# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Michael Scott' _publ_contact_author_address ; Chemistry University of Florida P.O. Box 117200 Gainesville FL 32611 UNITED STATES OF AMERICA ; _publ_contact_author_email MJSCOTT@CHEM.UFL.EDU _publ_section_title ; Metal salen complexes incorporating triphenoxymethanes: Efficient, size selective anion binding by phenolic donors with a visual report ; loop_ _publ_author_name 'Michael Scott' 'Eric R. Libra' data_salentripod _database_code_depnum_ccdc_archive 'CCDC 296133' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Salentripod _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H89 N3 O6' _chemical_formula_weight 1068.44 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8245(12) _cell_length_b 14.1393(12) _cell_length_c 17.9268(15) _cell_angle_alpha 70.554(2) _cell_angle_beta 89.380(2) _cell_angle_gamma 71.177(2) _cell_volume 3109.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type 'Corrected by Sadabs' _exptl_absorpt_correction_T_min 0.782141 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16607 _diffrn_reflns_av_R_equivalents 0.1274 _diffrn_reflns_av_sigmaI/netI 0.3228 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 24.75 _reflns_number_total 10576 _reflns_number_gt 3349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart CCD' _computing_cell_refinement 'Smart CCD' _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELX XP' _computing_publication_material 'Microsoft Word' _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. Phenolic hydrogens were found but refined with the O-H distance fixed at 0.85 angstroms. ; _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^)+(0.0566P)^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 10576 _refine_ls_number_parameters 753 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2843 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2043 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.017 _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 O1 O 0.3847(3) 0.3941(3) 0.0850(2) 0.0284(11) Uani 1 1 d D . . O2 O 0.4098(4) 0.7157(4) -0.0662(3) 0.0323(11) Uani 1 1 d D . . O3 O 0.6569(4) 0.4365(3) 0.1032(3) 0.0328(11) Uani 1 1 d D . . O4 O 0.0663(4) 0.2020(4) 0.3374(3) 0.0422(13) Uani 1 1 d D . . O5 O -0.0593(4) 0.1303(4) 0.5943(3) 0.0518(14) Uani 1 1 d D . . O6 O 0.2473(4) 0.1174(4) 0.4938(3) 0.0500(14) Uani 1 1 d D . . N1 N 0.3419(4) 0.2228(4) 0.1550(3) 0.0309(14) Uani 1 1 d . . . N2 N 0.1382(4) 0.2321(4) 0.1967(3) 0.0317(14) Uani 1 1 d . . . C1 C 0.2952(5) 0.1450(5) 0.1507(4) 0.0328(17) Uani 1 1 d . . . H1C H 0.3086 0.0881 0.2027 0.039 Uiso 1 1 calc R . . C2 C 0.3428(5) 0.0974(5) 0.0891(4) 0.0350(18) Uani 1 1 d . . . H2C H 0.4152 0.0576 0.1062 0.042 Uiso 1 1 calc R . . H2D H 0.3370 0.1541 0.0388 0.042 Uiso 1 1 calc R . . C3 C 0.2884(6) 0.0234(5) 0.0779(4) 0.047(2) Uani 1 1 d . . . H3B H 0.3180 -0.0042 0.0369 0.057 Uiso 1 1 calc R . . H3C H 0.2995 -0.0366 0.1271 0.057 Uiso 1 1 calc R . . C4 C 0.1754(6) 0.0803(6) 0.0550(4) 0.049(2) Uani 1 1 d . . . H4B H 0.1430 0.0308 0.0501 0.059 Uiso 1 1 calc R . . H4C H 0.1640 0.1368 0.0037 0.059 Uiso 1 1 calc R . . C5 C 0.1270(5) 0.1273(5) 0.1165(4) 0.0434(19) Uani 1 1 d . . . H5A H 0.1323 0.0701 0.1663 0.052 Uiso 1 1 calc R . . H5B H 0.0546 0.1667 0.0989 0.052 Uiso 1 1 calc R . . C6 C 0.1787(5) 0.2014(5) 0.1300(4) 0.0318(17) Uani 1 1 d . . . H6B H 0.1647 0.2651 0.0821 0.038 Uiso 1 1 calc R . . C7 C 0.3648(5) 0.2280(5) 0.2215(4) 0.0284(16) Uani 1 1 d . . . H7B H 0.3590 0.1765 0.2680 0.034 Uiso 1 1 calc R . . C8 C 0.4002(5) 0.3122(5) 0.2271(3) 0.0238(15) Uani 1 1 d . . . C9 C 0.4214(5) 0.3172(5) 0.3015(4) 0.0328(17) Uani 1 1 d . . . H9A H 0.4143 0.2649 0.3471 0.039 Uiso 1 1 calc R . . C10 C 0.4521(5) 0.3965(5) 0.3095(3) 0.0337(18) Uani 1 1 d . . . C11 C 0.4622(5) 0.4733(5) 0.2402(3) 0.0296(17) Uani 1 1 d . . . H11A H 0.4855 0.5261 0.2450 0.036 Uiso 1 1 calc R . . C12 C 0.4395(4) 0.4753(4) 0.1646(3) 0.0228(15) Uani 1 1 d . . . C13 C 0.4080(4) 0.3925(5) 0.1590(3) 0.0211(15) Uani 1 1 d . . . C14 C 0.4768(6) 0.4000(5) 0.3910(3) 0.049(2) Uani 1 1 d . . . H14A H 0.5261 0.3330 0.4228 0.073 Uiso 1 1 calc R . . H14B H 0.4151 0.4135 0.4167 0.073 Uiso 1 1 calc R . . H14C H 0.5046 0.4559 0.3847 0.073 Uiso 1 1 calc R . . C15 C 0.4446(4) 0.5646(5) 0.0896(3) 0.0243(15) Uani 1 1 d . . . H15A H 0.4616 0.5322 0.0484 0.029 Uiso 1 1 calc R . . C16 C 0.3423(4) 0.6536(5) 0.0583(4) 0.0218(15) Uani 1 1 d . . . C17 C 0.3294(5) 0.7274(5) -0.0190(4) 0.0234(15) Uani 1 1 d . . . C18 C 0.2385(5) 0.8127(5) -0.0510(3) 0.0261(16) Uani 1 1 d . . . C19 C 0.1577(5) 0.8190(5) -0.0031(4) 0.0290(16) Uani 1 1 d . . . H19A H 0.0960 0.8750 -0.0230 0.035 Uiso 1 1 calc R . . C20 C 0.1655(5) 0.7458(5) 0.0723(4) 0.0328(17) Uani 1 1 d . . . C21 C 0.2575(5) 0.6657(5) 0.1023(3) 0.0286(16) Uani 1 1 d . . . H21A H 0.2641 0.6176 0.1537 0.034 Uiso 1 1 calc R . . C22 C 0.2279(5) 0.8977(5) -0.1336(3) 0.0305(17) Uani 1 1 d . . . C23 C 0.3071(6) 0.9527(5) -0.1363(4) 0.050(2) Uani 1 1 d . . . H23A H 0.3751 0.9011 -0.1268 0.075 Uiso 1 1 calc R . . H23B H 0.2975 0.9847 -0.0960 0.075 Uiso 1 1 calc R . . H23C H 0.2986 1.0067 -0.1876 0.075 Uiso 1 1 calc R . . C24 C 0.2401(6) 0.8473(5) -0.1986(3) 0.052(2) Uani 1 1 d . . . H24A H 0.3065 0.7932 -0.1890 0.078 Uiso 1 1 calc R . . H24B H 0.2336 0.9012 -0.2497 0.078 Uiso 1 1 calc R . . H24C H 0.1877 0.8161 -0.1976 0.078 Uiso 1 1 calc R . . C25 C 0.1211(6) 0.9868(5) -0.1539(4) 0.057(2) Uani 1 1 d . . . H25A H 0.1180 1.0387 -0.2054 0.085 Uiso 1 1 calc R . . H25B H 0.1109 1.0206 -0.1147 0.085 Uiso 1 1 calc R . . H25C H 0.0684 0.9563 -0.1542 0.085 Uiso 1 1 calc R . . C26 C 0.0741(5) 0.7560(5) 0.1204(4) 0.051(2) Uani 1 1 d . . . H26A H 0.0605 0.6900 0.1379 0.077 Uiso 1 1 calc R . . H26B H 0.0148 0.8120 0.0879 0.077 Uiso 1 1 calc R . . H26C H 0.0891 0.7725 0.1659 0.077 Uiso 1 1 calc R . . C27 C 0.5330(5) 0.6032(5) 0.0997(3) 0.0230(15) Uani 1 1 d . . . C28 C 0.6329(5) 0.5388(5) 0.1036(3) 0.0248(16) Uani 1 1 d . . . C29 C 0.7175(5) 0.5725(5) 0.1084(3) 0.0238(15) Uani 1 1 d . . . C30 C 0.6931(5) 0.6739(5) 0.1123(3) 0.0305(17) Uani 1 1 d . . . H30A H 0.7468 0.6990 0.1152 0.037 Uiso 1 1 calc R . . C31 C 0.5952(5) 0.7395(5) 0.1120(3) 0.0305(17) Uani 1 1 d . . . C32 C 0.5149(5) 0.7040(5) 0.1044(3) 0.0278(16) Uani 1 1 d . . . H32A H 0.4477 0.7480 0.1024 0.033 Uiso 1 1 calc R . . C33 C 0.8288(5) 0.5009(5) 0.1119(4) 0.0312(17) Uani 1 1 d . . . C34 C 0.9057(5) 0.5594(5) 0.1108(4) 0.047(2) Uani 1 1 d . . . H34A H 0.9035 0.5781 0.1578 0.070 Uiso 1 1 calc R . . H34B H 0.8877 0.6229 0.0645 0.070 Uiso 1 1 calc R . . H34C H 0.9738 0.5137 0.1095 0.070 Uiso 1 1 calc R . . C35 C 0.8574(5) 0.4045(5) 0.1895(4) 0.0430(19) Uani 1 1 d . . . H35A H 0.8098 0.3669 0.1931 0.065 Uiso 1 1 calc R . . H35B H 0.8546 0.4284 0.2340 0.065 Uiso 1 1 calc R . . H35C H 0.9257 0.3578 0.1901 0.065 Uiso 1 1 calc R . . C36 C 0.8446(5) 0.4629(5) 0.0397(4) 0.046(2) Uani 1 1 d . . . H36A H 0.8020 0.4208 0.0405 0.069 Uiso 1 1 calc R . . H36B H 0.9154 0.4207 0.0424 0.069 Uiso 1 1 calc R . . H36C H 0.8262 0.5237 -0.0086 0.069 Uiso 1 1 calc R . . C37 C 0.5726(5) 0.8493(5) 0.1172(4) 0.046(2) Uani 1 1 d . . . H37A H 0.6361 0.8596 0.1266 0.069 Uiso 1 1 calc R . . H37B H 0.5319 0.8552 0.1602 0.069 Uiso 1 1 calc R . . H37C H 0.5356 0.9025 0.0682 0.069 Uiso 1 1 calc R . . C38 C 0.1398(5) 0.3221(5) 0.1989(4) 0.0339(17) Uani 1 1 d . . . H38A H 0.1555 0.3686 0.1540 0.041 Uiso 1 1 calc R . . C39 C 0.1182(5) 0.3542(5) 0.2683(4) 0.0294(17) Uani 1 1 d . . . C40 C 0.1398(5) 0.4421(5) 0.2714(4) 0.0296(17) Uani 1 1 d . . . H40A H 0.1596 0.4844 0.2263 0.036 Uiso 1 1 calc R . . C41 C 0.1331(5) 0.4687(5) 0.3387(4) 0.0365(18) Uani 1 1 d . . . C42 C 0.0958(5) 0.4090(5) 0.4031(4) 0.0355(18) Uani 1 1 d . . . H42A H 0.0865 0.4288 0.4479 0.043 Uiso 1 1 calc R . . C43 C 0.0719(5) 0.3206(5) 0.4030(4) 0.0327(17) Uani 1 1 d . . . C44 C 0.0834(5) 0.2926(5) 0.3355(4) 0.0334(17) Uani 1 1 d . . . C45 C 0.1651(6) 0.5579(6) 0.3436(4) 0.051(2) Uani 1 1 d . . . H45A H 0.2265 0.5575 0.3181 0.077 Uiso 1 1 calc R . . H45B H 0.1780 0.5491 0.3985 0.077 Uiso 1 1 calc R . . H45C H 0.1112 0.6246 0.3175 0.077 Uiso 1 1 calc R . . C46 C 0.0387(5) 0.2510(5) 0.4770(3) 0.0322(17) Uani 1 1 d . . . H46A H 0.0477 0.1833 0.4693 0.039 Uiso 1 1 calc R . . C47 C 0.1134(5) 0.2252(5) 0.5492(4) 0.0326(17) Uani 1 1 d . . . C48 C 0.2149(6) 0.1626(5) 0.5523(4) 0.0379(18) Uani 1 1 d . . . C49 C 0.2911(5) 0.1441(5) 0.6121(4) 0.0332(17) Uani 1 1 d . . . C50 C 0.2576(6) 0.1918(5) 0.6687(4) 0.0395(19) Uani 1 1 d . . . H50A H 0.3059 0.1810 0.7090 0.047 Uiso 1 1 calc R . . C51 C 0.1573(5) 0.2541(5) 0.6689(4) 0.0333(17) Uani 1 1 d . . . C52 C 0.0873(5) 0.2701(5) 0.6072(4) 0.0385(18) Uani 1 1 d . . . H52A H 0.0196 0.3131 0.6050 0.046 Uiso 1 1 calc R . . C53 C 0.4033(5) 0.0761(6) 0.6141(4) 0.0429(19) Uani 1 1 d . . . C54 C 0.4128(5) -0.0363(5) 0.6209(4) 0.055(2) Uani 1 1 d . . . H54A H 0.4835 -0.0761 0.6200 0.082 Uiso 1 1 calc R . . H54B H 0.3718 -0.0339 0.5770 0.082 Uiso 1 1 calc R . . H54C H 0.3893 -0.0700 0.6699 0.082 Uiso 1 1 calc R . . C55 C 0.4697(5) 0.0668(6) 0.6852(4) 0.055(2) Uani 1 1 d . . . H55A H 0.5406 0.0314 0.6812 0.083 Uiso 1 1 calc R . . H55B H 0.4494 0.0263 0.7334 0.083 Uiso 1 1 calc R . . H55C H 0.4609 0.1367 0.6858 0.083 Uiso 1 1 calc R . . C56 C 0.4452(6) 0.1312(6) 0.5388(4) 0.064(2) Uani 1 1 d . . . H56A H 0.5177 0.0950 0.5421 0.095 Uiso 1 1 calc R . . H56B H 0.4330 0.2039 0.5339 0.095 Uiso 1 1 calc R . . H56C H 0.4111 0.1294 0.4931 0.095 Uiso 1 1 calc R . . C57 C 0.1275(5) 0.3016(6) 0.7318(4) 0.050(2) Uani 1 1 d . . . H57A H 0.1837 0.3189 0.7481 0.075 Uiso 1 1 calc R . . H57B H 0.1111 0.2515 0.7766 0.075 Uiso 1 1 calc R . . H57C H 0.0686 0.3652 0.7112 0.075 Uiso 1 1 calc R . . C58 C -0.0742(5) 0.2960(5) 0.4901(3) 0.0316(17) Uani 1 1 d . . . C59 C -0.1161(6) 0.2315(6) 0.5495(4) 0.0357(18) Uani 1 1 d . . . C60 C -0.2189(6) 0.2692(6) 0.5637(4) 0.0402(19) Uani 1 1 d . . . C61 C -0.2785(5) 0.3729(6) 0.5152(4) 0.0416(19) Uani 1 1 d . . . H61A H -0.3469 0.3993 0.5239 0.050 Uiso 1 1 calc R . . C62 C -0.2404(6) 0.4383(5) 0.4545(4) 0.0403(19) Uani 1 1 d . . . C63 C -0.1375(5) 0.3985(6) 0.4436(4) 0.0365(18) Uani 1 1 d . . . H63A H -0.1099 0.4411 0.4042 0.044 Uiso 1 1 calc R . . C64 C -0.2634(6) 0.2017(6) 0.6308(4) 0.053(2) Uani 1 1 d . . . C65 C -0.3748(6) 0.2653(6) 0.6388(5) 0.073(3) Uani 1 1 d . . . H65A H -0.3773 0.3325 0.6419 0.109 Uiso 1 1 calc R . . H65B H -0.3972 0.2255 0.6862 0.109 Uiso 1 1 calc R . . H65C H -0.4192 0.2773 0.5933 0.109 Uiso 1 1 calc R . . C66 C -0.2589(6) 0.0972(6) 0.6155(4) 0.064(2) Uani 1 1 d . . . H66A H -0.1896 0.0603 0.6086 0.096 Uiso 1 1 calc R . . H66B H -0.3033 0.1155 0.5684 0.096 Uiso 1 1 calc R . . H66C H -0.2809 0.0520 0.6601 0.096 Uiso 1 1 calc R . . C67 C -0.2002(7) 0.1716(6) 0.7112(4) 0.076(3) Uani 1 1 d . . . H67A H -0.2052 0.2352 0.7217 0.114 Uiso 1 1 calc R . . H67B H -0.1295 0.1337 0.7087 0.114 Uiso 1 1 calc R . . H67C H -0.2267 0.1272 0.7531 0.114 Uiso 1 1 calc R . . C68 C -0.3066(5) 0.5482(5) 0.4028(4) 0.059(2) Uani 1 1 d . . . H68A H -0.2761 0.5990 0.4058 0.089 Uiso 1 1 calc R . . H68B H -0.3737 0.5647 0.4206 0.089 Uiso 1 1 calc R . . H68C H -0.3124 0.5510 0.3487 0.089 Uiso 1 1 calc R . . N3 N 0.1176(6) -0.0258(6) 0.5660(4) 0.075(2) Uani 1 1 d . . . C69 C 0.1676(7) -0.1148(8) 0.5934(5) 0.060(3) Uani 1 1 d . . . C70 C 0.2301(8) -0.2269(6) 0.6297(5) 0.084(3) Uani 1 1 d . . . H1 H 0.367(4) 0.338(3) 0.095(3) 0.028(19) Uiso 1 1 d D . . H2 H 0.470(3) 0.696(6) -0.045(4) 0.09(3) Uiso 1 1 d D . . H3 H 0.605(4) 0.418(6) 0.114(4) 0.08(3) Uiso 1 1 d D . . H4 H 0.076(5) 0.192(5) 0.293(2) 0.06(3) Uiso 1 1 d D . . H5 H -0.003(3) 0.096(5) 0.582(4) 0.082 Uiso 1 1 d D . . H6 H 0.206(5) 0.129(6) 0.453(3) 0.08(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.035(3) 0.032(3) 0.025(3) -0.010(2) 0.003(2) -0.020(3) O2 0.021(3) 0.042(3) 0.031(3) -0.007(2) 0.004(3) -0.013(3) O3 0.026(3) 0.023(3) 0.049(3) -0.013(2) 0.003(2) -0.008(2) O4 0.058(4) 0.040(3) 0.039(3) -0.019(3) 0.014(3) -0.026(3) O5 0.038(4) 0.043(4) 0.053(3) 0.006(3) 0.000(3) -0.010(3) O6 0.049(4) 0.051(4) 0.039(3) -0.013(3) -0.001(3) -0.006(3) N1 0.035(4) 0.025(3) 0.030(3) -0.006(3) 0.001(3) -0.011(3) N2 0.022(3) 0.033(4) 0.039(4) -0.013(3) -0.002(3) -0.007(3) C1 0.036(5) 0.036(4) 0.034(4) -0.013(4) 0.002(4) -0.021(4) C2 0.049(5) 0.027(4) 0.036(4) -0.017(4) 0.007(4) -0.016(4) C3 0.065(6) 0.043(5) 0.042(5) -0.022(4) 0.005(4) -0.022(5) C4 0.050(6) 0.054(5) 0.052(5) -0.019(4) -0.006(4) -0.027(5) C5 0.038(5) 0.042(5) 0.057(5) -0.020(4) -0.006(4) -0.018(4) C6 0.043(5) 0.028(4) 0.026(4) -0.011(3) 0.003(4) -0.013(4) C7 0.027(4) 0.020(4) 0.031(4) -0.002(3) -0.001(3) -0.006(3) C8 0.023(4) 0.018(4) 0.026(4) -0.003(3) -0.001(3) -0.006(3) C9 0.041(5) 0.023(4) 0.026(4) 0.007(3) -0.001(3) -0.015(4) C10 0.046(5) 0.027(4) 0.020(4) -0.004(3) -0.010(3) -0.006(4) C11 0.031(4) 0.027(4) 0.031(4) -0.009(4) -0.004(3) -0.010(3) C12 0.023(4) 0.018(4) 0.022(4) -0.002(3) -0.001(3) -0.005(3) C13 0.020(4) 0.021(4) 0.019(4) -0.007(3) -0.002(3) -0.002(3) C14 0.076(6) 0.047(5) 0.027(4) -0.011(4) 0.000(4) -0.026(5) C15 0.020(4) 0.025(4) 0.027(4) -0.011(3) 0.003(3) -0.005(3) C16 0.012(4) 0.026(4) 0.032(4) -0.015(4) 0.005(3) -0.007(3) C17 0.028(4) 0.025(4) 0.024(4) -0.014(3) 0.003(3) -0.013(3) C18 0.031(5) 0.015(4) 0.028(4) -0.002(3) -0.001(3) -0.007(3) C19 0.022(4) 0.021(4) 0.036(4) -0.007(4) -0.002(3) 0.000(3) C20 0.032(5) 0.034(5) 0.029(4) -0.008(4) 0.005(4) -0.010(4) C21 0.029(5) 0.025(4) 0.024(4) 0.001(3) -0.003(3) -0.009(4) C22 0.042(5) 0.023(4) 0.027(4) -0.005(3) 0.000(3) -0.015(4) C23 0.080(6) 0.031(5) 0.032(4) 0.003(4) 0.000(4) -0.025(5) C24 0.076(6) 0.046(5) 0.032(4) -0.013(4) -0.001(4) -0.019(5) C25 0.052(6) 0.048(5) 0.045(5) 0.002(4) -0.008(4) -0.004(5) C26 0.027(5) 0.059(5) 0.040(5) -0.002(4) 0.006(4) 0.003(4) C27 0.016(4) 0.025(4) 0.028(4) -0.011(3) 0.003(3) -0.006(3) C28 0.033(5) 0.024(4) 0.026(4) -0.013(3) 0.007(3) -0.016(4) C29 0.027(4) 0.020(4) 0.018(4) -0.001(3) -0.002(3) -0.006(3) C30 0.022(4) 0.032(4) 0.036(4) -0.005(4) -0.002(3) -0.014(4) C31 0.033(5) 0.030(4) 0.036(4) -0.016(4) 0.001(4) -0.016(4) C32 0.026(4) 0.031(4) 0.026(4) -0.009(3) 0.001(3) -0.010(3) C33 0.023(4) 0.041(5) 0.034(4) -0.011(4) -0.001(3) -0.019(4) C34 0.032(5) 0.044(5) 0.057(5) -0.006(4) -0.005(4) -0.015(4) C35 0.030(5) 0.041(5) 0.049(5) -0.005(4) 0.000(4) -0.010(4) C36 0.029(5) 0.055(5) 0.049(5) -0.017(4) 0.003(4) -0.009(4) C37 0.039(5) 0.039(5) 0.073(5) -0.032(4) 0.006(4) -0.019(4) C38 0.030(5) 0.043(5) 0.025(4) -0.008(4) 0.001(3) -0.012(4) C39 0.027(4) 0.030(4) 0.025(4) -0.007(4) 0.002(3) -0.004(3) C40 0.031(4) 0.021(4) 0.032(4) -0.004(3) 0.009(3) -0.008(3) C41 0.037(5) 0.034(4) 0.042(5) -0.015(4) 0.007(4) -0.016(4) C42 0.039(5) 0.031(4) 0.036(4) -0.017(4) 0.005(4) -0.008(4) C43 0.029(5) 0.033(5) 0.031(4) -0.006(4) -0.007(3) -0.008(4) C44 0.030(5) 0.036(5) 0.040(4) -0.017(4) 0.002(4) -0.016(4) C45 0.056(6) 0.061(6) 0.051(5) -0.027(4) 0.014(4) -0.032(5) C46 0.027(4) 0.035(4) 0.031(4) -0.011(4) 0.002(3) -0.006(4) C47 0.029(5) 0.040(5) 0.025(4) -0.011(4) 0.000(4) -0.007(4) C48 0.041(5) 0.041(5) 0.031(4) -0.012(4) 0.008(4) -0.014(4) C49 0.034(5) 0.026(4) 0.029(4) 0.004(4) -0.004(4) -0.011(4) C50 0.044(6) 0.045(5) 0.030(4) -0.002(4) 0.004(4) -0.027(4) C51 0.030(5) 0.037(5) 0.029(4) -0.005(4) 0.000(4) -0.012(4) C52 0.029(5) 0.040(5) 0.039(4) -0.012(4) 0.008(4) -0.003(4) C53 0.035(5) 0.034(5) 0.050(5) -0.007(4) 0.002(4) -0.008(4) C54 0.044(5) 0.041(5) 0.059(5) -0.005(4) 0.004(4) 0.000(4) C55 0.029(5) 0.069(6) 0.055(5) -0.015(5) -0.005(4) -0.008(4) C56 0.048(6) 0.084(7) 0.050(5) -0.007(5) 0.012(4) -0.029(5) C57 0.041(5) 0.064(6) 0.039(4) -0.022(4) 0.002(4) -0.006(4) C58 0.037(5) 0.030(4) 0.024(4) -0.002(4) -0.002(4) -0.014(4) C59 0.036(5) 0.035(5) 0.032(4) -0.006(4) -0.007(4) -0.012(4) C60 0.044(6) 0.050(5) 0.033(4) -0.013(4) 0.007(4) -0.026(4) C61 0.027(5) 0.051(5) 0.054(5) -0.023(4) 0.003(4) -0.018(4) C62 0.037(5) 0.031(5) 0.053(5) -0.014(4) -0.001(4) -0.012(4) C63 0.038(5) 0.049(5) 0.029(4) -0.016(4) 0.007(4) -0.020(4) C64 0.048(6) 0.068(6) 0.043(5) -0.011(5) 0.009(4) -0.029(5) C65 0.046(6) 0.083(7) 0.092(6) -0.022(6) 0.029(5) -0.035(5) C66 0.068(6) 0.065(6) 0.075(6) -0.025(5) 0.025(5) -0.045(5) C67 0.089(8) 0.085(7) 0.044(5) 0.005(5) 0.009(5) -0.045(6) C68 0.042(5) 0.034(5) 0.087(6) -0.009(5) 0.013(5) -0.006(4) N3 0.079(7) 0.057(5) 0.087(6) -0.020(5) -0.003(5) -0.024(5) C69 0.082(8) 0.085(7) 0.045(6) -0.039(6) 0.017(5) -0.053(7) C70 0.146(10) 0.022(5) 0.058(6) -0.004(4) -0.018(6) -0.005(6) _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 O1 C13 1.360(6) . ? O1 H1 0.857(19) . ? O2 C17 1.390(7) . ? O2 H2 0.84(2) . ? O3 C28 1.379(7) . ? O3 H3 0.84(2) . ? O4 C44 1.365(7) . ? O4 H4 0.86(2) . ? O5 C59 1.354(8) . ? O5 H5 0.85(2) . ? O6 C48 1.400(7) . ? O6 H6 0.87(2) . ? N1 C7 1.269(6) . ? N1 C1 1.465(7) . ? N2 C38 1.293(7) . ? N2 C6 1.450(7) . ? C1 C2 1.516(7) . ? C1 C6 1.534(8) . ? C1 H1C 0.9800 . ? C2 C3 1.534(7) . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.497(9) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.513(8) . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.524(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6B 0.9800 . ? C7 C8 1.457(7) . ? C7 H7B 0.9300 . ? C8 C13 1.394(7) . ? C8 C9 1.399(7) . ? C9 C10 1.370(7) . ? C9 H9A 0.9300 . ? C10 C11 1.392(7) . ? C10 C14 1.523(7) . ? C11 C12 1.383(7) . ? C11 H11A 0.9300 . ? C12 C13 1.407(7) . ? C12 C15 1.528(7) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.516(8) . ? C15 C27 1.524(7) . ? C15 H15A 0.9800 . ? C16 C17 1.402(7) . ? C16 C21 1.402(8) . ? C17 C18 1.392(8) . ? C18 C19 1.398(8) . ? C18 C22 1.539(8) . ? C19 C20 1.381(8) . ? C19 H19A 0.9300 . ? C20 C21 1.367(8) . ? C20 C26 1.519(8) . ? C21 H21A 0.9300 . ? C22 C23 1.526(8) . ? C22 C24 1.537(8) . ? C22 C25 1.551(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.375(8) . ? C27 C32 1.397(7) . ? C28 C29 1.411(7) . ? C29 C30 1.388(7) . ? C29 C33 1.533(8) . ? C30 C31 1.371(8) . ? C30 H30A 0.9300 . ? C31 C32 1.382(7) . ? C31 C37 1.516(7) . ? C32 H32A 0.9300 . ? C33 C35 1.533(8) . ? C33 C34 1.539(7) . ? C33 C36 1.547(8) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.458(8) . ? C38 H38A 0.9300 . ? C39 C40 1.385(7) . ? C39 C44 1.414(8) . ? C40 C41 1.374(8) . ? C40 H40A 0.9300 . ? C41 C42 1.389(8) . ? C41 C45 1.493(8) . ? C42 C43 1.394(8) . ? C42 H42A 0.9300 . ? C43 C44 1.385(8) . ? C43 C46 1.532(8) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.532(8) . ? C46 C58 1.532(8) . ? C46 H46A 0.9800 . ? C47 C52 1.378(8) . ? C47 C48 1.386(9) . ? C48 C49 1.411(8) . ? C49 C50 1.393(8) . ? C49 C53 1.533(9) . ? C50 C51 1.382(9) . ? C50 H50A 0.9300 . ? C51 C52 1.387(8) . ? C51 C57 1.486(8) . ? C52 H52A 0.9300 . ? C53 C54 1.514(8) . ? C53 C55 1.524(8) . ? C53 C56 1.529(8) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 C63 1.398(8) . ? C58 C59 1.408(8) . ? C59 C60 1.400(9) . ? C60 C61 1.405(9) . ? C60 C64 1.529(9) . ? C61 C62 1.395(8) . ? C61 H61A 0.9300 . ? C62 C63 1.390(9) . ? C62 C68 1.501(9) . ? C63 H63A 0.9300 . ? C64 C65 1.545(10) . ? C64 C67 1.550(9) . ? C64 C66 1.572(9) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? N3 C69 1.157(10) . ? C69 C70 1.457(11) . ? 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 C13 O1 H1 102(3) . . ? C17 O2 H2 118(5) . . ? C28 O3 H3 108(5) . . ? C44 O4 H4 111(4) . . ? C59 O5 H5 123(5) . . ? C48 O6 H6 122(5) . . ? C7 N1 C1 120.8(5) . . ? C38 N2 C6 117.8(5) . . ? N1 C1 C2 109.3(5) . . ? N1 C1 C6 108.6(5) . . ? C2 C1 C6 111.7(5) . . ? N1 C1 H1C 109.1 . . ? C2 C1 H1C 109.1 . . ? C6 C1 H1C 109.1 . . ? C1 C2 C3 110.4(5) . . ? C1 C2 H2C 109.6 . . ? C3 C2 H2C 109.6 . . ? C1 C2 H2D 109.6 . . ? C3 C2 H2D 109.6 . . ? H2C C2 H2D 108.1 . . ? C4 C3 C2 111.5(6) . