . . . . ? C158 C159 C160 C168 -179.3(19) . . . . ? C10 C159 C160 C168 4(3) . . . . ? C156 C155 C160 C159 -3(2) . . . . ? C156 C155 C160 C168 177.4(16) . . . . ? C22 C12 C161 C162 112(2) . . . . ? C30 C12 C161 C162 -65(2) . . . . ? C22 C12 C161 C166 -59(3) . . . . ? C30 C12 C161 C166 124.1(19) . . . . ? C12 C161 C162 C163 -177.7(17) . . . . ? C166 C161 C162 C163 -7(3) . . . . ? C161 C162 C163 C164 2(2) . . . . ? C161 C162 C163 N4 -177.7(14) . . . . ? C1 N4 C163 C162 -147.5(13) . . . . ? C65 N4 C163 C162 35(2) . . . . ? C1 N4 C163 C164 33(2) . . . . ? C65 N4 C163 C164 -144.9(14) . . . . ? C162 C163 C164 C165 1(2) . . . . ? N4 C163 C164 C165 -179.5(15) . . . . ? C163 C164 C165 C166 2(3) . . . . ? C163 C164 C165 C128 176.8(16) . . . . ? C130 C128 C165 C166 100(2) . . . . ? C129 C128 C165 C166 -77(3) . . . . ? C130 C128 C165 C164 -75(2) . . . . ? C129 C128 C165 C164 109(2) . . . . ? C164 C165 C166 C161 -7(3) . . . . ? C128 C165 C166 C161 178.0(18) . . . . ? C162 C161 C166 C165 10(3) . . . . ? C12 C161 C166 C165 -179(2) . . . . ? C169 C170 C171 C172 -178(2) . . . . ? C170 C171 C172 C173 -179(2) . . . . ? C171 C172 C173 C174 -171(2) . . . . ? C175 C176 C179 C180 137(6) . . . . ? C194 C189 C190 C191 0.0 . . . . ? C188 C189 C190 C191 179(2) . . . . ? C189 C190 C191 C192 0.0 . . . . ? C190 C191 C192 C193 0.0 . . . . ? C191 C192 C193 C194 0.0 . . . . ? C192 C193 C194 C189 0.0 . . . . ? C190 C189 C194 C193 0.0 . . . . ? C188 C189 C194 C193 -179(3) . . . . ? C200 C195 C196 C197 0.0 . . . . ? C195 C196 C197 C198 0.0 . . . . ? C196 C197 C198 C207 161(6) . . . . ? C196 C197 C198 C199 0.0 . . . . ? C207 C198 C199 C200 -161(6) . . . . ? C197 C198 C199 C200 0.0 . . . . ? C198 C199 C200 C195 0.0 . . . . ? C196 C195 C200 C199 0.0 . . . . ? C187 C201 C202 C203 172(3) . . . . ? C206 C201 C202 C203 0.0 . . . . ? C201 C202 C203 C204 0.0 . . . . ? C202 C203 C204 C205 0.0 . . . . ? C203 C204 C205 C206 0.0 . . . . ? C204 C205 C206 C201 0.0 . . . . ? C187 C201 C206 C205 -172(3) . . . . ? C202 C201 C206 C205 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.708 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.123 data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H102 Cl2 N4 O4 Pd' _chemical_formula_weight 1625.18 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' '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 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.121(15) _cell_length_b 13.230(5) _cell_length_c 25.781(12) _cell_angle_alpha 90.0000(11) _cell_angle_beta 125.4099(17) _cell_angle_gamma 90.0000(11) _cell_volume 8929(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9334 _cell_measurement_theta_min 3.0677 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'colorless' _exptl_crystal_colour 'block' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 0.321 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9386 _exptl_absorpt_correction_T_max 0.9386 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU MercuryCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12244 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3554 _reflns_number_gt 3016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1701P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3554 _refine_ls_number_parameters 542 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2161 _refine_ls_wR_factor_gt 0.2058 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.065 _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 0.0000 -0.01877(9) 0.2500 0.0569(5) Uani 1 2 d S . . C1 C 0.0002(3) 0.0835(6) 0.3061(4) 0.036(3) Uani 1 1 d . . . N1 N -0.0299(3) 0.1615(6) 0.2979(3) 0.035(2) Uani 1 1 d . . . C2 C -0.0135(3) 0.2039(7) 0.3555(4) 0.042(3) Uani 1 1 d . . . H1 H -0.0288 0.2590 0.3623 0.051 Uiso 1 1 calc R . . C3 C 0.0280(4) 0.1527(7) 0.3999(4) 0.038(3) Uani 1 1 d . . . H2 H 0.0481 0.1653 0.4444 0.046 Uiso 1 1 calc R . . N2 N 0.0361(3) 0.0802(5) 0.3705(3) 0.037(2) Uani 1 1 d . . . C4 C -0.0761(3) 0.1963(6) 0.2399(4) 0.029(2) Uani 1 1 d . . . C5 C -0.0760(3) 0.2410(7) 0.1910(4) 0.032(2) Uani 1 1 d . . . H3 H -0.0453 0.2448 0.1936 0.038 Uiso 1 1 calc R . . C6 C -0.1220(4) 0.2803(7) 0.1378(4) 0.040(3) Uani 1 1 d . . . C7 C -0.1658(4) 0.2796(7) 0.1366(4) 0.038(2) Uani 1 1 d . . . H4 H -0.1967 0.3057 0.1004 0.045 Uiso 1 1 calc R . . C8 C -0.1654(3) 0.2417(7) 0.1871(4) 0.037(2) Uani 1 1 d . . . C9 C -0.1199(3) 0.1969(6) 0.2383(4) 0.034(2) Uani 1 1 d . . . H5 H -0.1193 0.1666 0.2721 0.041 Uiso 1 1 calc R . . C10 C -0.1220(4) 0.3311(9) 0.0853(5) 0.045(3) Uani 1 1 d . . . C11 C -0.1465(4) 0.2872(10) 0.0262(5) 0.057(3) Uani 1 1 d . . . C12 C -0.1453(5) 0.3295(14) -0.0199(6) 0.083(5) Uani 1 1 d . . . H6 H -0.1623 0.2983 -0.0605 0.100 Uiso 1 1 calc R . . C13 C -0.1192(7) 0.4181(19) -0.0082(7) 0.124(7) Uani 1 1 d . . . H7 H -0.1172 0.4458 -0.0407 0.148 Uiso 1 1 calc R . . C14 C -0.0954(5) 0.4691(13) 0.0496(7) 0.099(6) Uani 1 1 d . . . H8 H -0.0790 0.5321 0.0557 0.119 Uiso 1 1 calc R . . C15 C -0.0963(4) 0.4249(10) 0.0995(5) 0.069(4) Uani 1 1 d . . . C16 C -0.1760(5) 0.1934(10) 0.0088(5) 0.074(4) Uani 1 1 d . . . H9 H -0.1794 0.1630 -0.0281 0.112 Uiso 1 1 calc R . . H10 H -0.2100 0.2082 -0.0018 0.112 Uiso 1 1 calc R . . H11 H -0.1583 0.1461 0.0447 0.112 Uiso 1 1 calc R . . C17 C -0.0751(5) 0.4788(10) 0.1604(6) 0.083(4) Uani 1 1 d . . . H12 H -0.1007 0.4802 0.1698 0.125 Uiso 1 1 calc R . . H13 H -0.0662 0.5481 0.1570 0.125 Uiso 1 1 calc R . . H14 H -0.0444 0.4436 0.1948 0.125 Uiso 1 1 calc R . . C18 C -0.2098(3) 0.2497(8) 0.1904(4) 0.040(3) Uani 1 1 d . . . C19 C -0.2232(4) 0.3437(8) 0.2010(4) 0.042(3) Uani 1 1 d . . . C20 C -0.2621(4) 0.3510(9) 0.2076(5) 0.055(3) Uani 1 1 d . . . H15 H -0.2706 0.4154 0.2154 0.066 Uiso 1 1 calc R . . C21 C -0.2900(4) 0.2665(11) 0.2032(5) 0.059(3) Uani 1 1 d . . . H16 H -0.3172 0.2740 0.2076 0.071 Uiso 1 1 calc R . . C22 C -0.2778(4) 0.1702(11) 0.1924(4) 0.060(3) Uani 1 1 d . . . H17 H -0.2962 0.1120 0.1901 0.072 Uiso 1 1 calc R . . C23 C -0.2369(4) 0.1624(9) 0.1850(5) 0.050(3) Uani 1 1 d . . . C24 C -0.1939(4) 0.4380(8) 0.2066(5) 0.060(3) Uani 1 1 d . . . H18 H -0.2081 0.4652 0.1641 0.090 Uiso 1 1 calc R . . H19 H -0.1578 0.4209 0.2274 0.090 Uiso 1 1 calc R . . H20 H -0.1968 0.4887 0.2321 0.090 Uiso 1 1 calc R . . C25 C -0.2255(5) 0.0617(10) 0.1728(6) 0.083(4) Uani 1 1 d . . . H21 H -0.2183 0.0664 0.1408 0.125 Uiso 1 1 calc R . . H22 H -0.2550 0.0173 0.1572 0.125 Uiso 1 1 calc R . . H23 H -0.1957 0.0340 0.2124 0.125 Uiso 1 1 calc R . . C26 C 0.0747(3) 0.0028(6) 0.4052(4) 0.031(2) Uani 1 1 d . . . C27 C 0.0739(3) -0.0513(7) 0.4494(4) 0.039(3) Uani 1 1 d . . . H24 H 0.0487 -0.0374 0.4567 0.047 Uiso 1 1 calc R . . C28 C 0.1096(3) -0.1266(6) 0.4838(4) 0.032(2) Uani 1 1 d . . . C29 C 0.1461(4) -0.1456(6) 0.4725(4) 0.037(3) Uani 1 1 d . . . H25 H 0.1704 -0.1977 0.4957 0.044 Uiso 1 1 calc R . . C30 C 0.1480(4) -0.0907(7) 0.4285(4) 0.037(2) Uani 1 1 d . . . C31 C 0.1107(3) -0.0154(7) 0.3928(4) 0.034(2) Uani 1 1 d . . . H26 H 0.1103 0.0219 0.3611 0.041 Uiso 1 1 calc R . . C32 C 0.1888(4) -0.1137(7) 0.4191(4) 0.041(3) Uani 1 1 d . . . C33 C 0.2395(5) -0.0890(8) 0.4656(5) 0.058(3) Uani 1 1 d . . . C34 C 0.2762(5) -0.1144(10) 0.4565(6) 0.069(4) Uani 1 1 d . . . H27 H 0.3107 -0.0962 0.4882 0.083 Uiso 1 1 calc R . . C35 C 0.2654(8) -0.1642(12) 0.4043(9) 0.098(6) Uani 1 1 d . . . H28 H 0.2916 -0.1795 0.3990 0.118 Uiso 1 1 calc R . . C36 C 0.2155(8) -0.1925(9) 0.3590(7) 0.083(5) Uani 1 1 d . . . H29 H 0.2076 -0.2297 0.3228 0.100 Uiso 1 1 calc R . . C37 C 0.1766(5) -0.1676(8) 0.3651(5) 0.054(3) Uani 1 1 d . . . C38 C 0.2550(4) -0.0362(10) 0.5265(5) 0.070(4) Uani 1 1 d . . . H30 H 0.2802 -0.0776 0.5632 0.104 Uiso 1 1 calc R . . H31 H 0.2249 -0.0265 0.5267 0.104 Uiso 1 1 calc R . . H32 H 0.2701 0.0297 0.5291 0.104 Uiso 1 1 calc R . . C39 C 0.1235(6) -0.2006(10) 0.3174(6) 0.087(5) Uani 1 1 d . . . H33 H 0.1107 -0.2365 0.3387 0.130 Uiso 1 1 calc R . . H34 H 0.1225 -0.2457 0.2865 0.130 Uiso 1 1 calc R . . H35 H 0.1020 -0.1413 0.2952 0.130 Uiso 1 1 calc R . . C40 C 0.1091(3) -0.1904(7) 0.5324(4) 0.036(2) Uani 1 1 d . . . C41 C 0.0730(4) -0.2650(7) 0.5105(4) 0.048(3) Uani 1 1 d . . . C42 C 0.0742(4) -0.3261(8) 0.5561(5) 0.057(3) Uani 1 1 d . . . H36 H 0.0488 -0.3764 0.5427 0.068 Uiso 1 1 calc R . . C43 C 0.1119(4) -0.3135(8) 0.6199(5) 0.051(3) Uani 1 1 d . . . H37 H 0.1136 -0.3569 0.6504 0.061 Uiso 1 1 calc R . . C44 C 0.1463(4) -0.2388(8) 0.6386(5) 0.045(3) Uani 1 1 d . . . H38 H 0.1719 -0.2308 0.6829 0.054 Uiso 1 1 calc R . . C45 C 0.1468(3) -0.1740(7) 0.5978(4) 0.037(3) Uani 1 1 d . . . C46 C 0.0322(5) -0.2824(8) 0.4413(5) 0.079(4) Uani 1 1 d . . . H39 H 0.0053 -0.2314 0.4260 0.118 Uiso 1 1 calc R . . H40 H 0.0175 -0.3499 0.4355 0.118 Uiso 1 1 calc R . . H41 H 0.0469 -0.2772 0.4172 0.118 Uiso 1 1 calc R . . C47 C 0.1864(4) -0.0934(8) 0.6202(5) 0.063(4) Uani 1 1 d . . . H42 H 0.2034 -0.0816 0.6658 0.094 Uiso 1 1 calc R . . H43 H 0.1702 -0.0308 0.5967 0.094 Uiso 1 1 calc R . . H44 H 0.2118 -0.1151 0.6128 0.094 Uiso 1 1 calc R . . O1 O 0.0092(5) -0.1416(10) 0.2949(6) 0.038(3) Uiso 0.50 1 d P . . C48 C 0.0099(8) -0.2241(12) 0.2680(7) 0.029(5) Uiso 0.50 1 d P . . O3 O 0.0091(5) -0.2203(10) 0.2162(6) 0.040(4) Uiso 0.50 1 d P . . O4 O 0.0112(5) -0.1231(9) 0.1962(6) 0.035(3) Uiso 0.50 1 d P . . C49 C -0.0693(5) 0.5872(9) 0.2979(6) 0.080(4) Uani 1 1 d . . . H45 H -0.0426 0.6366 0.3072 0.096 Uiso 1 1 calc R . . H46 H -0.0943 0.5831 0.2512 0.096 Uiso 1 1 calc R . . Cl1 Cl -0.04118(12) 0.4689(3) 0.32715(18) 0.0906(12) Uani 1 1 d . . . Cl2 Cl -0.09970(13) 0.6289(3) 0.3313(2) 0.1010(13) Uani 1 1 d . . . C50 C -0.0912(17) -0.023(3) 0.3829(16) 0.174(19) Uiso 0.50 1 d PD A 2 Cl3 Cl -0.0524(6) -0.1015(13) 0.4465(6) 0.189(6) Uiso 0.50 1 d PD A 2 Cl4 Cl -0.0716(3) -0.0570(7) 0.3359(4) 0.105(3) Uiso 0.50 1 d PD A 2 C51 C -0.0811(9) -0.1078(16) 0.3633(9) 0.117(11) Uiso 0.50 1 d PD B 1 Cl5 Cl -0.0668(6) 0.0166(12) 0.3840(7) 0.088(4) Uiso 0.25 1 d PD B 1 Cl6 Cl -0.0809(10) -0.178(2) 0.4203(11) 0.067(7) Uiso 0.13 1 d PD B 1 Cl7 Cl -0.1273(3) -0.0396(6) 0.2955(4) 0.034(2) Uiso 0.25 1 d PD B 1 Cl8 Cl -0.0905(6) -0.1318(12) 0.4235(6) 0.069(4) Uiso 0.25 1 d PD B 1 Cl9 Cl -0.0582(8) -0.0447(15) 0.4248(10) 0.037(5) Uiso 0.12 1 d P B 1 O5 O 0.0070(6) -0.3132(12) 0.2851(7) 0.066(4) Uiso 0.50 1 d P . . 