# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name Hosseini _publ_contact_author_email hosseini@unistra.fr loop_ _publ_author_name T.Lang E.Graf N.Kyritsakas M.W.Hosseini data_e1761a _database_code_depnum_ccdc_archive 'CCDC 894032' #TrackingRef '- New CIF for Compound2Zn.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C69 H65 N7 O11 Zn, 0.5(C H2 Cl2), 0.5(H2 O)' _chemical_formula_sum 'C138.50 H131 Cl N14 O23 Zn2' _chemical_formula_weight 2525.81 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' Zn Zn 0.2839 1.4301 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5277(4) _cell_length_b 15.3111(7) _cell_length_c 17.7296(5) _cell_angle_alpha 86.083(3) _cell_angle_beta 67.796(2) _cell_angle_gamma 77.863(3) _cell_volume 3323.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2596 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.00 _exptl_crystal_description needdle _exptl_crystal_colour purple _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1321 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9721 _exptl_absorpt_correction_T_max 0.9813 _exptl_absorpt_process_details sadabs _exptl_special_details ; Because of the flopiness of the ether chain some atoms had the same thermal parameters.Because of the flopiness of O5 the hydrogen atom on C42 were not introduced.Because of the flopiness of the ether chain we used many distance and angle restraints on the atoms of this chain ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34801 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.53 _reflns_number_total 14673 _reflns_number_gt 11540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1694P)^2^+3.2679P] 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 14673 _refine_ls_number_parameters 804 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2528 _refine_ls_wR_factor_gt 0.2357 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.015 _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 O13 O 0.3452(9) 0.0435(11) 0.4812(8) 0.126(5) Uani 0.50 1 d P . . Zn1 Zn 0.70585(3) 0.47066(3) 0.72823(2) 0.02149(15) Uani 1 1 d . . . N1 N 0.7513(2) 0.35005(19) 0.77874(17) 0.0243(6) Uani 1 1 d . . . C1 C 0.8512(3) 0.3152(2) 0.7826(2) 0.0243(7) Uani 1 1 d . . . C2 C 0.8458(3) 0.2341(3) 0.8291(2) 0.0311(8) Uani 1 1 d . . . H2 H 0.9039 0.1970 0.8408 0.037 Uiso 1 1 calc R . . C3 C 0.7432(3) 0.2207(3) 0.8530(2) 0.0315(8) Uani 1 1 d . . . H3 H 0.7153 0.1727 0.8851 0.038 Uiso 1 1 calc R . . C4 C 0.6837(3) 0.2926(2) 0.8209(2) 0.0256(7) Uani 1 1 d . . . C5 C 0.5751(3) 0.3017(2) 0.8296(2) 0.0260(7) Uani 1 1 d . . . C6 C 0.5191(3) 0.3666(2) 0.7930(2) 0.0260(7) Uani 1 1 d . . . C7 C 0.4088(3) 0.3707(3) 0.7977(2) 0.0314(8) Uani 1 1 d . . . H7 H 0.3607 0.3330 0.8286 0.038 Uiso 1 1 calc R . . C8 C 0.3878(3) 0.4385(3) 0.7494(2) 0.0329(8) Uani 1 1 d . . . H8 H 0.3218 0.4573 0.7401 0.040 Uiso 1 1 calc R . . C9 C 0.4837(3) 0.4770(2) 0.7145(2) 0.0267(7) Uani 1 1 d . . . N2 N 0.5619(2) 0.4332(2) 0.74280(17) 0.0252(6) Uani 1 1 d . . . C10 C 0.4955(3) 0.5471(2) 0.6590(2) 0.0269(7) Uani 1 1 d . . . C11 C 0.5881(3) 0.5860(2) 0.6256(2) 0.0263(7) Uani 1 1 d . . . C12 C 0.6019(3) 0.6550(3) 0.5640(2) 0.0319(8) Uani 1 1 d . . . H12 H 0.5509 0.6817 0.5401 0.038 Uiso 1 1 calc R . . C13 C 0.7006(3) 0.6736(3) 0.5474(2) 0.0310(8) Uani 1 1 d . . . H13 H 0.7321 0.7164 0.5096 0.037 Uiso 1 1 calc R . . C14 C 0.7503(3) 0.6171(2) 0.5972(2) 0.0252(7) Uani 1 1 d . . . N3 N 0.6803(2) 0.5641(2) 0.64394(17) 0.0240(6) Uani 1 1 d . . . C15 C 0.8564(3) 0.6128(2) 0.59354(19) 0.0227(7) Uani 1 1 d . . . C16 C 0.9121(3) 0.5472(2) 0.63047(19) 0.0226(7) Uani 1 1 d . . . C17 C 1.0248(3) 0.5382(3) 0.6210(2) 0.0271(7) Uani 1 1 d . . . H17 H 1.0722 0.5772 0.5920 0.032 Uiso 1 1 calc R . . C18 C 1.0498(3) 0.4641(3) 0.6612(2) 0.0277(7) Uani 1 1 d . . . H18 H 1.1186 0.4406 0.6650 0.033 Uiso 1 1 calc R . . C19 C 0.9530(3) 0.4272(2) 0.69725(19) 0.0232(7) Uani 1 1 d . . . N4 N 0.8696(2) 0.47960(19) 0.67827(16) 0.0215(6) Uani 1 1 d . . . C20 C 0.9458(3) 0.3499(2) 0.7447(2) 0.0234(7) Uani 1 1 d . . . C21 C 0.5152(3) 0.2316(2) 0.8784(2) 0.0268(7) Uani 1 1 d . . . C22 C 0.4419(4) 0.2503(3) 0.9576(3) 0.0475(12) Uani 1 1 d . . . H22 H 0.4297 0.3074 0.9813 0.057 Uiso 1 1 calc R . . C23 C 0.3861(4) 0.1853(3) 1.0028(3) 0.0525(13) Uani 1 1 d . . . H23 H 0.3361 0.1980 1.0572 0.063 Uiso 1 1 calc R . . C24 C 0.4035(3) 0.1030(3) 0.9685(2) 0.0342(9) Uani 1 1 d . . . C25 C 0.4730(4) 0.0850(3) 0.8886(3) 0.0447(11) Uani 1 1 d . . . H25 H 0.4830 0.0288 0.8643 0.054 Uiso 1 1 calc R . . C26 C 0.5280(4) 0.1499(3) 0.8443(3) 0.0445(11) Uani 1 1 d . . . H26 H 0.5757 0.1376 0.7893 0.053 Uiso 1 1 calc R . . C27 C 0.3463(4) 0.0362(3) 1.0159(3) 0.0447(11) Uani 1 1 d . . . N5 N 0.3015(4) -0.0162(3) 1.0548(3) 0.0668(14) Uani 1 1 d . . . C28 C 0.4043(3) 0.5830(3) 0.6304(2) 0.0282(7) Uani 1 1 d . . . C29 C 0.3481(3) 0.6703(3) 0.6498(2) 0.0322(8) Uani 1 1 d . . . H29 H 0.3649 0.7050 0.6841 0.039 Uiso 1 1 calc R . . C30 C 0.2680(3) 0.7076(3) 0.6199(3) 0.0339(8) Uani 1 1 d . . . C31 C 0.2422(3) 0.6590(3) 0.5702(3) 0.0373(9) Uani 1 1 d . . . H31 H 0.1878 0.6848 0.5492 0.045 Uiso 1 1 calc R . . C32 C 0.2979(3) 0.5703(3) 0.5511(2) 0.0375(9) Uani 1 1 d . . . H32 H 0.2809 0.5359 0.5167 0.045 Uiso 1 1 calc R . . C33 C 0.3774(3) 0.5320(3) 0.5816(2) 0.0329(8) Uani 1 1 d . . . H33 H 0.4133 0.4714 0.5692 0.039 Uiso 1 1 calc R . . O1 O 0.2207(2) 0.7953(2) 0.6431(2) 0.0476(8) Uani 1 1 d . . . C34 C 0.1336(4) 0.8368(4) 0.6188(4) 0.0558(13) Uani 1 1 d . . . H34A H 0.0743 0.8025 0.6392 0.067 Uiso 1 1 calc R . . H34B H 0.1591 0.8385 0.5586 0.067 Uiso 1 1 calc R . . C35 C 0.0929(5) 0.9294(4) 0.6533(4) 0.0605(14) Uani 1 1 d . . . H35A H 0.1539 0.9615 0.6382 0.073 Uiso 1 1 calc R . . H35B H 0.0383 0.9626 0.6317 0.073 Uiso 1 1 calc R . . O2 O 0.0448(3) 0.9229(2) 0.7393(2) 0.0527(8) Uani 1 1 d . . . C36 C -0.0001(4) 1.0069(3) 0.7782(4) 0.0574(13) Uani 1 1 d . . . H36A H -0.0655 1.0354 0.7665 0.069 Uiso 1 1 calc R . . H36B H 0.0537 1.0463 0.7584 0.069 Uiso 1 1 calc R . . C37 C -0.0303(4) 0.9921(3) 0.8683(4) 0.0594(14) Uani 1 1 d D . . H37A H -0.0727 1.0486 0.8980 0.071 Uiso 1 1 calc R . . H37B H -0.0772 0.9471 0.8859 0.071 Uiso 1 1 calc R . . O3 O 0.0629(3) 0.9625(2) 0.8890(3) 0.0638(10) Uani 1 1 d D . . C38 C 0.1015(8) 1.0436(7) 0.8949(9) 0.0799(16) Uani 0.621(8) 1 d PD B 1 H38A H 0.0469 1.0820 0.9407 0.096 Uiso 0.621(8) 1 calc PR B 1 H38B H 0.1141 1.0780 0.8439 0.096 Uiso 0.621(8) 1 calc PR B 1 C39 C 0.2041(7) 1.0143(7) 0.9088(7) 0.0799(16) Uani 0.621(8) 1 d PD B 1 H39A H 0.2180 1.0629 0.9351 0.096 Uiso 0.621(8) 1 calc PR B 1 H39B H 0.1997 0.9618 0.9449 0.096 Uiso 0.621(8) 1 calc PR B 1 O4 O 0.2908(6) 0.9912(5) 0.8305(5) 0.0799(16) Uani 0.621(8) 1 d PD B 1 C40 C 0.3101(7) 0.9034(7) 0.8015(7) 0.0799(16) Uani 0.621(8) 1 d PD B 1 H40A H 0.2459 0.8942 0.7912 0.096 Uiso 0.621(8) 1 calc PR B 1 H40B H 0.3209 0.8603 0.8433 0.096 Uiso 0.621(8) 1 calc PR B 1 C41 C 0.4141(8) 0.8861(9) 0.7204(7) 0.0799(16) Uani 0.621(8) 1 d PD B 1 H41A H 0.4209 0.8276 0.6964 0.096 Uiso 0.621(8) 1 calc PR B 1 H41B H 0.4069 0.9330 0.6805 0.096 Uiso 0.621(8) 1 calc PR B 1 O5 O 0.5115(6) 0.8868(5) 0.7378(6) 0.0799(16) Uani 0.621(8) 1 d PD B 1 C42 C 0.5546(4) 0.7955(4) 0.7643(4) 0.0675(16) Uani 1 1 d D . . C43 C 0.6568(4) 0.8047(3) 0.7729(3) 0.0452(11) Uani 1 1 d D B . C44 C 0.6922(5) 0.8871(3) 0.7600(3) 0.0592(15) Uani 1 1 d . . . H44 H 0.6497 0.9392 0.7470 0.071 Uiso 1 1 calc R B . C45 C 0.7899(5) 0.8900(4) 0.7667(3) 0.0570(13) Uani 1 1 d . B . H45 H 0.8158 0.9443 0.7587 0.068 Uiso 1 1 calc R . . C46 C 0.8473(5) 0.8146(3) 