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3C 109.3 . . ? C2 C3 H3C 109.3 . . ? H3B C3 H3C 108.0 . . ? C3 C4 C5 110.8(5) . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? C5 C4 H4C 109.5 . . ? H4B C4 H4C 108.1 . . ? C4 C5 C6 111.9(6) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N2 C6 C5 108.9(5) . . ? N2 C6 C1 107.8(5) . . ? C5 C6 C1 111.0(5) . . ? N2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? C1 C6 H6B 109.7 . . ? N1 C7 C8 121.9(6) . . ? N1 C7 H7B 119.0 . . ? C8 C7 H7B 119.0 . . ? C13 C8 C9 118.6(5) . . ? C13 C8 C7 121.2(5) . . ? C9 C8 C7 120.1(6) . . ? C10 C9 C8 122.1(6) . . ? C10 C9 H9A 118.9 . . ? C8 C9 H9A 118.9 . . ? C9 C10 C11 117.5(6) . . ? C9 C10 C14 121.7(6) . . ? C11 C10 C14 120.8(6) . . ? C12 C11 C10 123.4(6) . . ? C12 C11 H11A 118.3 . . ? C10 C11 H11A 118.3 . . ? C11 C12 C13 117.2(5) . . ? C11 C12 C15 122.3(5) . . ? C13 C12 C15 120.4(5) . . ? O1 C13 C8 121.3(5) . . ? O1 C13 C12 117.7(5) . . ? C8 C13 C12 121.0(5) . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C27 113.8(5) . . ? C16 C15 C12 113.3(5) . . ? C27 C15 C12 111.5(5) . . ? C16 C15 H15A 105.8 . . ? C27 C15 H15A 105.8 . . ? C12 C15 H15A 105.8 . . ? C17 C16 C21 117.2(6) . . ? C17 C16 C15 119.3(5) . . ? C21 C16 C15 123.5(6) . . ? O2 C17 C18 118.2(5) . . ? O2 C17 C16 119.2(6) . . ? C18 C17 C16 122.5(6) . . ? C17 C18 C19 116.6(5) . . ? C17 C18 C22 122.0(6) . . ? C19 C18 C22 121.4(6) . . ? C20 C19 C18 123.0(6) . . ? C20 C19 H19A 118.5 . . ? C18 C19 H19A 118.5 . . ? C21 C20 C19 118.4(6) . . ? C21 C20 C26 121.3(6) . . ? C19 C20 C26 120.3(6) . . ? C20 C21 C16 122.3(6) . . ? C20 C21 H21A 118.9 . . ? C16 C21 H21A 118.9 . . ? C23 C22 C24 110.7(5) . . ? C23 C22 C18 110.3(5) . . ? C24 C22 C18 110.5(5) . . ? C23 C22 C25 106.3(5) . . ? C24 C22 C25 107.0(5) . . ? C18 C22 C25 112.0(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.6(6) . . ? C28 C27 C15 120.1(5) . . ? C32 C27 C15 121.3(5) . . ? C27 C28 O3 121.8(5) . . ? C27 C28 C29 122.6(6) . . ? O3 C28 C29 115.6(6) . . ? C30 C29 C28 115.2(6) . . ? C30 C29 C33 122.3(6) . . ? C28 C29 C33 122.4(6) . . ? C31 C30 C29 124.5(6) . . ? C31 C30 H30A 117.8 . . ? C29 C30 H30A 117.8 . . ? C30 C31 C32 117.9(6) . . ? C30 C31 C37 122.4(6) . . ? C32 C31 C37 119.7(6) . . ? C31 C32 C27 121.2(6) . . ? C31 C32 H32A 119.4 . . ? C27 C32 H32A 119.4 . . ? C35 C33 C29 109.8(5) . . ? C35 C33 C34 107.0(5) . . ? C29 C33 C34 112.0(5) . . ? C35 C33 C36 110.0(5) . . ? C29 C33 C36 111.4(5) . . ? C34 C33 C36 106.6(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C31 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N2 C38 C39 123.3(6) . . ? N2 C38 H38A 118.3 . . ? C39 C38 H38A 118.3 . . ? C40 C39 C44 119.1(6) . . ? C40 C39 C38 119.5(6) . . ? C44 C39 C38 121.2(6) . . ? C41 C40 C39 122.2(6) . . ? C41 C40 H40A 118.9 . . ? C39 C40 H40A 118.9 . . ? C40 C41 C42 117.6(6) . . ? C40 C41 C45 121.8(6) . . ? C42 C41 C45 120.6(6) . . ? C41 C42 C43 122.4(6) . . ? C41 C42 H42A 118.8 . . ? C43 C42 H42A 118.8 . . ? C44 C43 C42 118.8(6) . . ? C44 C43 C46 119.7(6) . . ? C42 C43 C46 121.4(6) . . ? O4 C44 C43 118.7(6) . . ? O4 C44 C39 121.5(6) . . ? C43 C44 C39 119.7(6) . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 C47 108.7(5) . . ? C43 C46 C58 114.8(5) . . ? C47 C46 C58 113.0(5) . . ? C43 C46 H46A 106.6 . . ? C47 C46 H46A 106.6 . . ? C58 C46 H46A 106.6 . . ? C52 C47 C48 118.1(6) . . ? C52 C47 C46 123.0(6) . . ? C48 C47 C46 118.5(6) . . ? C47 C48 O6 121.1(6) . . ? C47 C48 C49 122.3(7) . . ? O6 C48 C49 116.6(6) . . ? C50 C49 C48 115.6(6) . . ? C50 C49 C53 122.7(6) . . ? C48 C49 C53 121.7(7) . . ? C51 C50 C49 124.4(7) . . ? C51 C50 H50A 117.8 . . ? C49 C50 H50A 117.8 . . ? C50 C51 C52 116.5(7) . . ? C50 C51 C57 121.1(6) . . ? C52 C51 C57 122.4(6) . . ? C47 C52 C51 123.0(7) . . ? C47 C52 H52A 118.5 . . ? C51 C52 H52A 118.5 . . ? C54 C53 C55 106.8(6) . . ? C54 C53 C56 111.5(6) . . ? C55 C53 C56 107.5(6) . . ? C54 C53 C49 111.4(6) . . ? C55 C53 C49 111.5(6) . . ? C56 C53 C49 108.2(6) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C63 C58 C59 119.0(6) . . ? C63 C58 C46 121.8(6) . . ? C59 C58 C46 119.1(6) . . ? O5 C59 C60 117.4(6) . . ? O5 C59 C58 121.5(7) . . ? C60 C59 C58 121.2(7) . . ? C59 C60 C61 117.2(6) . . ? C59 C60 C64 121.4(7) . . ? C61 C60 C64 121.3(7) . . ? C62 C61 C60 123.3(7) . . ? C62 C61 H61A 118.3 . . ? C60 C61 H61A 118.3 . . ? C63 C62 C61 117.6(7) . . ? C63 C62 C68 120.4(6) . . ? C61 C62 C68 122.1(7) . . ? C62 C63 C58 121.7(6) . . ? C62 C63 H63A 119.1 . . ? C58 C63 H63A 119.1 . . ? C60 C64 C65 111.2(7) . . ? C60 C64 C67 109.5(6) . . ? C65 C64 C67 106.2(6) . . ? C60 C64 C66 109.7(6) . . ? C65 C64 C66 110.8(6) . . ? C67 C64 C66 109.4(7) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C62 C68 H68A 109.5 . . ? C62 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C62 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N3 C69 C70 178.7(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.75 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.312 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.058 #===END data_Nisalen _database_code_depnum_ccdc_archive 'CCDC 296134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Chiral Ni Salen Tripd' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H90 N4 Ni O6' _chemical_formula_weight 1166.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.1800(9) _cell_length_b 13.7606(10) _cell_length_c 20.2871(14) _cell_angle_alpha 83.2670(10) _cell_angle_beta 77.1700(10) _cell_angle_gamma 66.1000(10) _cell_volume 3278.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type 'Corrected by Sadabs' _exptl_absorpt_correction_T_min 0.550717 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Corrected by Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18198 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14424 _reflns_number_gt 9890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart CCD' _computing_cell_refinement 'Smart CCD' _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELX XP' _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. Phenolic hydrogens were found but refined with the O-H distance fixed at 0.85 angstroms. One acetonitrile solavte molecule was badly disordered and the molecule was removed from the structure with Squeeze from the Platon Software Package. ; _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^)+(0.0724P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.18(2) _refine_ls_number_reflns 14424 _refine_ls_number_parameters 1525 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.90232(7) 0.62661(7) 0.15989(4) 0.0364(3) Uani 1 1 d . . . O1 O 0.9180(5) 0.5414(5) 0.0902(3) 0.0420(15) Uani 1 1 d . . . O2 O 0.8461(5) 0.5921(5) -0.1367(3) 0.0579(19) Uani 1 1 d D . . O3 O 1.0425(5) 0.5875(5) -0.0239(3) 0.0512(17) Uani 1 1 d D . . O4 O 0.8385(5) 0.7392(5) 0.1014(3) 0.0386(14) Uani 1 1 d . . . O5 O 0.6662(4) 0.7460(5) 0.0404(3) 0.0460(16) Uani 1 1 d D . . O6 O 0.8635(5) 0.7895(5) -0.1473(3) 0.0471(16) Uani 1 1 d D . . N1 N 0.9740(5) 0.5139(6) 0.2139(3) 0.0356(16) Uani 1 1 d . . . N2 N 0.8788(6) 0.7122(6) 0.2310(3) 0.0399(17) Uani 1 1 d . . . C1 C 1.0080(5) 0.5487(5) 0.2696(3) 0.0394(15) Uani 1 1 d . . . H1A H 1.0734 0.5684 0.2484 0.047 Uiso 1 1 calc R . . C2 C 1.0429(8) 0.4726(8) 0.3279(5) 0.055(3) Uani 1 1 d . . . H2B H 0.9792 0.4530 0.3513 0.066 Uiso 1 1 calc R . . H2C H 1.1071 0.4068 0.3106 0.066 Uiso 1 1 calc R . . C3 C 1.0762(6) 0.5200(6) 0.3759(4) 0.0522(19) Uani 1 1 d . . . H3B H 1.1430 0.5355 0.3535 0.063 Uiso 1 1 calc R . . H3C H 1.0969 0.4695 0.4144 0.063 Uiso 1 1 calc R . . C4 C 0.9785(7) 0.6223(6) 0.4016(4) 0.057(2) Uani 1 1 d . . . H4A H 1.0017 0.6537 0.4342 0.068 Uiso 1 1 calc R . . H4B H 0.9136 0.6052 0.4261 0.068 Uiso 1 1 calc R . . C5 C 0.9410(8) 0.7040(7) 0.3451(4) 0.050(2) Uani 1 1 d . . . H5B H 1.0025 0.7273 0.3228 0.060 Uiso 1 1 calc R . . H5C H 0.8740 0.7670 0.3635 0.060 Uiso 1 1 calc R . . C6 C 0.9115(6) 0.6485(5) 0.2937(3) 0.0408(15) Uani 1 1 d . . . H6B H 0.8469 0.6293 0.3176 0.049 Uiso 1 1 calc R . . C7 C 0.9938(7) 0.4150(8) 0.2059(5) 0.048(2) Uani 1 1 d . . . H7A H 1.0250 0.3653 0.2400 0.057 Uiso 1 1 calc R . . C8 C 0.9732(7) 0.3726(8) 0.1505(4) 0.039(2) Uani 1 1 d . . . C9 C 0.9914(7) 0.2658(7) 0.1510(4) 0.043(2) Uani 1 1 d . . . H9A H 1.0072 0.2230 0.1907 0.052 Uiso 1 1 calc R . . C10 C 0.9872(7) 0.2218(7) 0.0968(5) 0.049(2) Uani 1 1 d . . . C11 C 0.9605(7) 0.2848(8) 0.0389(4) 0.042(2) Uani 1 1 d . . . C12 C 0.9335(7) 0.3905(7) 0.0379(4) 0.040(2) Uani 1 1 d . . . C13 C 0.9380(7) 0.4365(6) 0.0923(4) 0.039(2) Uani 1 1 d . . . C14 C 1.0164(7) 0.1012(7) 0.0990(5) 0.049(2) Uani 1 1 d . . . H14A H 1.0438 0.0692 0.1407 0.074 Uiso 1 1 calc R . . H14B H 1.0752 0.0688 0.0598 0.074 Uiso 1 1 calc R . . H14C H 0.9486 0.0889 0.0978 0.074 Uiso 1 1 calc R . . C15 C 0.9102(6) 0.4577(7) -0.0261(4) 0.033(2) Uani 1 1 d . . . H15A H 0.8753 0.5329 -0.0112 0.039 Uiso 1 1 calc R . . C16 C 0.8298(7) 0.4484(7) -0.0632(4) 0.039(2) Uani 1 1 d . . . C17 C 0.8047(7) 0.5156(7) -0.1207(4) 0.032(2) Uani 1 1 d . . . C18 C 0.7412(7) 0.5037(7) -0.1636(4) 0.041(2) Uani 1 1 d . . . C19 C 0.6941(8) 0.4285(9) -0.1406(5) 0.058(3) Uani 1 1 d . . . H19A H 0.6459 0.4227 -0.1671 0.069 Uiso 1 1 calc R . . C20 C 0.7085(8) 0.3648(8) -0.0867(4) 0.050(2) Uani 1 1 d . . . C21 C 0.7783(6) 0.3785(7) -0.0469(4) 0.036(2) Uani 1 1 d . . . H21A H 0.7895 0.3362 -0.0066 0.044 Uiso 1 1 calc R . . C22 C 0.7276(8) 0.5675(10) -0.2287(5) 0.065(3) Uani 1 1 d . . . C23 C 0.6675(9) 0.6905(9) -0.2148(6) 0.087(4) Uani 1 1 d . . . H23A H 0.6608 0.7308 -0.2579 0.130 Uiso 1 1 calc R . . H23B H 0.7124 0.7109 -0.1909 0.130 Uiso 1 1 calc R . . H23C H 0.5919 0.7060 -0.1871 0.130 Uiso 1 1 calc R . . C24 C 0.8484(9) 0.5372(10) -0.2743(5) 0.081(4) Uani 1 1 d . . . H24A H 0.8422 0.5761 -0.3179 0.121 Uiso 1 1 calc R . . H24B H 0.8823 0.4606 -0.2817 0.121 Uiso 1 1 calc R . . H24C H 0.8961 0.5561 -0.2517 0.121 Uiso 1 1 calc R . . C25 C 0.6578(8) 0.5410(10) -0.2705(5) 0.084(4) Uani 1 1 d . . . H25A H 0.6555 0.5826 -0.3132 0.126 Uiso 1 1 calc R . . H25B H 0.5806 0.5584 -0.2448 0.126 Uiso 1 1 calc R . . H25C H 0.6930 0.4650 -0.2801 0.126 Uiso 1 1 calc R . . C26 C 0.6527(10) 0.2849(9) -0.0675(6) 0.082(4) Uani 1 1 d . . . H26A H 0.6182 0.2809 -0.1046 0.123 Uiso 1 1 calc R . . H26B H 0.5943 0.3077 -0.0266 0.123 Uiso 1 1 calc R . . H26C H 0.7099 0.2147 -0.0589 0.123 Uiso 1 1 calc R . . C27 C 1.0212(7) 0.4480(7) -0.0747(4) 0.037(2) Uani 1 1 d . . . C28 C 1.0848(7) 0.5099(7) -0.0741(4) 0.040(2) Uani 1 1 d . . . C29 C 1.1803(7) 0.5024(8) -0.1175(4) 0.045(2) Uani 1 1 d . . . C30 C 1.2193(7) 0.4274(7) -0.1681(5) 0.048(2) Uani 1 1 d . . . H30A H 1.2851 0.4206 -0.2013 0.058 Uiso 1 1 calc R . . C31 C 1.1596(8) 0.3610(8) -0.1696(5) 0.059(3) Uani 1 1 d . . . C32 C 1.0666(7) 0.3712(7) -0.1237(4) 0.047(2) Uani 1 1 d . . . H32A H 1.0300 0.3244 -0.1245 0.056 Uiso 1 1 calc R . . C33 C 1.2472(7) 0.5711(7) -0.1161(5) 0.050(3) Uani 1 1 d . . . C34 C 1.1716(8) 0.6901(8) -0.1219(5) 0.062(3) Uani 1 1 d . . . H34A H 1.1334 0.7025 -0.1602 0.093 Uiso 1 1 calc R . . H34B H 1.2182 0.7320 -0.1290 0.093 Uiso 1 1 calc R . . H34C H 1.1149 0.7116 -0.0801 0.093 Uiso 1 1 calc R . . C35 C 1.2948(7) 0.5452(7) -0.0525(5) 0.051(2) Uani 1 1 d . . . H35A H 1.3337 0.5917 -0.0502 0.076 Uiso 1 1 calc R . . H35B H 1.3485 0.4708 -0.0527 0.076 Uiso 1 1 calc R . . H35C H 1.2332 0.5560 -0.0132 0.076 Uiso 1 1 calc R . . C36 C 1.3487(8) 0.5444(9) -0.1759(5) 0.070(3) Uani 1 1 d . . . H36A H 1.3212 0.5599 -0.2186 0.106 Uiso 1 1 calc R . . H36B H 1.3978 0.4689 -0.1730 0.106 Uiso 1 1 calc R . . H36C H 1.3916 0.5876 -0.1741 0.106 Uiso 1 1 calc R . . C37 C 1.2043(8) 0.2824(9) -0.2228(6) 0.082(4) Uani 1 1 d . . . H37A H 1.2852 0.2659 -0.2390 0.123 Uiso 1 1 calc R . . H37B H 1.1641 0.3114 -0.2604 0.123 Uiso 1 1 calc R . . H37C H 1.1936 0.2173 -0.2044 0.123 Uiso 1 1 calc R . . C38 C 0.8323(7) 0.8125(7) 0.2317(4) 0.040(2) Uani 1 1 d . . . H38A H 0.8196 0.8446 0.2734 0.048 Uiso 1 1 calc R . . C39 C 0.7959(7) 0.8848(8) 0.1739(4) 0.037(2) Uani 1 1 d . . . C40 C 0.7562(7) 0.9957(7) 0.1793(4) 0.039(2) Uani 1 1 d . . . H40A H 0.7512 1.0228 0.2214 0.047 Uiso 1 1 calc R . . C41 C 0.7262(7) 1.0627(7) 0.1300(4) 0.041(2) Uani 1 1 d . . . C42 C 0.7412(6) 1.0234(7) 0.0669(4) 0.035(2) Uani 1 1 d . . . H42A H 0.7221 1.0721 0.0300 0.042 Uiso 1 1 calc R . . C43 C 0.7834(7) 0.9149(7) 0.0562(4) 0.037(2) Uani 1 1 d . . . C44 C 0.8074(7) 0.8406(7) 0.1115(4) 0.035(2) Uani 1 1 d . . . C45 C 0.6860(7) 1.1821(6) 0.1382(5) 0.050(2) Uani 1 1 d . . . H45A H 0.6500 1.1996 0.1854 0.076 Uiso 1 1 calc R . . H45B H 0.6314 1.2206 0.1089 0.076 Uiso 1 1 calc R . . H45C H 0.7509 1.2028 0.1256 0.076 Uiso 1 1 calc R . . C46 C 0.7995(7) 0.8702(7) -0.0143(4) 0.033(2) Uani 1 1 d . . . H46A H 0.8376 0.7911 -0.0095 0.039 Uiso 1 1 calc R . . C47 C 0.6845(6) 0.8933(7) -0.0324(4) 0.037(2) Uani 1 1 d . . . C48 C 0.6271(6) 0.8298(6) -0.0061(4) 0.036(2) Uani 1 1 d . . . C49 C 0.5238(7) 0.8480(7) -0.0250(5) 0.044(2) Uani 1 1 d . . . C50 C 0.4832(7) 0.9348(8) -0.0701(5) 0.050(2) Uani 1 1 d . . . H50A H 0.4148 0.9482 -0.0845 0.060 Uiso 1 1 calc R . . C51 C 0.5389(8) 0.9998(8) -0.0936(5) 0.054(3) Uani 1 1 d . . . C52 C 0.6385(7) 0.9791(7) -0.0734(4) 0.039(2) Uani 1 1 d . . . H52A H 0.6765 1.0257 -0.0883 0.047 Uiso 1 1 calc R . . C53 C 0.4572(7) 0.7794(8) 0.0025(5) 0.053(3) Uani 1 1 d . . . C54 C 0.5304(7) 0.6653(7) -0.0242(4) 0.053(2) Uani 1 1 d . . . H54A H 0.5376 0.6665 -0.0734 0.079 Uiso 1 1 calc R . . H54B H 0.4940 0.6168 -0.0030 0.079 Uiso 1 1 calc R . . H54C H 0.6057 0.6408 -0.0131 0.079 Uiso 1 1 calc R . . C55 C 0.4243(9) 0.7739(9) 0.0770(5) 0.063(3) Uani 1 1 d . . . H55A H 0.3748 0.8451 0.0935 0.094 Uiso 1 1 calc R . . H55B H 0.4922 0.7467 0.0970 0.094 Uiso 1 1 calc R . . H55C H 0.3840 0.7262 0.0898 0.094 Uiso 1 1 calc R . . C56 C 0.3491(8) 0.8142(9) -0.0259(7) 0.091(4) Uani 1 1 d . . . H56A H 0.2946 0.8825 -0.0072 0.137 Uiso 1 1 calc R . . H56B H 0.3163 0.7606 -0.0135 0.137 Uiso 1 1 calc R . . H56C H 0.3670 0.8217 -0.0753 0.137 Uiso 1 1 calc R . . C57 C 0.4921(9) 1.0879(9) -0.1438(5) 0.071(3) Uani 1 1 d . . . H57A H 0.4153 1.0963 -0.1456 0.106 Uiso 1 1 calc R . . H57B H 0.5403 1.0701 -0.1886 0.106 Uiso 1 1 calc R . . H57C H 0.4903 1.1544 -0.1298 0.106 Uiso 1 1 calc R . . C58 C 0.8766(7) 0.9058(7) -0.0742(5) 0.043(2) Uani 1 1 d . . . C59 C 0.8970(7) 0.8682(7) -0.1377(4) 0.038(2) Uani 1 1 d . . . C60 C 0.9481(7) 0.9121(7) -0.1938(4) 0.042(2) Uani 1 1 d . . . C61 C 0.9906(9) 0.9830(8) -0.1839(5) 0.064(3) Uani 1 1 d . . . H61A H 1.0255 1.0126 -0.2223 0.076 Uiso 1 1 calc R . . C62 C 0.9854(9) 1.0137(9) -0.1209(5) 0.064(3) Uani 1 1 d . . . C63 C 0.9250(8) 0.9778(8) -0.0635(5) 0.058(3) Uani 1 1 d . . . H63A H 0.9168 1.0006 -0.0195 0.069 Uiso 1 1 calc R . . C64 C 0.9498(9) 0.8807(8) -0.2648(4) 0.060(3) Uani 1 1 d . . . C65 C 1.0306(9) 0.7635(8) -0.2767(4) 0.064(3) Uani 1 1 d . . . H65A H 1.0036 0.7177 -0.2431 0.096 Uiso 1 1 calc R . . H65B H 1.1067 0.7538 -0.2722 0.096 Uiso 1 1 calc R . . H65C H 1.0328 0.7447 -0.3222 0.096 Uiso 1 1 calc R . . C66 C 0.9935(11) 0.9553(9) -0.3208(5) 0.089(4) Uani 1 1 d . . . H66A H 0.9454 1.0302 -0.3117 0.134 Uiso 1 1 calc R . . H66B H 0.9898 0.9392 -0.3658 0.134 Uiso 1 1 calc R . . H66C H 1.0718 0.9420 -0.3192 0.134 Uiso 1 1 calc R . . C67 C 0.8282(8) 0.9052(10) -0.2726(5) 0.082(4) Uani 1 1 d . . . H67A H 0.7991 0.8575 -0.2423 0.124 Uiso 1 1 calc R . . H67B H 0.8281 0.8944 -0.3195 0.124 Uiso 1 1 calc R . . H67C H 0.7801 0.9791 -0.2610 0.124 Uiso 1 1 calc R . . C68 C 1.0412(10) 1.0863(9) -0.1105(5) 0.090(4) Uani 1 1 d . . . H68A H 1.0846 1.0564 -0.0744 0.136 Uiso 1 1 calc R . . H68B H 0.9830 1.1567 -0.0980 0.136 Uiso 1 1 calc R . . H68C H 1.0920 1.0928 -0.1525 0.136 Uiso 1 1 calc R . . Ni2 Ni 0.42431(6) 1.17786(7) 0.25122(4) 0.0365(3) Uani 1 1 d . . . O7 O 0.4219(5) 1.2602(5) 0.3159(3) 0.0377(14) Uani 1 1 d . . . O8 O 0.2835(5) 1.2216(5) 0.4305(3) 0.0481(17) Uani 1 1 d D . . O9 O 0.4851(5) 1.2088(5) 0.5457(3) 0.0502(17) Uani 1 1 d D . . O10 O 0.4721(5) 1.0693(5) 0.3124(3) 0.0371(14) Uani 1 1 d . . . O11 O 0.4528(5) 1.0186(5) 0.5611(3) 0.0482(16) Uani 1 1 d . . . H11B H 0.4852 1.0376 0.5245 0.072 Uiso 1 1 calc R . . O12 O 0.6543(5) 1.0582(5) 0.3738(3) 0.0528(17) Uani 1 1 d D . . N3 N 0.3800(6) 1.2881(6) 0.1888(3) 0.0412(18) Uani 1 1 d . . . N4 N 0.4239(6) 1.0928(6) 0.1891(3) 0.0434(18) Uani 1 1 d . . . C69 C 0.3791(6) 1.2545(6) 0.1232(3) 0.0452(17) Uani 1 1 d . . . H69A H 0.4577 1.2331 0.0961 0.054 Uiso 1 1 calc R . . C70 C 0.2995(8) 1.3365(7) 0.0802(4) 0.046(2) Uani 1 1 d . . . H70A H 0.3208 1.3985 0.0684 0.055 Uiso 1 1 calc R . . H70B H 0.2205 1.3616 0.1056 0.055 Uiso 1 1 calc R . . C71 C 0.3107(7) 1.2799(6) 0.0137(3) 0.0531(19) Uani 1 1 d . . . H71A H 0.2554 1.3293 -0.0132 0.064 Uiso 1 1 calc R . . H71B H 0.3874 1.2637 -0.0139 0.064 Uiso 1 1 calc R . . C72 C 0.2910(6) 1.1791(6) 0.0284(4) 0.057(2) Uani 1 1 d . . . H72A H 0.3046 1.1444 -0.0146 0.068 Uiso 1 1 calc R . . H72B H 0.2112 1.1959 0.0508 0.068 Uiso 1 1 calc R . . C73 C 0.3700(8) 1.1014(8) 0.0747(4) 0.053(3) Uani 1 1 d . . . H73A H 0.3527 1.0371 0.0856 0.064 Uiso 1 1 calc R . . H73B H 0.4498 1.0791 0.0509 0.064 Uiso 1 1 calc R . . C74 C 0.3540(6) 1.1544(5) 0.1381(3) 0.0451(17) Uani 1 1 d . . . H74A H 0.2727 1.1765 0.1606 0.054 Uiso 1 1 calc R . . C75 C 0.3545(7) 1.3878(7) 0.1964(4) 0.042(2) Uani 1 1 d . . . H75A H 0.3291 1.4365 0.1605 0.050 Uiso 1 1 calc R . . C76 C 0.3624(7) 1.4288(7) 0.2554(5) 0.041(2) Uani 1 1 d . . . C77 C 0.3297(8) 1.5426(8) 0.2556(5) 0.050(3) Uani 1 1 d . . . H77A H 0.3072 1.5848 0.2168 0.060 Uiso 1 1 calc R . . C78 C 0.3306(7) 1.5923(7) 0.3127(4) 0.041(2) Uani 1 1 d . . . C79 C 0.3588(7) 1.5259(7) 0.3686(5) 0.043(2) Uani 1 1 d . . . H79A H 0.3546 1.5583 0.4086 0.052 Uiso 1 1 calc R . . C80 C 0.3939(6) 1.4124(7) 0.3713(4) 0.036(2) Uani 1 1 d . . . C81 C 0.3910(7) 1.3641(8) 0.3124(4) 0.038(2) Uani 1 1 d . . . C82 C 0.2961(9) 1.7113(7) 0.3152(5) 0.070(3) Uani 1 1 d . . . H82A H 0.3147 1.7397 0.2696 0.104 Uiso 1 1 calc R . . H82B H 0.3367 1.7258 0.3452 0.104 Uiso 1 1 calc R . . H82C H 0.2145 1.7452 0.3322 0.104 Uiso 1 1 calc R . . C83 C 0.4201(7) 1.3404(7) 0.4338(4) 0.040(2) Uani 1 1 d . . . H83A H 0.4538 1.2649 0.4195 0.048 Uiso 1 1 calc R . . C84 C 0.3044(7) 1.3595(7) 0.4824(4) 0.036(2) Uani 1 1 d . . . C85 C 0.2477(6) 1.2953(7) 0.4777(4) 0.0330(19) Uani 1 1 d . . . C86 C 0.1449(6) 1.3077(7) 0.5295(4) 0.041(2) Uani 1 1 d . . . C87 C 0.1123(7) 1.3844(8) 0.5772(4) 0.048(2) Uani 1 1 d . . . H87A H 0.0458 1.3929 0.6100 0.057 Uiso 1 1 calc R . . C88 C 0.1650(7) 1.4475(7) 0.5815(5) 0.045(2) Uani 1 1 d . . . C89 C 0.2641(6) 1.4348(7) 0.5332(4) 0.041(2) Uani 1 1 d . . . H89A H 0.3044 1.4779 0.5350 0.049 Uiso 1 1 calc R . . C90 C 0.0783(7) 1.2398(8) 0.5265(5) 0.050(3) Uani 1 1 d . . . C91 C -0.0239(7) 1.2589(8) 0.5853(6) 0.084(4) Uani 1 1 d . . . H91A H -0.0793 1.3320 0.5820 0.126 Uiso 1 1 calc R . . H91B H 0.0016 1.2477 0.6285 0.126 Uiso 1 1 calc R . . H91C H -0.0590 1.2091 0.5830 0.126 Uiso 1 1 calc R . . C92 C 0.0269(10) 1.2723(11) 0.4594(6) 0.098(4) Uani 1 1 d . . . H92A H -0.0154 1.3495 0.4573 0.147 Uiso 1 1 calc R . . H92B H -0.0240 1.2364 0.4596 0.147 Uiso 1 1 calc R . . H92C H 0.0884 1.2511 0.4198 0.147 Uiso 1 1 calc R . . C93 C 0.1523(8) 1.1217(8) 0.5294(5) 0.059(3) Uani 1 1 d . . . H93A H 0.2214 1.1065 0.4949 0.089 Uiso 1 1 calc R . . H93B H 0.1110 1.0806 0.5209 0.089 Uiso 1 1 calc R . . H93C H 0.1723 1.1019 0.5742 0.089 Uiso 1 1 calc R . . C94 C 0.1267(8) 1.5300(8) 0.6364(5) 