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 0.0602(9) 0.0302(6) 0.0368(7) 0.000 0.0031(6) 0.000 C1 0.038(6) 0.024(5) 0.029(5) 0.000(4) 0.010(5) -0.008(4) N1 0.029(4) 0.033(5) 0.030(5) 0.007(3) 0.011(4) 0.002(4) C2 0.032(6) 0.043(6) 0.034(6) -0.002(5) 0.009(5) -0.004(5) C3 0.042(6) 0.040(6) 0.028(5) 0.000(4) 0.017(5) 0.006(5) N2 0.031(5) 0.028(5) 0.033(5) 0.008(3) 0.008(4) 0.000(3) C4 0.018(5) 0.037(5) 0.017(5) 0.005(4) 0.001(4) -0.002(4) C5 0.030(5) 0.040(6) 0.022(5) 0.007(4) 0.013(4) 0.003(4) C6 0.040(7) 0.040(6) 0.031(6) 0.014(4) 0.016(5) 0.000(5) C7 0.024(6) 0.055(7) 0.033(6) 0.003(5) 0.016(5) -0.001(5) C8 0.030(6) 0.042(6) 0.023(5) 0.003(4) 0.007(5) 0.002(4) C9 0.035(6) 0.035(5) 0.027(5) 0.005(4) 0.015(5) -0.003(4) C10 0.029(6) 0.073(8) 0.034(6) 0.024(5) 0.019(5) 0.015(5) C11 0.040(7) 0.100(10) 0.026(7) 0.016(6) 0.016(6) 0.022(7) C12 0.047(8) 0.144(15) 0.040(8) 0.007(9) 0.015(7) -0.004(9) C13 0.077(12) 0.24(2) 0.045(10) 0.072(12) 0.032(9) 0.041(13) C14 0.049(8) 0.160(15) 0.069(10) 0.057(10) 0.024(7) -0.024(8) C15 0.046(7) 0.089(9) 0.043(7) 0.031(7) 0.009(6) -0.004(7) C16 0.078(9) 0.073(9) 0.039(7) 0.000(6) 0.015(6) 0.010(8) C17 0.063(8) 0.071(8) 0.083(9) 0.007(7) 0.023(7) -0.040(7) C18 0.023(6) 0.066(8) 0.018(5) 0.004(5) 0.004(4) -0.004(5) C19 0.029(6) 0.054(7) 0.030(6) 0.009(5) 0.011(5) 0.005(5) C20 0.050(7) 0.057(8) 0.059(7) 0.011(6) 0.032(6) 0.016(6) C21 0.037(7) 0.104(11) 0.032(6) 0.018(6) 0.018(5) 0.023(7) C22 0.045(7) 0.108(11) 0.023(6) 0.005(6) 0.018(5) -0.019(7) C23 0.045(7) 0.071(8) 0.035(6) -0.015(5) 0.023(5) -0.013(6) C24 0.057(8) 0.059(7) 0.062(8) 0.015(6) 0.033(6) 0.020(6) C25 0.112(11) 0.076(9) 0.099(10) -0.034(8) 0.082(10) -0.043(8) C26 0.021(5) 0.030(6) 0.020(5) 0.006(4) -0.001(4) 0.005(4) C27 0.033(6) 0.032(5) 0.031(5) -0.002(4) 0.006(5) 0.001(4) C28 0.032(6) 0.028(5) 0.015(5) 0.001(4) 0.002(4) 0.003(4) C29 0.043(6) 0.025(5) 0.032(6) 0.000(4) 0.016(5) 0.004(4) C30 0.046(6) 0.028(5) 0.031(6) 0.002(4) 0.019(5) 0.005(4) C31 0.034(6) 0.025(4) 0.022(5) -0.001(4) 0.003(4) -0.001(4) C32 0.051(7) 0.031(5) 0.026(5) 0.017(4) 0.015(5) 0.019(5) C33 0.067(9) 0.062(8) 0.057(8) 0.029(6) 0.042(7) 0.041(6) C34 0.066(8) 0.089(10) 0.067(9) 0.046(8) 0.046(8) 0.051(7) C35 0.151(17) 0.094(12) 0.094(12) 0.073(10) 0.096(13) 0.097(12) C36 0.156(15) 0.049(8) 0.065(10) 0.029(7) 0.076(11) 0.056(10) C37 0.078(9) 0.044(7) 0.041(7) 0.013(5) 0.035(7) 0.023(6) C38 0.031(6) 0.103(11) 0.051(7) -0.002(7) 0.010(5) 0.004(6) C39 0.133(13) 0.074(9) 0.049(8) -0.017(6) 0.051(9) -0.013(8) C40 0.034(6) 0.037(6) 0.036(6) 0.010(4) 0.019(5) 0.012(4) C41 0.050(7) 0.034(6) 0.032(6) 0.009(5) 0.008(5) 0.010(5) C42 0.062(8) 0.041(7) 0.064(8) 0.007(6) 0.035(7) 0.000(5) C43 0.060(8) 0.057(7) 0.038(6) 0.009(5) 0.030(6) 0.008(6) C44 0.051(7) 0.050(7) 0.031(6) 0.009(5) 0.021(5) 0.015(6) C45 0.032(6) 0.040(6) 0.024(5) 0.005(4) 0.007(4) 0.013(4) C46 0.079(9) 0.045(7) 0.062(8) -0.002(6) 0.012(7) -0.019(6) C47 0.074(8) 0.044(7) 0.031(6) -0.009(5) 0.008(6) -0.001(6) C49 0.087(10) 0.052(8) 0.079(9) 0.010(6) 0.035(8) 0.017(7) Cl1 0.071(2) 0.065(2) 0.117(3) 0.031(2) 0.045(2) 0.0137(17) Cl2 0.064(2) 0.107(3) 0.116(3) -0.013(2) 0.043(2) -0.002(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 O1 1.915(13) 2 ? Pd1 O1 1.915(13) . ? Pd1 C1 1.978(9) . ? Pd1 C1 1.978(9) 2 ? Pd1 O4 2.131(13) . ? Pd1 O4 2.131(13) 2 ? C1 N1 1.345(11) . ? C1 N2 1.367(10) . ? N1 C2 1.375(12) . ? N1 C4 1.441(10) . ? C2 C3 1.333(12) . ? C3 N2 1.339(11) . ? N2 C26 1.449(10) . ? C4 C9 1.380(12) . ? C4 C5 1.395(12) . ? C5 C6 1.409(12) . ? C6 C7 1.391(13) . ? C6 C10 1.512(13) . ? C7 C8 1.390(13) . ? C8 C9 1.413(12) . ? C8 C18 1.479(14) . ? C10 C11 1.373(15) . ? C10 C15 1.415(15) . ? C11 C12 1.336(17) . ? C11 C16 1.465(16) . ? C12 C13 1.37(2) . ? C13 C14 1.39(2) . ? C14 C15 1.428(16) . ? C15 C17 1.484(17) . ? C18 C19 1.393(14) . ? C18 C23 1.404(14) . ? C19 C20 1.359(15) . ? C19 C24 1.518(14) . ? C20 C21 1.395(16) . ? C21 C22 1.406(16) . ? C22 C23 1.438(15) . ? C23 C25 1.462(16) . ? C26 C27 1.359(13) . ? C26 C31 1.387(13) . ? C27 C28 1.384(12) . ? C28 C29 1.383(13) . ? C28 C40 1.519(12) . ? C29 C30 1.380(13) . ? C30 C31 1.413(12) . ? C30 C32 1.495(14) . ? C32 C33 1.391(15) . ? C32 C37 1.404(14) . ? C33 C34 1.370(15) . ? C33 C38 1.516(15) . ? C34 C35 1.349(19) . ? C35 C36 1.38(2) . ? C36 C37 1.385(18) . ? C37 C39 1.477(17) . ? C40 C41 1.370(13) . ? C40 C45 1.411(12) . ? C41 C42 1.408(14) . ? C41 C46 1.497(13) . ? C42 C43 1.375(14) . ? C43 C44 1.347(14) . ? C44 C45 1.363(13) . ? C45 C47 1.497(14) . ? O1 O4 0.849(15) 2 ? O1 O3 1.148(15) 2 ? O1 C48 1.30(2) . ? O1 C48 1.74(2) 2 ? C48 C48 0.76(3) 2 ? C48 O3 0.91(2) 2 ? C48 O5 1.28(2) . ? C48 O3 1.32(3) . ? C48 O5 1.64(2) 2 ? C48 O1 1.74(2) 2 ? O3 C48 0.91(2) 2 ? O3 O1 1.148(15) 2 ? O3 O5 1.325(18) 2 ? O3 O4 1.403(18) . ? O4 O1 0.849(15) 2 ? C49 Cl2 1.723(14) . ? C49 Cl1 1.744(11) . ? C50 Cl3 1.72(2) . ? C50 Cl4 1.72(2) . ? C51 Cl9 1.55(3) . ? C51 Cl5 1.709(19) . ? C51 Cl6 1.734(19) . ? C51 Cl7 1.750(18) . ? C51 Cl8 1.774(19) . ? Cl5 Cl9 1.23(3) . ? Cl5 Cl7 2.096(17) . ? Cl6 Cl8 0.71(3) . ? Cl6 Cl9 1.88(3) . ? Cl8 Cl9 1.54(3) . ? O5 O3 1.325(18) 2 ? O5 O5 1.59(3) 2 ? O5 C48 1.64(2) 2 ? 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 O1 64.0(8) 2 . ? O1 Pd1 C1 162.9(5) 2 . ? O1 Pd1 C1 101.8(5) . . ? O1 Pd1 C1 101.8(5) 2 2 ? O1 Pd1 C1 162.9(5) . 2 ? C1 Pd1 C1 93.7(5) . 2 ? O1 Pd1 O4 23.4(4) 2 . ? O1 Pd1 O4 79.6(6) . . ? C1 Pd1 O4 171.6(4) . . ? C1 Pd1 O4 84.1(4) 2 . ? O1 Pd1 O4 79.6(6) 2 2 ? O1 Pd1 O4 23.4(4) . 2 ? C1 Pd1 O4 84.1(4) . 2 ? C1 Pd1 O4 171.6(4) 2 2 ? O4 Pd1 O4 99.3(7) . 2 ? N1 C1 N2 103.9(8) . . ? N1 C1 Pd1 135.5(6) . . ? N2 C1 Pd1 120.6(7) . . ? C1 N1 C2 110.6(7) . . ? C1 N1 C4 128.5(8) . . ? C2 N1 C4 120.6(8) . . ? C3 C2 N1 106.7(9) . . ? C2 C3 N2 107.7(8) . . ? C3 N2 C1 111.1(7) . . ? C3 N2 C26 122.3(7) . . ? C1 N2 C26 126.2(8) . . ? C9 C4 C5 120.3(8) . . ? C9 C4 N1 116.9(8) . . ? C5 C4 N1 122.1(8) . . ? C4 C5 C6 119.2(9) . . ? C7 C6 C5 119.7(8) . . ? C7 C6 C10 120.6(8) . . ? C5 C6 C10 119.6(9) . . ? C8 C7 C6 121.5(9) . . ? C7 C8 C9 117.9(9) . . ? C7 C8 C18 122.8(8) . . ? C9 C8 C18 119.3(8) . . ? C4 C9 C8 121.2(9) . . ? C11 C10 C15 122.2(10) . . ? C11 C10 C6 120.4(10) . . ? C15 C10 C6 117.4(10) . . ? C12 C11 C10 121.0(13) . . ? C12 C11 C16 115.5(12) . . ? C10 C11 C16 123.5(11) . . ? C11 C12 C13 119.5(14) . . ? C12 C13 C14 122.5(14) . . ? C13 C14 C15 118.7(14) . . ? C10 C15 C14 116.0(12) . . ? C10 C15 C17 122.4(10) . . ? C14 C15 C17 121.4(12) . . ? C19 C18 C23 120.6(10) . . ? C19 C18 C8 119.5(9) . . ? C23 C18 C8 119.8(10) . . ? C20 C19 C18 120.0(10) . . ? C20 C19 C24 119.5(10) . . ? C18 C19 C24 120.5(10) . . ? C19 C20 C21 121.7(11) . . ? C20 C21 C22 120.2(11) . . ? C21 C22 C23 118.1(11) . . ? C18 C23 C22 119.3(11) . . ? C18 C23 C25 123.6(11) . . ? C22 C23 C25 117.1(11) . . ? C27 C26 C31 121.6(8) . . ? C27 C26 N2 117.8(9) . . ? C31 C26 N2 120.6(8) . . ? C26 C27 C28 120.4(10) . . ? C29 C28 C27 119.0(9) . . ? C29 C28 C40 119.2(8) . . ? C27 C28 C40 121.8(9) . . ? C30 C29 C28 121.7(9) . . ? C29 C30 C31 118.7(10) . . ? C29 C30 C32 119.2(8) . . ? C31 C30 C32 122.1(9) . . ? C26 C31 C30 118.6(9) . . ? C33 C32 C37 119.3(11) . . ? C33 C32 C30 120.8(9) . . ? C37 C32 C30 119.8(10) . . ? C34 C33 C32 119.3(12) . . ? C34 C33 C38 119.5(12) . . ? C32 C33 C38 121.2(10) . . ? C35 C34 C33 122.7(14) . . ? C34 C35 C36 118.6(14) . . ? C35 C36 C37 121.4(13) . . ? C36 C37 C32 118.7(12) . . ? C36 C37 C39 121.2(13) . . ? C32 C37 C39 120.0(12) . . ? C41 C40 C45 122.6(9) . . ? C41 C40 C28 118.2(8) . . ? C45 C40 C28 119.2(8) . . ? C40 C41 C42 117.5(9) . . ? C40 C41 C46 123.3(9) . . ? C42 C41 C46 119.2(10) . . ? C43 C42 C41 120.5(10) . . ? C44 C43 C42 119.3(10) . . ? C43 C44 C45 123.9(9) . . ? C44 C45 C40 116.1(9) . . ? C44 C45 C47 122.5(9) . . ? C40 C45 C47 121.3(9) . . ? O4 O1 O3 88.0(17) 2 2 ? O4 O1 C48 130(2) 2 . ? O3 O1 C48 43.0(11) 2 . ? O4 O1 C48 121.5(17) 2 2 ? O3 O1 C48 49.2(13) 2 2 ? C48 O1 C48 23.7(10) . 2 ? O4 O1 Pd1 92.7(14) 2 . ? O3 O1 Pd1 137.9(11) 2 . ? C48 O1 Pd1 115.8(12) . . ? C48 O1 Pd1 97.0(9) 2 . ? C48 C48 O3 104(4) 2 2 ? C48 C48 O5 104.1(15) 2 . ? O3 C48 O5 72.2(17) 2 . ? C48 C48 O1 112.9(19) 2 . ? O3 C48 O1 59.6(15) 2 . ? O5 C48 O1 124(2) . . ? C48 C48 O3 42(3) 2 . ? O3 C48 O3 145.5(19) 2 . ? O5 C48 O3 114.8(17) . . ? O1 C48 O3 120.7(17) . . ? C48 C48 O5 49.1(13) 2 2 ? O3 C48 O5 115.4(19) 2 2 ? O5 C48 O5 64.6(14) . 2 ? O1 C48 O5 161.4(15) . 2 ? O3 C48 O5 51.7(9) . 2 ? C48 C48 O1 43.3(15) 2 2 ? O3 C48 O1 114.6(18) 2 2 ? O5 C48 O1 147.0(14) . 2 ? O1 C48 O1 82.2(13) . 2 ? O3 C48 O1 41.2(8) . 2 ? O5 C48 O1 84.6(10) 2 2 ? C48 O3 O1 77.4(17) 2 2 ? C48 O3 C48 34.0(19) 2 . ? O1 O3 C48 89.6(15) 2 . ? C48 O3 O5 67.0(15) 2 2 ? O1 O3 O5 134.5(16) 2 2 ? C48 O3 O5 76.8(13) . 2 ? C48 O3 O4 113.8(18) 2 . ? O1 O3 O4 37.2(8) 2 . ? C48 O3 O4 115.5(14) . . ? O5 O3 O4 160.4(13) 2 . ? O1 O4 O3 54.8(13) 2 . ? O1 O4 Pd1 63.8(13) 2 . ? O3 O4 Pd1 106.9(10) . . ? Cl2 C49 Cl1 111.9(8) . . ? Cl3 C50 Cl4 99.0(13) . . ? Cl9 C51 Cl5 43.9(11) . . ? Cl9 C51 Cl6 69.7(14) . . ? Cl5 C51 Cl6 112.4(16) . . ? Cl9 C51 Cl7 111.6(15) . . ? Cl5 C51 Cl7 74.6(9) . . ? Cl6 C51 Cl7 134.9(18) . . ? Cl9 C51 Cl8 54.6(12) . . ? Cl5 C51 Cl8 92.9(13) . . ? Cl6 C51 Cl8 23.2(9) . . ? Cl7 C51 Cl8 119.4(15) . . ? Cl9 Cl5 C51 61.2(13) . . ? Cl9 Cl5 Cl7 107.7(13) . . ? C51 Cl5 Cl7 53.6(7) . . ? Cl8 Cl6 C51 82(2) . . ? Cl8 Cl6 Cl9 51(2) . . ? C51 Cl6 Cl9 50.6(11) . . ? C51 Cl7 Cl5 51.8(7) . . ? Cl6 Cl8 Cl9 108(3) . . ? Cl6 Cl8 C51 75.3(19) . . ? Cl9 Cl8 C51 55.3(12) . . ? Cl5 Cl9 Cl8 131.6(17) . . ? Cl5 Cl9 C51 74.9(13) . . ? Cl8 Cl9 C51 70.1(12) . . ? Cl5 Cl9 Cl6 132.7(17) . . ? Cl8 Cl9 Cl6 20.9(9) . . ? C51 Cl9 Cl6 59.8(10) . . ? C48 O5 O3 40.7(11) . 2 ? C48 O5 O5 68.8(11) . 2 ? O3 O5 O5 97.0(10) 2 2 ? C48 O5 C48 26.8(11) . 