0.7847(3) 0.0522(12) Uani 1 1 d . . . H46 H 0.9142 0.8150 0.7904 0.063 Uiso 1 1 calc R B . C47 C 0.8083(3) 0.7359(3) 0.7951(2) 0.0359(9) Uani 1 1 d . B . N7 N 0.7141(3) 0.7303(2) 0.78942(19) 0.0346(7) Uani 1 1 d . . . C48 C 0.8726(4) 0.6504(3) 0.8143(2) 0.0417(10) Uani 1 1 d . . . H48A H 0.8912 0.6049 0.7715 0.050 Uiso 1 1 calc R B . H48B H 0.9412 0.6612 0.8163 0.050 Uiso 1 1 calc R . . O6 O 0.8082(2) 0.61931(19) 0.89125(16) 0.0370(6) Uani 1 1 d . B . C49 C 0.8624(4) 0.5342(3) 0.9083(3) 0.0443(10) Uani 1 1 d . . . H49A H 0.9303 0.5400 0.9147 0.053 Uiso 1 1 calc R B . H49B H 0.8818 0.4921 0.8626 0.053 Uiso 1 1 calc R . . C50 C 0.7885(4) 0.4994(3) 0.9847(3) 0.0475(11) Uani 1 1 d . B . H50A H 0.8283 0.4447 1.0017 0.057 Uiso 1 1 calc R . . H50B H 0.7618 0.5447 1.0289 0.057 Uiso 1 1 calc R . . O7 O 0.6991(3) 0.4798(2) 0.9699(2) 0.0538(9) Uani 1 1 d . . . C51 C 0.6220(4) 0.4448(4) 1.0384(3) 0.0589(14) Uani 1 1 d . B . H51A H 0.5524 0.4529 1.0300 0.071 Uiso 1 1 calc R . . H51B H 0.6082 0.4797 1.0876 0.071 Uiso 1 1 calc R . . C52 C 0.6576(5) 0.3487(4) 1.0532(4) 0.0625(14) Uani 1 1 d . . . H52A H 0.5953 0.3264 1.0943 0.075 Uiso 1 1 calc R B . H52B H 0.6803 0.3143 1.0021 0.075 Uiso 1 1 calc R . . O8 O 0.7426(4) 0.3342(5) 1.0802(4) 0.0625(14) Uani 1 1 d D B . C53 C 0.7830(6) 0.2726(7) 1.1157(6) 0.0625(14) Uani 1 1 d D . . H53A H 0.8077 0.2195 1.0796 0.075 Uiso 1 1 calc R B . H53B H 0.7220 0.2598 1.1648 0.075 Uiso 1 1 calc R . . C54 C 0.8676(6) 0.2752(7) 1.1413(6) 0.0625(14) Uani 1 1 d . B . H54A H 0.8976 0.2134 1.1533 0.075 Uiso 1 1 calc R . . H54B H 0.8371 0.3100 1.1929 0.075 Uiso 1 1 calc R . . O9 O 0.9552(3) 0.3127(2) 1.0851(2) 0.0518(8) Uani 1 1 d . . . C55 C 1.0238(4) 0.2559(3) 1.0197(3) 0.0471(11) Uani 1 1 d . B . H55A H 0.9830 0.2430 0.9872 0.057 Uiso 1 1 calc R . . H55B H 1.0546 0.1988 1.0397 0.057 Uiso 1 1 calc R . . C56 C 1.1136(4) 0.3032(3) 0.9686(3) 0.0426(10) Uani 1 1 d . . . H56A H 1.0811 0.3613 0.9511 0.051 Uiso 1 1 calc R B . H56B H 1.1535 0.3155 1.0021 0.051 Uiso 1 1 calc R . . O10 O 1.1888(2) 0.2522(2) 0.89801(18) 0.0440(7) Uani 1 1 d . B . C57 C 1.1637(3) 0.2554(3) 0.8297(2) 0.0325(8) Uani 1 1 d . . . C58 C 1.0659(3) 0.3009(3) 0.8245(2) 0.0287(8) Uani 1 1 d . B . H58 H 1.0108 0.3331 0.8704 0.034 Uiso 1 1 calc R . . C59 C 1.0491(3) 0.2992(2) 0.7516(2) 0.0249(7) Uani 1 1 d . . . C60 C 1.1294(3) 0.2518(3) 0.6855(2) 0.0377(9) Uani 1 1 d . B . H60 H 1.1180 0.2498 0.6360 0.045 Uiso 1 1 calc R . . C61 C 1.2268(3) 0.2068(3) 0.6913(3) 0.0455(11) Uani 1 1 d . . . H61 H 1.2817 0.1743 0.6455 0.055 Uiso 1 1 calc R B . C62 C 1.2446(3) 0.2090(3) 0.7627(3) 0.0411(10) Uani 1 1 d . B . H62 H 1.3119 0.1789 0.7660 0.049 Uiso 1 1 calc R . . C63 C 0.9162(3) 0.6825(2) 0.5448(2) 0.0243(7) Uani 1 1 d . . . C64 C 1.0128(3) 0.6596(2) 0.4777(2) 0.0251(7) Uani 1 1 d . B . H64 H 1.0402 0.5986 0.4614 0.030 Uiso 1 1 calc R . . C65 C 1.0701(3) 0.7235(3) 0.4341(2) 0.0287(8) Uani 1 1 d . . . H65 H 1.1363 0.7067 0.3886 0.034 Uiso 1 1 calc R B . C66 C 1.0293(3) 0.8126(3) 0.4577(2) 0.0312(8) Uani 1 1 d . B . C67 C 0.9320(3) 0.8377(3) 0.5239(3) 0.0371(9) Uani 1 1 d . . . H67 H 0.9043 0.8988 0.5398 0.044 Uiso 1 1 calc R B . C68 C 0.8762(3) 0.7722(3) 0.5665(2) 0.0329(8) Uani 1 1 d . B . H68 H 0.8093 0.7891 0.6112 0.039 Uiso 1 1 calc R . . C69 C 1.0897(4) 0.8802(3) 0.4148(3) 0.0419(10) Uani 1 1 d . . . N6 N 1.1370(4) 0.9341(3) 0.3820(3) 0.0620(13) Uani 1 1 d . B . O11 O 0.6509(2) 0.55726(18) 0.83048(15) 0.0303(6) Uani 1 1 d D . . H11 H 0.6450 0.5268 0.8727 0.046 Uiso 1 1 calc RD B 4 Cl2 Cl 0.4573(15) -0.2395(17) 0.4005(9) 0.278(11) Uani 0.25 1 d PD . . Cl1 Cl 0.3900(14) -0.0781(18) 0.4461(9) 0.278(11) Uani 0.25 1 d PD . . C71 C 0.360(4) -0.156(2) 0.394(3) 0.278(11) Uani 0.25 1 d PD . . H71A H 0.2861 -0.1686 0.4221 0.333 Uiso 0.25 1 calc PR . . H71B H 0.3711 -0.1390 0.3365 0.333 Uiso 0.25 1 calc PR . . C38A C 0.1329(10) 1.0206(11) 0.9010(10) 0.078(2) Uani 0.379(8) 1 d PD B 2 H38C H 0.1141 1.0307 0.9597 0.094 Uiso 0.379(8) 1 calc PR B 2 H38D H 0.1221 1.0792 0.8749 0.094 Uiso 0.379(8) 1 calc PR B 2 C39A C 0.2572(14) 0.9680(14) 0.8592(8) 0.078(2) Uani 0.379(8) 1 d PD B 2 H39C H 0.3091 0.9966 0.8709 0.094 Uiso 0.379(8) 1 calc PR B 2 H39D H 0.2671 0.9041 0.8741 0.094 Uiso 0.379(8) 1 calc PR B 2 O4A O 0.2639(9) 0.9823(8) 0.7677(6) 0.078(2) Uani 0.379(8) 1 d PD B 2 O5A O 0.4756(10) 0.8693(9) 0.7695(8) 0.078(2) Uani 0.379(8) 1 d PD B 2 C40A C 0.3695(12) 0.9743(10) 0.7065(9) 0.078(2) Uani 0.379(8) 1 d PD B 2 H40C H 0.4083 1.0157 0.7194 0.094 Uiso 0.379(8) 1 calc PR B 2 H40D H 0.3629 0.9922 0.6536 0.094 Uiso 0.379(8) 1 calc PR B 2 C41A C 0.4368(15) 0.8788(13) 0.6987(10) 0.078(2) Uani 0.379(8) 1 d PD B 2 H41C H 0.3914 0.8345 0.7025 0.094 Uiso 0.379(8) 1 calc PR B 2 H41D H 0.4995 0.8701 0.6460 0.094 Uiso 0.379(8) 1 calc PR B 2 H11A H 0.658(4) 0.6112(15) 0.825(2) 0.039 Uiso 1 1 d D C 4 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 O13 0.066(6) 0.177(13) 0.120(10) 0.021(9) -0.034(7) 0.002(7) Zn1 0.0178(2) 0.0220(2) 0.0245(2) 0.00437(15) -0.00746(15) -0.00566(15) N1 0.0223(13) 0.0220(15) 0.0287(14) 0.0043(11) -0.0094(11) -0.0060(11) C1 0.0228(16) 0.0231(18) 0.0258(15) 0.0022(13) -0.0088(13) -0.0033(13) C2 0.0309(18) 0.0259(19) 0.0365(18) 0.0079(15) -0.0136(15) -0.0062(15) C3 0.0310(18) 0.0250(19) 0.0392(19) 0.0105(15) -0.0139(15) -0.0090(15) C4 0.0244(16) 0.0237(18) 0.0266(15) 0.0039(13) -0.0071(13) -0.0062(13) C5 0.0252(16) 0.0254(18) 0.0274(16) 0.0026(13) -0.0072(13) -0.0106(14) C6 0.0225(16) 0.0249(18) 0.0307(16) 0.0011(14) -0.0085(13) -0.0083(14) C7 0.0230(16) 0.032(2) 0.0400(19) 0.0061(15) -0.0108(15) -0.0121(15) C8 0.0223(17) 0.039(2) 0.042(2) 0.0060(16) -0.0143(15) -0.0114(15) C9 0.0235(16) 0.0257(18) 0.0319(17) 0.0005(14) -0.0111(14) -0.0056(14) N2 0.0226(13) 0.0251(16) 0.0293(14) 0.0037(11) -0.0106(11) -0.0070(12) C10 0.0222(16) 0.0262(19) 0.0319(17) 0.0002(14) -0.0107(13) -0.0027(14) C11 0.0239(16) 0.0267(19) 0.0302(16) 0.0035(14) -0.0123(13) -0.0056(14) C12 0.0293(18) 0.036(2) 0.0333(18) 0.0099(15) -0.0160(15) -0.0066(15) C13 0.0283(17) 0.034(2) 0.0327(17) 0.0125(15) -0.0130(15) -0.0099(15) C14 0.0237(16) 0.0250(18) 0.0251(15) 0.0032(13) -0.0074(13) -0.0054(13) N3 0.0206(13) 0.0245(15) 0.0282(14) 0.0034(11) -0.0101(11) -0.0066(11) C15 0.0236(15) 0.0224(17) 0.0220(14) 0.0022(12) -0.0072(12) -0.0075(13) C16 0.0206(15) 0.0239(17) 0.0234(15) 0.0020(13) -0.0069(12) -0.0075(13) C17 0.0215(16) 0.032(2) 0.0288(16) 0.0078(14) -0.0093(13) -0.0109(14) C18 0.0194(15) 0.034(2) 0.0315(17) 0.0048(14) -0.0101(13) -0.0083(14) C19 0.0206(15) 0.0268(18) 0.0231(14) 0.0015(13) -0.0087(12) -0.0060(13) N4 0.0174(12) 0.0218(15) 0.0245(13) 0.0031(11) -0.0073(10) -0.0043(11) C20 0.0218(15) 0.0236(18) 0.0252(15) 0.0021(13) -0.0098(12) -0.0042(13) C21 0.0238(16) 0.0276(19) 0.0303(17) 0.0064(14) -0.0099(14) -0.0098(14) C22 0.063(3) 0.039(2) 0.033(2) -0.0030(17) 0.000(2) -0.025(2) C23 0.065(3) 0.048(3) 0.033(2) 0.0050(19) 0.004(2) -0.028(2) C24 0.0265(17) 0.036(2) 0.041(2) 0.0157(17) -0.0128(15) -0.0132(16) C25 0.050(2) 0.033(2) 0.046(2) 0.0004(18) -0.006(2) -0.021(2) C26 0.051(2) 0.036(2) 0.037(2) -0.0031(17) 0.0019(18) -0.020(2) C27 0.036(2) 0.041(3) 0.058(3) 0.019(2) -0.0169(19) -0.0167(19) N5 0.053(2) 0.058(3) 0.083(3) 0.034(2) -0.016(2) -0.028(2) C28 0.0222(16) 0.033(2) 0.0322(17) 0.0063(14) -0.0130(14) -0.0074(14) C29 0.0277(18) 0.032(2) 0.042(2) -0.0004(16) -0.0186(16) -0.0059(15) C30 0.0246(17) 0.032(2) 0.046(2) 0.0025(16) -0.0150(16) -0.0040(15) C31 0.0254(18) 0.046(2) 0.045(2) 0.0068(18) -0.0189(16) -0.0074(17) C32 0.0278(18) 0.050(3) 