0.071(3) Uani 1 1 d . . . H94A H 0.1874 1.5540 0.6360 0.106 Uiso 1 1 calc R . . H94B H 0.1091 1.4977 0.6808 0.106 Uiso 1 1 calc R . . H94C H 0.0592 1.5909 0.6274 0.106 Uiso 1 1 calc R . . C95 C 0.5025(7) 1.3558(7) 0.4743(4) 0.034(2) Uani 1 1 d . . . C96 C 0.5243(7) 1.2916(8) 0.5304(5) 0.048(3) Uani 1 1 d . . . C97 C 0.5913(7) 1.2984(8) 0.5740(5) 0.046(2) Uani 1 1 d . . . C98 C 0.6391(7) 1.3727(7) 0.5563(4) 0.043(2) Uani 1 1 d . . . H98A H 0.6814 1.3830 0.5852 0.051 Uiso 1 1 calc R . . C99 C 0.6254(7) 1.4341(7) 0.4946(5) 0.047(2) Uani 1 1 d . . . C100 C 0.5572(7) 1.4293(7) 0.4555(5) 0.044(2) Uani 1 1 d . . . H10A H 0.5455 1.4738 0.4160 0.053 Uiso 1 1 calc R . . C101 C 0.6047(8) 1.2291(9) 0.6401(5) 0.057(3) Uani 1 1 d . . . C102 C 0.6628(11) 1.1136(11) 0.6287(7) 0.103(4) Uani 1 1 d . . . H10B H 0.6251 1.0928 0.5997 0.154 Uiso 1 1 calc R . . H10C H 0.6600 1.0745 0.6722 0.154 Uiso 1 1 calc R . . H10D H 0.7418 1.0970 0.6067 0.154 Uiso 1 1 calc R . . C103 C 0.6755(11) 1.2582(12) 0.6779(6) 0.105(5) Uani 1 1 d . . . H10E H 0.7422 1.2615 0.6463 0.157 Uiso 1 1 calc R . . H10F H 0.6996 1.2043 0.7135 0.157 Uiso 1 1 calc R . . H10G H 0.6302 1.3277 0.6982 0.157 Uiso 1 1 calc R . . C104 C 0.4858(8) 1.2532(10) 0.6841(5) 0.082(4) Uani 1 1 d . . . H10H H 0.4399 1.2353 0.6595 0.123 Uiso 1 1 calc R . . H10I H 0.4495 1.3289 0.6943 0.123 Uiso 1 1 calc R . . H10J H 0.4927 1.2106 0.7264 0.123 Uiso 1 1 calc R . . C105 C 0.6796(9) 1.5136(9) 0.4761(5) 0.073(3) Uani 1 1 d . . . H10K H 0.6946 1.5240 0.4269 0.109 Uiso 1 1 calc R . . H10L H 0.7509 1.4871 0.4926 0.109 Uiso 1 1 calc R . . H10M H 0.6286 1.5815 0.4970 0.109 Uiso 1 1 calc R . . C106 C 0.4697(8) 0.9895(8) 0.1879(5) 0.050(2) Uani 1 1 d . . . H10N H 0.4725 0.9554 0.1490 0.060 Uiso 1 1 calc R . . C107 C 0.5150(7) 0.9269(7) 0.2424(4) 0.038(2) Uani 1 1 d . . . C108 C 0.5611(8) 0.8149(8) 0.2323(4) 0.048(2) Uani 1 1 d . . . H10O H 0.5678 0.7892 0.1894 0.057 Uiso 1 1 calc R . . C109 C 0.5980(7) 0.7397(7) 0.2881(4) 0.040(2) Uani 1 1 d . . . C110 C 0.5848(7) 0.7876(8) 0.3489(4) 0.043(2) Uani 1 1 d . . . H11C H 0.6116 0.7414 0.3855 0.051 Uiso 1 1 calc R . . C111 C 0.5362(7) 0.8960(7) 0.3604(4) 0.034(2) Uani 1 1 d . . . C112 C 0.5078(7) 0.9633(7) 0.3052(4) 0.035(2) Uani 1 1 d . . . C113 C 0.6416(8) 0.6240(7) 0.2797(4) 0.049(2) Uani 1 1 d . . . H11D H 0.6574 0.5869 0.3228 0.073 Uiso 1 1 calc R . . H11E H 0.7115 0.6019 0.2454 0.073 Uiso 1 1 calc R . . H11F H 0.5851 0.6065 0.2651 0.073 Uiso 1 1 calc R . . C114 C 0.5186(6) 0.9364(7) 0.4289(4) 0.038(2) Uani 1 1 d . . . H11G H 0.4794 1.0156 0.4254 0.045 Uiso 1 1 calc R . . C115 C 0.4452(7) 0.8991(7) 0.4841(3) 0.036(2) Uani 1 1 d . . . C116 C 0.4269(7) 0.9364(7) 0.5503(4) 0.038(2) Uani 1 1 d . . . C117 C 0.3715(7) 0.8977(7) 0.6094(4) 0.041(2) Uani 1 1 d . . . C118 C 0.3276(8) 0.8263(7) 0.5962(5) 0.053(3) Uani 1 1 d . . . H11H H 0.2881 0.7990 0.6335 0.063 Uiso 1 1 calc R . . C119 C 0.3379(9) 0.7929(8) 0.5320(5) 0.058(3) Uani 1 1 d . . . C120 C 0.3993(7) 0.8295(7) 0.4791(4) 0.046(2) Uani 1 1 d . . . H12B H 0.4102 0.8038 0.4355 0.055 Uiso 1 1 calc R . . C121 C 0.3651(7) 0.9230(8) 0.6817(4) 0.048(2) Uani 1 1 d . . . C122 C 0.3246(10) 0.8561(8) 0.7332(5) 0.085(4) Uani 1 1 d . . . H12C H 0.2463 0.8695 0.7314 0.127 Uiso 1 1 calc R . . H12D H 0.3278 0.8731 0.7781 0.127 Uiso 1 1 calc R . . H12E H 0.3724 0.7811 0.7246 0.127 Uiso 1 1 calc R . . C123 C 0.2860(9) 1.0363(7) 0.6989(5) 0.066(3) Uani 1 1 d . . . H12F H 0.2102 1.0486 0.6924 0.099 Uiso 1 1 calc R . . H12G H 0.3138 1.0854 0.6692 0.099 Uiso 1 1 calc R . . H12H H 0.2829 1.0482 0.7461 0.099 Uiso 1 1 calc R . . C124 C 0.4808(9) 0.9117(8) 0.6917(5) 0.079(3) Uani 1 1 d . . . H12I H 0.4986 0.9709 0.6681 0.119 Uiso 1 1 calc R . . H12J H 0.5384 0.8443 0.6734 0.119 Uiso 1 1 calc R . . H12K H 0.4797 0.9127 0.7401 0.119 Uiso 1 1 calc R . . C125 C 0.2884(13) 0.7127(12) 0.5242(6) 0.130(7) Uani 1 1 d . . . H12L H 0.2204 0.7237 0.5591 0.195 Uiso 1 1 calc R . . H12M H 0.3444 0.6403 0.5291 0.195 Uiso 1 1 calc R . . H12N H 0.2687 0.7226 0.4794 0.195 Uiso 1 1 calc R . . C126 C 0.6319(7) 0.9140(6) 0.4457(4) 0.041(2) Uani 1 1 d . . . C127 C 0.6949(7) 0.9793(8) 0.4175(4) 0.047(3) Uani 1 1 d . . . C128 C 0.7982(7) 0.9606(8) 0.4359(5) 0.050(3) Uani 1 1 d . . . C129 C 0.8359(8) 0.8812(9) 0.4825(5) 0.058(3) Uani 1 1 d . . . H12O H 0.9044 0.8707 0.4958 0.070 Uiso 1 1 calc R . . C130 C 0.7800(8) 0.8130(8) 0.5128(4) 0.048(2) Uani 1 1 d . . . C131 C 0.6776(8) 0.8324(8) 0.4939(4) 0.048(2) Uani 1 1 d . . . H13A H 0.6368 0.7897 0.5139 0.058 Uiso 1 1 calc R . . C132 C 0.8629(7) 1.0345(9) 0.4091(5) 0.062(3) Uani 1 1 d . . . C133 C 0.9746(8) 0.9949(9) 0.4365(5) 0.078(4) Uani 1 1 d . . . H13B H 1.0142 1.0423 0.4194 0.116 Uiso 1 1 calc R . . H13C H 1.0229 0.9226 0.4214 0.116 Uiso 1 1 calc R . . H13D H 0.9572 0.9948 0.4861 0.116 Uiso 1 1 calc R . . C134 C 0.8977(9) 1.0213(9) 0.3285(5) 0.079(4) Uani 1 1 d . . . H13E H 0.8296 1.0394 0.3097 0.118 Uiso 1 1 calc R . . H13F H 0.9489 0.9475 0.3183 0.118 Uiso 1 1 calc R . . H13G H 0.9358 1.0688 0.3083 0.118 Uiso 1 1 calc R . . C135 C 0.7911(9) 1.1501(9) 0.4269(7) 0.118(5) Uani 1 1 d . . . H13H H 0.7220 1.1747 0.4081 0.177 Uiso 1 1 calc R . . H13I H 0.8341 1.1939 0.4078 0.177 Uiso 1 1 calc R . . H13J H 0.7709 1.1559 0.4761 0.177 Uiso 1 1 calc R . . C136 C 0.8228(8) 0.7237(10) 0.5646(5) 0.080(4) Uani 1 1 d . . . H13K H 0.7758 0.6820 0.5733 0.121 Uiso 1 1 calc R . . H13L H 0.8187 0.7544 0.6068 0.121 Uiso 1 1 calc R . . H13M H 0.9014 0.6775 0.5470 0.121 Uiso 1 1 calc R . . N6 N 0.8209(6) 1.3696(5) 0.3254(3) 0.079(2) Uani 1 1 d . . . C139 C 0.7614(7) 1.3445(6) 0.3108(3) 0.0571(18) Uani 1 1 d . . . C140 C 0.6812(7) 1.3092(7) 0.2877(4) 0.080(2) Uani 1 1 d . . . N7 N 0.1677(10) 1.6556(15) 0.1365(7) 0.201(9) Uani 1 1 d . . . C141 C 0.1284(9) 1.7222(14) 0.1049(8) 0.123(6) Uani 1 1 d . . . C142 C 0.0749(9) 1.7986(12) 0.0596(7) 0.129(6) Uani 1 1 d . . . N8 N 0.2010(13) 1.0116(14) 0.2385(7) 0.109(6) Uiso 0.513(11) 1 d PD A 1 C143 C 0.213(2) 1.018(2) 0.2916(9) 0.121(9) Uiso 0.513(11) 1 d PD A 1 N8' N 0.1397(12) 1.1673(11) 0.2854(8) 0.067(5) Uiso 0.487(11) 1 d PD A 2 C144 C 0.1849(12) 1.0942(11) 0.3162(7) 0.036(4) Uiso 0.487(11) 1 d PD A 2 C145 C 0.2415(11) 1.0057(11) 0.3568(7) 0.117(5) Uiso 1 1 d D . . H2 H 0.914(2) 0.571(5) -0.129(3) 0.041(18) Uiso 1 1 d D . . H3 H 0.989(5) 0.576(7) 0.007(3) 0.081 Uiso 1 1 d D . . H5 H 0.730(4) 0.724(6) 0.051(4) 0.080 Uiso 1 1 d D . . H6 H 0.799(3) 0.802(6) -0.123(3) 0.080 Uiso 1 1 d D . . H8 H 0.316(4) 1.240(5) 0.3941(19) 0.032(17) Uiso 1 1 d D . . H9 H 0.418(3) 1.210(6) 0.562(4) 0.082 Uiso 1 1 d D . . H11A H 0.954(6) 0.255(6) -0.003(4) 0.080 Uiso 1 1 d . . . H12 H 0.599(5) 1.055(6) 0.360(4) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0488(6) 0.0341(7) 0.0316(6) -0.0022(5) -0.0071(5) -0.0217(5) O1 0.064(3) 0.030(4) 0.032(3) -0.002(3) -0.008(3) -0.019(3) O2 0.060(4) 0.054(5) 0.075(5) 0.024(4) -0.029(3) -0.036(4) O3 0.088(5) 0.048(4) 0.038(3) -0.013(3) -0.004(3) -0.048(4) O4 0.050(3) 0.031(4) 0.041(3) -0.005(3) -0.015(2) -0.019(3) O5 0.047(3) 0.053(4) 0.053(4) 0.001(3) -0.016(3) -0.032(3) O6 0.062(4) 0.034(4) 0.055(4) -0.021(3) -0.003(3) -0.027(3) N1 0.043(3) 0.037(4) 0.030(3) -0.007(3) -0.001(3) -0.020(3) N2 0.053(4) 0.043(4) 0.029(3) -0.011(3) -0.005(3) -0.022(3) C1 0.045(4) 0.043(4) 0.039(4) -0.007(3) -0.011(3) -0.022(3) C2 0.061(5) 0.053(6) 0.063(6) 0.003(5) -0.030(5) -0.026(5) C3 0.060(5) 0.062(5) 0.038(4) 0.000(3) -0.010(3) -0.028(4) C4 0.072(5) 0.056(5) 0.045(4) -0.013(4) -0.020(4) -0.019(4) C5 0.068(5) 0.052(6) 0.028(4) -0.005(4) -0.029(4) -0.010(4) C6 0.058(4) 0.037(4) 0.028(3) -0.006(3) -0.006(3) -0.019(3) C7 0.049(5) 0.055(6) 0.037(5) 0.005(4) -0.007(4) -0.021(4) C8 0.045(5) 0.045(6) 0.028(4) -0.012(4) -0.006(4) -0.017(4) C9 0.047(5) 0.035(6) 0.038(5) 0.005(4) -0.010(4) -0.006(4) C10 0.053(5) 0.026(5) 0.065(6) -0.022(4) -0.015(5) -0.005(4) C11 0.045(5) 0.047(6) 0.035(5) 0.003(4) -0.016(4) -0.016(4) C12 0.054(6) 0.032(6) 0.038(5) -0.010(4) -0.001(4) -0.024(5) C13 0.044(5) 0.014(4) 0.057(6) 0.004(4) -0.007(4) -0.012(4) C14 0.058(5) 0.037(6) 0.066(6) -0.006(4) -0.022(4) -0.026(4) C15 0.033(4) 0.029(5) 0.044(5) -0.019(4) -0.005(4) -0.016(4) C16 0.034(4) 0.038(6) 0.037(5) -0.014(4) 0.007(4) -0.010(4) C17 0.041(5) 0.034(5) 0.027(4) 0.001(4) -0.011(4) -0.019(4) C18 0.052(5) 0.047(6) 0.028(4) 0.000(4) -0.008(4) -0.025(4) C19 0.051(5) 0.088(8) 0.055(6) -0.005(6) -0.015(4) -0.046(5) C20 0.064(6) 0.059(7) 0.043(5) -0.001(5) -0.009(4) -0.042(5) C21 0.046(5) 0.050(6) 0.027(4) 0.002(4) -0.016(3) -0.031(4) C22 0.054(6) 0.087(9) 0.071(7) 0.025(6) -0.029(5) -0.043(6) C23 0.086(7) 0.074(9) 0.094(9) 0.050(7) -0.051(6) -0.021(6) C24 0.083(7) 0.130(10) 0.048(6) 0.012(6) -0.019(5) -0.062(7) C25 0.076(6) 0.136(11) 0.079(7) 0.044(7) -0.046(6) -0.078(7) C26 0.100(8) 0.069(8) 0.107(9) 0.004(7) -0.032(7) -0.057(7) C27 0.042(5) 0.031(5) 0.047(5) 0.000(4) -0.019(4) -0.017(4) C28 0.052(5) 0.042(6) 0.037(5) -0.009(4) -0.009(4) -0.028(4) C29 0.053(5) 0.055(6) 0.046(5) -0.011(4) -0.008(4) -0.039(5) C30 0.038(5) 0.044(6) 0.071(6) -0.011(5) -0.012(4) -0.020(4) C31 0.057(6) 0.061(8) 0.056(6) -0.033(5) 0.010(5) -0.023(6) C32 0.064(6) 0.022(5) 0.058(6) -0.011(4) 0.002(5) -0.025(4) C33 0.051(5) 0.039(6) 0.078(7) -0.007(5) -0.008(5) -0.037(5) C34 0.059(6) 0.054(7) 0.078(7) -0.005(5) -0.005(5) -0.031(5) C35 0.050(5) 0.038(4) 0.074(6) 0.000(4) -0.025(4) -0.021(4) C36 0.072(7) 0.093(9) 0.062(6) -0.007(6) 0.009(5) -0.057(7) C37 0.062(6) 0.095(9) 0.106(9) -0.039(7) -0.003(6) -0.046(6) C38 0.053(4) 0.028(5) 0.039(4) -0.012(3) -0.012(3) -0.011(4) C39 0.041(4) 0.044(5) 0.027(4) -0.014(4) -0.004(3) -0.015(4) C40 0.042(5) 0.039(6) 0.045(5) -0.005(4) -0.013(4) -0.021(4) C41 0.049(5) 0.037(6) 0.043(5) -0.006(4) -0.010(4) -0.022(4) C42 0.039(4) 0.029(5) 0.044(5) 0.005(4) -0.010(4) -0.019(4) C43 0.044(5) 0.035(5) 0.030(4) -0.014(4) -0.003(4) -0.013(4) C44 0.037(4) 0.038(6) 0.031(4) 0.000(4) -0.001(4) -0.019(4) C45 0.047(5) 0.021(5) 0.084(7) -0.011(4) -0.012(4) -0.012(4) C46 0.052(5) 0.029(5) 0.024(4) 0.001(3) -0.006(4) -0.024(4) C47 0.035(4) 0.055(6) 0.031(4) 0.001(4) -0.015(3) -0.026(4) C48 0.047(5) 0.022(5) 0.038(5) -0.008(4) -0.013(4) -0.008(4) C49 0.045(5) 0.039(6) 0.056(6) -0.022(5) -0.003(4) -0.022(4) C50 0.038(5) 0.052(6) 0.067(6) -0.023(5) -0.015(4) -0.016(4) C51 0.053(6) 0.047(6) 0.058(6) -0.011(4) -0.007(4) -0.015(5) C52 0.042(4) 0.050(6) 0.033(4) -0.005(4) 0.001(3) -0.028(4) C53 0.053(5) 0.046(6) 0.061(6) -0.010(5) -0.008(5) -0.020(5) C54 0.058(5) 0.047(5) 0.068(5) -0.003(4) -0.025(4) -0.029(4) C55 0.077(7) 0.057(6) 0.070(6) -0.011(5) -0.012(5) -0.041(5) C56 0.053(6) 0.058(8) 0.170(13) 0.005(8) -0.022(7) -0.031(6) C57 0.084(7) 0.081(8) 0.055(6) 0.022(5) -0.021(5) -0.043(6) C58 0.050(5) 0.022(5) 0.064(6) 0.004(4) -0.019(5) -0.017(4) C59 0.057(5) 0.024(5) 0.031(5) 0.008(4) -0.013(4) -0.015(4) C60 0.058(5) 0.032(5) 0.037(5) -0.009(4) -0.007(4) -0.018(4) C61 0.107(8) 0.057(7) 0.035(5) -0.007(5) 0.013(5) -0.052(7) C62 0.079(7) 0.065(8) 0.063(7) -0.027(6) 0.013(6) -0.052(6) C63 0.088(7) 0.068(7) 0.046(5) -0.011(5) 0.005(5) -0.067(6) C64 0.099(7) 0.046(6) 0.036(5) 0.005(4) -0.020(5) -0.028(6) C65 0.098(7) 0.059(7) 0.032(4) -0.019(4) -0.014(4) -0.023(5) C66 0.173(11) 0.096(9) 0.035(5) 0.019(6) -0.031(6) -0.090(9) C67 0.067(6) 0.147(11) 0.046(5) -0.012(6) -0.032(4) -0.040(6) C68 0.147(10) 0.083(8) 0.071(7) -0.039(6) 0.044(7) -0.099(8) Ni2 0.0450(6) 0.0353(7) 0.0336(6) -0.0076(5) -0.0035(5) -0.0204(5) O7 0.058(3) 0.029(4) 0.035(3) -0.005(3) -0.005(3) -0.028(3) O8 0.051(4) 0.063(5) 0.046(4) -0.013(3) -0.001(3) -0.039(4) O9 0.060(4) 0.033(4) 0.069(4) 0.001(3) -0.011(3) -0.031(3) O10 0.053(3) 0.034(4) 0.030(3) -0.005(3) -0.006(2) -0.023(3) O11 0.069(4) 0.048(4) 0.042(3) 0.002(3) -0.010(3) -0.039(3) O12 0.066(4) 0.040(4) 0.063(4) 0.009(3) -0.009(3) -0.036(3) N3 0.050(4) 0.042(4) 0.036(4) -0.006(3) -0.002(3) -0.025(3) N4 0.059(4) 0.041(4) 0.031(4) 0.004(3) -0.017(3) -0.018(3) C69 0.057(4) 0.057(5) 0.036(4) -0.003(3) -0.012(3) -0.035(4) C70 0.073(6) 0.038(5) 0.035(4) -0.005(4) -0.012(4) -0.027(4) C71 0.081(5) 0.042(4) 0.043(4) 0.001(3) -0.022(4) -0.027(4) C72 0.058(5) 0.063(5) 0.057(5) -0.007(4) -0.017(4) -0.027(4) C73 0.080(6) 0.047(6) 0.034(4) -0.018(4) 0.007(4) -0.031(5) C74 0.045(4) 0.043(4) 0.049(4) -0.007(3) -0.006(3) -0.019(3) C75 0.054(5) 0.043(5) 0.036(4) 0.002(4) -0.010(4) -0.026(4) C76 0.052(5) 0.032(5) 0.046(5) -0.004(4) -0.004(4) -0.026(4) C77 0.069(6) 0.048(7) 0.051(6) -0.005(5) -0.017(5) -0.036(5) C78 0.052(5) 0.044(5) 0.040(5) 0.014(4) -0.015(4) -0.032(4) C79 0.045(5) 0.035(6) 0.059(6) -0.015(4) -0.004(4) -0.027(4) C80 0.033(5) 0.043(6) 0.037(5) -0.006(4) -0.003(4) -0.021(4) C81 0.049(5) 0.059(7) 0.021(4) -0.014(4) 0.000(3) -0.037(5) C82 0.115(8) 0.027(5) 0.064(7) 0.002(5) -0.030(6) -0.019(5) C83 0.054(5) 0.031(5) 0.039(5) 0.003(4) -0.013(4) -0.022(4) C84 0.040(5) 0.034(5) 0.034(5) -0.011(4) 0.001(4) -0.015(4) C85 0.036(4) 0.034(5) 0.031(4) -0.001(4) -0.002(3) -0.018(4) C86 0.035(4) 0.036(5) 0.054(6) 0.012(4) -0.015(4) -0.015(4) C87 0.047(5) 0.056(6) 0.041(5) -0.012(4) 0.015(4) -0.031(5) C88 0.049(5) 0.035(6) 0.056(6) -0.009(4) -0.007(4) -0.023(5) C89 0.028(4) 0.054(6) 0.047(5) -0.012(4) -0.008(4) -0.020(4) C90 0.038(5) 0.060(7) 0.056(6) 0.007(5) -0.015(4) -0.024(5) C91 0.046(6) 0.060(8) 0.149(11) -0.017(7) 0.002(6) -0.031(5) C92 0.122(9) 0.139(11) 0.098(9) 0.031(8) -0.063(7) -0.105(9) C93 0.069(6) 0.056(7) 0.075(7) 0.017(5) -0.029(5) -0.044(5) C94 0.091(7) 0.051(6) 0.064(6) -0.043(5) 0.034(6) -0.035(6) C95 0.046(5) 0.027(5) 0.042(5) -0.002(4) -0.017(4) -0.023(4) C96 0.040(5) 0.038(6) 0.067(6) -0.004(5) 0.000(5) -0.021(4) C97 0.031(4) 0.048(6) 0.065(6) -0.001(5) -0.011(4) -0.020(4) C98 0.056(5) 0.040(5) 0.041(5) -0.002(4) -0.019(4) -0.023(4) C99 0.042(5) 0.038(6) 0.073(6) 0.007(5) -0.021(4) -0.024(4) C100 0.043(5) 0.028(5) 0.063(6) -0.002(4) 0.001(4) -0.020(4) C101 0.069(6) 0.074(8) 0.038(5) 0.014(5) -0.020(5) -0.038(6) C102 0.112(10) 0.090(11) 0.121(11) 0.018(9) -0.042(9) -0.050(9) C103 0.135(11) 0.156(14) 0.048(7) 0.016(7) -0.046(7) -0.072(10) C104 0.064(6) 0.106(9) 0.057(7) 0.029(6) -0.004(5) -0.026(6) C105 0.086(7) 0.095(9) 0.079(8) 0.022(7) -0.040(6) -0.072(7) C106 0.068(5) 0.057(6) 0.036(5) -0.003(4) -0.010(4) -0.034(5) C107 0.044(4) 0.028(5) 0.045(5) 0.001(4) -0.001(4) -0.022(4) C108 0.058(5) 0.051(7) 0.036(5) -0.019(5) -0.007(4) -0.020(5) C109 0.040(5) 0.044(6) 0.038(5) -0.005(4) -0.003(4) -0.021(4) C110 0.051(5) 0.054(6) 0.035(5) -0.007(4) -0.005(4) -0.032(5) C111 0.040(4) 0.035(5) 0.037(5) 0.003(4) -0.004(4) -0.028(4) C112 0.039(4) 0.033(5) 0.036(5) -0.016(4) 0.002(4) -0.018(4) C113 0.070(6) 0.051(6) 0.030(4) -0.009(4) -0.009(4) -0.027(5) C114 0.036(4) 0.035(5) 0.052(5) -0.007(4) -0.010(4) -0.022(4) C115 0.050(5) 0.044(6) 0.019(4) -0.007(4) 0.003(4) -0.028(4) C116 0.040(5) 0.030(5) 0.056(6) -0.019(4) -0.009(4) -0.020(4) C117 0.052(5) 0.024(5) 0.039(5) -0.006(4) 0.005(4) -0.014(4) C118 0.068(6) 0.030(5) 0.056(6) -0.011(5) 0.012(5) -0.024(5) C119 0.094(7) 0.055(7) 0.042(6) -0.020(5) 0.021(5) -0.058(6) C120 0.062(5) 0.040(5) 0.034(5) -0.021(4) -0.003(4) -0.017(4) C121 0.055(5) 0.051(6) 0.044(5) -0.007(4) 0.001(4) -0.030(5) C122 0.113(8) 0.055(7) 0.044(6) -0.009(5) 0.017(6) -0.006(6) C123 0.101(7) 0.034(5) 0.050(5) -0.011(4) 0.015(5) -0.027(5) C124 0.105(8) 0.059(6) 0.045(5) -0.001(5) -0.005(5) -0.009(5) C125 0.203(15) 0.174(16) 0.080(9) -0.059(9) 0.044(10) -0.163(14) C126 0.059(5) 0.024(5) 0.043(5) -0.016(4) 0.007(4) -0.023(4) C127 0.052(5) 0.060(7) 0.042(5) -0.007(5) 0.003(4) -0.038(5) C128 0.043(5) 0.068(8) 0.046(6) -0.022(5) 0.003(4) -0.029(5) C129 0.055(6) 0.072(7) 0.045(6) -0.014(5) -0.015(5) -0.016(5) C130 0.053(5) 0.071(7) 0.030(4) -0.005(4) -0.012(4) -0.031(5) C131 0.062(6) 0.048(6) 0.041(5) -0.001(4) -0.010(4) -0.027(5) C132 0.043(5) 0.069(8) 0.083(8) -0.031(6) 0.010(5) -0.036(5) C133 0.054(6) 0.106(10) 0.094(8) -0.031(7) -0.002(6) -0.052(7) C134 0.075(7) 0.082(8) 0.094(8) -0.022(6) 0.024(6) -0.062(6) C135 0.072(7) 0.085(9) 0.205(14) -0.086(9) 0.051(8) -0.057(7) C136 0.057(6) 0.112(10) 0.051(6) 0.006(6) -0.021(5) -0.008(6) N6 0.109(6) 0.075(5) 0.075(5) 0.012(4) -0.019(4) -0.060(4) C139 0.077(5) 0.044(4) 0.040(4) 0.012(3) -0.004(4) -0.020(4) C140 0.088(5) 0.092(6) 0.068(5) -0.011(4) -0.033(4) -0.033(5) N7 0.098(8) 0.33(2) 0.144(11) 0.109(13) -0.043(7) -0.075(10) C141 0.045(6) 0.174(14) 0.149(12) 0.060(11) -0.023(7) -0.057(7) C142 0.048(5) 0.146(11) 0.143(11) 0.049(8) 0.013(5) -0.018(6) _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 Ni1 N1 1.836(7) . ? Ni1 O4 1.863(6) . ? Ni1 N2 1.863(7) . ? Ni1 O1 1.865(6) . ? O1 C13 1.354(9) . ? O2 C17 1.349(9) . ? O3 C28 1.417(10) . ? O4 C44 1.313(10) . ? O5 C48 1.402(9) . ? O6 C59 1.372(9) . ? N1 C7 1.301(11) . ? N1 C1 1.494(9) . ? N2 C38 1.263(10) . ? N2 C6 1.499(9) . ? C1 C6 1.487(9) . ? C1 C2 1.507(11) . ? C2 C3 1.462(12) . ? C3 C4 1.522(10) . ? C4 C5 1.523(10) . ? C5 C6 1.560(10) . ? C7 C8 1.445(13) . ? C8 C9 1.390(12) . ? C8 C13 1.433(12) . ? C9 C10 1.336(13) . ? C10 C11 1.398(12) . ? C10 C14 1.542(11) . ? C11 C12 1.349(12) . ? C12 C13 1.360(12) . ? C12 C15 1.516(11) . ? C15 C16 1.481(11) . ? C15 C27 1.537(10) . ? C16 C21 1.359(10) . ? C16 C17 1.412(11) . ? C17 C18 1.397(11) . ? C18 C19 1.397(12) . ? C18 C22 1.502(12) . ? C19 C20 1.316(12) . ? C20 C21 1.430(11) . ? C20 C26 1.525(12) . ? C22 C25 1.546(14) . ? C22 C24 1.568(13) . ? C22 C23 1.580(15) . ? C27 C32 1.391(12) . ? C27 C28 1.419(11) . ? C28 C29 1.339(10) . ? C29 C30 1.403(12) . ? C29 C33 1.538(11) . ? C30 C31 1.434(12) . ? C31 C32 1.331(11) . ? C31 C37 1.469(13) . ? C33 C35 1.500(12) . ? C33 C34 1.541(13) . ? C33 C36 1.544(11) . ? C38 C39 1.478(12) . ? C39 C40 1.408(12) . ? C39 C44 1.421(12) . ? C40 C41 1.292(12) . ? C41 C42 1.390(12) . ? C41 C45 1.526(11) . ? C42 C43 1.391(11) . ? C43 C44 1.424(12) . ? C43 C46 1.561(11) . ? C46 C47 1.538(11) . ? C46 C58 1.570(10) . ? C47 C48 1.365(10) . ? C47 C52 1.367(11) . ? C48 C49 1.413(11) . ? C49 C50 1.413(13) . ? C49 C53 1.516(12) . ? C50 C51 1.356(12) . ? C51 C52 1.371(12) . ? C51 C57 1.506(13) . ? C53 C55 1.479(12) . ? C53 C56 1.530(14) . ? C53 C54 1.559(12) . ? C58 C59 1.373(11) . ? C58 C63 1.436(11) . ? C59 C60 1.393(10) . ? C60 C61 1.359(12) . ? C60 C64 1.544(12) . ? C61 C62 1.372(13) . ? C62 C63 1.416(11) . ? C62 C68 1.515(13) . ? C64 C67 1.539(13) . ? C64 C65 1.542(13) . ? C64 C66 1.610(12) . ? Ni2 O7 1.819(6) . ? Ni2 N4 1.820(8) . ? Ni2 O10 1.822(6) . ? Ni2 N3 1.846(7) . ? O7 C81 1.317(11) . ? O8 C85 1.345(10) . ? O9 C96 1.410(10) . ? O10 C112 1.353(10) . ? O11 C116 1.360(9) . ? O12 C127 1.329(11) . ? N3 C75 1.294(11) . ? N3 C69 1.463(9) . ? N4 C106 1.301(12) . ? N4 C74 1.490(9) . ? C69 C74 1.525(9) . ? C69 C70 1.534(11) . ? C70 C71 1.585(11) . ? C71 C72 1.497(10) . ? C72 C73 1.552(12) . ? C73 C74 1.486(10) . ? C75 C76 1.421(13) . ? C76 C81 1.398(12) . ? C76 C77 1.446(12) . ? C77 C78 1.417(12) . ? C78 C79 1.389(12) . ? C78 C82 1.515(12) . ? C79 C80 1.436(11) . ? C80 C81 1.447(11) . ? C80 C83 1.528(11) . ? C83 C84 1.560(10) . ? C83 C95 1.589(11) . ? C84 C85 1.391(12) . ? C84 C89 1.407(11) . ? C85 C86 1.480(10) . ? C86 C87 1.386(12) . ? C86 C90 1.534(12) . ? C87 C88 1.334(12) . ? C88 C89 1.408(10) . ? C88 C94 1.538(11) . ? C90 C93 1.521(13) . ? C90 C91 1.544(12) . ? C90 C92 1.591(13) . ? C95 C96 1.365(12) . ? C95 C100 1.437(10) . ? C96 C97 1.415(13) . ? C97 C98 1.381(11) . ? C97 C101 1.550(12) . ? C98 C99 1.429(11) . ? C99 C100 1.350(12) . ? C99 C105 1.504(11) . ? C101 C102 1.479(15) . ? C101 C103 1.520(15) . ? C101 C104 1.546(12) . ? C106 C107 1.405(12) . ? C107 C112 1.393(12) . ? C107 