Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Miao Du' _publ_contact_author_address ; College of Chemistry and Life Sciences Tianjin Normal University Tianjin 300387 CHINA ; _publ_contact_author_email DUMIAO@PUBLIC.TPT.TJ.CN _publ_section_title ; Interplay of coordinative and supramolecular interactions in engineering unusual crystalline architectures of low-dimensional metal-pamoate complexes under co-ligand intervention ; loop_ _publ_author_name 'Miao Du' 'Cheng-Peng Li' 'Qian Yu' 'Xiao-Jun Zhao' data_1 _database_code_depnum_ccdc_archive 'CCDC 631540' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H30 N2 O8' _chemical_formula_weight 534.55 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.320(2) _cell_length_b 23.887(3) _cell_length_c 14.326(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.433(2) _cell_angle_gamma 90.00 _cell_volume 5356.6(13) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3148 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 20.50 _exptl_crystal_description Block _exptl_crystal_colour Pale-Yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.778975 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 28890 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9433 _reflns_number_gt 5376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0452P)^2^+1.4380P] 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 SHELXL _refine_ls_extinction_coef 0.0034(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9433 _refine_ls_number_parameters 718 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 O1 O 0.62715(11) 0.20630(9) 0.26499(16) 0.0789(6) Uani 1 1 d . . . H1 H 0.5759 0.2029 0.2379 0.118 Uiso 1 1 calc R . . O2 O 0.59225(11) 0.29644(9) 0.25740(14) 0.0731(6) Uani 1 1 d . . . O3 O 0.71018(10) 0.36988(7) 0.31914(13) 0.0620(5) Uani 1 1 d . . . H3 H 0.6619 0.3574 0.2957 0.093 Uiso 1 1 calc R . . O4 O 1.05286(10) 0.43194(8) 0.44488(12) 0.0554(4) Uani 1 1 d . . . H4 H 1.1032 0.4409 0.4665 0.083 Uiso 1 1 calc R . . O5 O 1.19558(11) 0.45127(8) 0.57611(14) 0.0696(5) Uani 1 1 d . . . O6 O 1.19676(11) 0.45968(9) 0.73130(13) 0.0717(5) Uani 1 1 d . . . H6 H 1.2485 0.4588 0.7394 0.108 Uiso 1 1 calc R . . O7 O 0.59753(12) 0.21280(9) 0.49665(17) 0.0842(6) Uani 1 1 d . . . H7 H 0.6477 0.2118 0.5291 0.126 Uiso 1 1 calc R . . O8 O 0.62254(11) 0.30445(9) 0.50457(15) 0.0762(6) Uani 1 1 d . . . O9 O 0.49769(11) 0.37226(7) 0.44118(14) 0.0646(5) Uani 1 1 d . . . H9 H 0.5468 0.3618 0.4669 0.097 Uiso 1 1 calc R . . O10 O 0.00743(11) 0.43690(8) 0.01694(13) 0.0676(5) Uani 1 1 d . . . H10 H -0.0443 0.4394 0.0084 0.101 Uiso 1 1 calc R . . O11 O 0.00792(12) 0.43907(8) 0.17259(14) 0.0688(5) Uani 1 1 d . . . O12 O 0.15048(11) 0.42108(8) 0.30536(12) 0.0631(5) Uani 1 1 d . . . H12 H 0.0995 0.4280 0.2824 0.095 Uiso 1 1 calc R . . O13 O 0.47049(12) 0.18642(9) 0.17934(15) 0.0774(6) Uani 1 1 d . . . O14 O 0.63601(13) 0.54779(10) 0.21772(15) 0.0840(6) Uani 1 1 d . . . O15 O 0.15645(12) 0.56576(8) 1.02541(15) 0.0712(5) Uani 1 1 d . . . O16 O 0.24691(12) 0.69832(9) 0.91668(15) 0.0779(6) Uani 1 1 d . . . N1 N 0.34030(13) 0.22411(9) 0.11218(14) 0.0526(5) Uani 1 1 d . . . N2 N 0.55426(15) 0.53214(10) 0.31981(19) 0.0691(7) Uani 1 1 d . . . N3 N 0.27672(17) 0.56879(10) 0.97737(18) 0.0679(6) Uani 1 1 d . . . N4 N 0.11812(13) 0.73823(9) 0.85243(14) 0.0515(5) Uani 1 1 d . . . C1 C 0.64578(17) 0.25941(12) 0.28092(19) 0.0569(7) Uani 1 1 d . . . C2 C 0.73713(14) 0.27079(10) 0.32883(17) 0.0472(6) Uani 1 1 d . . . C3 C 0.79367(15) 0.22767(11) 0.35638(17) 0.0502(6) Uani 1 1 d . . . H3A H 0.7737 0.1910 0.3481 0.060 Uiso 1 1 calc R . . C4 C 0.88106(14) 0.23749(10) 0.39690(16) 0.0452(6) Uani 1 1 d . . . C5 C 0.93994(16) 0.19286(11) 0.42397(18) 0.0544(6) Uani 1 1 d . . . H5 H 0.9198 0.1562 0.4178 0.065 Uiso 1 1 calc R . . C6 C 1.02482(16) 0.20214(12) 0.45856(19) 0.0612(7) Uani 1 1 d . . . H6A H 1.0627 0.1724 0.4775 0.073 Uiso 1 1 calc R . . C7 C 1.05467(16) 0.25727(12) 0.46529(19) 0.0583(7) Uani 1 1 d . . . H7A H 1.1132 0.2638 0.4875 0.070 Uiso 1 1 calc R . . C8 C 1.00072(14) 0.30165(11) 0.44032(17) 0.0501(6) Uani 1 1 d . . . H8 H 1.0229 0.3377 0.4449 0.060 Uiso 1 1 calc R . . C9 C 0.91105(14) 0.29368(10) 0.40735(15) 0.0417(5) Uani 1 1 d . . . C10 C 0.85217(14) 0.33915(10) 0.38264(15) 0.0430(6) Uani 1 1 d . . . C11 C 0.76686(14) 0.32665(10) 0.34381(16) 0.0459(6) Uani 1 1 d . . . C12 C 0.88216(14) 0.39981(10) 0.39350(17) 0.0479(6) Uani 1 1 d . . . H12A H 0.9190 0.4058 0.3518 0.057 Uiso 1 1 calc R . . H12B H 0.8326 0.4238 0.3699 0.057 Uiso 1 1 calc R . . C13 C 0.92986(14) 0.41838(9) 0.49574(17) 0.0435(6) Uani 1 1 d . . . C14 C 1.01503(15) 0.43215(9) 0.51788(17) 0.0451(6) Uani 1 1 d . . . C15 C 1.06384(15) 0.44442(9) 0.61539(17) 0.0472(6) Uani 1 1 d . . . C16 C 1.15675(16) 0.45224(10) 0.6378(2) 0.0537(7) Uani 1 1 d . . . C17 C 1.02373(16) 0.44575(10) 0.68721(18) 0.0499(6) Uani 1 1 d . . . H17 H 1.0554 0.4537 0.7507 0.060 Uiso 1 1 calc R . . C18 C 0.93597(16) 0.43542(9) 0.66736(18) 0.0476(6) Uani 1 1 d . . . C19 C 0.89443(18) 0.43678(11) 0.74215(19) 0.0593(7) Uani 1 1 d . . . H19 H 0.9258 0.4451 0.8056 0.071 Uiso 1 1 calc R . . C20 C 0.81016(19) 0.42612(12) 0.7222(2) 0.0694(8) Uani 1 1 d . . . H20 H 0.7837 0.4271 0.7718 0.083 Uiso 1 1 calc R . . C21 C 0.76265(18) 0.41358(12) 0.6270(2) 0.0688(8) Uani 1 1 d . . . H21 H 0.7044 0.4068 0.6138 0.083 Uiso 1 1 calc R . . C22 C 0.79953(16) 0.41102(10) 0.55291(19) 0.0549(7) Uani 1 1 d . . . H22 H 0.7665 0.4022 0.4903 0.066 Uiso 1 1 calc R . . C23 C 0.88830(15) 0.42173(9) 0.57081(18) 0.0452(6) Uani 1 1 d . . . C24 C 0.57330(17) 0.26453(13) 0.48106(19) 0.0597(7) Uani 1 1 d . . . C25 C 0.48144(15) 0.27224(11) 0.43281(17) 0.0494(6) Uani 1 1 d . . . C26 C 0.42920(15) 0.22665(11) 0.40396(17) 0.0512(6) Uani 1 1 d . . . H26 H 0.4529 0.1909 0.4121 0.061 Uiso 1 1 calc R . . C27 C 0.34089(14) 0.23276(10) 0.36246(16) 0.0455(6) Uani 1 1 d . . . C28 C 0.28749(16) 0.18549(11) 0.33493(17) 0.0556(7) Uani 1 1 d . . . H28 H 0.3116 0.1499 0.3407 0.067 Uiso 1 1 calc R . . C29 C 0.20180(17) 0.19121(12) 0.30036(19) 0.0620(7) Uani 1 1 d . . . H29 H 0.1671 0.1599 0.2818 0.074 Uiso 1 1 calc R . . C30 C 0.16608(17) 0.24460(13) 0.29293(19) 0.0623(7) Uani 1 1 d . . . H30 H 0.1070 0.2485 0.2709 0.075 Uiso 1 1 calc R . . C31 C 0.21543(15) 0.29116(11) 0.31712(17) 0.0534(6) Uani 1 1 d . . . H31 H 0.1895 0.3262 0.3111 0.064 Uiso 1 1 calc R . . C32 C 0.30515(14) 0.28744(10) 0.35106(16) 0.0444(6) Uani 1 1 d . . . C33 C 0.35920(14) 0.33542(10) 0.37538(16) 0.0458(6) Uani 1 1 d . . . C34 C 0.44553(15) 0.32672(11) 0.41602(17) 0.0491(6) Uani 1 1 d . . . C35 C 0.32340(15) 0.39449(10) 0.36142(17) 0.0529(6) Uani 1 1 d . . . H35A H 0.3703 0.4206 0.3847 0.064 Uiso 1 1 calc R . . H35B H 0.2851 0.3991 0.4018 0.064 Uiso 1 1 calc R . . C36 C 0.27542(15) 0.41012(10) 0.25751(17) 0.0476(6) Uani 1 1 d . . . C37 C 0.31765(15) 0.41351(9) 0.18327(18) 0.0477(6) Uani 1 1 d . . . C38 C 0.40697(16) 0.40631(11) 0.2027(2) 0.0589(7) Uani 1 1 d . . . H38 H 0.4398 0.3990 0.2660 0.071 Uiso 1 1 calc R . . C39 C 0.44567(18) 0.40987(12) 0.1301(2) 0.0702(8) Uani 1 1 d . . . H39 H 0.5044 0.4049 0.1445 0.084 Uiso 1 1 calc R . . C40 C 0.3978(2) 0.42096(13) 0.0339(2) 0.0748(9) Uani 1 1 d . . . H40 H 0.4250 0.4235 -0.0149 0.090 Uiso 1 1 calc R . . C41 C 0.31263(19) 0.42796(11) 0.0123(2) 0.0628(7) Uani 1 1 d . . . H41 H 0.2813 0.4351 -0.0516 0.075 Uiso 1 1 calc R . . C42 C 0.27017(17) 0.42465(10) 0.08557(18) 0.0516(6) Uani 1 1 d . . . C43 C 0.18153(16) 0.43120(10) 0.06380(18) 0.0521(6) Uani 1 1 d . . . H43 H 0.1499 0.4365 -0.0006 0.063 Uiso 1 1 calc R . . C44 C 0.14009(16) 0.42999(10) 0.13459(18) 0.0493(6) Uani 1 1 d . . . C45 C 0.04630(17) 0.43605(10) 0.1106(2) 0.0539(6) Uani 1 1 d . . . C46 C 0.18920(16) 0.42133(10) 0.23343(18) 0.0498(6) Uani 1 1 d . . . C47 C 0.28914(17) 0.27418(12) 0.0882(2) 0.0656(8) Uani 1 1 d . . . H47A H 0.3253 0.3065 0.1047 0.098 Uiso 1 1 calc R . . H47B H 0.2476 0.2748 0.1241 0.098 Uiso 1 1 calc R . . H47C H 0.2604 0.2746 0.0197 0.098 Uiso 1 1 calc R . . C48 C 0.29812(17) 0.17040(11) 0.09215(19) 0.0658(8) Uani 1 1 d . . . H48A H 0.3402 0.1414 0.0994 0.099 Uiso 1 1 calc R . . H48B H 0.2611 0.1701 0.0268 0.099 Uiso 1 1 calc R . . H48C H 0.2651 0.1641 0.1370 0.099 Uiso 1 1 calc R . . C49 C 0.42287(18) 0.22724(13) 0.1545(2) 0.0624(7) Uani 1 1 d . . . H49 H 0.4472 0.2627 0.1665 0.075 Uiso 1 1 calc R . . C50 C 0.4788(3) 0.54744(18) 0.3482(3) 0.1291(16) Uani 1 1 d . . . H50A H 0.4511 0.5786 0.3096 0.194 Uiso 1 1 calc R . . H50B H 0.4950 0.5577 0.4158 0.194 Uiso 1 1 calc R . . H50C H 0.4403 0.5162 0.3380 0.194 Uiso 1 1 calc R . . C51 C 0.6079(2) 0.48929(19) 0.3732(3) 0.1318(17) Uani 1 1 d . . . H51A H 0.5736 0.4615 0.3927 0.198 Uiso 1 1 d R . . H51B H 0.6473 0.5052 0.4299 0.198 Uiso 1 1 d R . . H51C H 0.6392 0.4723 0.3330 0.198 Uiso 1 1 d R . . C52 C 0.5727(2) 0.55800(14) 0.2467(2) 0.0805(9) Uani 1 1 d . . . H52 H 0.5356 0.5859 0.2146 0.097 Uiso 1 1 calc R . . C53 C 0.3156(3) 0.56979(15) 0.8980(3) 0.1051(12) Uani 1 1 d . . . H53A H 0.2723 0.5646 0.8374 0.158 Uiso 1 1 calc R . . H53B H 0.3570 0.5402 0.9067 0.158 Uiso 1 1 calc R . . H53C H 0.3433 0.6052 0.8974 0.158 Uiso 1 1 calc R . . C54 C 0.3310(2) 0.57643(15) 1.0752(2) 0.0931(10) Uani 1 1 d . . . H54A H 0.3488 0.6148 1.0845 0.140 Uiso 1 1 d R . . H54B H 0.3804 0.5528 1.0855 0.140 Uiso 1 1 d R . . H54C H 0.3001 0.5667 1.1208 0.140 Uiso 1 1 d R . . C55 C 0.1944(2) 0.56431(11) 0.9617(2) 0.0687(8) Uani 1 1 d . . . H55 H 0.1614 0.5597 0.8977 0.082 Uiso 1 1 calc R . . C56 C 0.07410(17) 0.68483(11) 0.8336(2) 0.0648(7) Uani 1 1 d . . . H56A H 0.1153 0.6551 0.8435 0.097 Uiso 1 1 calc R . . H56B H 0.0384 0.6839 0.7676 0.097 Uiso 1 1 calc R . . H56C H 0.0395 0.6801 0.8771 0.097 Uiso 1 1 calc R . . C57 C 0.06835(17) 0.78881(11) 0.8284(2) 0.0661(8) Uani 1 1 d . . . H57A H 0.1056 0.8207 0.8433 0.099 Uiso 1 1 calc R . . H57B H 0.0279 0.7906 0.8656 0.099 Uiso 1 1 calc R . . H57C H 0.0385 0.7888 0.7602 0.099 Uiso 1 1 calc R . . C58 C 0.20084(17) 0.73985(12) 0.89316(19) 0.0607(7) Uani 1 1 d . . . H58 H 0.2266 0.7749 0.9052 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0528(11) 0.0692(14) 0.1017(16) -0.0017(11) 0.0009(11) -0.0084(10) O2 0.0463(10) 0.0726(14) 0.0894(15) 0.0017(11) 0.0015(10) 0.0042(10) O3 0.0466(10) 0.0583(12) 0.0738(13) 0.0040(9) 0.0053(9) 0.0095(9) O4 0.0528(10) 0.0637(12) 0.0546(11) 0.0007(9) 0.0231(8) -0.0078(9) O5 0.0528(11) 0.0856(15) 0.0714(13) -0.0002(11) 0.0194(10) -0.0092(10) O6 0.0561(11) 0.0874(15) 0.0647(13) -0.0082(11) 0.0057(9) -0.0080(11) O7 0.0546(12) 0.0735(15) 0.1100(18) 0.0024(12) -0.0001(11) 0.0030(10) O8 0.0505(11) 0.0756(14) 0.0926(15) -0.0012(11) 0.0040(10) -0.0103(10) O9 0.0556(11) 0.0583(12) 0.0730(13) -0.0035(9) 0.0071(9) -0.0161(9) O10 0.0624(11) 0.0674(13) 0.0679(13) 0.0030(10) 0.0102(10) 0.0065(11) O11 0.0609(12) 0.0733(14) 0.0747(13) -0.0112(10) 0.0231(10) -0.0007(10) O12 0.0599(11) 0.0759(13) 0.0600(12) 0.0023(9) 0.0275(9) 0.0086(10) O13 0.0564(12) 0.0672(14) 0.0967(16) -0.0016(11) 0.0025(10) -0.0045(10) O14 0.0591(13) 0.1170(19) 0.0783(14) -0.0098(13) 0.0232(11) -0.0053(12) O15 0.0661(12) 0.0794(14) 0.0674(13) 0.0062(11) 0.0175(10) 0.0117(10) O16 0.0592(12) 0.0653(14) 0.0959(16) 0.0006(11) 0.0004(10) 0.0022(10) N1 0.0488(13) 0.0557(14) 0.0506(13) -0.0052(10) 0.0100(10) -0.0109(10) N2 0.0731(16) 0.0642(16) 0.0745(17) -0.0078(13) 0.0282(14) -0.0130(13) N3 0.0772(17) 0.0603(15) 0.0711(17) 0.0025(12) 0.0291(14) 0.0077(13) N4 0.0526(13) 0.0511(13) 0.0486(13) -0.0021(10) 0.0107(10) -0.0074(10) C1 0.0508(16) 0.0634(19) 0.0532(16) -0.0008(14) 0.0095(13) -0.0073(14) C2 0.0436(14) 0.0536(16) 0.0443(14) 0.0032(12) 0.0119(11) -0.0001(12) C3 0.0536(16) 0.0489(16) 0.0477(15) 0.0004(12) 0.0138(12) -0.0039(12) C4 0.0459(14) 0.0502(15) 0.0403(14) 0.0039(11) 0.0137(11) 0.0039(12) C5 0.0588(17) 0.0507(16) 0.0542(16) 0.0051(12) 0.0169(12) 0.0059(13) C6 0.0548(17) 0.0610(19) 0.0674(18) 0.0120(14) 0.0164(14) 0.0171(14) C7 0.0439(15) 0.068(2) 0.0610(17) 0.0001(14) 0.0122(12) 0.0075(13) C8 0.0443(14) 0.0528(16) 0.0539(16) -0.0053(12) 0.0151(11) 0.0016(12) C9 0.0440(13) 0.0484(15) 0.0343(12) 0.0000(10) 0.0137(10) 0.0022(11) C10 0.0458(14) 0.0462(15) 0.0375(13) -0.0005(10) 0.0126(10) 0.0008(11) C11 0.0445(14) 0.0503(16) 0.0424(14) 0.0035(11) 0.0112(11) 0.0069(12) C12 0.0456(13) 0.0485(15) 0.0488(15) 0.0030(11) 0.0119(11) 0.0015(11) C13 0.0482(14) 0.0347(13) 0.0482(14) 0.0033(10) 0.0147(11) 0.0013(10) C14 0.0501(15) 0.0382(14) 0.0506(15) 0.0032(11) 0.0200(12) 0.0001(11) C15 0.0506(15) 0.0376(14) 0.0527(16) 0.0011(11) 0.0137(12) -0.0019(11) C16 0.0521(16) 0.0405(15) 0.0647(18) 0.0025(13) 0.0103(14) -0.0035(12) C17 0.0595(16) 0.0430(15) 0.0452(15) -0.0036(11) 0.0118(12) -0.0035(12) C18 0.0587(16) 0.0356(13) 0.0513(15) -0.0014(11) 0.0199(13) 0.0007(11) C19 0.077(2) 0.0567(17) 0.0511(16) -0.0048(13) 0.0290(14) -0.0031(14) C20 0.078(2) 0.073(2) 0.072(2) -0.0073(16) 0.0442(17) -0.0024(16) C21 0.0576(17) 0.071(2) 0.085(2) -0.0082(16) 0.0319(16) -0.0003(14) C22 0.0522(16) 0.0548(16) 0.0611(17) -0.0045(13) 0.0215(13) 0.0025(12) C23 0.0512(15) 0.0345(13) 0.0529(15) 0.0009(11) 0.0193(12) 0.0001(11) C24 0.0498(16) 0.071(2) 0.0574(17) 0.0000(15) 0.0137(13) -0.0013(15) C25 0.0476(14) 0.0558(17) 0.0456(14) -0.0015(12) 0.0145(11) -0.0039(12) C26 0.0538(15) 0.0508(16) 0.0509(15) 0.0000(12) 0.0179(12) 0.0015(12) C27 0.0477(14) 0.0526(16) 0.0394(13) -0.0024(11) 0.0175(11) -0.0066(12) C28 0.0622(17) 0.0527(17) 0.0531(16) -0.0052(12) 0.0182(13) -0.0085(13) C29 0.0581(18) 0.064(2) 0.0630(18) -0.0079(14) 0.0157(14) -0.0202(14) C30 0.0449(15) 0.078(2) 0.0639(18) 0.0014(15) 0.0156(13) -0.0097(14) C31 0.0485(15) 0.0593(17) 0.0532(16) 0.0038(13) 0.0158(12) -0.0056(13) C32 0.0454(14) 0.0548(16) 0.0365(13) -0.0006(11) 0.0172(10) -0.0068(12) C33 0.0500(15) 0.0528(16) 0.0367(13) 0.0006(11) 0.0156(11) -0.0043(12) C34 0.0489(15) 0.0538(16) 0.0453(14) -0.0015(12) 0.0143(11) -0.0121(12) C35 0.0568(15) 0.0536(16) 0.0503(15) -0.0028(12) 0.0183(12) -0.0070(12) C36 0.0566(15) 0.0404(14) 0.0483(15) -0.0016(11) 0.0188(12) -0.0037(11) C37 0.0571(16) 0.0358(14) 0.0536(16) -0.0022(11) 0.0215(13) -0.0064(11) C38 0.0579(17) 0.0634(18) 0.0598(17) 0.0012(13) 0.0236(14) -0.0077(13) C39 0.0612(18) 0.079(2) 0.079(2) 0.0030(17) 0.0347(16) -0.0043(15) C40 0.089(2) 0.083(2) 0.066(2) 0.0052(16) 0.0441(18) -0.0017(18) C41 0.080(2) 0.0600(18) 0.0535(17) 0.0012(13) 0.0273(15) 0.0001(15) C42 0.0666(18) 0.0392(14) 0.0541(16) -0.0013(11) 0.0254(14) -0.0044(12) C43 0.0654(17) 0.0398(14) 0.0501(15) 0.0010(11) 0.0148(13) -0.0001(12) C44 0.0586(16) 0.0357(14) 0.0545(16) -0.0020(11) 0.0174(13) -0.0011(11) C45 0.0619(17) 0.0364(14) 0.0619(18) -0.0029(12) 0.0150(15) 0.0000(12) C46 0.0632(17) 0.0413(14) 0.0520(16) -0.0014(11) 0.0277(13) -0.0014(12) C47 0.0577(17) 0.0678(19) 0.0693(19) -0.0068(15) 0.0147(14) 0.0019(14) C48 0.0707(18) 0.0653(19) 0.0595(18) -0.0052(14) 0.0151(14) -0.0230(15) C49 0.0579(18) 0.0616(19) 0.0646(18) -0.0070(15) 0.0122(14) -0.0120(15) C50 0.128(3) 0.124(4) 0.166(4) -0.043(3) 0.092(3) -0.024(3) C51 0.105(3) 0.110(3) 0.165(4) 0.052(3) 0.014(3) -0.007(2) C52 0.079(2) 0.080(2) 0.076(2) -0.0020(18) 0.0102(18) -0.0003(18) C53 0.146(3) 0.088(3) 0.111(3) 0.001(2) 0.086(3) 0.009(2) C54 0.076(2) 0.109(3) 0.095(3) -0.017(2) 0.0259(19) -0.0088(19) C55 0.085(2) 0.0545(18) 0.061(2) 0.0019(14) 0.0123(17) 0.0167(16) C56 0.0654(17) 0.0627(18) 0.0634(18) -0.0022(14) 0.0138(14) -0.0165(14) C57 0.0587(16) 0.0607(19) 0.0745(19) -0.0023(15) 0.0118(14) 0.0015(14) C58 0.0538(18) 0.0598(18) 0.0632(18) -0.0027(14) 0.0081(14) -0.0090(14) _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 C1 1.309(3) . ? O1 H1 0.8200 . ? O2 C1 1.222(3) . ? O3 C11 1.365(3) . ? O3 H3 0.8200 . ? O4 C14 1.357(3) . ? O4 H4 0.8200 . ? O5 C16 1.224(3) . ? O6 C16 1.326(3) . ? O6 H6 0.8200 . ? O7 C24 1.297(3) . ? O7 H7 0.8200 . ? O8 C24 1.231(3) . ? O9 C34 1.365(3) . ? O9 H9 0.8200 . ? O10 C45 1.312(3) . ? O10 H10 0.8200 . ? O11 C45 1.226(3) . ? O12 C46 1.353(3) . ? O12 H12 0.8200 . ? O13 C49 1.235(3) . ? O14 C52 1.242(4) . ? O15 C55 1.239(3) . ? O16 C58 1.233(3) . ? N1 C49 1.314(3) . ? N1 C47 1.444(3) . ? N1 C48 1.446(3) . ? N2 C52 1.322(4) . ? N2 C51 1.422(4) . ? N2 C50 1.449(4) . ? N3 C55 1.303(4) . ? N3 C54 1.443(4) . ? N3 C53 1.451(4) . ? N4 C58 1.311(3) . ? N4 C57 1.442(3) . ? N4 C56 1.451(3) . ? C1 C2 1.479(3) . ? C2 C3 1.365(3) . ? C2 C11 1.415(3) . ? C3 C4 1.399(3) . ? C3 H3A 0.9300 . ? C4 C5 1.414(3) . ? C4 C9 1.422(3) . ? C5 C6 1.351(3) . ? C5 H5 0.9300 . ? C6 C7 1.398(4) . ? C6 H6A 0.9300 . ? C7 C8 1.360(3) . ? C7 H7A 0.9300 . ? C8 C9 1.418(3) . ? C8 H8 0.9300 . ? C9 C10 1.427(3) . ? C10 C11 1.378(3) . ? C10 C12 1.523(3) . ? C12 C13 1.518(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.375(3) . ? C13 C23 1.427(3) . ? C14 C15 1.429(3) . ? C15 C17 1.367(3) . ? C15 C16 1.470(3) . ? C17 C18 1.401(3) . ? C17 H17 0.9300 . ? C18 C23 1.420(3) . ? C18 C19 1.421(3) . ? C19 C20 1.347(4) . ? C19 H19 0.9300 . ? C20 C21 1.398(4) . ? C20 H20 0.9300 . ? C21 C22 1.361(4) . ? C21 H21 0.9300 . ? C22 C23 1.421(3) . ? C22 H22 0.9300 . ? C24 C25 1.474(3) . ? C25 C26 1.373(3) . ? C25 C34 1.419(3) . ? C26 C27 1.402(3) . ? C26 H26 0.9300 . ? C27 C28 1.413(3) . ? C27 C32 1.421(3) . ? C28 C29 1.352(3) . ? C28 H28 0.9300 . ? C29 C30 1.394(4) . ? C29 H29 0.9300 . ? C30 C31 1.359(3) . ? C30 H30 0.9300 . ? C31 C32 1.409(3) . ? C31 H31 0.9300 . ? C32 C33 1.428(3) . ? C33 C34 1.380(3) . ? C33 C35 1.518(3) . ? C35 C36 1.520(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C46 1.377(3) . ? C36 C37 1.424(3) . ? C37 C38 1.415(3) . ? C37 C42 1.420(3) . ? C38 C39 1.363(4) . ? C38 H38 0.9300 . ? C39 C40 1.404(4) . ? C39 H39 0.9300 . ? C40 C41 1.346(4) . ? C40 H40 0.9300 . ? C41 C42 1.414(3) . ? C41 H41 0.9300 . ? C42 C43 1.400(3) . ? C43 C44 1.369(3) . ? C43 H43 0.9300 . ? C44 C46 1.431(3) . ? C44 C45 1.478(3) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49 0.9300 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55 0.9300 . ? 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 H58 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 H1 109.5 . . ? C11 O3 H3 109.5 . . ? C14 O4 H4 109.5 . . ? C16 O6 H6 109.5 . . ? C24 O7 H7 109.5 . . ? C34 O9 H9 109.5 . . ? C45 O10 H10 109.5 . . ? C46 O12 H12 109.5 . . ? C49 N1 C47 120.8(2) . . ? C49 N1 C48 120.7(2) . . ? C47 N1 C48 118.5(2) . . ? C52 N2 C51 121.2(3) . . ? C52 N2 C50 120.5(3) . . ? C51 N2 C50 118.3(3) . . ? C55 N3 C54 119.8(3) . . ? C55 N3 C53 121.7(3) . . ? C54 N3 C53 118.3(3) . . ? C58 N4 C57 121.4(2) . . ? C58 N4 C56 120.1(2) . . ? C57 N4 C56 118.4(2) . . ? O2 C1 O1 122.7(2) . . ? O2 C1 C2 122.9(3) . . ? O1 C1 C2 114.4(2) . . ? C3 C2 C11 119.5(2) . . ? C3 C2 C1 120.4(2) . . ? C11 C2 C1 120.1(2) . . ? C2 C3 C4 121.3(2) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C3 C4 C5 121.4(2) . . ? C3 C4 C9 118.8(2) . . ? C5 C4 C9 119.7(2) . . ? C6 C5 C4 121.6(2) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 118.8(2) . . ? C5 C6 H6A 120.6 . . ? C7 C6 H6A 120.6 . . ? C8 C7 C6 122.0(2) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C7 C8 C9 120.9(2) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C4 117.0(2) . . ? C8 C9 C10 122.7(2) . . ? C4 C9 C10 120.3(2) . . ? C11 C10 C9 117.9(2) . . ? C11 C10 C12 120.4(2) . . ? C9 C10 C12 121.6(2) . . ? O3 C11 C10 118.3(2) . . ? O3 C11 C2 119.7(2) . . ? C10 C11 C2 122.0(2) . . ? C13 C12 C10 116.04(19) . . ? C13 C12 H12A 108.3 . . ? C10 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? C10 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C14 C13 C23 118.5(2) . . ? C14 C13 C12 120.1(2) . . ? C23 C13 C12 121.4(2) . . ? O4 C14 C13 118.2(2) . . ? O4 C14 C15 120.3(2) . . ? C13 C14 C15 121.5(2) . . ? C17 C15 C14 119.2(2) . . ? C17 C15 C16 121.1(2) . . ? C14 C15 C16 119.7(2) . . ? O5 C16 O6 121.6(2) . . ? O5 C16 C15 123.5(2) . . ? O6 C16 C15 114.9(2) . . ? C15 C17 C18 121.5(2) . . ? C15 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C23 119.0(2) . . ? C17 C18 C19 121.4(2) . . ? C23 C18 C19 119.5(2) . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.9(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 121.7(3) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 117.8(2) . . ? C18 C23 C13 120.1(2) . . ? C22 C23 C13 122.1(2) . . ? O8 C24 O7 123.2(2) . . ? O8 C24 C25 122.0(3) . . ? O7 C24 C25 114.8(2) . . ? C26 C25 C34 119.0(2) . . ? C26 C25 C24 120.3(2) . . ? C34 C25 C24 120.7(2) . . ? C25 C26 C27 121.4(2) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C28 120.9(2) . . ? C26 C27 C32 118.9(2) . . ? C28 C27 C32 120.1(2) . . ? C29 C28 C27 120.9(3) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C30 119.2(2) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 121.6(2) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C32 121.3(3) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C31 C32 C27 116.8(2) . . ? C31 C32 C33 122.9(2) . . ? C27 C32 C33 120.3(2) . . ? C34 C33 C32 117.9(2) . . ? C34 C33 C35 120.3(2) . . ? C32 C33 C35 121.7(2) . . ? O9 C34 C33 118.5(2) . . ? O9 C34 C25 119.3(2) . . ? C33 C34 C25 122.2(2) . . ? C33 C35 C36 115.46(19) . . ? C33 C35 H35A 108.4 . . ? C36 C35 H35A 108.4 . . ? C33 C35 H35B 108.4 . . ? C36 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? C46 C36 C37 118.6(2) . . ? C46 C36 C35 120.0(2) . . ? C37 C36 C35 121.4(2) . . ? C38 C37 C42 117.4(2) . . ? C38 C37 C36 122.4(2) . . ? C42 C37 C36 120.2(2) . . ? C39 C38 C37 121.1(3) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 120.8(3) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C41 C40 C39 120.0(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.9(3) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C43 C42 C41 121.4(2) . . ? C43 C42 C37 118.8(2) . . ? C41 C42 C37 119.8(2) . . ? C44 C43 C42 121.9(2) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C43 C44 C46 118.7(2) . . ? C43 C44 C45 121.4(2) . . ? C46 C44 C45 119.9(2) . . ? O11 C45 O10 122.8(2) . . ? O11 C45 C44 123.0(3) . . ? O10 C45 C44 114.2(2) . . ? O12 C46 C36 118.2(2) . . ? O12 C46 C44 120.2(2) . . ? C36 C46 C44 121.5(2) . . ? N1 C47 H47A 109.5 . . ? N1 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N1 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N1 C48 H48A 109.5 . . ? N1 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N1 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O13 C49 N1 124.6(3) . . ? O13 C49 H49 117.7 . . ? N1 C49 H49 117.7 . . ? N2 C50 H50A 109.5 . . ? N2 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N2 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N2 C51 H51A 109.5 . . ? N2 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O14 C52 N2 124.8(3) . . ? O14 C52 H52 117.6 . . ? N2 C52 H52 117.6 . . ? N3 C53 H53A 109.5 . . ? N3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N3 C54 H54A 109.5 . . ? N3 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N3 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O15 C55 N3 125.2(3) . . ? O15 C55 H55 117.4 . . ? N3 C55 H55 117.4 . . ? N4 C56 H56A 109.5 . . ? N4 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N4 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N4 C57 H57A 109.5 . . ? N4 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N4 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O16 C58 N4 124.7(3) . . ? O16 C58 H58 117.6 . . ? N4 C58 H58 117.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 177.9(2) . . . . ? O1 C1 C2 C3 -2.7(4) . . . . ? O2 C1 C2 C11 -4.0(4) . . . . ? O1 C1 C2 C11 175.4(2) . . . . ? C11 C2 C3 C4 -1.7(4) . . . . ? C1 C2 C3 C4 176.4(2) . . . . ? C2 C3 C4 C5 -178.9(2) . . . . ? C2 C3 C4 C9 -1.3(3) . . . . ? C3 C4 C5 C6 176.6(2) . . . . ? C9 C4 C5 C6 -0.9(4) . . . . ? C4 C5 C6 C7 -1.5(4) . . . . ? C5 C6 C7 C8 1.6(4) . . . . ? C6 C7 C8 C9 0.8(4) . . . . ? C7 C8 C9 C4 -3.2(3) . . . . ? C7 C8 C9 C10 178.5(2) . . . . ? C3 C4 C9 C8 -174.4(2) . . . . ? C5 C4 C9 C8 3.3(3) . . . . ? C3 C4 C9 C10 4.0(3) . . . . ? C5 C4 C9 C10 -178.4(2) . . . . ? C8 C9 C10 C11 174.8(2) . . . . ? C4 C9 C10 C11 -3.5(3) . . . . ? C8 C9 C10 C12 -2.1(3) . . . . ? C4 C9 C10 C12 179.7(2) . . . . ? C9 C10 C11 O3 -179.42(19) . . . . ? C12 C10 C11 O3 -2.5(3) . . . . ? C9 C10 C11 C2 0.4(3) . . . . ? C12 C10 C11 C2 177.3(2) . . . . ? C3 C2 C11 O3 -178.0(2) . . . . ? C1 C2 C11 O3 3.9(3) . . . . ? C3 C2 C11 C10 2.2(4) . . . . ? C1 C2 C11 C10 -175.9(2) . . . . ? C11 C10 C12 C13 122.4(2) . . . . ? C9 C10 C12 C13 -60.8(3) . . . . ? C10 C12 C13 C14 113.1(2) . . . . ? C10 C12 C13 C23 -66.5(3) . . . . ? C23 C13 C14 O4 -176.31(19) . . . . ? C12 C13 C14 O4 4.0(3) . . . . ? C23 C13 C14 C15 6.0(3) . . . . ? C12 C13 C14 C15 -173.7(2) . . . . ? O4 C14 C15 C17 178.4(2) . . . . ? C13 C14 C15 C17 -4.0(3) . . . . ? O4 C14 C15 C16 -5.1(3) . . . . ? C13 C14 C15 C16 172.6(2) . . . . ? C17 C15 C16 O5 179.8(2) . . . . ? C14 C15 C16 O5 3.3(4) . . . . ? C17 C15 C16 O6 0.9(3) . . . . ? C14 C15 C16 O6 -175.6(2) . . . . ? C14 C15 C17 C18 -0.1(3) . . . . ? C16 C15 C17 C18 -176.6(2) . . . . ? C15 C17 C18 C23 1.8(3) . . . . ? C15 C17 C18 C19 179.9(2) . . . . ? C17 C18 C19 C20 -179.2(2) . . . . ? C23 C18 C19 C20 -1.1(4) . . . . ? C18 C19 C20 C21 0.0(4) . . . . ? C19 C20 C21 C22 0.9(4) . . . . ? C20 C21 C22 C23 -0.6(4) . . . . ? C17 C18 C23 C22 179.5(2) . . . . ? C19 C18 C23 C22 1.3(3) . . . . ? C17 C18 C23 C13 0.3(3) . . . . ? C19 C18 C23 C13 -177.9(2) . . . . ? C21 C22 C23 C18 -0.5(3) . . . . ? C21 C22 C23 C13 178.7(2) . . . . ? C14 C13 C23 C18 -4.1(3) . . . . ? C12 C13 C23 C18 175.5(2) . . . . ? C14 C13 C23 C22 176.7(2) . . . . ? C12 C13 C23 C22 -3.6(3) . . . . ? O8 C24 C25 C26 177.2(2) . . . . ? O7 C24 C25 C26 -2.9(4) . . . . ? O8 C24 C25 C34 -3.2(4) . . . . ? O7 C24 C25 C34 176.7(2) . . . . ? C34 C25 C26 C27 -2.9(4) . . . . ? C24 C25 C26 C27 176.7(2) . . . . ? C25 C26 C27 C28 -178.7(2) . . . . ? C25 C26 C27 C32 -0.6(3) . . . . ? C26 C27 C28 C29 176.0(2) . . . . ? C32 C27 C28 C29 -2.1(4) . . . . ? C27 C28 C29 C30 -0.7(4) . . . . ? C28 C29 C30 C31 1.8(4) . . . . ? C29 C30 C31 C32 -0.1(4) . . . . ? C30 C31 C32 C27 -2.5(3) . . . . ? C30 C31 C32 C33 178.8(2) . . . . ? C26 C27 C32 C31 -174.5(2) . . . . ? C28 C27 C32 C31 3.6(3) . . . . ? C26 C27 C32 C33 4.2(3) . . . . ? C28 C27 C32 C33 -177.7(2) . . . . ? C31 C32 C33 C34 174.4(2) . . . . ? C27 C32 C33 C34 -4.3(3) . . . . ? C31 C32 C33 C35 -3.1(3) . . . . ? C27 C32 C33 C35 178.2(2) . . . . ? C32 C33 C34 O9 -178.9(2) . . . . ? C35 C33 C34 O9 -1.4(3) . . . . ? C32 C33 C34 C25 0.8(3) . . . . ? C35 C33 C34 C25 178.3(2) . . . . ? C26 C25 C34 O9 -177.5(2) . . . . ? C24 C25 C34 O9 2.9(4) . . . . ? C26 C25 C34 C33 2.8(4) . . . . ? C24 C25 C34 C33 -176.8(2) . . . . ? C34 C33 C35 C36 122.2(2) . . . . ? C32 C33 C35 C36 -60.4(3) . . . . ? C33 C35 C36 C46 114.7(2) . . . . ? C33 C35 C36 C37 -65.3(3) . . . . ? C46 C36 C37 C38 175.8(2) . . . . ? C35 C36 C37 C38 -4.3(3) . . . . ? C46 C36 C37 C42 -4.0(3) . . . . ? C35 C36 C37 C42 175.9(2) . . . . ? C42 C37 C38 C39 -0.1(4) . . . . ? C36 C37 C38 C39 -179.9(2) . . . . ? C37 C38 C39 C40 0.2(4) . . . . ? C38 C39 C40 C41 -0.3(5) . . . . ? C39 C40 C41 C42 0.4(4) . . . . ? C40 C41 C42 C43 -179.2(3) . . . . ? C40 C41 C42 C37 -0.3(4) . . . . ? C38 C37 C42 C43 179.1(2) . . . . ? C36 C37 C42 C43 -1.1(3) . . . . ? C38 C37 C42 C41 0.2(3) . . . . ? C36 C37 C42 C41 180.0(2) . . . . ? C41 C42 C43 C44 -177.7(2) . . . . ? C37 C42 C43 C44 3.4(3) . . . . ? C42 C43 C44 C46 -0.5(3) . . . . ? C42 C43 C44 C45 -179.0(2) . . . . ? C43 C44 C45 O11 -174.7(2) . . . . ? C46 C44 C45 O11 6.8(4) . . . . ? C43 C44 C45 O10 6.4(3) . . . . ? C46 C44 C45 O10 -172.1(2) . . . . ? C37 C36 C46 O12 -176.4(2) . . . . ? C35 C36 C46 O12 3.7(3) . . . . ? C37 C36 C46 C44 7.1(3) . . . . ? C35 C36 C46 C44 -172.9(2) . . . . ? C43 C44 C46 O12 178.6(2) . . . . ? C45 C44 C46 O12 -2.9(3) . . . . ? C43 C44 C46 C36 -4.9(3) . . . . ? C45 C44 C46 C36 173.6(2) . . . . ? C47 N1 C49 O13 178.2(3) . . . . ? C48 N1 C49 O13 0.7(4) . . . . ? C51 N2 C52 O14 0.4(5) . . . . ? C50 N2 C52 O14 179.7(3) . . . . ? C54 N3 C55 O15 -0.4(4) . . . . ? C53 N3 C55 O15 -176.5(3) . . . . ? C57 N4 C58 O16 179.0(3) . . . . ? C56 N4 C58 O16 1.