0.041(2) -0.0040(18) -0.0169(16) -0.0104(17) C33 0.0249(17) 0.032(2) 0.041(2) -0.0026(16) -0.0118(15) -0.0051(15) O1 0.0379(16) 0.0332(17) 0.078(2) -0.0024(15) -0.0343(16) 0.0035(13) C34 0.041(2) 0.055(3) 0.072(3) 0.003(2) -0.032(2) 0.010(2) C35 0.053(3) 0.045(3) 0.077(4) 0.002(3) -0.030(3) 0.014(2) O2 0.0439(17) 0.0326(17) 0.076(2) 0.0024(15) -0.0195(17) -0.0011(14) C36 0.044(3) 0.036(3) 0.082(4) 0.000(2) -0.016(2) 0.000(2) C37 0.043(3) 0.032(3) 0.086(4) 0.002(2) -0.010(2) 0.000(2) O3 0.064(2) 0.047(2) 0.076(3) -0.0036(18) -0.018(2) -0.0146(18) C38 0.068(2) 0.063(2) 0.126(4) 0.008(2) -0.051(2) -0.0218(19) C39 0.068(2) 0.063(2) 0.126(4) 0.008(2) -0.051(2) -0.0218(19) O4 0.068(2) 0.063(2) 0.126(4) 0.008(2) -0.051(2) -0.0218(19) C40 0.068(2) 0.063(2) 0.126(4) 0.008(2) -0.051(2) -0.0218(19) C41 0.068(2) 0.063(2) 0.126(4) 0.008(2) -0.051(2) -0.0218(19) O5 0.068(2) 0.063(2) 0.126(4) 0.008(2) -0.051(2) -0.0218(19) C42 0.052(3) 0.067(4) 0.073(4) 0.013(3) -0.019(3) -0.002(3) C43 0.045(2) 0.043(3) 0.0327(19) -0.0003(18) -0.0029(18) 0.0004(19) C44 0.085(4) 0.029(2) 0.038(2) 0.0013(18) -0.004(2) 0.006(2) C45 0.066(3) 0.048(3) 0.055(3) 0.004(2) -0.014(3) -0.027(3) C46 0.063(3) 0.049(3) 0.044(2) 0.004(2) -0.010(2) -0.029(2) C47 0.040(2) 0.037(2) 0.0275(17) -0.0015(15) -0.0046(15) -0.0168(18) N7 0.0369(17) 0.0325(18) 0.0304(15) 0.0013(13) -0.0073(13) -0.0088(14) C48 0.040(2) 0.055(3) 0.0311(19) -0.0021(18) -0.0110(17) -0.013(2) O6 0.0400(15) 0.0383(16) 0.0302(13) -0.0010(11) -0.0103(11) -0.0075(12) C49 0.051(3) 0.036(2) 0.046(2) -0.0013(18) -0.020(2) -0.003(2) C50 0.062(3) 0.045(3) 0.047(2) 0.009(2) -0.033(2) -0.016(2) O7 0.068(2) 0.059(2) 0.0513(18) 0.0216(16) -0.0359(17) -0.0288(18) C51 0.048(3) 0.070(4) 0.055(3) 0.018(3) -0.019(2) -0.011(2) C52 0.062(3) 0.065(4) 0.059(3) 0.016(3) -0.016(3) -0.026(3) O8 0.062(3) 0.065(4) 0.059(3) 0.016(3) -0.016(3) -0.026(3) C53 0.062(3) 0.065(4) 0.059(3) 0.016(3) -0.016(3) -0.026(3) C54 0.062(3) 0.065(4) 0.059(3) 0.016(3) -0.016(3) -0.026(3) O9 0.0526(19) 0.056(2) 0.0455(17) -0.0007(15) -0.0177(15) -0.0092(16) C55 0.064(3) 0.044(3) 0.037(2) 0.0046(18) -0.022(2) -0.014(2) C56 0.051(2) 0.049(3) 0.040(2) 0.0046(19) -0.0285(19) -0.014(2) O10 0.0393(16) 0.057(2) 0.0420(15) 0.0043(14) -0.0266(13) -0.0036(14) C57 0.0286(18) 0.038(2) 0.0358(18) 0.0088(16) -0.0184(15) -0.0082(16) C58 0.0254(16) 0.030(2) 0.0296(16) 0.0050(14) -0.0098(14) -0.0044(14) C59 0.0216(15) 0.0233(18) 0.0308(16) 0.0045(13) -0.0115(13) -0.0041(13) C60 0.0302(19) 0.049(3) 0.0319(18) -0.0003(17) -0.0127(15) -0.0014(17) C61 0.029(2) 0.060(3) 0.039(2) -0.007(2) -0.0115(17) 0.0087(19) C62 0.0242(18) 0.049(3) 0.049(2) 0.0042(19) -0.0168(17) 0.0020(17) C63 0.0240(16) 0.0269(19) 0.0249(15) 0.0048(13) -0.0112(13) -0.0088(14) C64 0.0282(17) 0.0252(18) 0.0236(15) 0.0022(13) -0.0106(13) -0.0078(14) C65 0.0258(17) 0.036(2) 0.0249(15) 0.0060(14) -0.0088(13) -0.0115(15) C66 0.0339(19) 0.031(2) 0.0364(18) 0.0152(16) -0.0201(16) -0.0152(16) C67 0.040(2) 0.0221(19) 0.048(2) 0.0049(16) -0.0158(18) -0.0062(16) C68 0.0300(18) 0.027(2) 0.0361(19) 0.0016(15) -0.0072(15) -0.0046(15) C69 0.040(2) 0.037(2) 0.056(2) 0.023(2) -0.025(2) -0.0167(19) N6 0.055(3) 0.049(3) 0.089(3) 0.035(2) -0.031(2) -0.028(2) O11 0.0321(13) 0.0287(14) 0.0301(12) 0.0024(10) -0.0101(11) -0.0092(11) Cl2 0.207(13) 0.58(3) 0.120(7) 0.031(12) -0.057(8) -0.253(19) Cl1 0.207(13) 0.58(3) 0.120(7) 0.031(12) -0.057(8) -0.253(19) C71 0.207(13) 0.58(3) 0.120(7) 0.031(12) -0.057(8) -0.253(19) C38A 0.081(5) 0.072(5) 0.078(4) -0.004(3) -0.031(3) -0.002(3) C39A 0.081(5) 0.072(5) 0.078(4) -0.004(3) -0.031(3) -0.002(3) O4A 0.081(5) 0.072(5) 0.078(4) -0.004(3) -0.031(3) -0.002(3) O5A 0.081(5) 0.072(5) 0.078(4) -0.004(3) -0.031(3) -0.002(3) C40A 0.081(5) 0.072(5) 0.078(4) -0.004(3) -0.031(3) -0.002(3) C41A 0.081(5) 0.072(5) 0.078(4) -0.004(3) -0.031(3) -0.002(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 Zn1 N2 2.063(3) . ? Zn1 N3 2.071(3) . ? Zn1 N1 2.074(3) . ? Zn1 N4 2.083(3) . ? Zn1 O11 2.120(3) . ? N1 C1 1.371(4) . ? N1 C4 1.379(4) . ? C1 C20 1.399(5) . ? C1 C2 1.443(5) . ? C2 C3 1.346(5) . ? C2 H2 0.9500 . ? C3 C4 1.439(5) . ? C3 H3 0.9500 . ? C4 C5 1.396(5) . ? C5 C6 1.396(5) . ? C5 C21 1.505(5) . ? C6 N2 1.378(4) . ? C6 C7 1.452(5) . ? C7 C8 1.353(6) . ? C7 H7 0.9500 . ? C8 C9 1.443(5) . ? C8 H8 0.9500 . ? C9 N2 1.370(5) . ? C9 C10 1.398(5) . ? C10 C11 1.407(5) . ? C10 C28 1.493(5) . ? C11 N3 1.375(4) . ? C11 C12 1.455(5) . ? C12 C13 1.342(5) . ? C12 H12 0.9500 . ? C13 C14 1.441(5) . ? C13 H13 0.9500 . ? C14 N3 1.371(4) . ? C14 C15 1.400(5) . ? C15 C16 1.404(5) . ? C15 C63 1.501(4) . ? C16 N4 1.373(4) . ? C16 C17 1.446(5) . ? C17 C18 1.350(5) . ? C17 H17 0.9500 . ? C18 C19 1.439(5) . ? C18 H18 0.9500 . ? C19 N4 1.378(4) . ? C19 C20 1.403(5) . ? C20 C59 1.494(5) . ? C21 C26 1.376(6) . ? C21 C22 1.386(5) . ? C22 C23 1.398(6) . ? C22 H22 0.9500 . ? C23 C24 1.373(7) . ? C23 H23 0.9500 . ? C24 C25 1.379(6) . ? C24 C27 1.440(5) . ? C25 C26 1.385(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 N5 1.140(6) . ? C28 C29 1.386(6) . ? C28 C33 1.394(6) . ? C29 C30 1.384(5) . ? C29 H29 0.9500 . ? C30 C31 1.372(6) . ? C30 O1 1.377(5) . ? C31 C32 1.402(6) . ? C31 H31 0.9500 . ? C32 C33 1.387(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? O1 C34 1.418(5) . ? C34 C35 1.491(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O2 1.420(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? O2 C36 1.405(6) . ? C36 C37 1.506(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O3 1.420(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O3 C38 1.468(10) . ? O3 C38A 1.504(14) . ? C38 C39 1.473(11) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O4 1.446(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? O4 C40 1.410(11) . ? C40 C41 1.577(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O5 1.465(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O5 C42 1.512(9) . ? C42 O5A 1.363(11) . ? C42 C43 1.484(8) . ? C43 N7 1.319(5) . ? C43 C44 1.415(7) . ? C44 C45 1.380(8) . ? C44 H44 0.9500 . ? C45 C46 1.342(8) . ? C45 H45 0.9500 . ? C46 C47 1.388(6) . ? C46 H46 0.9500 . ? C47 N7 1.336(5) . ? C47 C48 1.507(6) . ? C48 O6 1.425(5) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? O6 C49 1.428(5) . ? C49 C50 1.489(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O7 1.424(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? O7 C51 1.428(6) . ? C51 C52 1.487(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O8 1.376(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? O8 C53 1.244(8) . ? C53 C54 1.389(11) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O9 1.430(8) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? O9 C55 1.395(6) . ? C55 C56 1.506(6) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 O10 1.431(6) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? O10 C57 1.372(5) . ? C57 C62 1.385(6) . ? C57 C58 1.392(5) . ? C58 C59 1.398(5) . ? C58 H58 0.9500 . ? C59 C60 1.379(5) . ? C60 C61 1.390(6) . ? C60 H60 0.9500 . ? C61 C62 1.381(6) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C68 1.388(5) . ? C63 C64 1.391(5) . ? C64 C65 1.385(5) . ? C64 H64 0.9500 . ? C65 C66 1.388(6) . ? C65 H65 0.9500 . ? C66 C67 1.392(6) . ? C66 C69 1.448(5) . ? C67 C68 1.389(5) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 N6 1.142(6) . ? O11 H11 0.8400 . ? O11 H11A 0.847(17) . ? Cl2 C71 1.66(2) . ? Cl1 C71 1.76(2) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C38A C39A 1.611(16) . ? C38A H38C 0.9900 . ? C38A H38D 0.9900 . ? C39A O4A 1.593(15) . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? O4A C40A 1.416(14) . ? O5A C41A 1.521(15) . ? C40A C41A 1.536(16) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N3 89.05(11) . . ? N2 Zn1 N1 88.52(12) . . ? N3 Zn1 N1 160.97(12) . . ? N2 Zn1 N4 160.02(12) . . ? N3 Zn1 N4 87.67(11) . . ? N1 Zn1 N4 88.19(11) . . ? N2 Zn1 O11 99.91(11) . . ? N3 Zn1 O11 98.53(11) . . ? N1 Zn1 O11 100.49(11) . . ? N4 Zn1 O11 100.08(11) . . ? C1 N1 C4 106.5(3) . . ? C1 N1 Zn1 127.1(2) . . ? C4 N1 Zn1 126.2(2) . . ? N1 C1 C20 125.9(3) . . ? N1 C1 C2 109.4(3) . . ? C20 C1 C2 124.6(3) . . ? C3 C2 C1 107.4(3) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 107.2(3) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 125.2(3) . . ? N1 C4 C3 109.5(3) . . ? C5 C4 C3 125.3(3) . . ? C4 C5 C6 125.8(3) . . ? C4 C5 C21 116.9(3) . . ? C6 C5 C21 117.1(3) . . ? N2 C6 C5 125.6(3) . . ? N2 C6 C7 109.4(3) . . ? C5 C6 C7 124.9(3) . . ? C8 C7 C6 106.7(3) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C7 C8 C9 107.6(3) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? N2 C9 C10 125.5(3) . . ? N2 C9 C8 109.6(3) . . ? C10 C9 C8 125.0(3) . . ? C9 N2 C6 106.7(3) . . ? C9 N2 Zn1 126.8(2) . . ? C6 N2 Zn1 125.8(2) . . ? C9 C10 C11 125.4(3) . . ? C9 C10 C28 118.2(3) . . ? C11 C10 C28 116.4(3) . . ? N3 C11 C10 126.1(3) . . ? N3 C11 C12 109.1(3) . . ? C10 C11 C12 124.7(3) . . ? C13 C12 C11 106.8(3) . . ? C13 C12 H12 126.6 . . ? C11 C12 H12 126.6 . . ? C12 C13 C14 107.9(3) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? N3 C14 C15 125.6(3) . . ? N3 C14 C13 109.3(3) . . ? C15 C14 C13 125.0(3) . . ? C14 N3 C11 106.9(3) . . ? C14 N3 Zn1 127.0(2) . . ? C11 N3 Zn1 126.1(2) . . ? C14 C15 C16 125.2(3) . . ? C14 C15 C63 117.5(3) . . ? C16 C15 C63 117.4(3) . . ? N4 C16 C15 125.3(3) . . ? N4 C16 C17 109.5(3) . . ? C15 C16 C17 125.2(3) . . ? C18 C17 C16 107.1(3) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 107.3(3) . . ? C17 C18 H18 126.4 . . ? C19 C18 H18 126.4 . . ? N4 C19 C20 125.8(3) . . ? N4 C19 C18 109.6(3) . . ? C20 C19 C18 124.6(3) . . ? C16 N4 C19 106.4(3) . . ? C16 N4 Zn1 126.3(2) . . ? C19 N4 Zn1 126.5(2) . . ? C1 C20 C19 125.2(3) . . ? C1 C20 C59 118.1(3) . . ? C19 C20 C59 116.6(3) . . ? C26 C21 C22 118.9(3) . . ? C26 C21 C5 121.0(3) . . ? C22 C21 C5 120.1(3) . . ? C21 C22 C23 120.0(4) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.0(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.3(4) . . ? C23 C24 C27 119.4(4) . . ? C25 C24 C27 120.2(4) . . ? C24 C25 C26 119.3(4) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C21 C26 C25 121.4(4) . . ? C21 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? N5 C27 C24 178.6(6) . . ? C29 C28 C33 119.1(3) . . ? C29 C28 C10 119.4(3) . . ? C33 C28 C10 121.4(3) . . ? C30 C29 C28 121.0(4) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 O1 124.8(4) . . ? C31 C30 C29 120.7(4) . . ? O1 C30 C29 114.4(4) . . ? C30 C31 C32 118.6(4) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? C33 C32 C31 121.1(4) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C28 119.5(4) . . ? C32 C33 H33 120.2 . . ? C28 C33 H33 120.2 . . ? C30 O1 C34 117.8(4) . . ? O1 C34 C35 108.3(4) . . ? O1 C34 H34A 110.0 . . ? C35 C34 H34A 110.0 . . ? O1 C34 H34B 110.0 . . ? C35 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? O2 C35 C34 107.7(4) . . ? O2 C35 H35A 110.2 . . ? C34 C35 H35A 110.2 . . ? O2 C35 H35B 110.2 . . ? C34 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? C36 O2 C35 112.5(4) . . ? O2 C36 C37 107.4(4) . . ? O2 C36 H36A 110.2 . . ? C37 C36 H36A 110.2 . . ? O2 C36 H36B 110.2 . . ? C37 C36 H36B 110.2 . . ? H36A C36 H36B 108.5 . . ? O3 C37 C36 112.0(4) . . ? O3 C37 H37A 109.2 . . ? C36 C37 H37A 109.2 . . ? O3 C37 H37B 109.2 . . ? C36 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C37 O3 C38 105.7(5) . . ? C37 O3 C38A 126.2(7) . . ? O3 C38 C39 106.9(8) . . ? O3 C38 H38A 110.3 . . ? C39 C38 H38A 110.3 . . ? O3 C38 H38B 110.3 . . ? C39 C38 H38B 110.3 . . ? H38A C38 H38B 108.6 . . ? O4 C39 C38 107.7(9) . . ? O4 C39 H39A 110.2 . . ? C38 C39 H39A 110.2 . . ? O4 C39 H39B 110.2 . . ? C38 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? C40 O4 C39 116.8(8) . . ? O4 C40 C41 110.4(8) . . ? O4 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? O4 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? O5 C41 C40 109.7(9) . . ? O5 C41 H41A 109.7 . . ? C40 C41 H41A 109.7 . . ? O5 C41 H41B 109.7 . . ? C40 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? C41 O5 C42 110.7(7) . . ? O5A C42 C43 120.0(8) . . ? C43 C42 O5 104.5(5) . . ? N7 C43 C44 122.9(5) . . ? N7 C43 C42 115.3(4) . . ? C44 C43 C42 121.7(5) . . ? C45 C44 C43 118.5(5) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C46 C45 C44 118.5(5) . . ? C46 C45 H45 120.7 . . ? C44 C45 H45 120.7 . . ? C45 C46 C47 119.7(5) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? N7 C47 C46 123.7(4) . . ? N7 C47 C48 116.1(4) . . ? C46 C47 C48 120.3(4) . . ? C43 N7 C47 116.7(4) . . ? O6 C48 C47 108.6(3) . . ? O6 C48 H48A 110.0 . . ? C47 C48 H48A 110.0 . . ? O6 C48 H48B 110.0 . . ? C47 C48 H48B 110.0 . . ? H48A C48 H48B 108.3 . . ? C48 O6 C49 110.3(3) . . ? O6 C49 C50 109.0(4) . . ? O6 C49 H49A 109.9 . . ? C50 C49 H49A 109.9 . . ? O6 C49 H49B 109.9 . . ? C50 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? O7 C50 C49 108.5(4) . . ? O7 C50 H50A 110.0 . . ? C49 C50 H50A 110.0 . . ? O7 C50 H50B 110.0 . . ? C49 C50 H50B 110.0 . . ? H50A C50 H50B 108.4 . . ? C50 O7 C51 114.3(4) . . ? O7 C51 C52 113.9(4) . . ? O7 C51 H51A 108.8 . . ? C52 C51 H51A 108.8 . . ? O7 C51 H51B 108.8 . . ? C52 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? O8 C52 C51 112.3(5) . . ? O8 C52 H52A 109.2 . . ? C51 C52 H52A 109.2 . . ? O8 C52 H52B 109.2 . . ? C51 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? C53 O8 C52 135.3(7) . . ? O8 C53 C54 125.0(9) . . ? O8 C53 H53A 106.1 . . ? C54 C53 H53A 106.1 . . ? O8 C53 H53B 106.1 . . ? C54 C53 H53B 106.1 . . ? H53A C53 H53B 106.3 . . ? C53 C54 O9 115.7(7) . . ? C53 C54 H54A 108.4 . . ? O9 C54 H54A 108.4 . . ? C53 C54 H54B 108.4 . . ? O9 C54 H54B 108.4 . . ? H54A C54 H54B 107.4 . . ? C55 O9 C54 113.5(6) . . ? O9 C55 C56 107.0(4) . . ? O9 C55 H55A 110.3 . . ? C56 C55 H55A 110.3 . . ? O9 C55 H55B 110.3 . . ? C56 C55 H55B 110.3 . . ? H55A C55 H55B 108.6 . . ? O10 C56 C55 112.5(4) . . ? O10 C56 H56A 109.1 . . ? C55 C56 H56A 109.1 . . ? O10 C56 H56B 109.1 . . ? C55 C56 H56B 109.1 . . ? H56A C56 H56B 107.8 . . ? C57 O10 C56 119.0(3) . . ? O10 C57 C62 114.8(3) . . ? O10 C57 C58 124.8(4) . . ? C62 C57 C58 120.3(4) . . ? C57 C58 C59 119.8(3) . . ? C57 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? C60 C59 C58 119.6(3) . . ? C60 C59 C20 120.2(3) . . ? C58 C59 C20 120.2(3) . . ? C59 C60 C61 120.1(4) . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C62 C61 C60 120.7(4) . . ? C62 C61 H61 119.6 . . ? C60 C61 H61 119.6 . . ? C61 C62 C57 119.4(4) . . ? C61 C62 H62 120.3 . . ? C57 C62 H62 120.3 . . ? C68 C63 C64 118.4(3) . . ? C68 C63 C15 120.2(3) . . ? C64 C63 C15 121.4(3) . . ? C65 C64 C63 121.6(3) . . ? C65 C64 H64 119.2 . . ? C63 C64 H64 119.2 . . ? C64 C65 C66 119.0(3) . . ? C64 C65 H65 120.5 . . ? C66 C65 H65 120.5 . . ? C65 C66 C67 120.7(3) . . ? C65 C66 C69 119.9(4) . . ? C67 C66 C69 119.3(4) . . ? C68 C67 C66 119.1(4) . . ? C68 C67 H67 120.5 . . ? C66 C67 H67 120.5 . . ? C63 C68 C67 121.3(3) . . ? C63 C68 H68 119.4 . . ? C67 C68 H68 119.4 . . ? N6 C69 C66 179.1(6) . . ? Zn1 O11 H11A 122(3) . . ? H11 O11 H11A 125.1 . . ? Cl2 C71 Cl1 94.8(14) . . ? Cl2 C71 H71A 112.8 . . ? Cl1 C71 H71A 112.8 . . ? Cl2 C71 H71B 112.8 . . ? Cl1 C71 H71B 112.8 . . ? H71A C71 H71B 110.2 . . ? O3 C38A C39A 106.4(12) . . ? O3 C38A H38C 110.4 . . ? C39A C38A H38C 110.4 . . ? O3 C38A H38D 110.4 . . ? C39A C38A H38D 110.4 . . ? H38C C38A H38D 108.6 . . ? O4A C39A C38A 95.8(10) . . ? O4A C39A H39C 112.6 . . ? C38A C39A H39C 112.6 . . ? O4A C39A H39D 112.6 . . ? C38A C39A H39D 112.6 . . ? H39C C39A H39D 110.1 . . ? C40A O4A C39A 116.6(11) . . ? C42 O5A C41A 114.1(10) . . ? O4A C40A C41A 112.3(13) . . ? O4A C40A H40C 109.1 . . ? C41A C40A H40C 109.1 . . ? O4A C40A H40D 109.1 . . ? C41A C40A H40D 109.1 . . ? H40C C40A H40D 107.9 . . ? O5A C41A C40A 105.1(12) . . ? O5A C41A H41C 110.7 . . ? C40A C41A H41C 110.7 . . ? O5A C41A H41D 110.7 . . ? C40A C41A H41D 110.7 . . ? H41C C41A H41D 108.8 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.421 _refine_diff_density_min -1.360 _refine_diff_density_rms 0.151 # Attachment '- New CIF for Compound3Pd.cif' data_e1852a _database_code_depnum_ccdc_archive 'CCDC 894033' #TrackingRef '- New CIF for Compound3Pd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C69 H63 N7 O10 Pd), 2(C5 H12), 3(H2 O)' _chemical_formula_sum 'C148 H156 N14 O23 Pd2' _chemical_formula_weight 2711.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8196(12) _cell_length_b 17.1292(15) _cell_length_c 17.1532(17) _cell_angle_alpha 63.953(3) _cell_angle_beta 84.648(3) _cell_angle_gamma 64.883(3) _cell_volume 3518.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7380 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 22.98 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1418 _exptl_absorpt_coefficient_mu 0.328 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9711 _exptl_absorpt_correction_T_max 0.9838 _exptl_absorpt_process_details sadabs _exptl_special_details ;Because of the flopiness of the ether chain some atoms had the same thermal parameters.Because of the flopiness ofC47 the hydrogen atom on C46 were not introduced.Because of the flopiness of the ether chain we used many distance and angle restraints on the atoms of this chain ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12750 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 24.800 _reflns_number_total 11654 _reflns_number_gt 5276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6654 _refine_ls_number_parameters 680 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1510 _refine_ls_R_factor_gt 0.1132 _refine_ls_wR_factor_ref 0.3255 _refine_ls_wR_factor_gt 0.2997 _refine_ls_goodness_of_fit_ref 1.416 _refine_ls_restrained_S_all 1.219 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.003 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 0.97639(6) 0.65861(6) 0.87900(6) 0.0263(6) Uani 1 1 d . . . N1 N 0.8272(7) 0.7379(6) 0.8494(6) 0.0259(14) Uani 1 1 d . . . N2 N 0.9611(7) 0.5504(6) 0.8745(6) 0.0259(14) Uani 1 1 d . . . N3 N 1.1271(7) 0.5808(6) 0.9050(6) 0.0269(13) Uani 1 1 d . . . N4 N 0.9902(8) 0.7677(7) 0.8864(7) 0.0281(14) Uani 1 1 d . . . C1 C 0.7748(9) 0.8300(7) 0.8400(8) 0.0259(14) Uani 1 1 d . . . C2 C 0.6691(9) 0.8629(8) 0.8133(8) 0.0259(14) Uani 1 1 d . . . H2 H 0.6163 0.9243 0.8014 0.031 Uiso 1 1 calc R . . C3 C 0.6609(9) 0.7907(7) 0.8089(7) 0.0259(14) Uani 1 1 d . . . H3 H 0.6009 0.7919 0.7919 0.031 Uiso 1 1 calc R . . C4 C 0.7582(9) 0.7101(7) 0.8342(8) 0.0259(14) Uani 1 1 d . . . C5 C 0.7768(9) 0.6202(8) 0.8420(8) 0.024(3) Uani 1 1 d . . . C6 C 0.8734(9) 0.5446(8) 0.8653(8) 0.0259(14) Uani 1 1 d . . . C7 C 0.8952(8) 0.4476(7) 0.8775(7) 0.0259(14) Uani 1 1 d . . . H7 H 0.8479 0.4242 0.8761 0.031 Uiso 1 1 calc R . . C8 C 0.9953(8) 0.3990(8) 0.8911(7) 0.0259(14) Uani 1 1 d . . . H8 H 1.0326 0.3343 0.9001 0.031 Uiso 1 1 calc R . . C9 C 1.0364(9) 0.4622(7) 0.8895(8) 0.0259(14) Uani 1 1 d . . . C10 C 1.1430(9) 0.4361(7) 0.8943(8) 0.0259(14) Uani 1 1 d . . . C11 C 1.1795(9) 0.4967(8) 0.8995(8) 0.0269(13) Uani 1 1 d . . . C12 C 1.2848(9) 0.4740(8) 0.9030(8) 0.0269(13) Uani 1 1 d . . . H12 H 1.3372 0.4193 0.8999 0.032 Uiso 1 1 calc R . . C13 C 1.2957(9) 0.5433(7) 0.9114(8) 0.0269(13) Uani 1 1 d . . . H13 H 1.3575 0.5459 0.9170 0.032 Uiso 1 1 calc R . . C14 C 1.1977(9) 0.6134(8) 0.9106(8) 0.0269(13) Uani 1 1 d . . . C15 C 1.1735(9) 0.6972(8) 0.9148(8) 0.0269(13) Uani 1 1 d . . . C16 C 1.0793(9) 0.7676(8) 0.9056(8) 0.0281(14) Uani 1 1 d . . . C17 C 1.0550(9) 0.8565(8) 0.9131(8) 0.0281(14) Uani 1 1 d . . . H17 H 1.1012 0.8739 0.9284 0.034 Uiso 1 1 calc R . . C18 C 0.9553(9) 0.9085(8) 0.8942(8) 0.0281(14) Uani 1 1 d . . . H18 H 0.9183 0.9703 0.8922 0.034 Uiso 1 1 calc R . . C19 C 0.9143(9) 0.8537(8) 0.8775(8) 0.0281(14) Uani 1 1 d . . . C20 C 0.8114(9) 0.8850(8) 0.8541(8) 0.0281(14) Uani 1 1 d . . . C21 C 0.6909(10) 0.6023(9) 0.8241(10) 0.0397(15) Uani 1 1 d . . . C22 C 0.6953(10) 0.5728(9) 0.7584(9) 0.0397(15) Uani 1 1 d . . . H22 H 0.7517 0.5634 0.7266 0.048 Uiso 1 1 calc R . . C23 C 0.6186(10) 0.5580(9) 0.7415(9) 0.0397(15) Uani 1 1 d . . . C24 C 0.5321(10) 0.5726(9) 0.7875(9) 0.0397(15) Uani 1 1 d . . . H24 H 0.4781 0.5623 0.7748 0.048 Uiso 1 1 calc R . . C25 C 0.5296(10) 0.6021(9) 0.8511(9) 0.0397(15) Uani 1 1 d . . . H25 H 0.4728 0.6131 0.8823 0.048 Uiso 1 1 calc R . . C26 C 0.6089(10) 0.6157(9) 0.8699(9) 0.0397(15) Uani 1 1 d . . . H26 H 0.6067 0.6346 0.9148 0.048 Uiso 1 1 calc R . . O1 O 0.6287(8) 0.5247(7) 0.6802(7) 0.060(3) Uani 1 1 d . . . C27 C 0.5495(15) 0.5096(14) 0.6573(12) 0.075(5) Uani 1 1 d . . . H27A H 0.4915 0.5717 0.6235 0.090 Uiso 1 1 calc R . . H27B H 0.5270 0.4706 0.7102 0.090 Uiso 1 1 calc R . . C28 C 0.598(3) 0.453(2) 0.599(2) 0.075(5) Uani 1 1 d . . . H28A H 0.662883 0.400079 0.629994 0.090 Uiso 1 1 calc R . . H28B H 0.5573 0.4208 0.5956 0.090 Uiso 1 1 calc R . . O2 O 0.5986(11) 0.5220(16) 0.5148(11) 0.127(7) Uani 1 1 d . . . C29 C 0.6909(19) 0.509(3) 0.5061(17) 0.132(11) Uani 1 1 d . . . H29A H 0.741174 0.449027 0.547605 0.159 Uiso 1 1 calc R . . H29B H 0.7019 0.5578 0.5156 0.159 Uiso 1 1 calc R . . C30 C 0.7128(18) 0.5194(17) 0.416(2) 0.132(11) Uani 1 1 d . . . H30A H 0.6587 0.5778 0.3718 0.159 Uiso 1 1 calc R . . H30B H 0.7769 0.5251 0.4031 0.159 Uiso 1 1 calc R . . O3 O 0.7192(11) 0.4341(11) 0.4114(8) 0.097(5) Uani 1 1 d . . . C31 C 0.7278(16) 0.4311(14) 0.3310(13) 0.082(6) Uani 1 1 d . . . H31A H 0.7066 0.4972 0.2835 0.098 Uiso 1 1 calc R . . H31B H 0.6826 0.4051 0.3237 0.098 Uiso 1 1 calc R . . C32 C 0.8369(17) 0.3677(14) 0.3238(12) 0.087(7) Uani 1 1 d . . . H32A H 0.8623 0.3044 0.3759 0.105 Uiso 1 1 calc R . . H32B H 0.8388 0.3567 0.2715 0.105 Uiso 1 1 calc R . . O4 O 0.8999(12) 0.4157(10) 0.3173(10) 0.106(5) Uani 1 1 d . . . C33 C 0.9715(17) 0.3734(15) 0.3786(15) 0.100(8) Uani 1 1 d . . . H33A H 1.0114 0.3067 0.3863 0.120 Uiso 1 1 calc R . . H33B H 0.9420 0.3697 0.4336 0.120 Uiso 1 1 calc R . . C34 C 1.0388(13) 0.4186(12) 0.3649(11) 0.066(5) Uani 1 1 d . . . H34A H 1.0984 0.3750 0.4092 0.079 Uiso 1 1 calc R . . H34B H 1.0619 0.4314 0.3064 0.079 Uiso 1 1 calc R . . O5 O 0.9873(10) 0.5076(9) 0.3719(8) 0.076(4) Uani 1 1 d . . . C35 C 1.0524(18) 0.5492(16) 0.3667(14) 0.085(6) Uani 1 1 d . . . H35A H 1.0791 0.5641 0.3094 0.101 Uiso 1 1 calc R . . H35B H 1.1098 0.5032 0.4130 0.101 Uiso 1 1 calc R . . C36 C 1.0000(16) 0.6372(13) 0.3771(10) 0.064(5) Uani 1 1 d . . . C37 C 0.8993(17) 0.6758(13) 0.3846(12) 0.073(6) Uani 1 1 d . . . H37 H 0.8583 0.6463 0.3829 0.088 Uiso 1 1 calc R . . C38 C 0.8597(16) 0.7600(18) 0.3947(13) 0.073(6) Uani 1 1 d . . . H38 H 0.7898 0.7900 0.3978 0.088 Uiso 1 1 calc R . . C39 C 0.9204(16) 0.8009(16) 0.4004(12) 0.082(6) Uani 1 1 d . . . H39 H 0.8918 0.8575 0.4087 