C108 1.431(12) . ? C108 C109 1.468(12) . ? C109 C110 1.411(12) . ? C109 C113 1.474(12) . ? C110 C111 1.389(12) . ? C111 C112 1.384(12) . ? C111 C114 1.493(12) . ? C114 C115 1.496(10) . ? C114 C126 1.506(12) . ? C115 C120 1.347(11) . ? C115 C116 1.430(10) . ? C116 C117 1.424(10) . ? C117 C118 1.401(12) . ? C117 C121 1.524(12) . ? C118 C119 1.390(13) . ? C119 C120 1.371(10) . ? C119 C125 1.530(13) . ? C121 C122 1.466(12) . ? C121 C123 1.512(12) . ? C121 C124 1.527(13) . ? C126 C131 1.427(12) . ? C126 C127 1.447(11) . ? C127 C128 1.407(12) . ? C128 C129 1.365(13) . ? C128 C132 1.556(12) . ? C129 C130 1.422(13) . ? C130 C131 1.398(12) . ? C130 C136 1.527(13) . ? C132 C135 1.523(14) . ? C132 C133 1.555(14) . ? C132 C134 1.608(14) . ? N6 C139 1.082(9) . ? C139 C140 1.504(11) . ? N7 C141 1.071(16) . ? C141 C142 1.381(18) . ? N8 C143 1.139(16) . ? C143 C145 1.428(17) . ? N8' C144 1.136(16) . ? C144 C145 1.420(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 O4 176.3(3) . . ? N1 Ni1 N2 86.3(3) . . ? O4 Ni1 N2 95.1(3) . . ? N1 Ni1 O1 94.2(3) . . ? O4 Ni1 O1 84.5(3) . . ? N2 Ni1 O1 177.0(3) . . ? C13 O1 Ni1 129.1(5) . . ? C44 O4 Ni1 126.2(6) . . ? C7 N1 C1 122.9(7) . . ? C7 N1 Ni1 125.2(7) . . ? C1 N1 Ni1 111.9(5) . . ? C38 N2 C6 120.6(7) . . ? C38 N2 Ni1 126.8(6) . . ? C6 N2 Ni1 112.3(5) . . ? C6 C1 N1 105.2(5) . . ? C6 C1 C2 111.0(6) . . ? N1 C1 C2 119.4(6) . . ? C3 C2 C1 111.1(7) . . ? C2 C3 C4 109.5(7) . . ? C3 C4 C5 112.9(6) . . ? C4 C5 C6 106.8(7) . . ? C1 C6 N2 105.6(5) . . ? C1 C6 C5 111.4(6) . . ? N2 C6 C5 116.3(6) . . ? N1 C7 C8 126.9(9) . . ? C9 C8 C13 117.3(8) . . ? C9 C8 C7 120.5(8) . . ? C13 C8 C7 122.2(9) . . ? C10 C9 C8 121.5(9) . . ? C9 C10 C11 119.7(9) . . ? C9 C10 C14 118.8(9) . . ? C11 C10 C14 121.4(9) . . ? C12 C11 C10 120.9(9) . . ? C11 C12 C13 120.1(9) . . ? C11 C12 C15 120.8(8) . . ? C13 C12 C15 118.7(8) . . ? O1 C13 C12 120.6(8) . . ? O1 C13 C8 119.1(8) . . ? C12 C13 C8 120.1(8) . . ? C16 C15 C12 119.2(7) . . ? C16 C15 C27 110.5(6) . . ? C12 C15 C27 110.9(6) . . ? C21 C16 C17 116.5(8) . . ? C21 C16 C15 125.1(8) . . ? C17 C16 C15 118.4(7) . . ? O2 C17 C18 118.1(7) . . ? O2 C17 C16 119.5(7) . . ? C18 C17 C16 122.4(8) . . ? C19 C18 C17 114.4(8) . . ? C19 C18 C22 124.5(8) . . ? C17 C18 C22 121.2(7) . . ? C20 C19 C18 127.9(9) . . ? C19 C20 C21 114.4(8) . . ? C19 C20 C26 122.8(9) . . ? C21 C20 C26 122.8(8) . . ? C16 C21 C20 124.1(8) . . ? C18 C22 C25 113.8(8) . . ? C18 C22 C24 107.4(8) . . ? C25 C22 C24 105.3(9) . . ? C18 C22 C23 110.7(9) . . ? C25 C22 C23 107.4(9) . . ? C24 C22 C23 112.2(8) . . ? C32 C27 C28 115.5(7) . . ? C32 C27 C15 118.5(7) . . ? C28 C27 C15 126.0(8) . . ? C29 C28 O3 117.2(7) . . ? C29 C28 C27 125.6(8) . . ? O3 C28 C27 117.1(7) . . ? C28 C29 C30 116.6(8) . . ? C28 C29 C33 124.6(8) . . ? C30 C29 C33 118.8(7) . . ? C29 C30 C31 119.7(8) . . ? C32 C31 C30 120.3(9) . . ? C32 C31 C37 121.7(9) . . ? C30 C31 C37 118.0(8) . . ? C31 C32 C27 122.1(8) . . ? C35 C33 C29 109.4(7) . . ? C35 C33 C34 111.6(8) . . ? C29 C33 C34 110.5(7) . . ? C35 C33 C36 106.9(8) . . ? C29 C33 C36 110.1(8) . . ? C34 C33 C36 108.4(7) . . ? N2 C38 C39 126.2(8) . . ? C40 C39 C44 120.2(8) . . ? C40 C39 C38 120.6(8) . . ? C44 C39 C38 119.1(8) . . ? C41 C40 C39 123.5(9) . . ? C40 C41 C42 118.5(9) . . ? C40 C41 C45 121.3(9) . . ? C42 C41 C45 119.9(8) . . ? C41 C42 C43 122.0(8) . . ? C42 C43 C44 120.0(8) . . ? C42 C43 C46 122.3(8) . . ? C44 C43 C46 117.7(8) . . ? O4 C44 C39 125.4(8) . . ? O4 C44 C43 119.1(8) . . ? C39 C44 C43 115.5(8) . . ? C47 C46 C43 110.8(6) . . ? C47 C46 C58 110.6(6) . . ? C43 C46 C58 115.9(7) . . ? C48 C47 C52 120.1(7) . . ? C48 C47 C46 120.1(7) . . ? C52 C47 C46 119.7(7) . . ? C47 C48 O5 122.3(7) . . ? C47 C48 C49 120.2(8) . . ? O5 C48 C49 117.4(7) . . ? C48 C49 C50 117.0(7) . . ? C48 C49 C53 122.2(9) . . ? C50 C49 C53 120.8(8) . . ? C51 C50 C49 122.1(8) . . ? C50 C51 C52 118.6(9) . . ? C50 C51 C57 118.6(9) . . ? C52 C51 C57 122.8(9) . . ? C47 C52 C51 121.8(8) . . ? C55 C53 C49 115.5(9) . . ? C55 C53 C56 107.0(8) . . ? C49 C53 C56 112.4(8) . . ? C55 C53 C54 109.5(8) . . ? C49 C53 C54 107.4(7) . . ? C56 C53 C54 104.5(8) . . ? C59 C58 C63 119.7(7) . . ? C59 C58 C46 119.6(7) . . ? C63 C58 C46 120.7(8) . . ? O6 C59 C58 120.5(7) . . ? O6 C59 C60 118.7(8) . . ? C58 C59 C60 120.7(8) . . ? C61 C60 C59 118.8(8) . . ? C61 C60 C64 122.9(8) . . ? C59 C60 C64 118.2(8) . . ? C60 C61 C62 122.9(8) . . ? C61 C62 C63 119.3(9) . . ? C61 C62 C68 122.1(9) . . ? C63 C62 C68 118.6(9) . . ? C62 C63 C58 117.6(8) . . ? C67 C64 C65 113.6(9) . . ? C67 C64 C60 109.5(8) . . ? C65 C64 C60 109.9(8) . . ? C67 C64 C66 105.6(9) . . ? C65 C64 C66 109.2(8) . . ? C60 C64 C66 109.1(8) . . ? O7 Ni2 N4 177.7(3) . . ? O7 Ni2 O10 84.2(3) . . ? N4 Ni2 O10 94.2(3) . . ? O7 Ni2 N3 95.3(3) . . ? N4 Ni2 N3 86.4(3) . . ? O10 Ni2 N3 178.3(3) . . ? C81 O7 Ni2 126.6(5) . . ? C112 O10 Ni2 129.3(6) . . ? C75 N3 C69 118.5(7) . . ? C75 N3 Ni2 127.4(7) . . ? C69 N3 Ni2 114.1(5) . . ? C106 N4 C74 119.7(8) . . ? C106 N4 Ni2 127.8(6) . . ? C74 N4 Ni2 112.2(5) . . ? N3 C69 C74 105.6(5) . . ? N3 C69 C70 117.2(7) . . ? C74 C69 C70 111.6(6) . . ? C69 C70 C71 107.4(7) . . ? C72 C71 C70 112.8(6) . . ? C71 C72 C73 111.3(7) . . ? C74 C73 C72 109.8(7) . . ? C73 C74 N4 117.9(7) . . ? C73 C74 C69 111.1(6) . . ? N4 C74 C69 104.4(6) . . ? N3 C75 C76 123.7(9) . . ? C81 C76 C75 121.9(8) . . ? C81 C76 C77 121.4(9) . . ? C75 C76 C77 116.5(8) . . ? C78 C77 C76 121.2(9) . . ? C79 C78 C77 115.8(9) . . ? C79 C78 C82 121.3(9) . . ? C77 C78 C82 122.8(8) . . ? C78 C79 C80 125.6(9) . . ? C79 C80 C81 117.1(8) . . ? C79 C80 C83 125.3(8) . . ? C81 C80 C83 117.2(8) . . ? O7 C81 C76 124.9(8) . . ? O7 C81 C80 116.4(8) . . ? C76 C81 C80 118.6(9) . . ? C80 C83 C84 106.6(7) . . ? C80 C83 C95 117.1(6) . . ? C84 C83 C95 108.8(7) . . ? C85 C84 C89 121.3(7) . . ? C85 C84 C83 118.7(7) . . ? C89 C84 C83 119.7(7) . . ? O8 C85 C84 123.5(6) . . ? O8 C85 C86 119.4(7) . . ? C84 C85 C86 117.1(8) . . ? C87 C86 C85 116.9(8) . . ? C87 C86 C90 123.7(7) . . ? C85 C86 C90 119.4(8) . . ? C88 C87 C86 126.5(7) . . ? C87 C88 C89 117.0(8) . . ? C87 C88 C94 124.5(8) . . ? C89 C88 C94 118.5(8) . . ? C84 C89 C88 121.1(8) . . ? C93 C90 C86 111.3(7) . . ? C93 C90 C91 106.5(7) . . ? C86 C90 C91 113.2(9) . . ? C93 C90 C92 111.5(9) . . ? C86 C90 C92 108.6(7) . . ? C91 C90 C92 105.7(8) . . ? C96 C95 C100 118.3(8) . . ? C96 C95 C83 116.5(7) . . ? C100 C95 C83 125.3(7) . . ? C95 C96 O9 120.2(8) . . ? C95 C96 C97 123.8(8) . . ? O9 C96 C97 115.9(8) . . ? C98 C97 C96 116.7(8) . . ? C98 C97 C101 122.2(8) . . ? C96 C97 C101 121.0(8) . . ? C97 C98 C99 120.3(8) . . ? C100 C99 C98 121.5(7) . . ? C100 C99 C105 119.1(8) . . ? C98 C99 C105 119.2(8) . . ? C99 C100 C95 119.1(8) . . ? C102 C101 C103 106.7(10) . . ? C102 C101 C104 109.5(9) . . ? C103 C101 C104 109.4(9) . . ? C102 C101 C97 113.9(9) . . ? C103 C101 C97 108.9(8) . . ? C104 C101 C97 108.3(8) . . ? N4 C106 C107 121.9(9) . . ? C112 C107 C106 126.2(9) . . ? C112 C107 C108 119.3(8) . . ? C106 C107 C108 114.1(9) . . ? C107 C108 C109 120.0(8) . . ? C110 C109 C108 114.6(9) . . ? C110 C109 C113 124.4(8) . . ? C108 C109 C113 121.0(8) . . ? C111 C110 C109 126.2(9) . . ? C112 C111 C110 116.7(8) . . ? C112 C111 C114 122.4(8) . . ? C110 C111 C114 121.0(8) . . ? O10 C112 C111 118.6(8) . . ? O10 C112 C107 118.5(8) . . ? C111 C112 C107 122.9(8) . . ? C111 C114 C115 115.3(7) . . ? C111 C114 C126 109.1(7) . . ? C115 C114 C126 112.4(7) . . ? C120 C115 C116 116.1(6) . . ? C120 C115 C114 127.2(7) . . ? C116 C115 C114 116.6(7) . . ? O11 C116 C117 114.3(7) . . ? O11 C116 C115 122.2(7) . . ? C117 C116 C115 123.3(7) . . ? C118 C117 C116 113.9(8) . . ? C118 C117 C121 120.9(7) . . ? C116 C117 C121 125.1(8) . . ? C119 C118 C117 124.3(8) . . ? C120 C119 C118 117.1(8) . . ? C120 C119 C125 123.3(9) . . ? C118 C119 C125 119.5(8) . . ? C115 C120 C119 125.0(8) . . ? C122 C121 C123 105.5(7) . . ? C122 C121 C117 113.9(8) . . ? C123 C121 C117 112.4(8) . . ? C122 C121 C124 108.4(9) . . ? C123 C121 C124 105.8(8) . . ? C117 C121 C124 110.4(7) . . ? C131 C126 C127 117.3(8) . . ? C131 C126 C114 121.2(7) . . ? C127 C126 C114 121.4(8) . . ? O12 C127 C128 119.6(7) . . ? O12 C127 C126 119.5(8) . . ? C128 C127 C126 120.9(9) . . ? C129 C128 C127 118.1(8) . . ? C129 C128 C132 120.4(9) . . ? C127 C128 C132 121.3(9) . . ? C128 C129 C130 124.8(9) . . ? C131 C130 C129 116.3(9) . . ? C131 C130 C136 119.0(8) . . ? C129 C130 C136 124.7(9) . . ? C130 C131 C126 122.5(8) . . ? C135 C132 C133 110.3(9) . . ? C135 C132 C128 112.2(7) . . ? C133 C132 C128 110.5(9) . . ? C135 C132 C134 111.1(10) . . ? C133 C132 C134 107.0(7) . . ? C128 C132 C134 105.6(8) . . ? N6 C139 C140 177.8(8) . . ? N7 C141 C142 172(2) . . ? N8 C143 C145 170(3) . . ? N8' C144 C145 177.4(18) . . ? C144 C145 C143 45.7(12) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O1 0.88(2) 1.86(4) 2.697(7) 159(8) . O5 H5 O4 0.84(2) 2.02(5) 2.784(8) 151(8) . O8 H8 O7 0.84(2) 1.94(2) 2.762(7) 167(6) . O12 H12 O10 0.86(2) 2.04(3) 2.885(9) 168(8) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.392 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.053 #===END data_Pdsalen _database_code_depnum_ccdc_archive 'CCDC 296135' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'PdSalen tripdod' _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C72 H94 N2 O7 Pd' _chemical_formula_weight 1205.89 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.6011(11) _cell_length_b 21.7001(15) _cell_length_c 23.4994(16) _cell_angle_alpha 71.3800(10) _cell_angle_beta 86.2890(10) _cell_angle_gamma 71.1520(10) _cell_volume 7585.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_type 'Corrected by Sadabs' _exptl_absorpt_correction_T_min 0.723424 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Corrected by Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40023 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.1546 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 26424 _reflns_number_gt 13733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart CCD' _computing_cell_refinement 'Smart CCD' _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELX XP' _computing_publication_material 'Microsoft Word' _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. There were two several disordered ether molecules in the asymmetric unit, one per Pd(II) center. They were removed from the data by the Squeeze program in the Platon X-ray package. One cyclohexyl ring disordered in two positions. Phenolic hydrogens were found but refined with the O-H distance fixed at 0.85 angstroms. ; _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^)+(0.0558P)^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 26424 _refine_ls_number_parameters 1428 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 0.800 _refine_ls_restrained_S_all 0.800 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.96483(2) 0.402380(18) 0.557595(15) 0.02810(10) Uani 1 1 d . . . O1 O 0.84962(16) 0.39059(15) 0.55964(13) 0.0331(8) Uani 1 1 d . . . O2 O 0.7511(2) 0.27948(16) 0.47305(15) 0.0434(8) Uani 1 1 d D . . O3 O 0.69248(19) 0.28683(18) 0.67009(14) 0.0479(9) Uani 1 1 d D . . O4 O 1.00057(17) 0.34589(15) 0.50153(13) 0.0329(7) Uani 1 1 d . . . O5 O 0.90601(16) 0.25344(18) 0.53176(14) 0.0375(8) Uani 1 1 d D . . O6 O 1.0198(2) 0.3312(2) 0.31973(16) 0.0610(11) Uani 1 1 d D . . N1 N 0.9373(2) 0.4548(2) 0.61382(17) 0.0405(10) Uani 1 1 d . . . N2 N 1.0720(2) 0.42266(19) 0.55309(16) 0.0323(9) Uani 1 1 d . . . C1 C 1.0142(3) 0.4622(4) 0.6357(3) 0.077(2) Uani 1 1 d . . . H1A H 1.0427 0.4163 0.6635 0.092 Uiso 1 1 calc R . . C2 C 1.0031(3) 0.5076(3) 0.6734(2) 0.0474(14) Uani 1 1 d . . . H2B H 0.9760 0.4900 0.7101 0.057 Uiso 1 1 calc R . . H2C H 0.9661 0.5532 0.6519 0.057 Uiso 1 1 calc R . . C3 C 1.0877(3) 0.5117(4) 0.6891(3) 0.089(2) Uani 1 1 d . . . H3B H 1.0768 0.5501 0.7044 0.107 Uiso 1 1 calc R . . H3C H 1.1160 0.4703 0.7213 0.107 Uiso 1 1 calc R . . C4 C 1.1423(4) 0.5193(5) 0.6427(3) 0.113(3) Uani 1 1 d . . . H4A H 1.1974 0.5124 0.6597 0.136 Uiso 1 1 calc R . . H4B H 1.1216 0.5664 0.6166 0.136 Uiso 1 1 calc R . . C5 C 1.1562(3) 0.4730(3) 0.6037(2) 0.0525(15) Uani 1 1 d . . . H5B H 1.1938 0.4275 0.6248 0.063 Uiso 1 1 calc R . . H5C H 1.1823 0.4915 0.5668 0.063 Uiso 1 1 calc R . . C6 C 1.0701(4) 0.4691(4) 0.5891(3) 0.075(2) Uani 1 1 d . . . H6B H 1.0417 0.5150 0.5615 0.090 Uiso 1 1 calc R . . C7 C 0.8626(3) 0.4786(2) 0.6320(2) 0.0392(12) Uani 1 1 d . . . H7A H 0.8575 0.5043 0.6578 0.047 Uiso 1 1 calc R . . C8 C 0.7859(2) 0.4692(2) 0.6164(2) 0.0319(11) Uani 1 1 d . . . C9 C 0.7109(3) 0.5058(2) 0.6377(2) 0.0403(12) Uani 1 1 d . . . H9A H 0.7143 0.5343 0.6592 0.048 Uiso 1 1 calc R . . C10 C 0.6326(3) 0.5012(3) 0.6280(2) 0.0419(13) Uani 1 1 d . . . C11 C 0.6316(3) 0.4549(2) 0.59754(19) 0.0341(11) Uani 1 1 d . . . H11A H 0.5796 0.4500 0.5913 0.041 Uiso 1 1 calc R . . C12 C 0.7029(3) 0.4170(2) 0.57666(19) 0.0316(11) Uani 1 1 d . . . C13 C 0.7838(3) 0.4252(2) 0.58301(19) 0.0309(11) Uani 1 1 d . . . C14 C 0.5517(3) 0.5425(3) 0.6503(3) 0.0634(17) Uani 1 1 d . . . H14A H 0.5657 0.5691 0.6715 0.095 Uiso 1 1 calc R . . H14B H 0.5248 0.5118 0.6768 0.095 Uiso 1 1 calc R . . H14C H 0.5135 0.5726 0.6167 0.095 Uiso 1 1 calc R . . C15 C 0.6982(3) 0.3658(2) 0.54644(19) 0.0324(11) Uani 1 1 d . . . H15B H 0.7514 0.3273 0.5576 0.039 Uiso 1 1 calc R . . C16 C 0.6252(2) 0.3362(2) 0.5708(2) 0.0284(10) Uani 1 1 d . . . C17 C 0.6268(3) 0.2981(2) 0.6309(2) 0.0343(11) Uani 1 1 d . . . C18 C 0.5628(3) 0.2677(2) 0.6554(2) 0.0384(12) Uani 1 1 d . . . C19 C 0.4969(3) 0.2796(2) 0.6150(2) 0.0404(12) Uani 1 1 d . . . H19B H 0.4543 0.2601 0.6292 0.049 Uiso 1 1 calc R . . C20 C 0.4916(3) 0.3186(2) 0.5557(2) 0.0406(12) Uani 1 1 d . . . C21 C 0.5557(3) 0.3473(2) 0.5336(2) 0.0349(11) Uani 1 1 d . . . H21A H 0.5525 0.3742 0.4936 0.042 Uiso 1 1 calc R . . C22 C 0.5652(3) 0.2263(3) 0.7219(2) 0.0543(15) Uani 1 1 d . . . C23 C 0.5593(4) 0.2719(3) 0.7614(3) 0.080(2) Uani 1 1 d . . . H23A H 0.6074 0.2884 0.7551 0.120 Uiso 1 1 calc R . . H23B H 0.5593 0.2457 0.8029 0.120 Uiso 1 1 calc R . . H23C H 0.5077 0.3102 0.7509 0.120 Uiso 1 1 calc R . . C24 C 0.6462(3) 0.1646(3) 0.7393(3) 0.079(2) Uani 1 1 d . . . H24A H 0.6951 0.1800 0.7311 0.119 Uiso 1 1 calc R . . H24B H 0.6477 0.1347 0.7165 0.119 Uiso 1 1 calc R . . H24C H 0.6469 0.1402 0.7814 0.119 Uiso 1 1 calc R . . C25 C 0.4893(3) 0.1972(3) 0.7363(3) 0.074(2) Uani 1 1 d . . . H25D H 0.4895 0.1707 0.7105 0.110 Uiso 1 1 calc R . . H25E H 0.4367 0.2344 0.7299 0.110 Uiso 1 1 calc R . . H25F H 0.4950 0.1684 0.7775 0.110 Uiso 1 1 calc R . . C26 C 0.4156(3) 0.3329(3) 0.5157(2) 0.0680(18) Uani 1 1 d . . . H26D H 0.3811 0.3054 0.5366 0.102 Uiso 1 1 calc R . . H26E H 0.4350 0.3218 0.4797 0.102 Uiso 1 1 calc R . . H26F H 0.3825 0.3806 0.5054 0.102 Uiso 1 1 calc R . . C27 C 0.6920(2) 0.3936(2) 0.47841(19) 0.0285(10) Uani 1 1 d . . . C28 C 0.7168(3) 0.3489(2) 0.4440(2) 0.0359(12) Uani 1 1 d . . . C29 C 0.7016(2) 0.3724(3) 0.3815(2) 0.0344(11) Uani 1 1 d . . . C30 C 0.6645(2) 0.4421(3) 0.3546(2) 0.0360(12) Uani 1 1 d . . . H30A H 0.6536 0.4587 0.3132 0.043 Uiso 1 1 calc R . . C31 C 0.6425(3) 0.4887(3) 0.3867(2) 0.0384(12) Uani 1 1 d . . . C32 C 0.6566(2) 0.4633(2) 0.4485(2) 0.0331(11) Uani 1 1 d . . . H32A H 0.6420 0.4938 0.4705 0.040 Uiso 1 1 calc R . . C33 C 0.7236(3) 0.3217(3) 0.3451(2) 0.0478(13) Uani 1 1 d . . . C34 C 0.6735(3) 0.2708(3) 0.3660(2) 0.0605(16) Uani 1 1 d . . . H34A H 0.6879 0.2449 0.4077 0.091 Uiso 1 1 calc R . . H34B H 0.6878 0.2401 0.3425 0.091 Uiso 1 1 calc R . . H34C H 0.6136 0.2955 0.3611 0.091 Uiso 1 1 calc R . . C35 C 0.8191(3) 0.2825(3) 0.3514(2) 0.0626(16) Uani 1 1 d . . . H35A H 0.8350 0.2568 0.3928 0.094 Uiso 1 1 calc R . . H35B H 0.8503 0.3145 0.3372 0.094 Uiso 1 1 calc R . . H35C H 0.8320 0.2518 0.3279 0.094 Uiso 1 1 calc R . . C36 C 0.6993(3) 0.3605(3) 0.2772(2) 0.0676(17) Uani 1 1 d . . . H36A H 0.7103 0.3279 0.2557 0.101 Uiso 1 1 calc R . . H36B H 0.7327 0.3906 0.2615 0.101 Uiso 1 1 calc R . . H36C H 0.6399 0.3870 0.2724 0.101 Uiso 1 1 calc R . . C37 C 0.6040(3) 0.5646(3) 0.3532(2) 0.0558(15) Uani 1 1 d . . . H37D H 0.5633 0.5860 0.3778 0.084 Uiso 1 1 calc R . . H37E H 0.5760 0.5705 0.3164 0.084 Uiso 1 1 calc R . . H37F H 0.6483 0.5854 0.3443 0.084 Uiso 1 1 calc R . . C38 C 1.1317(3) 0.4070(2) 0.51834(19) 0.0350(12) Uani 1 1 d . . . H38B H 1.1762 0.4247 0.5170 0.042 Uiso 1 1 calc R . . C39 C 1.1374(3) 0.3652(2) 0.48115(19) 0.0326(11) Uani 1 1 d . . . C40 C 1.2140(3) 0.3504(3) 0.45000(19) 0.0386(12) Uani 1 1 d . . . H40A H 1.2546 0.3701 0.4539 0.046 Uiso 1 1 calc R . . C41 C 1.2313(3) 0.3089(3) 0.4147(2) 0.0426(13) Uani 1 1 d . . . C42 C 1.1715(3) 0.2762(3) 0.4129(2) 0.0422(13) Uani 1 1 d . . . H42A H 1.1835 0.2447 0.3919 0.051 Uiso 1 1 calc R . . C43 C 1.0950(2) 0.2894(2) 0.4416(2) 0.0343(11) Uani 1 1 d . . . C44 C 1.0747(3) 0.3344(2) 0.47647(19) 0.0312(11) Uani 1 1 d . . . C45 C 1.3134(3) 0.2938(3) 0.3822(2) 0.0609(16) Uani 1 1 d . . . H45A H 1.3483 0.3180 0.3902 0.091 Uiso 1 1 calc R . . H45B H 1.3008 0.3083 0.3398 0.091 Uiso 1 1 calc R . . H45C H 1.3433 0.2454 0.3961 0.091 Uiso 1 1 calc R . . C46 C 1.0336(3) 0.2487(2) 0.4435(2) 0.0348(11) Uani 1 1 d . . . H46A H 0.9756 0.2807 0.4408 0.042 Uiso 1 1 calc R . . C47 C 1.0406(3) 0.2188(3) 0.3919(2) 0.0407(13) Uani 1 1 d . . . C48 C 1.0320(3) 0.2618(3) 0.3323(3) 0.0495(14) Uani 1 1 d . . . C49 C 1.0335(3) 0.2388(4) 0.2816(3) 0.0608(17) Uani 1 1 d . . . C50 C 1.0401(3) 0.1684(4) 0.2973(3) 0.070(2) Uani 1 1 d . . . H50B H 1.0404 0.1505 0.2661 0.084 Uiso 1 1 calc R . . C51 C 1.0459(4) 0.1251(3) 0.3546(3) 0.077(2) Uani 1 1 d . . . C52 C 1.0465(3) 0.1505(3) 0.4012(3) 0.0643(17) Uani 1 1 d . . . H52B H 1.0511 0.1211 0.4405 0.077 Uiso 1 1 calc R . . C53 C 1.0283(4) 0.2870(4) 0.2166(3) 0.075(2) Uani 1 1 d . . . C54 C 1.1026(5) 0.3162(5) 0.2065(3) 0.137(4) Uani 1 1 d . . . H54D H 1.0997 0.3453 0.1656 0.205 Uiso 1 1 calc R . . H54E H 1.1556 0.2792 0.2144 0.205 Uiso 1 1 calc R . . H54F H 1.0992 0.3424 0.2332 0.205 Uiso 1 1 calc R . . C55 C 0.9416(4) 0.3449(4) 0.2035(3) 0.091(2) Uani 1 1 d . . . H55D H 0.9393 0.3750 0.1631 0.137 Uiso 1 1 calc R . . H55E H 0.9351 0.3703 0.2311 0.137 Uiso 1 1 calc R . . H55F H 0.8965 0.3252 0.2080 0.137 Uiso 1 1 calc R . . C56 C 1.0341(4) 0.2491(4) 0.1704(3) 0.101(3) Uani 1 1 d . . . H56D H 1.0340 0.2799 0.1306 0.151 Uiso 1 1 calc R . . H56E H 0.9860 0.2329 0.1735 0.151 Uiso 1 1 calc R . . H56F H 1.0857 0.2108 0.1782 0.151 Uiso 1 1 calc R . . C57 C 1.0519(5) 0.0519(3) 0.3654(4) 0.135(4) Uani 1 1 d . . . H57D H 1.0532 0.0436 0.3276 0.202 Uiso 1 1 calc R . . H57E H 1.0034 0.0431 0.3866 0.202 Uiso 1 1 calc R . . H57F H 1.1030 0.0222 0.3889 0.202 Uiso 1 1 calc R . . C58 C 1.0457(3) 0.1946(2) 0.5055(2) 0.0396(12) Uani 1 1 d . . . C59 C 0.9819(3) 0.1973(2) 0.5468(2) 0.0334(11) Uani 1 1 d . . . C60 C 0.9910(3) 0.1474(2) 0.6036(2) 0.0334(11) Uani 1 1 d . . . C61 C 1.0694(3) 0.0956(2) 0.6165(2) 0.0412(12) Uani 1 1 d . . . H61A H 1.0769 0.0605 0.6529 0.049 Uiso 1 1 calc R . . C62 C 1.1368(3) 0.0932(3) 0.5787(2) 0.0447(13) Uani 1 1 d . . . C63 C 1.1236(3) 0.1423(3) 0.5238(2) 0.0414(12) Uani 1 1 d . . . H63A H 1.1681 0.1410 0.4975 0.050 Uiso 1 1 calc R . . C64 C 0.9212(3) 0.1503(2) 0.6487(2) 0.0371(12) Uani 1 1 d . . . C65 C 0.8401(3) 0.1488(3) 0.6222(2) 0.0471(13) Uani 1 1 d . . . H65D H 0.8224 0.1862 0.5855 0.071 Uiso 1 1 calc R . . H65E H 0.7957 0.1531 0.6504 0.071 Uiso 1 1 calc R . . H65F H 0.8513 0.1061 0.6142 0.071 Uiso 1 1 calc R . . C66 C 0.9028(3) 0.2149(2) 0.6669(2) 0.0433(13) Uani 1 1 d . . . H66D H 0.9536 0.2145 0.6844 0.065 Uiso 1 1 calc R . . H66E H 0.8590 0.2160 0.6957 0.065 Uiso 1 