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.327 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.036 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 631541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H36 Mn N2 O12' _chemical_formula_weight 659.54 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' Mn Mn 0.3368 0.7283 '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 9.087(2) _cell_length_b 13.014(3) _cell_length_c 13.168(3) _cell_angle_alpha 87.749(3) _cell_angle_beta 89.854(3) _cell_angle_gamma 80.647(3) _cell_volume 1535.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3103 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.73 _exptl_crystal_description Lamellar _exptl_crystal_colour Pale-Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.784087 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 8397 _diffrn_reflns_av_R_equivalents 0.0141 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5351 _reflns_number_gt 4388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0640P)^2^+0.4319P] 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 5351 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.002 _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 Mn1 Mn 0.24111(4) 1.01005(2) 0.25426(2) 0.03947(13) Uani 1 1 d . . . O1 O 0.4154(2) 1.04824(18) 0.15802(18) 0.0775(6) Uani 1 1 d . . . O2 O 0.3071(3) 0.84563(15) 0.27197(18) 0.0796(6) Uani 1 1 d . . . O3 O 0.3663(2) 1.03323(15) 0.38968(14) 0.0639(5) Uani 1 1 d . . . H3A H 0.4473 1.0580 0.3878 0.096 Uiso 1 1 d R . . H3B H 0.3545 0.9948 0.4418 0.096 Uiso 1 1 d R . . O4 O 0.0614(2) 0.98426(14) 0.36266(13) 0.0559(5) Uani 1 1 d . . . H4A H 0.0018 1.0361 0.3840 0.084 Uiso 1 1 d R . . H4B H 0.1131 0.9483 0.4092 0.084 Uiso 1 1 d R . . O5 O 0.1188(2) 0.98467(14) 0.12204(13) 0.0616(5) Uani 1 1 d . . . H5A H 0.0529 0.9452 0.1254 0.092 Uiso 1 1 d R . . H5B H 0.1208 1.0224 0.0681 0.092 Uiso 1 1 d R . . O6 O 0.1435(2) 1.17535(12) 0.23354(12) 0.0531(4) Uani 1 1 d . . . H6A H 0.1251 1.1946 0.1718 0.080 Uiso 1 1 d R . . H6B H 0.0918 1.2122 0.2769 0.080 Uiso 1 1 d R . . O7 O 0.07128(16) 0.71255(12) 0.63760(12) 0.0400(4) Uani 1 1 d . . . H7 H 0.0669 0.7614 0.5959 0.060 Uiso 1 1 calc R . . O8 O 0.14896(18) 0.86160(12) 0.53661(12) 0.0474(4) Uani 1 1 d . . . O9 O 0.3740(2) 0.90194(15) 0.55516(15) 0.0654(6) Uani 1 1 d . . . O10 O 0.1060(2) 0.42081(13) 0.94879(12) 0.0570(5) Uani 1 1 d . . . H10 H 0.1057 0.3781 0.9963 0.086 Uiso 1 1 calc R . . O11 O 0.1030(2) 0.24697(14) 1.03953(13) 0.0612(5) Uani 1 1 d . . . O12 O 0.1138(2) 0.10372(14) 0.95210(13) 0.0614(5) Uani 1 1 d . . . N1 N 0.5914(3) 1.13047(18) 0.08734(19) 0.0634(7) Uani 1 1 d . . . N2 N 0.3358(2) 0.69160(14) 0.35649(16) 0.0444(5) Uani 1 1 d . . . C1 C 0.5362(5) 1.0718(3) 0.1553(3) 0.0859(10) Uani 1 1 d . . . H1 H 0.5998 1.0449 0.2085 0.103 Uiso 1 1 calc R . . C2 C 0.5117(6) 1.1780(4) 0.0019(4) 0.1278(17) Uani 1 1 d . . . H2A H 0.4289 1.1429 -0.0109 0.192 Uiso 1 1 calc R . . H2B H 0.5761 1.1737 -0.0561 0.192 Uiso 1 1 calc R . . H2C H 0.4756 1.2498 0.0145 0.192 Uiso 1 1 calc R . . C3 C 0.7419(5) 1.1514(4) 0.1010(4) 0.1230(18) Uani 1 1 d . . . H3A' H 0.7877 1.1101 0.1580 0.184 Uiso 1 1 calc R . . H3B' H 0.7387 1.2239 0.1132 0.184 Uiso 1 1 calc R . . H3C' H 0.7989 1.1339 0.0408 0.184 Uiso 1 1 calc R . . C4 C 0.3840(3) 0.7746(2) 0.3225(2) 0.0597(7) Uani 1 1 d . . . H4 H 0.4821 0.7812 0.3368 0.072 Uiso 1 1 calc R . . C5 C 0.4328(4) 0.6093(2) 0.4131(2) 0.0690(8) Uani 1 1 d . . . H5A' H 0.5282 0.6300 0.4230 0.103 Uiso 1 1 calc R . . H5B' H 0.4450 0.5466 0.3758 0.103 Uiso 1 1 calc R . . H5C' H 0.3890 0.5971 0.4780 0.103 Uiso 1 1 calc R . . C6 C 0.1842(3) 0.6764(3) 0.3420(3) 0.0804(10) Uani 1 1 d . . . H6A' H 0.1333 0.7316 0.2983 0.121 Uiso 1 1 calc R . . H6B' H 0.1347 0.6767 0.4065 0.121 Uiso 1 1 calc R . . H6C' H 0.1833 0.6107 0.3115 0.121 Uiso 1 1 calc R . . C7 C 0.2800(3) 0.84461(17) 0.57380(16) 0.0400(5) Uani 1 1 d . . . C8 C 0.3212(2) 0.75052(15) 0.64375(15) 0.0329(5) Uani 1 1 d . . . C9 C 0.4637(2) 0.72392(16) 0.67995(16) 0.0371(5) Uani 1 1 d . . . H9 H 0.5349 0.7643 0.6597 0.045 Uiso 1 1 calc R . . C10 C 0.5058(2) 0.63747(16) 0.74668(16) 0.0351(5) Uani 1 1 d . . . C11 C 0.6537(3) 0.61077(18) 0.78331(19) 0.0447(5) Uani 1 1 d . . . H11 H 0.7246 0.6511 0.7623 0.054 Uiso 1 1 calc R . . C12 C 0.6945(3) 0.5276(2) 0.8484(2) 0.0511(6) Uani 1 1 d . . . H12 H 0.7928 0.5099 0.8706 0.061 Uiso 1 1 calc R . . C13 C 0.5864(3) 0.4690(2) 0.8817(2) 0.0553(7) Uani 1 1 d . . . H13 H 0.6137 0.4124 0.9269 0.066 Uiso 1 1 calc R . . C14 C 0.4419(3) 0.49263(18) 0.84973(18) 0.0470(6) Uani 1 1 d . . . H14 H 0.3726 0.4528 0.8745 0.056 Uiso 1 1 calc R . . C15 C 0.3953(2) 0.57670(15) 0.77947(15) 0.0336(5) Uani 1 1 d . . . C16 C 0.2467(2) 0.60296(15) 0.74147(15) 0.0315(4) Uani 1 1 d . . . C17 C 0.2131(2) 0.68747(15) 0.67437(15) 0.0313(4) Uani 1 1 d . . . C18 C 0.1205(2) 0.54688(16) 0.77783(17) 0.0381(5) Uani 1 1 d . . . H18A H 0.0998 0.5642 0.8480 0.046 Uiso 1 1 calc R . . H18B H 0.0322 0.5756 0.7386 0.046 Uiso 1 1 calc R . . C19 C 0.1410(2) 0.42884(16) 0.77262(16) 0.0320(4) Uani 1 1 d . . . C20 C 0.1284(2) 0.37053(16) 0.86089(16) 0.0356(5) Uani 1 1 d . . . C21 C 0.1383(2) 0.26040(16) 0.86146(16) 0.0362(5) Uani 1 1 d . . . C22 C 0.1169(3) 0.19890(18) 0.95785(18) 0.0446(6) Uani 1 1 d . . . C23 C 0.1684(2) 0.21110(16) 0.77244(17) 0.0378(5) Uani 1 1 d . . . H23 H 0.1797 0.1388 0.7728 0.045 Uiso 1 1 calc R . . C24 C 0.1827(2) 0.26665(16) 0.68000(16) 0.0345(5) Uani 1 1 d . . . C25 C 0.2088(3) 0.21509(19) 0.58740(18) 0.0433(5) Uani 1 1 d . . . H25 H 0.2245 0.1427 0.5878 0.052 Uiso 1 1 calc R . . C26 C 0.2111(3) 0.2705(2) 0.49766(17) 0.0476(6) Uani 1 1 d . . . H26 H 0.2292 0.2361 0.4372 0.057 Uiso 1 1 calc R . . C27 C 0.1861(3) 0.3800(2) 0.49663(17) 0.0477(6) Uani 1 1 d . . . H27 H 0.1845 0.4174 0.4349 0.057 Uiso 1 1 calc R . . C28 C 0.1644(2) 0.43191(18) 0.58419(16) 0.0388(5) Uani 1 1 d . . . H28 H 0.1496 0.5044 0.5815 0.047 Uiso 1 1 calc R . . C29 C 0.1638(2) 0.37747(16) 0.67998(15) 0.0315(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0492(2) 0.0364(2) 0.0341(2) 0.00746(14) -0.00426(15) -0.01276(15) O1 0.0605(13) 0.0840(15) 0.0932(16) -0.0009(12) 0.0252(11) -0.0286(11) O2 0.1115(18) 0.0400(11) 0.0830(15) 0.0098(10) -0.0145(13) -0.0019(11) O3 0.0820(13) 0.0686(12) 0.0500(10) 0.0256(9) -0.0266(9) -0.0448(10) O4 0.0601(11) 0.0569(11) 0.0468(10) 0.0198(8) 0.0061(8) -0.0034(8) O5 0.0935(14) 0.0608(11) 0.0400(9) 0.0190(8) -0.0218(9) -0.0452(10) O6 0.0821(13) 0.0408(9) 0.0332(9) 0.0080(7) 0.0039(8) -0.0028(8) O7 0.0376(8) 0.0405(9) 0.0416(9) 0.0140(7) -0.0065(7) -0.0095(7) O8 0.0487(10) 0.0463(9) 0.0464(9) 0.0190(7) -0.0072(8) -0.0107(7) O9 0.0692(12) 0.0644(12) 0.0688(12) 0.0386(10) -0.0236(10) -0.0391(10) O10 0.0989(14) 0.0432(9) 0.0317(9) -0.0009(7) 0.0147(9) -0.0199(9) O11 0.0985(15) 0.0541(11) 0.0335(9) 0.0116(8) 0.0014(9) -0.0226(10) O12 0.0980(15) 0.0475(10) 0.0466(10) 0.0198(8) -0.0188(9) -0.0401(10) N1 0.0692(15) 0.0569(14) 0.0689(16) -0.0101(12) 0.0330(13) -0.0227(12) N2 0.0386(10) 0.0358(10) 0.0586(13) 0.0006(9) -0.0038(9) -0.0059(8) C1 0.102(3) 0.076(2) 0.082(2) -0.0191(19) 0.018(2) -0.015(2) C2 0.138(4) 0.142(4) 0.097(3) 0.024(3) 0.004(3) -0.009(3) C3 0.089(3) 0.151(4) 0.142(4) -0.079(3) 0.033(3) -0.040(3) C4 0.0589(16) 0.0503(16) 0.0708(19) -0.0014(14) -0.0019(14) -0.0118(13) C5 0.076(2) 0.0515(16) 0.074(2) 0.0026(14) -0.0108(16) 0.0055(14) C6 0.0503(17) 0.089(2) 0.106(3) -0.008(2) -0.0099(17) -0.0228(16) C7 0.0507(14) 0.0381(12) 0.0329(11) 0.0072(9) -0.0022(10) -0.0140(10) C8 0.0401(12) 0.0304(10) 0.0293(11) 0.0014(8) 0.0006(9) -0.0095(9) C9 0.0400(12) 0.0356(11) 0.0384(12) 0.0022(9) 0.0029(9) -0.0147(9) C10 0.0390(12) 0.0330(11) 0.0344(11) -0.0026(9) -0.0013(9) -0.0091(9) C11 0.0404(13) 0.0442(13) 0.0515(14) -0.0002(11) -0.0042(11) -0.0137(10) C12 0.0435(13) 0.0546(15) 0.0545(15) 0.0033(12) -0.0149(11) -0.0067(11) C13 0.0587(16) 0.0498(15) 0.0554(16) 0.0169(12) -0.0159(13) -0.0069(12) C14 0.0507(14) 0.0444(13) 0.0465(14) 0.0145(11) -0.0084(11) -0.0131(11) C15 0.0408(12) 0.0300(10) 0.0309(11) 0.0000(8) -0.0019(9) -0.0088(9) C16 0.0383(11) 0.0285(10) 0.0293(10) 0.0004(8) 0.0007(8) -0.0102(8) C17 0.0353(11) 0.0305(10) 0.0286(10) -0.0007(8) -0.0010(8) -0.0072(8) C18 0.0393(12) 0.0325(11) 0.0426(12) 0.0069(9) 0.0039(9) -0.0083(9) C19 0.0313(10) 0.0322(11) 0.0337(11) 0.0060(9) -0.0010(8) -0.0103(8) C20 0.0402(12) 0.0361(11) 0.0320(11) 0.0019(9) 0.0011(9) -0.0113(9) C21 0.0407(12) 0.0359(11) 0.0337(11) 0.0067(9) -0.0048(9) -0.0134(9) C22 0.0526(14) 0.0451(14) 0.0392(13) 0.0159(11) -0.0088(11) -0.0208(11) C23 0.0416(12) 0.0307(11) 0.0423(13) 0.0051(9) -0.0067(10) -0.0110(9) C24 0.0317(11) 0.0394(11) 0.0335(11) 0.0006(9) -0.0034(9) -0.0093(9) C25 0.0414(13) 0.0476(13) 0.0425(13) -0.0065(10) -0.0021(10) -0.0106(10) C26 0.0429(13) 0.0706(17) 0.0323(12) -0.0089(11) -0.0003(10) -0.0164(12) C27 0.0483(14) 0.0678(17) 0.0306(12) 0.0071(11) -0.0037(10) -0.0224(12) C28 0.0388(12) 0.0454(13) 0.0346(12) 0.0095(10) -0.0037(9) -0.0162(10) C29 0.0254(10) 0.0389(11) 0.0316(11) 0.0065(9) -0.0033(8) -0.0110(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 Mn1 O2 2.130(2) . ? Mn1 O5 2.1332(17) . ? Mn1 O1 2.135(2) . ? Mn1 O3 2.1748(17) . ? Mn1 O6 2.1963(17) . ? Mn1 O4 2.2240(17) . ? O1 C1 1.186(4) . ? O2 C4 1.237(3) . ? O3 H3A 0.8498 . ? O3 H3B 0.8501 . ? O4 H4A 0.8495 . ? O4 H4B 0.8505 . ? O5 H5A 0.8500 . ? O5 H5B 0.8496 . ? O6 H6A 0.8502 . ? O6 H6B 0.8501 . ? O7 C17 1.363(2) . ? O7 H7 0.8200 . ? O8 C7 1.271(3) . ? O9 C7 1.240(3) . ? O10 C20 1.351(3) . ? O10 H10 0.8200 . ? O11 C22 1.261(3) . ? O12 C22 1.249(3) . ? N1 C1 1.305(4) . ? N1 C2 1.406(5) . ? N1 C3 1.450(4) . ? N2 C4 1.294(3) . ? N2 C6 1.438(3) . ? N2 C5 1.454(3) . ? C1 H1 0.9300 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A' 0.9600 . ? C3 H3B' 0.9600 . ? C3 H3C' 0.9600 . ? C4 H4 0.9300 . ? C5 H5A' 0.9600 . ? C5 H5B' 0.9600 . ? C5 H5C' 0.9600 . ? C6 H6A' 0.9600 . ? C6 H6B' 0.9600 . ? C6 H6C' 0.9600 . ? C7 C8 1.501(3) . ? C8 C9 1.366(3) . ? C8 C17 1.426(3) . ? C9 C10 1.403(3) . ? C9 H9 0.9300 . ? C10 C11 1.414(3) . ? C10 C15 1.431(3) . ? C11 C12 1.358(3) . ? C11 H11 0.9300 . ? C12 C13 1.399(4) . ? C12 H12 0.9300 . ? C13 C14 1.363(4) . ? C13 H13 0.9300 . ? C14 C15 1.416(3) . ? C14 H14 0.9300 . ? C15 C16 1.425(3) . ? C16 C17 1.378(3) . ? C16 C18 1.523(3) . ? C18 C19 1.521(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.378(3) . ? C19 C29 1.413(3) . ? C20 C21 1.421(3) . ? C21 C23 1.364(3) . ? C21 C22 1.503(3) . ? C23 C24 1.408(3) . ? C23 H23 0.9300 . ? C24 C25 1.416(3) . ? C24 C29 1.424(3) . ? C25 C26 1.362(3) . ? C25 H25 0.9300 . ? C26 C27 1.404(4) . ? C26 H26 0.9300 . ? C27 C28 1.357(3) . ? C27 H27 0.9300 . ? C28 C29 1.423(3) . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O5 88.37(8) . . ? O2 Mn1 O1 100.15(10) . . ? O5 Mn1 O1 88.92(9) . . ? O2 Mn1 O3 90.71(8) . . ? O5 Mn1 O3 179.07(6) . . ? O1 Mn1 O3 91.41(9) . . ? O2 Mn1 O6 172.55(8) . . ? O5 Mn1 O6 86.69(7) . . ? O1 Mn1 O6 85.33(8) . . ? O3 Mn1 O6 94.20(7) . . ? O2 Mn1 O4 84.12(8) . . ? O5 Mn1 O4 94.87(7) . . ? O1 Mn1 O4 174.39(8) . . ? O3 Mn1 O4 84.86(7) . . ? O6 Mn1 O4 90.75(7) . . ? C1 O1 Mn1 145.4(3) . . ? C4 O2 Mn1 145.0(2) . . ? Mn1 O3 H3A 123.2 . . ? Mn1 O3 H3B 116.6 . . ? H3A O3 H3B 115.6 . . ? Mn1 O4 H4A 119.8 . . ? Mn1 O4 H4B 100.0 . . ? H4A O4 H4B 114.1 . . ? Mn1 O5 H5A 120.5 . . ? Mn1 O5 H5B 121.3 . . ? H5A O5 H5B 117.0 . . ? Mn1 O6 H6A 113.5 . . ? Mn1 O6 H6B 126.1 . . ? H6A O6 H6B 115.1 . . ? C17 O7 H7 109.5 . . ? C20 O10 H10 109.5 . . ? C1 N1 C2 123.7(4) . . ? C1 N1 C3 119.0(4) . . ? C2 N1 C3 117.2(4) . . ? C4 N2 C6 122.2(2) . . ? C4 N2 C5 121.2(2) . . ? C6 N2 C5 116.5(2) . . ? O1 C1 N1 128.5(4) . . ? O1 C1 H1 115.7 . . ? N1 C1 H1 115.7 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A' 109.5 . . ? N1 C3 H3B' 109.5 . . ? H3A' C3 H3B' 109.5 . . ? N1 C3 H3C' 109.5 . . ? H3A' C3 H3C' 109.5 . . ? H3B' C3 H3C' 109.5 . . ? O2 C4 N2 123.8(3) . . ? O2 C4 H4 118.1 . . ? N2 C4 H4 118.1 . . ? N2 C5 H5A' 109.5 . . ? N2 C5 H5B' 109.5 . . ? H5A' C5 H5B' 109.5 . . ? N2 C5 H5C' 109.5 . . ? H5A' C5 H5C' 109.5 . . ? H5B' C5 H5C' 109.5 . . ? N2 C6 H6A' 109.5 . . ? N2 C6 H6B' 109.5 . . ? H6A' C6 H6B' 109.5 . . ? N2 C6 H6C' 109.5 . . ? H6A' C6 H6C' 109.5 . . ? H6B' C6 H6C' 109.5 . . ? O9 C7 O8 123.2(2) . . ? O9 C7 C8 119.0(2) . . ? O8 C7 C8 117.78(19) . . ? C9 C8 C17 118.61(19) . . ? C9 C8 C7 120.38(19) . . ? C17 C8 C7 121.01(19) . . ? C8 C9 C10 121.99(19) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C9 C10 C11 121.3(2) . . ? C9 C10 C15 118.9(2) . . ? C11 C10 C15 119.7(2) . . ? C12 C11 C10 121.5(2) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 118.9(2) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 121.7(2) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 121.3(2) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 123.55(19) . . ? C14 C15 C10 116.8(2) . . ? C16 C15 C10 119.61(19) . . ? C17 C16 C15 118.67(18) . . ? C17 C16 C18 118.32(19) . . ? C15 C16 C18 122.84(18) . . ? O7 C17 C16 118.81(18) . . ? O7 C17 C8 119.05(18) . . ? C16 C17 C8 122.13(19) . . ? C19 C18 C16 118.69(18) . . ? C19 C18 H18A 107.6 . . ? C16 C18 H18A 107.6 . . ? C19 C18 H18B 107.6 . . ? C16 C18 H18B 107.6 . . ? H18A C18 H18B 107.1 . . ? C20 C19 C29 118.89(19) . . ? C20 C19 C18 118.58(19) . . ? C29 C19 C18 122.42(18) . . ? O10 C20 C19 118.20(19) . . ? O10 C20 C21 119.84(18) . . ? C19 C20 C21 121.96(19) . . ? C23 C21 C20 118.60(19) . . ? C23 C21 C22 120.4(2) . . ? C20 C21 C22 121.0(2) . . ? O12 C22 O11 124.2(2) . . ? O12 C22 C21 118.1(2) . . ? O11 C22 C21 117.7(2) . . ? C21 C23 C24 121.8(2) . . ? C21 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C25 121.4(2) . . ? C23 C24 C29 118.68(19) . . ? C25 C24 C29 119.8(2) . . ? C26 C25 C24 120.6(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 119.8(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 121.1(2) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 121.2(2) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C19 C29 C28 122.77(19) . . ? C19 C29 C24 119.83(18) . . ? C28 C29 C24 117.38(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn1 O1 C1 -89.4(4) . . . . ? O5 Mn1 O1 C1 -177.6(4) . . . . ? O3 Mn1 O1 C1 1.6(4) . . . . ? O6 Mn1 O1 C1 95.7(4) . . . . ? O5 Mn1 O2 C4 176.2(4) . . . . ? O1 Mn1 O2 C4 87.6(4) . . . . ? O3 Mn1 O2 C4 -4.0(4) . . . . ? O4 Mn1 O2 C4 -88.8(4) . . . . ? Mn1 O1 C1 N1 -148.5(3) . . . . ? C2 N1 C1 O1 0.2(6) . . . . ? C3 N1 C1 O1 178.2(3) . . . . ? Mn1 O2 C4 N2 133.1(3) . . . . ? C6 N2 C4 O2 -2.7(5) . . . . ? C5 N2 C4 O2 178.3(3) . . . . ? O9 C7 C8 C9 -5.1(3) . . . . ? O8 C7 C8 C9 175.1(2) . . . . ? O9 C7 C8 C17 174.5(2) . . . . ? O8 C7 C8 C17 -5.3(3) . . . . ? C17 C8 C9 C10 -0.6(3) . . . . ? C7 C8 C9 C10 179.0(2) . . . . ? C8 C9 C10 C11 179.8(2) . . . . ? C8 C9 C10 C15 -1.4(3) . . . . ? C9 C10 C11 C12 179.5(2) . . . . ? C15 C10 C11 C12 0.7(3) . . . . ? C10 C11 C12 C13 -1.6(4) . . . . ? C11 C12 C13 C14 0.6(4) . . . . ? C12 C13 C14 C15 1.3(4) . . . . ? C13 C14 C15 C16 178.2(2) . . . . ? C13 C14 C15 C10 -2.1(3) . . . . ? C9 C10 C15 C14 -177.7(2) . . . . ? C11 C10 C15 C14 1.1(3) . . . . ? C9 C10 C15 C16 2.0(3) . . . . ? C11 C10 C15 C16 -179.21(19) . . . . ? C14 C15 C16 C17 179.1(2) . . . . ? C10 C15 C16 C17 -0.6(3) . . . . ? C14 C15 C16 C18 3.8(3) . . . . ? C10 C15 C16 C18 -175.81(19) . . . . ? C15 C16 C17 O7 179.76(17) . . . . ? C18 C16 C17 O7 -4.8(3) . . . . ? C15 C16 C17 C8 -1.4(3) . . . . ? C18 C16 C17 C8 173.99(19) . . . . ? C9 C8 C17 O7 -179.13(18) . . . . ? C7 C8 C17 O7 1.3(3) . . . . ? C9 C8 C17 C16 2.1(3) . . . . ? C7 C8 C17 C16 -177.54(19) . . . . ? C17 C16 C18 C19 130.4(2) . . . . ? C15 C16 C18 C19 -54.4(3) . . . . ? C16 C18 C19 C20 122.3(2) . . . . ? C16 C18 C19 C29 -61.5(3) . . . . ? C29 C19 C20 O10 -179.72(19) . . . . ? C18 C19 C20 O10 -3.4(3) . . . . ? C29 C19 C20 C21 0.3(3) . . . . ? C18 C19 C20 C21 176.66(19) . . . . ? O10 C20 C21 C23 -176.8(2) . . . . ? C19 C20 C21 C23 3.2(3) . . . . ? O10 C20 C21 C22 3.0(3) . . . . ? C19 C20 C21 C22 -177.0(2) . . . . ? C23 C21 C22 O12 -6.5(3) . . . . ? C20 C21 C22 O12 173.8(2) . . . . ? C23 C21 C22 O11 173.6(2) . . . . ? C20 C21 C22 O11 -6.1(3) . . . . ? C20 C21 C23 C24 -3.0(3) . . . . ? C22 C21 C23 C24 177.2(2) . . . . ? C21 C23 C24 C25 -177.7(2) . . . . ? C21 C23 C24 C29 -0.6(3) . . . . ? C23 C24 C25 C26 175.0(2) . . . . ? C29 C24 C25 C26 -2.1(3) . . . . ? C24 C25 C26 C27 -0.6(3) . . . . ? C25 C26 C27 C28 2.2(3) . . . . ? C26 C27 C28 C29 -1.0(3) . . . . ? C20 C19 C29 C28 174.06(19) . . . . ? C18 C19 C29 C28 -2.2(3) . . . . ? C20 C19 C29 C24 -4.0(3) . . . . ? C18 C19 C29 C24 179.79(18) . . . . ? C27 C28 C29 C19 -179.8(2) . . . . ? C27 C28 C29 C24 -1.7(3) . . . . ? C23 C24 C29 C19 4.2(3) . . . . ? C25 C24 C29 C19 -178.64(19) . . . . ? C23 C24 C29 C28 -173.98(19) . . . . ? C25 C24 C29 C28 3.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.719 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.049 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 631542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H37 Cu N3 O10' _chemical_formula_weight 687.19 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1125(7) _cell_length_b 11.6950(8) _cell_length_c 27.4427(18) _cell_angle_alpha 90.00 _cell_angle_beta 94.8820(10) _cell_angle_gamma 90.00 _cell_volume 3233.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4520 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 24.84 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.741969 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 17170 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5708 _reflns_number_gt 4637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0418P)^2^+1.2390P] 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 5708 _refine_ls_number_parameters 423 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _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 Cu1 Cu 0.20735(2) 0.52464(2) 0.475747(8) 0.02953(9) Uani 1 1 d . . . O1 O 0.14013(16) 0.72354(15) 0.65174(5) 0.0444(4) Uani 1 1 d . . . H1 H 0.1086 0.7095 0.6239 0.067 Uiso 1 1 calc R . . O2 O 0.12808(16) 0.64063(14) 0.56534(5) 0.0432(4) Uani 1 1 d . . . O3 O 0.28438(15) 0.52214(13) 0.54356(5) 0.0363(4) Uani 1 1 d . . . O4 O 0.62019(15) 0.97153(13) 0.90923(5) 0.0385(4) Uani 1 1 d . . . O5 O 0.46586(17) 0.84167(14) 0.92109(5) 0.0450(4) Uani 1 1 d . . . O6 O 0.33332(18) 0.75195(15) 0.84760(5) 0.0473(4) Uani 1 1 d . . . H6 H 0.3624 0.7612 0.8761 0.071 Uiso 1 1 calc R . . O7 O 0.36409(15) 0.40204(14) 0.44872(5) 0.0417(4) Uani 1 1 d . . . O8 O 0.30124(16) 0.66588(14) 0.46289(6) 0.0434(4) Uani 1 1 d . . . O9 O 0.09542(14) 0.39566(13) 0.48990(5) 0.0355(3) Uani 1 1 d D . . H9A H 0.0813 0.3863 0.5197 0.053 Uiso 1 1 d RD . . H9B H 0.0259 0.3890 0.4704 0.053 Uiso 1 1 d RD . . N1 N 0.3904(2) 0.26658(17) 0.39122(7) 0.0435(5) Uani 1 1 d . . . N2 N 0.4861(2) 0.76344(16) 0.45043(7) 0.0419(5) Uani 1 1 d . . . C1 C 0.2307(2) 0.58148(18) 0.57502(7) 0.0318(5) Uani 1 1 d . . . C2 C 0.2939(2) 0.58240(18) 0.62631(7) 0.0306(5) Uani 1 1 d . . . C3 C 0.4005(2) 0.51354(19) 0.63833(8) 0.0362(5) Uani 1 1 d . . . H3 H 0.4312 0.4663 0.6144 0.043 Uiso 1 1 calc R . . C4 C 0.4654(2) 0.5116(2) 0.68555(8) 0.0381(5) Uani 1 1 d . . . C5 C 0.5764(3) 0.4407(2) 0.69726(9) 0.0526(7) Uani 1 1 d . . . H5 H 0.6073 0.3941 0.6732 0.063 Uiso 1 1 calc R . . C6 C 0.6390(3) 0.4394(3) 0.74313(10) 0.0643(8) Uani 1 1 d . . . H6A H 0.7130 0.3933 0.7503 0.077 Uiso 1 1 calc R . . C7 C 0.5906(3) 0.5082(3) 0.77932(10) 0.0636(8) Uani 1 1 d . . . H7 H 0.6325 0.5064 0.8108 0.076 Uiso 1 1 calc R . . C8 C 0.4839(3) 0.5777(2) 0.76958(8) 0.0493(6) Uani 1 1 d . . . H8 H 0.4538 0.6216 0.7946 0.059 Uiso 1 1 calc R . . C9 C 0.4173(2) 0.58456(19) 0.72200(7) 0.0353(5) Uani 1 1 d . . . C10 C 0.3084(2) 0.65918(18) 0.70990(7) 0.0316(5) Uani 1 1 d . . . C11 C 0.2467(2) 0.65497(18) 0.66302(7) 0.0317(5) Uani 1 1 d . . . C12 C 0.2550(2) 0.73863(19) 0.74784(7) 0.0355(5) Uani 1 1 d . . . H12A H 0.1764 0.7765 0.7328 0.043 Uiso 1 1 calc R . . H12B H 0.2274 0.6922 0.7745 0.043 Uiso 1 1 calc R . . C13 C 0.3504(2) 0.82986(19) 0.76938(7) 0.0311(5) Uani 1 1 d . . . C14 C 0.3986(2) 0.91842(18) 0.74015(7) 0.0294(5) Uani 1 1 d . . . C15 C 0.3532(2) 0.9340(2) 0.69017(7) 0.0369(5) Uani 1 1 d . . . H15 H 0.2901 0.8841 0.6755 0.044 Uiso 1 1 calc R . . C16 C 0.4002(3) 1.0203(2) 0.66330(8) 0.0440(6) Uani 1 1 d . . . H16 H 0.3681 1.0288 0.6307 0.053 Uiso 1 1 calc R . . C17 C 0.4959(3) 1.0966(2) 0.68375(8) 0.0479(6) Uani 1 1 d . . . H17 H 0.5281 1.1545 0.6648 0.057 Uiso 1 1 calc R . . C18 C 0.5415(2) 1.0853(2) 0.73170(8) 0.0449(6) Uani 1 1 d . . . H18 H 0.6055 1.1359 0.7452 0.054 Uiso 1 1 calc R . . C19 C 0.4935(2) 0.99839(19) 0.76108(7) 0.0335(5) Uani 1 1 d . . . C20 C 0.5348(2) 0.98979(19) 0.81113(8) 0.0348(5) Uani 1 1 d . . . H20 H 0.5991 1.0399 0.8247 0.042 Uiso 1 1 calc R . . C21 C 0.4831(2) 0.90985(18) 0.84037(7) 0.0301(5) Uani 1 1 d . . . C22 C 0.5258(2) 0.90722(19) 0.89399(7) 0.0330(5) Uani 1 1 d . . . C23 C 0.3874(2) 0.83080(19) 0.81900(7) 0.0323(5) Uani 1 1 d . . . C24 C 0.4957(3) 0.2069(2) 0.41973(10) 0.0637(8) Uani 1 1 d . . . H24A H 0.5317 0.2553 0.4458 0.096 Uiso 1 1 calc R . . H24B H 0.5643 0.1872 0.3991 0.096 Uiso 1 1 calc R . . H24C H 0.4609 0.1385 0.4332 0.096 Uiso 1 1 calc R . . C25 C 0.3523(3) 0.2253(3) 0.34201(11) 0.0751(10) Uani 1 1 d . . . H25A H 0.2791 0.2698 0.3277 0.113 Uiso 1 1 calc R . . H25B H 0.3265 0.1465 0.3434 0.113 Uiso 1 1 calc R . . H25C H 0.4261 0.2325 0.3224 0.113 Uiso 1 1 calc R . . C26 C 0.3370(2) 0.3590(2) 0.40839(9) 0.0450(6) Uani 1 1 d . . . H26 H 0.2721 0.3954 0.3879 0.054 Uiso 1 1 calc R . . C27 C 0.6290(3) 0.7639(2) 0.44729(11) 0.0605(7) Uani 1 1 d . . . H27A H 0.6652 0.6913 0.4580 0.091 Uiso 1 1 calc R . . H27B H 0.6685 0.8234 0.4678 0.091 Uiso 1 1 calc R . . H27C H 0.6476 0.7772 0.4140 0.091 Uiso 1 1 calc R . . C28 C 0.4149(3) 0.8706(2) 0.44461(12) 0.0687(9) Uani 1 1 d . . . H28A H 0.3543 0.8673 0.4158 0.103 Uiso 1 1 calc R . . H28B H 0.4768 0.9319 0.4416 0.103 Uiso 1 1 calc R . . H28C H 0.3663 0.8837 0.4727 0.103 Uiso 1 1 calc R . . C29 C 0.4232(2) 0.6690(2) 0.46017(7) 0.0379(5) Uani 1 1 d . . . H29 H 0.4718 0.6019 0.4652 0.045 Uiso 1 1 calc R . . O10 O 0.7566(3) 0.0394(2) 0.46174(10) 0.0974(8) Uani 1 1 d . . . N3 N 0.9662(3) 0.0614(2) 0.43931(9) 0.0627(6) Uani 1 1 d . . . C30 C 0.9554(4) -0.0356(4) 0.40805(17) 0.1273(19) Uani 1 1 d . . . H30A H 0.8769 -0.0779 0.4138 0.191 Uiso 1 1 calc R . . H30B H 1.0320 -0.0835 0.4146 0.191 Uiso 1 1 calc R . . H30C H 0.9501 -0.0110 0.3746 0.191 Uiso 1 1 calc R . . C31 C 1.0865(4) 0.1265(3) 0.44023(17) 0.1016(13) Uani 1 1 d . . . H31A H 1.0861 0.1716 0.4110 0.152 Uiso 1 1 calc R . . H31B H 1.1612 0.0756 0.4421 0.152 Uiso 1 1 calc R . . H31C H 1.0928 0.1761 0.4682 0.152 Uiso 1 1 calc R . . C32 C 0.8629(4) 0.0899(3) 0.46361(12) 0.0730(9) Uani 1 1 d . . . H32 H 0.8722 0.1538 0.4838 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03499(16) 0.03363(16) 0.01900(13) -0.00057(10) -0.00340(10) 0.00061(11) O1 0.0445(9) 0.0548(10) 0.0310(8) -0.0110(7) -0.0130(7) 0.0076(8) O2 0.0450(9) 0.0519(10) 0.0299(8) -0.0073(7) -0.0135(7) 0.0038(8) O3 0.0463(9) 0.0398(9) 0.0214(7) -0.0048(7) -0.0058(6) -0.0013(7) O4 0.0467(9) 0.0447(9) 0.0224(7) -0.0028(7) -0.0072(7) -0.0080(8) O5 0.0613(11) 0.0536(10) 0.0199(7) -0.0022(7) 0.0028(7) -0.0142(9) O6 0.0643(11) 0.0566(11) 0.0205(7) -0.0011(7) 0.0012(7) -0.0254(9) O7 0.0453(9) 0.0445(10) 0.0349(8) -0.0094(7) 0.0015(7) 0.0058(8) O8 0.0464(10) 0.0400(9) 0.0436(9) 0.0049(7) 0.0023(7) -0.0022(8) O9 0.0382(8) 0.0458(9) 0.0211(7) 0.0011(6) -0.0059(6) -0.0067(7) N1 0.0476(12) 0.0430(12) 0.0398(11) -0.0123(9) 0.0024(9) 0.0015(9) N2 0.0537(12) 0.0339(11) 0.0390(11) 0.0033(8) 0.0086(9) -0.0029(9) C1 0.0378(12) 0.0309(12) 0.0254(10) 0.0012(9) -0.0055(9) -0.0105(10) C2 0.0351(11) 0.0334(12) 0.0222(10) -0.0009(8) -0.0039(8) -0.0087(9) C3 0.0433(13) 0.0371(13) 0.0273(11) -0.0047(9) -0.0028(9) -0.0028(10) C4 0.0419(13) 0.0413(13) 0.0295(11) 0.0010(10) -0.0055(10) -0.0012(10) C5 0.0557(16) 0.0579(16) 0.0419(14) -0.0033(12) -0.0087(12) 0.0148(13) C6 0.0649(18) 0.074(2) 0.0495(16) 0.0045(14) -0.0197(14) 0.0211(16) C7 0.073(2) 0.080(2) 0.0339(13) 0.0021(13) -0.0208(13) 0.0171(16) C8 0.0609(16) 0.0554(16) 0.0291(12) -0.0019(11) -0.0106(11) 0.0046(13) C9 0.0418(13) 0.0376(13) 0.0251(10) 0.0021(9) -0.0050(9) -0.0070(10) C10 0.0360(12) 0.0358(12) 0.0225(10) -0.0022(9) -0.0010(9) -0.0088(10) C11 0.0316(11) 0.0363(12) 0.0261(10) -0.0004(9) -0.0048(9) -0.0061(9) C12 0.0367(12) 0.0466(14) 0.0228(10) -0.0031(9) 0.0002(9) -0.0071(10) C13 0.0335(11) 0.0368(12) 0.0228(10) -0.0069(9) 0.0013(8) -0.0007(9) C14 0.0342(11) 0.0329(12) 0.0211(10) -0.0043(8) 0.0019(8) 0.0048(9) C15 0.0464(13) 0.0375(12) 0.0260(10) -0.0050(9) -0.0025(9) 0.0045(10) C16 0.0638(16) 0.0445(14) 0.0229(11) 0.0022(10) -0.0007(11) 0.0079(12) C17 0.0670(17) 0.0454(15) 0.0317(12) 0.0086(11) 0.0063(11) -0.0042(13) C18 0.0529(15) 0.0448(15) 0.0365(12) 0.0012(11) 0.0007(11) -0.0111(12) C19 0.0361(12) 0.0378(13) 0.0263(10) -0.0023(9) 0.0002(9) 0.0003(9) C20 0.0360(12) 0.0393(13) 0.0284(11) -0.0047(9) -0.0016(9) -0.0049(10) C21 0.0336(11) 0.0355(12) 0.0209(10) -0.0050(9) -0.0004(8) 0.0016(9) C22 0.0392(12) 0.0359(13) 0.0234(10) -0.0054(9) -0.0003(9) 0.0043(10) C23 0.0366(12) 0.0383(13) 0.0220(10) -0.0017(9) 0.0035(9) -0.0040(10) C24 0.089(2) 0.0506(17) 0.0508(16) -0.0068(13) 0.0011(15) 0.0213(15) C25 0.079(2) 0.086(2) 0.0581(18) -0.0357(17) -0.0082(16) 0.0151(18) C26 0.0430(14) 0.0520(15) 0.0391(13) -0.0032(11) -0.0020(11) 0.0104(12) C27 0.0524(16) 0.0545(17) 0.0747(19) 0.0092(15) 0.0063(14) -0.0107(14) C28 0.084(2) 0.0410(16) 0.086(2) 0.0148(15) 0.0358(18) 0.0110(15) C29 0.0502(15) 0.0342(13) 0.0282(11) -0.0005(9) -0.0020(10) -0.0013(11) O10 0.0937(19) 0.0895(19) 0.113(2) -0.0038(15) 0.0333(16) -0.0072(16) N3 0.0653(16) 0.0583(15) 0.0635(15) -0.0066(12) -0.0006(13) -0.0040(13) C30 0.106(3) 0.150(4) 0.131(4) -0.091(3) 0.036(3) -0.031(3) C31 0.076(2) 0.069(2) 0.157(4) 0.005(2) -0.006(2) -0.007(2) C32 0.099(3) 0.0515(19) 0.068(2) -0.0003(15) 0.0019(19) 0.0061(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O9 1.9448(14) . ? Cu1 O8 1.9522(16) . ? Cu1 O3 1.9555(14) . ? Cu1 O4 1.9589(14) 4_575 ? Cu1 O7 2.3061(15) . ? O1 C11 1.358(3) . ? O1 H1 0.8200 . ? O2 C1 1.256(3) . ? O3 C1 1.266(3) . ? O4 C22 1.258(3) . ? O4 Cu1 1.9590(14) 4_676 ? O5 C22 1.259(3) . ? O6 C23 1.356(2) . ? O6 H6 0.8200 . ? O7 C26 1.225(3) . ? O8 C29 1.242(3) . ? O9 H9A 0.8500 . ? O9 H9B 0.8501 . ? N1 C26 1.313(3) . ? N1 C24 1.446(3) . ? N1 C25 1.455(3) . ? N2 C29 1.314(3) . ? N2 C28 1.448(3) . ? N2 C27 1.455(3) . ? C1 C2 1.496(3) . ? C2 C3 1.363(3) . ? C2 C11 1.430(3) . ? C3 C4 1.402(3) . ? C3 H3 0.9300 . ? C4 C5 1.410(3) . ? C4 C9 1.431(3) . ? C5 C6 1.360(3) . ? C5 H5 0.9300 . ? C6 C7 1.399(4) . ? C6 H6A 0.9300 . ? C7 C8 1.359(4) . ? C7 H7 0.9300 . ? C8 C9 1.419(3) . ? C8 H8 0.9300 . ? C9 C10 1.422(3) . ? C10 C11 1.383(3) . ? C10 C12 1.528(3) . ? C12 C13 1.524(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C23 1.381(3) . ? C13 C14 1.421(3) . ? C14 C15 1.421(3) . ? C14 C19 1.426(3) . ? C15 C16 1.360(3) . ? C15 H15 0.9300 . ? C16 C17 1.399(4) . ? C16 H16 0.9300 . ? C17 C18 1.363(3) . ? C17 H17 0.9300 . ? C18 C19 1.409(3) . ? C18 H18 0.9300 . ? C19 C20 1.405(3) . ? C20 C21 1.365(3) . ? C20 H20 0.9300 . ? C21 C23 1.428(3) . ? C21 C22 1.498(3) . ? 