0.098 Uiso 1 1 calc R . . C40 C 1.024(2) 0.7594(13) 0.3940(11) 0.082(6) Uani 1 1 d . . . N5 N 1.0602(12) 0.6794(12) 0.3798(9) 0.079(5) Uani 1 1 d . . . C41 C 1.0962(15) 0.7944(14) 0.3994(12) 0.073(6) Uani 1 1 d . . . H41A H 1.1483 0.7431 0.4490 0.088 Uiso 1 1 calc R . . H41B H 1.1298 0.8058 0.3455 0.088 Uiso 1 1 calc R . . O6 O 1.0575(11) 0.8772(9) 0.4102(8) 0.085(4) Uani 1 1 d . . . C42 C 1.0208(18) 0.9604(13) 0.3298(13) 0.098(8) Uani 1 1 d . . . H42A H 0.9553 0.9714 0.3072 0.118 Uiso 1 1 calc R . . H42B H 1.0684 0.9538 0.2861 0.118 Uiso 1 1 calc R . . C43 C 1.010(2) 1.0434(15) 0.3479(15) 0.105(8) Uani 1 1 d . . . H43A H 0.9677 1.1046 0.2976 0.126 Uiso 1 1 calc R . . H43B H 0.9730 1.0400 0.3997 0.126 Uiso 1 1 calc R . . O7 O 1.0941(12) 1.0458(9) 0.3616(8) 0.086(3) Uani 1 1 d . . . C44 C 1.0760(17) 1.1278(14) 0.3742(14) 0.086(3) Uani 1 1 d . . . H44A H 1.0249 1.1863 0.3277 0.103 Uiso 1 1 calc R . . H44B H 1.0504 1.1203 0.4313 0.103 Uiso 1 1 calc R . . C45 C 1.1652(14) 1.1368(13) 0.3718(12) 0.086(3) Uani 1 1 d D . . H45A H 1.1505 1.2040 0.3574 0.103 Uiso 1 1 calc R . . H45B H 1.2027 1.1211 0.3259 0.103 Uiso 1 1 calc R . . O8 O 1.2260(13) 1.0717(12) 0.4567(9) 0.086(3) Uani 1 1 d D . . C46 C 1.323(2) 1.086(3) 0.4545(17) 0.086(3) Uani 1 1 d D . . C47 C 1.375(5) 1.103(5) 0.516(2) 0.086(3) Uani 0.26(3) 1 d PD . . H47A H 1.3527 1.1720 0.4986 0.103 Uiso 0.26(3) 1 calc PR . . H47B H 1.4487 1.0702 0.5206 0.103 Uiso 0.26(3) 1 calc PR . . O9 O 1.3339(12) 1.0543(10) 0.6016(10) 0.113(5) Uani 1 1 d D . . C47A C 1.381(2) 1.0032(19) 0.5447(16) 0.086(3) Uani 0.74(3) 1 d PD . . H47C H 1.3672 0.9464 0.5614 0.103 Uiso 0.74(3) 1 calc PR . . H47D H 1.4540 0.9837 0.5459 0.103 Uiso 0.74(3) 1 calc PR . . C48 C 1.3776(16) 0.9992(16) 0.6845(14) 0.107(8) Uani 1 1 d . . . H48A H 1.3675 1.0412 0.7129 0.128 Uiso 1 1 calc R . . H48B H 1.4507 0.9649 0.6841 0.128 Uiso 1 1 calc R . . C49 C 1.3373(12) 0.9264(10) 0.7377(11) 0.061(5) Uani 1 1 d . . . H49A H 1.2641 0.9593 0.7386 0.073 Uiso 1 1 calc R . . H49B H 1.3497 0.8816 0.7120 0.073 Uiso 1 1 calc R . . O10 O 1.3876(8) 0.8750(7) 0.8242(7) 0.065(3) Uani 1 1 d . . . C50 C 1.3612(10) 0.8047(8) 0.8858(10) 0.041(4) Uani 1 1 d . . . C51 C 1.2825(11) 0.7888(9) 0.8692(10) 0.041(4) Uani 1 1 d . . . H51 H 1.2424 0.8290 0.8143 0.050 Uiso 1 1 calc R . . C52 C 1.2612(10) 0.7152(9) 0.9315(10) 0.041(4) Uani 1 1 d . . . C53 C 1.3217(10) 0.6564(10) 1.0104(10) 0.041(4) Uani 1 1 d . . . H53 H 1.3092 0.6042 1.0526 0.050 Uiso 1 1 calc R . . C54 C 1.4029(10) 0.6720(10) 1.0305(10) 0.041(4) Uani 1 1 d . . . H54 H 1.4432 0.6331 1.0853 0.050 Uiso 1 1 calc R . . C55 C 1.4186(10) 0.7479(10) 0.9641(10) 0.041(4) Uani 1 1 d . . . H55 H 1.4719 0.7603 0.9743 0.050 Uiso 1 1 calc R . . C56 C 1.2138(9) 0.3431(8) 0.8915(8) 0.027(3) Uani 1 1 d . . . C57 C 1.2044(9) 0.3300(8) 0.8185(8) 0.026(3) Uani 1 1 d . . . H57 H 1.1541 0.3791 0.7712 0.031 Uiso 1 1 calc R . . C58 C 1.2693(9) 0.2444(8) 0.8154(8) 0.031(3) Uani 1 1 d . . . H58 H 1.2632 0.2342 0.7665 0.037 Uiso 1 1 calc R . . C59 C 1.3426(11) 0.1748(8) 0.8843(10) 0.037(4) Uani 1 1 d . . . C60 C 1.3548(9) 0.1874(8) 0.9574(8) 0.031(3) Uani 1 1 d . . . H60 H 1.4072 0.1394 1.0032 0.037 Uiso 1 1 calc R . . C61 C 1.2862(10) 0.2745(9) 0.9613(9) 0.039(3) Uani 1 1 d . . . H61 H 1.2906 0.2848 1.0107 0.046 Uiso 1 1 calc R . . C62 C 1.4097(10) 0.0863(9) 0.8807(9) 0.039(3) Uani 1 1 d . . . N6 N 1.4629(9) 0.0140(8) 0.8795(9) 0.057(4) Uani 1 1 d . . . C63 C 0.7399(10) 0.9837(8) 0.8437(9) 0.034(3) Uani 1 1 d . . . C64 C 0.7046(11) 1.0587(8) 0.7613(8) 0.040(4) Uani 1 1 d . . . H64 H 0.7271 1.0488 0.7113 0.048 Uiso 1 1 calc R . . C65 C 0.6344(11) 1.1504(8) 0.7519(9) 0.042(4) Uani 1 1 d . . . H65 H 0.6090 1.2019 0.6950 0.051 Uiso 1 1 calc R . . C66 C 0.6022(10) 1.1666(8) 0.8237(10) 0.036(4) Uani 1 1 d . . . C67 C 0.6427(9) 1.0933(8) 0.9045(9) 0.030(3) Uani 1 1 d . . . H67 H 0.6237 1.1043 0.9545 0.036 Uiso 1 1 calc R . . C68 C 0.7124(9) 1.0012(8) 0.9151(9) 0.034(4) Uani 1 1 d . . . H68 H 0.7406 0.9510 0.9721 0.041 Uiso 1 1 calc R . . C69 C 0.5323(10) 1.2580(10) 0.8132(9) 0.033(3) Uani 1 1 d . . . N7 N 0.4757(10) 1.3322(9) 0.8061(8) 0.050(3) Uani 1 1 d . . . C70 C 1.1712(12) 0.0414(12) 0.8794(12) 0.070(5) Uani 1 1 d . . . H70A H 1.1643 -0.0103 0.9317 0.105 Uiso 1 1 calc R . . H70B H 1.2352 0.0426 0.8871 0.105 Uiso 1 1 calc R . . H70C H 1.1695 0.0299 0.8285 0.105 Uiso 1 1 calc R . . C71 C 1.0848(12) 0.1380(11) 0.8653(10) 0.054(5) Uani 1 1 d . . . H71A H 1.0939 0.1545 0.9116 0.065 Uiso 1 1 calc R . . H71B H 1.0873 0.1885 0.8084 0.065 Uiso 1 1 calc R . . C74 C 0.9850(13) 0.1375(12) 0.8662(10) 0.054(5) Uani 1 1 d . . . H74A H 0.9818 0.0891 0.9243 0.065 Uiso 1 1 calc R . . H74B H 0.9781 0.1170 0.8223 0.065 Uiso 1 1 calc R . . C72 C 0.8965(12) 0.2342(12) 0.8474(11) 0.062(5) Uani 1 1 d . . . H72A H 0.9044 0.2839 0.7927 0.074 Uiso 1 1 calc R . . H72B H 0.8997 0.2511 0.8950 0.074 Uiso 1 1 calc R . . C73 C 0.7897(15) 0.2389(19) 0.8379(14) 0.101(7) Uani 1 1 d . . . H73A H 0.7816 0.2320 0.7856 0.152 Uiso 1 1 calc R . . H73B H 0.7382 0.3009 0.8328 0.152 Uiso 1 1 calc R . . H73C H 0.7827 0.1867 0.8895 0.152 Uiso 1 1 calc R . . O12 O 0.2700(16) 0.7968(11) 0.6401(13) 0.144(6) Uani 1 1 d . . . O13 O 0.355(3) 0.800(2) 0.496(2) 0.144(6) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0071(8) 0.0217(7) 0.0483(8) -0.0200(5) 0.0014(5) 0.0005(6) N1 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) N2 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) N3 0.006(3) 0.020(2) 0.053(3) -0.024(2) -0.002(2) 0.004(2) N4 0.012(3) 0.020(2) 0.051(3) -0.023(2) 0.000(2) 0.003(2) C1 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C2 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C3 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C4 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C5 0.006(7) 0.025(6) 0.042(7) -0.018(6) 0.007(6) -0.004(6) C6 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C7 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C8 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C9 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C10 0.010(3) 0.017(2) 0.048(3) -0.020(2) -0.004(3) 0.005(2) C11 0.006(3) 0.020(2) 0.053(3) -0.024(2) -0.002(2) 0.004(2) C12 0.006(3) 0.020(2) 0.053(3) -0.024(2) -0.002(2) 0.004(2) C13 0.006(3) 0.020(2) 0.053(3) -0.024(2) -0.002(2) 0.004(2) C14 0.006(3) 0.020(2) 0.053(3) -0.024(2) -0.002(2) 0.004(2) C15 0.006(3) 0.020(2) 0.053(3) -0.024(2) -0.002(2) 0.004(2) C16 0.012(3) 0.020(2) 0.051(3) -0.023(2) 0.000(2) 0.003(2) C17 0.012(3) 0.020(2) 0.051(3) -0.023(2) 0.000(2) 0.003(2) C18 0.012(3) 0.020(2) 0.051(3) -0.023(2) 0.000(2) 0.003(2) C19 0.012(3) 0.020(2) 0.051(3) -0.023(2) 0.000(2) 0.003(2) C20 0.012(3) 0.020(2) 0.051(3) -0.023(2) 0.000(2) 0.003(2) C21 0.013(3) 0.045(3) 0.069(4) -0.034(3) -0.002(3) -0.008(3) C22 0.013(3) 0.045(3) 0.069(4) -0.034(3) -0.002(3) -0.008(3) C23 0.013(3) 0.045(3) 0.069(4) -0.034(3) -0.002(3) -0.008(3) C24 0.013(3) 0.045(3) 0.069(4) -0.034(3) -0.002(3) -0.008(3) C25 0.013(3) 0.045(3) 0.069(4) -0.034(3) -0.002(3) -0.008(3) C26 0.013(3) 0.045(3) 0.069(4) -0.034(3) -0.002(3) -0.008(3) O1 0.043(7) 0.073(7) 0.087(7) -0.048(6) -0.014(6) -0.026(6) C27 0.066(14) 0.086(12) 0.083(12) -0.042(10) 0.006(10) -0.036(11) C28 0.066(14) 0.086(12) 0.083(12) -0.042(10) 0.006(10) -0.036(11) O2 0.048(11) 0.220(19) 0.111(12) -0.074(13) 0.023(9) -0.059(12) C29 0.061(17) 0.094(17) 0.25(4) -0.10(2) -0.002(18) -0.005(13) C30 0.061(17) 0.094(17) 0.25(4) -0.10(2) -0.002(18) -0.005(13) O3 0.099(12) 0.111(11) 0.066(8) -0.037(8) 0.017(7) -0.036(9) C31 