2 ? O3 O5 C48 51.5(12) 2 2 ? O5 O5 C48 46.6(8) 2 2 ? _diffrn_measured_fraction_theta_max 0.451 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.451 _refine_diff_density_max 1.842 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.106 data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H102 N4 O3 Pd' _chemical_formula_weight 1514.26 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 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.854(4) _cell_length_b 17.0305(11) _cell_length_c 30.778(3) _cell_angle_alpha 90.0000(9) _cell_angle_beta 114.6495(11) _cell_angle_gamma 90.0000(9) _cell_volume 16605(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8806 _cell_measurement_theta_min 3.1005 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6400 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9596 _exptl_absorpt_correction_T_max 0.9863 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU MercuryCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29501 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 24.99 _reflns_number_total 7087 _reflns_number_gt 5837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalClear' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0776P)^2^+236.3146P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7087 _refine_ls_number_parameters 875 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2176 _refine_ls_wR_factor_gt 0.2086 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.118 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.27736(3) 0.62399(6) 0.77847(3) 0.0503(3) Uani 1 1 d . . . O1 O 0.2909(3) 0.5277(5) 0.8196(3) 0.067(2) Uani 1 1 d . . . O2 O 0.2913(3) 0.5988(5) 0.8474(3) 0.073(3) Uani 1 1 d . . . O3 O 0.2253(9) 0.4762(15) 0.8339(12) 0.328(14) Uani 1 1 d . . . C1 C 0.2652(3) 0.5878(6) 0.7129(3) 0.034(3) Uani 1 1 d . B . N1 N 0.2274(2) 0.5630(4) 0.6770(3) 0.034(2) Uani 1 1 d . . . C2 C 0.2330(3) 0.5303(6) 0.6381(3) 0.038(3) Uani 1 1 d . . . H1 H 0.2116 0.5105 0.6095 0.046 Uiso 1 1 calc R . . C3 C 0.2741(3) 0.5324(7) 0.6493(3) 0.047(3) Uani 1 1 d . B . H2 H 0.2876 0.5138 0.6301 0.056 Uiso 1 1 calc R . . N2 N 0.2938(2) 0.5670(5) 0.6941(3) 0.043(2) Uani 1 1 d . . . C4 C 0.1874(3) 0.5636(6) 0.6808(3) 0.036(3) Uani 1 1 d . . . C5 C 0.1772(3) 0.6259(7) 0.7023(3) 0.040(2) Uani 1 1 d . A . H3 H 0.1969 0.6672 0.7159 0.048 Uiso 1 1 calc R . . C6 C 0.1378(3) 0.6288(8) 0.7041(3) 0.048(3) Uani 1 1 d . . . C7 C 0.1096(4) 0.5666(8) 0.6837(4) 0.057(3) Uani 1 1 d . A . H4 H 0.0830 0.5673 0.6853 0.069 Uiso 1 1 calc R . . C8 C 0.1195(3) 0.5048(7) 0.6617(4) 0.046(3) Uani 1 1 d . . . C9 C 0.1590(3) 0.5039(7) 0.6613(3) 0.045(3) Uani 1 1 d . A . H5 H 0.1668 0.4606 0.6472 0.054 Uiso 1 1 calc R . . C10 C 0.1213(11) 0.685(2) 0.7261(12) 0.040(11) Uiso 0.41 1 d P A 2 C11 C 0.1030(10) 0.751(2) 0.6997(10) 0.043(9) Uiso 0.41 1 d P A 2 C12 C 0.0907(12) 0.812(2) 0.7246(13) 0.076(10) Uiso 0.41 1 d P A 2 H6 H 0.0736 0.8544 0.7066 0.091 Uiso 0.41 1 calc PR A 2 C13 C 0.1026(12) 0.811(2) 0.7723(13) 0.078(11) Uiso 0.41 1 d P A 2 H7 H 0.0991 0.8556 0.7886 0.094 Uiso 0.41 1 calc PR A 2 C14 C 0.1213(10) 0.738(2) 0.7986(12) 0.063(9) Uiso 0.41 1 d P A 2 H8 H 0.1257 0.7336 0.8311 0.075 Uiso 0.41 1 calc PR A 2 C15 C 0.1332(14) 0.672(3) 0.7771(16) 0.073(15) Uiso 0.41 1 d P A 2 C16 C 0.0836(12) 0.749(2) 0.6438(12) 0.072(11) Uiso 0.41 1 d P A 2 H9 H 0.0670 0.7008 0.6325 0.108 Uiso 0.41 1 calc PR A 2 H10 H 0.1064 0.7498 0.6330 0.108 Uiso 0.41 1 calc PR A 2 H11 H 0.0653 0.7947 0.6309 0.108 Uiso 0.41 1 calc PR A 2 C17 C 0.1530(12) 0.594(2) 0.8031(14) 0.074(11) Uiso 0.41 1 d P A 2 H12 H 0.1838 0.5962 0.8147 0.111 Uiso 0.41 1 calc PR A 2 H13 H 0.1421 0.5499 0.7806 0.111 Uiso 0.41 1 calc PR A 2 H14 H 0.1456 0.5858 0.8301 0.111 Uiso 0.41 1 calc PR A 2 C18 C 0.0866(9) 0.4570(19) 0.6433(10) 0.034(8) Uiso 0.41 1 d P A 2 C19 C 0.0876(10) 0.3854(19) 0.6640(11) 0.046(9) Uiso 0.41 1 d P A 2 C20 C 0.0576(10) 0.325(2) 0.6429(11) 0.056(9) Uiso 0.41 1 d P A 2 H15 H 0.0605 0.2752 0.6575 0.067 Uiso 0.41 1 calc PR A 2 C21 C 0.0220(10) 0.3432(18) 0.5975(10) 0.052(8) Uiso 0.41 1 d P A 2 H16 H 0.0003 0.3057 0.5822 0.062 Uiso 0.41 1 calc PR A 2 C22 C 0.0208(10) 0.416(2) 0.5774(11) 0.059(9) Uiso 0.41 1 d P A 2 H17 H -0.0026 0.4279 0.5482 0.070 Uiso 0.41 1 calc PR A 2 C23 C 0.0496(8) 0.4716(17) 0.5958(9) 0.031(7) Uiso 0.41 1 d P A 2 C24 C 0.1260(11) 0.366(2) 0.7150(11) 0.059(9) Uiso 0.41 1 d P A 2 H18 H 0.1246 0.4016 0.7394 0.089 Uiso 0.41 1 calc PR A 2 H19 H 0.1530 0.3735 0.7127 0.089 Uiso 0.41 1 calc PR A 2 H20 H 0.1237 0.3116 0.7239 0.089 Uiso 0.41 1 calc PR A 2 C25 C 0.0464(12) 0.553(2) 0.5752(14) 0.066(11) Uiso 0.41 1 d P A 2 H21 H 0.0574 0.5524 0.5506 0.099 Uiso 0.41 1 calc PR A 2 H22 H 0.0629 0.5895 0.6007 0.099 Uiso 0.41 1 calc PR A 2 H23 H 0.0167 0.5694 0.5609 0.099 Uiso 0.41 1 calc PR A 2 C26 C 0.3397(8) 0.5695(14) 0.7155(8) 0.044(8) Uiso 0.58 1 d P B 1 C27 C 0.3596(6) 0.5993(12) 0.6868(7) 0.039(6) Uiso 0.58 1 d P B 1 H24 H 0.3433 0.6119 0.6542 0.047 Uiso 0.58 1 calc PR B 1 C28 C 0.4031(6) 0.6097(12) 0.7072(7) 0.041(5) Uiso 0.58 1 d P B 1 C29 C 0.4254(7) 0.5889(13) 0.7547(7) 0.047(6) Uiso 0.58 1 d P B 1 H25 H 0.4550 0.5975 0.7686 0.056 Uiso 0.58 1 calc PR B 1 C30 C 0.4084(7) 0.5577(14) 0.7825(8) 0.045(7) Uiso 0.58 1 d P B 1 C31 C 0.3627(9) 0.5481(15) 0.7631(9) 0.043(9) Uiso 0.58 1 d P B 1 H26 H 0.3493 0.5282 0.7820 0.052 Uiso 0.58 1 calc PR B 1 C32 C 0.4259(6) 0.6336(14) 0.6764(8) 0.043(5) Uiso 0.58 1 d P B 1 C33 C 0.4261(8) 0.584(2) 0.6435(8) 0.058(7) Uiso 0.58 1 d P B 1 C34 C 0.4499(7) 0.6030(14) 0.6162(8) 0.065(7) Uiso 0.58 1 d P B 1 H27 H 0.4526 0.5679 0.5937 0.078 Uiso 0.58 1 calc PR B 1 C35 C 0.4692(9) 0.6794(19) 0.6260(9) 0.069(8) Uiso 0.58 1 d P B 1 H28 H 0.4838 0.6958 0.6075 0.083 Uiso 0.58 1 calc PR B 1 C36 C 0.4681(8) 0.7265(17) 0.6573(10) 0.063(8) Uiso 0.58 1 d P B 1 H29 H 0.4826 0.7753 0.6631 0.076 Uiso 0.58 1 calc PR B 1 C37 C 0.4445(7) 0.7039(15) 0.6835(7) 0.056(6) Uiso 0.58 1 d P B 1 C38 C 0.4042(7) 0.5041(15) 0.6327(8) 0.069(7) Uiso 0.58 1 d P B 1 H30 H 0.3763 0.5094 0.6061 0.104 Uiso 0.58 1 calc PR B 1 H31 H 0.4011 0.4850 0.6610 0.104 Uiso 0.58 1 calc PR B 1 H32 H 0.4212 0.4668 0.6239 0.104 Uiso 0.58 1 calc PR B 1 C39 C 0.4414(6) 0.7674(11) 0.7179(8) 0.039(5) Uiso 0.58 1 d P B 1 H33 H 0.4132 0.7662 0.7175 0.059 Uiso 0.58 1 calc PR B 1 H34 H 0.4466 0.8192 0.7076 0.059 Uiso 0.58 1 calc PR B 1 H35 H 0.4626 0.7569 0.7504 0.059 Uiso 0.58 1 calc PR B 1 C40 C 0.4361(7) 0.5314(15) 0.8326(7) 0.040(7) Uiso 0.58 1 d P B 1 C41 C 0.4669(7) 0.4758(14) 0.8401(8) 0.048(7) Uiso 0.58 1 d P B 1 C42 C 0.4902(7) 0.4508(15) 0.8855(8) 0.064(7) Uiso 0.58 1 d P B 1 H36 H 0.5122 0.4140 0.8908 0.077 Uiso 0.58 1 calc PR B 1 C43 C 0.4833(8) 0.4764(16) 0.9238(10) 0.066(8) Uiso 0.58 1 d P B 1 H37 H 0.4987 0.4541 0.9545 0.079 Uiso 0.58 1 calc PR B 1 C44 C 0.4545(9) 0.5333(16) 0.9182(9) 0.058(9) Uiso 0.58 1 d P B 1 H38 H 0.4509 0.5530 0.9451 0.070 Uiso 0.58 1 calc PR B 1 C45 C 0.4291(9) 0.5646(16) 0.8704(12) 0.060(10) Uiso 0.58 1 d P B 1 C46 C 0.4778(10) 0.4418(18) 0.7997(11) 0.098(10) Uiso 0.58 1 d P B 1 H39 H 0.4939 0.4807 0.7907 0.147 Uiso 0.58 1 calc PR B 1 H40 H 0.4517 0.4290 0.7719 0.147 Uiso 0.58 1 calc PR B 1 H41 H 0.4948 0.3941 0.8112 0.147 Uiso 0.58 1 calc PR B 1 C47 C 0.3970(9) 0.6286(19) 0.8648(10) 0.070(9) Uiso 0.58 1 d P B 1 H42 H 0.3905 0.6572 0.8349 0.105 Uiso 0.58 1 calc PR B 1 H43 H 0.4087 0.6651 0.8918 0.105 Uiso 0.58 1 calc PR B 1 H44 H 0.3711 0.6049 0.8641 0.105 Uiso 0.58 1 calc PR B 1 C48 C 0.1292(9) 0.7062(17) 0.7287(10) 0.052(9) Uiso 0.59 1 d P A 1 C49 C 0.1365(8) 0.7012(16) 0.7744(9) 0.052(8) Uiso 0.59 1 d P A 1 C50 C 0.1309(8) 0.7766(16) 0.7963(9) 0.065(7) Uiso 0.59 1 d P A 1 H45 H 0.1334 0.7768 0.8283 0.078 Uiso 0.59 1 calc PR A 1 C51 C 0.1229(9) 0.8405(19) 0.7724(11) 0.098(9) Uiso 0.59 1 d P A 1 H46 H 0.1255 0.8891 0.7885 0.117 Uiso 0.59 1 calc PR A 1 C52 C 0.1109(9) 0.8406(18) 0.7247(10) 0.094(9) Uiso 0.59 1 d P A 1 H47 H 0.0998 0.8877 0.7075 0.113 Uiso 0.59 1 calc PR A 1 C53 C 0.1139(9) 0.7771(18) 0.7000(10) 0.073(9) Uiso 0.59 1 d P A 1 C54 C 0.1524(7) 0.6320(13) 0.8046(8) 0.047(6) Uiso 0.59 1 d P A 1 H48 H 0.1796 0.6165 0.8049 0.071 Uiso 0.59 1 calc PR A 1 H49 H 0.1322 0.5888 0.7919 0.071 Uiso 0.59 1 calc PR A 1 H50 H 0.1561 0.6442 0.8372 0.071 Uiso 0.59 1 calc PR A 1 C55 C 0.0989(7) 0.7763(14) 0.6473(8) 0.056(7) Uiso 0.59 1 d P A 1 H51 H 0.0684 0.7659 0.6324 0.084 Uiso 0.59 1 calc PR A 1 H52 H 0.1137 0.7350 0.6382 0.084 Uiso 0.59 1 calc PR A 1 H53 H 0.1046 0.8273 0.6365 0.084 Uiso 0.59 1 calc PR A 1 C56 C 0.0897(6) 0.4289(14) 0.6374(7) 0.037(6) Uiso 0.59 1 d P A 1 C57 C 0.0972(8) 0.3589(15) 0.6617(9) 0.056(8) Uiso 0.59 1 d P A 1 C58 C 0.0691(8) 0.2952(16) 0.6373(8) 0.067(7) Uiso 0.59 1 d P A 1 H54 H 0.0722 0.2446 0.6514 0.080 Uiso 0.59 1 calc PR A 1 C59 C 0.0374(9) 0.3115(17) 0.5924(9) 0.081(8) Uiso 0.59 1 d P A 1 H55 H 0.0192 0.2694 0.5761 0.098 Uiso 0.59 1 calc PR A 1 C60 C 0.0305(7) 0.3780(17) 0.5710(8) 0.071(6) Uiso 0.59 1 d P A 1 H56 H 0.0073 0.3847 0.5408 0.085 Uiso 0.59 1 calc PR A 1 C61 C 0.0584(8) 0.4418(16) 0.5933(9) 0.069(8) Uiso 0.59 1 d P A 1 C62 C 0.1340(9) 0.3425(17) 0.7067(9) 0.075(9) Uiso 0.59 1 d P A 1 H57 H 0.1598 0.3585 0.7037 0.112 Uiso 0.59 1 calc PR A 1 H58 H 0.1353 0.2862 0.7136 0.112 Uiso 0.59 1 calc PR A 1 H59 H 0.1315 0.3720 0.7327 0.112 Uiso 0.59 1 calc PR A 1 C63 C 0.0484(8) 0.5219(15) 0.5676(9) 0.063(8) Uiso 0.59 1 d P A 1 H60 H 0.0307 0.5528 0.5790 0.094 Uiso 0.59 1 calc PR A 1 H61 H 0.0333 0.5135 0.5330 0.094 Uiso 0.59 1 calc PR A 1 H62 H 0.0747 0.5501 0.5743 0.094 Uiso 0.59 1 calc PR A 1 C64 C 0.3380(8) 0.5934(16) 0.7204(9) 0.016(7) Uiso 0.42 1 d P B 2 C65 C 0.3577(7) 0.6313(14) 0.6946(8) 0.020(6) Uiso 0.42 1 d P B 2 H63 H 0.3414 0.6470 0.6625 0.024 Uiso 0.42 1 calc PR B 2 C66 C 0.4012(8) 0.6460(16) 0.7155(9) 0.031(7) Uiso 0.42 1 d P B 2 C67 C 0.4239(7) 0.6236(16) 0.7624(7) 0.026(5) Uiso 0.42 1 d P B 2 H64 H 0.4532 0.6356 0.7772 0.032 Uiso 0.42 1 calc PR B 2 C68 C 0.4059(8) 0.5839(17) 0.7895(9) 0.024(7) Uiso 0.42 1 d P B 2 C69 C 0.3609(10) 0.5677(19) 0.7671(11) 0.024(9) Uiso 0.42 1 d P B 2 H65 H 0.3475 0.5404 0.7839 0.028 Uiso 0.42 1 calc PR B 2 C70 C 0.4224(9) 0.6742(19) 0.6888(9) 0.042(7) Uiso 0.42 1 d P B 2 C71 C 0.4285(9) 0.629(2) 0.6526(13) 0.056(8) Uiso 0.42 1 d P B 2 C72 C 0.4541(15) 0.657(3) 0.6268(15) 0.085(14) Uiso 0.42 1 d P B 2 H66 H 0.4604 0.6250 0.6053 0.102 Uiso 0.42 1 calc PR B 2 C73 C 0.4677(11) 0.734(2) 0.6378(14) 0.063(11) Uiso 0.42 1 d P B 2 H67 H 0.4817 0.7561 0.6200 0.075 Uiso 0.42 1 calc PR B 2 C74 C 0.4634(10) 0.781(2) 0.6707(11) 0.069(9) Uiso 0.42 1 d P B 2 H68 H 0.4749 0.8329 0.6770 0.082 Uiso 0.42 1 calc PR B 2 C75 C 0.4409(8) 0.7491(18) 0.6948(11) 0.037(7) Uiso 0.42 1 d P B 2 C76 C 0.4111(13) 0.549(3) 0.6371(12) 0.064(10) Uiso 0.42 1 d P B 2 H69 H 0.3804 0.5519 0.6188 0.096 Uiso 0.42 1 calc PR B 2 H70 H 0.4176 0.5156 0.6653 0.096 Uiso 0.42 1 calc PR B 2 H71 H 0.4239 0.5260 0.6171 0.096 Uiso 0.42 1 calc PR B 2 C77 C 0.4337(8) 0.8070(17) 0.7351(9) 0.050(7) Uiso 0.42 1 d P B 2 H72 H 0.4442 0.8599 0.7338 0.075 Uiso 0.42 1 calc PR B 2 H73 H 0.4491 0.7852 0.7672 0.075 Uiso 0.42 1 calc PR B 2 H74 H 0.4035 0.8097 0.7278 0.075 Uiso 0.42 1 calc PR B 2 C78 C 0.4317(8) 0.5551(16) 0.8393(10) 0.016(7) Uiso 0.42 1 d P B 2 C79 C 0.4677(9) 0.5065(18) 0.8481(9) 0.029(7) Uiso 0.42 1 d P B 2 C80 C 0.4942(8) 0.4859(16) 0.8963(9) 0.033(7) Uiso 0.42 1 d P B 2 H75 H 0.5189 0.4557 0.9024 0.040 Uiso 0.42 1 calc PR B 2 C81 C 0.4859(9) 0.5068(18) 0.9323(10) 0.031(7) Uiso 0.42 1 d P B 2 H76 H 0.5029 0.4887 0.9637 0.037 Uiso 0.42 1 calc PR B 2 C82 C 0.4506(9) 0.5578(17) 0.9232(10) 0.025(7) Uiso 0.42 1 d P B 2 H77 H 0.4470 0.5795 0.9498 0.030 Uiso 0.42 1 calc PR B 2 C83 C 0.4224(10) 0.5762(18) 0.8790(10) 0.025(9) Uiso 0.42 1 d P B 2 C84 C 0.4792(8) 0.4757(15) 0.8077(9) 0.027(6) Uiso 0.42 1 d P B 2 H78 H 0.5072 0.4954 0.8127 0.041 Uiso 