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 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29 0.9300 . ? O10 C32 1.224(4) . ? N3 C32 1.328(4) . ? N3 C30 1.421(4) . ? N3 C31 1.434(4) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32 0.9300 . ? 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 O9 Cu1 O8 173.02(7) . . ? O9 Cu1 O3 89.42(6) . . ? O8 Cu1 O3 91.38(6) . . ? O9 Cu1 O4 88.88(6) . 4_575 ? O8 Cu1 O4 89.97(7) . 4_575 ? O3 Cu1 O4 176.71(6) . 4_575 ? O9 Cu1 O7 90.55(6) . . ? O8 Cu1 O7 96.30(6) . . ? O3 Cu1 O7 93.89(6) . . ? O4 Cu1 O7 88.94(6) 4_575 . ? C11 O1 H1 109.5 . . ? C1 O3 Cu1 118.79(14) . . ? C22 O4 Cu1 126.28(14) . 4_676 ? C23 O6 H6 109.5 . . ? C26 O7 Cu1 116.03(15) . . ? C29 O8 Cu1 122.43(15) . . ? Cu1 O9 H9A 116.2 . . ? Cu1 O9 H9B 114.2 . . ? H9A O9 H9B 113.4 . . ? C26 N1 C24 120.6(2) . . ? C26 N1 C25 121.4(2) . . ? C24 N1 C25 117.8(2) . . ? C29 N2 C28 120.3(2) . . ? C29 N2 C27 121.1(2) . . ? C28 N2 C27 118.6(2) . . ? O2 C1 O3 123.52(19) . . ? O2 C1 C2 118.32(19) . . ? O3 C1 C2 118.15(19) . . ? C3 C2 C11 119.00(18) . . ? C3 C2 C1 119.30(19) . . ? C11 C2 C1 121.69(19) . . ? C2 C3 C4 122.1(2) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C3 C4 C5 121.4(2) . . ? C3 C4 C9 118.4(2) . . ? C5 C4 C9 120.2(2) . . ? C6 C5 C4 121.1(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 119.2(3) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C8 C7 C6 121.6(2) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 121.4(2) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C10 123.2(2) . . ? C8 C9 C4 116.5(2) . . ? C10 C9 C4 120.35(19) . . ? C11 C10 C9 118.36(19) . . ? C11 C10 C12 119.84(19) . . ? C9 C10 C12 121.73(18) . . ? O1 C11 C10 118.56(19) . . ? O1 C11 C2 119.75(17) . . ? C10 C11 C2 121.7(2) . . ? C13 C12 C10 116.14(17) . . ? C13 C12 H12A 108.3 . . ? C10 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? C10 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C23 C13 C14 118.28(19) . . ? C23 C13 C12 119.82(19) . . ? C14 C13 C12 121.83(17) . . ? C15 C14 C13 122.68(19) . . ? C15 C14 C19 117.16(19) . . ? C13 C14 C19 120.13(18) . . ? C16 C15 C14 121.3(2) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 121.2(2) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 119.4(2) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 121.1(2) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C20 C19 C18 121.5(2) . . ? C20 C19 C14 118.73(19) . . ? C18 C19 C14 119.71(19) . . ? C21 C20 C19 121.8(2) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C23 118.84(18) . . ? C20 C21 C22 119.91(19) . . ? C23 C21 C22 121.25(18) . . ? O4 C22 O5 123.87(18) . . ? O4 C22 C21 117.47(19) . . ? O5 C22 C21 118.65(19) . . ? O6 C23 C13 118.48(19) . . ? O6 C23 C21 119.69(17) . . ? C13 C23 C21 121.80(19) . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O7 C26 N1 126.5(2) . . ? O7 C26 H26 116.8 . . ? N1 C26 H26 116.8 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O8 C29 N2 122.5(2) . . ? O8 C29 H29 118.7 . . ? N2 C29 H29 118.7 . . ? C32 N3 C30 118.7(3) . . ? C32 N3 C31 124.0(3) . . ? C30 N3 C31 117.1(3) . . ? N3 C30 H30A 109.5 . . ? N3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O10 C32 N3 125.6(3) . . ? O10 C32 H32 117.2 . . ? N3 C32 H32 117.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Cu1 O3 C1 -90.20(15) . . . . ? O8 Cu1 O3 C1 82.87(15) . . . . ? O7 Cu1 O3 C1 179.29(15) . . . . ? O9 Cu1 O7 C26 75.04(18) . . . . ? O8 Cu1 O7 C26 -103.68(18) . . . . ? O3 Cu1 O7 C26 164.50(17) . . . . ? O4 Cu1 O7 C26 -13.83(18) 4_575 . . . ? O3 Cu1 O8 C29 71.17(17) . . . . ? O4 Cu1 O8 C29 -111.83(17) 4_575 . . . ? O7 Cu1 O8 C29 -22.90(17) . . . . ? Cu1 O3 C1 O2 1.6(3) . . . . ? Cu1 O3 C1 C2 -177.57(13) . . . . ? O2 C1 C2 C3 176.1(2) . . . . ? O3 C1 C2 C3 -4.8(3) . . . . ? O2 C1 C2 C11 -4.9(3) . . . . ? O3 C1 C2 C11 174.31(19) . . . . ? C11 C2 C3 C4 0.0(3) . . . . ? C1 C2 C3 C4 179.1(2) . . . . ? C2 C3 C4 C5 -179.4(2) . . . . ? C2 C3 C4 C9 0.0(3) . . . . ? C3 C4 C5 C6 179.9(3) . . . . ? C9 C4 C5 C6 0.5(4) . . . . ? C4 C5 C6 C7 1.1(5) . . . . ? C5 C6 C7 C8 -1.0(5) . . . . ? C6 C7 C8 C9 -0.7(5) . . . . ? C7 C8 C9 C10 -177.6(3) . . . . ? C7 C8 C9 C4 2.3(4) . . . . ? C3 C4 C9 C8 178.4(2) . . . . ? C5 C4 C9 C8 -2.1(3) . . . . ? C3 C4 C9 C10 -1.7(3) . . . . ? C5 C4 C9 C10 177.7(2) . . . . ? C8 C9 C10 C11 -176.8(2) . . . . ? C4 C9 C10 C11 3.3(3) . . . . ? C8 C9 C10 C12 0.2(3) . . . . ? C4 C9 C10 C12 -179.7(2) . . . . ? C9 C10 C11 O1 178.00(19) . . . . ? C12 C10 C11 O1 0.9(3) . . . . ? C9 C10 C11 C2 -3.3(3) . . . . ? C12 C10 C11 C2 179.60(19) . . . . ? C3 C2 C11 O1 -179.59(19) . . . . ? C1 C2 C11 O1 1.3(3) . . . . ? C3 C2 C11 C10 1.7(3) . . . . ? C1 C2 C11 C10 -177.35(19) . . . . ? C11 C10 C12 C13 -119.9(2) . . . . ? C9 C10 C12 C13 63.1(3) . . . . ? C10 C12 C13 C23 -118.8(2) . . . . ? C10 C12 C13 C14 64.2(3) . . . . ? C23 C13 C14 C15 -171.6(2) . . . . ? C12 C13 C14 C15 5.4(3) . . . . ? C23 C13 C14 C19 6.5(3) . . . . ? C12 C13 C14 C19 -176.48(19) . . . . ? C13 C14 C15 C16 179.3(2) . . . . ? C19 C14 C15 C16 1.1(3) . . . . ? C14 C15 C16 C17 0.5(4) . . . . ? C15 C16 C17 C18 -1.0(4) . . . . ? C16 C17 C18 C19 -0.3(4) . . . . ? C17 C18 C19 C20 -176.6(2) . . . . ? C17 C18 C19 C14 2.0(4) . . . . ? C15 C14 C19 C20 176.3(2) . . . . ? C13 C14 C19 C20 -1.9(3) . . . . ? C15 C14 C19 C18 -2.3(3) . . . . ? C13 C14 C19 C18 179.5(2) . . . . ? C18 C19 C20 C21 176.2(2) . . . . ? C14 C19 C20 C21 -2.4(3) . . . . ? C19 C20 C21 C23 1.9(3) . . . . ? C19 C20 C21 C22 -177.32(19) . . . . ? Cu1 O4 C22 O5 6.3(3) 4_676 . . . ? Cu1 O4 C22 C21 -173.82(13) 4_676 . . . ? C20 C21 C22 O4 -7.9(3) . . . . ? C23 C21 C22 O4 172.85(19) . . . . ? C20 C21 C22 O5 171.9(2) . . . . ? C23 C21 C22 O5 -7.3(3) . . . . ? C14 C13 C23 O6 174.81(19) . . . . ? C12 C13 C23 O6 -2.3(3) . . . . ? C14 C13 C23 C21 -7.1(3) . . . . ? C12 C13 C23 C21 175.84(19) . . . . ? C20 C21 C23 O6 -179.0(2) . . . . ? C22 C21 C23 O6 0.3(3) . . . . ? C20 C21 C23 C13 3.0(3) . . . . ? C22 C21 C23 C13 -177.8(2) . . . . ? Cu1 O7 C26 N1 -160.5(2) . . . . ? C24 N1 C26 O7 -2.4(4) . . . . ? C25 N1 C26 O7 -178.3(3) . . . . ? Cu1 O8 C29 N2 178.41(15) . . . . ? C28 N2 C29 O8 2.9(3) . . . . ? C27 N2 C29 O8 -179.7(2) . . . . ? C30 N3 C32 O10 0.2(6) . . . . ? C31 N3 C32 O10 176.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.260 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.045 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 631543' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H65 Cd N5 O15' _chemical_formula_weight 1196.56 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.323(2) _cell_length_b 11.0466(8) _cell_length_c 20.5022(16) _cell_angle_alpha 90.00 _cell_angle_beta 120.9050(10) _cell_angle_gamma 90.00 _cell_volume 5503.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6399 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.23 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 0.471 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.887713 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 17914 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.87 _reflns_number_total 6475 _reflns_number_gt 5059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II ' _computing_cell_refinement 'Bruker APEX II ' _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^)+(0.0931P)^2^+1.1808P] 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 6475 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _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 Cd1 Cd 1.0000 0.753077(19) 0.2500 0.03715(11) Uani 1 2 d S . . C1 C 1.04688(12) 0.5903(2) 0.19600(14) 0.0440(6) Uani 1 1 d . . . C2 C 1.06438(11) 0.4886(2) 0.16481(13) 0.0398(5) Uani 1 1 d . . . C3 C 1.02467(11) 0.4239(2) 0.09846(13) 0.0379(5) Uani 1 1 d . . . C4 C 1.03981(10) 0.3257(2) 0.07081(13) 0.0398(5) Uani 1 1 d . . . C5 C 1.09585(12) 0.2909(3) 0.10818(15) 0.0427(6) Uani 1 1 d . . . C6 C 1.11586(13) 0.1923(3) 0.08415(19) 0.0563(7) Uani 1 1 d . . . H6 H 1.0913 0.1483 0.0412 0.068 Uiso 1 1 calc R . . C7 C 1.16991(14) 0.1615(3) 0.1226(2) 0.0682(9) Uani 1 1 d . . . H7 H 1.1816 0.0974 0.1049 0.082 Uiso 1 1 calc R . . C8 C 1.20848(16) 0.2232(4) 0.1880(3) 0.0680(9) Uani 1 1 d . . . H8 H 1.2452 0.1992 0.2141 0.082 Uiso 1 1 calc R . . C9 C 1.19164(12) 0.3193(3) 0.21316(19) 0.0569(7) Uani 1 1 d . . . H9 H 1.2172 0.3611 0.2564 0.068 Uiso 1 1 calc R . . C10 C 1.13562(11) 0.3560(2) 0.17398(15) 0.0450(6) Uani 1 1 d . . . C11 C 1.11821(11) 0.4541(2) 0.20003(14) 0.0438(6) Uani 1 1 d . . . H11 H 1.1442 0.4968 0.2426 0.053 Uiso 1 1 calc R . . C12 C 0.99455(14) 0.2634(2) -0.00012(16) 0.0425(6) Uani 1 1 d . . . H12A H 1.0113 0.2069 -0.0186 0.051 Uiso 1 1 calc R . . H12B H 0.9750 0.3238 -0.0393 0.051 Uiso 1 1 calc R . . C13 C 0.95345(10) 0.1954(2) 0.01313(13) 0.0381(5) Uani 1 1 d . . . C14 C 0.97224(10) 0.0953(2) 0.05948(13) 0.0374(5) Uani 1 1 d . . . C15 C 0.93827(10) 0.0291(2) 0.07951(12) 0.0366(5) Uani 1 1 d . . . C16 C 0.96150(11) -0.0713(2) 0.13679(14) 0.0410(5) Uani 1 1 d . . . C17 C 0.88409(11) 0.0612(2) 0.04720(14) 0.0427(5) Uani 1 1 d . . . H17 H 0.8614 0.0172 0.0589 0.051 Uiso 1 1 calc R . . C18 C 0.86193(11) 0.1600(2) -0.00358(14) 0.0442(6) Uani 1 1 d . . . C19 C 0.80590(13) 0.1916(3) -0.03598(19) 0.0615(8) Uani 1 1 d . . . H19 H 0.7836 0.1468 -0.0239 0.074 Uiso 1 1 calc R . . C20 C 0.78410(15) 0.2878(4) -0.0852(2) 0.0737(10) Uani 1 1 d . . . H20 H 0.7472 0.3081 -0.1068 0.088 Uiso 1 1 calc R . . C21 C 0.81796(14) 0.3545(3) -0.10228(18) 0.0683(9) Uani 1 1 d . . . H21 H 0.8031 0.4193 -0.1358 0.082 Uiso 1 1 calc R . . C22 C 0.87260(13) 0.3277(3) -0.07113(15) 0.0535(7) Uani 1 1 d . . . H22 H 0.8941 0.3751 -0.0834 0.064 Uiso 1 1 calc R . . C23 C 0.89719(12) 0.2284(2) -0.02028(14) 0.0404(6) Uani 1 1 d . . . C24 C 0.7137(2) 0.9171(5) 0.9254(2) 0.1070(16) Uani 1 1 d . . . H24A H 0.7408 0.9803 0.9467 0.160 Uiso 1 1 calc R . . H24B H 0.6901 0.9305 0.8718 0.160 Uiso 1 1 calc R . . H24C H 0.7319 0.8403 0.9337 0.160 Uiso 1 1 calc R . . C25 C 0.6446(2) 0.8666(5) 0.9615(3) 0.1076(15) Uani 1 1 d . . . H25A H 0.6395 0.9059 0.9992 0.161 Uiso 1 1 calc R . . H25B H 0.6532 0.7828 0.9745 0.161 Uiso 1 1 calc R . . H25C H 0.6114 0.8729 0.9128 0.161 Uiso 1 1 calc R . . N1 N 0.6839(3) 0.9173(7) 0.9587(4) 0.276(6) Uani 1 1 d . . . H1A H 0.7107 0.9137 1.0079 0.331 Uiso 1 1 calc R . . H1B H 0.6727 0.9950 0.9516 0.331 Uiso 1 1 calc R . . O1 O 1.08125(9) 0.65183(18) 0.25016(11) 0.0584(5) Uani 1 1 d . . . O2 O 0.99540(9) 0.60859(18) 0.16651(12) 0.0516(5) Uani 1 1 d . . . O3 O 0.97130(8) 0.45637(18) 0.06104(10) 0.0494(4) Uani 1 1 d . . . H3A H 0.9666 0.5103 0.0846 0.074 Uiso 1 1 calc R . . O4 O 1.02523(8) 0.06045(18) 0.08764(11) 0.0483(4) Uani 1 1 d . . . H4A H 1.0325 0.0037 0.1171 0.072 Uiso 1 1 calc R . . O5 O 1.01136(8) -0.10044(18) 0.16427(11) 0.0525(5) Uani 1 1 d . . . O6 O 0.93198(8) -0.12135(17) 0.15799(11) 0.0522(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04232(16) 0.02461(15) 0.04356(17) 0.000 0.02135(12) 0.000 C1 0.0656(17) 0.0297(12) 0.0435(13) 0.0009(10) 0.0329(13) -0.0019(12) C2 0.0551(14) 0.0304(12) 0.0429(12) -0.0008(10) 0.0315(11) -0.0046(11) C3 0.0463(13) 0.0337(12) 0.0382(11) 0.0023(9) 0.0250(11) -0.0031(10) C4 0.0548(14) 0.0361(13) 0.0396(12) -0.0026(10) 0.0322(11) -0.0064(11) C5 0.0559(15) 0.0396(13) 0.0500(14) -0.0038(11) 0.0396(13) -0.0067(12) C6 0.0657(18) 0.0536(19) 0.0719(19) -0.0141(15) 0.0513(16) -0.0088(15) C7 0.072(2) 0.063(2) 0.098(2) -0.0107(19) 0.064(2) -0.0013(17) C8 0.0546(18) 0.069(2) 0.095(3) 0.001(2) 0.049(2) 0.0045(16) C9 0.0497(15) 0.0569(19) 0.0684(18) -0.0011(15) 0.0335(14) -0.0034(14) C10 0.0491(14) 0.0448(14) 0.0492(13) 0.0003(11) 0.0312(12) -0.0059(11) C11 0.0542(14) 0.0389(13) 0.0422(12) -0.0045(10) 0.0276(12) -0.0093(11) C12 0.0587(16) 0.0403(14) 0.0357(11) -0.0028(9) 0.0294(12) -0.0072(11) C13 0.0519(14) 0.0326(13) 0.0324(11) -0.0052(9) 0.0235(10) -0.0064(11) C14 0.0423(12) 0.0352(12) 0.0346(11) -0.0057(9) 0.0195(10) -0.0027(10) C15 0.0428(12) 0.0297(11) 0.0339(11) -0.0024(9) 0.0171(10) -0.0040(9) C16 0.0531(15) 0.0273(11) 0.0418(12) -0.0016(9) 0.0238(11) -0.0024(10) C17 0.0458(13) 0.0337(12) 0.0454(13) 0.0015(10) 0.0212(11) -0.0047(10) C18 0.0448(13) 0.0378(13) 0.0417(12) -0.0009(10) 0.0163(11) -0.0026(11) C19 0.0493(16) 0.055(2) 0.0647(19) 0.0077(16) 0.0179(14) -0.0013(15) C20 0.0492(18) 0.069(2) 0.074(2) 0.014(2) 0.0110(17) 0.0120(17) C21 0.070(2) 0.059(2) 0.0522(16) 0.0198(15) 0.0140(15) 0.0140(16) C22 0.0646(18) 0.0424(15) 0.0444(14) 0.0118(12) 0.0215(13) -0.0011(13) C23 0.0510(14) 0.0327(12) 0.0305(11) -0.0013(9) 0.0158(11) -0.0019(10) C24 0.096(3) 0.139(5) 0.083(3) -0.013(3) 0.044(3) -0.024(3) C25 0.108(3) 0.095(3) 0.130(4) 0.039(3) 0.068(3) 0.012(3) N1 0.258(7) 0.352(10) 0.376(10) -0.313(9) 0.278(8) -0.253(8) O1 0.0716(13) 0.0436(11) 0.0521(11) -0.0137(9) 0.0260(10) -0.0029(10) O2 0.0600(12) 0.0384(10) 0.0587(11) -0.0083(9) 0.0322(10) 0.0011(9) O3 0.0498(10) 0.0441(11) 0.0490(10) -0.0038(8) 0.0214(8) 0.0024(8) O4 0.0462(10) 0.0432(11) 0.0569(11) 0.0071(9) 0.0275(9) 0.0026(8) O5 0.0500(11) 0.0390(10) 0.0599(12) 0.0129(9) 0.0221(10) 0.0062(9) O6 0.0594(11) 0.0412(10) 0.0628(11) 0.0146(9) 0.0364(10) 0.0026(9) _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 Cd1 O2 2.2946(19) . ? Cd1 O2 2.2946(19) 2_755 ? Cd1 O6 2.3370(19) 2_765 ? Cd1 O6 2.3370(19) 1_565 ? Cd1 O5 2.528(2) 1_565 ? Cd1 O5 2.528(2) 2_765 ? Cd1 O1 2.557(2) 2_755 ? Cd1 O1 2.557(2) . ? C1 O1 1.238(3) . ? C1 O2 1.275(4) . ? C1 C2 1.497(3) . ? C2 C11 1.364(4) . ? C2 C3 1.433(3) . ? C3 O3 1.346(3) . ? C3 C4 1.390(3) . ? C4 C5 1.416(4) . ? C4 C12 1.522(4) . ? C5 C6 1.427(4) . ? C5 C10 1.430(4) . ? C6 C7 1.357(5) . ? C6 H6 0.9300 . ? C7 C8 1.397(5) . ? C7 H7 0.9300 . ? C8 C9 1.369(5) . ? C8 H8 0.9300 . ? C9 C10 1.421(4) . ? C9 H9 0.9300 . ? C10 C11 1.405(4) . ? C11 H11 0.9300 . ? C12 C13 1.523(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.374(3) . ? C13 C23 1.421(4) . ? C14 O4 1.358(3) . ? C14 C15 1.427(3) . ? C15 C17 1.369(4) . ? C15 C16 1.500(3) . ? C16 O6 1.252(3) . ? C16 O5 1.264(3) . ? C17 C18 1.413(3) . ? C17 H17 0.9300 . ? C18 C19 1.414(4) . ? C18 C23 1.427(4) . ? C19 C20 1.375(5) . ? C19 H19 0.9300 . ? C20 C21 1.389(5) . ? C20 H20 0.9300 . ? C21 C22 1.370(5) . ? C21 H21 0.9300 . ? C22 C23 1.424(4) . ? C22 H22 0.9300 . ? C24 N1 1.331(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N1 1.274(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? O3 H3A 0.8200 . ? O4 H4A 0.8200 . ? O5 Cd1 2.528(2) 1_545 ? O6 Cd1 2.3370(19) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O2 91.85(11) . 2_755 ? O2 Cd1 O6 136.26(7) . 2_765 ? O2 Cd1 O6 95.93(7) 2_755 2_765 ? O2 Cd1 O6 95.93(7) . 1_565 ? O2 Cd1 O6 136.26(7) 2_755 1_565 ? O6 Cd1 O6 107.18(10) 2_765 1_565 ? O2 Cd1 O5 84.57(8) . 1_565 ? O2 Cd1 O5 170.07(7) 2_755 1_565 ? O6 Cd1 O5 80.49(7) 2_765 1_565 ? O6 Cd1 O5 53.52(6) 1_565 1_565 ? O2 Cd1 O5 170.07(7) . 2_765 ? O2 Cd1 O5 84.57(8) 2_755 2_765 ? O6 Cd1 O5 53.52(6) 2_765 2_765 ? O6 Cd1 O5 80.49(7) 1_565 2_765 ? O5 Cd1 O5 100.41(10) 1_565 2_765 ? O2 Cd1 O1 89.34(7) . 2_755 ? O2 Cd1 O1 53.35(7) 2_755 2_755 ? O6 Cd1 O1 128.97(7) 2_765 2_755 ? O6 Cd1 O1 83.70(6) 1_565 2_755 ? O5 Cd1 O1 135.63(6) 1_565 2_755 ? O5 Cd1 O1 81.09(7) 2_765 2_755 ? O2 Cd1 O1 53.35(7) . . ? O2 Cd1 O1 89.34(7) 2_755 . ? O6 Cd1 O1 83.70(6) 2_765 . ? O6 Cd1 O1 128.97(7) 1_565 . ? O5 Cd1 O1 81.09(7) 1_565 . ? O5 Cd1 O1 135.63(6) 2_765 . ? O1 Cd1 O1 128.13(10) 2_755 . ? O1 C1 O2 121.3(3) . . ? O1 C1 C2 121.0(3) . . ? O2 C1 C2 117.7(2) . . ? C11 C2 C3 118.8(2) . . ? C11 C2 C1 120.6(2) . . ? C3 C2 C1 120.6(2) . . ? O3 C3 C4 117.8(2) . . ? O3 C3 C2 120.8(2) . . ? C4 C3 C2 121.3(2) . . ? C3 C4 C5 119.1(2) . . ? C3 C4 C12 117.2(2) . . ? C5 C4 C12 123.6(2) . . ? C4 C5 C6 123.6(3) . . ? C4 C5 C10 119.7(2) . . ? C6 C5 C10 116.7(3) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 121.9(3) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C9 C8 C7 119.2(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 120.8(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 120.9(3) . . ? C11 C10 C5 119.1(2) . . ? C9 C10 C5 120.0(3) . . ? C2 C11 C10 122.0(2) . . ? C2 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C4 C12 C13 113.5(2) . . ? C4 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? C4 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C23 118.7(2) . . ? C14 C13 C12 117.4(2) . . ? C23 C13 C12 123.9(2) . . ? O4 C14 C13 118.2(2) . . ? O4 C14 C15 119.6(2) . . ? C13 C14 C15 122.1(2) . . ? C17 C15 C14 118.8(2) . . ? C17 C15 C16 120.2(2) . . ? C14 C15 C16 121.0(2) . . ? O6 C16 O5 121.7(2) . . ? O6 C16 C15 119.7(2) . . ? O5 C16 C15 118.6(2) . . ? C15 C17 C18 121.3(2) . . ? C15 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C19 120.2(3) . . ? C17 C18 C23 119.0(2) . . ? C19 C18 C23 120.8(3) . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.2(3) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 121.9(3) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 121.2(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C13 C23 C22 123.8(3) . . ? C13 C23 C18 119.9(2) . . ? C22 C23 C18 116.4(3) . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C25 N1 C24 145.3(5) . . ? C25 N1 H1A 100.5 . . ? C24 N1 H1A 100.5 . . ? C25 N1 H1B 100.5 . . ? C24 N1 H1B 100.5 . . ? H1A N1 H1B 104.3 . . ? C1 O1 Cd1 86.92(17) . . ? C1 O2 Cd1 98.25(16) . . ? C3 O3 H3A 109.5 . . ? C14 O4 H4A 109.5 . . ? C16 O5 Cd1 87.77(15) . 1_545 ? C16 O6 Cd1 97.00(16) . 1_545 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.210 _refine_diff_density_min -1.676 _refine_diff_density_rms 0.074 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 631544' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H29 N3 O7 Zn' _chemical_formula_weight 680.99 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.4015(12) _cell_length_b 9.7313(9) _cell_length_c 26.458(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.2890(10) _cell_angle_gamma 90.00 _cell_volume 3173.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3391 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 21.73 _exptl_crystal_description Block _exptl_crystal_colour Pale-Yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.807228 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 15208 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5556 _reflns_number_gt 3897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0501P)^2^+1.0701P] 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 5556 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.25695(3) 0.60711(4) 0.167277(13) 0.04632(14) Uani 1 1 d . . . O1 O 0.28429(17) 0.7682(2) 0.12353(7) 0.0503(5) Uani 1 1 d . . . O2 O 0.2922(2) 0.6166(2) 0.06168(8) 0.0592(6) Uani 1 1 d . . . O3 O 0.31175(18) 0.6962(2) -0.02808(7) 0.0490(5) Uani 1 1 d . . . H3 H 0.3022 0.6439 -0.0047 0.074 Uiso 1 1 calc R . . O4 O 0.41164(16) 1.0389(2) -0.18329(8) 0.0530(6) Uani 1 1 d . . . H4 H 0.4226 1.0882 -0.2073 0.080 Uiso 1 1 calc R . . O5 O 0.36894(19) 1.1979(2) -0.25903(8) 0.0605(6) Uani 1 1 d . . . O6 O 0.20892(18) 1.3024(2) -0.27230(8) 0.0528(6) Uani 1 1 d . . . O7 O 0.0956(2) 0.5731(3) 0.13240(10) 0.0713(7) Uani 1 1 d . . . N1 N 0.4193(2) 0.5335(3) 0.17258(9) 0.0511(7) Uani 1 1 d . . . N2 N 0.2456(3) 0.3952(3) 0.18864(12) 0.0658(8) Uani 1 1 d . . . N3 N -0.0527(3) 0.6001(4) 0.07475(14) 0.0914(11) Uani 1 1 d . . . C1 C 0.3379(3) 0.3214(3) 0.18929(12) 0.0594(9) Uani 1 1 d . . . C2 C 0.1540(4) 0.3341(5) 0.19776(19) 0.0942(14) Uani 1 1 d . . . H2 H 0.0908 0.3859 0.1971 0.113 Uiso 1 1 calc R . . C3 C 0.1506(5) 0.1939(6) 0.2083(2) 0.1179(19) Uani 1 1 d . . . H3A H 0.0877 0.1528 0.2172 0.141 Uiso 1 1 calc R . . C4 C 0.2437(6) 0.1181(5) 0.2051(2) 0.1098(18) Uani 1 1 d . . . H4A H 0.2418 0.0231 0.2087 0.132 Uiso 1 1 calc R . . C5 C 0.3370(4) 0.1796(4) 0.19679(15) 0.0815(12) Uani 1 1 d . . . H5 H 0.4001 0.1284 0.1960 0.098 Uiso 1 1 calc R . . C6 C 0.4357(3) 0.3995(3) 0.18114(11) 0.0537(8) Uani 1 1 d . . . C7 C 0.5048(3) 0.6121(4) 0.16528(14) 0.0653(10) Uani 1 1 d . . . H7 H 0.4940 0.7054 0.1592 0.078 Uiso 1 1 calc R . . C8 C 0.6088(3) 0.5594(5) 0.16651(15) 0.0782(12) Uani 1 1 d . . . H8 H 0.6667 0.6168 0.1616 0.094 Uiso 1 1 calc R . . C9 C 0.6252(4) 0.4246(5) 0.17492(16) 0.0789(12) Uani 1 1 d . . . H9 H 0.6945 0.3879 0.1754 0.095 Uiso 1 1 calc R . . C10 C 0.5395(4) 0.3409(4) 0.18286(13) 0.0705(11) Uani 1 1 d . . . H10 H 0.5499 0.2476 0.1892 0.085 Uiso 1 1 calc R . . C11 C 0.2992(2) 0.7362(3) 0.07807(12) 0.0450(7) Uani 1 1 d . . . C12 C 0.3300(2) 0.8258(3) -0.00940(10) 0.0377(7) Uani 1 1 d . . . C13 C 0.3502(2) 0.9304(3) -0.04232(10) 0.0365(7) Uani 1 1 d . . . C14 C 0.3686(2) 1.0653(3) -0.02291(11) 0.0369(7) Uani 1 1 d . . . C15 C 0.3975(2) 1.1767(3) -0.05318(12) 0.0448(7) Uani 1 1 d . . . H15 H 0.4053 1.1620 -0.0873 0.054 Uiso 1 1 calc R . . C16 C 0.4141(3) 1.3058(3) -0.03315(13) 0.0535(8) Uani 1 1 d . . . H16 H 0.4330 1.3771 -0.0539 0.064 Uiso 1 1 calc R . . C17 C 0.4029(3) 1.3321(3) 0.01821(13) 0.0552(9) Uani 1 1 d . . . H17 H 0.4123 1.4205 0.0313 0.066 Uiso 1 1 calc R . . C18 C 0.3781(3) 1.2261(3) 0.04862(12) 0.0498(8) Uani 1 1 d . . . H18 H 0.3720 1.2430 0.0828 0.060 Uiso 1 1 calc R . . C19 C 0.3615(2) 1.0918(3) 0.02963(11) 0.0391(7) Uani 1 1 d . . . C20 C 0.3382(2) 0.9822(3) 0.06131(11) 0.0417(7) Uani 1 1 d . . . H20 H 0.3327 0.9994 0.0955 0.050 Uiso 1 1 calc R . . C21 C 0.3235(2) 0.8511(3) 0.04335(11) 0.0381(7) Uani 1 1 d . . . C22 C 0.3512(2) 0.8983(3) -0.09849(10) 0.0414(7) Uani 1 1 d . . . H22A H 0.4234 0.9160 -0.1078 0.050 Uiso 1 1 calc R . . H22B H 0.3366 0.8011 -0.1037 0.050 Uiso 1 1 calc R . . C23 C 0.2701(2) 0.9792(3) -0.13414(10) 0.0378(7) Uani 1 1 d . . . C24 C 0.3053(2) 1.0503(3) -0.17427(10) 0.0396(7) Uani 1 1 d . . . C25 C 0.2340(2) 1.1396(3) -0.20574(10) 0.0402(7) Uani 1 1 d . . . C26 C 0.2747(3) 1.2184(3) -0.24829(11) 0.0466(8) Uani 1 1 d . . . C27 C 0.1291(3) 1.1515(3) -0.19555(11) 0.0465(8) Uani 1 1 d . . . H27 H 0.0832 1.2117 -0.2149 0.056 Uiso 1 1 calc R . . C28 C 0.0881(3) 1.0761(3) -0.15683(12) 0.0483(8) Uani 1 1 d . . . C29 C -0.0218(3) 1.0900(4) -0.14690(15) 0.0664(10) Uani 1 1 d . . . H29 H -0.0673 1.1505 -0.1663 0.080 Uiso 1 1 calc R . . C30 C -0.0610(3) 1.0164(5) -0.10971(17) 0.0883(14) Uani 1 1 d . . . H30 H -0.1326 1.0276 -0.1030 0.106 Uiso 1 1 calc R . . C31 C 0.0072(3) 0.9225(5) -0.08107(16) 0.0808(13) Uani 1 1 d . . . H31 H -0.0206 0.8704 -0.0560 0.097 Uiso 1 1 calc R . . C32 C 0.1124(3) 0.9065(4) -0.08925(13) 0.0589(9) Uani 1 1 d . . . H32 H 0.1552 0.8426 -0.0702 0.071 Uiso 1 1 calc R . . C33 C 0.1586(2) 0.9863(3) -0.12674(11) 0.0432(7) Uani 1 1 d . . . C34 C 0.0503(3) 0.6175(5) 0.09249(18) 0.0844(13) Uani 1 1 d . . . H34 H 0.0925 0.6690 0.0725 0.101 Uiso 1 1 calc R . . C35 C -0.1241(4) 0.5311(7) 0.1050(2) 0.141(2) Uani 1 1 d . . . H35A H -0.0872 0.5138 0.1382 0.211 Uiso 1 1 calc R . . H35B H -0.1467 0.4455 0.0892 0.211 Uiso 1 1 calc R . . H35C H -0.1865 0.5876 0.1080 0.211 Uiso 1 1 calc R . . C36 C -0.1017(5) 0.6658(9) 0.0284(3) 0.189(4) Uani 1 1 d . . . H36A H -0.1516 0.7353 0.0368 0.283 Uiso 1 1 calc R . . H36B H -0.1397 0.5983 0.0068 0.283 Uiso 1 1 calc R . . H36C H -0.0460 0.7072 0.0109 0.283 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0586(3) 0.0403(2) 0.0408(2) -0.00115(17) 0.00850(16) -0.00018(18) O1 0.0604(14) 0.0543(13) 0.0370(12) 0.0071(10) 0.0091(10) 0.0052(11) O2 0.0834(18) 0.0427(13) 0.0534(14) 0.0065(11) 0.0165(12) 0.0004(12) O3 0.0659(15) 0.0386(12) 0.0422(12) -0.0002(10) 0.0041(11) -0.0024(11) O4 0.0411(13) 0.0722(16) 0.0476(13) 0.0125(11) 0.0130(10) 0.0043(11) O5 0.0544(15) 0.0775(17) 0.0508(14) 0.0180(12) 0.0115(11) -0.0033(12) O6 0.0644(15) 0.0502(13) 0.0438(12) 0.0093(10) 0.0062(11) 0.0039(11) O7 0.0673(18) 0.0788(18) 0.0656(17) 0.0009(14) -0.0026(14) -0.0161(14) N1 0.0661(19) 0.0430(16) 0.0432(15) -0.0035(12) 0.0014(13) 0.0047(14) N2 0.083(2) 0.0521(17) 0.0657(19) -0.0005(15) 0.0204(17) -0.0124(17) N3 0.056(2) 0.136(3) 0.080(2) -0.009(2) -0.0034(19) -0.019(2) C1 0.093(3) 0.045(2) 0.0385(18) 0.0034(15) -0.0012(18) 0.009(2) C2 0.100(4) 0.075(3) 0.114(4) 0.010(3) 0.040(3) -0.016(3) C3 0.136(5) 0.081(4) 0.143(5) 0.015(3) 0.046(4) -0.041(4) C4 0.155(6) 0.066(3) 0.109(4) 0.039(3) 0.013(4) -0.015(4) C5 0.114(4) 0.057(2) 0.070(3) 0.017(2) -0.007(2) 0.002(2) C6 0.078(3) 0.051(2) 0.0307(16) -0.0063(15) -0.0006(15) 0.0071(19) C7 0.064(2) 0.065(2) 0.068(2) -0.010(2) 