0.072(16) 0.085(13) 0.078(14) -0.045(11) 0.031(11) -0.020(12) C32 0.099(19) 0.082(13) 0.071(12) -0.025(10) -0.004(11) -0.037(14) O4 0.072(11) 0.077(8) 0.125(12) -0.005(8) -0.017(9) -0.031(8) C33 0.064(15) 0.072(12) 0.124(17) -0.026(12) -0.043(14) -0.003(13) C34 0.045(12) 0.069(11) 0.073(11) -0.022(9) -0.007(9) -0.023(10) O5 0.058(9) 0.058(7) 0.096(9) -0.030(7) -0.004(7) -0.013(7) C35 0.095(18) 0.085(15) 0.083(13) -0.033(11) 0.018(12) -0.051(15) C36 0.063(15) 0.052(10) 0.048(10) -0.006(8) 0.000(9) -0.016(11) C37 0.065(17) 0.050(10) 0.092(13) -0.034(10) -0.010(11) -0.007(11) C38 0.065(17) 0.050(10) 0.092(13) -0.034(10) -0.010(11) -0.007(11) C39 0.040(13) 0.094(14) 0.079(13) -0.034(11) 0.020(10) -0.010(12) C40 0.040(13) 0.094(14) 0.079(13) -0.034(11) 0.020(10) -0.010(12) N5 0.070(12) 0.085(12) 0.052(9) -0.014(8) -0.001(8) -0.022(11) C41 0.064(14) 0.076(13) 0.078(12) -0.026(10) -0.010(10) -0.034(12) O6 0.120(13) 0.063(8) 0.068(8) -0.017(7) 0.000(7) -0.045(8) C42 0.12(2) 0.075(13) 0.090(14) -0.014(12) -0.023(13) -0.046(14) C43 0.13(2) 0.085(14) 0.118(18) -0.054(13) 0.062(16) -0.061(16) O7 0.094(9) 0.072(6) 0.099(7) -0.045(5) 0.016(6) -0.037(6) C44 0.094(9) 0.072(6) 0.099(7) -0.045(5) 0.016(6) -0.037(6) C45 0.094(9) 0.072(6) 0.099(7) -0.045(5) 0.016(6) -0.037(6) O8 0.094(9) 0.072(6) 0.099(7) -0.045(5) 0.016(6) -0.037(6) C46 0.094(9) 0.072(6) 0.099(7) -0.045(5) 0.016(6) -0.037(6) C47 0.094(9) 0.072(6) 0.099(7) -0.045(5) 0.016(6) -0.037(6) C47A 0.094(9) 0.072(6) 0.099(7) -0.045(5) 0.016(6) -0.037(6) O9 0.112(14) 0.097(10) 0.095(10) -0.017(9) 0.014(9) -0.042(10) C48 0.062(16) 0.099(15) 0.099(16) -0.009(13) 0.009(12) -0.020(13) C49 0.025(10) 0.047(8) 0.084(11) -0.001(8) -0.005(8) -0.018(8) O10 0.035(7) 0.047(6) 0.108(9) -0.021(6) -0.009(6) -0.024(5) C50 0.011(8) 0.050(8) 0.079(10) -0.053(8) 0.010(7) -0.002(7) C51 0.011(8) 0.050(8) 0.079(10) -0.053(8) 0.010(7) -0.002(7) C52 0.011(8) 0.050(8) 0.079(10) -0.053(8) 0.010(7) -0.002(7) C53 0.011(8) 0.050(8) 0.079(10) -0.053(8) 0.010(7) -0.002(7) C54 0.011(8) 0.050(8) 0.079(10) -0.053(8) 0.010(7) -0.002(7) C55 0.011(8) 0.050(8) 0.079(10) -0.053(8) 0.010(7) -0.002(7) C56 0.011(8) 0.027(7) 0.041(8) -0.016(6) -0.010(6) -0.003(6) C57 0.009(7) 0.025(6) 0.040(7) -0.016(6) -0.008(6) 0.001(6) C58 0.011(8) 0.031(7) 0.050(8) -0.023(6) 0.003(6) -0.002(7) C59 0.027(9) 0.022(6) 0.072(10) -0.029(7) 0.003(7) -0.010(6) C60 0.017(8) 0.033(7) 0.054(8) -0.030(6) -0.004(6) -0.008(7) C61 0.009(6) 0.031(5) 0.070(7) -0.029(5) -0.008(5) 0.006(5) C62 0.009(6) 0.031(5) 0.070(7) -0.029(5) -0.008(5) 0.006(5) N6 0.025(8) 0.037(7) 0.102(10) -0.038(7) -0.012(7) 0.005(6) C63 0.025(9) 0.024(7) 0.050(9) -0.024(7) 0.000(7) 0.001(6) C64 0.038(10) 0.023(7) 0.041(8) -0.016(6) 0.006(7) 0.005(7) C65 0.043(10) 0.020(7) 0.045(9) -0.010(6) -0.013(7) 0.002(7) C66 0.020(9) 0.021(7) 0.064(10) -0.023(7) -0.010(7) 0.001(6) C67 0.016(8) 0.028(7) 0.052(8) -0.028(7) 0.007(6) -0.004(7) C68 0.014(8) 0.024(7) 0.054(9) -0.007(6) 0.005(6) -0.011(6) C69 0.008(8) 0.036(8) 0.063(9) -0.036(7) 0.011(7) -0.004(7) N7 0.029(8) 0.050(8) 0.075(8) -0.037(7) -0.002(6) -0.009(7) C70 0.026(10) 0.068(11) 0.108(14) -0.051(10) -0.018(9) 0.004(9) C71 0.044(11) 0.060(10) 0.057(9) -0.022(8) -0.010(8) -0.023(9) C74 0.075(14) 0.070(10) 0.053(9) -0.048(8) 0.023(9) -0.043(10) C72 0.041(11) 0.063(10) 0.082(11) -0.036(9) 0.013(9) -0.021(9) C73 0.056(14) 0.18(2) 0.120(16) -0.111(17) 0.020(12) -0.049(15) O12 0.156(17) 0.097(10) 0.162(14) -0.069(10) -0.010(11) -0.022(10) O13 0.156(17) 0.097(10) 0.162(14) -0.069(10) -0.010(11) -0.022(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.995(9) . ? Pd1 N1 2.011(9) . ? Pd1 N4 2.022(10) . ? Pd1 N3 2.024(10) . ? N1 C1 1.371(15) . ? N1 C4 1.383(16) . ? N2 C9 1.369(14) . ? N2 C6 1.373(15) . ? N3 C11 1.359(16) . ? N3 C14 1.406(16) . ? N4 C19 1.373(16) . ? N4 C16 1.389(16) . ? C1 C20 1.378(17) . ? C1 C2 1.463(17) . ? C2 C3 1.328(16) . ? C2 H2 0.9500 . ? C3 C4 1.440(17) . ? C3 H3 0.9500 . ? C4 C5 1.390(17) . ? C5 C6 1.402(17) . ? C5 C21 1.515(18) . ? C6 C7 1.469(16) . ? C7 C8 1.340(16) . ? C7 H7 0.9500 . ? C8 C9 1.441(16) . ? C8 H8 0.9500 . ? C9 C10 1.447(16) . ? C10 C11 1.395(17) . ? C10 C56 1.510(18) . ? C11 C12 1.439(17) . ? C12 C13 1.332(17) . ? C12 H12 0.9500 . ? C13 C14 1.435(17) . ? C13 H13 0.9500 . ? C14 C15 1.359(17) . ? C15 C16 1.369(18) . ? C15 C52 1.533(19) . ? C16 C17 1.471(17) . ? C17 C18 1.341(17) . ? C17 H17 0.9500 . ? C18 C19 1.444(18) . ? C18 H18 0.9500 . ? C19 C20 1.416(17) . ? C20 C63 1.504(18) . ? C21 C26 1.37(2) . ? C21 C22 1.41(2) . ? C22 C23 1.345(18) . ? C22 H22 0.9500 . ? C23 O1 1.370(18) . ? C23 C24 1.43(2) . ? C24 C25 1.38(2) . ? C24 H24 0.9500 . ? C25 C26 1.382(18) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? O1 C27 1.43(2) . ? C27 C28 1.61(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O2 1.41(3) . ? O2 C29 1.30(3) . ? C29 C30 1.50(4) . ? C30 O3 1.46(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O3 C31 1.40(2) . ? C31 C32 1.55(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O4 1.45(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? O4 C33 1.28(2) . ? C33 C34 1.45(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O5 1.44(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O5 C35 1.40(2) . ? C35 C36 1.46(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.37(3) . ? C36 N5 1.38(2) . ? C37 C38 1.39(3) . ? C37 H37 0.9500 . ? C38 C39 1.38(3) . ? C38 H38 0.9500 . ? C39 C40 1.41(3) . ? C39 H39 0.9500 . ? C40 N5 1.37(2) . ? C40 C41 1.46(3) . ? C41 O6 1.38(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O6 C42 1.41(2) . ? C42 C43 1.52(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O7 1.32(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O7 C44 1.42(2) . ? C44 C45 1.39(3) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 O8 1.464(15) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? O8 C46 1.555(18) . ? C46 C47 1.544(15) . ? C46 C47A 1.558(19) . ? C47 O9 1.55(2) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? O9 C48 1.34(2) . ? O9 C47A 1.520(19) . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C48 C49 1.51(2) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 O10 1.426(18) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? O10 C50 1.388(15) . ? C50 C55 1.355(19) . ? C50 C51 1.385(19) . ? C51 C52 1.386(19) . ? C51 H51 0.9500 . ? C52 C53 1.384(19) . ? C53 C54 1.438(19) . ? C53 H53 0.9500 . ? C54 C55 1.396(19) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C61 1.378(17) . ? C56 C57 1.393(18) . ? C57 C58 1.393(18) . ? C57 H57 0.9500 . ? C58 C59 1.378(18) . ? C58 H58 0.9500 . ? C59 C60 1.402(19) . ? C59 C62 1.44(2) . ? C60 C61 1.432(19) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 N6 1.161(17) . ? C63 C64 1.375(17) . ? C63 C68 1.373(19) . ? C64 C65 1.413(19) . ? C64 H64 0.9500 . ? C65 C66 1.38(2) . ? C65 H65 0.9500 . ? C66 C67 1.358(17) . ? C66 C69 1.40(2) . ? C67 C68 1.411(18) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 N7 1.146(16) . ? C70 C71 1.53(2) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C74 1.48(2) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C74 C72 1.53(2) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C72 C73 1.57(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N1 89.7(4) . . ? N2 Pd1 N4 178.6(4) . . ? N1 Pd1 N4 89.9(4) . . ? N2 Pd1 N3 90.6(4) . . ? N1 Pd1 N3 178.3(4) . . ? N4 Pd1 N3 89.9(4) . . ? C1 N1 C4 107.0(10) . . ? C1 N1 Pd1 126.4(8) . . ? C4 N1 Pd1 126.5(8) . . ? C9 N2 C6 105.7(9) . . ? C9 N2 Pd1 126.4(8) . . ? C6 N2 Pd1 127.5(8) . . ? C11 N3 C14 106.4(10) . . ? C11 