0.42 1 calc PR B 2 H79 H 0.4582 0.4941 0.7768 0.041 Uiso 0.42 1 calc PR B 2 H80 H 0.4796 0.4182 0.8082 0.041 Uiso 0.42 1 calc PR B 2 C85 C 0.3849(10) 0.622(2) 0.8705(11) 0.047(9) Uiso 0.42 1 d P B 2 H81 H 0.3609 0.5872 0.8643 0.070 Uiso 0.42 1 calc PR B 2 H82 H 0.3787 0.6567 0.8428 0.070 Uiso 0.42 1 calc PR B 2 H83 H 0.3898 0.6546 0.8988 0.070 Uiso 0.42 1 calc PR B 2 C86 C 0.2671(3) 0.7410(6) 0.7656(4) 0.045(3) Uani 1 1 d . D . N3 N 0.2539(3) 0.7890(5) 0.7267(3) 0.042(2) Uani 1 1 d . . . C87 C 0.2461(3) 0.8652(7) 0.7361(4) 0.049(3) Uani 1 1 d . . . H84 H 0.2363 0.9074 0.7140 0.059 Uiso 1 1 calc R . . C88 C 0.2551(4) 0.8670(7) 0.7827(4) 0.054(3) Uani 1 1 d . D . H85 H 0.2532 0.9113 0.8005 0.065 Uiso 1 1 calc R . . N4 N 0.2679(3) 0.7920(6) 0.8002(3) 0.055(3) Uani 1 1 d . . . C89 C 0.2431(3) 0.7687(6) 0.6763(3) 0.039(3) Uani 1 1 d . . . C90 C 0.2006(4) 0.7772(6) 0.6451(3) 0.051(3) Uani 1 1 d . C . H86 H 0.1802 0.7874 0.6575 0.061 Uiso 1 1 calc R . . C91 C 0.1880(3) 0.7706(6) 0.5957(4) 0.041(3) Uani 1 1 d . . . C92 C 0.2190(4) 0.7572(6) 0.5792(4) 0.051(3) Uani 1 1 d . C . H87 H 0.2109 0.7545 0.5457 0.061 Uiso 1 1 calc R . . C93 C 0.2608(4) 0.7477(8) 0.6091(4) 0.062(4) Uani 1 1 d . . . C94 C 0.2731(4) 0.7537(7) 0.6589(4) 0.060(4) Uani 1 1 d . C . H88 H 0.3019 0.7475 0.6804 0.072 Uiso 1 1 calc R . . C95 C 0.1408(9) 0.7754(17) 0.5614(9) 0.025(8) Uiso 0.51 1 d P C 1 C96 C 0.1187(16) 0.708(3) 0.5381(17) 0.08(2) Uiso 0.51 1 d P C 1 C97 C 0.0721(12) 0.723(2) 0.5109(13) 0.059(13) Uiso 0.51 1 d P C 1 H89 H 0.0547 0.6796 0.4963 0.070 Uiso 0.51 1 calc PR C 1 C98 C 0.0543(9) 0.7899(16) 0.5056(9) 0.052(8) Uiso 0.51 1 d P C 1 H90 H 0.0251 0.7944 0.4850 0.062 Uiso 0.51 1 calc PR C 1 C99 C 0.0770(8) 0.8582(15) 0.5301(8) 0.047(7) Uiso 0.51 1 d P C 1 H91 H 0.0632 0.9075 0.5261 0.056 Uiso 0.51 1 calc PR C 1 C100 C 0.1193(8) 0.8512(15) 0.5596(9) 0.045(8) Uiso 0.51 1 d P C 1 C101 C 0.1417(10) 0.6359(19) 0.5384(12) 0.065(10) Uiso 0.51 1 d P C 1 H92 H 0.1223 0.5982 0.5157 0.097 Uiso 0.51 1 calc PR C 1 H93 H 0.1534 0.6132 0.5706 0.097 Uiso 0.51 1 calc PR C 1 H94 H 0.1647 0.6480 0.5291 0.097 Uiso 0.51 1 calc PR C 1 C102 C 0.1423(4) 0.9216(9) 0.5888(7) 0.054(6) Uiso 0.51 1 d P C 1 H95 H 0.1264 0.9695 0.5746 0.080 Uiso 0.51 1 calc PR C 1 H96 H 0.1705 0.9249 0.5892 0.080 Uiso 0.51 1 calc PR C 1 H97 H 0.1448 0.9161 0.6216 0.080 Uiso 0.51 1 calc PR C 1 C103 C 0.2905(3) 0.7249(7) 0.5857(4) 0.050(5) Uiso 0.61 1 d PR C 1 C104 C 0.2870(3) 0.6613(7) 0.5560(4) 0.037(4) Uiso 0.61 1 d PR C 1 C105 C 0.3178(3) 0.6485(7) 0.5391(4) 0.061(6) Uiso 0.61 1 d PR C 1 H98 H 0.3148 0.6059 0.5180 0.074 Uiso 0.61 1 calc PR C 1 C106 C 0.3526(8) 0.6970(16) 0.5526(8) 0.070(7) Uiso 0.61 1 d P C 1 H99 H 0.3744 0.6827 0.5432 0.084 Uiso 0.61 1 calc PR C 1 C107 C 0.3581(7) 0.7706(17) 0.5810(9) 0.057(6) Uiso 0.61 1 d P C 1 H100 H 0.3796 0.8088 0.5867 0.068 Uiso 0.61 1 calc PR C 1 C108 C 0.3262(7) 0.7741(15) 0.5981(8) 0.054(7) Uiso 0.61 1 d P C 1 C109 C 0.2459(7) 0.6090(13) 0.5366(7) 0.062(7) Uiso 0.61 1 d P C 1 H101 H 0.2260 0.6291 0.5055 0.093 Uiso 0.61 1 calc PR C 1 H102 H 0.2327 0.6109 0.5592 0.093 Uiso 0.61 1 calc PR C 1 H103 H 0.2533 0.5546 0.5331 0.093 Uiso 0.61 1 calc PR C 1 C110 C 0.3310(6) 0.8530(14) 0.6265(8) 0.050(6) Uiso 0.61 1 d P C 1 H104 H 0.3036 0.8793 0.6153 0.075 Uiso 0.61 1 calc PR C 1 H105 H 0.3513 0.8872 0.6212 0.075 Uiso 0.61 1 calc PR C 1 H106 H 0.3413 0.8415 0.6607 0.075 Uiso 0.61 1 calc PR C 1 C111 C 0.2825(8) 0.7723(13) 0.8487(8) 0.036(7) Uiso 0.57 1 d P D 1 C112 C 0.3263(6) 0.7776(10) 0.8841(6) 0.023(4) Uiso 0.57 1 d P D 1 H107 H 0.3479 0.7910 0.8743 0.028 Uiso 0.57 1 calc PR D 1 C113 C 0.3361(8) 0.7631(14) 0.9319(8) 0.049(7) Uiso 0.57 1 d P D 1 C114 C 0.3038(10) 0.7426(14) 0.9441(10) 0.059(7) Uiso 0.57 1 d P D 1 H108 H 0.3102 0.7342 0.9769 0.070 Uiso 0.57 1 calc PR D 1 C115 C 0.2622(9) 0.7335(14) 0.9112(9) 0.059(7) Uiso 0.57 1 d P D 1 C116 C 0.2521(4) 0.7450(7) 0.8637(4) 0.049(6) Uiso 0.57 1 d P D 1 H109 H 0.2243 0.7344 0.8407 0.059 Uiso 0.57 1 calc PR D 1 C117 C 0.3822(4) 0.7669(7) 0.9682(4) 0.039(5) Uiso 0.57 1 d PR D 1 C118 C 0.4012(4) 0.8401(7) 0.9816(4) 0.038(5) Uiso 0.57 1 d PR D 1 C119 C 0.4430(4) 0.8455(7) 1.0147(4) 0.057(6) Uiso 0.57 1 d PR D 1 H110 H 0.4559 0.8955 1.0238 0.068 Uiso 0.57 1 d PR D 1 C120 C 0.4668(8) 0.7757(13) 1.0349(8) 0.063(6) Uiso 0.57 1 d P D 1 H111 H 0.4952 0.7790 1.0583 0.076 Uiso 0.57 1 calc PR D 1 C121 C 0.4486(8) 0.7070(16) 1.0204(9) 0.054(8) Uiso 0.57 1 d P D 1 H112 H 0.4650 0.6607 1.0316 0.065 Uiso 0.57 1 calc PR D 1 C122 C 0.4043(6) 0.6992(11) 0.9879(7) 0.047(5) Uiso 0.57 1 d P D 1 C123 C 0.3756(8) 0.9181(14) 0.9649(9) 0.059(8) Uiso 0.57 1 d P D 1 H113 H 0.3841 0.9548 0.9918 0.089 Uiso 0.57 1 calc PR D 1 H114 H 0.3454 0.9068 0.9533 0.089 Uiso 0.57 1 calc PR D 1 H115 H 0.3812 0.9415 0.9391 0.089 Uiso 0.57 1 calc PR D 1 C124 C 0.3833(7) 0.6212(15) 0.9786(8) 0.069(6) Uiso 0.57 1 d P D 1 H116 H 0.3611 0.6208 0.9902 0.103 Uiso 0.57 1 calc PR D 1 H117 H 0.4042 0.5805 0.9951 0.103 Uiso 0.57 1 calc PR D 1 H118 H 0.3708 0.6107 0.9441 0.103 Uiso 0.57 1 calc PR D 1 C125 C 0.2290(9) 0.7094(15) 0.9249(8) 0.066(6) Uiso 0.57 1 d P D 1 C126 C 0.2232(9) 0.6364(18) 0.9337(9) 0.071(8) Uiso 0.57 1 d P D 1 C127 C 0.1919(9) 0.5997(17) 0.9422(9) 0.085(8) Uiso 0.57 1 d P D 1 H119 H 0.1910 0.5459 0.9498 0.102 Uiso 0.57 1 calc PR D 1 C128 C 0.1542(7) 0.6708(16) 0.9363(7) 0.046(6) Uiso 0.57 1 d P D 1 H120 H 0.1276 0.6564 0.9357 0.055 Uiso 0.57 1 calc PR D 1 C129 C 0.1620(10) 0.7363(19) 0.9330(9) 0.094(8) Uiso 0.57 1 d P D 1 H121 H 0.1433 0.7737 0.9365 0.112 Uiso 0.57 1 calc PR D 1 C130 C 0.1980(9) 0.770(2) 0.9239(9) 0.060(8) Uiso 0.57 1 d P D 1 C131 C 0.2572(9) 0.5683(15) 0.9342(9) 0.091(8) Uiso 0.57 1 d P D 1 H122 H 0.2811 0.5673 0.9656 0.136 Uiso 0.57 1 calc PR D 1 H123 H 0.2672 0.5804 0.9096 0.136 Uiso 0.57 1 calc PR D 1 H124 H 0.2432 0.5170 0.9276 0.136 Uiso 0.57 1 calc PR D 1 C132 C 0.2018(10) 0.8476(19) 0.9188(10) 0.093(9) Uiso 0.57 1 d P D 1 H125 H 0.2275 0.8668 0.9452 0.139 Uiso 0.57 1 calc PR D 1 H126 H 0.1772 0.8747 0.9193 0.139 Uiso 0.57 1 calc PR D 1 H127 H 0.2036 0.8578 0.8884 0.139 Uiso 0.57 1 calc PR D 1 C133 C 0.1432(12) 0.797(2) 0.5641(13) 0.053(13) Uiso 0.49 1 d P C 2 C134 C 0.1168(10) 0.726(2) 0.5380(11) 0.027(10) Uiso 0.49 1 d P C 2 C135 C 0.0764(12) 0.738(2) 0.5054(13) 0.055(13) Uiso 0.49 1 d P C 2 H128 H 0.0589 0.6968 0.4869 0.065 Uiso 0.49 1 calc PR C 2 C136 C 0.0623(9) 0.8173(17) 0.5011(9) 0.047(8) Uiso 0.49 1 d P C 2 H129 H 0.0332 0.8279 0.4826 0.056 Uiso 0.49 1 calc PR C 2 C137 C 0.0888(8) 0.8793(17) 0.5225(8) 0.049(7) Uiso 0.49 1 d P C 2 H130 H 0.0784 0.9315 0.5155 0.059 Uiso 0.49 1 calc PR C 2 C138 C 0.1297(9) 0.8669(18) 0.5537(9) 0.047(8) Uiso 0.49 1 d P C 2 C139 C 0.1320(9) 0.6375(18) 0.5462(10) 0.044(8) Uiso 0.49 1 d P C 2 H131 H 0.1547 0.6302 0.5356 0.066 Uiso 0.49 1 calc PR C 2 H132 H 0.1083 0.6029 0.5278 0.066 Uiso 0.49 1 calc PR C 2 H133 H 0.1426 0.6248 0.5802 0.066 Uiso 0.49 1 calc PR C 2 C140 C 0.1599(6) 0.9339(12) 0.5772(10) 0.087(10) Uiso 0.49 1 d P C 2 H134 H 0.1474 0.9834 0.5615 0.131 Uiso 0.49 1 calc PR C 2 H135 H 0.1865 0.9249 0.5743 0.131 Uiso 0.49 1 calc PR C 2 H136 H 0.1654 0.9366 0.6111 0.131 Uiso 0.49 1 calc PR C 2 C141 C 0.2960(6) 0.7565(10) 0.5930(7) 0.045(8) Uiso 0.39 1 d PR C 2 C142 C 0.2960(6) 0.6945(11) 0.5635(7) 0.058(9) Uiso 0.39 1 d PR C 2 C143 C 0.3276(6) 0.6890(11) 0.5474(7) 0.085(13) Uiso 0.39 1 d PR C 2 H137 H 0.3279 0.6484 0.5264 0.102 Uiso 0.39 1 calc PR C 2 C144 C 0.3553(11) 0.740(3) 0.5618(14) 0.057(10) Uiso 0.39 1 d P C 2 H138 H 0.3785 0.7307 0.5538 0.069 Uiso 0.39 1 calc PR C 2 C145 C 0.3586(15) 0.815(3) 0.5908(16) 0.111(17) Uiso 0.39 1 d P C 2 H139 H 0.3781 0.8572 0.5966 0.133 Uiso 0.39 1 calc PR C 2 C146 C 0.3262(9) 0.809(2) 0.6067(11) 0.035(7) Uiso 0.39 1 d P C 2 C147 C 0.2637(10) 0.6310(19) 0.5423(10) 0.044(8) Uiso 0.39 1 d P C 2 H140 H 0.2429 0.6478 0.5108 0.067 Uiso 0.39 1 calc PR C 2 H141 H 0.2494 0.6210 0.5632 0.067 Uiso 0.39 1 calc PR C 2 H142 H 0.2776 0.5829 0.5389 0.067 Uiso 0.39 1 calc PR C 2 C148 C 0.3257(12) 0.889(2) 0.6369(13) 0.079(13) Uiso 0.39 1 d P C 2 H143 H 0.2998 0.9190 0.6190 0.118 Uiso 0.39 1 calc PR C 2 H144 H 0.3503 0.9218 0.6415 0.118 Uiso 0.39 1 calc PR C 2 H145 H 0.3267 0.8744 0.6681 0.118 Uiso 0.39 1 calc PR C 2 C149 C 0.2692(13) 0.772(2) 0.8510(13) 0.055(13) Uiso 0.43 1 d P D 2 C150 C 0.3075(12) 0.7642(18) 0.8792(12) 0.055(10) Uiso 0.43 1 d P D 2 H146 H 0.3288 0.7705 0.8680 0.066 Uiso 0.43 1 calc PR D 2 C151 C 0.3197(15) 0.743(2) 0.9329(14) 0.072(13) Uiso 0.43 1 d P D 2 C152 C 0.2828(13) 0.7456(19) 0.9426(14) 0.062(10) Uiso 0.43 1 d P D 2 H147 H 0.2859 0.7391 0.9746 0.074 Uiso 0.43 1 calc PR D 2 C153 C 0.2433(9) 0.7567(15) 0.9069(9) 0.037(7) Uiso 0.43 1 d P D 2 C154 C 0.2356(8) 0.7718(14) 0.8598(8) 0.032(6) Uiso 0.43 1 d P D 2 H148 H 0.2081 0.7810 0.8358 0.039 Uiso 0.43 1 calc PR D 2 C155 C 0.3624(9) 0.7370(17) 0.9679(10) 0.052(7) Uiso 0.43 1 d P D 2 C156 C 0.3883(10) 0.799(2) 0.9808(11) 0.054(7) Uiso 0.43 1 d P D 2 C157 C 0.4349(14) 0.788(3) 1.0155(14) 0.106(13) Uiso 0.43 1 d P D 2 H149 H 0.4561 0.8272 1.0248 0.127 Uiso 0.43 1 calc PR D 2 C158 C 0.4407(15) 0.712(3) 1.0307(15) 0.080(15) Uiso 0.43 1 d P D 2 H150 H 0.4680 0.7026 1.0554 0.096 Uiso 0.43 1 calc PR D 2 C159 C 0.4182(9) 0.6502(17) 1.0195(10) 0.054(7) Uiso 0.43 1 d P D 2 H151 H 0.4289 0.5995 1.0314 0.065 Uiso 0.43 1 calc PR D 2 C160 C 0.3746(10) 0.664(2) 0.9869(11) 0.063(8) Uiso 0.43 1 d P D 2 C161 C 0.3783(11) 0.886(2) 0.9622(13) 0.070(11) Uiso 0.43 1 d P D 2 H152 H 0.4003 0.9211 0.9839 0.105 Uiso 0.43 1 calc PR D 2 H153 H 0.3508 0.9018 0.9611 0.105 Uiso 0.43 1 calc PR D 2 H154 H 0.3775 0.8896 0.9301 0.105 Uiso 0.43 1 calc PR D 2 C162 C 0.3463(11) 0.5968(19) 0.9751(12) 0.081(10) Uiso 0.43 1 d P D 2 H155 H 0.3283 0.6004 0.9924 0.121 Uiso 0.43 1 calc PR D 2 H156 H 0.3630 0.5484 0.9843 0.121 Uiso 0.43 1 calc PR D 2 H157 H 0.3286 0.5961 0.9406 0.121 Uiso 0.43 1 calc PR D 2 C163 C 0.2047(10) 0.737(2) 0.9225(9) 0.033(8) Uiso 0.43 1 d P D 2 C164 C 0.1932(10) 0.6709(19) 0.9307(10) 0.059(8) Uiso 0.43 1 d P D 2 C165 C 0.1648(10) 0.638(2) 0.9404(10) 0.052(9) Uiso 0.43 1 d P D 2 H158 H 0.1632 0.5858 0.9510 0.062 Uiso 0.43 1 calc PR D 2 C166 C 0.1281(11) 0.7202(18) 0.9276(10) 0.063(8) Uiso 0.43 1 d P D 2 H159 H 0.1005 0.7118 0.9257 0.076 Uiso 0.43 1 calc PR D 2 C167 C 0.1400(9) 0.7935(17) 0.9208(9) 0.057(8) Uiso 0.43 1 d P D 2 H160 H 0.1219 0.8366 0.9184 0.068 Uiso 0.43 1 calc PR D 2 C168 C 0.1788(10) 0.8077(19) 0.9172(10) 0.052(8) Uiso 0.43 1 d P D 2 C169 C 0.2266(9) 0.596(2) 0.9341(10) 0.042(7) Uiso 0.43 1 d P D 2 H161 H 0.2143 0.5465 0.9381 0.063 Uiso 0.43 1 calc PR D 2 H162 