1 calc R . . H66F H 0.8840 0.2547 0.6320 0.065 Uiso 1 1 calc R . . C67 C 0.9474(3) 0.0892(3) 0.7061(2) 0.0570(15) Uani 1 1 d . . . H67D H 0.9952 0.0908 0.7257 0.085 Uiso 1 1 calc R . . H67E H 0.9629 0.0473 0.6961 0.085 Uiso 1 1 calc R . . H67F H 0.9006 0.0909 0.7324 0.085 Uiso 1 1 calc R . . C68 C 1.2224(3) 0.0379(3) 0.5975(3) 0.0641(16) Uani 1 1 d . . . H68A H 1.2589 0.0411 0.5641 0.096 Uiso 1 1 calc R . . H68B H 1.2146 -0.0064 0.6104 0.096 Uiso 1 1 calc R . . H68C H 1.2479 0.0439 0.6300 0.096 Uiso 1 1 calc R . . Pd2 Pd 0.58007(2) -0.068989(19) 0.088796(15) 0.02943(10) Uani 1 1 d . A . O1' O 0.55520(17) -0.02667(15) 0.15538(13) 0.0337(8) Uani 1 1 d . . . O2' O 0.4711(2) 0.16841(19) 0.17429(14) 0.0543(10) Uani 1 1 d D . . O3' O 0.70015(17) -0.06888(15) 0.22349(12) 0.0344(7) Uani 1 1 d D . . O4' O 0.69818(17) -0.06345(16) 0.08813(13) 0.0384(8) Uani 1 1 d . . . O5' O 0.9198(2) -0.20765(16) 0.15346(14) 0.0444(8) Uani 1 1 d D . . O6' O 0.8235(2) -0.00299(16) 0.20611(13) 0.0380(8) Uani 1 1 d D . . N1' N 0.4655(2) -0.0743(2) 0.08614(17) 0.0385(10) Uani 1 1 d . . . N2' N 0.5961(2) -0.1062(2) 0.02210(17) 0.0403(10) Uani 1 1 d . . . C1' C 0.4641(4) -0.1265(5) 0.0562(4) 0.027(2) Uiso 0.582(11) 1 d P A 1 H1'A H 0.4952 -0.1732 0.0814 0.032 Uiso 0.582(11) 1 calc PR A 1 C1A' C 0.4519(7) -0.0899(7) 0.0276(6) 0.032(3) Uiso 0.418(11) 1 d P A 2 H1AA H 0.4398 -0.0485 -0.0075 0.038 Uiso 0.418(11) 1 calc PR A 2 C2' C 0.3733(3) -0.1218(3) 0.0384(2) 0.0573(16) Uani 1 1 d . . . C3' C 0.3866(5) -0.1768(6) 0.0081(5) 0.042(3) Uiso 0.582(11) 1 d P A 1 H3'B H 0.3322 -0.1801 -0.0009 0.050 Uiso 0.582(11) 1 calc PR A 1 H3'C H 0.4206 -0.2212 0.0344 0.050 Uiso 0.582(11) 1 calc PR A 1 C3A' C 0.3753(7) -0.1418(7) -0.0223(6) 0.035(3) Uiso 0.418(11) 1 d P A 2 H3AA H 0.3282 -0.1589 -0.0230 0.042 Uiso 0.418(11) 1 calc PR A 2 H3AB H 0.3671 -0.1008 -0.0567 0.042 Uiso 0.418(11) 1 calc PR A 2 C4' C 0.4348(5) -0.1550(6) -0.0528(4) 0.037(3) Uiso 0.582(11) 1 d P A 1 H4'A H 0.4380 -0.1855 -0.0760 0.045 Uiso 0.582(11) 1 calc PR A 1 H4'B H 0.4038 -0.1085 -0.0769 0.045 Uiso 0.582(11) 1 calc PR A 1 C4A' C 0.4558(8) -0.1944(9) -0.0283(7) 0.051(4) Uiso 0.418(11) 1 d P A 2 H4AA H 0.4518 -0.2081 -0.0632 0.061 Uiso 0.418(11) 1 calc PR A 2 H4AB H 0.4680 -0.2347 0.0072 0.061 Uiso 0.418(11) 1 calc PR A 2 C5' C 0.5280(3) -0.1595(3) -0.0356(2) 0.0615(18) Uani 1 1 d . . . C6' C 0.5108(5) -0.1056(5) -0.0006(4) 0.023(2) Uiso 0.582(11) 1 d P A 1 H6'B H 0.4787 -0.0596 -0.0264 0.028 Uiso 0.582(11) 1 calc PR A 1 C6A' C 0.5316(8) -0.1416(9) 0.0220(7) 0.049(4) Uiso 0.418(11) 1 d P A 2 H6AA H 0.5421 -0.1829 0.0571 0.058 Uiso 0.418(11) 1 calc PR A 2 C7' C 0.4016(3) -0.0462(2) 0.1135(2) 0.0392(13) Uani 1 1 d . A . H7'A H 0.3491 -0.0491 0.1054 0.047 Uiso 1 1 calc R . . C8' C 0.4038(3) -0.0110(2) 0.1552(2) 0.0337(11) Uani 1 1 d . . . C9' C 0.3252(3) 0.0148(3) 0.1794(2) 0.0423(13) Uani 1 1 d . A . H9'A H 0.2769 0.0108 0.1649 0.051 Uiso 1 1 calc R . . C10' C 0.3163(3) 0.0452(3) 0.2229(2) 0.0523(15) Uani 1 1 d . . . C11' C 0.3907(3) 0.0505(3) 0.2431(2) 0.0488(14) Uani 1 1 d . A . H11B H 0.3867 0.0708 0.2730 0.059 Uiso 1 1 calc R . . C12' C 0.4696(3) 0.0270(2) 0.2208(2) 0.0344(11) Uani 1 1 d . . . C13' C 0.4779(3) -0.0043(2) 0.17580(19) 0.0322(11) Uani 1 1 d . A . C14' C 0.2313(3) 0.0707(4) 0.2503(3) 0.103(3) Uani 1 1 d . A . H14D H 0.1894 0.0567 0.2358 0.155 Uiso 1 1 calc R . . H14E H 0.2132 0.1199 0.2390 0.155 Uiso 1 1 calc R . . H14F H 0.2375 0.0516 0.2933 0.155 Uiso 1 1 calc R . . C15' C 0.5498(2) 0.0304(2) 0.24765(19) 0.0331(11) Uani 1 1 d . A . H15A H 0.5888 0.0367 0.2148 0.040 Uiso 1 1 calc R . . C16' C 0.5338(3) 0.0909(2) 0.2712(2) 0.0332(11) Uani 1 1 d . . . C17' C 0.4965(3) 0.1583(3) 0.2328(2) 0.0404(12) Uani 1 1 d . A . C18' C 0.4852(3) 0.2165(3) 0.2495(2) 0.0382(12) Uani 1 1 d . . . C19' C 0.5129(3) 0.2043(3) 0.3084(2) 0.0431(13) Uani 1 1 d . A . H19A H 0.5060 0.2418 0.3214 0.052 Uiso 1 1 calc R . . C20' C 0.5497(3) 0.1394(3) 0.3482(2) 0.0396(12) Uani 1 1 d . . . C21' C 0.5608(3) 0.0834(2) 0.3288(2) 0.0350(11) Uani 1 1 d . A . H21B H 0.5870 0.0396 0.3548 0.042 Uiso 1 1 calc R . . C22' C 0.4469(3) 0.2895(3) 0.2063(2) 0.0545(14) Uani 1 1 d . A . C23' C 0.3527(4) 0.3017(3) 0.1884(3) 0.078(2) Uani 1 1 d . . . H23D H 0.3201 0.2957 0.2238 0.116 Uiso 1 1 calc R A . H23E H 0.3513 0.2694 0.1689 0.116 Uiso 1 1 calc R . . H23F H 0.3288 0.3475 0.1615 0.116 Uiso 1 1 calc R . . C24' C 0.4994(4) 0.3024(3) 0.1496(3) 0.087(2) Uani 1 1 d . . . H24D H 0.5571 0.2947 0.1612 0.130 Uiso 1 1 calc R A . H24E H 0.4751 0.3489 0.1242 0.130 Uiso 1 1 calc R . . H24F H 0.4985 0.2716 0.1282 0.130 Uiso 1 1 calc R . . C25' C 0.4447(4) 0.3449(3) 0.2343(3) 0.0659(16) Uani 1 1 d . . . H25A H 0.5014 0.3386 0.2469 0.099 Uiso 1 1 calc R A . H25B H 0.4094 0.3412 0.2684 0.099 Uiso 1 1 calc R . . H25C H 0.4219 0.3894 0.2051 0.099 Uiso 1 1 calc R . . C26' C 0.5787(4) 0.1291(3) 0.4113(2) 0.0627(16) Uani 1 1 d . A . H26A H 0.5611 0.1724 0.4187 0.094 Uiso 1 1 calc R . . H26B H 0.6396 0.1099 0.4155 0.094 Uiso 1 1 calc R . . H26C H 0.5537 0.0983 0.4397 0.094 Uiso 1 1 calc R . . C27' C 0.5927(2) -0.0399(2) 0.29285(19) 0.0309(11) Uani 1 1 d . . . C28' C 0.6649(3) -0.0859(2) 0.27962(18) 0.0286(10) Uani 1 1 d . A . C29' C 0.7060(3) -0.1507(3) 0.3217(2) 0.0365(12) Uani 1 1 d . . . C30' C 0.6697(3) -0.1652(3) 0.3771(2) 0.0459(13) Uani 1 1 d . A . H30B H 0.6965 -0.2065 0.4065 0.055 Uiso 1 1 calc R . . C31' C 0.5949(3) -0.1212(3) 0.3910(2) 0.0443(13) Uani 1 1 d . . . C32' C 0.5569(3) -0.0611(3) 0.3482(2) 0.0429(13) Uani 1 1 d . A . H32B H 0.5048 -0.0328 0.3559 0.051 Uiso 1 1 calc R . . C33' C 0.7851(3) -0.2031(2) 0.3072(2) 0.0423(13) Uani 1 1 d . A . C34' C 0.7606(3) -0.2248(3) 0.2558(3) 0.0593(16) Uani 1 1 d . . . H34D H 0.8095 -0.2577 0.2465 0.089 Uiso 1 1 calc R A . H34E H 0.7411 -0.1852 0.2209 0.089 Uiso 1 1 calc R . . H34F H 0.7160 -0.2448 0.2683 0.089 Uiso 1 1 calc R . . C35' C 0.8577(3) -0.1734(3) 0.2882(2) 0.0474(14) Uani 1 1 d . . . H35D H 0.8720 -0.1590 0.3197 0.071 Uiso 1 1 calc R A . H35E H 0.8405 -0.1348 0.2523 0.071 Uiso 1 1 calc R . . H35F H 0.9066 -0.2078 0.2807 0.071 Uiso 1 1 calc R . . C36' C 0.8172(4) -0.2667(3) 0.3616(3) 0.091(2) Uani 1 1 d . . . H36D H 0.8317 -0.2540 0.3942 0.136 Uiso 1 1 calc R A . H36E H 0.8668 -0.2986 0.3516 0.136 Uiso 1 1 calc R . . H36F H 0.7735 -0.2878 0.3735 0.136 Uiso 1 1 calc R . . C37' C 0.5584(4) -0.1410(3) 0.4530(2) 0.0706(18) Uani 1 1 d . A . H37A H 0.5240 -0.1002 0.4616 0.106 Uiso 1 1 calc R . . H37B H 0.6042 -0.1659 0.4827 0.106 Uiso 1 1 calc R . . H37C H 0.5241 -0.1693 0.4536 0.106 Uiso 1 1 calc R . . C38' C 0.6621(3) -0.1134(3) -0.0096(2) 0.0466(14) Uani 1 1 d . A . H38A H 0.6602 -0.1288 -0.0420 0.056 Uiso 1 1 calc R . . C39' C 0.7389(3) -0.1001(2) -0.0001(2) 0.0367(12) Uani 1 1 d . . . C40' C 0.8032(3) -0.1130(2) -0.0413(2) 0.0394(12) Uani 1 1 d . A . H40B H 0.7917 -0.1264 -0.0729 0.047 Uiso 1 1 calc R . . C41' C 0.8816(3) -0.1066(2) -0.03670(19) 0.0351(11) Uani 1 1 d . . . C42' C 0.8968(3) -0.0889(2) 0.0131(2) 0.0355(11) Uani 1 1 d . A . H42B H 0.9505 -0.0861 0.0183 0.043 Uiso 1 1 calc R . . C43' C 0.8370(3) -0.0753(2) 0.05478(18) 0.0304(11) Uani 1 1 d . . . C44' C 0.7535(3) -0.0792(2) 0.04862(19) 0.0301(11) Uani 1 1 d . A . C45' C 0.9498(3) -0.1225(3) -0.0810(2) 0.0515(14) Uani 1 1 d . A . H45D H 0.9244 -0.1252 -0.1153 0.077 Uiso 1 1 calc R . . H45E H 0.9925 -0.1655 -0.0621 0.077 Uiso 1 1 calc R . . H45F H 0.9755 -0.0868 -0.0937 0.077 Uiso 1 1 calc R . . C46' C 0.8604(2) -0.0599(2) 0.10968(19) 0.0321(11) Uani 1 1 d . A . H46B H 0.8242 -0.0758 0.1418 0.038 Uiso 1 1 calc R . . C47' C 0.8415(2) 0.0158(2) 0.09998(19) 0.0290(10) Uani 1 1 d . . . C48' C 0.8249(2) 0.0410(2) 0.14881(19) 0.0304(11) Uani 1 1 d . A . C49' C 0.8149(2) 0.1099(2) 0.1429(2) 0.0303(11) Uani 1 1 d . . . C50' C 0.8208(2) 0.1521(2) 0.0854(2) 0.0337(11) Uani 1 1 d . A . H50A H 0.8139 0.1979 0.0798 0.040 Uiso 1 1 calc R . . C51' C 0.8365(3) 0.1292(3) 0.0361(2) 0.0376(12) Uani 1 1 d . . . C52' C 0.8458(2) 0.0616(2) 0.04435(19) 0.0316(11) Uani 1 1 d . A . H52A H 0.8554 0.0461 0.0111 0.038 Uiso 1 1 calc R . . C53' C 0.7994(3) 0.1370(3) 0.1970(2) 0.0402(12) Uani 1 1 d . A . C54' C 0.8763(3) 0.0986(3) 0.2424(2) 0.0626(16) Uani 1 1 d . . . H54A H 0.9274 0.1031 0.2226 0.094 Uiso 1 1 calc R A . H54B H 0.8809 0.0509 0.2583 0.094 Uiso 1 1 calc R . . H54C H 0.8683 0.1179 0.2747 0.094 Uiso 1 1 calc R . . C55' C 0.7173(3) 0.1271(3) 0.2271(2) 0.0608(16) Uani 1 1 d . . . H55A H 0.6705 0.1491 0.1979 0.091 Uiso 1 1 calc R A . H55B H 0.7057 0.1471 0.2590 0.091 Uiso 1 1 calc R . . H55C H 0.7244 0.0790 0.2432 0.091 Uiso 1 1 calc R . . C56' C 0.7873(3) 0.2133(3) 0.1786(2) 0.0587(15) Uani 1 1 d . . . H56A H 0.7376 0.2383 0.1522 0.088 Uiso 1 1 calc R A . H56B H 0.8364 0.2220 0.1582 0.088 Uiso 1 1 calc R . . H56C H 0.7803 0.2276 0.2137 0.088 Uiso 1 1 calc R . . C57' C 0.8424(3) 0.1781(3) -0.0250(2) 0.0547(15) Uani 1 1 d . A . H57A H 0.8963 0.1603 -0.0412 0.082 Uiso 1 1 calc R . . H57B H 0.8376 0.2220 -0.0213 0.082 Uiso 1 1 calc R . . H57C H 0.7971 0.1832 -0.0513 0.082 Uiso 1 1 calc R . . C58' C 0.9532(2) -0.1025(2) 0.13217(18) 0.0304(11) Uani 1 1 d . . . C59' C 0.9779(3) -0.1727(2) 0.15233(19) 0.0334(11) Uani 1 1 d . A . C60' C 1.0621(3) -0.2148(2) 0.17272(19) 0.0359(11) Uani 1 1 d . . . C61' C 1.1201(3) -0.1795(3) 0.1700(2) 0.0394(12) Uani 1 1 d . A . H61B H 1.1763 -0.2049 0.1832 0.047 Uiso 1 1 calc R . . C62' C 1.0982(3) -0.1090(3) 0.1486(2) 0.0365(12) Uani 1 1 d . . . C63' C 1.0144(3) -0.0704(2) 0.12978(19) 0.0334(11) Uani 1 1 d . A . H63B H 0.9989 -0.0228 0.1155 0.040 Uiso 1 1 calc R . . C64' C 1.0903(3) -0.2936(3) 0.1924(2) 0.0486(14) Uani 1 1 d . A . C65' C 1.0801(4) -0.3172(3) 0.1381(2) 0.0641(16) Uani 1 1 d . . . H65A H 1.0223 -0.2963 0.1223 0.096 Uiso 1 1 calc R A . H65B H 1.0939 -0.3662 0.1511 0.096 Uiso 1 1 calc R . . H65C H 1.1178 -0.3037 0.1074 0.096 Uiso 1 1 calc R . . C66' C 1.1848(3) -0.3265(3) 0.2137(3) 0.0723(18) Uani 1 1 d . . . H66A H 1.1946 -0.3110 0.2459 0.108 Uiso 1 1 calc R A . H66B H 1.2198 -0.3133 0.1809 0.108 Uiso 1 1 calc R . . H66C H 1.1989 -0.3755 0.2277 0.108 Uiso 1 1 calc R . . C67' C 1.0390(3) -0.3232(3) 0.2447(2) 0.0546(14) Uani 1 1 d . . . H67A H 1.0482 -0.3109 0.2790 0.082 Uiso 1 1 calc R A . H67B H 1.0573 -0.3722 0.2548 0.082 Uiso 1 1 calc R . . H67C H 0.9795 -0.3048 0.2330 0.082 Uiso 1 1 calc R . . C68' C 1.1650(3) -0.0738(3) 0.1448(2) 0.0537(15) Uani 1 1 d . A . H68D H 1.2152 -0.1059 0.1682 0.081 Uiso 1 1 calc R . . H68E H 1.1428 -0.0358 0.1601 0.081 Uiso 1 1 calc R . . H68F H 1.1792 -0.0575 0.1036 0.081 Uiso 1 1 calc R . . H2 H 0.7983 0.2607 0.4908 0.065(18) Uiso 1 1 d RD . . H3 H 0.7248 0.3086 0.6515 0.069(19) Uiso 1 1 d RD . . H5 H 0.9061 0.2934 0.5120 0.20(4) Uiso 1 1 d RD . . H6 H 1.0454 0.3318 0.3495 0.11(3) Uiso 1 1 d RD . . H2' H 0.4608 0.1360 0.1677 0.09(2) Uiso 1 1 d RD . . H3' H 0.6590 -0.0595 0.1995 0.056(16) Uiso 1 1 d RD . . H5' H 0.8711 -0.1801 0.1397 0.047(16) Uiso 1 1 d RD . . H6' H 0.7793 -0.0142 0.2095 0.08(2) Uiso 1 1 d RD . . 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 0.02335(18) 0.0311(2) 0.0358(2) -0.01478(18) 0.00155(15) -0.01247(16) O1 0.0240(16) 0.037(2) 0.049(2) -0.0262(17) 0.0036(14) -0.0119(14) O2 0.0377(19) 0.035(2) 0.058(2) -0.0192(18) -0.0079(17) -0.0068(16) O3 0.0361(18) 0.068(3) 0.042(2) -0.0070(19) -0.0048(16) -0.0286(19) O4 0.0280(16) 0.041(2) 0.0386(19) -0.0212(16) 0.0054(14) -0.0148(14) O5 0.0245(16) 0.036(2) 0.053(2) -0.0186(18) 0.0025(14) -0.0066(14) O6 0.079(3) 0.076(3) 0.046(2) -0.024(2) 0.000(2) -0.044(2) N1 0.031(2) 0.048(3) 0.055(3) -0.032(2) -0.0048(19) -0.0114(19) N2 0.028(2) 0.047(3) 0.034(2) -0.023(2) 0.0084(17) -0.0186(18) C1 0.030(3) 0.133(6) 0.116(5) -0.095(5) 0.012(3) -0.035(3) C2 0.029(3) 0.065(4) 0.066(4) -0.042(3) 0.000(2) -0.017(2) C3 0.029(3) 0.143(7) 0.148(6) -0.114(6) 0.007(4) -0.030(4) C4 0.083(5) 0.222(9) 0.146(7) -0.152(7) 0.061(5) -0.114(6) C5 0.040(3) 0.086(4) 0.062(4) -0.047(3) 0.015(3) -0.039(3) C6 0.065(4) 0.145(6) 0.082(4) -0.088(5) 0.036(3) -0.074(4) C7 0.025(2) 0.050(3) 0.057(3) -0.032(3) 0.007(2) -0.018(2) C8 0.021(2) 0.038(3) 0.042(3) -0.018(2) 0.001(2) -0.012(2) C9 0.033(3) 0.045(3) 0.054(3) -0.027(3) 0.005(2) -0.017(2) C10 0.024(2) 0.057(4) 0.055(3) -0.031(3) 0.009(2) -0.015(2) C11 0.030(2) 0.040(3) 0.041(3) -0.016(2) 0.000(2) -0.020(2) C12 0.025(2) 0.039(3) 0.038(3) -0.017(2) 0.003(2) -0.016(2) C13 0.028(2) 0.031(3) 0.035(3) -0.008(2) 0.001(2) -0.012(2) C14 0.033(3) 0.091(5) 0.095(5) -0.067(4) 0.017(3) -0.023(3) C15 0.028(2) 0.034(3) 0.043(3) -0.014(2) 0.002(2) -0.018(2) C16 0.023(2) 0.030(3) 0.038(3) -0.016(2) 0.002(2) -0.010(2) C17 0.027(2) 0.034(3) 0.043(3) -0.013(2) -0.007(2) -0.009(2) C18 0.030(2) 0.037(3) 0.043(3) -0.005(3) 0.002(2) -0.012(2) C19 0.029(2) 0.035(3) 0.062(4) -0.013(3) 0.002(2) -0.017(2) C20 0.030(3) 0.039(3) 0.055(3) -0.010(3) -0.005(2) -0.016(2) C21 0.032(2) 0.032(3) 0.043(3) -0.010(2) 0.000(2) -0.015(2) C22 0.037(3) 0.063(4) 0.053(4) 0.003(3) 0.000(3) -0.023(3) C23 0.073(4) 0.111(6) 0.051(4) -0.021(4) 0.007(3) -0.028(4) C24 0.048(3) 0.080(5) 0.076(5) 0.024(4) -0.009(3) -0.022(3) C25 0.039(3) 0.088(5) 0.069(4) 0.010(4) 0.007(3) -0.023(3) C26 0.048(3) 0.091(5) 0.073(4) -0.016(4) -0.015(3) -0.038(3) C27 0.020(2) 0.028(3) 0.039(3) -0.009(2) 0.0014(19) -0.010(2) C28 0.023(2) 0.035(3) 0.057(3) -0.022(3) 0.000(2) -0.011(2) C29 0.022(2) 0.049(3) 0.040(3) -0.024(3) 0.004(2) -0.012(2) C30 0.025(2) 0.050(4) 0.036(3) -0.016(3) 0.007(2) -0.015(2) C31 0.025(2) 0.039(3) 0.055(3) -0.019(3) 0.007(2) -0.012(2) C32 0.027(2) 0.040(3) 0.042(3) -0.022(3) 0.009(2) -0.016(2) C33 0.047(3) 0.054(4) 0.050(3) -0.025(3) -0.004(2) -0.015(3) C34 0.058(3) 0.057(4) 0.083(4) -0.043(3) -0.005(3) -0.019(3) C35 0.042(3) 0.080(5) 0.078(4) -0.052(4) 0.007(3) -0.010(3) C36 0.068(4) 0.088(5) 0.059(4) -0.051(4) -0.002(3) -0.013(3) C37 0.058(3) 0.053(4) 0.059(4) -0.024(3) 0.002(3) -0.016(3) C38 0.032(3) 0.047(3) 0.033(3) -0.012(3) 0.001(2) -0.023(2) C39 0.026(2) 0.041(3) 0.033(3) -0.013(2) -0.003(2) -0.011(2) C40 0.029(2) 0.058(4) 0.036(3) -0.018(3) 0.006(2) -0.020(2) C41 0.030(3) 0.061(4) 0.048(3) -0.029(3) 0.012(2) -0.019(2) C42 0.033(3) 0.051(3) 0.050(3) -0.030(3) 0.003(2) -0.010(2) C43 0.022(2) 0.042(3) 0.043(3) -0.017(3) 0.000(2) -0.012(2) C44 0.027(2) 0.035(3) 0.036(3) -0.015(2) -0.002(2) -0.012(2) C45 0.047(3) 0.093(5) 0.062(4) -0.042(4) 0.021(3) -0.034(3) C46 0.025(2) 0.036(3) 0.044(3) -0.017(3) -0.003(2) -0.004(2) C47 0.021(2) 0.051(4) 0.053(3) -0.028(3) -0.001(2) -0.004(2) C48 0.035(3) 0.069(4) 0.068(4) -0.046(4) 0.010(3) -0.025(3) C49 0.030(3) 0.106(6) 0.071(4) -0.065(4) 0.010(3) -0.020(3) C50 0.036(3) 0.098(6) 0.098(5) -0.083(5) -0.006(3) 0.001(3) C51 0.073(4) 0.065(5) 0.100(6) -0.053(4) -0.038(4) 0.002(3) C52 0.063(4) 0.049(4) 0.081(4) -0.035(4) -0.027(3) 0.002(3) C53 0.070(4) 0.140(7) 0.058(4) -0.063(4) 0.015(3) -0.060(4) C54 0.149(7) 0.274(12) 0.078(5) -0.090(7) 0.053(5) -0.162(8) C55 0.115(6) 0.108(6) 0.064(5) -0.039(4) -0.005(4) -0.039(5) C56 0.097(5) 0.168(8) 0.075(5) -0.081(5) 0.014(4) -0.053(5) C57 0.167(8) 0.064(5) 0.173(8) -0.065(6) -0.094(7) 0.009(5) C58 0.031(3) 0.043(3) 0.057(3) -0.031(3) -0.003(2) -0.013(2) C59 0.030(2) 0.030(3) 0.047(3) -0.018(3) -0.006(2) -0.010(2) C60 0.036(3) 0.025(3) 0.042(3) -0.015(2) -0.006(2) -0.007(2) C61 0.045(3) 0.036(3) 0.045(3) -0.013(3) -0.008(2) -0.014(2) C62 0.035(3) 0.040(3) 0.058(4) -0.020(3) -0.009(3) -0.005(2) C63 0.031(3) 0.049(3) 0.053(3) -0.027(3) 0.004(2) -0.014(2) C64 0.034(3) 0.045(3) 0.035(3) -0.015(3) -0.007(2) -0.013(2) C65 0.046(3) 0.047(3) 0.054(3) -0.016(3) -0.002(2) -0.022(3) C66 0.035(3) 0.051(3) 0.053(3) -0.027(3) 0.001(2) -0.015(2) C67 0.056(3) 0.055(4) 0.054(4) -0.016(3) 0.003(3) -0.011(3) C68 0.046(3) 0.055(4) 0.081(4) -0.024(3) -0.015(3) 0.002(3) Pd2 0.02712(19) 0.0376(2) 0.0299(2) -0.01508(19) 0.00267(15) -0.01448(17) O1' 0.0265(16) 0.043(2) 0.0394(19) -0.0232(17) 0.0030(14) -0.0109(14) O2' 0.076(3) 0.049(2) 0.039(2) -0.0188(19) -0.0086(18) -0.014(2) O3' 0.0257(16) 0.047(2) 0.0307(18) -0.0131(16) 0.0011(14) -0.0104(14) O4' 0.0279(17) 0.059(2) 0.043(2) -0.0306(18) 0.0051(15) -0.0187(16) O5' 0.046(2) 0.041(2) 0.050(2) -0.0125(18) 0.0032(17) -0.0218(18) O6' 0.047(2) 0.042(2) 0.0305(19) -0.0115(17) 0.0025(15) -0.0216(17) N1' 0.028(2) 0.050(3) 0.053(3) -0.032(2) 0.0055(19) -0.0181(19) N2' 0.034(2) 0.063(3) 0.044(3) -0.032(2) 0.0133(19) -0.029(2) C2' 0.039(3) 0.089(5) 0.082(4) -0.066(4) 0.017(3) -0.036(3) C5' 0.047(3) 0.118(5) 0.073(4) -0.075(4) 0.023(3) -0.057(3) C7' 0.023(2) 0.055(4) 0.047(3) -0.024(3) -0.001(2) -0.014(2) C8' 0.028(2) 0.038(3) 0.037(3) -0.013(2) -0.001(2) -0.011(2) C9' 0.019(2) 0.057(4) 0.052(3) -0.024(3) -0.004(2) -0.006(2) C10' 0.025(3) 0.073(4) 0.063(4) -0.039(3) 0.004(2) -0.004(3) C11' 0.032(3) 0.055(4) 0.065(4) -0.040(3) -0.004(2) -0.001(2) C12' 0.027(2) 0.045(3) 0.038(3) -0.026(3) 0.003(2) -0.009(2) C13' 0.029(2) 0.033(3) 0.028(3) -0.005(2) 0.006(2) -0.008(2) C14' 0.030(3) 0.187(8) 0.128(6) -0.118(6) 0.013(3) -0.015(4) C15' 0.027(2) 0.045(3) 0.030(3) -0.017(2) 0.001(2) -0.011(2) C16' 0.029(2) 0.038(3) 0.037(3) -0.019(3) 0.004(2) -0.009(2) C17' 0.037(3) 0.055(4) 0.036(3) -0.028(3) 0.008(2) -0.013(3) C18' 0.039(3) 0.041(3) 0.036(3) -0.016(3) 0.006(2) -0.012(2) C19' 0.043(3) 0.056(4) 0.048(3) -0.032(3) 0.013(2) -0.025(3) C20' 0.045(3) 0.047(3) 0.035(3) -0.018(3) 0.004(2) -0.020(3) C21' 0.031(2) 0.040(3) 0.040(3) -0.019(3) 0.006(2) -0.014(2) C22' 0.066(4) 0.051(4) 0.050(3) -0.025(3) 0.006(3) -0.014(3) C23' 0.073(4) 0.063(4) 0.088(5) -0.031(4) -0.034(4) 0.005(3) C24' 0.133(6) 0.048(4) 0.057(4) -0.005(3) 0.021(4) -0.014(4) C25' 0.087(4) 0.048(4) 0.069(4) -0.026(3) 0.013(3) -0.025(3) C26' 0.086(4) 0.072(4) 0.045(3) -0.026(3) 0.001(3) -0.036(3) C27' 0.027(2) 0.046(3) 0.028(3) -0.020(2) 0.004(2) -0.013(2) C28' 0.031(2) 0.043(3) 0.019(2) -0.014(2) 0.0047(19) -0.019(2) C29' 0.036(3) 0.048(3) 0.030(3) -0.010(3) 0.001(2) -0.021(2) C30' 0.055(3) 0.037(3) 0.043(3) -0.006(3) -0.004(3) -0.017(3) C31' 0.047(3) 0.045(4) 0.042(3) -0.014(3) 0.015(2) -0.019(3) C32' 0.032(3) 0.050(4) 0.056(3) -0.030(3) 0.011(2) -0.014(2) C33' 0.038(3) 0.035(3) 0.047(3) -0.004(3) 0.000(2) -0.010(2) C34' 0.033(3) 0.065(4) 0.101(5) -0.052(4) 0.020(3) -0.021(3) C35' 0.026(2) 0.062(4) 0.057(3) -0.028(3) -0.001(2) -0.007(2) C36' 0.088(5) 0.061(5) 0.072(5) 0.003(4) 0.015(4) 0.020(3) C37' 0.083(4) 0.080(5) 0.047(4) -0.018(3) 0.028(3) -0.031(4) C38' 0.042(3) 0.074(4) 0.049(3) -0.044(3) 0.012(2) -0.031(3) C39' 0.042(3) 0.049(3) 0.034(3) -0.024(3) 0.006(2) -0.025(2) C40' 0.043(3) 0.054(3) 0.034(3) -0.025(3) 0.005(2) -0.021(2) C41' 0.033(3) 0.046(3) 0.033(3) -0.017(2) 0.008(2) -0.019(2) C42' 0.034(3) 0.040(3) 0.041(3) -0.017(3) 0.004(2) -0.020(2) C43' 0.028(2) 0.038(3) 0.027(3) -0.013(2) 0.0032(19) -0.012(2) C44' 0.025(2) 0.039(3) 0.033(3) -0.015(2) 0.005(2) -0.014(2) C45' 0.044(3) 0.071(4) 0.053(3) -0.039(3) 0.013(2) -0.020(3) C46' 0.023(2) 0.045(3) 0.034(3) -0.018(2) 0.0054(19) -0.014(2) C47' 0.024(2) 0.035(3) 0.031(3) -0.010(2) 0.0018(19) -0.014(2) C48' 0.027(2) 0.040(3) 0.028(3) -0.009(2) 0.0033(19) -0.016(2) C49' 0.025(2) 0.029(3) 0.040(3) -0.013(2) 0.002(2) -0.009(2) C50' 0.027(2) 0.033(3) 0.045(3) -0.014(3) 0.011(2) -0.014(2) C51' 0.026(2) 0.049(4) 0.036(3) -0.012(3) 0.006(2) -0.012(2) C52' 0.032(2) 0.037(3) 0.030(3) -0.015(2) 0.008(2) -0.014(2) C53' 0.043(3) 0.041(3) 0.043(3) -0.022(3) 0.010(2) -0.014(2) C54' 0.077(4) 0.068(4) 0.058(4) -0.031(3) -0.010(3) -0.028(3) C55' 0.063(4) 0.071(4) 0.064(4) -0.043(3) 0.035(3) -0.028(3) C56' 0.078(4) 0.044(4) 0.067(4) -0.034(3) 0.016(3) -0.023(3) C57' 0.077(4) 0.048(4) 0.040(3) -0.008(3) 0.017(3) -0.030(3) C58' 0.025(2) 0.041(3) 0.028(3) -0.011(2) 0.0024(19) -0.014(2) C59' 0.038(3) 0.031(3) 0.031(3) -0.006(2) 0.004(2) -0.016(2) C60' 0.039(3) 0.033(3) 0.030(3) -0.008(2) 0.006(2) -0.006(2) C61' 0.031(3) 0.045(4) 0.036(3) -0.012(3) 0.004(2) -0.005(2) C62' 0.023(2) 0.048(3) 0.038(3) -0.015(3) 0.001(2) -0.010(2) C63' 0.037(3) 0.033(3) 0.033(3) -0.008(2) 0.000(2) -0.017(2) C64' 0.054(3) 0.044(4) 0.040(3) -0.008(3) 0.006(3) -0.011(3) C65' 0.091(4) 0.042(4) 0.058(4) -0.018(3) 0.012(3) -0.019(3) C66' 0.060(4) 0.049(4) 0.085(5) -0.006(4) -0.006(3) 0.000(3) C67' 0.069(4) 0.035(3) 0.056(4) -0.009(3) 0.003(3) -0.018(3) C68' 0.033(3) 0.074(4) 0.056(4) -0.014(3) 0.003(2) -0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 1.948(4) . ? Pd1 N2 1.955(3) . ? Pd1 O1 2.006(3) . ? Pd1 O4 2.013(3) . ? O1 C13 1.310(5) . ? O2 C28 1.379(5) . ? O2 H2 0.8264 . ? O3 C17 1.382(5) . ? O3 H3 0.8385 . ? O4 C44 1.314(5) . ? O5 C59 1.410(5) . ? O5 H5 0.8439 . ? O6 C48 1.387(6) . ? O6 H6 0.8481 . ? N1 C7 1.283(5) . ? N1 C1 1.480(5) . ? N2 C38 1.273(5) . ? N2 C6 1.501(6) . ? C1 C6 1.392(7) . ? C1 C2 1.486(6) . ? C1 H1A 0.9800 . ? C2 C3 1.511(6) . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.376(8) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.521(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.524(6) . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6B 0.9800 . ? C7 C8 1.439(5) . ? C7 H7A 0.9300 . ? C8 C9 1.401(6) . ? C8 C13 1.426(6) . ? C9 C10 1.374(5) . ? C9 H9A 0.9300 . ? C10 C11 1.411(6) . ? C10 C14 1.522(6) . ? C11 C12 1.369(6) . ? C11 H11A 0.9300 . ? C12 C13 1.433(5) . ? C12 C15 1.520(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C27 1.515(6) . ? C15 C16 1.545(5) . ? C15 H15B 0.9800 . ? C16 C17 1.387(6) . ? C16 C21 1.403(5) . ? C17 C18 1.423(6) . ? C18 C19 1.400(6) . ? C18 C22 1.530(6) . ? C19 C20 1.370(6) . ? C19 H19B 0.9300 . ? C20 C21 1.393(6) . ? C20 C26 1.512(6) . ? C21 H21A 0.9300 . ? C22 C24 1.526(7) . ? C22 C23 1.538(8) . ? C22 C25 1.556(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25D 0.9600 . ? C25 H25E 0.9600 . ? C25 H25F 0.9600 . ? C26 H26D 0.9600 . ? C26 H26E 0.9600 . ? C26 H26F 0.9600 . ? C27 C32 1.388(6) . ? C27 C28 1.401(6) . ? C28 C29 1.401(6) . ? C29 C30 1.380(6) . ? C29 C33 1.542(6) . ? C30 C31 1.390(6) . ? C30 H30A 0.9300 . ? C31 C32 1.385(6) . ? C31 C37 1.517(7) . ? C32 H32A 0.9300 . ? C33 C35 1.529(6) . ? C33 C34 1.532(7) . ? C33 C36 1.558(7) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37D 0.9600 . ? C37 H37E 0.9600 . ? C37 H37F 0.9600 . ? C38 C39 1.428(6) . ? C38 H38B 0.9300 . ? C39 C40 1.422(6) . ? C39 C44 1.433(5) . ? C40 C41 1.362(6) . ? C40 H40A 0.9300 . ? C41 C42 1.405(6) . ? C41 C45 1.512(6) . ? C42 C43 1.387(6) . ? C42 H42A 0.9300 . ? C43 C44 1.414(6) . ? C43 C46 1.541(6) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C58 1.527(6) . ? C46 C47 1.529(6) . ? C46 H46A 0.9800 . ? C47 C52 1.398(7) . ? C47 C48 1.399(7) . ? C48 C49 1.429(7) . ? C49 C50 1.421(8) . ? C49 C53 1.540(8) . ? C50 C51 1.362(8) . ? C50 H50B 0.9300 . ? C51 C52 1.377(7) . ? C51 C57 1.497(8) . ? C52 H52B 0.9300 . ? C53 C54 1.533(7) . ? C53 C56 1.541(7) . ? C53 C55 1.545(9) . ? C54 H54D 0.9600 . ? C54 H54E 0.9600 . ? C54 H54F 0.9600 . ? C55 H55D 0.9600 . ? C55 H55E 0.9600 . ? C55 H55F 0.9600 . ? C56 H56D 0.9600 . ? C56 H56E 0.9600 . ? C56 H56F 0.9600 . ? C57 H57D 0.9600 . ? C57 H57E 0.9600 . ? C57 H57F 0.9600 . ? C58 C59 1.390(6) . ? C58 C63 1.400(6) . ? C59 C60 1.405(6) . ? C60 C61 1.392(6) . ? C60 C64 1.518(6) . ? C61 C62 1.380(6) . ? C61 H61A 0.9300 . ? C62 C63 1.364(6) . ? C62 C68 1.515(6) . ? C63 H63A 0.9300 . ? C64 C67 1.525(6) . ? C64 C66 1.525(6) . ? C64 C65 1.534(5) . ? C65 H65D 0.9600 . ? C65 H65E 0.9600 . ? C65 H65F 0.9600 . ? C66 H66D 0.9600 . ? C66 H66E 0.9600 . ? C66 H66F 0.9600 . ? C67 H67D 0.9600 . ? C67 H67E 0.9600 . ? C67 H67F 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? Pd2 N2' 1.948(4) . ? Pd2 N1' 1.949(3) . ? Pd2 O4' 2.002(3) . ? Pd2 O1' 2.013(3) . ? O1' C13' 1.334(5) . ? O2' C17' 1.393(5) . ? O2' H2' 0.8348 . ? O3' C28' 1.395(5) . ? O3' H3' 0.8435 . ? O4' C44' 1.308(5) . ? O5' C59' 1.403(5) . ? O5' H5' 0.8446 . ? O6' C48' 1.384(5) . ? O6' H6' 0.8361 . ? N1' C7' 1.286(5) . ? N1' C1' 1.519(8) . ? N1' C1A' 1.563(11) . ? N2' C38' 1.278(5) . ? N2' C6A' 1.507(12) . ? N2' C6' 1.541(7) . ? C1' C6' 1.516(13) . ? C1' C2' 1.552(8) . ? C1' H1'A 0.9800 . ? C1A' C6A' 1.46(2) . ? C1A' C2' 1.635(11) . ? C1A' H1AA 0.9800 . ? C2' C3' 1.529(9) . ? C2' C3A' 1.615(12) . ? C3' C4' 1.605(14) . ? C3' H3'B 0.9700 . ? C3' H3'C 0.9700 . ? C3A' C4A' 1.482(19) . ? C3A' H3AA 0.9700 . ? C3A' H3AB 0.9700 . ? C4' C5' 1.588(8) . ? C4' H4'A 0.9700 . ? C4' H4'B 0.9700 . ? C4A' C5' 1.586(13) . ? C4A' H4AA 0.9700 . ? C4A' H4AB 0.9700 . ? C5' C6A' 1.533(13) . ? C5' C6' 1.579(9) . ? C6' H6'B 0.9800 . ? C6A' H6AA 0.9800 . ? C7' C8' 1.431(6) . ? C7' H7'A 0.9300 . ? C8' C9' 1.405(6) . ? C8' C13' 1.415(5) . ? C9' C10' 1.361(6) . ? C9' H9'A 0.9300 . ? C10' C11' 1.404(6) . ? C10' C14' 1.522(7) . ? C11' C12' 1.378(6) . ? C11' H11B 0.9300 . ? C12' C13' 1.407(6) . ? C12' C15' 1.541(5) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.523(6) . ? C15' C27' 1.525(6) . ? C15' H15A 0.9800 . ? C16' C21' 1.395(6) . ? C16' C17' 1.408(6) . ? C17' C18' 1.392(6) . ? C18' C19' 1.403(6) . ? C18' C22' 1.533(7) . ? C19' C20' 1.380(6) . ? C19' H19A 0.9300 . ? C20' C21' 1.385(6) . ? C20' C26' 1.513(6) . ? C21' H21B 0.9300 . ? C22' C25' 1.533(7) . ? C22' C24' 1.543(7) . ? C22' C23' 1.561(7) . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25' H25A 0.9600 . ? C25' H25B 0.9600 . ? C25' H25C 0.9600 . ? C26' H26A 0.9600 . ? C26' H26B 0.9600 . ? C26' H26C 0.9600 . ? C27' C28' 1.381(6) . ? C27' C32' 1.397(6) . ? C28' C29' 1.414(6) . ? C29' C30' 1.383(6) . ? C29' C33' 1.537(6) . ? C30' C31' 1.393(7) . ? C30' H30B 0.9300 . ? C31' C32' 1.350(6) . ? C31' C37' 1.525(6) . ? C32' H32B 0.9300 . ? C33' C36' 1.521(7) . ? C33' C35' 1.521(6) . ? C33' C34' 1.547(6) . ? C34' H34D 0.9600 . ? C34' H34E 0.9600 . ? C34' H34F 0.9600 . ? C35' H35D 0.9600 . ? C35' H35E 0.9600 . ? C35' H35F 0.9600 . ? C36' H36D 0.9600 . ? C36' H36E 0.9600 . ? C36' H36F 0.9600 . ? C37' H37A 0.9600 . ? C37' H37B 0.9600 . ? C37' H37C 0.9600 . ? C38' C39' 1.441(5) . ? C38' H38A 0.9300 . ? C39' C40' 1.414(6) . ? C39' C44' 1.419(6) . ? C40' C41' 1.368(5) . ? C40' H40B 0.9300 . ? C41' C42' 1.402(6) . ? C41' C45' 1.519(6) . ? C42' C43' 1.379(6) . ? C42' H42B 0.9300 . ? C43' C44' 1.435(5) . ? C43' C46' 1.533(5) . ? C45' H45D 0.9600 . ? C45' H45E 0.9600 . ? C45' H45F 0.9600 . ? C46' C47' 1.513(6) . ? C46' C58' 1.542(5) . ? C46' H46B 0.9800 . ? C47' C52' 1.381(6) . ? C47' C48' 1.398(6) . ? C48' C49' 1.411(6) . ? C49' C50' 1.387(6) . ? C49' C53' 1.538(6) . ? C50' C51' 1.377(6) . ? C50' H50A 0.9300 . ? C51' C52' 1.375(6) . ? C51' C57' 1.508(6) . ? C52' H52A 0.9300 . ? C53' C56' 1.518(6) . ? C53' C55' 1.541(6) . ? C53' C54' 1.544(6) . ? C54' H54A 0.9600 . ? C54' H54B 0.9600 . ? C54' H54C 0.9600 . ? C55' H55A 0.9600 . ? C55' H55B 0.9600 . ? C55' H55C 0.9600 . ? C56' H56A 0.9600 . ? C56' H56B 0.9600 . ? C56' H56C 0.9600 . ? C57' H57A 0.9600 . ? C57' H57B 0.9600 . ? C57' H57C 0.9600 . ? C58' C59' 1.369(6) . ? C58' C63' 1.395(5) . ? C59' C60' 1.414(6) . ? C60' C61' 1.399(6) . ? C60' C64' 1.536(7) . ? C61' C62' 1.378(6) . ? C61' H61B 0.9300 . ? C62' C63' 1.387(6) . ? C62' C68' 1.521(6) . ? C63' H63B 0.9300 . ? C64' C67' 1.537(6) . ? C64' C66' 1.540(6) . ? C64' C65' 1.555(7) . ? C65' H65A 0.9600 . ? C65' H65B 0.9600 . ? C65' H65C 0.9600 . ? C66' H66A 0.9600 . ? C66' H66B 0.9600 . ? C66' H66C 0.9600 . ? C67' H67A 0.9600 . ? C67' H67B 0.9600 . ? C67' H67C 0.9600 . ? C68' H68D 0.9600 . ? C68' H68E 0.9600 . ? C68' H68F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 83.38(15) . . ? N1 Pd1 O1 94.03(13) . . ? N2 Pd1 O1 174.92(14) . . ? N1 Pd1 O4 176.54(13) . . ? N2 Pd1 O4 93.84(13) . . ? O1 Pd1 O4 88.90(11) . . ? C13 O1 Pd1 123.4(3) . . ? C28 O2 H2 124.7 . . ? C17 O3 H3 108.4 . . ? C44 O4 Pd1 124.2(3) . . ? C59 O5 H5 121.7 . . ? C48 O6 H6 102.2 . . ? C7 N1 C1 122.9(4) . . ? C7 N1 Pd1 125.2(3) . . ? C1 N1 Pd1 111.8(3) . . ? C38 N2 C6 122.8(4) . . ? C38 N2 Pd1 125.5(3) . . ? C6 N2 Pd1 111.1(3) . . ? C6 C1 N1 108.9(5) . . ? C6 C1 C2 117.1(5) . . ? N1 C1 C2 118.5(4) . . ? C6 C1 H1A 103.4 . . ? N1 C1 H1A 103.4 . . ? C2 C1 H1A 103.4 . . ? C1 C2 C3 111.3(4) . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? C1 C2 H2C 109.4 . . ? C3 C2 H2C 109.4 . . ? H2B C2 H2C 108.0 . . ? C4 C3 C2 115.6(5) . . ? C4 C3 H3B 108.4 . . ? C2 C3 H3B 108.4 . . ? C4 C3 H3C 108.4 . . ? C2 C3 H3C 108.4 . . ? H3B C3 H3C 107.4 . . ? C3 C4 C5 118.3(5) . . ? C3 C4 H4A 107.7 . . ? C5 C4 H4A 107.7 . . ? C3 C4 H4B 107.7 . . ? C5 C4 H4B 107.7 . . ? H4A C4 H4B 107.1 . . ? C4 C5 C6 108.7(4) . . ? C4 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? C4 C5 H5C 110.0 . . ? C6 C5 H5C 110.0 . . ? H5B C5 H5C 108.3 . . ? C1 C6 N2 111.4(4) . . ? C1 C6 C5 117.1(4) . . ? N2 C6 C5 116.1(4) . . ? C1 C6 H6B 103.3 . . ? N2 C6 H6B 103.3 . . ? C5 C6 H6B 103.3 . . ? N1 C7 C8 126.3(4) . . ? N1 C7 H7A 116.9 . . ? C8 C7 H7A 116.9 . . ? C9 C8 C13 120.7(4) . . ? C9 C8 C7 115.2(4) . . ? C13 C8 C7 124.1(4) . . ? C10 C9 C8 122.5(4) . . ? C10 C9 H9A 118.7 . . ? C8 C9 H9A 118.7 . . ? C9 C10 C11 116.5(4) . . ? C9 C10 C14 121.7(4) . . ? C11 C10 C14 121.8(4) . . ? C12 C11 C10 123.6(4) . . ? C12 C11 H11A 118.2 . . ? C10 C11 H11A 118.2 . . ? C11 C12 C13 120.0(4) . . ? C11 C12 C15 121.1(4) . . ? C13 C12 C15 118.9(4) . . ? O1 C13 C8 125.4(4) . . ? O1 C13 C12 118.1(4) . . ? C8 C13 C12 116.5(4) . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C27 C15 C12 114.0(4) . . ? C27 C15 C16 110.9(3) . . ? C12 C15 C16 111.2(3) . . ? C27 C15 H15B 106.8 . . ? C12 C15 H15B 106.8 . . ? C16 C15 H15B 106.8 . . ? C17 C16 C21 118.3(4) . . ? C17 C16 C15 120.1(3) . . ? C21 C16 C15 121.6(4) . . ? O3 C17 C16 121.0(4) . . ? O3 C17 C18 116.5(4) . . ? C16 C17 C18 122.5(4) . . ? C19 C18 C17 115.7(4) . . ? C19 C18 C22 122.5(4) . . ? C17 C18 C22 121.9(4) . . ? C20 C19 C18 123.7(4) . . ? C20 C19 H19B 118.2 . . ? C18 C19 H19B 118.2 . . ? C19 C20 C21 118.8(4) . . ? C19 C20 C26 120.7(4) . . ? C21 C20 C26 120.5(5) . . ? C20 C21 C16 121.0(4) . . ? C20 C21 H21A 119.5 . . ? C16 C21 H21A 119.5 . . ? C24 C22 C18 111.1(4) . . ? C24 C22 C23 109.8(5) . . ? C18 C22 C23 110.4(5) . . ? C24 C22 C25 106.4(5) . . ? C18 C22 C25 111.3(4) . . ? C23 C22 C25 107.8(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25D 109.5 . . ? C22 C25 H25E 109.5 . . ? H25D C25 H25E 109.5 . . ? C22 C25 H25F 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? C20 C26 H26D 109.5 . . ? C20 C26 H26E 109.5 . . ? H26D C26 H26E 109.5 . . ? C20 C26 H26F 109.5 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C32 C27 C28 118.0(4) . . ? C32 C27 C15 121.2(4) . . ? C28 C27 C15 120.6(4) . . ? O2 C28 C29 119.3(4) . . ? O2 C28 C27 118.7(4) . . ? C29 C28 C27 121.7(4) . . ? C30 C29 C28 117.3(4) . . ? C30 C29 C33 121.8(4) . . ? C28 C29 C33 120.8(4) . . ? C29 C30 C31 122.9(4) . . ? C29 C30 H30A 118.6 . . ? C31 C30 H30A 118.6 . . ? C32 C31 C30 118.1(4) . . ? C32 C31 C37 122.5(4) . . ? C30 C31 C37 119.4(5) . . ? C31 C32 C27 121.9(4) . . ? C31 C32 H32A 119.1 . . ? C27 C32 H32A 119.1 . . ? C35 C33 C34 109.6(4) . . ? C35 C33 C29 110.4(4) . . ? C34 C33 C29 110.9(4) . . ? C35 C33 C36 108.1(4) . . ? C34 C33 C36 106.9(4) . . ? C29 C33 C36 110.7(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C31 C37 H37D 109.5 . . ? C31 C37 H37E 109.5 . . ? H37D C37 H37E 109.5 . . ? C31 C37 H37F 109.5 . . ? H37D C37 H37F 109.5 . . ? H37E C37 H37F 109.5 . . ? N2 C38 C39 126.6(4) . . ? N2 C38 H38B 116.7 . . ? C39 C38 H38B 116.7 . . ? C40 C39 C38 116.1(4) . . ? C40 C39 C44 119.0(4) . . ? C38 C39 C44 124.8(4) . . ? C41 C40 C39 123.7(4) . . ? C41 C40 H40A 118.2 . . ? C39 C40 H40A 118.2 . . ? C40 C41 C42 116.8(4) . . ? C40 C41 C45 122.7(4) . . ? C42 C41 C45 120.3(4) . . ? C43 C42 C41 122.0(4) . . ? C43 C42 H42A 119.0 . . ? C41 C42 H42A 119.0 . . ? C42 C43 C44 121.7(4) . . ? C42 C43 C46 121.2(4) . . ? C44 C43 C46 116.7(4) . . ? O4 C44 C43 118.9(4) . . ? O4 C44 C39 124.5(4) . . ? C43 C44 C39 116.6(4) . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C58 C46 C47 113.2(4) . . ? C58 C46 C43 107.4(3) . . ? C47 C46 C43 114.8(4) . . ? C58 C46 H46A 107.0 . . ? C47 C46 H46A 107.0 . . ? C43 C46 H46A 107.0 . . ? C52 C47 C48 117.0(5) . . ? C52 C47 C46 122.6(5) . . ? C48 C47 C46 120.1(5) . . ? O6 C48 C47 120.2(4) . . ? O6 C48 C49 116.1(6) . . ? C47 C48 C49 123.7(6) . . ? C50 C49 C48 113.5(6) . . ? C50 C49 C53 124.4(5) . . ? C48 C49 C53 122.0(6) . . ? C51 C50 C49 124.8(5) . . ? C51 C50 H50B 117.6 . . ? C49 C50 H50B 117.6 . . ? C50 C51 C52 118.4(6) . . ? C50 C51 C57 119.8(6) . . ? C52 C51 C57 121.9(7) . . ? C51 C52 C47 122.6(6) . . ? C51 C52 H52B 118.7 . . ? C47 C52 H52B 118.7 . . ? C54 C53 C49 110.1(5) . . ? C54 C53 C56 107.2(5) . . ? C49 C53 C56 111.7(6) . . ? C54 C53 C55 111.3(7) . . ? C49 C53 C55 110.1(5) . . ? C56 C53 C55 106.3(5) . . ? C53 C54 H54D 109.5 . . ? C53 C54 H54E 109.5 . . ? H54D C54 H54E 109.5 . . ? C53 C54 H54F 109.5 . . ? H54D C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? C53 C55 H55D 109.5 . . ? C53 C55 H55E 109.5 . . ? H55D C55 H55E 109.5 . . ? C53 C55 H55F 109.5 . . ? H55D C55 H55F 109.5 . . ? H55E C55 H55F 109.5 . . ? C53 C56 H56D 109.5 . . ? C53 C56 H56E 109.5 . . ? H56D C56 H56E 109.5 . . ? C53 C56 H56F 109.5 . . ? H56D C56 H56F 109.5 . . ? H56E C56 H56F 109.5 . . ? C51 C57 H57D 109.5 . . ? C51 C57 H57E 109.5 . . ? H57D C57 H57E 109.5 . . ? C51 C57 H57F 109.5 . . ? H57D C57 H57F 109.5 . . ? H57E C57 H57F 109.5 . . ? C59 C58 C63 117.5(5) . . ? C59 C58 C46 121.7(4) . . ? C63 C58 C46 120.7(4) . . ? C58 C59 C60 122.7(4) . . ? C58 C59 O5 118.6(4) . . ? C60 C59 O5 118.7(4) . . ? C61 C60 C59 115.4(4) . . ? C61 C60 C64 121.9(4) . . ? C59 C60 C64 122.7(4) . . ? C62 C61 C60 124.2(5) . . ? C62 C61 H61A 117.9 . . ? C60 C61 H61A 117.9 . . ? C63 C62 C61 117.6(4) . . ? C63 C62 C68 121.0(5) . . ? C61 C62 C68 121.3(5) . . ? C62 C63 C58 122.4(4) . . ? C62 C63 H63A 118.8 . . ? C58 C63 H63A 118.8 . . ? C60 C64 C67 111.7(4) . . ? C60 C64 C66 110.1(4) . . ? C67 C64 C66 107.0(4) . . ? C60 C64 C65 110.4(4) . . ? C67 C64 C65 107.2(4) . . ? C66 C64 C65 110.3(4) . . ? C64 C65 H65D 109.5 . . ? C64 C65 H65E 109.5 . . ? H65D C65 H65E 109.5 . . ? C64 C65 H65F 109.5 . . ? H65D C65 H65F 109.5 . . ? H65E C65 H65F 109.5 . . ? C64 C66 H66D 109.5 . . ? C64 C66 H66E 109.5 . . ? H66D C66 H66E 109.5 . . ? C64 C66 H66F 109.5 . . ? H66D C66 H66F 109.5 . . ? H66E C66 H66F 109.5 . . ? C64 C67 H67D 109.5 . . ? C64 C67 H67E 109.5 . . ? H67D C67 H67E 109.5 . . ? C64 C67 H67F 109.5 . . ? H67D C67 H67F 109.5 . . ? H67E C67 H67F 109.5 . . ? C62 C68 H68A 109.5 . . ? C62 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C62 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N2' Pd2 N1' 83.40(15) . . ? N2' Pd2 O4' 94.51(13) . . ? N1' Pd2 O4' 177.73(14) . . ? N2' Pd2 O1' 176.03(14) . . ? N1' Pd2 O1' 93.44(13) . . ? O4' Pd2 O1' 88.62(11) . . ? C13' O1' Pd2 124.5(3) . . ? C17' O2' H2' 117.1 . . ? C28' O3' H3' 102.8 . . ? C44' O4' Pd2 123.4(2) . . ? C59' O5' H5' 111.4 . . ? C48' O6' H6' 109.8 . . ? C7' N1' C1' 122.8(4) . . ? C7' N1' C1A' 120.9(5) . . ? C1' N1' C1A' 31.4(4) . . ? C7' N1' Pd2 125.6(3) . . ? C1' N1' Pd2 110.8(3) . . ? C1A' N1' Pd2 109.1(4) . . ? C38' N2' C6A' 122.5(6) . . ? C38' N2' C6' 121.4(4) . . ? C6A' N2' C6' 29.3(5) . . ? C38' N2' Pd2 125.1(3) . . ? C6A' N2' Pd2 110.8(5) . . ? C6' N2' Pd2 111.2(3) . . ? C6' C1' N1' 101.7(6) . . ? C6' C1' C2' 108.7(6) . . ? N1' C1' C2' 114.1(5) . . ? C6' C1' H1'A 110.7 . . ? N1' C1' H1'A 110.7 . . ? C2' C1' H1'A 110.7 . . ? C6A' C1A' N1' 105.0(9) . . ? C6A' C1A' C2' 110.5(11) . . ? N1' C1A' C2' 107.3(7) . . ? C6A' C1A' H1AA 111.3 . . ? N1' C1A' H1AA 111.3 . . ? C2' C1A' H1AA 111.3 . . ? C3' C2' C1' 105.4(5) . . ? C3' C2' C3A' 30.8(4) . . ? C1' C2' C3A' 110.2(5) . . ? C3' C2' C1A' 112.0(6) . . ? C1' C2' C1A' 30.2(4) . . ? C3A' C2' C1A' 100.3(7) . . ? C2' C3' C4' 107.4(8) . . ? C2' C3' H3'B 110.2 . . ? C4' C3' H3'B 110.2 . . ? C2' C3' H3'C 110.2 . . ? C4' C3' H3'C 110.2 . . ? H3'B C3' H3'C 108.5 . . ? C4A' C3A' C2' 113.6(10) . . ? C4A' C3A' H3AA 108.9 . . ? C2' C3A' H3AA 108.9 . . ? C4A' C3A' H3AB 108.9 . . ? C2' C3A' H3AB 108.9 . . ? H3AA C3A' H3AB 107.7 . . ? C5' C4' C3' 108.5(7) . . ? C5' C4' H4'A 110.0 . . ? C3' C4' H4'A 110.0 . . ? C5' C4' H4'B 110.0 . . ? C3' C4' H4'B 110.0 . . ? H4'A C4' H4'B 108.4 . . ? C3A' C4A' C5' 106.0(11) . . ? C3A' C4A' H4AA 110.5 . . ? C5' C4A' H4AA 110.5 . . ? C3A' C4A' H4AB 110.5 . . ? C5' C4A' H4AB 110.5 . . ? H4AA C4A' H4AB 108.7 . . ? C6A' C5' C6' 28.7(5) . . ? C6A' C5' C4A' 106.9(8) . . ? C6' C5' C4A' 113.2(6) . . ? C6A' C5' C4' 112.7(6) . . ? C6' C5' C4' 103.1(5) . . ? C4A' C5' C4' 30.6(5) . . ? C1' C6' N2' 104.2(6) . . ? C1' C6' C5' 110.8(7) . . ? N2' C6' C5' 109.6(5) . . ? C1' C6' H6'B 110.7 . . ? N2' C6' H6'B 110.7 . . ? C5' C6' H6'B 110.7 . . ? C1A' C6A' N2' 101.9(11) . . ? C1A' C6A' C5' 110.3(11) . . ? N2' C6A' C5' 114.0(9) . . ? C1A' C6A' H6AA 110.1 . . ? N2' C6A' H6AA 110.1 . . ? C5' C6A' H6AA 110.1 . . ? N1' C7' C8' 126.2(4) . . ? N1' C7' H7'A 116.9 . . ? C8' C7' H7'A 116.9 . . ? C9' C8' C13' 119.3(4) . . ? C9' C8' C7' 115.0(4) . . ? C13' C8' C7' 125.5(4) . . ? C10' C9' C8' 123.2(4) . . ? C10' C9' H9'A 118.4 . . ? C8' C9' H9'A 118.4 . . ? C9' C10' C11' 116.5(4) . . ? C9' C10' C14' 122.8(4) . . ? C11' C10' C14' 120.7(5) . . ? C12' C11' C10' 123.1(4) . . ? C12' C11' H11B 118.4 . . ? C10' C11' H11B 118.4 . . ? C11' C12' C13' 119.8(4) . . ? C11' C12' C15' 120.5(4) . . ? C13' C12' C15' 119.6(4) . . ? O1' C13' C12' 118.2(4) . . ? O1' C13' C8' 123.7(4) . . ? C12' C13' C8' 118.1(4) . . ? C10' C14' H14D 109.5 . . ? C10' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C10' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C16' C15' C27' 115.2(3) . . ? C16' C15' C12' 114.3(3) . . ? C27' C15' C12' 107.4(3) . . ? C16' C15' H15A 106.4 . . ? C27' C15' H15A 106.4 . . ? C12' C15' H15A 106.4 . . ? C21' C16' C17' 117.1(4) . . ? C21' C16' C15' 122.8(4) . . ? C17' C16' C15' 119.9(4) . . ? C18' C17' O2' 117.3(4) . . ? C18' C17' C16' 123.5(4) . . ? O2' C17' C16' 119.2(4) . . ? C17' C18' C19' 115.6(4) . . ? C17' C18' C22' 122.7(4) . . ? C19' C18' C22' 121.7(4) . . ? C20' C19' C18' 123.5(5) . . ? C20' C19' H19A 118.3 . . ? C18' C19' H19A 118.3 . . ? C19' C20' C21' 118.4(4) . . ? C19' C20' C26' 121.4(5) . . ? C21' C20' C26' 120.3(5) . . ? C20' C21' C16' 121.9(4) . . ? C20' C21' H21B 119.0 . . ? C16' C21' H21B 119.0 . . ? C18' C22' C25' 112.8(4) . . ? C18' C22' C24' 111.4(4) . . ? C25' C22' C24' 105.9(5) . . ? C18' C22' C23' 109.7(4) . . ? C25' C22' C23' 106.6(4) . . ? C24' C22' C23' 110.3(5) . . ? C22' C23' H23D 109.5 . . ? C22' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C22' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C22' C24' H24D 109.5 . . ? C22' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C22' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C22' C25' H25A 109.5 . . ? C22' C25' H25B 109.5 . . ? H25A C25' H25B 109.5 . . ? C22' C25' H25C 109.5 . . ? H25A C25' H25C 109.5 . . ? H25B C25' H25C 109.5 . . ? C20' C26' H26A 109.5 . . ? C20' C26' H26B 109.5 . . ? H26A C26' H26B 109.5 . . ? C20' C26' H26C 109.5 . . ? H26A C26' H26C 109.5 . . ? H26B C26' H26C 109.5 . . ? C28' C27' C32' 117.8(4) . . ? C28' C27' C15' 121.7(4) . . ? C32' C27' C15' 120.4(4) . . ? C27' C28' O3' 120.1(4) . . ? C27' C28' C29' 122.0(4) . . ? O3' C28' C29' 117.9(4) . . ? C30' C29' C28' 116.1(4) . . ? C30' C29' C33' 121.3(4) . . ? C28' C29' C33' 