0.0105(19) -0.003(2) C8 0.064(3) 0.098(3) 0.073(3) -0.026(2) 0.009(2) -0.002(2) C9 0.074(3) 0.090(3) 0.072(3) -0.027(2) 0.002(2) 0.013(3) C10 0.098(3) 0.064(2) 0.048(2) -0.0086(18) -0.003(2) 0.032(2) C11 0.0436(19) 0.0471(19) 0.0444(19) 0.0071(15) 0.0051(14) 0.0060(15) C12 0.0364(17) 0.0374(16) 0.0385(16) -0.0036(13) 0.0005(12) 0.0037(13) C13 0.0337(16) 0.0406(16) 0.0350(15) 0.0007(12) 0.0033(12) 0.0064(12) C14 0.0303(16) 0.0408(16) 0.0395(16) 0.0007(13) 0.0027(12) 0.0053(12) C15 0.0415(18) 0.0488(19) 0.0434(17) 0.0013(15) 0.0016(14) -0.0006(15) C16 0.053(2) 0.0456(19) 0.061(2) 0.0054(17) 0.0023(16) -0.0077(16) C17 0.058(2) 0.0395(18) 0.067(2) -0.0082(17) 0.0016(18) -0.0017(16) C18 0.051(2) 0.050(2) 0.0481(19) -0.0113(16) 0.0051(15) 0.0005(15) C19 0.0338(16) 0.0415(17) 0.0415(16) -0.0056(14) 0.0025(12) 0.0026(13) C20 0.0412(18) 0.0480(18) 0.0359(16) -0.0022(14) 0.0051(13) 0.0061(14) C21 0.0330(16) 0.0427(17) 0.0386(16) 0.0028(13) 0.0035(13) 0.0067(12) C22 0.0425(17) 0.0475(17) 0.0345(15) -0.0010(14) 0.0048(13) 0.0054(14) C23 0.0397(17) 0.0404(16) 0.0329(15) -0.0032(13) 0.0016(13) 0.0000(13) C24 0.0385(18) 0.0460(17) 0.0337(16) -0.0045(13) 0.0012(13) -0.0020(14) C25 0.0456(18) 0.0413(17) 0.0328(15) -0.0007(12) 0.0003(13) -0.0030(13) C26 0.061(2) 0.0437(18) 0.0339(16) 0.0008(14) 0.0005(15) -0.0053(16) C27 0.050(2) 0.0471(18) 0.0405(17) 0.0050(14) -0.0011(15) 0.0063(15) C28 0.0399(18) 0.057(2) 0.0474(18) 0.0018(15) 0.0032(14) 0.0010(15) C29 0.045(2) 0.083(3) 0.072(2) 0.018(2) 0.0076(18) 0.0095(19) C30 0.044(2) 0.128(4) 0.096(3) 0.029(3) 0.022(2) 0.005(2) C31 0.053(2) 0.111(3) 0.080(3) 0.041(3) 0.011(2) -0.004(2) C32 0.047(2) 0.073(2) 0.056(2) 0.0184(18) 0.0032(16) -0.0057(17) C33 0.0422(18) 0.0455(18) 0.0411(17) 0.0011(14) 0.0007(14) -0.0038(14) C34 0.059(3) 0.114(4) 0.080(3) 0.004(3) 0.008(2) -0.019(3) C35 0.083(4) 0.193(6) 0.148(5) -0.019(5) 0.015(4) -0.060(4) C36 0.095(5) 0.316(11) 0.142(6) 0.081(7) -0.044(4) -0.028(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 Zn1 O6 1.974(2) 4_576 ? Zn1 O1 2.000(2) . ? Zn1 N1 2.127(3) . ? Zn1 O7 2.135(3) . ? Zn1 N2 2.147(3) . ? O1 C11 1.275(3) . ? O2 C11 1.242(4) . ? O3 C12 1.364(3) . ? O3 H3 0.8200 . ? O4 C24 1.370(3) . ? O4 H4 0.8200 . ? O5 C26 1.248(4) . ? O6 C26 1.274(4) . ? O6 Zn1 1.974(2) 4_575 ? O7 C34 1.220(5) . ? N1 C7 1.338(4) . ? N1 C6 1.335(4) . ? N2 C2 1.328(5) . ? N2 C1 1.350(5) . ? N3 C34 1.322(5) . ? N3 C35 1.426(6) . ? N3 C36 1.456(7) . ? C1 C5 1.394(5) . ? C1 C6 1.467(5) . ? C2 C3 1.395(6) . ? C2 H2 0.9300 . ? C3 C4 1.380(7) . ? C3 H3A 0.9300 . ? C4 C5 1.341(7) . ? C4 H4A 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.403(5) . ? C7 C8 1.385(5) . ? C7 H7 0.9300 . ? C8 C9 1.342(6) . ? C8 H8 0.9300 . ? C9 C10 1.373(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C21 1.499(4) . ? C12 C13 1.380(4) . ? C12 C21 1.428(4) . ? C13 C14 1.419(4) . ? C13 C22 1.520(4) . ? C14 C15 1.417(4) . ? C14 C19 1.426(4) . ? C15 C16 1.370(4) . ? C15 H15 0.9300 . ? C16 C17 1.404(5) . ? C16 H16 0.9300 . ? C17 C18 1.364(4) . ? C17 H17 0.9300 . ? C18 C19 1.407(4) . ? C18 H18 0.9300 . ? C19 C20 1.406(4) . ? C20 C21 1.366(4) . ? C20 H20 0.9300 . ? C22 C23 1.521(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.378(4) . ? C23 C33 1.419(4) . ? C24 C25 1.439(4) . ? C25 C27 1.363(4) . ? C25 C26 1.495(4) . ? C27 C28 1.400(4) . ? C27 H27 0.9300 . ? C28 C33 1.418(4) . ? C28 C29 1.422(4) . ? C29 C30 1.350(5) . ? C29 H29 0.9300 . ? C30 C31 1.408(6) . ? C30 H30 0.9300 . ? C31 C32 1.355(5) . ? C31 H31 0.9300 . ? C32 C33 1.428(4) . ? C32 H32 0.9300 . ? C34 H34 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 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 O6 Zn1 O1 101.79(9) 4_576 . ? O6 Zn1 N1 117.67(9) 4_576 . ? O1 Zn1 N1 94.76(10) . . ? O6 Zn1 O7 93.88(10) 4_576 . ? O1 Zn1 O7 94.68(10) . . ? N1 Zn1 O7 144.24(10) . . ? O6 Zn1 N2 100.43(10) 4_576 . ? O1 Zn1 N2 157.77(10) . . ? N1 Zn1 N2 75.41(12) . . ? O7 Zn1 N2 83.08(12) . . ? C11 O1 Zn1 113.92(19) . . ? C12 O3 H3 109.5 . . ? C24 O4 H4 109.5 . . ? C26 O6 Zn1 117.1(2) . 4_575 ? C34 O7 Zn1 129.8(3) . . ? C7 N1 C6 118.3(3) . . ? C7 N1 Zn1 123.9(2) . . ? C6 N1 Zn1 117.7(2) . . ? C2 N2 C1 120.0(4) . . ? C2 N2 Zn1 124.1(3) . . ? C1 N2 Zn1 115.8(2) . . ? C34 N3 C35 119.8(4) . . ? C34 N3 C36 122.7(4) . . ? C35 N3 C36 116.9(5) . . ? N2 C1 C5 120.6(4) . . ? N2 C1 C6 115.8(3) . . ? C5 C1 C6 123.6(4) . . ? N2 C2 C3 121.3(5) . . ? N2 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 117.8(5) . . ? C4 C3 H3A 121.1 . . ? C2 C3 H3A 121.1 . . ? C5 C4 C3 120.9(5) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C1 119.0(5) . . ? C4 C5 H5 120.5 . . ? C1 C5 H5 120.5 . . ? N1 C6 C10 121.6(4) . . ? N1 C6 C1 114.7(3) . . ? C10 C6 C1 123.7(3) . . ? N1 C7 C8 122.4(4) . . ? N1 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? C9 C8 C7 119.3(4) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 120.0(4) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C6 118.4(4) . . ? C9 C10 H10 120.8 . . ? C6 C10 H10 120.8 . . ? O2 C11 O1 123.2(3) . . ? O2 C11 C21 119.7(3) . . ? O1 C11 C21 117.1(3) . . ? O3 C12 C13 119.2(2) . . ? O3 C12 C21 119.3(3) . . ? C13 C12 C21 121.5(3) . . ? C12 C13 C14 119.2(2) . . ? C12 C13 C22 119.1(3) . . ? C14 C13 C22 121.7(2) . . ? C13 C14 C15 123.0(3) . . ? C13 C14 C19 119.7(3) . . ? C15 C14 C19 117.3(3) . . ? C16 C15 C14 121.3(3) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 121.0(3) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C18 C17 C16 119.1(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 121.7(3) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C20 C19 C18 121.6(3) . . ? C20 C19 C14 118.8(3) . . ? C18 C19 C14 119.6(3) . . ? C21 C20 C19 122.0(3) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C12 118.8(3) . . ? C20 C21 C11 120.8(3) . . ? C12 C21 C11 120.4(3) . . ? C23 C22 C13 115.1(2) . . ? C23 C22 H22A 108.5 . . ? C13 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? C13 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C24 C23 C33 118.6(3) . . ? C24 C23 C22 119.6(3) . . ? C33 C23 C22 121.8(2) . . ? O4 C24 C23 119.1(3) . . ? O4 C24 C25 119.4(2) . . ? C23 C24 C25 121.5(3) . . ? C27 C25 C24 118.5(3) . . ? C27 C25 C26 120.9(3) . . ? C24 C25 C26 120.6(3) . . ? O5 C26 O6 123.6(3) . . ? O5 C26 C25 119.4(3) . . ? O6 C26 C25 117.0(3) . . ? C25 C27 C28 122.1(3) . . ? C25 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C27 C28 C33 118.8(3) . . ? C27 C28 C29 121.2(3) . . ? C33 C28 C29 120.0(3) . . ? C30 C29 C28 120.9(4) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.6(4) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 121.4(4) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 121.0(3) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C23 C33 C28 120.2(3) . . ? C23 C33 C32 122.7(3) . . ? C28 C33 C32 117.1(3) . . ? O7 C34 N3 126.7(4) . . ? O7 C34 H34 116.7 . . ? N3 C34 H34 116.7 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zn1 O1 C11 -168.8(2) 4_576 . . . ? N1 Zn1 O1 C11 71.6(2) . . . . ? O7 Zn1 O1 C11 -73.9(2) . . . . ? N2 Zn1 O1 C11 9.3(4) . . . . ? O6 Zn1 O7 C34 117.0(4) 4_576 . . . ? O1 Zn1 O7 C34 14.8(4) . . . . ? N1 Zn1 O7 C34 -90.0(4) . . . . ? N2 Zn1 O7 C34 -142.9(4) . . . . ? O6 Zn1 N1 C7 -83.5(3) 4_576 . . . ? O1 Zn1 N1 C7 22.4(3) . . . . ? O7 Zn1 N1 C7 127.2(3) . . . . ? N2 Zn1 N1 C7 -177.8(3) . . . . ? O6 Zn1 N1 C6 100.0(2) 4_576 . . . ? O1 Zn1 N1 C6 -154.0(2) . . . . ? O7 Zn1 N1 C6 -49.2(3) . . . . ? N2 Zn1 N1 C6 5.7(2) . . . . ? O6 Zn1 N2 C2 61.5(4) 4_576 . . . ? O1 Zn1 N2 C2 -116.7(4) . . . . ? N1 Zn1 N2 C2 177.6(4) . . . . ? O7 Zn1 N2 C2 -31.2(4) . . . . ? O6 Zn1 N2 C1 -122.8(2) 4_576 . . . ? O1 Zn1 N2 C1 59.1(4) . . . . ? N1 Zn1 N2 C1 -6.6(2) . . . . ? O7 Zn1 N2 C1 144.6(3) . . . . ? C2 N2 C1 C5 3.5(6) . . . . ? Zn1 N2 C1 C5 -172.5(3) . . . . ? C2 N2 C1 C6 -177.2(4) . . . . ? Zn1 N2 C1 C6 6.8(4) . . . . ? C1 N2 C2 C3 0.2(7) . . . . ? Zn1 N2 C2 C3 175.8(4) . . . . ? N2 C2 C3 C4 -5.0(9) . . . . ? C2 C3 C4 C5 6.1(9) . . . . ? C3 C4 C5 C1 -2.6(8) . . . . ? N2 C1 C5 C4 -2.3(6) . . . . ? C6 C1 C5 C4 178.5(4) . . . . ? C7 N1 C6 C10 0.4(5) . . . . ? Zn1 N1 C6 C10 177.0(2) . . . . ? C7 N1 C6 C1 179.3(3) . . . . ? Zn1 N1 C6 C1 -4.0(3) . . . . ? N2 C1 C6 N1 -1.9(4) . . . . ? C5 C1 C6 N1 177.3(3) . . . . ? N2 C1 C6 C10 177.0(3) . . . . ? C5 C1 C6 C10 -3.7(5) . . . . ? C6 N1 C7 C8 -0.2(5) . . . . ? Zn1 N1 C7 C8 -176.7(3) . . . . ? N1 C7 C8 C9 0.5(6) . . . . ? C7 C8 C9 C10 -0.9(6) . . . . ? C8 C9 C10 C6 1.0(6) . . . . ? N1 C6 C10 C9 -0.7(5) . . . . ? C1 C6 C10 C9 -179.6(3) . . . . ? Zn1 O1 C11 O2 3.3(4) . . . . ? Zn1 O1 C11 C21 -178.20(19) . . . . ? O3 C12 C13 C14 179.7(3) . . . . ? C21 C12 C13 C14 2.2(4) . . . . ? O3 C12 C13 C22 0.2(4) . . . . ? C21 C12 C13 C22 -177.3(3) . . . . ? C12 C13 C14 C15 175.4(3) . . . . ? C22 C13 C14 C15 -5.0(4) . . . . ? C12 C13 C14 C19 -2.7(4) . . . . ? C22 C13 C14 C19 176.9(2) . . . . ? C13 C14 C15 C16 179.6(3) . . . . ? C19 C14 C15 C16 -2.3(4) . . . . ? C14 C15 C16 C17 -0.1(5) . . . . ? C15 C16 C17 C18 1.8(5) . . . . ? C16 C17 C18 C19 -1.2(5) . . . . ? C17 C18 C19 C20 178.7(3) . . . . ? C17 C18 C19 C14 -1.2(5) . . . . ? C13 C14 C19 C20 1.2(4) . . . . ? C15 C14 C19 C20 -177.0(3) . . . . ? C13 C14 C19 C18 -178.9(3) . . . . ? C15 C14 C19 C18 2.9(4) . . . . ? C18 C19 C20 C21 -179.1(3) . . . . ? C14 C19 C20 C21 0.8(4) . . . . ? C19 C20 C21 C12 -1.2(4) . . . . ? C19 C20 C21 C11 179.8(3) . . . . ? O3 C12 C21 C20 -177.8(3) . . . . ? C13 C12 C21 C20 -0.3(4) . . . . ? O3 C12 C21 C11 1.2(4) . . . . ? C13 C12 C21 C11 178.7(3) . . . . ? O2 C11 C21 C20 -175.9(3) . . . . ? O1 C11 C21 C20 5.5(4) . . . . ? O2 C11 C21 C12 5.1(4) . . . . ? O1 C11 C21 C12 -173.5(3) . . . . ? C12 C13 C22 C23 121.5(3) . . . . ? C14 C13 C22 C23 -58.0(4) . . . . ? C13 C22 C23 C24 127.4(3) . . . . ? C13 C22 C23 C33 -51.3(4) . . . . ? C33 C23 C24 O4 -176.9(3) . . . . ? C22 C23 C24 O4 4.4(4) . . . . ? C33 C23 C24 C25 5.3(4) . . . . ? C22 C23 C24 C25 -173.4(3) . . . . ? O4 C24 C25 C27 -178.8(3) . . . . ? C23 C24 C25 C27 -0.9(4) . . . . ? O4 C24 C25 C26 0.6(4) . . . . ? C23 C24 C25 C26 178.5(3) . . . . ? Zn1 O6 C26 O5 4.8(4) 4_575 . . . ? Zn1 O6 C26 C25 -174.04(19) 4_575 . . . ? C27 C25 C26 O5 -174.9(3) . . . . ? C24 C25 C26 O5 5.8(4) . . . . ? C27 C25 C26 O6 4.0(4) . . . . ? C24 C25 C26 O6 -175.4(3) . . . . ? C24 C25 C27 C28 -2.4(4) . . . . ? C26 C25 C27 C28 178.2(3) . . . . ? C25 C27 C28 C33 1.1(5) . . . . ? C25 C27 C28 C29 -179.9(3) . . . . ? C27 C28 C29 C30 179.6(4) . . . . ? C33 C28 C29 C30 -1.4(6) . . . . ? C28 C29 C30 C31 -1.3(7) . . . . ? C29 C30 C31 C32 1.5(7) . . . . ? C30 C31 C32 C33 1.1(7) . . . . ? C24 C23 C33 C28 -6.5(4) . . . . ? C22 C23 C33 C28 172.2(3) . . . . ? C24 C23 C33 C32 174.1(3) . . . . ? C22 C23 C33 C32 -7.3(4) . . . . ? C27 C28 C33 C23 3.4(4) . . . . ? C29 C28 C33 C23 -175.6(3) . . . . ? C27 C28 C33 C32 -177.1(3) . . . . ? C29 C28 C33 C32 3.9(5) . . . . ? C31 C32 C33 C23 175.7(4) . . . . ? C31 C32 C33 C28 -3.8(5) . . . . ? Zn1 O7 C34 N3 -174.8(3) . . . . ? C35 N3 C34 O7 4.6(8) . . . . ? C36 N3 C34 O7 175.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.953 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.052 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 631545' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Cd N3 O7.5' _chemical_formula_weight 737.03 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 15.7420(9) _cell_length_b 9.3890(5) _cell_length_c 22.7454(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.8190(10) _cell_angle_gamma 90.00 _cell_volume 3349.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5296 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.73 _exptl_crystal_description Block _exptl_crystal_colour Pale-Yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.856850 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 17565 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5889 _reflns_number_gt 4830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0383P)^2^+1.4947P] 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 5889 _refine_ls_number_parameters 433 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.031 _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 Cd1 Cd 0.375977(12) 0.29110(2) 0.426929(8) 0.03926(8) Uani 1 1 d . . . O1 O 0.33665(12) 0.4076(2) 0.33288(8) 0.0564(5) Uani 1 1 d . . . O2 O 0.46596(12) 0.4416(2) 0.37324(7) 0.0480(5) Uani 1 1 d . . . O3 O 0.58182(10) 0.5429(2) 0.31525(7) 0.0457(4) Uani 1 1 d . . . H3 H 0.5606 0.4997 0.3417 0.069 Uiso 1 1 calc R . . O4 O 0.72496(13) 0.76188(18) 0.12073(9) 0.0512(5) Uani 1 1 d . . . H4 H 0.7482 0.7888 0.0918 0.077 Uiso 1 1 calc R . . O5 O 0.80847(13) 0.7482(2) 0.03040(9) 0.0539(5) Uani 1 1 d . . . O6 O 0.82724(12) 0.5431(2) -0.01305(8) 0.0496(5) Uani 1 1 d . . . O7 O 0.24922(14) 0.1747(2) 0.40157(10) 0.0653(6) Uani 1 1 d . . . N1 N 0.50310(14) 0.2321(2) 0.48156(9) 0.0396(5) Uani 1 1 d . . . N2 N 0.44087(15) 0.1010(2) 0.38113(9) 0.0463(5) Uani 1 1 d . . . N3 N 0.10579(19) 0.1979(4) 0.39150(15) 0.0835(9) Uani 1 1 d . . . C1 C 0.41063(17) 0.4534(3) 0.32989(11) 0.0412(6) Uani 1 1 d . . . C2 C 0.43565(15) 0.5217(3) 0.27450(10) 0.0368(6) Uani 1 1 d . . . C3 C 0.52263(15) 0.5600(3) 0.26896(10) 0.0334(5) Uani 1 1 d . . . C4 C 0.54880(14) 0.6116(3) 0.21688(10) 0.0330(5) Uani 1 1 d . . . C5 C 0.48718(15) 0.6367(3) 0.16887(10) 0.0408(6) Uani 1 1 d . . . C6 C 0.5079(2) 0.6973(3) 0.11451(13) 0.0585(8) Uani 1 1 d . . . H6 H 0.5635 0.7262 0.1100 0.070 Uiso 1 1 calc R . . C7 C 0.4465(2) 0.7131(5) 0.06896(15) 0.0830(12) Uani 1 1 d . . . H7 H 0.4614 0.7508 0.0334 0.100 Uiso 1 1 calc R . . C8 C 0.3617(2) 0.6741(5) 0.07429(16) 0.0950(15) Uani 1 1 d . . . H8 H 0.3211 0.6858 0.0425 0.114 Uiso 1 1 calc R . . C9 C 0.3388(2) 0.6193(5) 0.12565(13) 0.0777(11) Uani 1 1 d . . . H9 H 0.2823 0.5940 0.1290 0.093 Uiso 1 1 calc R . . C10 C 0.39991(17) 0.6000(3) 0.17447(11) 0.0513(7) Uani 1 1 d . . . C11 C 0.37757(16) 0.5415(3) 0.22743(11) 0.0483(7) Uani 1 1 d . . . H11 H 0.3212 0.5153 0.2307 0.058 Uiso 1 1 calc R . . C12 C 0.64333(15) 0.6388(3) 0.21216(10) 0.0360(5) Uani 1 1 d . . . H12A H 0.6510 0.7388 0.2032 0.043 Uiso 1 1 calc R . . H12B H 0.6736 0.6203 0.2503 0.043 Uiso 1 1 calc R . . C13 C 0.68396(14) 0.5507(3) 0.16609(10) 0.0318(5) Uani 1 1 d . . . C14 C 0.72320(14) 0.6177(3) 0.12178(10) 0.0335(5) Uani 1 1 d . . . C15 C 0.76033(14) 0.5394(3) 0.07670(10) 0.0330(5) Uani 1 1 d . . . C16 C 0.80170(15) 0.6142(3) 0.02864(11) 0.0400(6) Uani 1 1 d . . . C17 C 0.75758(15) 0.3945(3) 0.07796(10) 0.0379(6) Uani 1 1 d . . . H17 H 0.7815 0.3433 0.0485 0.046 Uiso 1 1 calc R . . C18 C 0.71963(16) 0.3202(3) 0.12246(11) 0.0399(6) Uani 1 1 d . . . C19 C 0.7164(2) 0.1693(3) 0.12393(14) 0.0579(8) Uani 1 1 d . . . H19 H 0.7387 0.1177 0.0939 0.069 Uiso 1 1 calc R . . C20 C 0.6820(2) 0.0987(3) 0.16786(15) 0.0679(9) Uani 1 1 d . . . H20 H 0.6793 -0.0003 0.1675 0.082 Uiso 1 1 calc R . . C21 C 0.6504(2) 0.1757(3) 0.21382(14) 0.0589(8) Uani 1 1 d . . . H21 H 0.6283 0.1270 0.2447 0.071 Uiso 1 1 calc R . . C22 C 0.65127(17) 0.3203(3) 0.21437(12) 0.0430(6) Uani 1 1 d . . . H22 H 0.6301 0.3686 0.2457 0.052 Uiso 1 1 calc R . . C23 C 0.68393(14) 0.3990(3) 0.16810(10) 0.0342(5) Uani 1 1 d . . . C24 C 0.52985(18) 0.2934(3) 0.53274(11) 0.0465(7) Uani 1 1 d . . . H24 H 0.4973 0.3668 0.5467 0.056 Uiso 1 1 calc R . . C25 C 0.6027(2) 0.2538(3) 0.56570(13) 0.0532(7) Uani 1 1 d . . . H25 H 0.6202 0.3012 0.6006 0.064 Uiso 1 1 calc R . . C26 C 0.64931(18) 0.1432(3) 0.54629(13) 0.0526(7) Uani 1 1 d . . . H26 H 0.6982 0.1122 0.5684 0.063 Uiso 1 1 calc R . . C27 C 0.62328(17) 0.0781(3) 0.49370(12) 0.0466(7) Uani 1 1 d . . . H27 H 0.6544 0.0027 0.4799 0.056 Uiso 1 1 calc R . . C28 C 0.55016(16) 0.1260(3) 0.46148(11) 0.0383(6) Uani 1 1 d . . . C29 C 0.51872(17) 0.0617(3) 0.40385(11) 0.0419(6) Uani 1 1 d . . . C30 C 0.5675(2) -0.0356(3) 0.37502(14) 0.0594(8) Uani 1 1 d . . . H30 H 0.6218 -0.0605 0.3911 0.071 Uiso 1 1 calc R . . C31 C 0.5350(3) -0.0937(4) 0.32319(15) 0.0695(9) Uani 1 1 d . . . H31 H 0.5673 -0.1579 0.3033 0.083 Uiso 1 1 calc R . . C32 C 0.4547(3) -0.0576(4) 0.30016(14) 0.0732(10) Uani 1 1 d . . . H32 H 0.4310 -0.0985 0.2653 0.088 Uiso 1 1 calc R . . C33 C 0.4098(2) 0.0415(3) 0.33032(13) 0.0625(8) Uani 1 1 d . . . H33 H 0.3557 0.0679 0.3146 0.075 Uiso 1 1 calc R . . C34 C 0.1816(3) 0.2340(4) 0.40803(19) 0.0805(11) Uani 1 1 d . . . H34 H 0.1866 0.3198 0.4284 0.097 Uiso 1 1 calc R . . C35 C 0.0949(5) 0.0866(9) 0.3483(4) 0.245(5) Uani 1 1 d U . . H35A H 0.1472 0.0727 0.3303 0.368 Uiso 1 1 calc R . . H35B H 0.0506 0.1128 0.3187 0.368 Uiso 1 1 calc R . . H35C H 0.0794 -0.0001 0.3671 0.368 Uiso 1 1 calc R . . C36 C 0.0293(3) 0.2786(6) 0.4011(3) 0.136(2) Uani 1 1 d U . . H36A H 0.0439 0.3569 0.4272 0.204 Uiso 1 1 calc R . . H36B H -0.0108 0.2179 0.4184 0.204 Uiso 1 1 calc R . . H36C H 0.0044 0.3144 0.3640 0.204 Uiso 1 1 calc R . . O8 O 0.2500 0.2153(4) 0.2500 0.1163(17) Uani 1 2 d SU . . 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 Cd1 0.03956(12) 0.04387(13) 0.03604(11) -0.00052(8) 0.01310(8) 0.00270(9) O1 0.0422(11) 0.0815(15) 0.0478(11) 0.0059(10) 0.0182(9) -0.0110(10) O2 0.0512(11) 0.0606(12) 0.0330(9) 0.0037(9) 0.0089(8) -0.0067(9) O3 0.0360(10) 0.0710(13) 0.0300(9) 0.0030(9) 0.0022(7) -0.0049(9) O4 0.0669(13) 0.0318(10) 0.0598(13) -0.0031(8) 0.0339(10) -0.0096(9) O5 0.0671(14) 0.0454(12) 0.0528(12) 0.0020(9) 0.0258(10) -0.0144(10) O6 0.0579(12) 0.0526(12) 0.0419(10) 0.0004(9) 0.0259(9) -0.0003(9) O7 0.0484(13) 0.0729(15) 0.0759(15) -0.0062(12) 0.0135(11) -0.0091(11) N1 0.0417(12) 0.0377(12) 0.0406(12) 0.0002(10) 0.0115(10) 0.0016(10) N2 0.0577(15) 0.0421(13) 0.0398(12) -0.0036(10) 0.0077(10) 0.0022(11) N3 0.0500(18) 0.101(3) 0.099(2) -0.004(2) 0.0017(16) -0.0152(17) C1 0.0434(16) 0.0434(15) 0.0391(14) -0.0049(12) 0.0183(12) 0.0012(12) C2 0.0338(13) 0.0444(15) 0.0337(13) -0.0036(11) 0.0115(10) 0.0002(11) C3 0.0330(13) 0.0388(14) 0.0290(12) -0.0042(10) 0.0066(10) 0.0012(10) C4 0.0312(12) 0.0361(13) 0.0331(12) -0.0032(10) 0.0101(10) 0.0009(10) C5 0.0360(14) 0.0530(16) 0.0346(13) 0.0032(12) 0.0093(11) 0.0073(12) C6 0.0480(17) 0.082(2) 0.0475(16) 0.0224(16) 0.0159(13) 0.0131(15) C7 0.069(2) 0.134(4) 0.0473(18) 0.036(2) 0.0119(17) 0.024(2) C8 0.056(2) 0.174(5) 0.054(2) 0.031(2) -0.0092(17) 0.020(2) C9 0.0414(17) 0.140(4) 0.0504(18) 0.019(2) -0.0029(14) 0.009(2) C10 0.0356(14) 0.077(2) 0.0416(15) 0.0084(14) 0.0039(12) 0.0082(14) C11 0.0283(13) 0.072(2) 0.0460(15) 0.0033(14) 0.0095(11) -0.0004(13) C12 0.0347(13) 0.0388(14) 0.0358(13) -0.0039(11) 0.0113(10) -0.0038(11) C13 0.0262(12) 0.0369(13) 0.0332(12) -0.0010(10) 0.0073(9) -0.0012(10) C14 0.0320(13) 0.0324(13) 0.0371(12) -0.0017(10) 0.0093(10) -0.0052(10) C15 0.0284(12) 0.0388(14) 0.0328(12) 0.0000(10) 0.0078(10) -0.0025(10) C16 0.0325(13) 0.0509(17) 0.0375(13) 0.0035(12) 0.0083(11) -0.0033(12) C17 0.0379(14) 0.0405(15) 0.0370(13) -0.0039(11) 0.0126(10) 0.0032(11) C18 0.0403(14) 0.0359(14) 0.0449(14) 0.0021(11) 0.0117(11) 0.0036(11) C19 0.071(2) 0.0382(16) 0.068(2) -0.0020(14) 0.0289(16) 0.0068(14) C20 0.086(2) 0.0317(16) 0.091(2) 0.0113(16) 0.0333(19) 0.0043(16) C21 0.0612(19) 0.0500(18) 0.069(2) 0.0221(15) 0.0257(16) 0.0042(15) C22 0.0405(15) 0.0426(16) 0.0477(15) 0.0096(12) 0.0144(12) 0.0047(12) C23 0.0271(12) 0.0390(14) 0.0370(12) 0.0026(11) 0.0050(10) 0.0010(10) C24 0.0541(17) 0.0438(16) 0.0426(15) -0.0040(13) 0.0096(13) -0.0009(13) C25 0.0559(18) 0.0519(17) 0.0503(17) 0.0003(13) -0.0043(14) -0.0084(14) C26 0.0440(16) 0.0505(18) 0.0627(18) 0.0102(15) -0.0001(14) -0.0069(14) C27 0.0417(15) 0.0392(15) 0.0606(17) 0.0087(13) 0.0142(13) 0.0013(12) C28 0.0398(14) 0.0334(14) 0.0443(14) 0.0056(11) 0.0185(11) -0.0041(11) C29 0.0492(16) 0.0343(14) 0.0449(14) 0.0023(11) 0.0186(12) -0.0013(12) C30 0.066(2) 0.0485(18) 0.067(2) -0.0089(15) 0.0222(16) 0.0071(15) C31 0.095(3) 0.052(2) 0.065(2) -0.0143(17) 0.0272(19) 0.0068(19) C32 0.113(3) 0.059(2) 0.0479(18) -0.0169(16) 0.0100(19) 0.000(2) C33 0.081(2) 0.060(2) 0.0466(17) -0.0067(15) 0.0000(15) 0.0046(17) C34 0.065(3) 0.081(3) 0.093(3) -0.003(2) -0.008(2) -0.012(2) C35 0.129(6) 0.255(10) 0.348(11) -0.171(9) 0.007(6) -0.056(6) C36 0.059(3) 0.167(6) 0.180(6) -0.002(4) -0.003(3) 0.010(3) O8 0.147(4) 0.087(3) 0.105(3) 0.000 -0.047(3) 0.000 _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 Cd1 O6 2.2473(18) 4_566 ? Cd1 O7 2.305(2) . ? Cd1 N1 2.332(2) . ? Cd1 N2 2.343(2) . ? Cd1 O2 2.4053(18) . ? Cd1 O1 2.4361(19) . ? O1 C1 1.249(3) . ? O2 C1 1.264(3) . ? O3 C3 1.356(3) . ? O3 H3 0.8200 . ? O4 C14 1.355(3) . ? O4 H4 0.8200 . ? O5 C16 1.263(3) . ? O6 C16 1.253(3) . ? O6 Cd1 2.2473(18) 4_665 ? O7 C34 1.221(4) . ? N1 C24 1.335(3) . ? N1 C28 1.344(3) . ? N2 C33 1.339(4) . ? N2 C29 1.341(3) . ? N3 C34 1.267(4) . ? N3 C35 1.434(7) . ? N3 C36 1.454(6) . ? C1 C2 1.496(3) . ? C2 C11 1.361(3) . ? C2 C3 1.431(3) . ? C3 C4 1.375(3) . ? C4 C5 1.418(3) . ? C4 C12 1.522(3) . ? C5 C6 1.423(4) . ? C5 C10 1.433(4) . ? C6 C7 1.364(4) . ? C6 H6 0.9300 . ? C7 C8 1.400(5) . ? C7 H7 0.9300 . ? C8 C9 1.353(5) . ? C8 H8 0.9300 . ? C9 C10 1.419(4) . ? C9 H9 0.9300 . ? C10 C11 1.395(4) . ? C11 H11 0.9300 . ? C12 C13 1.518(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.377(3) . ? C13 C23 1.425(3) . ? C14 C15 1.426(3) . ? C15 C17 1.362(3) . ? C15 C16 1.494(3) . ? C17 C18 1.403(3) . ? C17 H17 0.9300 . ? C18 C19 1.419(4) . ? C18 C23 1.428(3) . ? C19 C20 1.350(4) . ? C19 H19 0.9300 . ? C20 C21 1.397(4) . ? C20 H20 0.9300 . ? C21 C22 1.358(4) . ? C21 H21 0.9300 . ? C22 C23 1.417(3) . ? C22 H22 0.9300 . ? C24 C25 1.368(4) . ? C24 H24 0.9300 . ? C25 C26 1.366(4) . ? C25 H25 0.9300 . ? C26 C27 1.375(4) . ? C26 H26 0.9300 . ? C27 C28 1.387(4) . ? C27 H27 0.9300 . ? C28 C29 1.490(4) . ? C29 C30 1.393(4) . ? C30 C31 1.359(4) . ? C30 H30 0.9300 . ? C31 C32 1.371(5) . ? C31 H31 0.9300 . ? C32 C33 1.384(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 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 O6 Cd1 O7 98.50(8) 4_566 . ? O6 Cd1 N1 99.34(7) 4_566 . ? O7 Cd1 N1 134.96(8) . . ? O6 Cd1 N2 168.86(7) 4_566 . ? O7 Cd1 N2 85.89(8) . . ? N1 Cd1 N2 70.69(7) . . ? O6 Cd1 O2 98.46(7) 4_566 . ? O7 Cd1 O2 133.29(7) . . ? N1 Cd1 O2 83.95(7) . . ? N2 Cd1 O2 85.66(7) . . ? O6 Cd1 O1 98.50(7) 4_566 . ? O7 Cd1 O1 80.94(7) . . ? N1 Cd1 O1 135.89(7) . . ? N2 Cd1 O1 92.28(7) . . ? O2 Cd1 O1 53.65(6) . . ? C1 O1 Cd1 91.89(16) . . ? C1 O2 Cd1 92.92(15) . . ? C3 O3 H3 109.5 . . ? C14 O4 H4 109.5 . . ? C16 O6 Cd1 103.81(17) . 4_665 ? C34 O7 Cd1 119.9(2) . . ? C24 N1 C28 118.3(2) . . ? C24 N1 Cd1 123.79(18) . . ? C28 N1 Cd1 117.89(17) . . ? C33 N2 C29 118.2(2) . . ? C33 N2 Cd1 124.1(2) . . ? C29 N2 Cd1 117.18(16) . . ? C34 N3 C35 117.0(4) . . ? C34 N3 C36 126.0(4) . . ? C35 N3 C36 115.4(4) . . ? O1 C1 O2 120.8(2) . . ? O1 C1 C2 120.4(2) . . ? O2 C1 C2 118.8(2) . . ? C11 C2 C3 118.7(2) . . ? C11 C2 C1 120.9(2) . . ? C3 C2 C1 120.2(2) . . ? O3 C3 C4 118.4(2) . . ? O3 C3 C2 120.1(2) . . ? C4 C3 C2 121.5(2) . . ? C3 C4 C5 119.1(2) . . ? C3 C4 C12 119.0(2) . . ? C5 C4 C12 121.8(2) . . ? C4 C5 C6 122.9(2) . . ? C4 C5 C10 119.4(2) . . ? C6 C5 C10 117.7(2) . . ? C7 C6 C5 120.3(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 121.7(3) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 120.0(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.8(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 121.5(3) . . ? C11 C10 C5 119.0(2) . . ? C9 C10 C5 119.5(3) . . ? C2 C11 C10 122.1(2) . . ? C2 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C13 C12 C4 115.36(19) . . ? C13 C12 H12A 108.4 . . ? C4 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? C4 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C23 118.8(2) . . ? C14 C13 C12 119.8(2) . . ? C23 C13 C12 121.4(2) . . ? O4 C14 C13 118.7(2) . . ? O4 C14 C15 119.5(2) . . ? C13 C14 C15 121.8(2) . . ? C17 C15 C14 118.9(2) . . ? C17 C15 C16 120.1(2) . . ? C14 C15 C16 120.9(2) . . ? O6 C16 O5 121.5(2) . . ? O6 C16 C15 119.4(2) . . ? O5 C16 C15 119.1(2) . . ? C15 C17 C18 121.9(2) . . ? C15 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 122.1(2) . . ? C17 C18 C23 119.0(2) . . ? C19 C18 C23 118.9(2) . . ? C20 C19 C18 121.7(3) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 119.3(3) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 121.4(3) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 121.2(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C13 123.1(2) . . ? C22 C23 C18 117.4(2) . . ? C13 C23 C18 119.5(2) . . ? N1 C24 C25 123.3(3) . . ? N1 C24 H24 118.3 . . ? C25 C24 H24 118.3 . . ? C26 C25 C24 118.5(3) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 119.4(3) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 119.3(3) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? N1 C28 C27 121.2(2) . . ? N1 C28 C29 116.6(2) . . ? C27 C28 C29 122.2(2) . . ? N2 C29 C30 121.5(3) . . ? N2 C29 C28 116.9(2) . . ? C30 C29 C28 121.6(3) . . ? C31 C30 C29 119.3(3) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 120.0(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 118.0(3) . . ? C31 C32 H32 121.0 . . ? C33 C32 H32 121.0 . . ? N2 C33 C32 123.0(3) . . ? N2 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? O7 C34 N3 130.7(4) . . ? O7 C34 H34 114.7 . . ? N3 C34 H34 114.7 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Cd1 O1 C1 99.16(16) 4_566 . . . ? O7 Cd1 O1 C1 -163.52(17) . . . . ? N1 Cd1 O1 C1 -13.8(2) . . . . ? N2 Cd1 O1 C1 -78.05(16) . . . . ? O2 Cd1 O1 C1 4.87(15) . . . . ? O6 Cd1 O2 C1 -99.17(15) 4_566 . . . ? O7 Cd1 O2 C1 11.0(2) . . . . ? N1 Cd1 O2 C1 162.25(16) . . . . ? N2 Cd1 O2 C1 91.23(16) . . . . ? O1 Cd1 O2 C1 -4.81(14) . . . . ? O6 Cd1 O7 C34 19.5(3) 4_566 . . . ? N1 Cd1 O7 C34 131.9(3) . . . . ? N2 Cd1 O7 C34 -170.8(3) . . . . ? O2 Cd1 O7 C34 -90.7(3) . . . . ? O1 Cd1 O7 C34 -77.8(3) . . . . ? O6 Cd1 N1 C24 -1.2(2) 4_566 . . . ? O7 Cd1 N1 C24 -113.3(2) . . . . ? N2 Cd1 N1 C24 -176.1(2) . . . . ? O2 Cd1 N1 C24 96.4(2) . . . . ? O1 Cd1 N1 C24 111.4(2) . . . . ? O6 Cd1 N1 C28 175.82(17) 4_566 . . . ? O7 Cd1 N1 C28 63.7(2) . . . . ? N2 Cd1 N1 C28 0.95(17) . . . . ? O2 Cd1 N1 C28 -86.56(17) . . . . ? O1 Cd1 N1 C28 -71.5(2) . . . . ? O6 Cd1 N2 C33 155.1(3) 4_566 . . . ? O7 Cd1 N2 C33 41.4(2) . . . . ? N1 Cd1 N2 C33 -177.7(3) . . . . ? O2 Cd1 N2 C33 -92.6(2) . . . . ? O1 Cd1 N2 C33 -39.3(2) . . . . ? O6 Cd1 N2 C29 -33.1(5) 4_566 . . . ? O7 Cd1 N2 C29 -146.77(19) . . . . ? N1 Cd1 N2 C29 -5.88(17) . . . . ? O2 Cd1 N2 C29 79.21(18) . . . . ? O1 Cd1 N2 C29 132.49(18) . . . . ? Cd1 O1 C1 O2 -8.7(3) . . . . ? Cd1 O1 C1 C2 170.5(2) . . . . ? Cd1 O2 C1 O1 8.8(3) . . . . ? Cd1 O2 C1 C2 -170.4(2) . . . . ? O1 C1 C2 C11 3.2(4) . . . . ? O2 C1 C2 C11 -177.6(3) . . . . ? O1 C1 C2 C3 -173.2(2) . . . . ? O2 C1 C2 C3 6.0(4) . . . . ? C11 C2 C3 O3 179.3(2) . . . . ? C1 C2 C3 O3 -4.2(4) . . . . ? C11 C2 C3 C4 -2.1(4) . . . . ? C1 C2 C3 C4 174.4(2) . . . . ? O3 C3 C4 C5 -177.0(2) . . . . ? C2 C3 C4 C5 4.5(4) . . . . ? O3 C3 C4 C12 3.6(3) . . . . ? C2 C3 C4 C12 -174.9(2) . . . . ? C3 C4 C5 C6 176.4(3) . . . . ? C12 C4 C5 C6 -4.2(4) . . . . ? C3 C4 C5 C10 -3.7(4) . . . . ? C12 C4 C5 C10 175.7(2) . . . . ? C4 C5 C6 C7 177.1(3) . . . . ? C10 C5 C6 C7 -2.8(5) . . . . ? C5 C6 C7 C8 1.5(6) . . . . ? C6 C7 C8 C9 0.1(7) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C8 C9 C10 C11 -179.0(4) . . . . ? C8 C9 C10 C5 -1.1(6) . . . . ? C4 C5 C10 C11 0.7(4) . . . . ? C6 C5 C10 C11 -179.5(3) . . . . ? C4 C5 C10 C9 -177.3(3) . . . . ? C6 C5 C10 C9 2.6(5) . . . . ? C3 C2 C11 C10 -1.0(4) . . . . ? C1 C2 C11 C10 -177.5(3) . . . . ? C9 C10 C11 C2 179.6(3) . . . . ? C5 C10 C11 C2 1.7(5) . . . . ? C3 C4 C12 C13 117.9(2) . . . . ? C5 C4 C12 C13 -61.5(3) . . . . ? C4 C12 C13 C14 122.1(2) . . . . ? C4 C12 C13 C23 -59.1(3) . . . . ? C23 C13 C14 O4 -178.5(2) . . . . ? C12 C13 C14 O4 0.4(3) . . . . ? C23 C13 C14 C15 2.7(3) . . . . ? C12 C13 C14 C15 -178.4(2) . . . . ? O4 C14 C15 C17 -179.5(2) . . . . ? C13 C14 C15 C17 -0.7(4) . . . . ? O4 C14 C15 C16 0.5(3) . . . . ? C13 C14 C15 C16 179.3(2) . . . . ? Cd1 O6 C16 O5 -1.5(3) 4_665 . . . ? Cd1 O6 C16 C15 177.02(17) 4_665 . . . ? C17 C15 C16 O6 6.0(4) . . . . ? C14 C15 C16 O6 -173.9(2) . . . . ? C17 C15 C16 O5 -175.4(2) . . . . ? C14 C15 C16 O5 4.6(3) . . . . ? C14 C15 C17 C18 -0.3(4) . . . . ? C16 C15 C17 C18 179.7(2) . . . . ? C15 C17 C18 C19 179.9(3) . . . . ? C15 C17 C18 C23 -0.8(4) . . . . ? C17 C18 C19 C20 178.1(3) . . . . ? C23 C18 C19 C20 -1.2(5) . . . . ? C18 C19 C20 C21 -1.5(5) . . . . ? C19 C20 C21 C22 2.0(5) . . . . ? C20 C21 C22 C23 0.3(5) . . . . ? C21 C22 C23 C13 178.2(3) . . . . ? C21 C22 C23 C18 -3.0(4) . . . . ? C14 C13 C23 C22 174.9(2) . . . . ? C12 C13 C23 C22 -3.9(4) . . . . ? C14 C13 C23 C18 -3.8(3) . . . . ? C12 C13 C23 C18 177.3(2) . . . . ? C17 C18 C23 C22 -175.9(2) . . . . ? C19 C18 C23 C22 3.4(4) . . . . ? C17 C18 C23 C13 2.9(4) . . . . ? C19 C18 C23 C13 -177.8(2) . . . . ? C28 N1 C24 C25 0.1(4) . . . . ? Cd1 N1 C24 C25 177.1(2) . . . . ? N1 C24 C25 C26 -2.0(5) . . . . ? C24 C25 C26 C27 2.0(4) . . . . ? C25 C26 C27 C28 -0.1(4) . . . . ? C24 N1 C28 C27 1.9(4) . . . . ? Cd1 N1 C28 C27 -175.31(18) . . . . ? C24 N1 C28 C29 -179.2(2) . . . . ? Cd1 N1 C28 C29 3.6(3) . . . . ? C26 C27 C28 N1 -1.9(4) . . . . ? C26 C27 C28 C29 179.3(2) . . . . ? C33 N2 C29 C30 1.7(4) . . . . ? Cd1 N2 C29 C30 -170.6(2) . . . . ? C33 N2 C29 C28 -177.9(2) . . . . ? Cd1 N2 C29 C28 9.8(3) . . . . ? N1 C28 C29 N2 -9.0(3) . . . . ? C27 C28 C29 N2 169.9(2) . . . . ? N1 C28 C29 C30 171.5(2) . . . . ? C27 C28 C29 C30 -9.6(4) . . . . ? N2 C29 C30 C31 -1.1(4) . . . . ? C28 C29 C30 C31 178.4(3) . . . . ? C29 C30 C31 C32 -0.7(5) . . . . ? C30 C31 C32 C33 1.8(5) . . . . ? C29 N2 C33 C32 -0.5(5) . . . . ? Cd1 N2 C33 C32 171.2(2) . . . . ? C31 C32 C33 N2 -1.2(5) . . . . ? Cd1 O7 C34 N3 171.3(4) . . . . ? C35 N3 C34 O7 -14.5(8) . . . . ? C36 N3 C34 O7 -179.