H 0.2537 0.6047 0.9615 0.063 Uiso 0.43 1 calc PR D 2 H163 H 0.2310 0.5945 0.9047 0.063 Uiso 0.43 1 calc PR D 2 C170 C 0.1899(9) 0.8906(16) 0.9073(10) 0.049(7) Uiso 0.43 1 d P D 2 H164 H 0.1805 0.8978 0.8728 0.073 Uiso 0.43 1 calc PR D 2 H165 H 0.2205 0.8983 0.9235 0.073 Uiso 0.43 1 calc PR D 2 H166 H 0.1757 0.9290 0.9193 0.073 Uiso 0.43 1 calc PR D 2 C171 C 0.0650(8) 0.5165(17) 0.4062(9) 0.220(12) Uiso 1 1 d D . . H167 H 0.0374 0.5303 0.4055 0.329 Uiso 1 1 calc R . . H168 H 0.0857 0.5567 0.4239 0.329 Uiso 1 1 calc R . . H169 H 0.0740 0.4655 0.4220 0.329 Uiso 1 1 calc R . . C172 C 0.0614(11) 0.512(3) 0.3553(12) 0.37(3) Uiso 1 1 d D . . H170 H 0.0708 0.5626 0.3474 0.446 Uiso 1 1 calc R . . H171 H 0.0813 0.4710 0.3543 0.446 Uiso 1 1 calc R . . C173 C 0.0183(12) 0.4933(19) 0.3170(10) 0.34(2) Uiso 1 1 d D . . H172 H 0.0109 0.5321 0.2908 0.409 Uiso 1 1 calc R . . H173 H -0.0029 0.4969 0.3305 0.409 Uiso 1 1 calc R . . C174 C 0.018(3) 0.4077(19) 0.2965(15) 1.5(3) Uiso 1 1 d D . . H174 H -0.0074 0.4015 0.2657 1.790 Uiso 1 1 calc R . . H175 H 0.0433 0.3990 0.2909 1.790 Uiso 1 1 calc R . . C175 C 0.0159(17) 0.3483(19) 0.3326(16) 0.42(3) Uiso 1 1 d D . . H176 H 0.0380 0.3624 0.3643 0.509 Uiso 1 1 calc R . . H177 H -0.0117 0.3541 0.3343 0.509 Uiso 1 1 calc R . . C176 C 0.0214(10) 0.2626(18) 0.3235(11) 0.243(14) Uiso 1 1 d D . . H178 H 0.0131 0.2299 0.3443 0.364 Uiso 1 1 calc R . . H179 H 0.0511 0.2525 0.3304 0.364 Uiso 1 1 calc R . . H180 H 0.0037 0.2499 0.2900 0.364 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 0.0561(6) 0.0539(5) 0.0284(4) 0.0044(5) 0.0053(3) -0.0061(6) O1 0.082(6) 0.052(5) 0.059(5) 0.009(4) 0.020(5) -0.011(5) O2 0.100(7) 0.072(6) 0.037(4) 0.011(4) 0.016(4) -0.022(5) O3 0.33(3) 0.26(3) 0.51(4) -0.01(3) 0.30(3) 0.04(2) C1 0.021(6) 0.037(6) 0.040(6) 0.015(5) 0.009(5) -0.007(5) N1 0.024(5) 0.037(5) 0.030(4) 0.008(4) 0.001(4) -0.005(4) C2 0.026(6) 0.058(7) 0.024(5) -0.003(5) 0.004(4) 0.004(5) C3 0.029(7) 0.071(8) 0.028(6) 0.008(6) -0.002(5) 0.008(6) N2 0.019(5) 0.063(6) 0.034(5) 0.010(4) -0.003(4) 0.001(4) C4 0.019(6) 0.040(7) 0.037(6) 0.010(5) 0.000(5) -0.003(5) C5 0.032(6) 0.048(7) 0.044(6) 0.020(6) 0.019(5) 0.015(6) C6 0.043(7) 0.063(8) 0.034(5) -0.003(6) 0.011(5) 0.001(7) C7 0.052(8) 0.091(10) 0.036(6) 0.020(7) 0.025(6) 0.011(8) C8 0.023(6) 0.058(8) 0.046(7) 0.002(6) 0.004(5) -0.004(6) C9 0.037(7) 0.059(8) 0.040(6) 0.001(6) 0.015(5) 0.007(6) C86 0.039(7) 0.049(7) 0.034(6) 0.000(5) 0.003(5) -0.005(5) N3 0.038(5) 0.047(6) 0.030(5) 0.004(4) 0.003(4) -0.004(4) C87 0.054(7) 0.035(7) 0.041(6) 0.001(6) 0.003(5) -0.007(6) C88 0.072(8) 0.042(7) 0.035(6) -0.009(6) 0.007(5) -0.010(7) N4 0.065(7) 0.058(7) 0.030(5) 0.000(5) 0.009(5) -0.005(5) C89 0.036(7) 0.040(7) 0.036(6) 0.007(5) 0.009(5) -0.002(5) C90 0.061(8) 0.051(7) 0.029(6) 0.001(5) 0.008(6) -0.011(6) C91 0.045(7) 0.034(6) 0.036(6) 0.007(5) 0.009(5) 0.006(5) C92 0.060(8) 0.049(7) 0.028(6) 0.012(5) 0.004(6) 0.008(6) C93 0.064(9) 0.078(9) 0.038(7) 0.023(6) 0.017(6) 0.017(7) C94 0.051(8) 0.083(10) 0.034(6) 0.027(6) 0.004(6) -0.011(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 C1 1.980(10) . ? Pd1 O1 2.005(7) . ? Pd1 O2 2.014(7) . ? Pd1 C86 2.035(11) . ? O1 O2 1.478(11) . ? C1 N1 1.385(11) . ? C1 N2 1.388(12) . ? N1 C2 1.405(12) . ? N1 C4 1.447(12) . ? C2 C3 1.325(13) . ? C2 H1 0.9500 . ? C3 N2 1.391(12) . ? C3 H2 0.9500 . ? N2 C26 1.46(2) . ? N2 C64 1.48(3) . ? C4 C9 1.370(14) . ? C4 C5 1.374(14) . ? C5 C6 1.398(14) . ? C5 H3 0.9500 . ? C6 C7 1.402(16) . ? C6 C10 1.43(4) . ? C6 C48 1.61(3) . ? C7 C8 1.371(15) . ? C7 H4 0.9500 . ? C8 C18 1.32(3) . ? C8 C9 1.383(14) . ? C8 C56 1.63(2) . ? C9 H5 0.9500 . ? C10 C11 1.38(5) . ? C10 C15 1.46(5) . ? C11 C12 1.45(4) . ? C11 C16 1.57(4) . ? C12 C13 1.35(4) . ? C12 H6 0.9500 . ? C13 C14 1.48(5) . ? C13 H7 0.9500 . ? C14 C15 1.44(5) . ? C14 H8 0.9500 . ? C15 C17 1.56(6) . ? C16 H9 0.9800 . ? C16 H10 0.9800 . ? C16 H11 0.9800 . ? C17 H12 0.9800 . ? C17 H13 0.9800 . ? C17 H14 0.9800 . ? C18 C19 1.37(4) . ? C18 C23 1.51(4) . ? C19 C20 1.41(4) . ? C19 C24 1.62(4) . ? C20 C21 1.46(4) . ? C20 H15 0.9500 . ? C21 C22 1.38(4) . ? C21 H16 0.9500 . ? C22 C23 1.32(4) . ? C22 H17 0.9500 . ? C23 C25 1.51(4) . ? C24 H18 0.9800 . ? C24 H19 0.9800 . ? C24 H20 0.9800 . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C25 H23 0.9800 . ? C26 C31 1.39(3) . ? C26 C27 1.42(3) . ? C27 C28 1.39(3) . ? C27 H24 0.9500 . ? C28 C29 1.38(3) . ? C28 C32 1.52(3) . ? C29 C30 1.34(3) . ? C29 H25 0.9500 . ? C30 C31 1.46(3) . ? C30 C40 1.50(3) . ? C31 H26 0.9500 . ? C32 C33 1.32(3) . ? C32 C37 1.34(3) . ? C33 C34 1.44(3) . ? C33 C38 1.53(4) . ? C34 C35 1.44(4) . ? C34 H27 0.9500 . ? C35 C36 1.27(4) . ? C35 H28 0.9500 . ? C36 C37 1.43(3) . ? C36 H29 0.9500 . ? C37 C39 1.55(3) . ? C38 H30 0.9800 . ? C38 H31 0.9800 . ? C38 H32 0.9800 . ? C39 H33 0.9800 . ? C39 H34 0.9800 . ? C39 H35 0.9800 . ? C40 C41 1.38(3) . ? C40 C45 1.41(4) . ? C41 C42 1.36(3) . ? C41 C46 1.56(4) . ? C42 C43 1.37(3) . ? C42 H36 0.9500 . ? C43 C44 1.35(4) . ? C43 H37 0.9500 . ? C44 C45 1.46(4) . ? C44 H38 0.9500 . ? C45 C47 1.52(4) . ? C46 H39 0.9800 . ? C46 H40 0.9800 . ? C46 H41 0.9800 . ? C47 H42 0.9800 . ? C47 H43 0.9800 . ? C47 H44 0.9800 . ? C48 C49 1.32(3) . ? C48 C53 1.46(4) . ? C49 C54 1.46(3) . ? C49 C50 1.50(3) . ? C50 C51 1.28(4) . ? C50 H45 0.9500 . ? C51 C52 1.35(3) . ? C51 H46 0.9500 . ? C52 C53 1.35(3) . ? C52 H47 0.9500 . ? C53 C55 1.48(3) . ? C54 H48 0.9800 . ? C54 H49 0.9800 . ? C54 H50 0.9800 . ? C55 H51 0.9800 . ? C55 H52 0.9800 . ? C55 H53 0.9800 . ? C56 C61 1.36(3) . ? C56 C57 1.37(3) . ? C57 C58 1.44(3) . ? C57 C62 1.47(3) . ? C58 C59 1.39(3) . ? C58 H54 0.9500 . ? C59 C60 1.28(3) . ? C59 H55 0.9500 . ? C60 C61 1.43(3) . ? C60 H56 0.9500 . ? C61 C63 1.54(3) . ? C62 H57 0.9800 . ? C62 H58 0.9800 . ? C62 H59 0.9800 . ? C63 H60 0.9800 . ? C63 H61 0.9800 . ? C63 H62 0.9800 . ? C64 C69 1.39(4) . ? C64 C65 1.41(3) . ? C65 C66 1.40(3) . ? C65 H63 0.9500 . ? C66 C67 1.38(3) . ? C66 C70 1.40(4) . ? C67 C68 1.41(3) . ? C67 H64 0.9500 . ? C68 C69 1.45(4) . ? C68 C78 1.50(3) . ? C69 H65 0.9500 . ? C70 C75 1.41(4) . ? C70 C71 1.44(5) . ? C71 C72 1.50(5) . ? C71 C76 1.50(5) . ? C72 C73 1.39(6) . ? C72 H66 0.9500 . ? C73 C74 1.35(5) . ? C73 H67 0.9500 . ? C74 C75 1.40(4) . ? C74 H68 0.9500 . ? C75 C77 1.68(4) . ? C76 H69 0.9800 . ? C76 H70 0.9800 . ? C76 H71 0.9800 . ? C77 H72 0.9800 . ? C77 H73 0.9800 . ? C77 H74 0.9800 . ? C78 C83 1.43(4) . ? C78 C79 1.43(4) . ? C79 C80 1.43(3) . ? C79 C84 1.55(4) . ? C80 C81 1.31(4) . ? C80 H75 0.9500 . ? C81 C82 1.44(4) . ? C81 H76 0.9500 . ? C82 C83 1.34(4) . ? C82 H77 0.9500 . ? C83 C85 1.46(5) . ? C84 H78 0.9800 . ? C84 H79 0.9800 . ? C84 H80 0.9800 . ? C85 H81 0.9800 . ? C85 H82 0.9800 . ? C85 H83 0.9800 . ? C86 N3 1.361(12) . ? C86 N4 1.365(13) . ? N3 C87 1.380(13) . ? N3 C89 1.478(12) . ? C87 C88 1.335(14) . ? C87 H84 0.9500 . ? C88 N4 1.386(14) . ? C88 H85 0.9500 . ? N4 C111 1.40(2) . ? N4 C149 1.58(4) . ? C89 C94 1.381(15) . ? C89 C90 1.397(14) . ? C90 C91 1.402(13) . ? C90 H86 0.9500 . ? C91 C92 1.393(15) . ? C91 C133 1.52(4) . ? C91 C95 1.54(3) . ? C92 C93 1.370(15) . ? C92 H87 0.9500 . ? C93 C94 1.414(15) . ? C93 C141 1.51(2) . ? C93 C103 1.534(16) . ? C94 H88 0.9500 . ? C95 C96 1.40(5) . ? C95 C100 1.48(4) . ? C96 C101 1.47(6) . ? C96 C97 1.51(6) . ? C97 C98 1.27(5) . ? C97 H89 0.9500 . ? C98 C99 1.43(4) . ? C98 H90 0.9500 . ? C99 C100 1.38(3) . ? C99 H91 0.9500 . ? C100 C102 1.51(3) . ? C101 H92 0.9800 . ? C101 H93 0.9800 . ? C101 H94 0.9800 . ? C102 H95 0.9800 . ? C102 H96 0.9800 . ? C102 H97 0.9800 . ? C103 C104 1.3903 . ? C103 C108 1.42(3) . ? C104 C105 1.3915(18) . ? C104 C109 1.58(2) . ? C105 C106 1.38(3) . ? C105 H98 0.9500 . ? C106 C107 1.49(4) . ? C106 H99 0.9500 . ? C107 C108 1.41(3) . ? C107 H100 0.9500 . ? C108 C110 1.57(3) . ? C109 H101 0.9800 . ? C109 H102 0.9800 . ? C109 H103 0.9800 . ? C110 H104 0.9800 . ? C110 H105 0.9800 . ? C110 H106 0.9800 . ? C111 C116 1.40(3) . ? C111 C112 1.46(3) . ? C112 C113 1.39(3) . ? C112 H107 0.9500 . ? C113 C114 1.37(4) . ? C113 C117 1.53(3) . ? C114 C115 1.39(4) . ? C114 H108 0.9500 . ? C115 C116 1.37(3) . ? C115 C125 1.45(3) . ? C116 H109 0.9500 . ? C117 C122 1.38(2) . ? C117 C118 1.3900 . ? C118 C119 1.3900 . ? C118 C123 1.56(3) . ? C119 C120 1.43(3) . ? C119 H110 0.9500 . ? C120 C121 1.32(3) . ? C120 H111 0.9500 . ? C121 C122 1.45(3) . ? C121 H112 0.9500 . ? C122 C124 1.49(3) . ? C123 H113 0.9800 . ? C123 H114 0.9800 . ? C123 H115 0.9800 . ? C124 H116 0.9800 . ? C124 H117 0.9800 . ? C124 H118 0.9800 . ? C125 C126 1.31(3) . ? C125 C130 1.48(4) . ? C126 C127 1.38(4) . ? C126 C131 1.65(4) . ? C127 C128 1.74(4) . ? C127 H119 0.9500 . ? C128 C129 1.16(3) . ? C128 H120 0.9500 . ? C129 C130 1.51(4) . ? C129 H121 0.9500 . ? C130 C132 1.35(4) . ? C131 H122 0.9800 . ? C131 H123 0.9800 . ? C131 H124 0.9800 . ? C132 H125 0.9800 . ? C132 H126 0.9800 . ? C132 H127 0.9800 . ? C133 C138 1.27(4) . ? C133 C134 1.53(5) . ? C134 C135 1.36(5) . ? C134 C139 1.58(5) . ? C135 C136 1.42(5) . ? C135 H128 0.9500 . ? C136 C137 1.38(4) . ? C136 H129 0.9500 . ? C137 C138 1.36(3) . ? C137 H130 0.9500 . ? C138 C140 1.52(3) . ? C139 H131 0.9800 . ? C139 H132 0.9800 . ? C139 H133 0.9800 . ? C140 H134 0.9800 . ? C140 H135 0.9800 . ? C140 H136 0.9800 . ? C141 C146 1.31(4) . ? C141 C142 1.3897(18) . ? C142 C143 1.389(3) . ? C142 C147 1.50(4) . ? C143 C144 1.23(4) . ? C143 H137 0.9500 . ? C144 C145 1.55(6) . ? C144 H138 0.9500 . ? C145 C146 1.41(5) . ? C145 H139 0.9500 . ? C146 C148 1.66(5) . ? C147 H140 0.9800 . ? C147 H141 0.9800 . ? C147 H142 0.9800 . ? C148 H143 0.9800 . ? C148 H144 0.9800 . ? C148 H145 0.9800 . ? C149 C150 1.26(5) . ? C149 C154 1.31(4) . ? C150 C151 1.56(5) . ? C150 H146 0.9500 . ? C151 C155 1.43(5) . ? C151 C152 1.44(6) . ? C152 C153 1.37(5) . ? C152 H147 0.9500 . ? C153 C154 1.38(3) . ? C153 C163 1.64(4) . ? C154 H148 0.9500 . ? C155 C156 1.34(4) . ? C155 C160 1.36(4) . ? C156 C157 1.54(5) . ? C156 C161 1.57(5) . ? C157 C158 1.37(6) . ? C157 H149 0.9500 . ? C158 C159 1.27(5) . ? C158 H150 0.9500 . ? C159 C160 1.45(4) . ? C159 H151 0.9500 . ? C160 C162 1.46(4) . ? C161 H152 0.9800 . ? C161 H153 0.9800 . ? C161 H154 0.9800 . ? C162 H155 0.9800 . ? C162 H156 0.9800 . ? C162 H157 0.9800 . ? C163 C164 1.25(4) . ? C163 C168 1.48(5) . ? C164 C165 1.28(4) . ? C164 C169 1.70(4) . ? C165 C166 1.83(5) . ? C165 H158 0.9500 . ? C166 C167 1.36(4) . ? C166 H159 0.9500 . ? C167 C168 1.42(4) . ? C167 H160 0.9500 . ? C168 C170 1.53(4) . ? C169 H161 0.9800 . ? C169 H162 0.9800 . ? C169 H163 0.9800 . ? C170 H164 0.9800 . ? C170 H165 0.9800 . ? C170 H166 0.9800 . ? C171 C172 1.522(19) . ? C171 