122.6(4) . . ? C29' C30' C31' 123.3(5) . . ? C29' C30' H30B 118.4 . . ? C31' C30' H30B 118.4 . . ? C32' C31' C30' 117.9(5) . . ? C32' C31' C37' 121.8(5) . . ? C30' C31' C37' 120.3(5) . . ? C31' C32' C27' 122.5(5) . . ? C31' C32' H32B 118.7 . . ? C27' C32' H32B 118.7 . . ? C36' C33' C35' 107.6(4) . . ? C36' C33' C29' 110.9(4) . . ? C35' C33' C29' 111.6(4) . . ? C36' C33' C34' 108.5(5) . . ? C35' C33' C34' 109.5(4) . . ? C29' C33' C34' 108.6(4) . . ? C33' C34' H34D 109.5 . . ? C33' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C33' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C33' C35' H35D 109.5 . . ? C33' C35' H35E 109.5 . . ? H35D C35' H35E 109.5 . . ? C33' C35' H35F 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C33' C36' H36D 109.5 . . ? C33' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C33' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C31' C37' H37A 109.5 . . ? C31' C37' H37B 109.5 . . ? H37A C37' H37B 109.5 . . ? C31' C37' H37C 109.5 . . ? H37A C37' H37C 109.5 . . ? H37B C37' H37C 109.5 . . ? N2' C38' C39' 126.6(4) . . ? N2' C38' H38A 116.7 . . ? C39' C38' H38A 116.7 . . ? C40' C39' C44' 120.5(4) . . ? C40' C39' C38' 115.5(4) . . ? C44' C39' C38' 123.9(4) . . ? C41' C40' C39' 122.9(4) . . ? C41' C40' H40B 118.5 . . ? C39' C40' H40B 118.5 . . ? C40' C41' C42' 116.2(4) . . ? C40' C41' C45' 121.3(4) . . ? C42' C41' C45' 122.4(4) . . ? C43' C42' C41' 124.0(4) . . ? C43' C42' H42B 118.0 . . ? C41' C42' H42B 118.0 . . ? C42' C43' C44' 119.9(4) . . ? C42' C43' C46' 120.5(4) . . ? C44' C43' C46' 119.5(4) . . ? O4' C44' C39' 126.1(4) . . ? O4' C44' C43' 117.5(4) . . ? C39' C44' C43' 116.4(4) . . ? C41' C45' H45D 109.5 . . ? C41' C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? C41' C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? C47' C46' C43' 113.5(4) . . ? C47' C46' C58' 112.7(3) . . ? C43' C46' C58' 110.8(4) . . ? C47' C46' H46B 106.4 . . ? C43' C46' H46B 106.4 . . ? C58' C46' H46B 106.4 . . ? C52' C47' C48' 117.4(4) . . ? C52' C47' C46' 122.2(4) . . ? C48' C47' C46' 120.2(4) . . ? O6' C48' C47' 120.1(4) . . ? O6' C48' C49' 117.5(4) . . ? C47' C48' C49' 122.3(4) . . ? C50' C49' C48' 116.3(4) . . ? C50' C49' C53' 121.5(4) . . ? C48' C49' C53' 122.2(4) . . ? C51' C50' C49' 123.1(4) . . ? C51' C50' H50A 118.5 . . ? C49' C50' H50A 118.5 . . ? C52' C51' C50' 118.4(4) . . ? C52' C51' C57' 121.6(4) . . ? C50' C51' C57' 120.0(5) . . ? C51' C52' C47' 122.6(4) . . ? C51' C52' H52A 118.7 . . ? C47' C52' H52A 118.7 . . ? C56' C53' C49' 112.1(4) . . ? C56' C53' C55' 106.6(4) . . ? C49' C53' C55' 109.8(4) . . ? C56' C53' C54' 108.2(4) . . ? C49' C53' C54' 109.7(4) . . ? C55' C53' C54' 110.3(4) . . ? C53' C54' H54A 109.5 . . ? C53' C54' H54B 109.5 . . ? H54A C54' H54B 109.5 . . ? C53' C54' H54C 109.5 . . ? H54A C54' H54C 109.5 . . ? H54B C54' H54C 109.5 . . ? C53' C55' H55A 109.5 . . ? C53' C55' H55B 109.5 . . ? H55A C55' H55B 109.5 . . ? C53' C55' H55C 109.5 . . ? H55A C55' H55C 109.5 . . ? H55B C55' H55C 109.5 . . ? C53' C56' H56A 109.5 . . ? C53' C56' H56B 109.5 . . ? H56A C56' H56B 109.5 . . ? C53' C56' H56C 109.5 . . ? H56A C56' H56C 109.5 . . ? H56B C56' H56C 109.5 . . ? C51' C57' H57A 109.5 . . ? C51' C57' H57B 109.5 . . ? H57A C57' H57B 109.5 . . ? C51' C57' H57C 109.5 . . ? H57A C57' H57C 109.5 . . ? H57B C57' H57C 109.5 . . ? C59' C58' C63' 118.6(4) . . ? C59' C58' C46' 120.6(4) . . ? C63' C58' C46' 120.8(4) . . ? C58' C59' O5' 121.0(4) . . ? C58' C59' C60' 123.6(4) . . ? O5' C59' C60' 115.4(4) . . ? C61' C60' C59' 115.0(4) . . ? C61' C60' C64' 121.7(4) . . ? C59' C60' C64' 123.2(4) . . ? C62' C61' C60' 123.2(4) . . ? C62' C61' H61B 118.4 . . ? C60' C61' H61B 118.4 . . ? C61' C62' C63' 119.1(4) . . ? C61' C62' C68' 120.7(4) . . ? C63' C62' C68' 120.2(4) . . ? C62' C63' C58' 120.5(4) . . ? C62' C63' H63B 119.7 . . ? C58' C63' H63B 119.7 . . ? C60' C64' C67' 112.0(4) . . ? C60' C64' C66' 112.2(4) . . ? C67' C64' C66' 106.6(4) . . ? C60' C64' C65' 109.6(4) . . ? C67' C64' C65' 109.6(4) . . ? C66' C64' C65' 106.7(5) . . ? C64' C65' H65A 109.5 . . ? C64' C65' H65B 109.5 . . ? H65A C65' H65B 109.5 . . ? C64' C65' H65C 109.5 . . ? H65A C65' H65C 109.5 . . ? H65B C65' H65C 109.5 . . ? C64' C66' H66A 109.5 . . ? C64' C66' H66B 109.5 . . ? H66A C66' H66B 109.5 . . ? C64' C66' H66C 109.5 . . ? H66A C66' H66C 109.5 . . ? H66B C66' H66C 109.5 . . ? C64' C67' H67A 109.5 . . ? C64' C67' H67B 109.5 . . ? H67A C67' H67B 109.5 . . ? C64' C67' H67C 109.5 . . ? H67A C67' H67C 109.5 . . ? H67B C67' H67C 109.5 . . ? C62' C68' H68D 109.5 . . ? C62' C68' H68E 109.5 . . ? H68D C68' H68E 109.5 . . ? C62' C68' H68F 109.5 . . ? H68D C68' H68F 109.5 . . ? H68E C68' H68F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O5 0.83 2.02 2.804(4) 157.5 . O5 H5 O4 0.84 2.18 2.824(4) 133.3 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.546 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.072 #===END data_NisalenF _database_code_depnum_ccdc_archive 'CCDC 296136' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common NiSalenFluorideComplex _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C88 H130 F N3 Ni O7' _chemical_formula_weight 1419.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7248(9) _cell_length_b 17.0299(11) _cell_length_c 22.1543(14) _cell_angle_alpha 71.4080(10) _cell_angle_beta 89.0850(10) _cell_angle_gamma 72.8510(10) _cell_volume 4672.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description ? _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type 'Corrected by Sadabs' _exptl_absorpt_correction_T_min 0.831478 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Corrected by Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29793 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19891 _reflns_number_gt 12735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart CCD' _computing_cell_refinement 'Smart CCD' _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELX XP' _computing_publication_material 'Microsoft Word' _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. There was a several disordered ether molecule in the asymmetric unit. It was removed from the data by the Squeeze program in the Platon X-ray package. One n-butyl arm badly disordered. ; _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^)+(0.1121P)^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 19891 _refine_ls_number_parameters 913 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1731 _refine_ls_wR_factor_gt 0.1610 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.006 _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 Ni1 Ni 0.35503(2) 0.472648(17) 0.464260(12) 0.03297(10) Uani 1 1 d . . . F1 F 0.34000(12) 0.44736(8) 0.24188(6) 0.0530(4) Uani 1 1 d . . . O1 O 0.42083(11) 0.39206(9) 0.42571(7) 0.0359(3) Uani 1 1 d . . . O2 O 0.53060(15) 0.37754(10) 0.24027(8) 0.0488(4) Uani 1 1 d D . . O3 O 0.24912(14) 0.34640(12) 0.30896(8) 0.0551(5) Uani 1 1 d D . . O4 O 0.28288(11) 0.53991(9) 0.38508(7) 0.0370(3) Uani 1 1 d . . . O5 O 0.10452(19) 0.52523(15) 0.23577(11) 0.0786(6) Uani 1 1 d D . . O6 O 0.36493(15) 0.58814(11) 0.16522(8) 0.0488(4) Uani 1 1 d D . . N1 N 0.44561(14) 0.42138(11) 0.53748(8) 0.0371(4) Uani 1 1 d . . . N2 N 0.27566(14) 0.53962(12) 0.50876(8) 0.0382(4) Uani 1 1 d . . . C1 C 0.42205(19) 0.47108(15) 0.58313(10) 0.0429(5) Uani 1 1 d . . . H1A H 0.4462 0.5220 0.5662 0.052 Uiso 1 1 calc R . . C2 C 0.4682(2) 0.42479(16) 0.65162(10) 0.0476(6) Uani 1 1 d . . . H2B H 0.5423 0.4068 0.6529 0.057 Uiso 1 1 calc R . . H2C H 0.4468 0.3734 0.6702 0.057 Uiso 1 1 calc R . . C3 C 0.4317(2) 0.48757(18) 0.68916(12) 0.0573(7) Uani 1 1 d . . . H3B H 0.4579 0.4579 0.7336 0.069 Uiso 1 1 calc R . . H3C H 0.4592 0.5359 0.6726 0.069 Uiso 1 1 calc R . . C4 C 0.3167(2) 0.5222(2) 0.68530(12) 0.0616(7) Uani 1 1 d . . . H4A H 0.2975 0.5640 0.7080 0.074 Uiso 1 1 calc R . . H4B H 0.2896 0.4747 0.7062 0.074 Uiso 1 1 calc R . . C5 C 0.2693(2) 0.56589(17) 0.61647(11) 0.0478(6) Uani 1 1 d . . . H5A H 0.1953 0.5823 0.6159 0.057 Uiso 1 1 calc R . . H5B H 0.2886 0.6183 0.5970 0.057 Uiso 1 1 calc R . . C6 C 0.30597(19) 0.50417(16) 0.57882(11) 0.0458(6) Uani 1 1 d . . . H6A H 0.2808 0.4541 0.5972 0.055 Uiso 1 1 calc R . . C7 C 0.53036(18) 0.35916(14) 0.54654(10) 0.0400(5) Uani 1 1 d . . . H7A H 0.5717 0.3443 0.5838 0.048 Uiso 1 1 calc R . . C8 C 0.56577(17) 0.31118(14) 0.50386(10) 0.0364(5) Uani 1 1 d . . . C9 C 0.66221(18) 0.24621(15) 0.51919(11) 0.0431(5) Uani 1 1 d . . . H9A H 0.7002 0.2361 0.5568 0.052 Uiso 1 1 calc R . . C10 C 0.70120(18) 0.19816(16) 0.48089(12) 0.0477(6) Uani 1 1 d . . . C11 C 0.63881(18) 0.21085(14) 0.42667(11) 0.0439(6) Uani 1 1 d . . . H11A H 0.6633 0.1767 0.4010 0.053 Uiso 1 1 calc R . . C12 C 0.54265(18) 0.27173(14) 0.40969(10) 0.0388(5) Uani 1 1 d . . . C13 C 0.50588(16) 0.32818(13) 0.44670(10) 0.0337(5) Uani 1 1 d . . . C14 C 0.8067(2) 0.13179(19) 0.49560(15) 0.0670(8) Uani 1 1 d . . . H14A H 0.8416 0.1360 0.5311 0.101 Uiso 1 1 calc R . . H14B H 0.8451 0.1430 0.4589 0.101 Uiso 1 1 calc R . . H14C H 0.8004 0.0744 0.5061 0.101 Uiso 1 1 calc R . . C15 C 0.46811(18) 0.27822(14) 0.35721(10) 0.0373(5) Uani 1 1 d . . . H15A H 0.4352 0.3403 0.3345 0.045 Uiso 1 1 calc R . . C16 C 0.52222(19) 0.23805(15) 0.30811(11) 0.0434(5) Uani 1 1 d . . . C17 C 0.5545(2) 0.28953(15) 0.25354(11) 0.0449(6) Uani 1 1 d . . . C18 C 0.6155(2) 0.25208(16) 0.21181(12) 0.0538(7) Uani 1 1 d . . . C19 C 0.6411(3) 0.16264(17) 0.22685(13) 0.0648(8) Uani 1 1 d . . . H19A H 0.6823 0.1370 0.2003 0.078 Uiso 1 1 calc R . . C20 C 0.6088(2) 0.10919(16) 0.27932(13) 0.0604(8) Uani 1 1 d . . . C21 C 0.5494(2) 0.14822(15) 0.31984(11) 0.0498(6) Uani 1 1 d . . . H21A H 0.5272 0.1137 0.3555 0.060 Uiso 1 1 calc R . . C22 C 0.6519(3) 0.30870(18) 0.15204(13) 0.0622(8) Uani 1 1 d . . . C23 C 0.5612(3) 0.37634(18) 0.10736(12) 0.0631(8) Uani 1 1 d . . . H23A H 0.5207 0.3475 0.0929 0.095 Uiso 1 1 calc R . . H23B H 0.5858 0.4118 0.0713 0.095 Uiso 1 1 calc R . . H23C H 0.5201 0.4123 0.1298 0.095 Uiso 1 1 calc R . . C24 C 0.7214(2) 0.3539(2) 0.17311(14) 0.0685(8) Uani 1 1 d . . . H24A H 0.6837 0.3894 0.1969 0.103 Uiso 1 1 calc R . . H24B H 0.7436 0.3897 0.1360 0.103 Uiso 1 1 calc R . . H24C H 0.7800 0.3105 0.1994 0.103 Uiso 1 1 calc R . . C25 C 0.7144(3) 0.2530(2) 0.11327(16) 0.0912(13) Uani 1 1 d . . . H25A H 0.6725 0.2246 0.0995 0.137 Uiso 1 1 calc R . . H25B H 0.7732 0.2100 0.1396 0.137 Uiso 1 1 calc R . . H25C H 0.7363 0.2898 0.0766 0.137 Uiso 1 1 calc R . . C26 C 0.6387(3) 0.01127(17) 0.29250(15) 0.0805(11) Uani 1 1 d . . . H26A H 0.6468 -0.0005 0.2528 0.121 Uiso 1 1 calc R . . H26B H 0.5860 -0.0106 0.3139 0.121 Uiso 1 1 calc R . . H26C H 0.7020 -0.0167 0.3191 0.121 Uiso 1 1 calc R . . C27 C 0.38318(18) 0.23968(14) 0.38785(10) 0.0381(5) Uani 1 1 d . . . C28 C 0.2808(2) 0.27731(15) 0.36412(11) 0.0449(6) Uani 1 1 d . . . C29 C 0.2031(2) 0.24442(17) 0.39582(12) 0.0490(6) Uani 1 1 d . . . C30 C 0.2348(2) 0.17009(17) 0.44979(12) 0.0519(6) Uani 1 1 d . . . H30A H 0.1855 0.1464 0.4707 0.062 Uiso 1 1 calc R . . C31 C 0.3364(2) 0.12998(16) 0.47362(11) 0.0482(6) Uani 1 1 d . . . C32 C 0.4085(2) 0.16708(15) 0.44294(11) 0.0436(5) Uani 1 1 d . . . H32A H 0.4764 0.1426 0.4598 0.052 Uiso 1 1 calc R . . C33 C 0.0890(2) 0.2897(2) 0.37363(14) 0.0627(8) Uani 1 1 d . . . C34 C 0.0637(3) 0.2942(3) 0.30541(15) 0.0828(10) Uani 1 1 d . . . H34A H 0.0978 0.3303 0.2762 0.124 Uiso 1 1 calc R . . H34B H -0.0089 0.3185 0.2948 0.124 Uiso 1 1 calc R . . H34C H 0.0863 0.2367 0.3024 0.124 Uiso 1 1 calc R . . C35 C 0.0209(3) 0.2400(2) 0.41625(17) 0.0842(10) Uani 1 1 d . . . H35A H 0.0417 0.1809 0.4165 0.126 Uiso 1 1 calc R . . H35B H -0.0493 0.2677 0.3995 0.126 Uiso 1 1 calc R . . H35C H 0.0283 0.2408 0.4591 0.126 Uiso 1 1 calc R . . C36 C 0.0578(2) 0.3810(2) 0.37848(17) 0.0800(10) Uani 1 1 d . . . H36A H 0.1015 0.4124 0.3547 0.120 Uiso 1 1 calc R . . H36B H 0.0642 0.3772 0.4225 0.120 Uiso 1 1 calc R . . H36C H -0.0119 0.4110 0.3612 0.120 Uiso 1 1 calc R . . C37 C 0.3665(3) 0.04905(19) 0.53238(13) 0.0700(9) Uani 1 1 d . . . H37A H 0.4380 0.0339 0.5449 0.105 Uiso 1 1 calc R . . H37B H 0.3532 0.0019 0.5227 0.105 Uiso 1 1 calc R . . H37C H 0.3272 0.0602 0.5667 0.105 Uiso 1 1 calc R . . C38 C 0.19622(18) 0.60549(15) 0.48595(11) 0.0425(5) Uani 1 1 d . . . H38A H 0.1605 0.6304 0.5147 0.051 Uiso 1 1 calc R . . C39 C 0.15733(17) 0.64449(15) 0.41981(11) 0.0404(5) Uani 1 1 d . . . C40 C 0.06982(19) 0.71916(16) 0.40358(12) 0.0482(6) Uani 1 1 d . . . H40A H 0.0404 0.7399 0.4358 0.058 Uiso 1 1 calc R . . C41 C 0.02764(19) 0.76130(16) 0.34265(13) 0.0498(6) Uani 1 1 d . . . C42 C 0.0771(2) 0.73046(15) 0.29495(12) 0.0491(6) Uani 1 1 d . . . H42A H 0.0501 0.7598 0.2528 0.059 Uiso 1 1 calc R . . C43 C 0.16385(18) 0.65883(15) 0.30723(11) 0.0416(5) Uani 1 1 d . . . C44 C 0.20484(17) 0.61070(14) 0.37238(10) 0.0372(5) Uani 1 1 d . . . C45 C -0.0696(2) 0.83771(17) 0.32595(15) 0.0643(8) Uani 1 1 d . . . H45A H -0.0788 0.8635 0.3592 0.097 Uiso 1 1 calc R . . H45B H -0.1270 0.8179 0.3219 0.097 Uiso 1 1 calc R . . H45C H -0.0647 0.8801 0.2863 0.097 Uiso 1 1 calc R . . C46 C 0.21976(18) 0.63370(15) 0.25271(10) 0.0416(5) Uani 1 1 d . . . H46A H 0.2518 0.5705 0.2679 0.050 Uiso 1 1 calc R . . C47 C 0.1443(2) 0.65670(16) 0.19442(12) 0.0490(6) Uani 1 1 d . . . C48 C 0.0874(2) 0.60339(18) 0.19108(13) 0.0534(6) Uani 1 1 d . . . C49 C 0.0085(2) 0.6297(2) 0.14197(14) 0.0663(8) Uani 1 1 d . . . C50 C -0.0031(3) 0.7104(2) 0.09500(17) 0.0894(11) Uani 1 1 d . . . H50A H -0.0545 0.7299 0.0620 0.107 Uiso 1 1 calc R . . C51 C 0.0570(3) 0.7633(2) 0.09453(16) 0.0921(12) Uani 1 1 d . . . C52 C 0.1283(3) 0.7365(2) 0.14529(13) 0.0746(9) Uani 1 1 d . . . H52A H 0.1671 0.7723 0.1473 0.090 Uiso 1 1 calc R . . C53 C -0.0593(3) 0.5739(3) 0.14062(16) 0.0788(10) Uani 1 1 d . . . C54 C 0.0011(3) 0.4881(3) 0.1349(2) 0.1077(14) Uani 1 1 d . . . H54A H 0.0525 0.4576 0.1702 0.162 Uiso 1 1 calc R . . H54B H 0.0334 0.4975 0.0956 0.162 Uiso 1 1 calc R . . H54C H -0.0438 0.4541 0.1353 0.162 Uiso 1 1 calc R . . C55 C -0.1422(3) 0.6202(3) 0.0818(2) 0.1105(14) Uani 1 1 d . . . H55A H -0.1818 0.6763 0.0833 0.166 Uiso 1 1 calc R . . H55B H -0.1866 0.5854 0.0834 0.166 Uiso 1 1 calc R . . H55C H -0.1089 0.6272 0.0429 0.166 Uiso 1 1 calc R . . C56 C -0.1167(3) 0.5590(3) 0.2004(2) 0.1171(16) Uani 1 1 d . . . H56A H -0.0689 0.5358 0.2376 0.176 Uiso 1 1 calc R . . H56B H -0.1532 0.5185 0.2012 0.176 Uiso 1 1 calc R . . H56C H -0.1644 0.6132 0.2003 0.176 Uiso 1 1 calc R . . C57 C 0.0420(5) 0.8499(3) 0.0384(2) 0.141(2) Uani 1 1 d . . . H57A H 0.0776 0.8844 0.0502 0.212 Uiso 1 1 calc R . . H57B H -0.0296 0.8815 0.0294 0.212 Uiso 1 1 calc R . . H57C H 0.0689 0.8372 0.0012 0.212 Uiso 1 1 calc R . . C58 C 0.30477(18) 0.67626(14) 0.23233(10) 0.0416(5) Uani 1 1 d . . . C59 C 0.36936(19) 0.65377(14) 0.18675(10) 0.0422(5) Uani 1 1 d . . . C60 C 0.4366(2) 0.70087(15) 0.15952(11) 0.0468(6) Uani 1 1 d . . . C61 C 0.4423(2) 0.76620(16) 0.18330(13) 0.0546(7) Uani 1 1 d . . . H61A H 0.4870 0.7978 0.1664 0.065 Uiso 1 1 calc R . . C62 C 0.3844(2) 0.78573(17) 0.23084(14) 0.0566(7) Uani 1 1 d . . . C63 C 0.3143(2) 0.74205(16) 0.25392(12) 0.0491(6) Uani 1 1 d . . . H63A H 0.2726 0.7569 0.2846 0.059 Uiso 1 1 calc R . . C64 C 0.5012(2) 0.68164(16) 0.10558(11) 0.0530(6) Uani 1 1 d . . . C65 C 0.5639(3) 0.7458(2) 0.08093(15) 0.0723(9) Uani 1 1 d . . . H65A H 0.5184 0.8043 0.0663 0.108 Uiso 1 1 calc R . . H65B H 0.6011 0.7336 0.0462 0.108 Uiso 1 1 calc R . . H65C H 0.6112 0.7394 0.1149 0.108 Uiso 1 1 calc R . . C66 C 0.4304(3) 0.6925(2) 0.04873(13) 0.0728(9) Uani 1 1 d . . . H66A H 0.3856 0.7512 0.0332 0.109 Uiso 1 1 calc R . . H66B H 0.3905 0.6531 0.0621 0.109 Uiso 1 1 calc R . . H66C H 0.4708 0.6798 0.0153 0.109 Uiso 1 1 calc R . . C67 C 0.5777(3) 0.58937(18) 0.12957(14) 0.0660(8) Uani 1 1 d . . . H67A H 0.5415 0.5481 0.1478 0.099 Uiso 1 1 calc R . . H67B H 0.6266 0.5862 0.1614 0.099 Uiso 1 1 calc R . . H67C H 0.6125 0.5762 0.0944 0.099 Uiso 1 1 calc R . . C68 C 0.3971(3) 0.8553(2) 0.2569(2) 0.0909(12) Uani 1 1 d . . . H68A H 0.4005 0.8343 0.3028 0.136 Uiso 1 1 calc R . . H68B H 0.3399 0.9070 0.2408 0.136 Uiso 1 1 calc R . . H68C H 0.4591 0.8684 0.2436 0.136 Uiso 1 1 calc R . . N3 N 0.3038(3) 0.22892(18) 0.16602(12) 0.0779(8) Uani 1 1 d . . . C1A C 0.3094(3) 0.1861(2) 0.23795(14) 0.0726(9) Uani 1 1 d . . . H1AA H 0.3659 0.1964 0.2567 0.087 Uiso 1 1 calc R . . H1AB H 0.2473 0.2163 0.2528 0.087 Uiso 1 1 calc R . . C1B C 0.2952(3) 0.3239(2) 0.15685(14) 0.0735(9) Uani 1 1 d . . . H1BA H 0.2431 0.3447 0.1830 0.088 Uiso 1 1 calc R . . H1BB H 0.3597 0.3254 0.1730 0.088 Uiso 1 1 calc R . . C1C C 0.4047(4) 0.1919(3) 0.14030(19) 0.1045(14) Uani 1 1 d . . . H1CA H 0.4134 0.2368 0.1026 0.125 Uiso 1 1 calc R . . H1CB H 0.4598 0.1792 0.1722 0.125 Uiso 1 1 calc R . . C1D C 0.2130(5) 0.2219(3) 0.13198(17) 0.131(2) Uani 1 1 d . A . H1DA H 0.2136 0.2500 0.0865 0.157 Uiso 1 1 calc R . . H1DB H 0.2227 0.1608 0.1389 0.157 Uiso 1 1 calc R . . C2A C 0.3223(3) 0.0908(2) 0.26487(15) 0.0774(10) Uani 1 1 d . . . H2AA H 0.3880 0.0582 0.2553 0.093 Uiso 1 1 calc R . . H2AB H 0.2691 0.0777 0.2451 0.093 Uiso 1 1 calc R . . C2B C 0.2694(3) 0.3870(2) 0.08909(15) 0.0875(11) Uani 1 1 d . . . H2BA H 0.2033 0.3891 0.0726 0.105 Uiso 1 1 calc R . . H2BB H 0.3205 0.3678 0.0618 0.105 Uiso 1 1 calc R . . C2C C 0.4164(7) 0.1140(4) 0.1235(3) 0.193(4) Uani 1 1 d . . . H2CA H 0.3627 0.1267 0.0907 0.231 Uiso 1 1 calc R . . H2CB H 0.4068 0.0689 0.1608 0.231 Uiso 1 1 calc R . . C2D C 0.1092(5) 0.2602(4) 0.1514(2) 0.1272(18) Uani 1 1 d . . . C3A C 0.3163(3) 0.0637(2) 0.33602(15) 0.0803(10) Uani 1 1 d . . . H3AA H 0.3571 0.0908 0.3531 0.096 Uiso 1 1 calc R . . H3AB H 0.2459 0.0880 0.3439 0.096 Uiso 1 1 calc R . . C3B C 0.2669(3) 0.4764(2) 0.08909(15) 0.0725(9) Uani 1 1 d . . . H3BA H 0.3346 0.4744 0.1028 0.087 Uiso 1 1 calc R . . H3BB H 0.2202 0.4928 0.1195 0.087 Uiso 1 1 calc R . . C3C C 0.5171(6) 0.0797(3) 0.0999(2) 0.158(3) Uani 1 1 d . . . H3CA H 0.5271 0.1238 0.0622 0.190 Uiso 1 1 calc R . . H3CB H 0.5715 0.0663 0.1325 0.190 Uiso 1 1 calc R . . C3D C 0.0101(8) 0.2997(10) 0.0951(8) 0.114(5) Uani 0.456(14) 1 d P A 1 H3DA H -0.0524 0.3264 0.1115 0.136 Uiso 0.456(14) 1 calc PR A 1 H3DB H 0.0229 0.3430 0.0578 0.136 Uiso 0.456(14) 1 calc PR A 1 C3D' C 0.0661(9) 0.2310(7) 0.0982(4) 0.111(4) Uani 0.544(14) 1 d P A 2 H3DC H 0.0890 0.2538 0.0564 0.133 Uiso 0.544(14) 1 calc PR A 2 H3DD H 0.0807 0.1685 0.1102 0.133 Uiso 0.544(14) 1 calc PR A 2 C4A C 0.3488(4) -0.0292(2) 0.37304(17) 0.0999(13) Uani 1 1 d . . . H4AA H 0.3429 -0.0366 0.4176 0.150 Uiso 1 1 calc R . . H4AB H 0.4188 -0.0550 0.3666 0.150 Uiso 1 1 calc R . . H4AC H 0.3062 -0.0570 0.3593 0.150 Uiso 1 1 calc R . . C4B C 0.2330(4) 0.5448(3) 0.02331(18) 0.1129(15) Uani 1 1 d . . . H4BA H 0.2355 0.5999 0.0248 0.169 Uiso 1 1 calc R . . H4BB H 0.1643 0.5497 0.0107 0.169 Uiso 1 1 calc R . . H4BC H 0.2779 0.5280 -0.0071 0.169 Uiso 1 1 calc R . . C4C C 0.5225(8) 0.0006(5) 0.0843(4) 0.252(5) Uani 1 1 d . . . H4CA H 0.5928 -0.0329 0.0860 0.378 Uiso 1 1 calc R . . H4CB H 0.4903 0.0168 0.0421 0.378 Uiso 1 1 calc R . . H4CC H 0.4878 -0.0336 0.1147 0.378 Uiso 1 1 calc R . . C4D C 0.0010(8) 0.2227(8) 0.0781(5) 0.103(4) Uani 0.456(14) 1 d P A 1 H4DA H -0.0543 0.2419 0.0456 0.154 Uiso 0.456(14) 1 calc PR A 1 H4DB H -0.0123 0.1807 0.1155 0.154 Uiso 0.456(14) 1 calc PR A 1 H4DC H 0.0637 0.1964 0.0626 0.154 Uiso 0.456(14) 1 calc PR A 1 C4D' C -0.0366(13) 0.2741(9) 0.1029(8) 0.146(5) Uani 0.544(14) 1 d P A 2 H4DD H -0.0801 0.2618 0.0759 0.220 Uiso 0.544(14) 1 calc PR A 2 H4DE H -0.0472 0.3357 0.0895 0.220 Uiso 0.544(14) 1 calc PR