N3 Pd1 125.4(8) . . ? C14 N3 Pd1 126.4(8) . . ? C19 N4 C16 106.8(10) . . ? C19 N4 Pd1 127.2(8) . . ? C16 N4 Pd1 125.9(8) . . ? N1 C1 C20 127.7(11) . . ? N1 C1 C2 108.7(10) . . ? C20 C1 C2 123.6(10) . . ? C3 C2 C1 107.0(10) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 108.5(10) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? N1 C4 C5 127.1(11) . . ? N1 C4 C3 108.5(10) . . ? C5 C4 C3 124.4(11) . . ? C4 C5 C6 122.2(11) . . ? C4 C5 C21 119.6(11) . . ? C6 C5 C21 118.2(11) . . ? N2 C6 C5 126.2(10) . . ? N2 C6 C7 110.0(10) . . ? C5 C6 C7 123.6(11) . . ? C8 C7 C6 105.9(10) . . ? C8 C7 H7 127.0 . . ? C6 C7 H7 127.0 . . ? C7 C8 C9 107.9(10) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? N2 C9 C8 110.4(10) . . ? N2 C9 C10 126.4(10) . . ? C8 C9 C10 122.9(10) . . ? C11 C10 C9 120.7(10) . . ? C11 C10 C56 120.5(10) . . ? C9 C10 C56 118.8(10) . . ? N3 C11 C10 128.1(11) . . ? N3 C11 C12 109.5(10) . . ? C10 C11 C12 122.4(11) . . ? C13 C12 C11 107.9(11) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.0 . . ? C12 C13 C14 107.8(11) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? C15 C14 N3 124.0(11) . . ? C15 C14 C13 127.7(12) . . ? N3 C14 C13 108.3(10) . . ? C14 C15 C16 127.0(12) . . ? C14 C15 C52 116.6(11) . . ? C16 C15 C52 116.4(11) . . ? C15 C16 N4 125.7(11) . . ? C15 C16 C17 126.0(12) . . ? N4 C16 C17 108.4(10) . . ? C18 C17 C16 107.1(11) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 107.9(11) . . ? C17 C18 H18 126.1 . . ? C19 C18 H18 126.1 . . ? N4 C19 C20 125.4(11) . . ? N4 C19 C18 109.8(10) . . ? C20 C19 C18 124.8(11) . . ? C1 C20 C19 123.2(11) . . ? C1 C20 C63 119.2(11) . . ? C19 C20 C63 117.6(11) . . ? C26 C21 C22 120.0(12) . . ? C26 C21 C5 121.1(13) . . ? C22 C21 C5 119.0(13) . . ? C23 C22 C21 119.2(14) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 O1 117.0(13) . . ? C22 C23 C24 121.8(15) . . ? O1 C23 C24 121.1(12) . . ? C25 C24 C23 117.6(13) . . ? C25 C24 H24 121.2 . . ? C23 C24 H24 121.2 . . ? C26 C25 C24 120.8(14) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C21 C26 C25 120.5(15) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C23 O1 C27 120.2(13) . . ? O1 C27 C28 104.5(16) . . ? O1 C27 H27A 110.8 . . ? C28 C27 H27A 110.8 . . ? O1 C27 H27B 110.8 . . ? C28 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? O2 C28 C27 107(2) . . ? C29 O2 C28 107(2) . . ? O2 C29 C30 109.1(18) . . ? O3 C30 C29 108(2) . . ? O3 C30 H30A 110.1 . . ? C29 C30 H30A 110.1 . . ? O3 C30 H30B 110.1 . . ? C29 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C31 O3 C30 118.8(18) . . ? O3 C31 C32 111.5(17) . . ? O3 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? O3 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? O4 C32 C31 109.3(18) . . ? O4 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? O4 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? C33 O4 C32 117.3(15) . . ? O4 C33 C34 115.5(18) . . ? O4 C33 H33A 108.4 . . ? C34 C33 H33A 108.4 . . ? O4 C33 H33B 108.4 . . ? C34 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? O5 C34 C33 109.5(18) . . ? O5 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? O5 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? C35 O5 C34 111.2(16) . . ? O5 C35 C36 110.4(19) . . ? O5 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? O5 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? C37 C36 N5 122(2) . . ? C37 C36 C35 124(2) . . ? N5 C36 C35 115(2) . . ? C36 C37 C38 117(2) . . ? C36 C37 H37 121.4 . . ? C38 C37 H37 121.4 . . ? C39 C38 C37 121(2) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C40 121(2) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.6 . . ? N5 C40 C39 117(2) . . ? N5 C40 C41 116(2) . . ? C39 C40 C41 126(2) . . ? C40 N5 C36 122(2) . . ? O6 C41 C40 115.7(18) . . ? O6 C41 H41A 108.4 . . ? C40 C41 H41A 108.4 . . ? O6 C41 H41B 108.4 . . ? C40 C41 H41B 108.4 . . ? H41A C41 H41B 107.4 . . ? C41 O6 C42 112.0(15) . . ? O6 C42 C43 106.2(17) . . ? O6 C42 H42A 110.5 . . ? C43 C42 H42A 110.5 . . ? O6 C42 H42B 110.5 . . ? C43 C42 H42B 110.5 . . ? H42A C42 H42B 108.7 . . ? O7 C43 C42 115(2) . . ? O7 C43 H43A 108.4 . . ? C42 C43 H43A 108.4 . . ? O7 C43 H43B 108.4 . . ? C42 C43 H43B 108.4 . . ? H43A C43 H43B 107.5 . . ? C43 O7 C44 111.4(17) . . ? C45 C44 O7 108.9(19) . . ? C45 C44 H44A 109.9 . . ? O7 C44 H44A 109.9 . . ? C45 C44 H44B 109.9 . . ? O7 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? C44 C45 O8 109.8(17) . . ? C44 C45 H45A 109.7 . . ? O8 C45 H45A 109.7 . . ? C44 C45 H45B 109.7 . . ? O8 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? C45 O8 C46 109.2(13) . . ? C47 C46 O8 133(3) . . ? C47 C46 C47A 59(3) . . ? O8 C46 C47A 100(2) . . ? C46 C47 O9 99(2) . . ? C46 C47 H47A 112.2 . . ? O9 C47 H47A 112.1 . . ? C46 C47 H47B 112.0 . . ? O9 C47 H47B 112.0 . . ? H47A C47 H47B 109.7 . . ? C48 O9 C47A 111.2(19) . . ? C48 O9 C47 131(3) . . ? C47A O9 C47 59(3) . . ? O9 C47A C46 99(2) . . ? O9 C47A H47C 112.0 . . ? C46 C47A H47C 112.0 . . ? O9 C47A H47D 112.0 . . ? C46 C47A H47D 112.0 . . ? H47C C47A H47D 109.7 . . ? O9 C48 C49 113.3(18) . . ? O9 C48 H48A 108.9 . . ? C49 C48 H48A 108.9 . . ? O9 C48 H48B 108.9 . . ? C49 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? O10 C49 C48 107.6(13) . . ? O10 C49 H49A 110.2 . . ? C48 C49 H49A 110.2 . . ? O10 C49 H49B 110.2 . . ? C48 C49 H49B 110.2 . . ? H49A C49 H49B 108.5 . . ? C50 O10 C49 117.9(10) . . ? C55 C50 O10 117.2(12) . . ? C55 C50 C51 119.8(13) . . ? O10 C50 C51 123.0(13) . . ? C50 C51 C52 121.1(13) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C53 C52 C51 118.6(13) . . ? C53 C52 C15 119.6(12) . . ? C51 C52 C15 121.9(12) . . ? C52 C53 C54 121.8(13) . . ? C52 C53 H53 119.1 . . ? C54 C53 H53 119.1 . . ? C55 C54 C53 115.7(13) . . ? C55 C54 H54 122.2 . . ? C53 C54 H54 122.2 . . ? C50 C55 C54 123.0(12) . . ? C50 C55 H55 118.5 . . ? C54 C55 H55 118.5 . . ? C61 C56 C57 122.4(13) . . ? C61 C56 C10 118.4(12) . . ? C57 C56 C10 119.1(10) . . ? C58 C57 C56 119.5(11) . . ? C58 C57 H57 120.2 . . ? C56 C57 H57 120.2 . . ? C59 C58 C57 119.1(13) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 122.2(13) . . ? C58 C59 C62 118.9(14) . . ? C60 C59 C62 118.8(12) . . ? C59 C60 C61 118.4(12) . . ? C59 C60 H60 120.8 . . ? C61 C60 H60 120.8 . . ? C56 C61 C60 118.2(14) . . ? C56 C61 H61 120.9 . . ? C60 C61 H61 120.9 . . ? N6 C62 C59 178.4(16) . . ? C64 C63 C68 119.3(12) . . ? C64 C63 C20 119.7(13) . . ? C68 C63 C20 121.0(11) . . ? C63 C64 C65 119.4(14) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? C66 C65 C64 121.2(11) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C67 C66 C65 118.5(12) . . ? C67 C66 C69 120.8(15) . . ? C65 C66 C69 120.6(12) . . ? C66 C67 C68 120.9(14) . . ? C66 C67 H67 119.5 . . ? C68 C67 H67 119.5 . . ? C63 C68 C67 120.4(11) . . ? C63 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? N7 C69 C66 178.9(15) . . ? C71 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C74 C71 C70 113.0(14) . . ? C74 C71 H71A 109.0 . . ? C70 C71 H71A 109.0 . . ? C74 C71 H71B 109.0 . . ? C70 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? C71 C74 C72 114.6(14) . . ? C71 C74 H74A 108.6 . . ? C72 C74 H74A 108.6 . . ? C71 C74 H74B 108.6 . . ? C72 C74 H74B 108.6 . . ? H74A C74 H74B 107.6 . . ? C74 C72 C73 115.8(15) . . ? C74 C72 H72A 108.3 . . ? C73 C72 H72A 108.3 . . ? C74 C72 H72B 108.3 . . ? C73 C72 H72B 108.3 . . ? H72A C72 H72B 107.4 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 24.80 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 2.697 _refine_diff_density_min -2.129 _refine_diff_density_rms 0.217