H167 0.9800 . ? C171 H168 0.9800 . ? C171 H169 0.9800 . ? C172 C173 1.51(2) . ? C172 H170 0.9900 . ? C172 H171 0.9900 . ? C173 C174 1.58(2) . ? C173 H172 0.9900 . ? C173 H173 0.9900 . ? C174 C175 1.52(2) . ? C174 H174 0.9900 . ? C174 H175 0.9900 . ? C175 C176 1.513(19) . ? C175 H176 0.9900 . ? C175 H177 0.9900 . ? C176 H178 0.9800 . ? C176 H179 0.9800 . ? C176 H180 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 C1 Pd1 O1 106.5(4) . . ? C1 Pd1 O2 149.6(4) . . ? O1 Pd1 O2 43.2(3) . . ? C1 Pd1 C86 99.2(4) . . ? O1 Pd1 C86 154.2(4) . . ? O2 Pd1 C86 111.1(4) . . ? O2 O1 Pd1 68.8(4) . . ? O1 O2 Pd1 68.1(4) . . ? N1 C1 N2 101.5(8) . . ? N1 C1 Pd1 129.5(7) . . ? N2 C1 Pd1 128.1(7) . . ? C1 N1 C2 112.1(8) . . ? C1 N1 C4 124.1(8) . . ? C2 N1 C4 123.5(8) . . ? C3 C2 N1 106.8(9) . . ? C3 C2 H1 126.6 . . ? N1 C2 H1 126.6 . . ? C2 C3 N2 107.4(9) . . ? C2 C3 H2 126.3 . . ? N2 C3 H2 126.3 . . ? C1 N2 C3 112.3(8) . . ? C1 N2 C26 130.4(12) . . ? C3 N2 C26 117.0(12) . . ? C1 N2 C64 117.3(13) . . ? C3 N2 C64 129.8(13) . . ? C26 N2 C64 17.5(13) . . ? C9 C4 C5 119.9(10) . . ? C9 C4 N1 120.3(10) . . ? C5 C4 N1 119.8(9) . . ? C4 C5 C6 120.2(11) . . ? C4 C5 H3 119.9 . . ? C6 C5 H3 119.9 . . ? C5 C6 C7 118.1(11) . . ? C5 C6 C10 129.8(18) . . ? C7 C6 C10 112.0(18) . . ? C5 C6 C48 115.2(14) . . ? C7 C6 C48 126.6(14) . . ? C10 C6 C48 15.1(19) . . ? C8 C7 C6 121.9(11) . . ? C8 C7 H4 119.1 . . ? C6 C7 H4 119.1 . . ? C18 C8 C7 109.5(17) . . ? C18 C8 C9 132.6(17) . . ? C7 C8 C9 117.9(11) . . ? C18 C8 C56 17.3(15) . . ? C7 C8 C56 126.4(13) . . ? C9 C8 C56 115.7(12) . . ? C4 C9 C8 121.9(11) . . ? C4 C9 H5 119.0 . . ? C8 C9 H5 119.0 . . ? C11 C10 C6 117(3) . . ? C11 C10 C15 128(3) . . ? C6 C10 C15 115(3) . . ? C10 C11 C12 116(3) . . ? C10 C11 C16 120(3) . . ? C12 C11 C16 121(3) . . ? C13 C12 C11 122(3) . . ? C13 C12 H6 118.8 . . ? C11 C12 H6 118.8 . . ? C12 C13 C14 119(3) . . ? C12 C13 H7 120.7 . . ? C14 C13 H7 120.7 . . ? C15 C14 C13 123(4) . . ? C15 C14 H8 118.5 . . ? C13 C14 H8 118.6 . . ? C14 C15 C10 112(4) . . ? C14 C15 C17 125(4) . . ? C10 C15 C17 123(3) . . ? C11 C16 H9 109.5 . . ? C11 C16 H10 109.5 . . ? H9 C16 H10 109.5 . . ? C11 C16 H11 109.5 . . ? H9 C16 H11 109.5 . . ? H10 C16 H11 109.5 . . ? C15 C17 H12 109.5 . . ? C15 C17 H13 109.5 . . ? H12 C17 H13 109.5 . . ? C15 C17 H14 109.5 . . ? H12 C17 H14 109.5 . . ? H13 C17 H14 109.5 . . ? C8 C18 C19 120(2) . . ? C8 C18 C23 123(2) . . ? C19 C18 C23 116(3) . . ? C18 C19 C20 124(3) . . ? C18 C19 C24 119(3) . . ? C20 C19 C24 117(3) . . ? C19 C20 C21 117(3) . . ? C19 C20 H15 121.3 . . ? C21 C20 H15 121.3 . . ? C22 C21 C20 118(3) . . ? C22 C21 H16 121.0 . . ? C20 C21 H16 121.0 . . ? C23 C22 C21 125(3) . . ? C23 C22 H17 117.4 . . ? C21 C22 H17 117.4 . . ? C22 C23 C25 124(3) . . ? C22 C23 C18 119(3) . . ? C25 C23 C18 116(3) . . ? C19 C24 H18 109.5 . . ? C19 C24 H19 109.5 . . ? H18 C24 H19 109.5 . . ? C19 C24 H20 109.5 . . ? H18 C24 H20 109.5 . . ? H19 C24 H20 109.5 . . ? C23 C25 H21 109.5 . . ? C23 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C23 C25 H23 109.5 . . ? H21 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C31 C26 C27 122(2) . . ? C31 C26 N2 121(2) . . ? C27 C26 N2 117.2(18) . . ? C28 C27 C26 119.2(19) . . ? C28 C27 H24 120.4 . . ? C26 C27 H24 120.4 . . ? C29 C28 C27 118.0(18) . . ? C29 C28 C32 121.1(18) . . ? C27 C28 C32 120.5(17) . . ? C30 C29 C28 125(2) . . ? C30 C29 H25 117.5 . . ? C28 C29 H25 117.5 . . ? C29 C30 C31 119(2) . . ? C29 C30 C40 120(2) . . ? C31 C30 C40 121(2) . . ? C26 C31 C30 117(2) . . ? C26 C31 H26 121.5 . . ? C30 C31 H26 121.5 . . ? C33 C32 C37 123(3) . . ? C33 C32 C28 119(2) . . ? C37 C32 C28 119(2) . . ? C32 C33 C34 120(3) . . ? C32 C33 C38 125(2) . . ? C34 C33 C38 115(2) . . ? C35 C34 C33 114(3) . . ? C35 C34 H27 122.8 . . ? C33 C34 H27 122.8 . . ? C36 C35 C34 125(3) . . ? C36 C35 H28 117.5 . . ? C34 C35 H28 117.5 . . ? C35 C36 C37 118(3) . . ? C35 C36 H29 121.1 . . ? C37 C36 H29 121.1 . . ? C32 C37 C36 120(2) . . ? C32 C37 C39 125(2) . . ? C36 C37 C39 115(2) . . ? C41 C40 C45 122(2) . . ? C41 C40 C30 120(2) . . ? C45 C40 C30 118(2) . . ? C42 C41 C40 119(2) . . ? C42 C41 C46 118(2) . . ? C40 C41 C46 124(2) . . ? C41 C42 C43 123(2) . . ? C41 C42 H36 118.6 . . ? C43 C42 H36 118.6 . . ? C44 C43 C42 120(3) . . ? C44 C43 H37 119.9 . . ? C42 C43 H37 119.9 . . ? C43 C44 C45 120(3) . . ? C43 C44 H38 120.1 . . ? C45 C44 H38 120.1 . . ? C40 C45 C44 116(2) . . ? C40 C45 C47 125(3) . . ? C44 C45 C47 119(3) . . ? C49 C48 C53 124(3) . . ? C49 C48 C6 117(2) . . ? C53 C48 C6 119(2) . . ? C48 C49 C54 126(2) . . ? C48 C49 C50 115(3) . . ? C54 C49 C50 119(2) . . ? C51 C50 C49 120(3) . . ? C51 C50 H45 119.8 . . ? C49 C50 H45 119.8 . . ? C50 C51 C52 122(3) . . ? C50 C51 H46 119.2 . . ? C52 C51 H46 119.2 . . ? C53 C52 C51 123(3) . . ? C53 C52 H47 118.3 . . ? C51 C52 H47 118.3 . . ? C52 C53 C48 115(3) . . ? C52 C53 C55 123(3) . . ? C48 C53 C55 122(2) . . ? C61 C56 C57 125(2) . . ? C61 C56 C8 114.9(19) . . ? C57 C56 C8 119.9(17) . . ? C56 C57 C58 116(2) . . ? C56 C57 C62 125(2) . . ? C58 C57 C62 119(2) . . ? C59 C58 C57 117(2) . . ? C59 C58 H54 121.6 . . ? C57 C58 H54 121.6 . . ? C60 C59 C58 126(3) . . ? C60 C59 H55 117.0 . . ? C58 C59 H55 117.0 . . ? C59 C60 C61 119(2) . . ? C59 C60 H56 120.6 . . ? C61 C60 H56 120.6 . . ? C56 C61 C60 117(2) . . ? C56 C61 C63 125(2) . . ? C60 C61 C63 117(2) . . ? C69 C64 C65 121(2) . . ? C69 C64 N2 119(2) . . ? C65 C64 N2 118.4(19) . . ? C66 C65 C64 121(2) . . ? C66 C65 H63 119.5 . . ? C64 C65 H63 119.5 . . ? C67 C66 C70 120(2) . . ? C67 C66 C65 118(2) . . ? C70 C66 C65 122(2) . . ? C66 C67 C68 123(2) . . ? C66 C67 H64 118.3 . . ? C68 C67 H64 118.3 . . ? C67 C68 C69 118(2) . . ? C67 C68 C78 123(2) . . ? C69 C68 C78 119(2) . . ? C64 C69 C68 118(3) . . ? C64 C69 H65 120.9 . . ? C68 C69 H65 120.9 . . ? C66 C70 C75 124(3) . . ? C66 C70 C71 124(3) . . ? C75 C70 C71 112(3) . . ? C70 C71 C72 124(3) . . ? C70 C71 C76 124(3) . . ? C72 C71 C76 112(4) . . ? C73 C72 C71 113(4) . . ? C73 C72 H66 123.7 . . ? C71 C72 H66 123.7 . . ? C74 C73 C72 128(4) . . ? C74 C73 H67 116.1 . . ? C72 C73 H67 116.1 . . ? C73 C74 C75 115(4) . . ? C73 C74 H68 122.4 . . ? C75 C74 H68 122.4 . . ? C74 C75 C70 128(3) . . ? C74 C75 C77 117(3) . . ? C70 C75 C77 115(2) . . ? C71 C76 H69 109.5 . . ? C71 C76 H70 109.5 . . ? H69 C76 H70 109.5 . . ? C71 C76 H71 109.5 . . ? H69 C76 H71 109.5 . . ? H70 C76 H71 109.5 . . ? C75 C77 H72 109.5 . . ? C75 C77 H73 109.5 . . ? H72 C77 H73 109.5 . . ? C75 C77 H74 109.5 . . ? H72 C77 H74 109.5 . . ? H73 C77 H74 109.5 . . ? C83 C78 C79 118(2) . . ? C83 C78 C68 123(2) . . ? C79 C78 C68 119(3) . . ? C80 C79 C78 118(2) . . ? C80 C79 C84 119(2) . . ? C78 C79 C84 123(2) . . ? C81 C80 C79 123(3) . . ? C81 C80 H75 118.7 . . ? C79 C80 H75 118.7 . . ? C80 C81 C82 118(3) . . ? C80 C81 H76 120.8 . . ? C82 C81 H76 120.8 . . ? C83 C82 C81 123(3) . . ? C83 C82 H77 118.6 . . ? C81 C82 H77 118.6 . . ? C82 C83 C78 118(3) . . ? C82 C83 C85 122(3) . . ? C78 C83 C85 119(3) . . ? C79 C84 H78 109.5 . . ? C79 C84 H79 109.5 . . ? H78 C84 H79 109.5 . . ? C79 C84 H80 109.5 . . ? H78 C84 H80 109.5 . . ? H79 C84 H80 109.5 . . ? C83 C85 H81 109.5 . . ? C83 C85 H82 109.5 . . ? H81 C85 H82 109.5 . . ? C83 C85 H83 109.5 . . ? H81 C85 H83 109.5 . . ? H82 C85 H83 109.5 . . ? N3 C86 N4 101.2(9) . . ? N3 C86 Pd1 136.6(8) . . ? N4 C86 Pd1 121.7(8) . . ? C86 N3 C87 113.9(9) . . ? C86 N3 C89 128.9(9) . . ? C87 N3 C89 116.9(8) . . ? C88 C87 N3 105.5(10) . . ? C88 C87 H84 127.2 . . ? N3 C87 H84 127.2 . . ? C87 C88 N4 106.8(10) . . ? C87 C88 H85 126.6 . . ? N4 C88 H85 126.6 . . ? C86 N4 C88 112.6(9) . . ? C86 N4 C111 124.0(13) . . ? C88 N4 C111 123.3(12) . . ? C86 N4 C149 128.4(16) . . ? C88 N4 C149 116.8(16) . . ? C111 N4 C149 17.9(16) . . ? C94 C89 C90 120.8(10) . . ? C94 C89 N3 123.1(9) . . ? C90 C89 N3 115.4(10) . . ? C89 C90 C91 119.9(11) . . ? C89 C90 H86 120.0 . . ? C91 C90 H86 120.0 . . ? C92 C91 C90 118.0(10) . . ? C92 C91 C133 124.2(16) . . ? C90 C91 C133 116.3(17) . . ? C92 C91 C95 121.9(13) . . ? C90 C91 C95 120.0(13) . . ? C133 C91 C95 14.1(18) . . ? C93 C92 C91 123.0(10) . . ? C93 C92 H87 118.5 . . ? C91 C92 H87 118.5 . . ? C92 C93 C94 118.4(11) . . ? C92 C93 C141 123.3(12) . . ? C94 C93 C141 115.5(12) . . ? C92 C93 C103 116.7(10) . . ? C94 C93 C103 124.7(11) . . ? C141 C93 C103 22.1(8) . . ? C89 C94 C93 119.8(11) . . ? C89 C94 H88 120.1 . . ? C93 C94 H88 120.1 . . ? C96 C95 C100 122(3) . . ? C96 C95 C91 121(3) . . ? C100 C95 C91 117(2) . . ? C95 C96 C101 120(4) . . ? C95 C96 C97 112(4) . . ? C101 C96 C97 127(4) . . ? C98 C97 C96 126(4) . . ? C98 C97 H89 117.2 . . ? C96 C97 H89 117.2 . . ? C97 C98 C99 122(3) . . ? C97 C98 H90 119.2 . . ? C99 C98 H90 119.2 . . ? C100 C99 C98 119(2) . . ? C100 C99 H91 120.6 . . ? C98 C99 H91 120.6 . . ? C99 C100 C95 119(2) . . ? C99 C100 C102 119(2) . . ? C95 C100 C102 122(2) . . ? C104 C103 C108 117.5(11) . . ? C104 C103 C93 128.0(7) . . ? C108 C103 C93 114.4(13) . . ? C103 C104 C105 120.0 . . ? C103 C104 C109 120.2(9) . . ? C105 C104 C109 119.4(9) . . ? C106 C105 C104 120.8(12) . . ? C106 C105 H98 119.6 . . ? C104 C105 H98 119.6 . . ? C105 C106 C107 124(2) . . ? C105 C106 H99 118.0 . . ? C107 C106 H99 118.0 . . ? C108 C107 C106 109(2) . . ? C108 C107 H100 125.5 . . ? C106 C107 H100 125.5 . . ? C107 C108 C103 128(2) . . ? C107 C108 C110 109(2) . . ? C103 C108 C110 122.2(18) . . ? C116 C111 N4 116.2(19) . . ? C116 C111 C112 118.4(19) . . ? N4 C111 C112 125(2) . . ? C113 C112 C111 120(2) . . ? C113 C112 H107 120.1 . . ? C111 C112 H107 120.1 . . ? C114 C113 C112 118(2) . . ? C114 C113 C117 122.9(18) . . ? C112 C113 C117 119(2) . . ? C113 C114 C115 124(3) . . ? C113 C114 H108 118.1 . . ? C115 C114 H108 118.1 . . ? C116 C115 C114 119(2) . . ? C116 C115 C125 118(2) . . ? C114 C115 C125 123(3) . . ? C115 C116 C111 120.5(16) . . ? C115 C116 H109 119.7 . . ? C111 C116 H109 119.7 . . ? C122 C117 C118 120.7(10) . . ? C122 C117 C113 120.6(15) . . ? C118 C117 C113 118.7(10) . . ? C117 C118 C119 120.0 . . ? C117 C118 C123 121.9(10) . . ? C119 C118 C123 117.8(10) . . ? C118 C119 C120 120.3(11) . . ? C118 C119 H110 119.8 . . ? C120 C119 H110 119.9 . . ? C121 C120 C119 119(2) . . ? C121 C120 H111 120.7 . . ? C119 C120 H111 120.7 . . ? C120 C121 C122 123(2) . . ? C120 C121 H112 118.7 . . ? C122 C121 H112 118.7 . . ? C117 C122 C121 117.6(18) . . ? C117 C122 C124 121.7(18) . . ? C121 C122 C124 120.6(19) . . ? C126 C125 C115 123(3) . . ? C126 C125 C130 119(3) . . ? C115 C125 C130 118(2) . . ? C125 C126 C127 132(3) . . ? C125 C126 C131 120(3) . . ? C127 C126 C131 108(3) . . ? C126 C127 C128 107(2) . . ? C126 C127 H119 126.6 . . ? C128 