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.442 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.052 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 631546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H36 Mn N4 O9' _chemical_formula_weight 855.74 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.649(2) _cell_length_b 22.963(4) _cell_length_c 11.545(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.7380(10) _cell_angle_gamma 90.00 _cell_volume 3737.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2448 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 24.74 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.773218 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10048 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3293 _reflns_number_gt 2605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0353P)^2^+1.9332P] 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 3293 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Mn1 Mn 0.5000 0.604088(19) 0.7500 0.03333(13) Uani 1 2 d S . . O1 O 0.40573(9) 0.44913(7) 0.52160(12) 0.0444(4) Uani 1 1 d . . . O2 O 0.33372(9) 0.39308(7) 0.60847(12) 0.0489(4) Uani 1 1 d . . . O3 O 0.17335(8) 0.35095(6) 0.47459(12) 0.0377(3) Uani 1 1 d . . . H3 H 0.2234 0.3579 0.5376 0.057 Uiso 1 1 calc R . . O4 O 0.53218(9) 0.53292(6) 0.65608(12) 0.0428(4) Uani 1 1 d . . . H4A H 0.4895 0.5068 0.6338 0.064 Uiso 1 1 d R . . H4B H 0.5474 0.5456 0.5984 0.064 Uiso 1 1 d R . . N1 N 0.59128(10) 0.66593(7) 0.69937(14) 0.0352(4) Uani 1 1 d . . . N2 N 0.63629(11) 0.62219(7) 0.93645(14) 0.0386(4) Uani 1 1 d . . . C1 C 0.65766(15) 0.60182(10) 1.05375(18) 0.0468(5) Uani 1 1 d . . . H1 H 0.6134 0.5785 1.0654 0.056 Uiso 1 1 calc R . . C2 C 0.74306(16) 0.61372(10) 1.16002(19) 0.0511(6) Uani 1 1 d . . . H2 H 0.7549 0.5989 1.2406 0.061 Uiso 1 1 calc R . . C3 C 0.80883(15) 0.64734(10) 1.14421(19) 0.0471(5) Uani 1 1 d . . . H3A H 0.8664 0.6553 1.2141 0.057 Uiso 1 1 calc R . . C4 C 0.78995(13) 0.66997(9) 1.02316(18) 0.0384(5) Uani 1 1 d . . . C5 C 0.85474(14) 0.70556(9) 0.9984(2) 0.0450(5) Uani 1 1 d . . . H5 H 0.9134 0.7142 1.0656 0.054 Uiso 1 1 calc R . . C6 C 0.83340(14) 0.72702(9) 0.8807(2) 0.0452(5) Uani 1 1 d . . . H6 H 0.8774 0.7499 0.8675 0.054 Uiso 1 1 calc R . . C7 C 0.74337(13) 0.71485(8) 0.77554(19) 0.0369(5) Uani 1 1 d . . . C8 C 0.71636(15) 0.73747(9) 0.6518(2) 0.0459(5) Uani 1 1 d . . . H8 H 0.7574 0.7616 0.6352 0.055 Uiso 1 1 calc R . . C9 C 0.62988(15) 0.72397(9) 0.5561(2) 0.0471(5) Uani 1 1 d . . . H9 H 0.6112 0.7387 0.4736 0.056 Uiso 1 1 calc R . . C10 C 0.56964(14) 0.68767(9) 0.58395(18) 0.0411(5) Uani 1 1 d . . . H10 H 0.5110 0.6783 0.5176 0.049 Uiso 1 1 calc R . . C11 C 0.67814(12) 0.67948(8) 0.79576(17) 0.0323(4) Uani 1 1 d . . . C12 C 0.70149(13) 0.65628(8) 0.92125(17) 0.0338(4) Uani 1 1 d . . . C13 C 0.33536(12) 0.42075(9) 0.51508(17) 0.0330(4) Uani 1 1 d . . . C14 C 0.24792(11) 0.41870(8) 0.38860(16) 0.0276(4) Uani 1 1 d . . . C15 C 0.16747(12) 0.38416(8) 0.37364(16) 0.0279(4) Uani 1 1 d . . . C16 C 0.08544(11) 0.38276(7) 0.25969(16) 0.0266(4) Uani 1 1 d . . . C17 C 0.0000 0.34749(11) 0.2500 0.0300(6) Uani 1 2 d S . . H17A H 0.0201 0.3225 0.3250 0.036 Uiso 0.50 1 calc PR . . H17B H -0.0201 0.3225 0.1750 0.036 Uiso 0.50 1 calc PR . . C18 C 0.08558(11) 0.41266(8) 0.15101(16) 0.0268(4) Uani 1 1 d . . . C19 C 0.01032(13) 0.40869(8) 0.02565(17) 0.0339(4) Uani 1 1 d . . . H19 H -0.0431 0.3867 0.0124 0.041 Uiso 1 1 calc R . . C20 C 0.01483(13) 0.43653(9) -0.07593(17) 0.0384(5) Uani 1 1 d . . . H20 H -0.0355 0.4329 -0.1571 0.046 Uiso 1 1 calc R . . C21 C 0.09310(14) 0.47041(9) -0.06125(17) 0.0388(5) Uani 1 1 d . . . H21 H 0.0946 0.4895 -0.1315 0.047 Uiso 1 1 calc R . . C22 C 0.16692(13) 0.47506(8) 0.05714(17) 0.0352(4) Uani 1 1 d . . . H22 H 0.2193 0.4975 0.0676 0.042 Uiso 1 1 calc R . . C23 C 0.16563(12) 0.44639(8) 0.16499(16) 0.0290(4) Uani 1 1 d . . . C24 C 0.24382(12) 0.44951(8) 0.28573(16) 0.0302(4) Uani 1 1 d . . . H24 H 0.2945 0.4734 0.2958 0.036 Uiso 1 1 calc R . . O5 O 0.5000 0.32592(13) 0.7500 0.1251(14) Uani 1 2 d S . . H5' H 0.4511 0.3466 0.7411 0.188 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0330(2) 0.0390(3) 0.0300(2) 0.000 0.01552(18) 0.000 O1 0.0320(7) 0.0657(10) 0.0343(7) -0.0070(7) 0.0132(6) -0.0158(7) O2 0.0348(7) 0.0778(11) 0.0303(7) 0.0117(7) 0.0105(6) -0.0065(7) O3 0.0290(7) 0.0480(9) 0.0329(7) 0.0137(6) 0.0106(6) -0.0006(6) O4 0.0416(7) 0.0497(9) 0.0467(8) -0.0116(7) 0.0282(7) -0.0118(7) N1 0.0369(9) 0.0370(9) 0.0323(9) 0.0017(7) 0.0157(7) 0.0027(7) N2 0.0435(9) 0.0421(10) 0.0322(9) 0.0012(7) 0.0183(7) 0.0015(8) C1 0.0541(13) 0.0541(14) 0.0334(11) 0.0035(10) 0.0200(10) -0.0005(11) C2 0.0624(14) 0.0564(15) 0.0305(11) 0.0012(10) 0.0164(10) 0.0104(12) C3 0.0450(12) 0.0489(14) 0.0366(12) -0.0061(10) 0.0076(10) 0.0091(11) C4 0.0374(11) 0.0365(11) 0.0382(11) -0.0072(9) 0.0133(9) 0.0081(9) C5 0.0348(11) 0.0413(13) 0.0507(13) -0.0107(10) 0.0107(10) 0.0009(10) C6 0.0379(11) 0.0372(12) 0.0618(14) -0.0067(11) 0.0228(10) -0.0030(9) C7 0.0396(11) 0.0288(11) 0.0461(12) -0.0014(9) 0.0223(9) 0.0028(9) C8 0.0529(13) 0.0359(12) 0.0592(14) 0.0075(10) 0.0341(12) 0.0009(10) C9 0.0565(14) 0.0444(13) 0.0448(12) 0.0133(10) 0.0263(11) 0.0051(11) C10 0.0430(11) 0.0428(12) 0.0347(11) 0.0060(9) 0.0143(9) 0.0047(10) C11 0.0358(10) 0.0274(10) 0.0348(10) -0.0028(8) 0.0162(9) 0.0050(8) C12 0.0361(10) 0.0314(11) 0.0351(10) -0.0037(8) 0.0165(9) 0.0047(8) C13 0.0275(10) 0.0444(12) 0.0281(10) -0.0033(9) 0.0130(8) 0.0016(9) C14 0.0252(9) 0.0304(10) 0.0290(9) -0.0014(8) 0.0135(8) 0.0021(8) C15 0.0274(9) 0.0301(10) 0.0295(9) 0.0033(8) 0.0154(7) 0.0042(8) C16 0.0243(9) 0.0259(10) 0.0319(9) -0.0008(8) 0.0143(7) 0.0017(7) C17 0.0267(13) 0.0305(15) 0.0335(14) 0.000 0.0138(11) 0.000 C18 0.0253(9) 0.0283(10) 0.0289(9) -0.0022(7) 0.0136(8) 0.0040(7) C19 0.0292(9) 0.0388(12) 0.0327(10) -0.0015(8) 0.0125(8) 0.0013(8) C20 0.0388(11) 0.0450(12) 0.0276(10) -0.0003(9) 0.0109(8) 0.0050(9) C21 0.0494(12) 0.0405(12) 0.0298(10) 0.0059(9) 0.0202(9) 0.0065(10) C22 0.0378(10) 0.0352(11) 0.0363(11) 0.0032(9) 0.0196(9) -0.0018(9) C23 0.0294(9) 0.0302(10) 0.0305(10) 0.0007(8) 0.0158(8) 0.0034(8) C24 0.0265(9) 0.0316(10) 0.0353(10) -0.0018(8) 0.0161(8) -0.0018(8) O5 0.105(2) 0.074(2) 0.106(2) 0.000 -0.0383(19) 0.000 _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 Mn1 O4 2.1387(14) 2_656 ? Mn1 O4 2.1387(13) . ? Mn1 N1 2.2637(16) . ? Mn1 N1 2.2637(16) 2_656 ? Mn1 N2 2.3168(16) . ? Mn1 N2 2.3168(16) 2_656 ? O1 C13 1.253(2) . ? O2 C13 1.261(2) . ? O3 C15 1.362(2) . ? O3 H3 0.8200 . ? O4 H4A 0.8501 . ? O4 H4B 0.8502 . ? N1 C10 1.322(2) . ? N1 C11 1.367(2) . ? N2 C1 1.331(2) . ? N2 C12 1.356(2) . ? C1 C2 1.394(3) . ? C1 H1 0.9300 . ? C2 C3 1.361(3) . ? C2 H2 0.9300 . ? C3 C4 1.397(3) . ? C3 H3A 0.9300 . ? C4 C12 1.409(3) . ? C4 C5 1.424(3) . ? C5 C6 1.344(3) . ? C5 H5 0.9300 . ? C6 C7 1.432(3) . ? C6 H6 0.9300 . ? C7 C11 1.401(3) . ? C7 C8 1.402(3) . ? C8 C9 1.360(3) . ? C8 H8 0.9300 . ? C9 C10 1.396(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.434(3) . ? C13 C14 1.507(2) . ? C14 C24 1.360(2) . ? C14 C15 1.434(2) . ? C15 C16 1.383(2) . ? C16 C18 1.431(2) . ? C16 C17 1.525(2) . ? C17 C16 1.525(2) 2 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.418(2) . ? C18 C23 1.421(2) . ? C19 C20 1.364(3) . ? C19 H19 0.9300 . ? C20 C21 1.398(3) . ? C20 H20 0.9300 . ? C21 C22 1.357(3) . ? C21 H21 0.9300 . ? C22 C23 1.416(2) . ? C22 H22 0.9300 . ? C23 C24 1.401(2) . ? C24 H24 0.9300 . ? O5 H5' 0.8680 . ? 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 O4 Mn1 O4 80.35(7) 2_656 . ? O4 Mn1 N1 157.55(5) 2_656 . ? O4 Mn1 N1 91.98(5) . . ? O4 Mn1 N1 91.98(5) 2_656 2_656 ? O4 Mn1 N1 157.55(5) . 2_656 ? N1 Mn1 N1 102.29(8) . 2_656 ? O4 Mn1 N2 89.46(6) 2_656 . ? O4 Mn1 N2 106.48(5) . . ? N1 Mn1 N2 72.41(6) . . ? N1 Mn1 N2 94.42(6) 2_656 . ? O4 Mn1 N2 106.48(5) 2_656 2_656 ? O4 Mn1 N2 89.46(6) . 2_656 ? N1 Mn1 N2 94.42(6) . 2_656 ? N1 Mn1 N2 72.41(6) 2_656 2_656 ? N2 Mn1 N2 159.32(9) . 2_656 ? C15 O3 H3 109.5 . . ? Mn1 O4 H4A 111.5 . . ? Mn1 O4 H4B 110.1 . . ? H4A O4 H4B 117.1 . . ? C10 N1 C11 117.62(17) . . ? C10 N1 Mn1 125.66(13) . . ? C11 N1 Mn1 116.64(12) . . ? C1 N2 C12 117.63(17) . . ? C1 N2 Mn1 127.26(14) . . ? C12 N2 Mn1 115.09(12) . . ? N2 C1 C2 123.2(2) . . ? N2 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.0(2) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.10(19) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C12 117.17(19) . . ? C3 C4 C5 123.65(19) . . ? C12 C4 C5 119.18(18) . . ? C6 C5 C4 121.80(19) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 120.45(19) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C11 C7 C8 117.74(18) . . ? C11 C7 C6 119.42(18) . . ? C8 C7 C6 122.83(19) . . ? C9 C8 C7 119.78(19) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 118.84(19) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N1 C10 C9 123.65(19) . . ? N1 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N1 C11 C7 122.35(17) . . ? N1 C11 C12 117.70(17) . . ? C7 C11 C12 119.95(17) . . ? N2 C12 C4 122.84(18) . . ? N2 C12 C11 117.97(16) . . ? C4 C12 C11 119.18(18) . . ? O1 C13 O2 123.65(16) . . ? O1 C13 C14 118.61(16) . . ? O2 C13 C14 117.74(16) . . ? C24 C14 C15 118.47(15) . . ? C24 C14 C13 120.57(16) . . ? C15 C14 C13 120.96(15) . . ? O3 C15 C16 119.39(15) . . ? O3 C15 C14 118.50(15) . . ? C16 C15 C14 122.10(15) . . ? C15 C16 C18 117.94(15) . . ? C15 C16 C17 120.28(14) . . ? C18 C16 C17 121.70(13) . . ? C16 C17 C16 115.9(2) . 2 ? C16 C17 H17A 108.3 . . ? C16 C17 H17A 108.3 2 . ? C16 C17 H17B 108.3 . . ? C16 C17 H17B 108.3 2 . ? H17A C17 H17B 107.4 . . ? C19 C18 C23 116.85(16) . . ? C19 C18 C16 123.18(16) . . ? C23 C18 C16 119.92(15) . . ? C20 C19 C18 121.15(17) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 121.76(17) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C22 C21 C20 118.92(17) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 121.19(18) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C24 C23 C22 120.73(16) . . ? C24 C23 C18 119.12(16) . . ? C22 C23 C18 120.12(16) . . ? C14 C24 C23 122.13(16) . . ? C14 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Mn1 N1 C10 142.78(16) 2_656 . . . ? O4 Mn1 N1 C10 73.62(16) . . . . ? N1 Mn1 N1 C10 -88.93(16) 2_656 . . . ? N2 Mn1 N1 C10 -179.71(17) . . . . ? N2 Mn1 N1 C10 -15.99(16) 2_656 . . . ? O4 Mn1 N1 C11 -33.9(2) 2_656 . . . ? O4 Mn1 N1 C11 -103.02(13) . . . . ? N1 Mn1 N1 C11 94.43(13) 2_656 . . . ? N2 Mn1 N1 C11 3.65(12) . . . . ? N2 Mn1 N1 C11 167.37(13) 2_656 . . . ? O4 Mn1 N2 C1 -15.12(17) 2_656 . . . ? O4 Mn1 N2 C1 -94.89(17) . . . . ? N1 Mn1 N2 C1 178.33(18) . . . . ? N1 Mn1 N2 C1 76.82(17) 2_656 . . . ? N2 Mn1 N2 C1 126.00(17) 2_656 . . . ? O4 Mn1 N2 C12 163.09(13) 2_656 . . . ? O4 Mn1 N2 C12 83.33(13) . . . . ? N1 Mn1 N2 C12 -3.46(12) . . . . ? N1 Mn1 N2 C12 -104.97(13) 2_656 . . . ? N2 Mn1 N2 C12 -55.79(12) 2_656 . . . ? C12 N2 C1 C2 -0.2(3) . . . . ? Mn1 N2 C1 C2 178.01(16) . . . . ? N2 C1 C2 C3 -0.6(3) . . . . ? C1 C2 C3 C4 0.8(3) . . . . ? C2 C3 C4 C12 -0.1(3) . . . . ? C2 C3 C4 C5 179.88(19) . . . . ? C3 C4 C5 C6 -179.2(2) . . . . ? C12 C4 C5 C6 0.8(3) . . . . ? C4 C5 C6 C7 0.4(3) . . . . ? C5 C6 C7 C11 -1.1(3) . . . . ? C5 C6 C7 C8 178.10(19) . . . . ? C11 C7 C8 C9 -1.0(3) . . . . ? C6 C7 C8 C9 179.75(19) . . . . ? C7 C8 C9 C10 0.1(3) . . . . ? C11 N1 C10 C9 -0.8(3) . . . . ? Mn1 N1 C10 C9 -177.43(14) . . . . ? C8 C9 C10 N1 0.9(3) . . . . ? C10 N1 C11 C7 -0.2(3) . . . . ? Mn1 N1 C11 C7 176.70(13) . . . . ? C10 N1 C11 C12 179.57(17) . . . . ? Mn1 N1 C11 C12 -3.5(2) . . . . ? C8 C7 C11 N1 1.1(3) . . . . ? C6 C7 C11 N1 -179.63(17) . . . . ? C8 C7 C11 C12 -178.65(17) . . . . ? C6 C7 C11 C12 0.6(3) . . . . ? C1 N2 C12 C4 0.9(3) . . . . ? Mn1 N2 C12 C4 -177.54(14) . . . . ? C1 N2 C12 C11 -178.63(17) . . . . ? Mn1 N2 C12 C11 3.0(2) . . . . ? C3 C4 C12 N2 -0.7(3) . . . . ? C5 C4 C12 N2 179.28(17) . . . . ? C3 C4 C12 C11 178.76(17) . . . . ? C5 C4 C12 C11 -1.2(3) . . . . ? N1 C11 C12 N2 0.3(3) . . . . ? C7 C11 C12 N2 -179.93(16) . . . . ? N1 C11 C12 C4 -179.22(16) . . . . ? C7 C11 C12 C4 0.6(3) . . . . ? O1 C13 C14 C24 -3.4(3) . . . . ? O2 C13 C14 C24 177.33(17) . . . . ? O1 C13 C14 C15 176.32(16) . . . . ? O2 C13 C14 C15 -2.9(3) . . . . ? C24 C14 C15 O3 176.67(16) . . . . ? C13 C14 C15 O3 -3.1(2) . . . . ? C24 C14 C15 C16 -2.0(3) . . . . ? C13 C14 C15 C16 178.22(16) . . . . ? O3 C15 C16 C18 -172.76(15) . . . . ? C14 C15 C16 C18 5.9(2) . . . . ? O3 C15 C16 C17 4.0(2) . . . . ? C14 C15 C16 C17 -177.28(16) . . . . ? C15 C16 C17 C16 109.51(16) . . . 2 ? C18 C16 C17 C16 -73.83(15) . . . 2 ? C15 C16 C18 C19 172.24(16) . . . . ? C17 C16 C18 C19 -4.5(3) . . . . ? C15 C16 C18 C23 -5.0(2) . . . . ? C17 C16 C18 C23 178.23(16) . . . . ? C23 C18 C19 C20 -0.6(3) . . . . ? C16 C18 C19 C20 -177.93(17) . . . . ? C18 C19 C20 C21 -0.4(3) . . . . ? C19 C20 C21 C22 0.8(3) . . . . ? C20 C21 C22 C23 -0.1(3) . . . . ? C21 C22 C23 C24 177.35(18) . . . . ? C21 C22 C23 C18 -0.9(3) . . . . ? C19 C18 C23 C24 -177.07(16) . . . . ? C16 C18 C23 C24 0.4(2) . . . . ? C19 C18 C23 C22 1.2(2) . . . . ? C16 C18 C23 C22 178.67(16) . . . . ? C15 C14 C24 C23 -3.0(3) . . . . ? C13 C14 C24 C23 176.77(16) . . . . ? C22 C23 C24 C14 -174.54(17) . . . . ? C18 C23 C24 C14 3.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.211 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.038 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 631547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H38 Cu N4 O9' _chemical_formula_weight 794.29 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.080(7) _cell_length_b 10.678(5) _cell_length_c 22.186(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.950(7) _cell_angle_gamma 90.00 _cell_volume 3727(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2187 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 20.32 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.806107 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 19855 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6557 _reflns_number_gt 3814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0973P)^2^+0.8936P] 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 6557 _refine_ls_number_parameters 502 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1983 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.67595(4) -0.23095(5) 0.99816(3) 0.0460(2) Uani 1 1 d . . . O1 O 0.7941(2) -0.0786(3) 0.90224(16) 0.0583(9) Uani 1 1 d . . . O2 O 0.6645(2) -0.0867(3) 0.92286(15) 0.0499(8) Uani 1 1 d . . . O3 O 0.8257(2) 0.0740(4) 0.82112(17) 0.0610(10) Uani 1 1 d . . . H3 H 0.8344 0.0193 0.8476 0.092 Uiso 1 1 calc R . . O4 O 0.7253(3) 0.3947(3) 0.61836(15) 0.0662(11) Uani 1 1 d . . . H4 H 0.7126 0.4459 0.5904 0.099 Uiso 1 1 calc R . . O5 O 0.7033(2) 0.6062(3) 0.56477(16) 0.0584(9) Uani 1 1 d . . . O6 O 0.7215(2) 0.7814(3) 0.61971(17) 0.0629(10) Uani 1 1 d . . . O7 O 0.7955(2) -0.2515(3) 0.99018(15) 0.0533(9) Uani 1 1 d D . . H7A H 0.7923 -0.1862 0.9675 0.080 Uiso 1 1 d RD . . H7B H 0.8254 -0.2444 1.0267 0.080 Uiso 1 1 d RD . . N1 N 0.5514(3) -0.2314(3) 1.00073(17) 0.0449(10) Uani 1 1 d . . . N2 N 0.6397(3) -0.3841(3) 0.94579(18) 0.0462(10) Uani 1 1 d . . . C1 C 0.5083(4) -0.1515(5) 1.0289(2) 0.0593(14) Uani 1 1 d . . . H1 H 0.5376 -0.0875 1.0527 0.071 Uiso 1 1 calc R . . C2 C 0.4209(4) -0.1610(6) 1.0237(3) 0.0672(16) Uani 1 1 d . . . H2 H 0.3927 -0.1032 1.0436 0.081 Uiso 1 1 calc R . . C3 C 0.3764(4) -0.2543(6) 0.9898(3) 0.0633(16) Uani 1 1 d . . . H3A H 0.3180 -0.2610 0.9867 0.076 Uiso 1 1 calc R . . C4 C 0.4195(3) -0.3407(5) 0.9592(2) 0.0509(13) Uani 1 1 d . . . C5 C 0.3803(4) -0.4411(5) 0.9207(3) 0.0626(15) Uani 1 1 d . . . H5 H 0.3222 -0.4545 0.9160 0.075 Uiso 1 1 calc R . . C6 C 0.4255(4) -0.5158(5) 0.8914(3) 0.0620(15) Uani 1 1 d . . . H6 H 0.3980 -0.5794 0.8663 0.074 Uiso 1 1 calc R . . C7 C 0.5140(3) -0.5005(4) 0.8977(2) 0.0484(12) Uani 1 1 d . . . C8 C 0.5644(4) -0.5750(5) 0.8684(3) 0.0649(16) Uani 1 1 d . . . H8 H 0.5395 -0.6380 0.8418 0.078 Uiso 1 1 calc R . . C9 C 0.6488(5) -0.5568(5) 0.8783(3) 0.0742(18) Uani 1 1 d . . . H9 H 0.6825 -0.6074 0.8590 0.089 Uiso 1 1 calc R . . C10 C 0.6853(4) -0.4610(5) 0.9179(3) 0.0619(15) Uani 1 1 d . . . H10 H 0.7440 -0.4502 0.9251 0.074 Uiso 1 1 calc R . . C11 C 0.5550(3) -0.4057(4) 0.9358(2) 0.0438(12) Uani 1 1 d . . . C12 C 0.5075(3) -0.3240(4) 0.9665(2) 0.0427(11) Uani 1 1 d . . . C13 C 0.7172(3) -0.0465(4) 0.8930(2) 0.0450(12) Uani 1 1 d . . . C14 C 0.6858(3) 0.0442(4) 0.8417(2) 0.0447(12) Uani 1 1 d . . . C15 C 0.7410(3) 0.1013(4) 0.8067(2) 0.0473(12) Uani 1 1 d . . . C16 C 0.7107(3) 0.1832(4) 0.7593(2) 0.0459(12) Uani 1 1 d . . . C17 C 0.6219(3) 0.2048(4) 0.7419(2) 0.0478(12) Uani 1 1 d . . . C18 C 0.5832(4) 0.2773(4) 0.6908(2) 0.0523(13) Uani 1 1 d . . . H18 H 0.6172 0.3157 0.6669 0.063 Uiso 1 1 calc R . . C19 C 0.4978(4) 0.2926(5) 0.6753(3) 0.0632(16) Uani 1 1 d . . . H19 H 0.4746 0.3404 0.6409 0.076 Uiso 1 1 calc R . . C20 C 0.4439(4) 0.2388(5) 0.7095(3) 0.0655(16) Uani 1 1 d . . . H20 H 0.3856 0.2520 0.6986 0.079 Uiso 1 1 calc R . . C21 C 0.4773(3) 0.1668(5) 0.7590(3) 0.0599(14) Uani 1 1 d . . . H21 H 0.4415 0.1295 0.7818 0.072 Uiso 1 1 calc R . . C22 C 0.5663(3) 0.1477(4) 0.7763(2) 0.0473(12) Uani 1 1 d . . . C23 C 0.6007(3) 0.0710(4) 0.8266(2) 0.0470(12) Uani 1 1 d . . . H23 H 0.5648 0.0374 0.8503 0.056 Uiso 1 1 calc R . . C24 C 0.7717(3) 0.2425(4) 0.7231(2) 0.0508(13) Uani 1 1 d . . . H24A H 0.7541 0.2176 0.6803 0.061 Uiso 1 1 calc R . . H24B H 0.8279 0.2079 0.7383 0.061 Uiso 1 1 calc R . . C25 C 0.7786(3) 0.3854(5) 0.7255(2) 0.0480(12) Uani 1 1 d . . . C26 C 0.7529(3) 0.4554(5) 0.6723(2) 0.0483(12) Uani 1 1 d . . . C27 C 0.7526(3) 0.5889(4) 0.6739(2) 0.0458(12) Uani 1 1 d . . . C28 C 0.7242(3) 0.6670(5) 0.6171(3) 0.0517(13) Uani 1 1 d . . . C29 C 0.7810(3) 0.6481(5) 0.7280(2) 0.0516(13) Uani 1 1 d . . . H29 H 0.7780 0.7350 0.7292 0.062 Uiso 1 1 calc R . . C30 C 0.8153(3) 0.5824(5) 0.7830(2) 0.0499(13) Uani 1 1 d . . . C31 C 0.8536(3) 0.6441(6) 0.8377(3) 0.0631(15) Uani 1 1 d . . . H31 H 0.8522 0.7311 0.8390 0.076 Uiso 1 1 calc R . . C32 C 0.8924(4) 0.5807(7) 0.8882(3) 0.0720(17) Uani 1 1 d . . . H32 H 0.9200 0.6229 0.9233 0.086 Uiso 1 1 calc R . . C33 C 0.8902(4) 0.4497(7) 0.8864(3) 0.0692(16) Uani 1 1 d . . . H33 H 0.9163 0.4057 0.9213 0.083 Uiso 1 1 calc R . . C34 C 0.8519(3) 0.3844(5) 0.8361(2) 0.0558(14) Uani 1 1 d . . . H34 H 0.8503 0.2974 0.8373 0.067 Uiso 1 1 calc R . . C35 C 0.8141(3) 0.4491(5) 0.7818(2) 0.0495(12) Uani 1 1 d . . . O8 O 0.0833(3) 0.2259(5) 0.9097(2) 0.0932(14) Uani 1 1 d U . . N3 N 0.0632(3) 0.3371(5) 0.8229(3) 0.0781(15) Uani 1 1 d U . . C36 C 0.0186(7) 0.2385(10) 0.7889(5) 0.154(4) Uani 1 1 d U . . H36A H 0.0567 0.1907 0.7698 0.231 Uiso 1 1 calc R . . H36B H -0.0263 0.2720 0.7577 0.231 Uiso 1 1 calc R . . H36C H -0.0052 0.1853 0.8159 0.231 Uiso 1 1 calc R . . C37 C 0.0686(7) 0.4409(11) 0.7863(5) 0.177(4) Uani 1 1 d U . . H37A H 0.1205 0.4851 0.8022 0.266 Uiso 1 1 calc R . . H37B H 0.0211 0.4952 0.7865 0.266 Uiso 1 1 calc R . . H37C H 0.0680 0.4142 0.7449 0.266 Uiso 1 1 calc R . . C38 C 0.0917(5) 0.3255(9) 0.8793(4) 0.110(3) Uani 1 1 d U . . H38 H 0.1207 0.3929 0.9005 0.133 Uiso 1 1 calc R . . O9 O 0.8346(6) 0.1396(8) 0.5509(4) 0.183(3) Uani 1 1 d U . . N4 N 0.9091(4) 0.3166(7) 0.5544(3) 0.108(2) Uani 1 1 d U . . C39 C 0.9560(8) 0.4059(13) 0.5947(6) 0.204(5) Uani 1 1 d U . . H39A H 0.9267 0.4847 0.5897 0.305 Uiso 1 1 calc R . . H39B H 1.0113 0.4158 0.5852 0.305 Uiso 1 1 calc R . . H39C H 0.9620 0.3779 0.6365 0.305 Uiso 1 1 calc R . . C40 C 0.8779(10) 0.3421(15) 0.4919(7) 0.234(6) Uani 1 1 d U . . H40A H 0.9237 0.3696 0.4735 0.352 Uiso 1 1 calc R . . H40B H 0.8355 0.4066 0.4879 0.352 Uiso 1 1 calc R . . H40C H 0.8531 0.2676 0.4716 0.352 Uiso 1 1 calc R . . C41 C 0.8810(7) 0.2172(11) 0.5808(6) 0.150(4) Uani 1 1 d U . . H41 H 0.8973 0.2071 0.6232 0.180 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0498(4) 0.0400(4) 0.0474(4) -0.0045(3) 0.0080(3) 0.0002(3) O1 0.050(2) 0.061(2) 0.063(2) 0.0191(18) 0.0107(18) 0.0108(18) O2 0.050(2) 0.050(2) 0.048(2) 0.0061(16) 0.0076(17) -0.0011(16) O3 0.053(2) 0.067(3) 0.063(2) 0.0200(19) 0.0129(18) 0.0154(19) O4 0.105(3) 0.051(2) 0.038(2) 0.0021(16) 0.005(2) -0.001(2) O5 0.070(3) 0.051(2) 0.050(2) 0.0081(17) 0.0029(18) 0.0019(18) O6 0.072(3) 0.043(2) 0.072(3) 0.0064(18) 0.011(2) 0.0098(18) O7 0.054(2) 0.050(2) 0.053(2) 0.0035(15) 0.0056(17) 0.0024(16) N1 0.053(3) 0.042(2) 0.041(2) -0.0039(19) 0.0119(19) 0.007(2) N2 0.047(3) 0.041(2) 0.054(2) -0.0028(19) 0.018(2) 0.0007(19) C1 0.069(4) 0.058(3) 0.052(3) -0.006(3) 0.014(3) 0.011(3) C2 0.072(4) 0.076(4) 0.060(4) 0.006(3) 0.028(3) 0.025(3) C3 0.046(3) 0.085(4) 0.061(4) 0.017(3) 0.016(3) 0.017(3) C4 0.049(3) 0.059(3) 0.045(3) 0.016(2) 0.012(2) 0.006(3) C5 0.054(3) 0.068(4) 0.061(4) 0.018(3) -0.001(3) -0.014(3) C6 0.068(4) 0.051(3) 0.065(4) 0.002(3) 0.009(3) -0.016(3) C7 0.055(3) 0.040(3) 0.050(3) 0.002(2) 0.010(3) -0.005(2) C8 0.087(5) 0.046(3) 0.064(4) -0.016(3) 0.021(3) -0.011(3) C9 0.095(5) 0.053(4) 0.083(4) -0.025(3) 0.036(4) 0.002(3) C10 0.060(4) 0.057(3) 0.075(4) -0.012(3) 0.028(3) 0.001(3) C11 0.052(3) 0.038(3) 0.041(3) 0.005(2) 0.009(2) -0.003(2) C12 0.047(3) 0.047(3) 0.036(3) 0.005(2) 0.013(2) 0.002(2) C13 0.049(3) 0.037(3) 0.049(3) -0.001(2) 0.009(3) 0.002(2) C14 0.050(3) 0.038(3) 0.045(3) 0.000(2) 0.008(2) 0.002(2) C15 0.047(3) 0.046(3) 0.048(3) 0.000(2) 0.008(2) 0.009(2) C16 0.058(3) 0.036(3) 0.043(3) -0.002(2) 0.010(2) 0.004(2) C17 0.058(3) 0.037(3) 0.044(3) -0.007(2) 0.002(3) 0.004(2) C18 0.072(4) 0.038(3) 0.043(3) -0.003(2) 0.002(3) 0.004(3) C19 0.073(4) 0.050(3) 0.055(3) -0.011(3) -0.015(3) 0.019(3) C20 0.055(4) 0.063(4) 0.069(4) -0.010(3) -0.009(3) 0.013(3) C21 0.056(4) 0.052(3) 0.067(4) -0.005(3) 0.001(3) 0.006(3) C22 0.050(3) 0.037(3) 0.052(3) -0.006(2) 0.006(2) 0.005(2) C23 0.053(3) 0.039(3) 0.049(3) 0.000(2) 0.010(2) -0.002(2) C24 0.063(4) 0.047(3) 0.043(3) 0.007(2) 0.012(3) 0.006(2) C25 0.055(3) 0.046(3) 0.045(3) 0.001(2) 0.014(2) 0.002(2) C26 0.055(3) 0.046(3) 0.043(3) -0.002(2) 0.009(2) -0.001(2) C27 0.052(3) 0.043(3) 0.044(3) 0.001(2) 0.014(2) 0.003(2) C28 0.046(3) 0.046(3) 0.064(4) 0.007(3) 0.013(3) 0.003(2) C29 0.055(3) 0.039(3) 0.064(4) -0.004(2) 0.021(3) 0.001(2) C30 0.047(3) 0.056(3) 0.050(3) -0.005(2) 0.017(2) -0.004(2) C31 0.059(4) 0.073(4) 0.060(4) -0.017(3) 0.018(3) -0.008(3) C32 0.067(4) 0.099(5) 0.049(4) -0.015(3) 0.011(3) -0.009(4) C33 0.057(4) 0.096(5) 0.052(4) 0.003(3) 0.007(3) 0.012(3) C34 0.056(3) 0.068(4) 0.045(3) 0.003(3) 0.013(3) 0.008(3) C35 0.043(3) 0.061(3) 0.046(3) 0.002(2) 0.014(2) 0.003(2) O8 0.085(3) 0.100(3) 0.088(3) 0.023(2) 0.004(2) -0.004(2) N3 0.075(3) 0.086(3) 0.071(3) 0.009(3) 0.010(2) 0.008(3) C36 0.142(5) 0.162(6) 0.159(5) -0.026(4) 0.032(4) 0.000(4) C37 0.186(6) 0.175(6) 0.176(6) 0.028(5) 0.050(4) 0.016(5) C38 0.099(4) 0.127(5) 0.104(4) -0.001(4) 0.019(4) 0.010(4) O9 0.173(5) 0.167(5) 0.208(5) -0.010(4) 0.035(4) 0.002(4) N4 0.110(4) 0.103(4) 0.109(4) 0.015(3) 0.018(3) 0.012(3) C39 0.202(7) 0.196(7) 0.207(7) -0.008(5) 0.028(5) -0.002(5) C40 0.242(8) 0.239(8) 0.222(8) 0.004(5) 0.048(5) 0.004(5) C41 0.146(6) 0.149(6) 0.153(6) 0.005(4) 0.026(4) 0.004(4) _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 Cu1 O5 1.971(3) 4_566 ? Cu1 O7 1.980(4) . ? Cu1 N1 2.015(4) . ? Cu1 N2 2.021(4) . ? Cu1 O2 2.252(3) . ? O1 C13 1.259(6) . ? O2 C13 1.253(6) . ? O3 C15 1.366(6) . ? O3 H3 0.8200 . ? O4 C26 1.353(5) . ? O4 H4 0.8200 . ? O5 C28 1.313(6) . ? O5 Cu1 1.971(3) 4_565 ? O6 C28 1.224(6) . ? O7 H7A 0.8546 . ? O7 H7B 0.8549 . ? N1 C1 1.334(6) . ? N1 C12 1.353(6) . ? N2 C10 1.335(6) . ? N2 C11 1.353(6) . ? C1 C2 1.390(8) . ? C1 H1 0.9300 . ? C2 C3 1.360(8) . ? C2 H2 0.9300 . ? C3 C4 1.409(7) . ? C3 H3A 0.9300 . ? C4 C12 1.402(7) . ? C4 C5 1.432(7) . ? C5 C6 1.335(8) . ? C5 H5 0.9300 . ? C6 C7 1.411(7) . ? C6 H6 0.9300 . ? C7 C8 1.389(7) . ? C7 C11 1.394(6) . ? C8 C9 1.344(8) . ? C8 H8 0.9300 . ? C9 C10 1.396(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.424(6) . ? C13 C14 1.501(6) . ? C14 C23 1.370(6) . ? C14 C15 1.430(7) . ? C15 C16 1.377(6) . ? C16 C17 1.419(7) . ? C16 C24 1.527(7) . ? C17 C18 1.408(7) . ? C17 C22 1.426(7) . ? C18 C19 1.356(8) . ? C18 H18 0.9300 . ? C19 C20 1.388(8) . ? C19 H19 0.9300 . ? C20 C21 1.357(7) . ? C20 H20 0.9300 . ? C21 C22 1.417(7) . ? C21 H21 0.9300 . ? C22 C23 1.401(6) . ? C23 H23 0.9300 . ? C24 C25 1.530(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.386(7) . ? C25 C35 1.434(7) . ? C26 C27 1.425(7) . ? C27 C29 1.349(7) . ? C27 C28 1.501(7) . ? C29 C30 1.416(7) . ? C29 H29 0.9300 . ? C30 C31 1.405(7) . ? C30 C35 1.424(7) . ? C31 C32 1.346(8) . ? C31 H31 0.9300 . ? C32 C33 1.400(9) . ? C32 H32 0.9300 . ? C33 C34 1.351(7) . ? C33 H33 0.9300 . ? C34 C35 1.412(7) . ? C34 H34 0.9300 . ? O8 C38 1.281(9) . ? N3 C38 1.247(9) . ? N3 C37 1.387(11) . ? N3 C36 1.403(10) . ? 