A 2 H4DF H -0.0527 0.2544 0.1464 0.220 Uiso 0.544(14) 1 calc PR A 2 H2 H 0.476(2) 0.403(2) 0.2519(18) 0.118(15) Uiso 1 1 d D . . H3 H 0.295(2) 0.3721(18) 0.2991(14) 0.075(10) Uiso 1 1 d D . . H6 H 0.352(2) 0.5470(16) 0.1930(12) 0.076(10) Uiso 1 1 d D . . H5 H 0.1669(16) 0.501(2) 0.2561(14) 0.082 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03496(16) 0.03378(16) 0.02891(15) -0.00942(11) -0.00072(10) -0.00947(11) F1 0.0706(10) 0.0379(7) 0.0464(8) -0.0042(6) 0.0016(7) -0.0211(7) O1 0.0391(8) 0.0355(8) 0.0321(7) -0.0122(6) -0.0013(6) -0.0083(7) O2 0.0684(12) 0.0341(9) 0.0458(10) -0.0147(7) 0.0170(9) -0.0173(8) O3 0.0516(11) 0.0604(11) 0.0419(10) 0.0012(8) -0.0009(8) -0.0200(9) O4 0.0370(8) 0.0368(8) 0.0340(8) -0.0127(6) -0.0036(6) -0.0052(7) O5 0.0824(16) 0.0747(14) 0.0721(14) -0.0017(11) -0.0154(12) -0.0378(13) O6 0.0789(13) 0.0381(9) 0.0367(9) -0.0135(7) 0.0077(8) -0.0274(9) N1 0.0430(11) 0.0381(10) 0.0268(9) -0.0092(7) 0.0002(8) -0.0089(8) N2 0.0389(10) 0.0446(11) 0.0318(9) -0.0130(8) 0.0010(8) -0.0132(9) C1 0.0517(14) 0.0461(13) 0.0341(12) -0.0124(10) 0.0027(10) -0.0205(11) C2 0.0579(16) 0.0490(14) 0.0315(12) -0.0097(10) -0.0028(10) -0.0133(12) C3 0.0731(19) 0.0664(17) 0.0348(13) -0.0173(12) -0.0011(12) -0.0237(15) C4 0.076(2) 0.0760(19) 0.0364(13) -0.0228(13) 0.0081(13) -0.0237(16) C5 0.0502(15) 0.0573(15) 0.0380(12) -0.0204(11) 0.0066(11) -0.0144(12) C6 0.0528(15) 0.0526(14) 0.0370(12) -0.0168(11) 0.0077(11) -0.0216(12) C7 0.0443(13) 0.0408(12) 0.0305(11) -0.0056(9) -0.0052(9) -0.0128(10) C8 0.0365(12) 0.0341(11) 0.0338(11) -0.0055(9) 0.0012(9) -0.0100(9) C9 0.0415(13) 0.0407(13) 0.0383(12) -0.0026(10) -0.0033(10) -0.0107(10) C10 0.0381(13) 0.0414(13) 0.0539(15) -0.0079(11) 0.0043(11) -0.0067(10) C11 0.0441(14) 0.0361(12) 0.0469(13) -0.0114(10) 0.0118(11) -0.0085(10) C12 0.0447(13) 0.0322(11) 0.0358(11) -0.0065(9) 0.0063(10) -0.0115(10) C13 0.0359(12) 0.0303(11) 0.0332(11) -0.0066(8) 0.0014(9) -0.0114(9) C14 0.0464(16) 0.0660(19) 0.0734(19) -0.0180(15) 0.0038(14) -0.0003(14) C15 0.0482(13) 0.0305(11) 0.0317(11) -0.0104(8) 0.0062(9) -0.0101(10) C16 0.0536(15) 0.0391(12) 0.0373(12) -0.0153(10) 0.0108(10) -0.0112(11) C17 0.0601(16) 0.0346(12) 0.0403(13) -0.0139(10) 0.0095(11) -0.0135(11) C18 0.0746(19) 0.0451(14) 0.0444(14) -0.0183(11) 0.0213(13) -0.0191(13) C19 0.094(2) 0.0457(15) 0.0543(16) -0.0233(12) 0.0315(15) -0.0150(15) C20 0.091(2) 0.0348(13) 0.0499(15) -0.0157(11) 0.0193(14) -0.0097(13) C21 0.0695(17) 0.0369(13) 0.0387(13) -0.0111(10) 0.0135(12) -0.0121(12) C22 0.088(2) 0.0498(15) 0.0501(15) -0.0194(12) 0.0320(15) -0.0215(15) C23 0.095(2) 0.0575(17) 0.0403(14) -0.0152(12) 0.0199(14) -0.0303(16) C24 0.075(2) 0.0640(18) 0.0603(18) -0.0109(14) 0.0221(15) -0.0237(16) C25 0.139(3) 0.0632(19) 0.068(2) -0.0237(16) 0.061(2) -0.027(2) C26 0.133(3) 0.0380(15) 0.0619(18) -0.0186(13) 0.0350(19) -0.0124(17) C27 0.0498(14) 0.0326(11) 0.0331(11) -0.0137(9) 0.0070(10) -0.0113(10) C28 0.0569(16) 0.0434(13) 0.0336(12) -0.0110(10) 0.0058(11) -0.0159(11) C29 0.0516(15) 0.0536(15) 0.0436(13) -0.0159(11) 0.0089(11) -0.0192(12) C30 0.0621(17) 0.0569(15) 0.0427(14) -0.0162(11) 0.0166(12) -0.0279(13) C31 0.0606(17) 0.0453(14) 0.0375(12) -0.0111(10) 0.0098(11) -0.0174(12) C32 0.0528(15) 0.0379(12) 0.0382(12) -0.0132(10) 0.0065(10) -0.0105(11) C33 0.0519(16) 0.074(2) 0.0567(17) -0.0101(14) 0.0075(13) -0.0235(15) C34 0.063(2) 0.114(3) 0.065(2) -0.0111(19) 0.0014(16) -0.0369(19) C35 0.060(2) 0.103(3) 0.083(2) -0.0115(19) 0.0193(17) -0.0356(19) C36 0.0496(18) 0.084(2) 0.084(2) -0.0081(18) 0.0007(16) -0.0080(16) C37 0.078(2) 0.0597(18) 0.0555(17) 0.0029(14) 0.0126(15) -0.0207(16) C38 0.0418(13) 0.0474(13) 0.0409(12) -0.0203(10) 0.0058(10) -0.0114(11) C39 0.0363(12) 0.0404(12) 0.0432(12) -0.0140(10) -0.0013(10) -0.0090(10) C40 0.0442(14) 0.0437(14) 0.0567(15) -0.0205(11) 0.0037(11) -0.0089(11) C41 0.0418(14) 0.0403(13) 0.0590(15) -0.0113(11) -0.0041(11) -0.0055(11) C42 0.0500(15) 0.0405(13) 0.0480(14) -0.0062(11) -0.0083(11) -0.0098(11) C43 0.0411(13) 0.0393(12) 0.0403(12) -0.0096(10) -0.0054(10) -0.0097(10) C44 0.0396(12) 0.0353(12) 0.0376(11) -0.0124(9) -0.0025(9) -0.0119(10) C45 0.0505(16) 0.0462(15) 0.079(2) -0.0116(14) -0.0020(14) 0.0004(13) C46 0.0497(14) 0.0343(12) 0.0353(12) -0.0080(9) -0.0094(10) -0.0077(10) C47 0.0555(16) 0.0445(14) 0.0434(13) -0.0138(11) -0.0107(11) -0.0102(12) C48 0.0504(15) 0.0557(16) 0.0525(15) -0.0173(12) -0.0051(12) -0.0137(12) C49 0.0651(19) 0.087(2) 0.0605(18) -0.0334(16) -0.0013(14) -0.0335(17) C50 0.083(2) 0.095(3) 0.075(2) -0.0007(19) -0.0368(19) -0.031(2) C51 0.114(3) 0.078(2) 0.067(2) 0.0051(17) -0.042(2) -0.033(2) C52 0.093(2) 0.0706(19) 0.0503(16) -0.0014(14) -0.0286(16) -0.0294(18) C53 0.060(2) 0.115(3) 0.074(2) -0.033(2) 0.0034(16) -0.043(2) C54 0.109(3) 0.106(3) 0.134(4) -0.046(3) -0.004(3) -0.064(3) C55 0.085(3) 0.163(4) 0.097(3) -0.039(3) -0.019(2) -0.060(3) C56 0.104(3) 0.176(5) 0.092(3) -0.034(3) 0.015(2) -0.084(3) C57 0.187(5) 0.110(3) 0.098(3) 0.032(3) -0.059(3) -0.072(4) C58 0.0483(14) 0.0383(12) 0.0342(11) -0.0102(9) -0.0071(10) -0.0086(10) C59 0.0571(15) 0.0346(12) 0.0344(12) -0.0085(9) -0.0047(10) -0.0158(11) C60 0.0644(16) 0.0378(13) 0.0377(12) -0.0077(10) -0.0012(11) -0.0197(12) C61 0.0663(18) 0.0448(14) 0.0566(16) -0.0169(12) 0.0011(13) -0.0223(13) C62 0.0675(18) 0.0465(15) 0.0663(17) -0.0284(13) -0.0007(14) -0.0217(13) C63 0.0569(16) 0.0443(14) 0.0496(14) -0.0227(11) -0.0025(12) -0.0122(12) C64 0.0749(19) 0.0485(14) 0.0390(13) -0.0099(11) 0.0073(12) -0.0286(13) C65 0.095(2) 0.0653(19) 0.0642(19) -0.0166(15) 0.0225(17) -0.0422(18) C66 0.100(2) 0.089(2) 0.0366(14) -0.0160(14) 0.0100(15) -0.044(2) C67 0.084(2) 0.0549(17) 0.0588(17) -0.0186(13) 0.0252(16) -0.0220(15) C68 0.101(3) 0.095(3) 0.123(3) -0.079(2) 0.029(2) -0.053(2) N3 0.122(2) 0.0825(19) 0.0528(15) -0.0302(13) 0.0185(15) -0.0576(18) C1A 0.106(3) 0.071(2) 0.0570(17) -0.0251(15) 0.0073(17) -0.0473(19) C1B 0.109(3) 0.071(2) 0.0587(18) -0.0233(15) 0.0034(17) -0.053(2) C1C 0.169(4) 0.082(3) 0.082(3) -0.033(2) 0.021(3) -0.059(3) C1D 0.277(7) 0.122(3) 0.0468(19) -0.022(2) -0.001(3) -0.144(5) C2A 0.121(3) 0.066(2) 0.068(2) -0.0326(16) 0.0258(19) -0.051(2) C2B 0.126(3) 0.098(3) 0.060(2) -0.0237(18) 0.004(2) -0.068(2) C2C 0.381(11) 0.137(4) 0.144(5) -0.100(4) 0.149(6) -0.150(6) C2D 0.135(4) 0.176(5) 0.099(3) -0.034(3) -0.009(3) -0.099(4) C3A 0.121(3) 0.071(2) 0.065(2) -0.0271(16) 0.0187(19) -0.048(2) C3B 0.085(2) 0.077(2) 0.0656(19) -0.0199(16) 0.0004(16) -0.0438(18) C3C 0.276(8) 0.094(3) 0.096(3) -0.040(3) 0.077(4) -0.038(4) C3D 0.059(6) 0.124(10) 0.219(13) -0.119(10) 0.052(7) -0.051(6) C3D' 0.134(10) 0.117(8) 0.099(6) -0.042(5) -0.006(6) -0.057(7) C4A 0.165(4) 0.075(2) 0.078(2) -0.0330(19) 0.029(3) -0.056(3) C4B 0.154(4) 0.113(3) 0.077(3) -0.006(2) 0.007(3) -0.076(3) C4C 0.430(14) 0.172(6) 0.257(9) -0.159(6) 0.210(9) -0.156(8) C4D 0.071(6) 0.142(10) 0.120(8) -0.063(7) -0.006(5) -0.046(6) C4D' 0.145(12) 0.119(9) 0.200(13) -0.090(9) -0.009(10) -0.033(8) _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 Ni1 N2 1.8466(18) . ? Ni1 O1 1.8495(14) . ? Ni1 N1 1.8603(17) . ? Ni1 O4 1.8641(14) . ? O1 C13 1.307(2) . ? O2 C17 1.368(3) . ? O2 H2 0.831(18) . ? O3 C28 1.366(3) . ? O3 H3 0.853(18) . ? O4 C44 1.308(3) . ? O5 C48 1.338(3) . ? O5 H5 0.890(18) . ? O6 C59 1.364(3) . ? O6 H6 0.836(17) . ? N1 C7 1.289(3) . ? N1 C1 1.489(3) . ? N2 C38 1.280(3) . ? N2 C6 1.490(3) . ? C1 C2 1.516(3) . ? C1 C6 1.519(3) . ? C1 H1A 0.9800 . ? C2 C3 1.524(3) . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.506(4) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.525(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.512(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9800 . ? C7 C8 1.429(3) . ? C7 H7A 0.9300 . ? C8 C9 1.415(3) . ? C8 C13 1.422(3) . ? C9 C10 1.359(3) . ? C9 H9A 0.9300 . ? C10 C11 1.408(4) . ? C10 C14 1.516(3) . ? C11 C12 1.385(3) . ? C11 H11A 0.9300 . ? C12 C13 1.433(3) . ? C12 C15 1.517(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.533(3) . ? C15 C27 1.547(3) . ? C15 H15A 0.9800 . ? C16 C17 1.401(3) . ? C16 C21 1.400(3) . ? C17 C18 1.414(3) . ? C18 C19 1.385(4) . ? C18 C22 1.543(3) . ? C19 C20 1.387(4) . ? C19 H19A 0.9300 . ? C20 C21 1.397(3) . ? C20 C26 1.524(4) . ? C21 H21A 0.9300 . ? C22 C23 1.524(4) . ? C22 C25 1.546(4) . ? C22 C24 1.547(4) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.392(3) . ? C27 C28 1.393(3) . ? C28 C29 1.421(3) . ? C29 C30 1.396(3) . ? C29 C33 1.536(4) . ? C30 C31 1.387(4) . ? C30 H30A 0.9300 . ? C31 C32 1.384(3) . ? C31 C37 1.517(3) . ? C32 H32A 0.9300 . ? C33 C36 1.525(5) . ? C33 C34 1.529(4) . ? C33 C35 1.552(4) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.438(3) . ? C38 H38A 0.9300 . ? C39 C44 1.415(3) . ? C39 C40 1.418(3) . ? C40 C41 1.354(3) . ? C40 H40A 0.9300 . ? C41 C42 1.405(4) . ? C41 C45 1.516(3) . ? C42 C43 1.386(3) . ? C42 H42A 0.9300 . ? C43 C44 1.439(3) . ? C43 C46 1.529(3) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C58 1.538(3) . ? C46 C47 1.541(3) . ? C46 H46A 0.9800 . ? C47 C48 1.380(4) . ? C47 C52 1.403(4) . ? C48 C49 1.413(4) . ? C49 C50 1.401(4) . ? C49 C53 1.519(4) . ? C50 C51 1.387(5) . ? C50 H50A 0.9300 . ? C51 C52 1.369(4) . ? C51 C57 1.556(5) . ? C52 H52A 0.9300 . ? C53 C54 1.497(5) . ? C53 C56 1.521(5) . ? C53 C55 1.574(5) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 C63 1.390(3) . ? C58 C59 1.404(3) . ? C59 C60 1.403(3) . ? C60 C61 1.396(3) . ? C60 C64 1.538(4) . ? C61 C62 1.376(4) . ? C61 H61A 0.9300 . ? C62 C63 1.379(4) . ? C62 C68 1.527(4) . ? C63 H63A 0.9300 . ? C64 C66 1.533(4) . ? C64 C67 1.538(4) . ? C64 C65 1.547(4) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? N3 C1A 1.519(4) . ? N3 C1D 1.521(6) . ? N3 C1C 1.526(5) . ? N3 C1B 1.534(4) . ? C1A C2A 1.495(4) . ? C1A H1AA 0.9700 . ? C1A H1AB 0.9700 . ? C1B C2B 1.516(4) . ? C1B H1BA 0.9700 . ? C1B H1BB 0.9700 . ? C1C C2C 1.453(6) . ? C1C H1CA 0.9700 . ? C1C H1CB 0.9700 . ? C1D C2D 1.500(7) . ? C1D H1DA 0.9700 . ? C1D H1DB 0.9700 . ? C2A C3A 1.503(4) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C2B C3B 1.512(4) . ? C2B H2BA 0.9700 . ? C2B H2BB 0.9700 . ? C2C C3C 1.489(8) . ? C2C H2CA 0.9700 . ? C2C H2CB 0.9700 . ? C2D C3D' 1.598(11) . ? C2D C3D 1.684(15) . ? C3A C4A 1.463(4) . ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C3B C4B 1.522(4) . ? C3B H3BA 0.9700 . ? C3B H3BB 0.9700 . ? C3C C4C 1.475(7) . ? C3C H3CA 0.9700 . ? C3C H3CB 0.9700 . ? C3D C4D 1.51(2) . ? C3D H3DA 0.9700 . ? C3D H3DB 0.9700 . ? C3D' C4D' 1.40(2) . ? C3D' H3DC 0.9700 . ? C3D' H3DD 0.9700 . ? C4A H4AA 0.9600 . ? C4A H4AB 0.9600 . ? C4A H4AC 0.9600 . ? C4B H4BA 0.9600 . ? C4B H4BB 0.9600 . ? C4B H4BC 0.9600 . ? C4C H4CA 0.9600 . ? C4C H4CB 0.9600 . ? C4C H4CC 0.9600 . ? C4D H4DA 0.9600 . ? C4D H4DB 0.9600 . ? C4D H4DC 0.9600 . ? C4D' H4DD 0.9600 . ? C4D' H4DE 0.9600 . ? C4D' H4DF 0.9600 . ? 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 N2 Ni1 O1 169.66(7) . . ? N2 Ni1 N1 85.75(8) . . ? O1 Ni1 N1 94.43(7) . . ? N2 Ni1 O4 95.14(7) . . ? O1 Ni1 O4 86.98(6) . . ? N1 Ni1 O4 167.20(7) . . ? C13 O1 Ni1 127.49(13) . . ? C17 O2 H2 118(3) . . ? C28 O3 H3 110(2) . . ? C44 O4 Ni1 127.32(14) . . ? C48 O5 H5 116(2) . . ? C59 O6 H6 114(2) . . ? C7 N1 C1 119.62(19) . . ? C7 N1 Ni1 126.88(15) . . ? C1 N1 Ni1 112.52(14) . . ? C38 N2 C6 120.29(19) . . ? C38 N2 Ni1 126.40(16) . . ? C6 N2 Ni1 113.02(14) . . ? N1 C1 C2 117.80(19) . . ? N1 C1 C6 104.72(19) . . ? C2 C1 C6 112.11(19) . . ? N1 C1 H1A 107.2 . . ? C2 C1 H1A 107.2 . . ? C6 C1 H1A 107.2 . . ? C1 C2 C3 108.2(2) . . ? C1 C2 H2B 110.1 . . ? C3 C2 H2B 110.1 . . ? C1 C2 H2C 110.1 . . ? C3 C2 H2C 110.1 . . ? H2B C2 H2C 108.4 . . ? C4 C3 C2 112.4(2) . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3C 109.1 . . ? C2 C3 H3C 109.1 . . ? H3B C3 H3C 107.9 . . ? C3 C4 C5 112.2(2) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 109.9(2) . . ? C6 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? C6 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N2 C6 C5 117.0(2) . . ? N2 C6 C1 103.85(18) . . ? C5 C6 C1 111.3(2) . . ? N2 C6 H6A 108.1 . . ? C5 C6 H6A 108.1 . . ? C1 C6 H6A 108.1 . . ? N1 C7 C8 125.2(2) . . ? N1 C7 H7A 117.4 . . ? C8 C7 H7A 117.4 . . ? C9 C8 C13 120.1(2) . . ? C9 C8 C7 118.9(2) . . ? C13 C8 C7 120.98(19) . . ? C10 C9 C8 122.3(2) . . ? C10 C9 H9A 118.8 . . ? C8 C9 H9A 118.8 . . ? C9 C10 C11 117.4(2) . . ? C9 C10 C14 122.3(2) . . ? C11 C10 C14 120.3(2) . . ? C12 C11 C10 123.2(2) . . ? C12 C11 H11A 118.4 . . ? C10 C11 H11A 118.4 . . ? C11 C12 C13 119.2(2) . . ? C11 C12 C15 124.2(2) . . ? C13 C12 C15 116.46(19) . . ? O1 C13 C8 124.32(19) . . ? O1 C13 C12 118.40(19) . . ? C8 C13 C12 117.28(19) . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 C16 112.21(19) . . ? C12 C15 C27 109.13(17) . . ? C16 C15 C27 113.77(18) . . ? C12 C15 H15A 107.1 . . ? C16 C15 H15A 107.1 . . ? C27 C15 H15A 107.1 . . ? C17 C16 C21 118.5(2) . . ? C17 C16 C15 120.3(2) . . ? C21 C16 C15 120.8(2) . . ? O2 C17 C16 120.7(2) . . ? O2 C17 C18 118.0(2) . . ? C16 C17 C18 121.3(2) . . ? C19 C18 C17 117.2(2) . . ? C19 C18 C22 121.5(2) . . ? C17 C18 C22 121.2(2) . . ? C20 C19 C18 123.7(2) . . ? C20 C19 H19A 118.2 . . ? C18 C19 H19A 118.2 . . ? C19 C20 C21 117.6(2) . . ? C19 C20 C26 120.9(2) . . ? C21 C20 C26 121.5(2) . . ? C20 C21 C16 121.7(2) . . ? C20 C21 H21A 119.2 . . ? C16 C21 H21A 119.2 . . ? C23 C22 C18 111.0(2) . . ? C23 C22 C25 106.9(3) . . ? C18 C22 C25 111.3(2) . . ? C23 C22 C24 110.3(2) . . ? C18 C22 C24 109.2(2) . . ? C25 C22 C24 108.1(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 118.3(2) . . ? C32 C27 C15 119.2(2) . . ? C28 C27 C15 122.44(19) . . ? O3 C28 C27 122.5(2) . . ? O3 C28 C29 116.1(2) . . ? C27 C28 C29 121.4(2) . . ? C30 C29 C28 117.0(2) . . ? C30 C29 C33 120.9(2) . . ? C28 C29 C33 122.1(2) . . ? C31 C30 C29 122.9(2) . . ? C31 C30 H30A 118.6 . . ? C29 C30 H30A 118.6 . . ? C32 C31 C30 117.9(2) . . ? C32 C31 C37 121.4(2) . . ? C30 C31 C37 120.6(2) . . ? C31 C32 C27 122.5(2) . . ? C31 C32 H32A 118.8 . . ? C27 C32 H32A 118.8 . . ? C36 C33 C34 110.1(3) . . ? C36 C33 C29 109.6(3) . . ? C34 C33 C29 112.2(2) . . ? C36 C33 C35 107.3(3) . . ? C34 C33 C35 106.0(3) . . ? C29 C33 C35 111.5(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C31 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N2 C38 C39 125.8(2) . . ? N2 C38 H38A 117.1 . . ? C39 C38 H38A 117.1 . . ? C44 C39 C40 121.0(2) . . ? C44 C39 C38 121.6(2) . . ? C40 C39 C38 117.4(2) . . ? C41 C40 C39 122.1(2) . . ? C41 C40 H40A 118.9 . . ? C39 C40 H40A 118.9 . . ? C40 C41 C42 117.2(2) . . ? C40 C41 C45 122.0(2) . . ? C42 C41 C45 120.8(2) . . ? C43 C42 C41 123.7(2) . . ? C43 C42 H42A 118.1 . . ? C41 C42 H42A 118.1 . . ? C42 C43 C44 119.1(2) . . ? C42 C43 C46 121.1(2) . . ? C44 C43 C46 119.75(19) . . ? O4 C44 C39 123.44(19) . . ? O4 C44 C43 119.84(19) . . ? C39 C44 C43 116.7(2) . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 C58 112.56(19) . . ? C43 C46 C47 111.07(19) . . ? C58 C46 C47 109.71(18) . . ? C43 C46 H46A 107.8 . . ? C58 C46 H46A 107.8 . . ? C47 C46 H46A 107.8 . . ? C48 C47 C52 119.0(2) . . ? C48 C47 C46 121.7(2) . . ? C52 C47 C46 119.1(2) . . ? O5 C48 C47 120.2(2) . . ? O5 C48 C49 118.1(3) . . ? C47 C48 C49 121.8(3) . . ? C50 C49 C48 115.6(3) . . ? C50 C49 C53 122.4(3) . . ? C48 C49 C53 122.0(3) . . ? C51 C50 C49 124.2(3) . . ? C51 C50 H50A 117.9 . . ? C49 C50 H50A 117.9 . . ? C52 C51 C50 117.4(3) . . ? C52 C51 C57 122.1(4) . . ? C50 C51 C57 120.5(3) . . ? C51 C52 C47 121.8(3) . . ? C51 C52 H52A 119.1 . . ? C47 C52 H52A 119.1 . . ? C54 C53 C49 111.8(3) . . ? C54 C53 C56 109.5(4) . . ? C49 C53 C56 110.5(3) . . ? C54 C53 C55 107.0(3) . . ? C49 C53 C55 111.0(3) . . ? C56 C53 C55 106.9(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C63 C58 C59 118.6(2) . . ? C63 C58 C46 121.6(2) . . ? C59 C58 C46 119.6(2) . . ? O6 C59 C60 117.9(2) . . ? O6 C59 C58 120.9(2) . . ? C60 C59 C58 121.1(2) . . ? C61 C60 C59 117.2(2) . . ? C61 C60 C64 121.3(2) . . ? C59 C60 C64 121.5(2) . . ? C62 C61 C60 122.6(3) . . ? C62 C61 H61A 118.7 . . ? C60 C61 H61A 118.7 . . ? C61 C62 C63 118.9(2) . . ? C61 C62 C68 120.2(3) . . ? C63 C62 C68 120.9(3) . . ? C62 C63 C58 121.4(2) . . ? C62 C63 H63A 119.3 . . ? C58 C63 H63A 119.3 . . ? C66 C64 C67 110.8(2) . . ? C66 C64 C60 109.5(2) . . ? C67 C64 C60 110.5(2) . . ? C66 C64 C65 107.0(2) . . ? C67 C64 C65 107.3(3) . . ? C60 C64 C65 111.6(2) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C62 C68 H68A 109.5 . . ? C62 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C62 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C1A N3 C1D 111.9(3) . . ? C1A N3 C1C 110.4(3) . . ? C1D N3 C1C 112.0(3) . . ? C1A N3 C1B 104.5(2) . . ? C1D N3 C1B 111.7(3) . . ? C1C N3 C1B 105.9(3) . . ? C2A C1A N3 119.4(3) . . ? C2A C1A H1AA 107.5 . . ? N3 C1A H1AA 107.5 . . ? C2A C1A H1AB 107.5 . . ? N3 C1A H1AB 107.5 . . ? H1AA C1A H1AB 107.0 . . ? C2B C1B N3 116.5(2) . . ? C2B C1B H1BA 108.2 . . ? N3 C1B H1BA 108.2 . . ? C2B C1B H1BB 108.2 . . ? N3 C1B H1BB 108.2 . . ? H1BA C1B H1BB 107.3 . . ? C2C C1C N3 117.0(4) . . ? C2C C1C H1CA 108.0 . . ? N3 C1C H1CA 108.0 . . ? C2C C1C H1CB 108.0 . . ? N3 C1C H1CB 108.0 . . ? H1CA C1C H1CB 107.3 . . ? C2D C1D N3 116.5(3) . . ? C2D C1D H1DA 108.2 . . ? N3 C1D H1DA 108.2 . . ? C2D C1D H1DB 108.2 . . ? N3 C1D H1DB 108.2 . . ? H1DA C1D H1DB 107.3 . . ? C1A C2A C3A 110.6(3) . . ? C1A C2A H2AA 109.5 . . ? C3A C2A H2AA 109.5 . . ? C1A C2A H2AB 109.5 . . ? C3A C2A H2AB 109.5 . . ? H2AA C2A H2AB 108.1 . . ? C1B C2B C3B 109.1(3) . . ? C1B C2B H2BA 109.9 . . ? C3B C2B H2BA 109.9 . . ? C1B C2B H2BB 109.9 . . ? C3B C2B H2BB 109.9 . . ? H2BA C2B H2BB 108.3 . . ? C1C C2C C3C 114.7(6) . . ? C1C C2C H2CA 108.6 . . ? C3C C2C H2CA 108.6 . . ? C1C C2C H2CB 108.6 . . ? C3C C2C H2CB 108.6 . . ? H2CA C2C H2CB 107.6 . . ? C1D C2D C3D' 85.6(6) . . ? C1D C2D C3D 117.0(6) . . ? C3D' C2D C3D 41.9(5) . . ? C4A C3A C2A 118.8(3) . . ? C4A C3A H3AA 107.6 . . ? C2A C3A H3AA 107.6 . . ? C4A C3A H3AB 107.6 . . ? C2A C3A H3AB 107.6 . . ? H3AA C3A H3AB 107.0 . . ? C2B C3B C4B 112.0(3) . . ? C2B C3B H3BA 109.2 . . ? C4B C3B H3BA 109.2 . . ? C2B C3B H3BB 109.2 . . ? C4B C3B H3BB 109.2 . . ? H3BA C3B H3BB 107.9 . . ? C4C C3C C2C 111.1(6) . . ? C4C C3C H3CA 109.4 . . ? C2C C3C H3CA 109.4 . . ? C4C C3C H3CB 109.4 . . ? C2C C3C H3CB 109.4 . . ? H3CA C3C H3CB 108.0 . . ? C4D C3D C2D 106.2(10) . . ? C4D C3D H3DA 110.5 . . ? C2D C3D H3DA 110.5 . . ? C4D C3D H3DB 110.5 . . ? C2D C3D H3DB 110.5 . . ? H3DA C3D H3DB 108.7 . . ? C4D' C3D' C2D 94.0(10) . . ? C4D' C3D' H3DC 112.9 . . ? C2D C3D' H3DC 112.9 . . ? C4D' C3D' H3DD 112.9 . . ? C2D C3D' H3DD 112.9 . . ? H3DC C3D' H3DD 110.3 . . ? C3A C4A H4AA 109.5 . . ? C3A C4A H4AB 109.5 . . ? H4AA C4A H4AB 109.5 . . ? C3A C4A H4AC 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? C3B C4B H4BA 109.5 . . ? C3B C4B H4BB 109.5 . . ? H4BA C4B H4BB 109.5 . . ? C3B C4B H4BC 109.5 . . ? H4BA C4B H4BC 109.5 . . ? H4BB C4B H4BC 109.5 . . ? C3C C4C H4CA 109.5 . . ? C3C C4C H4CB 109.5 . . ? H4CA C4C H4CB 109.5 . . ? C3C C4C H4CC 109.5 . . ? H4CA C4C H4CC 109.5 . . ? H4CB C4C H4CC 109.5 . . ? C3D' C4D' H4DD 109.5 . . ? C3D' C4D' H4DE 109.5 . . ? H4DD C4D' H4DE 109.5 . . ? C3D' C4D' H4DF 109.5 . . ? H4DD C4D' H4DF 109.5 . . ? H4DE C4D' H4DF 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 F1 0.831(18) 1.78(3) 2.539(2) 151(4) . O3 H3 F1 0.853(18) 1.74(2) 2.509(2) 148(3) . O5 H5 F1 0.890(18) 2.34(2) 3.098(3) 143(3) . O6 H6 F1 0.836(17) 1.749(18) 2.573(2) 168(3) . _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.876 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.061 #===END