C127 H119 126.6 . . ? C129 C128 C127 119(3) . . ? C129 C128 H120 120.6 . . ? C127 C128 H120 120.6 . . ? C128 C129 C130 128(3) . . ? C128 C129 H121 115.8 . . ? C130 C129 H121 115.8 . . ? C132 C130 C125 125(3) . . ? C132 C130 C129 121(3) . . ? C125 C130 C129 113(3) . . ? C138 C133 C91 128(3) . . ? C138 C133 C134 122(3) . . ? C91 C133 C134 110(3) . . ? C135 C134 C133 118(3) . . ? C135 C134 C139 116(3) . . ? C133 C134 C139 125(3) . . ? C134 C135 C136 115(3) . . ? C134 C135 H128 122.4 . . ? C136 C135 H128 122.4 . . ? C137 C136 C135 123(3) . . ? C137 C136 H129 118.5 . . ? C135 C136 H129 118.5 . . ? C138 C137 C136 121(3) . . ? C138 C137 H130 119.5 . . ? C136 C137 H130 119.5 . . ? C133 C138 C137 119(3) . . ? C133 C138 C140 118(3) . . ? C137 C138 C140 122(3) . . ? C134 C139 H131 109.5 . . ? C134 C139 H132 109.5 . . ? H131 C139 H132 109.5 . . ? C134 C139 H133 109.5 . . ? H131 C139 H133 109.5 . . ? H132 C139 H133 109.5 . . ? C138 C140 H134 109.5 . . ? C138 C140 H135 109.5 . . ? H134 C140 H135 109.5 . . ? C138 C140 H136 109.5 . . ? H134 C140 H136 109.5 . . ? H135 C140 H136 109.5 . . ? C146 C141 C142 120.7(19) . . ? C146 C141 C93 128(2) . . ? C142 C141 C93 111.0(9) . . ? C143 C142 C141 119.99(11) . . ? C143 C142 C147 111.0(13) . . ? C141 C142 C147 128.9(13) . . ? C144 C143 C142 116(2) . . ? C144 C143 H137 121.8 . . ? C142 C143 H137 121.8 . . ? C143 C144 C145 131(4) . . ? C143 C144 H138 114.7 . . ? C145 C144 H138 114.7 . . ? C146 C145 C144 105(4) . . ? C146 C145 H139 127.4 . . ? C144 C145 H139 127.4 . . ? C141 C146 C145 126(4) . . ? C141 C146 C148 123(3) . . ? C145 C146 C148 109(4) . . ? C142 C147 H140 109.5 . . ? C142 C147 H141 109.5 . . ? H140 C147 H141 109.5 . . ? C142 C147 H142 109.5 . . ? H140 C147 H142 109.5 . . ? H141 C147 H142 109.5 . . ? C146 C148 H143 109.5 . . ? C146 C148 H144 109.5 . . ? H143 C148 H144 109.5 . . ? C146 C148 H145 109.5 . . ? H143 C148 H145 109.5 . . ? H144 C148 H145 109.5 . . ? C150 C149 C154 130(4) . . ? C150 C149 N4 107(3) . . ? C154 C149 N4 123(3) . . ? C149 C150 C151 120(4) . . ? C149 C150 H146 120.1 . . ? C151 C150 H146 120.1 . . ? C155 C151 C152 126(4) . . ? C155 C151 C150 123(4) . . ? C152 C151 C150 110(3) . . ? C153 C152 C151 122(3) . . ? C153 C152 H147 119.2 . . ? C151 C152 H147 119.2 . . ? C152 C153 C154 124(3) . . ? C152 C153 C163 114(2) . . ? C154 C153 C163 121(2) . . ? C149 C154 C153 115(3) . . ? C149 C154 H148 122.6 . . ? C153 C154 H148 122.6 . . ? C156 C155 C160 123(3) . . ? C156 C155 C151 121(3) . . ? C160 C155 C151 116(3) . . ? C155 C156 C157 119(3) . . ? C155 C156 C161 128(3) . . ? C157 C156 C161 112(3) . . ? C158 C157 C156 109(4) . . ? C158 C157 H149 125.7 . . ? C156 C157 H149 125.7 . . ? C159 C158 C157 135(5) . . ? C159 C158 H150 112.6 . . ? C157 C158 H150 112.6 . . ? C158 C159 C160 114(3) . . ? C158 C159 H151 123.2 . . ? C160 C159 H151 123.2 . . ? C155 C160 C159 120(3) . . ? C155 C160 C162 124(3) . . ? C159 C160 C162 116(3) . . ? C156 C161 H152 109.5 . . ? C156 C161 H153 109.5 . . ? H152 C161 H153 109.5 . . ? C156 C161 H154 109.5 . . ? H152 C161 H154 109.5 . . ? H153 C161 H154 109.5 . . ? C160 C162 H155 109.5 . . ? C160 C162 H156 109.5 . . ? H155 C162 H156 109.5 . . ? C160 C162 H157 109.5 . . ? H155 C162 H157 109.5 . . ? H156 C162 H157 109.5 . . ? C164 C163 C168 122(3) . . ? C164 C163 C153 128(3) . . ? C168 C163 C153 109(2) . . ? C163 C164 C165 142(4) . . ? C163 C164 C169 115(3) . . ? C165 C164 C169 103(3) . . ? C164 C165 C166 99(3) . . ? C164 C165 H158 130.7 . . ? C166 C165 H158 130.7 . . ? C167 C166 C165 120(3) . . ? C167 C166 H159 119.8 . . ? C165 C166 H159 119.8 . . ? C166 C167 C168 122(3) . . ? C166 C167 H160 119.0 . . ? C168 C167 H160 119.0 . . ? C167 C168 C163 114(3) . . ? C167 C168 C170 120(3) . . ? C163 C168 C170 126(3) . . ? C164 C169 H161 109.5 . . ? C164 C169 H162 109.5 . . ? H161 C169 H162 109.5 . . ? C164 C169 H163 109.5 . . ? H161 C169 H163 109.5 . . ? H162 C169 H163 109.5 . . ? C168 C170 H164 109.5 . . ? C168 C170 H165 109.5 . . ? H164 C170 H165 109.5 . . ? C168 C170 H166 109.5 . . ? H164 C170 H166 109.5 . . ? H165 C170 H166 109.5 . . ? C172 C171 H167 109.5 . . ? C172 C171 H168 109.5 . . ? H167 C171 H168 109.5 . . ? C172 C171 H169 109.5 . . ? H167 C171 H169 109.5 . . ? H168 C171 H169 109.5 . . ? C173 C172 C171 116(2) . . ? C173 C172 H170 108.2 . . ? C171 C172 H170 108.2 . . ? C173 C172 H171 108.2 . . ? C171 C172 H171 108.2 . . ? H170 C172 H171 107.4 . . ? C172 C173 C174 110(2) . . ? C172 C173 H172 109.6 . . ? C174 C173 H172 109.6 . . ? C172 C173 H173 109.6 . . ? C174 C173 H173 109.6 . . ? H172 C173 H173 108.1 . . ? C175 C174 C173 109(2) . . ? C175 C174 H174 110.0 . . ? C173 C174 H174 110.0 . . ? C175 C174 H175 110.0 . . ? C173 C174 H175 110.0 . . ? H174 C174 H175 108.3 . . ? C176 C175 C174 117(2) . . ? C176 C175 H176 107.9 . . ? C174 C175 H176 107.9 . . ? C176 C175 H177 107.9 . . ? C174 C175 H177 107.9 . . ? H176 C175 H177 107.2 . . ? C175 C176 H178 109.5 . . ? C175 C176 H179 109.5 . . ? H178 C176 H179 109.5 . . ? C175 C176 H180 109.5 . . ? H178 C176 H180 109.5 . . ? H179 C176 H180 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 -177.2(5) . . . . ? C86 Pd1 O1 O2 -1.0(11) . . . . ? C1 Pd1 O2 O1 5.2(10) . . . . ? C86 Pd1 O2 O1 179.5(5) . . . . ? O1 Pd1 C1 N1 87.6(9) . . . . ? O2 Pd1 C1 N1 83.9(12) . . . . ? C86 Pd1 C1 N1 -90.7(9) . . . . ? O1 Pd1 C1 N2 -79.1(9) . . . . ? O2 Pd1 C1 N2 -82.8(11) . . . . ? C86 Pd1 C1 N2 102.6(9) . . . . ? N2 C1 N1 C2 -1.2(10) . . . . ? Pd1 C1 N1 C2 -170.5(7) . . . . ? N2 C1 N1 C4 173.3(8) . . . . ? Pd1 C1 N1 C4 3.9(13) . . . . ? C1 N1 C2 C3 1.3(11) . . . . ? C4 N1 C2 C3 -173.2(9) . . . . ? N1 C2 C3 N2 -0.8(12) . . . . ? N1 C1 N2 C3 0.7(10) . . . . ? Pd1 C1 N2 C3 170.2(7) . . . . ? N1 C1 N2 C26 -173.3(15) . . . . ? Pd1 C1 N2 C26 -3.7(19) . . . . ? N1 C1 N2 C64 172.6(13) . . . . ? Pd1 C1 N2 C64 -17.8(16) . . . . ? C2 C3 N2 C1 0.1(12) . . . . ? C2 C3 N2 C26 174.9(13) . . . . ? C2 C3 N2 C64 -170.6(15) . . . . ? C1 N1 C4 C9 -142.2(9) . . . . ? C2 N1 C4 C9 31.6(13) . . . . ? C1 N1 C4 C5 40.4(13) . . . . ? C2 N1 C4 C5 -145.8(9) . . . . ? C9 C4 C5 C6 -0.4(14) . . . . ? N1 C4 C5 C6 177.0(8) . . . . ? C4 C5 C6 C7 0.3(14) . . . . ? C4 C5 C6 C10 177(2) . . . . ? C4 C5 C6 C48 -178.1(13) . . . . ? C5 C6 C7 C8 -1.2(15) . . . . ? C10 C6 C7 C8 -178.5(17) . . . . ? C48 C6 C7 C8 176.9(15) . . . . ? C6 C7 C8 C18 -176.4(15) . . . . ? C6 C7 C8 C9 2.2(16) . . . . ? C6 C7 C8 C56 179.2(12) . . . . ? C5 C4 C9 C8 1.4(15) . . . . ? N1 C4 C9 C8 -176.0(9) . . . . ? C18 C8 C9 C4 175.9(19) . . . . ? C7 C8 C9 C4 -2.3(15) . . . . ? C56 C8 C9 C4 -179.6(11) . . . . ? C5 C6 C10 C11 85(3) . . . . ? C7 C6 C10 C11 -98(3) . . . . ? C48 C6 C10 C11 68(8) . . . . ? C5 C6 C10 C15 -84(4) . . . . ? C7 C6 C10 C15 93(3) . . . . ? C48 C6 C10 C15 -101(9) . . . . ? C6 C10 C11 C12 -173(3) . . . . ? C15 C10 C11 C12 -6(6) . . . . ? C6 C10 C11 C16 26(5) . . . . ? C15 C10 C11 C16 -167(4) . . . . ? C10 C11 C12 C13 11(6) . . . . ? C16 C11 C12 C13 172(4) . . . . ? C11 C12 C13 C14 -13(6) . . . . ? C12 C13 C14 C15 10(6) . . . . ? C13 C14 C15 C10 -5(6) . . . . ? C13 C14 C15 C17 -180(4) . . . . ? C11 C10 C15 C14 3(6) . . . . ? C6 C10 C15 C14 171(3) . . . . ? C11 C10 C15 C17 179(4) . . . . ? C6 C10 C15 C17 -14(5) . . . . ? C7 C8 C18 C19 -108(3) . . . . ? C9 C8 C18 C19 74(4) . . . . ? C56 C8 C18 C19 60(5) . . . . ? C7 C8 C18 C23 81(3) . . . . ? C9 C8 C18 C23 -97(3) . . . . ? C56 C8 C18 C23 -111(7) . . . . ? C8 C18 C19 C20 -169(3) . . . . ? C23 C18 C19 C20 3(5) . . . . ? C8 C18 C19 C24 9(5) . . . . ? C23 C18 C19 C24 -179(3) . . . . ? C18 C19 C20 C21 -4(5) . . . . ? C24 C19 C20 C21 178(3) . . . . ? C19 C20 C21 C22 2(5) . . . . ? C20 C21 C22 C23 1(5) . . . . ? C21 C22 C23 C25 -176(3) . . . . ? C21 C22 C23 C18 -2(5) . . . . ? C8 C18 C23 C22 172(3) . . . . ? C19 C18 C23 C22 1(4) . . . . ? C8 C18 C23 C25 -14(4) . . . . ? C19 C18 C23 C25 175(3) . . . . ? C1 N2 C26 C31 40(3) . . . . ? C3 N2 C26 C31 -134(2) . . . . ? C64 N2 C26 C31 86(6) . . . . ? C1 N2 C26 C27 -136.1(17) . . . . ? C3 N2 C26 C27 50(2) . . . . ? C64 N2 C26 C27 -90(6) . . . . ? C31 C26 C27 C28 -2(4) . . . . ? N2 C26 C27 C28 173.9(18) . . . . ? C26 C27 C28 C29 1(3) . . . . ? C26 C27 C28 C32 174(2) . . . . ? C27 C28 C29 C30 2(4) . . . . ? C32 C28 C29 C30 -171(2) . . . . ? C28 C29 C30 C31 -4(4) . . . . ? C28 C29 C30 C40 175(2) . . . . ? C27 C26 C31 C30 0(4) . . . . ? N2 C26 C31 C30 -175.7(19) . . . . ? C29 C30 C31 C26 3(4) . . . . ? C40 C30 C31 C26 -176(2) . . . . ? C29 C28 C32 C33 107(2) . . . . ? C27 C28 C32 C33 -65(3) . . . . ? C29 C28 C32 C37 -74(3) . . . . ? C27 C28 C32 C37 114(2) . . . . ? C37 C32 C33 C34 5(3) . . . . ? C28 C32 C33 C34 -175.7(19) . . . . ? C37 C32 C33 C38 -178(2) . . . . ? C28 C32 C33 C38 2(3) . . . . ? C32 C33 C34 C35 -4(3) . . . . ? C38 C33 C34 C35 178.2(19) . . . . ? C33 C34 C35 C36 4(4) . . . . ? C34 C35 C36 C37 -3(4) . . . . ? C33 C32 C37 C36 -4(3) . . . . ? C28 C32 C37 C36 176.5(19) . . . . ? C33 C32 C37 C39 174(2) . . . . ? C28 C32 C37 C39 -6(3) . . . . ? C35 C36 C37 C32 3(4) . . . . ? C35 C36 C37 C39 -175(2) . . . . ? C29 C30 C40 C41 -58(3) . . . . ? C31 C30 C40 C41 121(3) . . . . ? C29 C30 C40 C45 123(3) . . . . ? C31 C30 C40 C45 -59(3) . . . . ? C45 C40 C41 C42 2(4) . . . . ? C30 C40 C41 C42 -177(2) . . . . ? C45 C40 C41 C46 -176(2) . . . . ? C30 C40 C41 C46 5(4) . . . . ? C40 C41 C42 C43 2(4) . . . . ? C46 C41 C42 C43 -180(3) . . . . ? C41 C42 C43 C44 -5(4) . . . . ? C42 C43 C44 C45 3(4) . . . . ? C41 C40 C45 C44 -4(4) . . . . ? C30 C40 C45 C44 176(2) . . . . ? C41 C40 C45 C47 177(3) . . . . ? C30 C40 C45 C47 -4(4) . . . . ? C43 C44 C45 C40 1(4) . . . . ? C43 C44 C45 C47 -180(3) . . . . ? C5 C6 C48 C49 -96(2) . . . . ? C7 C6 C48 C49 85(3) . . . . ? C10 C6 C48 C49 69(8) . . . . ? C5 C6 C48 C53 84(3) . . . . ? C7 C6 C48 C53 -94(3) . . . . ? C10 C6 C48 C53 -111(9) . . . . ? C53 C48 C49 C54 -179(3) . . . . ? C6 C48 C49 C54 1(4) . . . . ? C53 C48 C49 C50 -4(4) . . . . ? C6 C48 C49 C50 175.9(19) . . . . ? C48 C49 C50 C51 -5(4) . . . . ? C54 C49 C50 C51 170(3) . . . . ? C49 C50 C51 C52 14(5) . . . . ? C50 C51 C52 C53 -13(5) . . . . ? C51 C52 C53 C48 3(5) . . . . ? C51 C52 C53 C55 177(3) . . . . ? C49 C48 C53 C52 5(5) . . . . ? C6 C48 C53 C52 -175(2) . . . . ? C49 C48 C53 C55 -169(3) . . . . ? C6 C48 C53 C55 11(4) . . . . ? C18 C8 C56 C61 65(5) . . . . ? C7 C8 C56 C61 79(2) . . . . ? C9 C8 C56 C61 -104(2) . . . . ? C18 C8 C56 C57 -115(6) . . . . ? C7 C8 C56 C57 -101(2) . . . . ? C9 C8 C56 C57 76(2) . . . . ? C61 C56 C57 C58 0(4) . . . . ? C8 C56 C57 C58 179.7(19) . . . . ? C61 C56 C57 C62 172(3) . . . . ? C8 C56 C57 C62 -8(4) . . . . ? C56 C57 C58 C59 -1(4) . . . . ? C62 C57 C58 C59 -173(2) . . . . ? C57 