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 H38 0.9300 . ? O9 C41 1.216(11) . ? N4 C41 1.335(12) . ? N4 C40 1.399(14) . ? N4 C39 1.414(13) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41 0.9300 . ? 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 O5 Cu1 O7 94.09(15) 4_566 . ? O5 Cu1 N1 92.85(15) 4_566 . ? O7 Cu1 N1 172.64(14) . . ? O5 Cu1 N2 166.27(16) 4_566 . ? O7 Cu1 N2 91.64(15) . . ? N1 Cu1 N2 81.05(16) . . ? O5 Cu1 O2 93.72(14) 4_566 . ? O7 Cu1 O2 86.60(13) . . ? N1 Cu1 O2 95.39(14) . . ? N2 Cu1 O2 99.06(14) . . ? C13 O2 Cu1 131.7(3) . . ? C15 O3 H3 109.5 . . ? C26 O4 H4 109.5 . . ? C28 O5 Cu1 107.8(3) . 4_565 ? Cu1 O7 H7A 91.2 . . ? Cu1 O7 H7B 105.7 . . ? H7A O7 H7B 116.0 . . ? C1 N1 C12 117.9(4) . . ? C1 N1 Cu1 128.9(4) . . ? C12 N1 Cu1 113.1(3) . . ? C10 N2 C11 116.7(4) . . ? C10 N2 Cu1 130.1(4) . . ? C11 N2 Cu1 113.1(3) . . ? N1 C1 C2 122.0(5) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 120.4(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C12 C4 C3 116.5(5) . . ? C12 C4 C5 118.2(5) . . ? C3 C4 C5 125.3(5) . . ? C6 C5 C4 121.5(5) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 121.4(5) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C11 116.8(5) . . ? C8 C7 C6 124.1(5) . . ? C11 C7 C6 119.1(5) . . ? C9 C8 C7 120.5(5) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 119.2(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 122.8(5) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C7 123.8(4) . . ? N2 C11 C12 116.1(4) . . ? C7 C11 C12 120.1(5) . . ? N1 C12 C4 123.7(4) . . ? N1 C12 C11 116.5(4) . . ? C4 C12 C11 119.8(5) . . ? O2 C13 O1 124.7(4) . . ? O2 C13 C14 117.7(4) . . ? O1 C13 C14 117.6(5) . . ? C23 C14 C15 118.6(4) . . ? C23 C14 C13 118.8(4) . . ? C15 C14 C13 122.6(4) . . ? O3 C15 C16 119.5(5) . . ? O3 C15 C14 118.9(4) . . ? C16 C15 C14 121.6(5) . . ? C15 C16 C17 119.1(5) . . ? C15 C16 C24 120.1(5) . . ? C17 C16 C24 120.7(4) . . ? C18 C17 C16 124.0(5) . . ? C18 C17 C22 116.4(5) . . ? C16 C17 C22 119.5(4) . . ? C19 C18 C17 121.7(6) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C18 C19 C20 121.8(5) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C21 C20 C19 119.3(6) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 120.6(6) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 120.6(5) . . ? C23 C22 C17 119.2(5) . . ? C21 C22 C17 120.2(5) . . ? C14 C23 C22 121.7(5) . . ? C14 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C16 C24 C25 116.4(4) . . ? C16 C24 H24A 108.2 . . ? C25 C24 H24A 108.2 . . ? C16 C24 H24B 108.2 . . ? C25 C24 H24B 108.2 . . ? H24A C24 H24B 107.3 . . ? C26 C25 C35 118.8(5) . . ? C26 C25 C24 120.1(4) . . ? C35 C25 C24 121.1(4) . . ? O4 C26 C25 118.7(4) . . ? O4 C26 C27 120.0(4) . . ? C25 C26 C27 121.3(4) . . ? C29 C27 C26 119.3(4) . . ? C29 C27 C28 118.3(5) . . ? C26 C27 C28 122.4(4) . . ? O6 C28 O5 122.0(5) . . ? O6 C28 C27 121.5(5) . . ? O5 C28 C27 116.5(4) . . ? C27 C29 C30 122.3(5) . . ? C27 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 122.3(5) . . ? C31 C30 C35 119.0(5) . . ? C29 C30 C35 118.6(4) . . ? C32 C31 C30 121.9(6) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C31 C32 C33 118.2(5) . . ? C31 C32 H32 120.9 . . ? C33 C32 H32 120.9 . . ? C34 C33 C32 123.0(6) . . ? C34 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? C33 C34 C35 119.6(6) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C30 118.2(5) . . ? C34 C35 C25 122.4(5) . . ? C30 C35 C25 119.4(4) . . ? C38 N3 C37 127.7(8) . . ? C38 N3 C36 120.4(8) . . ? C37 N3 C36 111.8(8) . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N3 C38 O8 123.6(9) . . ? N3 C38 H38 118.2 . . ? O8 C38 H38 118.2 . . ? C41 N4 C40 120.3(10) . . ? C41 N4 C39 116.3(10) . . ? C40 N4 C39 122.0(10) . . ? N4 C39 H39A 109.5 . . ? N4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O9 C41 N4 121.8(12) . . ? O9 C41 H41 119.1 . . ? N4 C41 H41 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cu1 O2 C13 93.9(4) 4_566 . . . ? O7 Cu1 O2 C13 0.0(4) . . . . ? N1 Cu1 O2 C13 -172.9(4) . . . . ? N2 Cu1 O2 C13 -91.1(4) . . . . ? O5 Cu1 N1 C1 12.9(4) 4_566 . . . ? N2 Cu1 N1 C1 -179.5(4) . . . . ? O2 Cu1 N1 C1 -81.2(4) . . . . ? O5 Cu1 N1 C12 -170.1(3) 4_566 . . . ? N2 Cu1 N1 C12 -2.4(3) . . . . ? O2 Cu1 N1 C12 95.9(3) . . . . ? O5 Cu1 N2 C10 -115.9(7) 4_566 . . . ? O7 Cu1 N2 C10 -1.1(5) . . . . ? N1 Cu1 N2 C10 179.8(5) . . . . ? O2 Cu1 N2 C10 85.7(5) . . . . ? O5 Cu1 N2 C11 67.9(8) 4_566 . . . ? O7 Cu1 N2 C11 -177.4(3) . . . . ? N1 Cu1 N2 C11 3.5(3) . . . . ? O2 Cu1 N2 C11 -90.5(3) . . . . ? C12 N1 C1 C2 -0.3(7) . . . . ? Cu1 N1 C1 C2 176.7(4) . . . . ? N1 C1 C2 C3 0.7(8) . . . . ? C1 C2 C3 C4 -0.7(8) . . . . ? C2 C3 C4 C12 0.3(7) . . . . ? C2 C3 C4 C5 -178.3(5) . . . . ? C12 C4 C5 C6 -1.3(7) . . . . ? C3 C4 C5 C6 177.3(5) . . . . ? C4 C5 C6 C7 0.9(8) . . . . ? C5 C6 C7 C8 -179.9(5) . . . . ? C5 C6 C7 C11 0.5(8) . . . . ? C11 C7 C8 C9 1.6(8) . . . . ? C6 C7 C8 C9 -177.9(5) . . . . ? C7 C8 C9 C10 -0.7(9) . . . . ? C11 N2 C10 C9 2.3(8) . . . . ? Cu1 N2 C10 C9 -173.8(4) . . . . ? C8 C9 C10 N2 -1.4(9) . . . . ? C10 N2 C11 C7 -1.3(7) . . . . ? Cu1 N2 C11 C7 175.5(4) . . . . ? C10 N2 C11 C12 179.2(4) . . . . ? Cu1 N2 C11 C12 -4.1(5) . . . . ? C8 C7 C11 N2 -0.6(7) . . . . ? C6 C7 C11 N2 179.0(4) . . . . ? C8 C7 C11 C12 178.9(4) . . . . ? C6 C7 C11 C12 -1.5(7) . . . . ? C1 N1 C12 C4 -0.1(7) . . . . ? Cu1 N1 C12 C4 -177.5(3) . . . . ? C1 N1 C12 C11 178.4(4) . . . . ? Cu1 N1 C12 C11 1.0(5) . . . . ? C3 C4 C12 N1 0.1(7) . . . . ? C5 C4 C12 N1 178.8(4) . . . . ? C3 C4 C12 C11 -178.4(4) . . . . ? C5 C4 C12 C11 0.3(7) . . . . ? N2 C11 C12 N1 2.1(6) . . . . ? C7 C11 C12 N1 -177.5(4) . . . . ? N2 C11 C12 C4 -179.3(4) . . . . ? C7 C11 C12 C4 1.1(7) . . . . ? Cu1 O2 C13 O1 -3.4(7) . . . . ? Cu1 O2 C13 C14 175.1(3) . . . . ? O2 C13 C14 C23 -5.2(7) . . . . ? O1 C13 C14 C23 173.5(4) . . . . ? O2 C13 C14 C15 176.5(4) . . . . ? O1 C13 C14 C15 -4.8(7) . . . . ? C23 C14 C15 O3 -179.4(4) . . . . ? C13 C14 C15 O3 -1.0(7) . . . . ? C23 C14 C15 C16 0.9(7) . . . . ? C13 C14 C15 C16 179.3(4) . . . . ? O3 C15 C16 C17 175.9(4) . . . . ? C14 C15 C16 C17 -4.4(7) . . . . ? O3 C15 C16 C24 0.2(7) . . . . ? C14 C15 C16 C24 179.9(4) . . . . ? C15 C16 C17 C18 -174.0(4) . . . . ? C24 C16 C17 C18 1.7(7) . . . . ? C15 C16 C17 C22 4.0(7) . . . . ? C24 C16 C17 C22 179.7(4) . . . . ? C16 C17 C18 C19 178.4(4) . . . . ? C22 C17 C18 C19 0.4(7) . . . . ? C17 C18 C19 C20 0.7(8) . . . . ? C18 C19 C20 C21 -1.4(8) . . . . ? C19 C20 C21 C22 0.9(8) . . . . ? C20 C21 C22 C23 -178.5(5) . . . . ? C20 C21 C22 C17 0.3(7) . . . . ? C18 C17 C22 C23 177.9(4) . . . . ? C16 C17 C22 C23 -0.2(7) . . . . ? C18 C17 C22 C21 -0.9(7) . . . . ? C16 C17 C22 C21 -179.0(4) . . . . ? C15 C14 C23 C22 3.0(7) . . . . ? C13 C14 C23 C22 -175.4(4) . . . . ? C21 C22 C23 C14 175.4(5) . . . . ? C17 C22 C23 C14 -3.3(7) . . . . ? C15 C16 C24 C25 -118.7(5) . . . . ? C17 C16 C24 C25 65.7(6) . . . . ? C16 C24 C25 C26 -115.8(5) . . . . ? C16 C24 C25 C35 66.3(6) . . . . ? C35 C25 C26 O4 175.1(4) . . . . ? C24 C25 C26 O4 -2.8(7) . . . . ? C35 C25 C26 C27 -6.8(7) . . . . ? C24 C25 C26 C27 175.3(5) . . . . ? O4 C26 C27 C29 -179.4(5) . . . . ? C25 C26 C27 C29 2.5(8) . . . . ? O4 C26 C27 C28 -1.2(8) . . . . ? C25 C26 C27 C28 -179.3(4) . . . . ? Cu1 O5 C28 O6 2.8(6) 4_565 . . . ? Cu1 O5 C28 C27 -176.4(3) 4_565 . . . ? C29 C27 C28 O6 -4.5(7) . . . . ? C26 C27 C28 O6 177.3(5) . . . . ? C29 C27 C28 O5 174.8(4) . . . . ? C26 C27 C28 O5 -3.4(7) . . . . ? C26 C27 C29 C30 3.3(8) . . . . ? C28 C27 C29 C30 -175.0(4) . . . . ? C27 C29 C30 C31 172.6(5) . . . . ? C27 C29 C30 C35 -4.4(7) . . . . ? C29 C30 C31 C32 -174.2(5) . . . . ? C35 C30 C31 C32 2.8(8) . . . . ? C30 C31 C32 C33 -3.3(9) . . . . ? C31 C32 C33 C34 0.8(9) . . . . ? C32 C33 C34 C35 2.0(9) . . . . ? C33 C34 C35 C30 -2.4(7) . . . . ? C33 C34 C35 C25 174.8(5) . . . . ? C31 C30 C35 C34 0.1(7) . . . . ? C29 C30 C35 C34 177.2(4) . . . . ? C31 C30 C35 C25 -177.2(5) . . . . ? C29 C30 C35 C25 -0.1(7) . . . . ? C26 C25 C35 C34 -171.6(5) . . . . ? C24 C25 C35 C34 6.2(7) . . . . ? C26 C25 C35 C30 5.5(7) . . . . ? C24 C25 C35 C30 -176.6(5) . . . . ? C37 N3 C38 O8 179.6(8) . . . . ? C36 N3 C38 O8 0.4(12) . . . . ? C40 N4 C41 O9 7.4(17) . . . . ? C39 N4 C41 O9 174.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.861 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.070 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 631548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.5 H34.5 N3.5 O8.5 Zn' _chemical_formula_weight 759.58 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.913(2) _cell_length_b 10.4978(16) _cell_length_c 22.979(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.159(2) _cell_angle_gamma 90.00 _cell_volume 3752.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2454 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 20.38 _exptl_crystal_description Lamellar _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.768642 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 19342 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6602 _reflns_number_gt 4447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II ' _computing_cell_refinement 'Bruker APEX II ' _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^)+(0.1267P)^2^+2.5771P] 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 6602 _refine_ls_number_parameters 503 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.2192 _refine_ls_wR_factor_gt 0.1935 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.079 _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 Zn1 Zn 0.31930(4) 0.78262(5) 0.50431(2) 0.0431(2) Uani 1 1 d . . . O1 O 0.2811(2) 0.7421(4) 0.39854(18) 0.0639(10) Uani 1 1 d . . . O2 O 0.2986(2) 0.9308(4) 0.44107(16) 0.0619(10) Uani 1 1 d . . . O3 O 0.2801(3) 1.1325(3) 0.37956(15) 0.0624(10) Uani 1 1 d . . . H3 H 0.2902 1.0863 0.4090 0.094 Uiso 1 1 calc R . . O4 O 0.1726(2) 1.4244(4) 0.17420(18) 0.0586(10) Uani 1 1 d . . . H4 H 0.1622 1.4772 0.1473 0.10(3) Uiso 1 1 calc R . . O5 O 0.1995(2) 1.5708(3) 0.09083(16) 0.0589(10) Uani 1 1 d . . . O6 O 0.3322(2) 1.5940(3) 0.07558(14) 0.0464(8) Uani 1 1 d . . . O7 O 0.1911(2) 0.7517(4) 0.50607(16) 0.0554(9) Uani 1 1 d . . . H7A H 0.1605 0.7582 0.4709 0.083 Uiso 1 1 d R . . H7B H 0.1919 0.8181 0.5282 0.083 Uiso 1 1 d R . . N1 N 0.3593(3) 0.6130(4) 0.55296(18) 0.0450(10) Uani 1 1 d . . . N2 N 0.4537(3) 0.7706(3) 0.50183(17) 0.0421(9) Uani 1 1 d . . . C1 C 0.3125(4) 0.5367(5) 0.5800(3) 0.0592(14) Uani 1 1 d . . . H1 H 0.2533 0.5486 0.5727 0.071 Uiso 1 1 calc R . . C2 C 0.3490(4) 0.4397(6) 0.6188(3) 0.0735(18) Uani 1 1 d . . . H2 H 0.3143 0.3892 0.6373 0.088 Uiso 1 1 calc R . . C3 C 0.4347(4) 0.4191(5) 0.6292(3) 0.0655(16) Uani 1 1 d . . . H3A H 0.4596 0.3557 0.6556 0.079 Uiso 1 1 calc R . . C4 C 0.4854(3) 0.4936(5) 0.6003(2) 0.0487(12) Uani 1 1 d . . . C5 C 0.5759(4) 0.4754(5) 0.6076(2) 0.0568(14) Uani 1 1 d . . . H5 H 0.6028 0.4111 0.6325 0.068 Uiso 1 1 calc R . . C6 C 0.6226(3) 0.5492(5) 0.5791(2) 0.0565(14) Uani 1 1 d . . . H6 H 0.6812 0.5342 0.5838 0.068 Uiso 1 1 calc R . . C7 C 0.5835(3) 0.6512(5) 0.5413(2) 0.0486(12) Uani 1 1 d . . . C8 C 0.6286(4) 0.7331(6) 0.5108(3) 0.0574(14) Uani 1 1 d . . . H8 H 0.6870 0.7206 0.5128 0.069 Uiso 1 1 calc R . . C9 C 0.5870(4) 0.8305(6) 0.4783(3) 0.0631(15) Uani 1 1 d . . . H9 H 0.6171 0.8868 0.4589 0.076 Uiso 1 1 calc R . . C10 C 0.4992(4) 0.8461(5) 0.4740(2) 0.0564(14) Uani 1 1 d . . . H10 H 0.4713 0.9122 0.4508 0.068 Uiso 1 1 calc R . . C11 C 0.4958(3) 0.6732(4) 0.5344(2) 0.0402(11) Uani 1 1 d . . . C12 C 0.4455(3) 0.5908(4) 0.5640(2) 0.0404(11) Uani 1 1 d . . . C13 C 0.2795(3) 0.8599(5) 0.3945(3) 0.0539(13) Uani 1 1 d . . . C14 C 0.2534(3) 0.9248(5) 0.3350(2) 0.0451(11) Uani 1 1 d . . . C15 C 0.2528(3) 1.0605(5) 0.3301(2) 0.0458(12) Uani 1 1 d . . . C16 C 0.2273(3) 1.1215(5) 0.2756(2) 0.0441(11) Uani 1 1 d . . . C17 C 0.1937(3) 1.0461(5) 0.2248(2) 0.0442(11) Uani 1 1 d . . . C18 C 0.1529(3) 1.1015(6) 0.1695(2) 0.0527(13) Uani 1 1 d . . . H18 H 0.1510 1.1896 0.1652 0.063 Uiso 1 1 calc R . . C19 C 0.1165(4) 1.0249(7) 0.1225(2) 0.0655(16) Uani 1 1 d . . . H19 H 0.0891 1.0623 0.0868 0.079 Uiso 1 1 calc R . . C20 C 0.1194(4) 0.8929(7) 0.1268(3) 0.0698(17) Uani 1 1 d . . . H20 H 0.0941 0.8431 0.0943 0.084 Uiso 1 1 calc R . . C21 C 0.1587(4) 0.8373(6) 0.1779(3) 0.0663(16) Uani 1 1 d . . . H21 H 0.1624 0.7489 0.1798 0.080 Uiso 1 1 calc R . . C22 C 0.1948(3) 0.9106(5) 0.2293(2) 0.0487(12) Uani 1 1 d . . . C23 C 0.2268(3) 0.8539(5) 0.2845(2) 0.0484(12) Uani 1 1 d . . . H23 H 0.2301 0.7656 0.2870 0.058 Uiso 1 1 calc R . . C24 C 0.2313(3) 1.2667(5) 0.2733(2) 0.0478(12) Uani 1 1 d . . . H24A H 0.2483 1.2981 0.3138 0.057 Uiso 1 1 calc R . . H24B H 0.1738 1.2982 0.2573 0.057 Uiso 1 1 calc R . . C25 C 0.2920(3) 1.3251(4) 0.2366(2) 0.0413(11) Uani 1 1 d . . . C26 C 0.2595(3) 1.4019(4) 0.1889(2) 0.0436(11) Uani 1 1 d . . . C27 C 0.3135(3) 1.4594(4) 0.1538(2) 0.0400(11) Uani 1 1 d . . . C28 C 0.2791(3) 1.5474(4) 0.1036(2) 0.0416(11) Uani 1 1 d . . . C29 C 0.4003(3) 1.4369(4) 0.1693(2) 0.0435(11) Uani 1 1 d . . . H29 H 0.4358 1.4717 0.1461 0.052 Uiso 1 1 calc R . . C30 C 0.4370(3) 1.3638(4) 0.2186(2) 0.0430(11) Uani 1 1 d . . . C31 C 0.5271(3) 1.3476(5) 0.2355(3) 0.0570(14) Uani 1 1 d . . . H31 H 0.5625 1.3834 0.2125 0.068 Uiso 1 1 calc R . . C32 C 0.5624(4) 1.2800(5) 0.2852(3) 0.0639(16) Uani 1 1 d . . . H32 H 0.6217 1.2694 0.2959 0.077 Uiso 1 1 calc R . . C33 C 0.5100(4) 1.2271(5) 0.3198(3) 0.0570(14) Uani 1 1 d . . . H33 H 0.5349 1.1828 0.3542 0.068 Uiso 1 1 calc R . . C34 C 0.4225(3) 1.2382(5) 0.3046(2) 0.0487(12) Uani 1 1 d . . . H34 H 0.3891 1.2001 0.3284 0.058 Uiso 1 1 calc R . . C35 C 0.3819(3) 1.3065(4) 0.2534(2) 0.0411(11) Uani 1 1 d . . . C36 C 0.0989(14) 0.186(2) 0.5048(6) 0.177(10) Uani 0.50 1 d PDU . . H36A H 0.1149 0.2690 0.5209 0.266 Uiso 0.50 1 calc PR . . H36B H 0.1428 0.1257 0.5214 0.266 Uiso 0.50 1 calc PR . . H36C H 0.0455 0.1611 0.5147 0.266 Uiso 0.50 1 calc PR . . C37 C 0.0467(9) 0.0874(13) 0.4094(8) 0.112(6) Uani 0.50 1 d PD . . H37A H 0.0282 0.1142 0.3687 0.168 Uiso 0.50 1 calc PR . . H37B H -0.0024 0.0625 0.4248 0.168 Uiso 0.50 1 calc PR . . H37C H 0.0852 0.0164 0.4113 0.168 Uiso 0.50 1 calc PR . . C38 C 0.1219(7) 0.2910(10) 0.4172(6) 0.086(5) Uani 0.50 1 d PD . . H38 H 0.1145 0.2894 0.3760 0.103 Uiso 0.50 1 calc PR . . N3 N 0.0893(4) 0.1889(7) 0.4435(4) 0.045(2) Uani 0.50 1 d PD . . O8 O 0.1575(6) 0.3783(9) 0.4418(6) 0.114(4) Uani 0.50 1 d PD . . C39 C 0.9847(6) 0.2620(9) 0.2149(5) 0.133(3) Uani 1 1 d DU . . H39A H 0.9982 0.3273 0.1891 0.200 Uiso 1 1 calc R . . H39B H 1.0369 0.2282 0.2385 0.200 Uiso 1 1 calc R . . H39C H 0.9503 0.2975 0.2405 0.200 Uiso 1 1 calc R . . C40 C 0.9253(7) 0.0547(10) 0.2123(5) 0.182(5) Uani 1 1 d DU . . H40A H 0.8832 0.0011 0.1878 0.273 Uiso 1 1 calc R . . H40B H 0.9051 0.0794 0.2472 0.273 Uiso 1 1 calc R . . H40C H 0.9784 0.0090 0.2238 0.273 Uiso 1 1 calc R . . C41 C 0.9102(5) 0.1763(8) 0.1214(3) 0.096(2) Uani 1 1 d D . . H41 H 0.8795 0.1101 0.0998 0.115 Uiso 1 1 calc R . . N4 N 0.9384(3) 0.1632(5) 0.1802(2) 0.0706(14) Uani 1 1 d D . . O9 O 0.9240(3) 0.2735(5) 0.0951(2) 0.0904(15) Uani 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 Zn1 0.0488(4) 0.0407(4) 0.0392(4) 0.0026(2) 0.0080(3) 0.0029(2) O1 0.063(3) 0.055(2) 0.073(3) 0.023(2) 0.013(2) 0.0085(18) O2 0.073(3) 0.069(2) 0.041(2) 0.0135(19) 0.0035(19) 0.002(2) O3 0.102(3) 0.050(2) 0.0305(19) 0.0006(16) 0.0033(19) -0.001(2) O4 0.044(2) 0.073(3) 0.060(2) 0.025(2) 0.0148(17) 0.0127(17) O5 0.047(2) 0.068(2) 0.060(2) 0.0229(19) 0.0094(18) 0.0070(18) O6 0.050(2) 0.0483(19) 0.0407(19) 0.0044(15) 0.0078(16) -0.0015(15) O7 0.056(2) 0.056(2) 0.053(2) -0.0072(17) 0.0071(18) -0.0003(17) N1 0.050(3) 0.038(2) 0.050(2) 0.0014(18) 0.016(2) 0.0015(18) N2 0.052(2) 0.038(2) 0.036(2) 0.0008(17) 0.0110(19) -0.0048(18) C1 0.058(3) 0.052(3) 0.077(4) 0.008(3) 0.033(3) -0.002(3) C2 0.087(5) 0.053(3) 0.090(5) 0.021(3) 0.041(4) -0.002(3) C3 0.079(4) 0.049(3) 0.071(4) 0.012(3) 0.023(3) 0.006(3) C4 0.058(3) 0.043(3) 0.046(3) -0.001(2) 0.014(2) 0.004(2) C5 0.067(4) 0.045(3) 0.054(3) 0.001(3) 0.004(3) 0.013(3) C6 0.046(3) 0.061(3) 0.059(3) -0.012(3) 0.004(3) 0.010(3) C7 0.049(3) 0.053(3) 0.044(3) -0.014(2) 0.009(2) -0.002(2) C8 0.046(3) 0.069(4) 0.059(3) -0.013(3) 0.014(3) -0.012(3) C9 0.067(4) 0.072(4) 0.056(4) -0.007(3) 0.024(3) -0.024(3) C10 0.078(4) 0.048(3) 0.047(3) 0.000(2) 0.021(3) -0.013(3) C11 0.047(3) 0.037(2) 0.037(3) -0.008(2) 0.008(2) -0.002(2) C12 0.046(3) 0.038(2) 0.038(3) -0.004(2) 0.009(2) 0.001(2) C13 0.043(3) 0.062(3) 0.057(4) 0.016(3) 0.011(3) 0.004(2) C14 0.046(3) 0.047(3) 0.043(3) 0.006(2) 0.010(2) 0.001(2) C15 0.050(3) 0.046(3) 0.041(3) 0.002(2) 0.010(2) 0.001(2) C16 0.047(3) 0.046(3) 0.041(3) 0.004(2) 0.013(2) 0.002(2) C17 0.038(3) 0.058(3) 0.038(3) 0.001(2) 0.011(2) 0.000(2) C18 0.048(3) 0.070(3) 0.041(3) 0.007(3) 0.012(2) 0.002(3) C19 0.056(4) 0.100(5) 0.038(3) 0.002(3) 0.006(3) -0.006(3) C20 0.072(4) 0.091(5) 0.046(4) -0.012(3) 0.011(3) -0.021(3) C21 0.079(4) 0.066(4) 0.059(4) -0.018(3) 0.027(3) -0.017(3) C22 0.047(3) 0.056(3) 0.046(3) -0.010(2) 0.018(2) -0.011(2) C23 0.043(3) 0.048(3) 0.057(3) 0.009(3) 0.016(2) -0.001(2) C24 0.057(3) 0.047(3) 0.040(3) 0.007(2) 0.012(2) 0.009(2) C25 0.055(3) 0.036(2) 0.033(2) 0.001(2) 0.009(2) 0.002(2) C26 0.038(3) 0.045(3) 0.047(3) 0.000(2) 0.007(2) 0.008(2) C27 0.045(3) 0.036(2) 0.038(3) -0.002(2) 0.005(2) 0.002(2) C28 0.049(3) 0.037(2) 0.040(3) 0.000(2) 0.011(2) -0.002(2) C29 0.048(3) 0.037(2) 0.046(3) -0.005(2) 0.011(2) -0.003(2) C30 0.043(3) 0.039(2) 0.044(3) -0.004(2) 0.002(2) 0.001(2) C31 0.050(3) 0.055(3) 0.063(4) -0.006(3) 0.006(3) 0.001(2) C32 0.049(3) 0.062(4) 0.070(4) -0.006(3) -0.012(3) 0.014(3) C33 0.070(4) 0.045(3) 0.046(3) -0.003(2) -0.009(3) 0.010(3) C34 0.058(3) 0.041(3) 0.042(3) -0.003(2) -0.001(2) 0.000(2) C35 0.049(3) 0.031(2) 0.039(3) -0.0070(19) 0.000(2) 0.006(2) C36 0.181(11) 0.175(11) 0.178(11) -0.001(5) 0.040(5) 0.004(5) C37 0.114(13) 0.077(10) 0.150(16) -0.021(10) 0.038(12) -0.012(9) C38 0.042(7) 0.094(11) 0.111(12) 0.013(9) -0.005(7) 0.036(7) N3 0.044(5) 0.036(4) 0.055(5) 0.014(4) 0.009(4) 0.017(3) O8 0.049(5) 0.052(5) 0.233(14) -0.006(7) 0.016(7) 0.000(4) C39 0.119(5) 0.148(5) 0.133(5) -0.015(4) 0.028(4) -0.003(4) C40 0.191(7) 0.177(7) 0.182(6) 0.018(5) 0.049(5) 0.010(5) C41 0.085(5) 0.111(6) 0.090(6) -0.011(5) 0.014(4) 0.010(5) N4 0.063(3) 0.072(3) 0.075(4) 0.009(3) 0.010(3) 0.011(3) O9 0.089(3) 0.094(4) 0.078(3) 0.027(3) -0.004(3) -0.019(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 O6 2.064(3) 4_586 ? Zn1 O7 2.075(3) . ? Zn1 O2 2.107(3) . ? Zn1 N1 2.127(4) . ? Zn1 N2 2.156(4) . ? Zn1 O1 2.416(4) . ? Zn1 C13 2.600(5) . ? O1 C13 1.240(6) . ? O2 C13 1.287(7) . ? O3 C15 1.359(6) . ? O3 H3 0.8200 . ? O4 C26 1.374(5) . ? O4 H4 0.8200 . ? O5 C28 1.264(6) . ? O6 C28 1.263(5) . ? O6 Zn1 2.064(3) 4_585 ? O7 H7A 0.8539 . ? O7 H7B 0.8621 . ? N1 C1 1.332(6) . ? N1 C12 1.362(6) . ? N2 C10 1.324(6) . ? N2 C11 1.358(6) . ? C1 C2 1.397(8) . ? C1 H1 0.9300 . ? C2 C3 1.352(8) . ? C2 H2 0.9300 . ? C3 C4 1.389(7) . ? C3 H3A 0.9300 . ? C4 C12 1.385(7) . ? C4 C5 1.428(7) . ? C5 C6 1.336(8) . ? C5 H5 0.9300 . ? C6 C7 1.435(7) . ? C6 H6 0.9300 . ? C7 C11 1.390(7) . ? C7 C8 1.399(8) . ? C8 C9 1.354(8) . ? C8 H8 0.9300 . ? C9 C10 1.389(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.443(6) . ? C13 C14 1.505(7) . ? C14 C23 1.368(7) . ? C14 C15 1.429(7) . ? C15 C16 1.387(7) . ? C16 C17 1.419(7) . ? C16 C24 1.527(7) . ? C17 C18 1.425(7) . ? C17 C22 1.425(7) . ? C18 C19 1.374(8) . ? C18 H18 0.9300 . ? C19 C20 1.389(9) . ? C19 H19 0.9300 . ? C20 C21 1.342(8) . ? C20 H20 0.9300 . ? C21 C22 1.426(7) . ? C21 H21 0.9300 . ? C22 C23 1.396(7) . ? C23 H23 0.9300 . ? C24 C25 1.536(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.373(6) . ? C25 C35 1.415(7) . ? C26 C27 1.430(6) . ? C27 C29 1.372(6) . ? C27 C28 1.488(6) . ? C29 C30 1.391(7) . ? C29 H29 0.9300 . ? C30 C31 1.414(7) . ? C30 C35 1.436(7) . ? C31 C32 1.361(8) . ? C31 H31 0.9300 . ? C32 C33 1.384(9) . ? C32 H32 0.9300 . ? C33 C34 1.366(8) . ? C33 H33 0.9300 . ? C34 C35 1.413(7) . ? C34 H34 0.9300 . ? C36 N3 1.385(10) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N3 1.410(9) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 O8 1.160(9) . ? C38 N3 1.384(9) . ? C38 H38 0.9300 . ? C39 N4 1.416(7) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 N4 1.395(8) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 O9 1.229(7) . ? C41 N4 1.339(7) . ? C41 H41 0.9300 . ? 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 O6 Zn1 O7 90.97(14) 4_586 . ? O6 Zn1 O2 93.37(15) 4_586 . ? O7 Zn1 O2 96.73(15) . . ? O6 Zn1 N1 98.02(14) 4_586 . ? O7 Zn1 N1 92.60(15) . . ? O2 Zn1 N1 165.14(15) . . ? O6 Zn1 N2 97.11(14) 4_586 . ? O7 Zn1 N2 167.65(15) . . ? O2 Zn1 N2 92.11(15) . . ? N1 Zn1 N2 77.07(14) . . ? O6 Zn1 O1 150.54(13) 4_586 . ? O7 Zn1 O1 87.25(14) . . ? O2 Zn1 O1 57.74(14) . . ? N1 Zn1 O1 111.44(14) . . ? N2 Zn1 O1 90.22(14) . . ? O6 Zn1 C13 122.52(16) 4_586 . ? O7 Zn1 C13 91.62(15) . . ? O2 Zn1 C13 29.42(16) . . ? N1 Zn1 C13 139.14(17) . . ? N2 Zn1 C13 91.87(15) . . ? O1 Zn1 C13 28.33(15) . . ? C13 O1 Zn1 84.1(3) . . ? C13 O2 Zn1 97.0(3) . . ? C15 O3 H3 109.5 . . ? C26 O4 H4 109.5 . . ? C28 O6 Zn1 132.9(3) . 4_585 ? Zn1 O7 H7A 109.5 . . ? Zn1 O7 H7B 89.5 . . ? H7A O7 H7B 115.5 . . ? C1 N1 C12 116.7(4) . . ? C1 N1 Zn1 127.8(3) . . ? C12 N1 Zn1 114.8(3) . . ? C10 N2 C11 117.4(5) . . ? C10 N2 Zn1 128.6(4) . . ? C11 N2 Zn1 114.0(3) . . ? N1 C1 C2 122.6(5) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.9(5) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C12 C4 C3 117.7(5) . . ? C12 C4 C5 119.5(5) . . ? C3 C4 C5 122.8(5) . . ? C6 C5 C4 121.1(5) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C11 C7 C8 116.7(5) . . ? C11 C7 C6 119.3(5) . . ? C8 C7 C6 124.0(5) . . ? C9 C8 C7 119.8(5) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.7(5) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 122.6(5) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N2 C11 C7 123.7(4) . . ? N2 C11 C12 116.9(4) . . ? C7 C11 C12 119.4(4) . . ? N1 C12 C4 123.7(4) . . ? N1 C12 C11 116.5(4) . . ? C4 C12 C11 119.7(4) . . ? O1 C13 O2 121.1(5) . . ? O1 C13 C14 121.1(5) . . ? O2 C13 C14 117.8(5) . . ? O1 C13 Zn1 67.6(3) . . ? O2 C13 Zn1 53.5(2) . . ? C14 C13 Zn1 170.8(4) . . ? C23 C14 C15 118.7(5) . . ? C23 C14 C13 120.1(5) . . ? C15 C14 C13 121.3(5) . . ? O3 C15 C16 118.6(4) . . ? O3 C15 C14 119.5(4) . . ? C16 C15 C14 121.8(5) . . ? C15 C16 C17 118.2(4) . . ? C15 C16 C24 119.1(4) . . ? C17 C16 C24 122.6(4) . . ? C16 C17 C18 121.9(5) . . ? C16 C17 C22 120.0(4) . . ? C18 C17 C22 117.9(5) . . ? C19 C18 C17 120.0(6) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 121.7(6) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C21 C20 C19 119.9(6) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 121.5(6) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C17 119.2(5) . . ? C23 C22 C21 121.9(5) . . ? C17 C22 C21 118.8(5) . . ? C14 C23 C22 121.8(5) . . ? C14 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C16 C24 C25 117.0(4) . . ? C16 C24 H24A 108.1 . . ? C25 C24 H24A 108.1 . . ? C16 C24 H24B 108.1 . . ? C25 C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? C26 C25 C35 119.2(4) . . ? C26 C25 C24 119.9(4) . . ? C35 C25 C24 120.8(4) . . ? C25 C26 O4 119.2(4) . . ? C25 C26 C27 122.0(4) . . ? O4 C26 C27 118.8(4) . . ? C29 C27 C26 118.1(4) . . ? C29 C27 C28 119.6(4) . . ? C26 C27 C28 122.2(4) . . ? O6 C28 O5 123.5(4) . . ? O6 C28 C27 117.3(4) . . ? O5 C28 C27 119.1(4) . . ? C27 C29 C30 122.3(5) . . ? C27 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C29 C30 C31 121.1(5) . . ? C29 C30 C35 119.0(4) . . ? C31 C30 C35 119.9(5) . . ? C32 C31 C30 120.6(5) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 119.9(5) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 121.6(5) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 121.2(5) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C25 123.8(5) . . ? C34 C35 C30 116.8(4) . . ? C25 C35 C30 119.4(4) . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O8 C38 N3 126.1(13) . . ? O8 C38 H38 117.0 . . ? N3 C38 H38 117.0 . . ? C38 N3 C36 119.4(14) . . ? C38 N3 C37 121.5(11) . . ? C36 N3 C37 119.1(15) . . ? N4 C39 H39A 109.5 . . ? N4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O9 C41 N4 121.7(7) . . ? O9 C41 H41 119.2 . . ? N4 C41 H41 119.2 . . ? C41 N4 C40 124.1(8) . . ? C41 N4 C39 121.1(7) . . ? C40 N4 C39 114.8(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zn1 O1 C13 11.5(4) 4_586 . . . ? O7 Zn1 O1 C13 98.6(3) . . . . ? O2 Zn1 O1 C13 -1.2(3) . . . . ? N1 Zn1 O1 C13 -169.7(3) . . . . ? N2 Zn1 O1 C13 -93.5(3) . . . . ? O6 Zn1 O2 C13 -172.7(3) 4_586 . . . ? O7 Zn1 O2 C13 -81.3(3) . . . . ? N1 Zn1 O2 C13 47.3(7) . . . . ? N2 Zn1 O2 C13 90.1(3) . . . . ? O1 Zn1 O2 C13 1.1(3) . . . . ? O6 Zn1 N1 C1 82.2(4) 4_586 . . . ? O7 Zn1 N1 C1 -9.1(5) . . . . ? O2 Zn1 N1 C1 -138.1(6) . . . . ? N2 Zn1 N1 C1 177.7(5) . . . . ? O1 Zn1 N1 C1 -97.2(4) . . . . ? C13 Zn1 N1 C1 -104.6(5) . . . . ? O6 Zn1 N1 C12 -88.3(3) 4_586 . . . ? O7 Zn1 N1 C12 -179.6(3) . . . . ? O2 Zn1 N1 C12 51.4(8) . . . . ? N2 Zn1 N1 C12 7.2(3) . . . . ? O1 Zn1 N1 C12 92.3(3) . . . . ? C13 Zn1 N1 C12 84.9(4) . . . . ? O6 Zn1 N2 C10 -86.8(4) 4_586 . . . ? O7 Zn1 N2 C10 142.7(6) . . . . ? O2 Zn1 N2 C10 6.9(4) . . . . ? N1 Zn1 N2 C10 176.6(4) . . . . ? O1 Zn1 N2 C10 64.6(4) . . . . ? C13 Zn1 N2 C10 36.3(4) . . . . ? O6 Zn1 N2 C11 91.9(3) 4_586 . . . ? O7 Zn1 N2 C11 -38.6(8) . . . . ? O2 Zn1 N2 C11 -174.4(3) . . . . ? N1 Zn1 N2 C11 -4.7(3) . . . . ? O1 Zn1 N2 C11 -116.7(3) . . . . ? C13 Zn1 N2 C11 -145.0(3) . . . . ? C12 N1 C1 C2 1.2(8) . . . . ? Zn1 N1 C1 C2 -169.2(4) . . . . ? N1 C1 C2 C3 -1.1(9) . . . . ? C1 C2 C3 C4 -1.2(9) . . . . ? C2 C3 C4 C12 3.2(8) . . . . ? C2 C3 C4 C5 -178.0(5) . . . . ? C12 C4 C5 C6 -1.1(8) . . . . ? C3 C4 C5 C6 -179.9(5) . . . . ? C4 C5 C6 C7 1.5(8) . . . . ? C5 C6 C7 C11 0.0(7) . . . . ? C5 C6 C7 C8 179.1(5) . . . . ? C11 C7 C8 C9 2.2(8) . . . . ? C6 C7 C8 C9 -176.9(5) . . . . ? C7 C8 C9 C10 -1.9(8) . . . . ? C11 N2 C10 C9 -1.5(7) . . . . ? Zn1 N2 C10 C9 177.1(4) . . . . ? C8 C9 C10 N2 1.6(8) . . . . ? C10 N2 C11 C7 1.9(7) . . . . ? Zn1 N2 C11 C7 -177.0(3) . . . . ? C10 N2 C11 C12 -179.4(4) . . . . ? Zn1 N2 C11 C12 1.8(5) . . . . ? C8 C7 C11 N2 -2.2(7) . . . . ? C6 C7 C11 N2 177.0(4) . . . . ? C8 C7 C11 C12 179.1(4) . . . . ? C6 C7 C11 C12 -1.7(7) . . . . ? C1 N1 C12 C4 1.1(7) . . . . ? Zn1 N1 C12 C4 172.7(4) . . . . ? C1 N1 C12 C11 179.7(4) . . . . ? Zn1 N1 C12 C11 -8.7(5) . . . . ? C3 C4 C12 N1 -3.3(7) . . . . ? C5 C4 C12 N1 177.9(4) . . . . ? C3 C4 C12 C11 178.2(5) . . . . ? C5 C4 C12 C11 -0.6(7) . . . . ? N2 C11 C12 N1 4.6(6) . . . . ? C7 C11 C12 N1 -176.6(4) . . . . ? N2 C11 C12 C4 -176.7(4) . . . . ? C7 C11 C12 C4 2.0(7) . . . . ? Zn1 O1 C13 O2 1.9(5) . . . . ? Zn1 O1 C13 C14 -176.8(4) . . . . ? Zn1 O2 C13 O1 -2.2(5) . . . . ? Zn1 O2 C13 C14 176.6(4) . . . . ? O6 Zn1 C13 O1 -173.3(3) 4_586 . . . ? O7 Zn1 C13 O1 -81.2(3) . . . . ? O2 Zn1 C13 O1 178.0(5) . . . . ? N1 Zn1 C13 O1 14.7(4) . . . . ? N2 Zn1 C13 O1 87.0(3) . . . . ? O6 Zn1 C13 O2 8.7(4) 4_586 . . . ? O7 Zn1 C13 O2 100.9(3) . . . . ? N1 Zn1 C13 O2 -163.3(3) . . . . ? N2 Zn1 C13 O2 -91.0(3) . . . . ? O1 Zn1 C13 O2 -178.0(5) . . . . ? O2 C13 C14 C23 -175.5(4) . . . . ? O1 C13 C14 C15 -179.1(5) . . . . ? O2 C13 C14 C15 2.2(7) . . . . ? C23 C14 C15 O3 -179.1(4) . . . . ? C13 C14 C15 O3 3.2(7) . . . . ? C23 C14 C15 C16 -1.1(7) . . . . ? C13 C14 C15 C16 -178.8(4) . . . . ? O3 C15 C16 C17 -176.0(4) . . . . ? C14 C15 C16 C17 5.9(7) . . . . ? O3 C15 C16 C24 0.3(7) . . . . ? C14 C15 C16 C24 -177.7(4) . . . . ? C15 C16 C17 C18 169.3(4) . . . . ? C24 C16 C17 C18 -6.9(7) . . . . ? C15 C16 C17 C22 -6.3(7) . . . . ? C24 C16 C17 C22 177.5(4) . . . . ? C16 C17 C18 C19 -175.9(5) . . . . ? C22 C17 C18 C19 -0.2(7) . . . . ? C17 C18 C19 C20 -1.2(8) . . . . ? C18 C19 C20 C21 -0.1(9) . . . . ? C19 C20 C21 C22 2.7(9) . . . . ? C16 C17 C22 C23 2.0(7) . . . . ? C18 C17 C22 C23 -173.8(4) . . . . ? C16 C17 C22 C21 178.4(4) . . . . ? C18 C17 C22 C21 2.6(7) . . . . ? C20 C21 C22 C23 172.3(5) . . . . ? C20 C21 C22 C17 -4.0(8) . . . . ? C15 C14 C23 C22 -3.5(7) . . . . ? C13 C14 C23 C22 174.2(4) . . . . ? C17 C22 C23 C14 3.1(7) . . . . ? C21 C22 C23 C14 -173.3(5) . . . . ? C15 C16 C24 C25 117.5(5) . . . . ? C17 C16 C24 C25 -66.3(6) . . . . ? C16 C24 C25 C26 119.3(5) . . . . ? C16 C24 C25 C35 -64.3(6) . . . . ? C35 C25 C26 O4 -177.1(4) . . . . ? C24 C25 C26 O4 -0.6(7) . . . . ? C35 C25 C26 C27 2.8(7) . . . . ? C24 C25 C26 C27 179.4(4) . . . . ? C25 C26 C27 C29 -0.6(7) . . . . ? O4 C26 C27 C29 179.4(4) . . . . ? C25 C26 C27 C28 -177.3(4) . . . . ? O4 C26 C27 C28 2.7(7) . . . . ? Zn1 O6 C28 O5 0.5(7) 4_585 . . . ? Zn1 O6 C28 C27 179.9(3) 4_585 . . . ? C29 C27 C28 O6 2.8(6) . . . . ? C26 C27 C28 O6 179.5(4) . . . . ? C29 C27 C28 O5 -177.7(4) . . . . ? C26 C27 C28 O5 -1.0(7) . . . . ? C26 C27 C29 C30 -1.9(7) . . . . ? C28 C27 C29 C30 174.9(4) . . . . ? C27 C29 C30 C31 -176.6(4) . . . . ? C27 C29 C30 C35 2.0(7) . . . . ? C29 C30 C31 C32 177.4(5) . . . . ? C35 C30 C31 C32 -1.2(7) . . . . ? C30 C31 C32 C33 -0.3(8) . . . . ? C31 C32 C33 C34 1.6(8) . . . . ? C32 C33 C34 C35 -1.2(8) . . . . ? C33 C34 C35 C25 -177.7(4) . . . . ? C33 C34 C35 C30 -0.4(7) . . . . ? C26 C25 C35 C34 174.5(4) . . . . ? C24 C25 C35 C34 -1.9(7) . . . . ? C26 C25 C35 C30 -2.7(7) . . . . ? C24 C25 C35 C30 -179.2(4) . . . . ? C29 C30 C35 C34 -177.1(4) . . . . ? C31 C30 C35 C34 1.5(7) . . . . ? C29 C30 C35 C25 0.3(6) . . . . ? C31 C30 C35 C25 179.0(4) . . . . ? O8 C38 N3 C36 -0.4(13) . . . . ? O8 C38 N3 C37 179.8(13) . . . . ? O9 C41 N4 C40 -179.4(8) . . . . ? O9 C41 N4 C39 0.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.968 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.099 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 631549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H29 Cd N3 O7' _chemical_formula_weight 752.04 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.8834(19) _cell_length_b 15.273(2) _cell_length_c 19.365(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.135(8) _cell_angle_gamma 90.00 _cell_volume 3299.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4789 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 22.89 _exptl_crystal_description Rhombous _exptl_crystal_colour Pale-Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas Nnoe _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.759111 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 17710 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5817 _reflns_number_gt 4619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0493P)^2^+0.8703P] 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 5817 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Cd1 Cd 0.099519(18) 0.286936(13) 0.352671(11) 0.04042(9) Uani 1 1 d . . . O1 O 0.2582(2) 0.30090(16) 0.47226(12) 0.0616(6) Uani 1 1 d . . . O2 O 0.1023(2) 0.21699(14) 0.45908(12) 0.0569(6) Uani 1 1 d . . . O3 O -0.0896(2) 0.24241(16) 0.28632(14) 0.0676(7) Uani 1 1 d . . . O4 O 0.2100(2) 0.18887(16) 0.31701(13) 0.0664(7) Uani 1 1 d . . . O5 O 0.38531(18) 0.09051(15) 0.31775(11) 0.0553(6) Uani 1 1 d . . . H5 H 0.3399 0.1155 0.3350 0.083 Uiso 1 1 calc R . . O6 O 0.4120(2) 0.33005(17) 0.59838(12) 0.0609(6) Uani 1 1 d . . . H6 H 0.3782 0.3330 0.5537 0.091 Uiso 1 1 calc R . . N1 N -0.0065(2) 0.40289(19) 0.38012(16) 0.0600(7) Uani 1 1 d . . . N2 N 0.1668(2) 0.41649(18) 0.31880(15) 0.0557(7) Uani 1 1 d . . . C1 C 0.1994(3) 0.2503(2) 0.49880(17) 0.0472(7) Uani 1 1 d . . . C2 C 0.2450(2) 0.23271(18) 0.57962(15) 0.0401(7) Uani 1 1 d . . . C3 C 0.1838(3) 0.1774(2) 0.60886(16) 0.0439(7) Uani 1 1 d . . . H3 H 0.1164 0.1487 0.5778 0.053 Uiso 1 1 calc R . . C4 C 0.2201(2) 0.16277(18) 0.68496(16) 0.0425(7) Uani 1 1 d . . . C5 C 0.1544(3) 0.1068(2) 0.71533(19) 0.0592(9) Uani 1 1 d . . . H5A H 0.0876 0.0776 0.6841 0.071 Uiso 1 1 calc R . . C6 C 0.1870(3) 0.0949(3) 0.7888(2) 0.0683(10) Uani 1 1 d . . . H6A H 0.1429 0.0579 0.8079 0.082 Uiso 1 1 calc R . . C7 C 0.2873(3) 0.1386(2) 0.83577(19) 0.0575(8) Uani 1 1 d . . . H7 H 0.3091 0.1306 0.8863 0.069 Uiso 1 1 calc R . . C8 C 0.3539(3) 0.1926(2) 0.80937(16) 0.0468(7) Uani 1 1 d . . . H8 H 0.4202 0.2209 0.8420 0.056 Uiso 1 1 calc R . . C9 C 0.3237(2) 0.20620(17) 0.73269(16) 0.0385(6) Uani 1 1 d . . . C10 C 0.3911(2) 0.26160(19) 0.70241(15) 0.0376(6) Uani 1 1 d . . . C11 C 0.3505(3) 0.27502(18) 0.62742(16) 0.0418(7) Uani 1 1 d . . . C12 C 0.1707(3) 0.1908(2) 0.24774(19) 0.0502(8) Uani 1 1 d . . . C13 C 0.2259(2) 0.13274(19) 0.20672(16) 0.0440(7) Uani 1 1 d . . . C14 C 0.1716(3) 0.1215(2) 0.13220(17) 0.0505(8) Uani 1 1 d . . . H14 H 0.0994 0.1497 0.1081 0.061 Uiso 1 1 calc R . . C15 C 0.2218(3) 0.0689(2) 0.09191(16) 0.0480(7) Uani 1 1 d . . . C16 C 0.1630(3) 0.0542(2) 0.01586(19) 0.0657(9) Uani 1 1 d . . . H16 H 0.0888 0.0800 -0.0078 0.079 Uiso 1 1 calc R . . C17 C 0.2131(4) 0.0030(3) -0.0234(2) 0.0741(11) Uani 1 1 d . . . H17 H 0.1720 -0.0078 -0.0729 0.089 Uiso 1 1 calc R . . C18 C 0.3258(4) -0.0329(2) 0.0110(2) 0.0679(10) Uani 1 1 d . . . H18 H 0.3613 -0.0657 -0.0164 0.081 Uiso 1 1 calc R . . C19 C 0.3853(3) -0.0210(2) 0.08401(18) 0.0541(8) Uani 1 1 d . . . H19 H 0.4608 -0.0460 0.1054 0.065 Uiso 1 1 calc R . . C20 C 0.3355(3) 0.02822(18) 0.12845(16) 0.0428(7) Uani 1 1 d . . . C21 C 0.3901(2) 0.03695(17) 0.20602(16) 0.0387(6) Uani 1 1 d . . . C22 C 0.3341(2) 0.08673(19) 0.24359(15) 0.0416(7) Uani 1 1 d . . . C23 C 0.5000 0.3127(3) 0.7500 0.0446(10) Uani 1 2 d S . . H23A H 0.4745 0.3504 0.7821 0.053 Uiso 0.50 1 calc PR . . H23B H 0.5255 0.3504 0.7179 0.053 Uiso 0.50 1 calc PR . . C24 C 0.5000 -0.0143(3) 0.2500 0.0422(9) Uani 1 2 d S . . H24A H 0.4782 -0.0520 0.2837 0.051 Uiso 0.50 1 calc PR . . H24B H 0.5218 -0.0520 0.2163 0.051 Uiso 0.50 1 calc PR . . C25 C 0.0293(3) 0.4833(2) 0.3688(2) 0.0720(11) Uani 1 1 d . . . C26 C 0.1209(3) 0.4902(2) 0.3367(2) 0.0691(10) Uani 1 1 d . . . C27 C 0.2492(4) 0.4227(3) 0.2879(3) 0.0839(13) Uani 1 1 d . . . H27 H 0.2801 0.3716 0.2753 0.101 Uiso 1 1 calc R . . C28 C 0.2913(6) 0.5022(4) 0.2734(4) 0.141(3) Uani 1 1 d . . . H28 H 0.3511 0.5049 0.2526 0.169 Uiso 1 1 calc R . . C29 C 0.2440(6) 0.5758(4) 0.2900(5) 0.159(3) Uani 1 1 d . . . H29 H 0.2688 0.6297 0.2781 0.191 Uiso 1 1 calc R . . C30 C 0.1591(5) 0.5733(3) 0.3244(4) 0.121(2) Uani 1 1 d . . . C31 C 0.1085(7) 0.6485(4) 0.3443(5) 0.186(4) Uani 1 1 d . . . H31 H 0.1360 0.7035 0.3370 0.223 Uiso 1 1 calc R . . C32 C 0.0238(7) 0.6426(4) 0.3728(6) 0.187(4) Uani 1 1 d . . . H32 H -0.0085 0.6936 0.3844 0.224 Uiso 1 1 calc R . . C33 C -0.0212(5) 0.5592(3) 0.3869(4) 0.1163(19) Uani 1 1 d . . . C34 C -0.1103(6) 0.5475(4) 0.4167(4) 0.150(3) Uani 1 1 d . . . H34 H -0.1452 0.5963 0.4300 0.180 Uiso 1 1 calc R . . C35 C -0.1476(5) 0.4671(4) 0.4270(4) 0.132(2) Uani 1 1 d . . . H35 H -0.2089 0.4597 0.4460 0.159 Uiso 1 1 calc R . . C36 C -0.0923(4) 0.3956(3) 0.4085(3) 0.0898(13) Uani 1 1 d . . . H36 H -0.1168 0.3399 0.4164 0.108 Uiso 1 1 calc R . . O7 O 0.4130(9) 0.3580(8) 0.1784(5) 0.339(6) Uani 1 1 d . . . N3 N 0.4387(6) 0.3105(6) 0.0747(5) 0.155(3) Uani 1 1 d . . . C37 C 0.4497(9) 0.2334(6) 0.0384(5) 0.184(4) Uani 1 1 d . . . H37A H 0.4409 0.1837 0.0664 0.276 Uiso 1 1 calc R . . H37B H 0.5272 0.2317 0.0332 0.276 Uiso 1 1 calc R . . H37C H 0.3886 0.2320 -0.0094 0.276 Uiso 1 1 calc R . . C38 C 0.4447(9) 0.3972(6) 0.0442(6) 0.250(6) Uani 1 1 d . . . H38A H 0.4360 0.4413 0.0774 0.376 Uiso 1 1 calc R . . H38B H 0.3814 0.4031 -0.0024 0.376 Uiso 1 1 calc R . . H38C H 0.5207 0.4043 0.0377 0.376 Uiso 1 1 calc R . . C39 C 0.4222(9) 0.2977(8) 0.1329(8) 0.206(5) Uani 1 1 d . . . H39 H 0.4155 0.2397 0.1458 0.247 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04020(13) 0.04504(14) 0.03263(13) -0.00195(9) 0.00819(9) 0.00126(9) O1 0.0546(13) 0.0898(17) 0.0358(12) 0.0064(11) 0.0097(11) -0.0106(12) O2 0.0512(13) 0.0694(15) 0.0368(12) 0.0004(10) -0.0019(10) -0.0075(11) O3 0.0524(14) 0.0624(14) 0.0754(17) 0.0031(13) 0.0060(12) -0.0245(12) O4 0.0693(15) 0.0790(16) 0.0483(15) -0.0026(12) 0.0168(12) 0.0314(13) O5 0.0502(12) 0.0703(15) 0.0390(12) -0.0029(10) 0.0071(10) 0.0187(11) O6 0.0541(13) 0.0839(16) 0.0377(12) 0.0126(12) 0.0070(10) -0.0164(12) N1 0.0501(16) 0.0628(18) 0.069(2) -0.0138(15) 0.0237(15) 0.0013(13) N2 0.0556(16) 0.0522(17) 0.0602(18) -0.0024(13) 0.0211(14) -0.0077(13) C1 0.0463(18) 0.0525(18) 0.0387(17) -0.0006(15) 0.0092(15) 0.0105(15) C2 0.0378(15) 0.0453(17) 0.0341(15) 0.0009(12) 0.0083(12) 0.0070(12) C3 0.0369(15) 0.0504(17) 0.0405(17) -0.0051(14) 0.0082(13) 0.0005(13) C4 0.0390(15) 0.0442(17) 0.0441(17) 0.0019(13) 0.0141(13) 0.0063(13) C5 0.0534(19) 0.065(2) 0.059(2) 0.0057(17) 0.0199(17) -0.0092(16) C6 0.066(2) 0.084(3) 0.064(2) 0.018(2) 0.033(2) -0.007(2) C7 0.060(2) 0.071(2) 0.0460(19) 0.0115(17) 0.0243(16) 0.0069(18) C8 0.0444(16) 0.0586(19) 0.0361(16) 0.0043(14) 0.0124(14) 0.0105(14) C9 0.0360(14) 0.0411(16) 0.0375(15) 0.0022(12) 0.0115(12) 0.0103(12) C10 0.0345(14) 0.0434(16) 0.0297(15) -0.0009(12) 0.0042(12) 0.0049(12) C11 0.0382(15) 0.0485(18) 0.0370(16) 0.0037(13) 0.0108(13) 0.0026(13) C12 0.0419(17) 0.0491(18) 0.055(2) -0.0025(15) 0.0104(15) 0.0056(14) C13 0.0394(15) 0.0442(16) 0.0441(17) 0.0002(13) 0.0090(13) 0.0059(13) C14 0.0452(17) 0.0544(19) 0.0454(18) 0.0073(15) 0.0072(14) 0.0072(14) C15 0.0474(17) 0.0534(19) 0.0385(17) 0.0013(14) 0.0085(14) -0.0033(14) C16 0.069(2) 0.073(2) 0.044(2) 0.0060(17) 0.0053(17) 0.0015(19) C17 0.100(3) 0.082(3) 0.0368(19) -0.0046(18) 0.019(2) -0.013(2) C18 0.090(3) 0.067(2) 0.054(2) -0.0113(18) 0.034(2) -0.009(2) C19 0.0593(19) 0.0527(19) 0.053(2) -0.0055(15) 0.0224(16) -0.0047(16) C20 0.0447(16) 0.0418(16) 0.0403(17) -0.0024(13) 0.0126(13) -0.0085(13) C21 0.0338(14) 0.0358(15) 0.0442(17) 0.0008(12) 0.0106(13) -0.0052(12) C22 0.0384(15) 0.0438(16) 0.0373(16) -0.0001(13) 0.0061(13) 0.0008(13) C23 0.046(2) 0.046(2) 0.037(2) 0.000 0.0085(19) 0.000 C24 0.040(2) 0.037(2) 0.050(3) 0.000 0.0156(19) 0.000 C25 0.064(2) 0.054(2) 0.094(3) -0.015(2) 0.023(2) 0.0044(18) C26 0.070(2) 0.045(2) 0.090(3) -0.0015(18) 0.024(2) -0.0038(17) C27 0.083(3) 0.082(3) 0.104(4) -0.001(2) 0.055(3) -0.017(2) C28 0.139(5) 0.104(4) 0.228(8) -0.001(5) 0.125(5) -0.036(4) C29 0.152(6) 0.084(4) 0.271(10) 0.020(5) 0.111(7) -0.038(4) C30 0.120(4) 0.051(3) 0.211(7) 0.002(3) 0.080(5) -0.015(3) C31 0.210(8) 0.041(3) 0.348(13) -0.005(4) 0.150(9) -0.006(4) C32 0.184(7) 0.053(3) 0.358(13) -0.035(5) 0.138(8) 0.013(4) C33 0.106(4) 0.069(3) 0.180(6) -0.031(3) 0.057(4) 0.016(3) C34 0.124(5) 0.110(5) 0.243(9) -0.056(5) 0.096(5) 0.023(4) C35 0.105(4) 0.138(5) 0.189(7) -0.044(5) 0.097(4) 0.004(4) C36 0.081(3) 0.093(3) 0.113(4) -0.021(3) 0.055(3) -0.001(2) O7 0.372(14) 0.401(15) 0.278(10) -0.039(10) 0.157(10) 0.095(11) N3 0.125(5) 0.200(7) 0.177(7) -0.005(6) 0.099(5) 0.003(4) C37 0.238(11) 0.192(8) 0.137(7) 0.002(6) 0.086(7) -0.040(7) C38 0.297(13) 0.185(9) 0.379(17) 0.069(9) 0.256(13) -0.006(8) C39 0.143(7) 0.210(11) 0.270(16) -0.068(10) 0.080(9) 0.021(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 Cd1 O4 2.251(2) . ? Cd1 O3 2.275(2) . ? Cd1 O2 2.311(2) . ? Cd1 N2 2.312(3) . ? Cd1 N1 2.338(3) . ? Cd1 O1 2.441(2) . ? Cd1 C1 2.723(3) . ? O1 C1 1.263(4) . ? O2 C1 1.253(4) . ? O3 C12 1.244(4) 2 ? O4 C12 1.260(4) . ? O5 C22 1.355(3) . ? O5 H5 0.8200 . ? O6 C11 1.356(4) . ? O6 H6 0.8200 . ? N1 C36 1.319(5) . ? N1 C25 1.343(5) . ? N2 C27 1.315(4) . ? N2 C26 1.348(4) . ? C1 C2 1.494(4) . ? C2 C3 1.359(4) . ? C2 C11 1.431(4) . ? C3 C4 1.404(4) . ? C3 H3 0.9300 . ? C4 C5 1.415(4) . ? C4 C9 1.424(4) . ? C5 C6 1.352(5) . ? C5 H5A 0.9300 . ? C6 C7 1.395(5) . ? C6 H6A 0.9300 . ? C7 C8 1.358(4) . ? C7 H7 0.9300 . ? C8 C9 1.418(4) . ? C8 H8 0.9300 . ? C9 C10 1.423(4) . ? C10 C11 1.379(4) . ? C10 C23 1.520(3) . ? C12 O3 1.244(4) 2 ? C12 C13 1.486(4) . ? C13 C14 1.374(4) . ? C13 C22 1.423(4) . ? C14 C15 1.389(4) . ? C14 H14 0.9300 . ? C15 C16 1.414(4) . ? C15 C20 1.433(4) . ? C16 C17 1.361(5) . ? C16 H16 0.9300 . ? C17 C18 1.387(6) . ? C17 H17 0.9300 . ? C18 C19 1.357(5) . ? C18 H18 0.9300 . ? C19 C20 1.417(4) . ? C19 H19 0.9300 . ? C20 C21 1.423(4) . ? C21 C22 1.372(4) . ? C21 C24 1.509(3) . ? C23 C10 1.520(3) 2_656 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C21 1.509(3) 2_655 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C33 1.404(6) . ? C25 C26 1.430(6) . ? C26 C30 1.395(6) . ? C27 C28 1.379(7) . ? C27 H27 0.9300 . ? C28 C29 1.344(8) . ? C28 H28 0.9300 . ? C29 C30 1.388(8) . ? C29 H29 0.9300 . ? C30 C31 1.411(8) . ? C31 C32 1.308(9) . ? C31 H31 0.9300 . ? C32 C33 1.442(9) . ? C32 H32 0.9300 . ? C33 C34 1.382(8) . ? C34 C35 1.343(8) . ? C34 H34 0.9300 . ? C35 C36 1.384(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O7 C39 1.305(11) . ? N3 C39 1.224(14) . ? N3 C37 1.401(10) . ? N3 C38 1.462(10) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39 0.9300 . ? 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 O4 Cd1 O3 101.23(10) . . ? O4 Cd1 O2 97.76(9) . . ? O3 Cd1 O2 94.23(8) . . ? O4 Cd1 N2 100.79(10) . . ? O3 Cd1 N2 117.80(9) . . ? O2 Cd1 N2 138.44(9) . . ? O4 Cd1 N1 172.07(10) . . ? O3 Cd1 N1 81.37(10) . . ? O2 Cd1 N1 89.48(9) . . ? N2 Cd1 N1 71.48(10) . . ? O4 Cd1 O1 90.44(9) . . ? O3 Cd1 O1 148.46(8) . . ? O2 Cd1 O1 54.91(7) . . ? N2 Cd1 O1 87.98(9) . . ? N1 Cd1 O1 91.08(9) . . ? O4 Cd1 C1 95.18(9) . . ? O3 Cd1 C1 121.20(10) . . ? O2 Cd1 C1 27.29(9) . . ? N2 Cd1 C1 113.64(10) . . ? N1 Cd1 C1 89.76(10) . . ? O1 Cd1 C1 27.63(8) . . ? C1 O1 Cd1 88.74(18) . . ? C1 O2 Cd1 95.0(2) . . ? C12 O3 Cd1 157.4(2) 2 . ? C12 O4 Cd1 105.62(19) . . ? C22 O5 H5 109.5 . . ? C11 O6 H6 109.5 . . ? C36 N1 C25 118.6(3) . . ? C36 N1 Cd1 125.8(3) . . ? C25 N1 Cd1 115.5(2) . . ? C27 N2 C26 119.2(3) . . ? C27 N2 Cd1 125.1(3) . . ? C26 N2 Cd1 115.6(2) . . ? O2 C1 O1 121.3(3) . . ? O2 C1 C2 119.7(3) . . ? O1 C1 C2 119.0(3) . . ? O2 C1 Cd1 57.70(16) . . ? O1 C1 Cd1 63.63(16) . . ? C2 C1 Cd1 175.4(2) . . ? C3 C2 C11 119.1(3) . . ? C3 C2 C1 119.7(3) . . ? C11 C2 C1 121.2(3) . . ? C2 C3 C4 121.4(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 C9 119.5(3) . . ? C5 C4 C9 119.3(3) . . ? C6 C5 C4 121.3(3) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 119.5(3) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C8 C7 C6 121.5(3) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 120.9(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C10 122.9(3) . . ? C8 C9 C4 117.5(3) . . ? C10 C9 C4 119.6(3) . . ? C11 C10 C9 118.7(3) . . ? C11 C10 C23 118.6(2) . . ? C9 C10 C23 122.5(2) . . ? O6 C11 C10 119.0(3) . . ? O6 C11 C2 119.3(3) . . ? C10 C11 C2 121.7(3) . . ? O3 C12 O4 121.0(3) 2 . ? O3 C12 C13 119.9(3) 2 . ? O4 C12 C13 119.0(3) . . ? C14 C13 C22 118.8(3) . . ? C14 C13 C12 120.2(3) . . ? C22 C13 C12 121.0(3) . . ? C13 C14 C15 121.7(3) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C16 121.5(3) . . ? C14 C15 C20 119.2(3) . . ? C16 C15 C20 119.3(3) . . ? C17 C16 C15 121.2(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 119.6(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 121.8(3) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C21 123.9(3) . . ? C19 C20 C15 116.7(3) . . ? C21 C20 C15 119.4(3) . . ? C22 C21 C20 118.9(3) . . ? C22 C21 C24 118.1(2) . . ? C20 C21 C24 122.6(2) . . ? O5 C22 C21 117.6(2) . . ? O5 C22 C13 120.7(2) . . ? C21 C22 C13 121.8(3) . . ? C10 C23 C10 118.2(3) . 2_656 ? C10 C23 H23A 107.8 . . ? C10 C23 H23A 107.8 2_656 . ? C10 C23 H23B 107.8 . . ? C10 C23 H23B 107.8 2_656 . ? H23A C23 H23B 107.1 . . ? C21 C24 C21 117.6(3) 2_655 . ? C21 C24 H24A 107.9 2_655 . ? C21 C24 H24A 107.9 . . ? C21 C24 H24B 107.9 2_655 . ? C21 C24 H24B 107.9 . . ? H24A C24 H24B 107.2 . . ? N1 C25 C33 121.9(4) . . ? N1 C25 C26 118.0(3) . . ? C33 C25 C26 120.1(4) . . ? N2 C26 C30 122.0(4) . . ? N2 C26 C25 119.1(3) . . ? C30 C26 C25 118.9(4) . . ? N2 C27 C28 122.4(4) . . ? N2 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C29 C28 C27 118.5(5) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C28 C29 C30 121.7(5) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C29 C30 C26 116.2(5) . . ? C29 C30 C31 123.9(5) . . ? C26 C30 C31 119.9(5) . . ? C32 C31 C30 121.4(6) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 122.0(6) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C34 C33 C25 116.9(5) . . ? C34 C33 C32 125.5(5) . . ? C25 C33 C32 117.6(5) . . ? C35 C34 C33 121.3(5) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 118.2(5) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? N1 C36 C35 123.1(5) . . ? N1 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? C39 N3 C37 113.6(10) . . ? C39 N3 C38 124.2(10) . . ? C37 N3 C38 122.2(8) . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N3 C38 H38A 109.5 . . ? N3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 O7 125.9(15) . . ? N3 C39 H39 117.1 . . ? O7 C39 H39 117.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cd1 O1 C1 -100.4(2) . . . . ? O3 Cd1 O1 C1 12.2(3) . . . . ? O2 Cd1 O1 C1 -1.20(17) . . . . ? N2 Cd1 O1 C1 158.8(2) . . . . ? N1 Cd1 O1 C1 87.41(19) . . . . ? O4 Cd1 O2 C1 86.26(19) . . . . ? O3 Cd1 O2 C1 -171.79(19) . . . . ? N2 Cd1 O2 C1 -29.8(2) . . . . ? N1 Cd1 O2 C1 -90.48(19) . . . . ? O1 Cd1 O2 C1 1.21(18) . . . . ? O4 Cd1 O3 C12 26.6(6) . . . 2 ? O2 Cd1 O3 C12 -72.1(6) . . . 2 ? N2 Cd1 O3 C12 135.3(6) . . . 2 ? N1 Cd1 O3 C12 -161.0(6) . . . 2 ? O1 Cd1 O3 C12 -83.1(7) . . . 2 ? C1 Cd1 O3 C12 -76.5(6) . . . 2 ? O3 Cd1 O4 C12 52.2(2) . . . . ? O2 Cd1 O4 C12 148.1(2) . . . . ? N2 Cd1 O4 C12 -69.2(2) . . . . ? O1 Cd1 O4 C12 -157.3(2) . . . . ? C1 Cd1 O4 C12 175.5(2) . . . . ? O3 Cd1 N1 C36 55.2(3) . . . . ? O2 Cd1 N1 C36 -39.1(3) . . . . ? N2 Cd1 N1 C36 178.5(4) . . . . ? O1 Cd1 N1 C36 -94.0(3) . . . . ? C1 Cd1 N1 C36 -66.4(3) . . . . ? O3 Cd1 N1 C25 -128.3(3) . . . . ? O2 Cd1 N1 C25 137.4(3) . . . . ? N2 Cd1 N1 C25 -5.0(3) . . . . ? O1 Cd1 N1 C25 82.5(3) . . . . ? C1 Cd1 N1 C25 110.1(3) . . . . ? O4 Cd1 N2 C27 -0.5(3) . . . . ? O3 Cd1 N2 C27 -109.5(3) . . . . ? O2 Cd1 N2 C27 114.4(3) . . . . ? N1 Cd1 N2 C27 -178.6(4) . . . . ? O1 Cd1 N2 C27 89.5(3) . . . . ? C1 Cd1 N2 C27 100.1(3) . . . . ? O4 Cd1 N2 C26 -176.7(3) . . . . ? O3 Cd1 N2 C26 74.4(3) . . . . ? O2 Cd1 N2 C26 -61.7(3) . . . . ? N1 Cd1 N2 C26 5.2(2) . . . . ? O1 Cd1 N2 C26 -86.6(3) . . . . ? C1 Cd1 N2 C26 -76.1(3) . . . . ? Cd1 O2 C1 O1 -2.2(3) . . . . ? Cd1 O2 C1 C2 175.5(2) . . . . ? Cd1 O1 C1 O2 2.1(3) . . . . ? Cd1 O1 C1 C2 -175.7(2) . . . . ? O4 Cd1 C1 O2 -96.88(19) . . . . ? O3 Cd1 C1 O2 9.6(2) . . . . ? N2 Cd1 C1 O2 158.94(18) . . . . ? N1 Cd1 C1 O2 89.34(19) . . . . ? O1 Cd1 C1 O2 -177.9(3) . . . . ? O4 Cd1 C1 O1 81.0(2) . . . . ? O3 Cd1 C1 O1 -172.55(17) . . . . ? O2 Cd1 C1 O1 177.9(3) . . . . ? N2 Cd1 C1 O1 -23.2(2) . . . . ? N1 Cd1 C1 O1 -92.80(19) . . . . ? O2 C1 C2 C3 3.2(4) . . . . ? O1 C1 C2 C3 -179.0(3) . . . . ? O2 C1 C2 C11 -175.1(3) . . . . ? O1 C1 C2 C11 2.8(4) . . . . ? C11 C2 C3 C4 1.7(4) . . . . ? C1 C2 C3 C4 -176.6(3) . . . . ? C2 C3 C4 C5 178.5(3) . . . . ? C2 C3 C4 C9 -0.4(4) . . . . ? C3 C4 C5 C6 -177.8(3) . . . . ? C5 C6 C7 C8 -0.5(6) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 C10 -179.6(3) . . . . ? C7 C8 C9 C4 1.3(4) . . . . ? C3 C4 C9 C8 177.2(3) . . . . ? C5 C4 C9 C8 -1.7(4) . . . . ? C3 C4 C9 C10 -2.0(4) . . . . ? C5 C4 C9 C10 179.1(3) . . . . ? C8 C9 C10 C11 -176.0(3) . . . . ? C4 C9 C10 C11 3.1(4) . . . . ? C8 C9 C10 C23 -1.5(4) . . . . ? C4 C9 C10 C23 177.7(3) . . . . ? C9 C10 C11 O6 177.8(3) . . . . ? C23 C10 C11 O6 3.0(4) . . . . ? C9 C10 C11 C2 -1.9(4) . . . . ? C23 C10 C11 C2 -176.7(3) . . . . ? C3 C2 C11 O6 179.8(3) . . . . ? C1 C2 C11 O6 -2.0(4) . . . . ? C3 C2 C11 C10 -0.5(4) . . . . ? C1 C2 C11 C10 177.8(3) . . . . ? Cd1 O4 C12 O3 2.2(4) . . . 2 ? Cd1 O4 C12 C13 179.9(2) . . . . ? O3 C12 C13 C14 -14.3(5) 2 . . . ? O4 C12 C13 C14 168.0(3) . . . . ? O3 C12 C13 C22 166.9(3) 2 . . . ? O4 C12 C13 C22 -10.8(5) . . . . ? C22 C13 C14 C15 -2.3(5) . . . . ? C12 C13 C14 C15 178.8(3) . . . . ? C13 C14 C15 C16 177.1(3) . . . . ? C13 C14 C15 C20 -2.6(5) . . . . ? C14 C15 C16 C17 179.6(3) . . . . ? C20 C15 C16 C17 -0.7(5) . . . . ? C15 C16 C17 C18 -2.4(6) . . . . ? C16 C17 C18 C19 2.8(6) . . . . ? C17 C18 C19 C20 0.1(5) . . . . ? C18 C19 C20 C21 175.0(3) . . . . ? C18 C19 C20 C15 -3.1(5) . . . . ? C14 C15 C20 C19 -176.9(3) . . . . ? C16 C15 C20 C19 3.4(4) . . . . ? C14 C15 C20 C21 4.9(4) . . . . ? C16 C15 C20 C21 -174.8(3) . . . . ? C19 C20 C21 C22 179.7(3) . . . . ? C15 C20 C21 C22 -2.2(4) . . . . ? C19 C20 C21 C24 -7.3(4) . . . . ? C15 C20 C21 C24 170.8(3) . . . . ? C20 C21 C22 O5 177.0(2) . . . . ? C24 C21 C22 O5 3.7(4) . . . . ? C20 C21 C22 C13 -2.8(4) . . . . ? C24 C21 C22 C13 -176.1(3) . . . . ? C14 C13 C22 O5 -174.7(3) . . . . ? C12 C13 C22 O5 4.2(4) . . . . ? C14 C13 C22 C21 5.1(4) . . . . ? C12 C13 C22 C21 -176.1(3) . . . . ? C11 C10 C23 C10 -121.5(3) . . . 2_656 ? C9 C10 C23 C10 63.9(2) . . . 2_656 ? C22 C21 C24 C21 -65.8(2) . . . 2_655 ? C20 C21 C24 C21 121.2(3) . . . 2_655 ? C36 N1 C25 C33 0.5(6) . . . . ? Cd1 N1 C25 C33 -176.2(4) . . . . ? C36 N1 C25 C26 -178.8(4) . . . . ? Cd1 N1 C25 C26 4.4(5) . . . . ? C27 N2 C26 C30 -0.8(6) . . . . ? Cd1 N2 C26 C30 175.6(4) . . . . ? C27 N2 C26 C25 178.6(4) . . . . ? Cd1 N2 C26 C25 -5.1(5) . . . . ? N1 C25 C26 N2 0.4(6) . . . . ? C33 C25 C26 N2 -179.0(4) . . . . ? N1 C25 C26 C30 179.8(4) . . . . ? C33 C25 C26 C30 0.4(7) . . . . ? C26 N2 C27 C28 0.5(7) . . . . ? Cd1 N2 C27 C28 -175.6(5) . . . . ? N2 C27 C28 C29 -1.7(10) . . . . ? C27 C28 C29 C30 3.3(12) . . . . ? C28 C29 C30 C26 -3.5(12) . . . . ? C28 C29 C30 C31 178.7(8) . . . . ? N2 C26 C30 C29 2.3(9) . . . . ? C25 C26 C30 C29 -177.1(6) . . . . ? N2 C26 C30 C31 -179.8(6) . . . . ? C25 C26 C30 C31 0.8(9) . . . . ? N1 C25 C33 C34 -0.2(8) . . . . ? N1 C25 C33 C32 179.8(6) . . . . ? C26 C25 C33 C32 -0.9(9) . . . . ? C31 C32 C33 C34 -179.9(9) . . . . ? C31 C32 C33 C25 0.1(14) . . . . ? C25 C33 C34 C35 -0.8(11) . . . . ? C32 C33 C34 C35 179.2(8) . . . . ? C33 C34 C35 C36 1.5(12) . . . . ? C25 N1 C36 C35 0.2(7) . . . . ? Cd1 N1 C36 C35 176.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.420 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.055 #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 631550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H36 Cu N4 O8' _chemical_formula_weight 752.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.6316(10) _cell_length_b 11.0803(8) _cell_length_c 11.7201(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.2420(10) _cell_angle_gamma 90.00 _cell_volume 1804.