C58 C59 C60 -1(4) . . . . ? C58 C59 C60 C61 3(5) . . . . ? C57 C56 C61 C60 1(4) . . . . ? C8 C56 C61 C60 -178(2) . . . . ? C57 C56 C61 C63 176(2) . . . . ? C8 C56 C61 C63 -4(4) . . . . ? C59 C60 C61 C56 -3(4) . . . . ? C59 C60 C61 C63 -178(3) . . . . ? C1 N2 C64 C69 62(3) . . . . ? C3 N2 C64 C69 -128(2) . . . . ? C26 N2 C64 C69 -80(6) . . . . ? C1 N2 C64 C65 -130(2) . . . . ? C3 N2 C64 C65 40(3) . . . . ? C26 N2 C64 C65 88(6) . . . . ? C69 C64 C65 C66 -1(4) . . . . ? N2 C64 C65 C66 -169(2) . . . . ? C64 C65 C66 C67 -1(4) . . . . ? C64 C65 C66 C70 172(3) . . . . ? C70 C66 C67 C68 -170(3) . . . . ? C65 C66 C67 C68 3(4) . . . . ? C66 C67 C68 C69 -2(4) . . . . ? C66 C67 C68 C78 176(3) . . . . ? C65 C64 C69 C68 2(5) . . . . ? N2 C64 C69 C68 170(2) . . . . ? C67 C68 C69 C64 -1(4) . . . . ? C78 C68 C69 C64 -178(3) . . . . ? C67 C66 C70 C75 -74(4) . . . . ? C65 C66 C70 C75 113(3) . . . . ? C67 C66 C70 C71 105(3) . . . . ? C65 C66 C70 C71 -68(4) . . . . ? C66 C70 C71 C72 -175(3) . . . . ? C75 C70 C71 C72 4(4) . . . . ? C66 C70 C71 C76 3(4) . . . . ? C75 C70 C71 C76 -178(3) . . . . ? C70 C71 C72 C73 -7(5) . . . . ? C76 C71 C72 C73 175(3) . . . . ? C71 C72 C73 C74 6(6) . . . . ? C72 C73 C74 C75 -3(5) . . . . ? C73 C74 C75 C70 0(5) . . . . ? C73 C74 C75 C77 -178(3) . . . . ? C66 C70 C75 C74 178(3) . . . . ? C71 C70 C75 C74 -1(4) . . . . ? C66 C70 C75 C77 -3(4) . . . . ? C71 C70 C75 C77 178(2) . . . . ? C67 C68 C78 C83 125(3) . . . . ? C69 C68 C78 C83 -58(4) . . . . ? C67 C68 C78 C79 -53(4) . . . . ? C69 C68 C78 C79 124(3) . . . . ? C83 C78 C79 C80 -4(4) . . . . ? C68 C78 C79 C80 174(2) . . . . ? C83 C78 C79 C84 176(2) . . . . ? C68 C78 C79 C84 -6(4) . . . . ? C78 C79 C80 C81 3(4) . . . . ? C84 C79 C80 C81 -177(3) . . . . ? C79 C80 C81 C82 -5(4) . . . . ? C80 C81 C82 C83 9(4) . . . . ? C81 C82 C83 C78 -11(4) . . . . ? C81 C82 C83 C85 175(3) . . . . ? C79 C78 C83 C82 8(4) . . . . ? C68 C78 C83 C82 -170(3) . . . . ? C79 C78 C83 C85 -177(3) . . . . ? C68 C78 C83 C85 5(4) . . . . ? C1 Pd1 C86 N3 3.3(12) . . . . ? O1 Pd1 C86 N3 -173.1(8) . . . . ? O2 Pd1 C86 N3 -173.8(10) . . . . ? C1 Pd1 C86 N4 173.9(9) . . . . ? O1 Pd1 C86 N4 -2.4(15) . . . . ? O2 Pd1 C86 N4 -3.2(10) . . . . ? N4 C86 N3 C87 -1.1(12) . . . . ? Pd1 C86 N3 C87 170.8(9) . . . . ? N4 C86 N3 C89 -174.4(9) . . . . ? Pd1 C86 N3 C89 -2.5(18) . . . . ? C86 N3 C87 C88 1.0(13) . . . . ? C89 N3 C87 C88 175.2(9) . . . . ? N3 C87 C88 N4 -0.4(12) . . . . ? N3 C86 N4 C88 0.8(12) . . . . ? Pd1 C86 N4 C88 -172.7(8) . . . . ? N3 C86 N4 C111 -175.4(15) . . . . ? Pd1 C86 N4 C111 11.2(19) . . . . ? N3 C86 N4 C149 163(2) . . . . ? Pd1 C86 N4 C149 -10(2) . . . . ? C87 C88 N4 C86 -0.2(13) . . . . ? C87 C88 N4 C111 176.0(16) . . . . ? C87 C88 N4 C149 -164.7(18) . . . . ? C86 N3 C89 C94 -77.0(15) . . . . ? C87 N3 C89 C94 109.9(12) . . . . ? C86 N3 C89 C90 112.4(12) . . . . ? C87 N3 C89 C90 -60.7(12) . . . . ? C94 C89 C90 C91 -0.1(16) . . . . ? N3 C89 C90 C91 170.8(9) . . . . ? C89 C90 C91 C92 -1.3(15) . . . . ? C89 C90 C91 C133 -167.9(18) . . . . ? C89 C90 C91 C95 176.7(15) . . . . ? C90 C91 C92 C93 2.2(17) . . . . ? C133 C91 C92 C93 167.7(19) . . . . ? C95 C91 C92 C93 -175.7(16) . . . . ? C91 C92 C93 C94 -1.7(18) . . . . ? C91 C92 C93 C141 -161.7(13) . . . . ? C91 C92 C93 C103 173.8(10) . . . . ? C90 C89 C94 C93 0.7(17) . . . . ? N3 C89 C94 C93 -169.5(10) . . . . ? C92 C93 C94 C89 0.2(18) . . . . ? C141 C93 C94 C89 161.8(12) . . . . ? C103 C93 C94 C89 -174.9(11) . . . . ? C92 C91 C95 C96 70(3) . . . . ? C90 C91 C95 C96 -107(3) . . . . ? C133 C91 C95 C96 174(11) . . . . ? C92 C91 C95 C100 -117(2) . . . . ? C90 C91 C95 C100 65(2) . . . . ? C133 C91 C95 C100 -14(8) . . . . ? C100 C95 C96 C101 176(3) . . . . ? C91 C95 C96 C101 -12(5) . . . . ? C100 C95 C96 C97 2(5) . . . . ? C91 C95 C96 C97 173(3) . . . . ? C95 C96 C97 C98 5(6) . . . . ? C101 C96 C97 C98 -169(4) . . . . ? C96 C97 C98 C99 -7(6) . . . . ? C97 C98 C99 C100 1(4) . . . . ? C98 C99 C100 C95 6(4) . . . . ? C98 C99 C100 C102 -175(2) . . . . ? C96 C95 C100 C99 -7(4) . . . . ? C91 C95 C100 C99 -179(2) . . . . ? C96 C95 C100 C102 174(3) . . . . ? C91 C95 C100 C102 2(3) . . . . ? C92 C93 C103 C104 -55.2(13) . . . . ? C94 C93 C103 C104 120.1(11) . . . . ? C141 C93 C103 C104 -168(3) . . . . ? C92 C93 C103 C108 127.4(14) . . . . ? C94 C93 C103 C108 -57.4(18) . . . . ? C141 C93 C103 C108 14(2) . . . . ? C108 C103 C104 C105 -0.8(11) . . . . ? C93 C103 C104 C105 -178.2(7) . . . . ? C108 C103 C104 C109 -173.8(16) . . . . ? C93 C103 C104 C109 8.8(10) . . . . ? C103 C104 C105 C106 2.0(12) . . . . ? C109 C104 C105 C106 175.0(17) . . . . ? C104 C105 C106 C107 -7(2) . . . . ? C105 C106 C107 C108 10(3) . . . . ? C106 C107 C108 C103 -9(3) . . . . ? C106 C107 C108 C110 -178.0(16) . . . . ? C104 C103 C108 C107 5(3) . . . . ? C93 C103 C108 C107 -177.0(19) . . . . ? C104 C103 C108 C110 172.9(13) . . . . ? C93 C103 C108 C110 -9(2) . . . . ? C86 N4 C111 C116 -92(2) . . . . ? C88 N4 C111 C116 92.2(19) . . . . ? C149 N4 C111 C116 18(5) . . . . ? C86 N4 C111 C112 88(2) . . . . ? C88 N4 C111 C112 -88(2) . . . . ? C149 N4 C111 C112 -162(8) . . . . ? C116 C111 C112 C113 -6(3) . . . . ? N4 C111 C112 C113 174.3(19) . . . . ? C111 C112 C113 C114 1(3) . . . . ? C111 C112 C113 C117 178.5(17) . . . . ? C112 C113 C114 C115 2(4) . . . . ? C117 C113 C114 C115 -175(2) . . . . ? C113 C114 C115 C116 0(4) . . . . ? C113 C114 C115 C125 178(2) . . . . ? C114 C115 C116 C111 -6(3) . . . . ? C125 C115 C116 C111 177(2) . . . . ? N4 C111 C116 C115 -171.9(18) . . . . ? C112 C111 C116 C115 8(3) . . . . ? C114 C113 C117 C122 71(3) . . . . ? C112 C113 C117 C122 -107(2) . . . . ? C114 C113 C117 C118 -108(2) . . . . ? C112 C113 C117 C118 74.7(19) . . . . ? C122 C117 C118 C119 1.2(11) . . . . ? C113 C117 C118 C119 179.9(11) . . . . ? C122 C117 C118 C123 -172.2(17) . . . . ? C113 C117 C118 C123 6.5(15) . . . . ? C117 C118 C119 C120 0.2(11) . . . . ? C123 C118 C119 C120 173.9(17) . . . . ? C118 C119 C120 C121 2(3) . . . . ? C119 C120 C121 C122 -5(4) . . . . ? C118 C117 C122 C121 -4(2) . . . . ? C113 C117 C122 C121 176.9(18) . . . . ? C118 C117 C122 C124 172.6(14) . . . . ? C113 C117 C122 C124 -6(3) . . . . ? C120 C121 C122 C117 7(4) . . . . ? C120 C121 C122 C124 -170(2) . . . . ? C116 C115 C125 C126 99(3) . . . . ? C114 C115 C125 C126 -79(3) . . . . ? C116 C115 C125 C130 -75(3) . . . . ? C114 C115 C125 C130 107(3) . . . . ? C115 C125 C126 C127 -172(3) . . . . ? C130 C125 C126 C127 1(4) . . . . ? C115 C125 C126 C131 5(4) . . . . ? C130 C125 C126 C131 179(2) . . . . ? C125 C126 C127 C128 3(4) . . . . ? C131 C126 C127 C128 -174.8(17) . . . . ? C126 C127 C128 C129 -10(3) . . . . ? C127 C128 C129 C130 13(4) . . . . ? C126 C125 C130 C132 175(3) . . . . ? C115 C125 C130 C132 -12(4) . . . . ? C126 C125 C130 C129 -1(3) . . . . ? C115 C125 C130 C129 173(2) . . . . ? C128 C129 C130 C132 177(3) . . . . ? C128 C129 C130 C125 -7(4) . . . . ? C92 C91 C133 C138 -88(4) . . . . ? C90 C91 C133 C138 77(4) . . . . ? C95 C91 C133 C138 -174(12) . . . . ? C92 C91 C133 C134 81(3) . . . . ? C90 C91 C133 C134 -113(2) . . . . ? C95 C91 C133 C134 -4(7) . . . . ? C138 C133 C134 C135 -5(5) . . . . ? C91 C133 C134 C135 -176(3) . . . . ? C138 C133 C134 C139 176(3) . . . . ? C91 C133 C134 C139 6(4) . . . . ? C133 C134 C135 C136 -3(5) . . . . ? C139 C134 C135 C136 176(3) . . . . ? C134 C135 C136 C137 9(5) . . . . ? C135 C136 C137 C138 -7(5) . . . . ? C91 C133 C138 C137 176(3) . . . . ? C134 C133 C138 C137 8(5) . . . . ? C91 C133 C138 C140 -4(5) . . . . ? C134 C133 C138 C140 -173(3) . . . . ? C136 C137 C138 C133 -2(5) . . . . ? C136 C137 C138 C140 179(3) . . . . ? C92 C93 C141 C146 116(2) . . . . ? C94 C93 C141 C146 -45(3) . . . . ? C103 C93 C141 C146 -165(4) . . . . ? C92 C93 C141 C142 -70.8(13) . . . . ? C94 C93 C141 C142 128.6(10) . . . . ? C103 C93 C141 C142 8(2) . . . . ? C146 C141 C142 C143 -1.7(17) . . . . ? C93 C141 C142 C143 -175.8(9) . . . . ? C146 C141 C142 C147 -177(3) . . . . ? C93 C141 C142 C147 8.9(15) . . . . ? C141 C142 C143 C144 2(2) . . . . ? C147 C142 C143 C144 178(3) . . . . ? C142 C143 C144 C145 -8(4) . . . . ? C143 C144 C145 C146 11(5) . . . . ? C142 C141 C146 C145 7(4) . . . . ? C93 C141 C146 C145 180(3) . . . . ? C142 C141 C146 C148 173.4(19) . . . . ? C93 C141 C146 C148 -14(4) . . . . ? C144 C145 C146 C141 -10(5) . . . . ? C144 C145 C146 C148 -178(3) . . . . ? C86 N4 C149 C150 87(3) . . . . ? C88 N4 C149 C150 -112(3) . . . . ? C111 N4 C149 C150 4(5) . . . . ? C86 N4 C149 C154 -98(3) . . . . ? C88 N4 C149 C154 64(4) . . . . ? C111 N4 C149 C154 -180(9) . . . . ? C154 C149 C150 C151 5(6) . . . . ? N4 C149 C150 C151 -179(3) . . . . ? C149 C150 C151 C155 -177(3) . . . . ? C149 C150 C151 C152 -6(5) . . . . ? C155 C151 C152 C153 176(3) . . . . ? C150 C151 C152 C153 6(4) . . . . ? C151 C152 C153 C154 -4(5) . . . . ? C151 C152 C153 C163 166(3) . . . . ? C150 C149 C154 C153 -3(5) . . . . ? N4 C149 C154 C153 -177(2) . . . . ? C152 C153 C154 C149 2(4) . . . . ? C163 C153 C154 C149 -168(3) . . . . ? C152 C151 C155 C156 -104(4) . . . . ? C150 C151 C155 C156 65(5) . . . . ? C152 C151 C155 C160 76(4) . . . . ? C150 C151 C155 C160 -115(4) . . . . ? C160 C155 C156 C157 5(5) . . . . ? C151 C155 C156 C157 -175(3) . . . . ? C160 C155 C156 C161 -179(3) . . . . ? C151 C155 C156 C161 0(5) . . . . ? C155 C156 C157 C158 -5(5) . . . . ? C161 C156 C157 C158 179(3) . . . . ? C156 C157 C158 C159 8(7) . . . . ? C157 C158 C159 C160 -8(7) . . . . ? C156 C155 C160 C159 -6(5) . . . . ? C151 C155 C160 C159 175(3) . . . . ? C156 C155 C160 C162 177(3) . . . . ? C151 C155 C160 C162 -3(5) . . . . ? C158 C159 C160 C155 6(5) . . . . ? C158 C159 C160 C162 -176(3) . . . . ? C152 C153 C163 C164 -71(4) . . . . ? C154 C153 C163 C164 100(4) . . . . ? C152 C153 C163 C168 120(3) . . . . ? C154 C153 C163 C168 -69(3) . . . . ? C168 C163 C164 C165 -7(6) . . . . ? C153 C163 C164 C165 -175(4) . . . . ? C168 C163 C164 C169 178(2) . . . . ? C153 C163 C164 C169 10(4) . . . . ? C163 C164 C165 C166 12(5) . . . . ? C169 C164 C165 C166 -172.8(18) . . . . ? C164 C165 C166 C167 -12(3) . . . . ? C165 C166 C167 C168 8(4) . . . . ? C166 C167 C168 C163 -1(4) . . . . ? C166 C167 C168 C170 177(2) . . . . ? C164 C163 C168 C167 -2(4) . . . . ? C153 C163 C168 C167 169(2) . . . . ? C164 C163 C168 C170 180(3) . . . . ? C153 C163 C168 C170 -10(3) . . . . ? C171 C172 C173 C174 -110(3) . . . . ? C172 C173 C174 C175 76(6) . . . . ? C173 C174 C175 C176 -171(4) . . . . ? _diffrn_measured_fraction_theta_max 0.485 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.485 _refine_diff_density_max 0.958 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.086 # ÿÿ