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4011 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.64 _exptl_crystal_description Block _exptl_crystal_colour Blue-Green _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.865489 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 9556 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3197 _reflns_number_gt 2726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0612P)^2^+0.7303P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3197 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Cu1 Cu 0.5000 0.75300(2) 0.7500 0.02809(14) Uani 1 2 d S . . O1 O 0.40111(10) 0.75884(11) 0.59057(13) 0.0361(3) Uani 1 1 d . . . O2 O 0.29589(10) 0.63120(15) 0.62728(13) 0.0478(4) Uani 1 1 d . . . O3 O 0.13281(10) 0.60012(15) 0.47610(13) 0.0465(4) Uani 1 1 d . . . H3 H 0.1763 0.5963 0.5403 0.070 Uiso 1 1 calc R . . O4 O 0.38564(13) 0.77359(17) 0.87551(16) 0.0563(5) Uani 1 1 d . . . N1 N 0.5000 0.93580(18) 0.7500 0.0241(4) Uani 1 2 d S . . N2 N 0.5000 1.57285(19) 0.7500 0.0279(5) Uani 1 2 d S . . N3 N 0.23347(16) 0.7181(3) 0.8600(3) 0.0735(7) Uani 1 1 d . . . C1 C 0.25065(14) 0.73362(17) 0.44029(18) 0.0307(4) Uani 1 1 d . . . C2 C 0.15864(13) 0.67642(18) 0.40120(18) 0.0331(4) Uani 1 1 d . . . C3 C 0.09395(13) 0.6980(2) 0.28824(18) 0.0358(5) Uani 1 1 d . . . C4 C 0.11975(14) 0.7797(2) 0.21041(18) 0.0372(5) Uani 1 1 d . . . C5 C 0.05922(16) 0.8051(3) 0.0919(2) 0.0510(6) Uani 1 1 d . . . H5 H 0.0005 0.7653 0.0623 0.061 Uiso 1 1 calc R . . C6 C 0.08542(19) 0.8862(3) 0.0212(2) 0.0636(7) Uani 1 1 d . . . H6 H 0.0436 0.9025 -0.0551 0.076 Uiso 1 1 calc R . . C7 C 0.1743(2) 0.9461(3) 0.0607(2) 0.0650(8) Uani 1 1 d . . . H7 H 0.1913 1.0011 0.0109 0.078 Uiso 1 1 calc R . . C8 C 0.23535(17) 0.9228(2) 0.1726(2) 0.0536(6) Uani 1 1 d . . . H8 H 0.2945 0.9620 0.1988 0.064 Uiso 1 1 calc R . . C9 C 0.21030(14) 0.84007(19) 0.24990(19) 0.0381(5) Uani 1 1 d . . . C10 C 0.27395(14) 0.81421(19) 0.36553(18) 0.0355(5) Uani 1 1 d . . . H10 H 0.3332 0.8530 0.3915 0.043 Uiso 1 1 calc R . . C11 C 0.0000 0.6272(3) 0.2500 0.0418(7) Uani 1 2 d S . . H11A H -0.0008 0.5752 0.3163 0.050 Uiso 0.50 1 calc PR . . H11B H 0.0008 0.5752 0.1837 0.050 Uiso 0.50 1 calc PR . . C12 C 0.32036(13) 0.70522(18) 0.56179(17) 0.0314(4) Uani 1 1 d . . . C13 C 0.51995(13) 0.99867(16) 0.85247(16) 0.0282(4) Uani 1 1 d . . . H13 H 0.5343 0.9564 0.9245 0.034 Uiso 1 1 calc R . . C14 C 0.52029(14) 1.12281(16) 0.85644(16) 0.0292(4) Uani 1 1 d . . . H14 H 0.5340 1.1627 0.9297 0.035 Uiso 1 1 calc R . . C15 C 0.5000 1.1882(2) 0.7500 0.0262(5) Uani 1 2 d S . . C16 C 0.5000 1.3215(2) 0.7500 0.0274(6) Uani 1 2 d S . . C17 C 0.47079(15) 1.38691(17) 0.83369(18) 0.0348(4) Uani 1 1 d . . . H17 H 0.4512 1.3471 0.8919 0.042 Uiso 1 1 calc R . . C18 C 0.47112(15) 1.51109(18) 0.82976(18) 0.0353(4) Uani 1 1 d . . . H18 H 0.4502 1.5537 0.8853 0.042 Uiso 1 1 calc R . . C19 C 0.2657(3) 0.6455(4) 0.9690(4) 0.1174(15) Uani 1 1 d . . . H19A H 0.3206 0.6833 1.0252 0.176 Uiso 1 1 calc R . . H19B H 0.2832 0.5664 0.9495 0.176 Uiso 1 1 calc R . . H19C H 0.2147 0.6391 1.0039 0.176 Uiso 1 1 calc R . . C20 C 0.1350(3) 0.7087(7) 0.7849(5) 0.183(3) Uani 1 1 d . . . H20A H 0.1204 0.7736 0.7278 0.274 Uiso 1 1 calc R . . H20B H 0.0933 0.7133 0.8338 0.274 Uiso 1 1 calc R . . H20C H 0.1254 0.6329 0.7431 0.274 Uiso 1 1 calc R . . C21 C 0.2986(2) 0.7777(3) 0.8250(2) 0.0565(7) Uani 1 1 d . . . H21 H 0.2766 0.8261 0.7571 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0263(2) 0.01389(19) 0.0328(2) 0.000 -0.00707(14) 0.000 O1 0.0293(8) 0.0258(7) 0.0390(8) 0.0003(5) -0.0095(6) -0.0037(5) O2 0.0341(8) 0.0608(11) 0.0383(8) 0.0102(8) -0.0032(6) -0.0077(7) O3 0.0289(7) 0.0562(10) 0.0437(8) 0.0130(8) -0.0040(6) -0.0077(7) O4 0.0513(11) 0.0697(12) 0.0449(9) -0.0077(8) 0.0107(8) -0.0201(9) N1 0.0266(11) 0.0169(10) 0.0268(11) 0.000 0.0054(9) 0.000 N2 0.0271(11) 0.0175(10) 0.0321(11) 0.000 -0.0007(9) 0.000 N3 0.0392(12) 0.1015(19) 0.0778(17) -0.0290(16) 0.0155(12) -0.0095(13) C1 0.0232(9) 0.0305(10) 0.0322(10) -0.0052(8) -0.0002(8) 0.0035(7) C2 0.0243(10) 0.0343(11) 0.0359(11) 0.0014(8) 0.0024(8) 0.0023(8) C3 0.0219(9) 0.0398(11) 0.0379(11) -0.0012(9) -0.0020(8) 0.0020(9) C4 0.0274(10) 0.0444(12) 0.0341(11) 0.0009(9) 0.0015(8) 0.0079(9) C5 0.0325(11) 0.0706(17) 0.0401(12) 0.0062(12) -0.0027(10) 0.0029(11) C6 0.0526(15) 0.088(2) 0.0408(13) 0.0208(14) 0.0014(11) 0.0099(14) C7 0.0577(16) 0.080(2) 0.0562(15) 0.0286(15) 0.0154(13) 0.0036(14) C8 0.0421(13) 0.0618(16) 0.0548(14) 0.0147(12) 0.0120(11) -0.0015(11) C9 0.0289(10) 0.0420(12) 0.0398(11) 0.0039(9) 0.0054(9) 0.0044(9) C10 0.0231(9) 0.0378(11) 0.0398(11) -0.0015(9) 0.0016(8) -0.0002(8) C11 0.0248(14) 0.0406(17) 0.0484(17) 0.000 -0.0053(12) 0.000 C12 0.0261(10) 0.0274(10) 0.0336(10) -0.0059(9) -0.0011(8) 0.0030(8) C13 0.0347(10) 0.0217(9) 0.0256(9) 0.0017(7) 0.0056(8) -0.0003(8) C14 0.0387(11) 0.0216(9) 0.0252(9) -0.0027(7) 0.0070(8) -0.0008(8) C15 0.0309(14) 0.0178(13) 0.0291(13) 0.000 0.0083(11) 0.000 C16 0.0302(14) 0.0192(13) 0.0302(14) 0.000 0.0055(11) 0.000 C17 0.0479(12) 0.0221(10) 0.0376(10) -0.0004(8) 0.0177(9) -0.0015(9) C18 0.0448(12) 0.0232(10) 0.0389(11) -0.0048(8) 0.0146(9) 0.0017(9) C19 0.111(3) 0.112(3) 0.145(4) 0.034(3) 0.063(3) -0.026(3) C20 0.0382(19) 0.357(9) 0.143(5) -0.111(5) 0.014(2) -0.022(3) C21 0.0634(18) 0.0563(15) 0.0429(14) -0.0032(12) 0.0068(12) 0.0057(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9740(14) 2_656 ? Cu1 O1 1.9740(14) . ? Cu1 N2 1.996(2) 1_545 ? Cu1 N1 2.026(2) . ? O1 C12 1.270(2) . ? O2 C12 1.250(3) . ? O3 C2 1.355(2) . ? O3 H3 0.8200 . ? O4 C21 1.226(3) . ? N1 C13 1.339(2) . ? N1 C13 1.339(2) 2_656 ? N2 C18 1.330(2) . ? N2 C18 1.330(2) 2_656 ? N2 Cu1 1.996(2) 1_565 ? N3 C21 1.325(4) . ? N3 C20 1.438(5) . ? N3 C19 1.457(5) . ? C1 C10 1.367(3) . ? C1 C2 1.428(3) . ? C1 C12 1.503(3) . ? C2 C3 1.386(3) . ? C3 C4 1.417(3) . ? C3 C11 1.523(3) . ? C4 C5 1.422(3) . ? C4 C9 1.426(3) . ? C5 C6 1.356(4) . ? C5 H5 0.9300 . ? C6 C7 1.403(4) . ? C6 H6 0.9300 . ? C7 C8 1.361(3) . ? C7 H7 0.9300 . ? C8 C9 1.415(3) . ? C8 H8 0.9300 . ? C9 C10 1.413(3) . ? C10 H10 0.9300 . ? C11 C3 1.523(3) 2 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C14 1.376(3) . ? C13 H13 0.9300 . ? C14 C15 1.392(2) . ? C14 H14 0.9300 . ? C15 C14 1.392(2) 2_656 ? C15 C16 1.477(4) . ? C16 C17 1.390(2) 2_656 ? C16 C17 1.390(2) . ? C17 C18 1.377(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 176.24(7) 2_656 . ? O1 Cu1 N2 91.88(4) 2_656 1_545 ? O1 Cu1 N2 91.88(4) . 1_545 ? O1 Cu1 N1 88.12(4) 2_656 . ? O1 Cu1 N1 88.12(4) . . ? N2 Cu1 N1 180.000(1) 1_545 . ? C12 O1 Cu1 125.54(13) . . ? C2 O3 H3 109.5 . . ? C13 N1 C13 117.3(2) . 2_656 ? C13 N1 Cu1 121.34(11) . . ? C13 N1 Cu1 121.34(11) 2_656 . ? C18 N2 C18 118.0(2) . 2_656 ? C18 N2 Cu1 120.98(11) . 1_565 ? C18 N2 Cu1 120.98(11) 2_656 1_565 ? C21 N3 C20 121.7(4) . . ? C21 N3 C19 118.6(3) . . ? C20 N3 C19 119.0(4) . . ? C10 C1 C2 118.93(18) . . ? C10 C1 C12 120.85(18) . . ? C2 C1 C12 120.22(18) . . ? O3 C2 C3 118.75(17) . . ? O3 C2 C1 119.70(17) . . ? C3 C2 C1 121.55(19) . . ? C2 C3 C4 119.03(18) . . ? C2 C3 C11 118.39(18) . . ? C4 C3 C11 122.49(16) . . ? C3 C4 C5 123.0(2) . . ? C3 C4 C9 119.89(18) . . ? C5 C4 C9 117.1(2) . . ? C6 C5 C4 121.3(2) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 121.5(2) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 119.3(2) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 121.3(2) . . ? C10 C9 C4 118.85(19) . . ? C8 C9 C4 119.79(19) . . ? C1 C10 C9 121.71(18) . . ? C1 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C3 C11 C3 118.0(3) . 2 ? C3 C11 H11A 107.8 . . ? C3 C11 H11A 107.8 2 . ? C3 C11 H11B 107.8 . . ? C3 C11 H11B 107.8 2 . ? H11A C11 H11B 107.1 . . ? O2 C12 O1 124.43(17) . . ? O2 C12 C1 118.66(17) . . ? O1 C12 C1 116.92(18) . . ? N1 C13 C14 123.21(17) . . ? N1 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C15 119.51(17) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C14 117.3(2) 2_656 . ? C14 C15 C16 121.37(12) 2_656 . ? C14 C15 C16 121.37(12) . . ? C17 C16 C17 117.2(2) 2_656 . ? C17 C16 C15 121.41(12) 2_656 . ? C17 C16 C15 121.41(12) . . ? C18 C17 C16 119.48(19) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? N2 C18 C17 122.90(19) . . ? N2 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 N3 124.8(3) . . ? O4 C21 H21 117.6 . . ? N3 C21 H21 117.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 O1 C12 53.24(15) 1_545 . . . ? N1 Cu1 O1 C12 -126.76(15) . . . . ? O1 Cu1 N1 C13 -30.12(11) 2_656 . . . ? O1 Cu1 N1 C13 149.88(11) . . . . ? O1 Cu1 N1 C13 149.88(11) 2_656 . . 2_656 ? O1 Cu1 N1 C13 -30.12(11) . . . 2_656 ? C10 C1 C2 O3 -177.28(18) . . . . ? C12 C1 C2 O3 2.7(3) . . . . ? C10 C1 C2 C3 2.0(3) . . . . ? C12 C1 C2 C3 -178.03(18) . . . . ? O3 C2 C3 C4 178.71(19) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? O3 C2 C3 C11 -4.8(3) . . . . ? C1 C2 C3 C11 175.95(18) . . . . ? C2 C3 C4 C5 178.3(2) . . . . ? C11 C3 C4 C5 2.0(3) . . . . ? C2 C3 C4 C9 -1.3(3) . . . . ? C11 C3 C4 C9 -177.71(19) . . . . ? C3 C4 C5 C6 178.3(3) . . . . ? C9 C4 C5 C6 -2.1(4) . . . . ? C4 C5 C6 C7 1.7(4) . . . . ? C5 C6 C7 C8 -0.4(5) . . . . ? C6 C7 C8 C9 -0.5(4) . . . . ? C7 C8 C9 C10 179.1(2) . . . . ? C7 C8 C9 C4 0.0(4) . . . . ? C3 C4 C9 C10 1.8(3) . . . . ? C5 C4 C9 C10 -177.9(2) . . . . ? C3 C4 C9 C8 -179.1(2) . . . . ? C5 C4 C9 C8 1.2(3) . . . . ? C2 C1 C10 C9 -1.5(3) . . . . ? C12 C1 C10 C9 178.53(18) . . . . ? C8 C9 C10 C1 -179.4(2) . . . . ? C4 C9 C10 C1 -0.4(3) . . . . ? C2 C3 C11 C3 123.6(2) . . . 2 ? C4 C3 C11 C3 -59.99(18) . . . 2 ? Cu1 O1 C12 O2 -7.4(3) . . . . ? Cu1 O1 C12 C1 172.76(12) . . . . ? C10 C1 C12 O2 179.81(19) . . . . ? C2 C1 C12 O2 -0.2(3) . . . . ? C10 C1 C12 O1 -0.4(3) . . . . ? C2 C1 C12 O1 179.63(17) . . . . ? C13 N1 C13 C14 0.32(14) 2_656 . . . ? Cu1 N1 C13 C14 -179.68(14) . . . . ? N1 C13 C14 C15 -0.6(3) . . . . ? C13 C14 C15 C14 0.29(13) . . . 2_656 ? C13 C14 C15 C16 -179.71(13) . . . . ? C14 C15 C16 C17 -33.74(14) 2_656 . . 2_656 ? C14 C15 C16 C17 146.26(14) . . . 2_656 ? C14 C15 C16 C17 146.26(14) 2_656 . . . ? C14 C15 C16 C17 -33.74(14) . . . . ? C17 C16 C17 C18 0.57(14) 2_656 . . . ? C15 C16 C17 C18 -179.43(14) . . . . ? C18 N2 C18 C17 0.62(15) 2_656 . . . ? Cu1 N2 C18 C17 -179.38(15) 1_565 . . . ? C16 C17 C18 N2 -1.2(3) . . . . ? C20 N3 C21 O4 -168.1(4) . . . . ? C19 N3 C21 O4 2.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.639 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.048 #===END data_12 _database_code_depnum_ccdc_archive 'CCDC 631551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H32 Cd N4 O7' _chemical_formula_weight 829.13 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6265(13) _cell_length_b 16.8941(16) _cell_length_c 19.4796(18) _cell_angle_alpha 90.00 _cell_angle_beta 107.2390(10) _cell_angle_gamma 90.00 _cell_volume 4282.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5841 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 21.45 _exptl_crystal_description Block _exptl_crystal_colour Pale-Yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.650794 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'APEX II 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 22734 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7568 _reflns_number_gt 4982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.1311P)^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 7568 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1772 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.23851(3) 0.17139(2) 0.16233(2) 0.05528(19) Uani 1 1 d . . . O1W O 0.3041(14) 0.4975(11) 0.0802(11) 0.413(10) Uiso 1 1 d . . . H1WA H 0.2556 0.4891 0.0418 0.619 Uiso 1 1 d R . . H1WB H 0.3088 0.4643 0.1146 0.619 Uiso 1 1 d R . . O1 O 0.1991(3) 0.2468(2) 0.0425(2) 0.0687(11) Uani 1 1 d . . . O2 O 0.1108(3) 0.1431(3) 0.0572(2) 0.0682(11) Uani 1 1 d . . . O3 O -0.0647(3) 0.1134(2) -0.0232(2) 0.0718(12) Uani 1 1 d . . . H3 H -0.0252 0.1154 0.0177 0.108 Uiso 1 1 calc R . . O4 O -0.4302(3) 0.1799(2) -0.2346(2) 0.0710(12) Uani 1 1 d . . . H4 H -0.4883 0.1852 -0.2623 0.107 Uiso 1 1 calc R . . O5 O -0.6099(3) 0.2390(3) -0.2831(2) 0.0765(12) Uani 1 1 d . . . O6 O -0.6682(4) 0.3189(3) -0.2160(3) 0.0861(14) Uani 1 1 d . . . N1 N -0.1740(3) 0.5549(3) 0.2929(2) 0.0608(12) Uani 1 1 d . . . N2 N 0.1196(4) 0.2632(3) 0.1839(3) 0.0654(12) Uani 1 1 d . . . N3 N 0.3677(3) 0.1032(3) 0.1323(3) 0.0642(12) Uani 1 1 d . . . N4 N 0.7989(5) -0.0909(4) 0.0740(4) 0.0915(17) Uani 1 1 d . . . C1 C 0.0329(4) 0.2971(4) -0.0752(3) 0.0590(14) Uani 1 1 d . . . H1 H 0.0918 0.3282 -0.0619 0.071 Uiso 1 1 calc R . . C2 C 0.0311(4) 0.2283(3) -0.0388(3) 0.0533(13) Uani 1 1 d . . . C3 C -0.0603(4) 0.1826(3) -0.0577(3) 0.0554(14) Uani 1 1 d . . . C4 C -0.1478(4) 0.2073(3) -0.1114(3) 0.0574(13) Uani 1 1 d . . . C5 C -0.1424(4) 0.2765(3) -0.1507(3) 0.0596(14) Uani 1 1 d . . . C6 C -0.2243(5) 0.3018(4) -0.2103(3) 0.0742(17) Uani 1 1 d . . . H6 H -0.2848 0.2726 -0.2240 0.089 Uiso 1 1 calc R . . C7 C -0.2159(6) 0.3688(4) -0.2484(4) 0.089(2) Uani 1 1 d . . . H7 H -0.2711 0.3846 -0.2869 0.107 Uiso 1 1 calc R . . C8 C -0.1277(6) 0.4122(4) -0.2303(4) 0.096(2) Uani 1 1 d . . . H8 H -0.1220 0.4558 -0.2579 0.115 Uiso 1 1 calc R . . C9 C -0.0470(6) 0.3920(4) -0.1713(4) 0.085(2) Uani 1 1 d . . . H9 H 0.0107 0.4243 -0.1573 0.102 Uiso 1 1 calc R . . C10 C -0.0512(5) 0.3224(3) -0.1320(3) 0.0602(14) Uani 1 1 d . . . C11 C 0.1202(4) 0.2048(4) 0.0221(3) 0.0571(13) Uani 1 1 d . . . C12 C -0.2464(4) 0.1575(3) -0.1258(3) 0.0637(15) Uani 1 1 d . . . H12A H -0.2657 0.1391 -0.1752 0.076 Uiso 1 1 calc R . . H12B H -0.2319 0.1112 -0.0949 0.076 Uiso 1 1 calc R . . C13 C -0.3366(4) 0.2015(3) -0.1134(3) 0.0567(14) Uani 1 1 d . . . C14 C -0.4263(4) 0.2114(3) -0.1696(3) 0.0547(13) Uani 1 1 d . . . C15 C -0.5109(4) 0.2557(3) -0.1611(3) 0.0597(14) Uani 1 1 d . . . C16 C -0.5067(5) 0.2851(4) -0.0955(3) 0.0714(17) Uani 1 1 d . . . H16 H -0.5628 0.3130 -0.0902 0.086 Uiso 1 1 calc R . . C17 C -0.4196(5) 0.2748(3) -0.0350(3) 0.0684(16) Uani 1 1 d . . . C18 C -0.4171(6) 0.3036(5) 0.0331(4) 0.089(2) Uani 1 1 d . . . H18 H -0.4743 0.3300 0.0384 0.107 Uiso 1 1 calc R . . C19 C -0.3328(7) 0.2940(5) 0.0921(4) 0.099(2) Uani 1 1 d . . . H19 H -0.3309 0.3152 0.1366 0.118 Uiso 1 1 calc R . . C20 C -0.2478(6) 0.2502(4) 0.0826(3) 0.087(2) Uani 1 1 d . . . H20 H -0.1909 0.2411 0.1221 0.105 Uiso 1 1 calc R . . C21 C -0.2479(5) 0.2219(4) 0.0187(3) 0.0697(17) Uani 1 1 d . . . H21 H -0.1905 0.1944 0.0150 0.084 Uiso 1 1 calc R . . C22 C -0.3335(4) 0.2325(3) -0.0443(3) 0.0610(15) Uani 1 1 d . . . C23 C -0.6027(4) 0.2723(4) -0.2235(3) 0.0653(16) Uani 1 1 d . . . C24 C 0.4176(5) 0.1338(4) 0.0908(4) 0.0831(19) Uani 1 1 d . . . H24 H 0.3941 0.1816 0.0684 0.100 Uiso 1 1 calc R . . C25 C 0.5019(5) 0.1004(4) 0.0779(4) 0.0814(19) Uani 1 1 d . . . H25 H 0.5349 0.1265 0.0490 0.098 Uiso 1 1 calc R . . C26 C 0.5384(4) 0.0275(3) 0.1080(3) 0.0583(14) Uani 1 1 d . . . C27 C 0.4839(5) -0.0048(4) 0.1507(4) 0.085(2) Uani 1 1 d . . . H27 H 0.5039 -0.0536 0.1724 0.102 Uiso 1 1 calc R . . C28 C 0.4021(5) 0.0326(4) 0.1619(4) 0.084(2) Uani 1 1 d . . . H28 H 0.3682 0.0085 0.1913 0.101 Uiso 1 1 calc R . . C29 C 0.6290(4) -0.0127(3) 0.0962(3) 0.0588(14) Uani 1 1 d . . . C30 C 0.6949(5) 0.0231(4) 0.0663(4) 0.0753(17) Uani 1 1 d . . . H30 H 0.6847 0.0760 0.0528 0.090 Uiso 1 1 calc R . . C31 C 0.7770(5) -0.0171(4) 0.0552(4) 0.0845(19) Uani 1 1 d . . . H31 H 0.8191 0.0097 0.0331 0.101 Uiso 1 1 calc R . . C32 C 0.7346(7) -0.1260(4) 0.1009(6) 0.127(4) Uani 1 1 d . . . H32 H 0.7454 -0.1794 0.1121 0.152 Uiso 1 1 calc R . . C33 C 0.6503(6) -0.0900(4) 0.1144(5) 0.109(3) Uani 1 1 d . . . H33 H 0.6088 -0.1185 0.1358 0.130 Uiso 1 1 calc R . . C34 C 0.0743(6) 0.3220(4) 0.1409(4) 0.089(2) Uani 1 1 d . . . H34 H 0.0872 0.3269 0.0968 0.107 Uiso 1 1 calc R . . C35 C 0.0110(6) 0.3750(4) 0.1572(4) 0.095(2) Uani 1 1 d . . . H35 H -0.0190 0.4142 0.1241 0.114 Uiso 1 1 calc R . . C36 C -0.0102(4) 0.3723(3) 0.2219(3) 0.0593(14) Uani 1 1 d . . . C37 C 0.0318(6) 0.3093(4) 0.2649(4) 0.085(2) Uani 1 1 d . . . H37 H 0.0177 0.3019 0.3083 0.102 Uiso 1 1 calc R . . C38 C 0.0948(6) 0.2571(4) 0.2437(4) 0.0826(19) Uani 1 1 d . . . H38 H 0.1215 0.2146 0.2739 0.099 Uiso 1 1 calc R . . C39 C -0.0712(4) 0.4329(3) 0.2458(3) 0.0573(13) Uani 1 1 d . . . C40 C -0.1518(5) 0.4741(4) 0.1987(3) 0.0691(16) Uani 1 1 d . . . H40 H -0.1725 0.4616 0.1500 0.083 Uiso 1 1 calc R . . C41 C -0.2005(5) 0.5327(4) 0.2240(3) 0.0678(16) Uani 1 1 d . . . H41 H -0.2550 0.5586 0.1916 0.081 Uiso 1 1 calc R . . C42 C -0.1005(5) 0.5140(4) 0.3374(3) 0.0680(16) Uani 1 1 d . . . H42 H -0.0824 0.5270 0.3859 0.082 Uiso 1 1 calc R . . C43 C -0.0481(4) 0.4530(3) 0.3167(3) 0.0635(15) Uani 1 1 d . . . H43 H 0.0027 0.4256 0.3509 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0378(2) 0.0659(3) 0.0570(3) -0.00454(18) 0.00605(18) -0.00023(17) O1 0.046(2) 0.085(3) 0.067(2) -0.006(2) 0.0048(18) -0.002(2) O2 0.054(2) 0.078(3) 0.061(2) 0.006(2) -0.0009(19) 0.001(2) O3 0.054(2) 0.079(3) 0.067(2) 0.019(2) -0.0065(19) 0.0013(19) O4 0.056(2) 0.081(3) 0.061(2) -0.004(2) -0.0058(19) 0.006(2) O5 0.049(2) 0.093(3) 0.072(3) 0.006(2) -0.005(2) 0.003(2) O6 0.060(3) 0.101(3) 0.082(3) 0.009(2) -0.002(2) 0.022(3) N1 0.051(3) 0.068(3) 0.060(3) -0.001(2) 0.012(2) 0.005(2) N2 0.063(3) 0.072(3) 0.062(3) -0.009(2) 0.021(2) 0.002(2) N3 0.049(3) 0.072(3) 0.070(3) -0.004(2) 0.016(2) -0.006(2) N4 0.075(4) 0.095(4) 0.113(5) -0.011(4) 0.042(4) 0.008(4) C1 0.047(3) 0.072(3) 0.058(3) -0.008(3) 0.014(2) -0.007(3) C2 0.041(3) 0.063(3) 0.053(3) 0.000(3) 0.010(2) 0.004(2) C3 0.049(3) 0.060(3) 0.052(3) 0.005(2) 0.007(2) 0.001(2) C4 0.046(3) 0.065(3) 0.056(3) 0.000(3) 0.006(2) 0.001(3) C5 0.052(3) 0.066(3) 0.057(3) 0.007(3) 0.011(3) 0.004(3) C6 0.058(4) 0.092(4) 0.066(4) 0.021(3) 0.008(3) 0.000(3) C7 0.086(5) 0.098(5) 0.071(4) 0.030(4) 0.006(4) 0.001(4) C8 0.094(5) 0.092(5) 0.095(5) 0.043(4) 0.018(4) -0.012(4) C9 0.076(4) 0.093(5) 0.084(4) 0.023(4) 0.021(4) -0.007(4) C10 0.059(3) 0.065(3) 0.056(3) 0.005(3) 0.015(3) 0.001(3) C11 0.049(3) 0.065(3) 0.054(3) -0.005(3) 0.010(3) 0.005(3) C12 0.050(3) 0.064(3) 0.063(3) 0.008(3) -0.003(3) -0.002(3) C13 0.044(3) 0.057(3) 0.062(3) 0.011(3) 0.006(2) -0.007(2) C14 0.045(3) 0.058(3) 0.052(3) 0.006(3) 0.000(2) -0.007(3) C15 0.052(3) 0.058(3) 0.060(3) 0.008(3) 0.001(3) -0.005(3) C16 0.062(4) 0.070(4) 0.074(4) 0.008(3) 0.008(3) 0.003(3) C17 0.066(4) 0.069(4) 0.064(4) 0.004(3) 0.010(3) -0.001(3) C18 0.087(5) 0.099(5) 0.078(5) -0.017(4) 0.020(4) -0.001(4) C19 0.114(7) 0.115(6) 0.057(4) 0.000(4) 0.010(4) -0.006(5) C20 0.078(5) 0.109(6) 0.061(4) 0.010(4) -0.001(4) -0.026(4) C21 0.063(4) 0.082(4) 0.055(3) 0.011(3) 0.004(3) -0.009(3) C22 0.054(3) 0.065(3) 0.057(3) 0.011(3) 0.007(3) -0.010(3) C23 0.047(3) 0.067(4) 0.070(4) 0.009(3) -0.001(3) -0.005(3) C24 0.082(5) 0.077(4) 0.099(5) 0.024(4) 0.040(4) 0.023(4) C25 0.078(4) 0.075(4) 0.108(5) 0.022(4) 0.052(4) 0.017(4) C26 0.051(3) 0.059(3) 0.064(3) -0.006(3) 0.016(3) -0.007(3) C27 0.080(5) 0.064(4) 0.119(6) 0.020(4) 0.044(4) 0.011(3) C28 0.082(5) 0.064(4) 0.124(6) 0.018(4) 0.058(4) 0.006(4) C29 0.050(3) 0.057(3) 0.066(3) -0.007(3) 0.013(3) -0.002(3) C30 0.067(4) 0.069(4) 0.097(5) 0.010(3) 0.035(4) 0.002(3) C31 0.069(4) 0.095(5) 0.099(5) 0.005(4) 0.038(4) 0.006(4) C32 0.100(6) 0.066(5) 0.236(12) 0.029(6) 0.084(7) 0.030(4) C33 0.096(6) 0.075(5) 0.180(9) 0.039(5) 0.079(6) 0.013(4) C34 0.122(6) 0.085(5) 0.072(4) 0.013(4) 0.045(4) 0.044(4) C35 0.125(6) 0.092(5) 0.069(4) 0.017(4) 0.030(4) 0.042(5) C36 0.053(3) 0.061(3) 0.065(3) -0.006(3) 0.020(3) -0.001(3) C37 0.110(6) 0.076(4) 0.088(5) 0.023(4) 0.061(4) 0.033(4) C38 0.098(5) 0.081(4) 0.079(4) 0.020(4) 0.042(4) 0.030(4) C39 0.050(3) 0.056(3) 0.067(3) 0.003(3) 0.021(3) -0.002(3) C40 0.063(4) 0.079(4) 0.060(3) -0.010(3) 0.010(3) 0.003(3) C41 0.059(4) 0.073(4) 0.063(4) -0.002(3) 0.006(3) 0.011(3) C42 0.069(4) 0.077(4) 0.054(3) -0.001(3) 0.012(3) 0.019(3) C43 0.058(3) 0.069(4) 0.060(3) 0.001(3) 0.011(3) 0.009(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 Cd1 O2 2.310(4) . ? Cd1 N3 2.319(5) . ? Cd1 O6 2.339(5) 4_666 ? Cd1 N2 2.369(5) . ? Cd1 N1 2.421(5) 2_545 ? Cd1 O5 2.528(4) 4_666 ? Cd1 O1 2.572(4) . ? O1W H1WA 0.8502 . ? O1W H1WB 0.8617 . ? O1 C11 1.250(7) . ? O2 C11 1.273(7) . ? O3 C3 1.358(6) . ? O3 H3 0.8200 . ? O4 C14 1.360(7) . ? O4 H4 0.8200 . ? O5 C23 1.267(7) . ? O5 Cd1 2.528(4) 4_465 ? O6 C23 1.231(8) . ? O6 Cd1 2.339(5) 4_465 ? N1 C42 1.311(7) . ? N1 C41 1.336(7) . ? N1 Cd1 2.421(5) 2 ? N2 C38 1.310(8) . ? N2 C34 1.328(8) . ? N3 C24 1.307(8) . ? N3 C28 1.347(8) . ? N4 C32 1.291(10) . ? N4 C31 1.308(8) . ? C1 C2 1.365(8) . ? C1 C10 1.404(8) . ? C1 H1 0.9300 . ? C2 C3 1.419(7) . ? C2 C11 1.478(7) . ? C3 C4 1.396(7) . ? C4 C5 1.412(8) . ? C4 C12 1.538(8) . ? C5 C6 1.417(7) . ? C5 C10 1.417(8) . ? C6 C7 1.376(9) . ? C6 H6 0.9300 . ? C7 C8 1.362(10) . ? C7 H7 0.9300 . ? C8 C9 1.377(9) . ? C8 H8 0.9300 . ? C9 C10 1.413(8) . ? C9 H9 0.9300 . ? C12 C13 1.517(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.388(7) . ? C13 C22 1.431(8) . ? C14 C15 1.426(8) . ? C15 C16 1.356(8) . ? C15 C23 1.490(7) . ? C16 C17 1.413(8) . ? C16 H16 0.9300 . ? C17 C18 1.404(9) . ? C17 C22 1.432(9) . ? C18 C19 1.373(10) . ? C18 H18 0.9300 . ? C19 C20 1.432(11) . ? C19 H19 0.9300 . ? C20 C21 1.332(9) . ? C20 H20 0.9300 . ? C21 C22 1.433(7) . ? C21 H21 0.9300 . ? C24 C25 1.368(9) . ? C24 H24 0.9300 . ? C25 C26 1.390(8) . ? C25 H25 0.9300 . ? C26 C27 1.381(8) . ? C26 C29 1.486(8) . ? C27 C28 1.354(9) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.349(8) . ? C29 C33 1.361(8) . ? C30 C31 1.379(9) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.393(11) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.346(9) . ? C34 H34 0.9300 . ? C35 C36 1.375(9) . ? C35 H35 0.9300 . ? C36 C37 1.369(8) . ? C36 C39 1.478(8) . ? C37 C38 1.378(9) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C43 1.364(8) . ? C39 C40 1.392(8) . ? C40 C41 1.362(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.381(8) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 N3 95.88(15) . . ? O2 Cd1 O6 162.31(17) . 4_666 ? N3 Cd1 O6 93.74(17) . 4_666 ? O2 Cd1 N2 85.29(15) . . ? N3 Cd1 N2 168.58(18) . . ? O6 Cd1 N2 88.21(17) 4_666 . ? O2 Cd1 N1 83.85(15) . 2_545 ? N3 Cd1 N1 94.08(16) . 2_545 ? O6 Cd1 N1 80.68(16) 4_666 2_545 ? N2 Cd1 N1 97.35(17) . 2_545 ? O2 Cd1 O5 143.50(15) . 4_666 ? N3 Cd1 O5 79.44(15) . 4_666 ? O6 Cd1 O5 53.19(16) 4_666 4_666 ? N2 Cd1 O5 92.84(15) . 4_666 ? N1 Cd1 O5 132.37(15) 2_545 4_666 ? O2 Cd1 O1 52.99(13) . . ? N3 Cd1 O1 89.27(15) . . ? O6 Cd1 O1 142.12(14) 4_666 . ? N2 Cd1 O1 82.35(15) . . ? N1 Cd1 O1 136.80(13) 2_545 . ? O5 Cd1 O1 90.59(14) 4_666 . ? H1WA O1W H1WB 115.8 . . ? C11 O1 Cd1 86.3(3) . . ? C11 O2 Cd1 97.9(3) . . ? C3 O3 H3 109.5 . . ? C14 O4 H4 109.5 . . ? C23 O5 Cd1 87.2(3) . 4_465 ? C23 O6 Cd1 96.9(4) . 4_465 ? C42 N1 C41 116.3(5) . . ? C42 N1 Cd1 118.5(4) . 2 ? C41 N1 Cd1 124.9(4) . 2 ? C38 N2 C34 115.3(6) . . ? C38 N2 Cd1 118.4(4) . . ? C34 N2 Cd1 126.3(4) . . ? C24 N3 C28 115.8(6) . . ? C24 N3 Cd1 122.2(4) . . ? C28 N3 Cd1 121.7(4) . . ? C32 N4 C31 115.2(6) . . ? C2 C1 C10 122.2(5) . . ? C2 C1 H1 118.9 . . ? C10 C1 H1 118.9 . . ? C1 C2 C3 118.5(5) . . ? C1 C2 C11 120.6(5) . . ? C3 C2 C11 120.8(5) . . ? O3 C3 C4 118.3(5) . . ? O3 C3 C2 120.3(4) . . ? C4 C3 C2 121.5(5) . . ? C3 C4 C5 118.9(5) . . ? C3 C4 C12 118.7(5) . . ? C5 C4 C12 122.5(4) . . ? C4 C5 C6 122.7(5) . . ? C4 C5 C10 119.8(5) . . ? C6 C5 C10 117.6(5) . . ? C7 C6 C5 121.3(6) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C6 120.7(6) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 120.5(6) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 120.5(6) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C1 C10 C9 121.7(6) . . ? C1 C10 C5 119.0(5) . . ? C9 C10 C5 119.3(5) . . ? O1 C11 O2 120.5(5) . . ? O1 C11 C2 121.7(5) . . ? O2 C11 C2 117.5(5) . . ? C13 C12 C4 114.1(5) . . ? C13 C12 H12A 108.7 . . ? C4 C12 H12A 108.7 . . ? C13 C12 H12B 108.7 . . ? C4 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C22 118.1(5) . . ? C14 C13 C12 119.9(5) . . ? C22 C13 C12 122.0(5) . . ? O4 C14 C13 118.1(5) . . ? O4 C14 C15 120.2(4) . . ? C13 C14 C15 121.7(5) . . ? C16 C15 C14 119.5(5) . . ? C16 C15 C23 119.4(6) . . ? C14 C15 C23 121.1(5) . . ? C15 C16 C17 122.1(6) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 121.7(7) . . ? C18 C17 C22 120.1(6) . . ? C16 C17 C22 118.2(6) . . ? C19 C18 C17 122.1(8) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 117.4(7) . . ? C18 C19 H19 121.3 . . ? C20 C19 H19 121.3 . . ? C21 C20 C19 122.0(6) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 122.1(7) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C13 C22 C17 120.3(5) . . ? C13 C22 C21 123.3(6) . . ? C17 C22 C21 116.3(6) . . ? O6 C23 O5 122.0(5) . . ? O6 C23 C15 119.1(6) . . ? O5 C23 C15 118.8(6) . . ? N3 C24 C25 124.7(6) . . ? N3 C24 H24 117.6 . . ? C25 C24 H24 117.6 . . ? C24 C25 C26 120.2(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 114.5(6) . . ? C27 C26 C29 122.2(5) . . ? C25 C26 C29 123.4(5) . . ? C28 C27 C26 121.9(6) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? N3 C28 C27 122.9(6) . . ? N3 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C30 C29 C33 115.2(6) . . ? C30 C29 C26 123.5(5) . . ? C33 C29 C26 121.4(6) . . ? C29 C30 C31 121.4(6) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? N4 C31 C30 123.5(7) . . ? N4 C31 H31 118.2 . . ? C30 C31 H31 118.2 . . ? N4 C32 C33 124.9(7) . . ? N4 C32 H32 117.5 . . ? C33 C32 H32 117.5 . . ? C29 C33 C32 119.6(7) . . ? C29 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? N2 C34 C35 124.0(7) . . ? N2 C34 H34 118.0 . . ? C35 C34 H34 118.0 . . ? C34 C35 C36 121.2(6) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 115.0(6) . . ? C37 C36 C39 121.2(5) . . ? C35 C36 C39 123.8(5) . . ? C36 C37 C38 120.0(6) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? N2 C38 C37 124.3(6) . . ? N2 C38 H38 117.9 . . ? C37 C38 H38 117.9 . . ? C43 C39 C40 116.3(5) . . ? C43 C39 C36 120.5(5) . . ? C40 C39 C36 123.1(5) . . ? C41 C40 C39 119.9(5) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? N1 C41 C40 123.5(5) . . ? N1 C41 H41 118.2 . . ? C40 C41 H41 118.2 . . ? N1 C42 C43 124.0(5) . . ? N1 C42 H42 118.0 . . ? C43 C42 H42 118.0 . . ? C39 C43 C42 119.8(5) . . ? C39 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cd1 O1 C11 8.5(3) . . . . ? N3 Cd1 O1 C11 106.4(3) . . . . ? O6 Cd1 O1 C11 -158.4(3) 4_666 . . . ? N2 Cd1 O1 C11 -81.4(3) . . . . ? N1 Cd1 O1 C11 11.2(4) 2_545 . . . ? O5 Cd1 O1 C11 -174.1(3) 4_666 . . . ? N3 Cd1 O2 C11 -93.0(4) . . . . ? O6 Cd1 O2 C11 144.4(5) 4_666 . . . ? N2 Cd1 O2 C11 75.6(4) . . . . ? N1 Cd1 O2 C11 173.5(4) 2_545 . . . ? O5 Cd1 O2 C11 -12.8(5) 4_666 . . . ? O1 Cd1 O2 C11 -8.4(3) . . . . ? O2 Cd1 N2 C38 123.7(5) . . . . ? N3 Cd1 N2 C38 -140.0(8) . . . . ? O6 Cd1 N2 C38 -39.9(5) 4_666 . . . ? N1 Cd1 N2 C38 40.5(5) 2_545 . . . ? O5 Cd1 N2 C38 -92.9(5) 4_666 . . . ? O1 Cd1 N2 C38 176.9(5) . . . . ? O2 Cd1 N2 C34 -56.5(6) . . . . ? N3 Cd1 N2 C34 39.9(11) . . . . ? O6 Cd1 N2 C34 140.0(6) 4_666 . . . ? N1 Cd1 N2 C34 -139.7(6) 2_545 . . . ? O5 Cd1 N2 C34 87.0(6) 4_666 . . . ? O1 Cd1 N2 C34 -3.3(6) . . . . ? O2 Cd1 N3 C24 81.2(5) . . . . ? O6 Cd1 N3 C24 -113.6(5) 4_666 . . . ? N2 Cd1 N3 C24 -14.1(11) . . . . ? N1 Cd1 N3 C24 165.5(5) 2_545 . . . ? O5 Cd1 N3 C24 -62.2(5) 4_666 . . . ? O1 Cd1 N3 C24 28.6(5) . . . . ? O2 Cd1 N3 C28 -104.9(5) . . . . ? O6 Cd1 N3 C28 60.2(5) 4_666 . . . ? N2 Cd1 N3 C28 159.8(7) . . . . ? N1 Cd1 N3 C28 -20.7(5) 2_545 . . . ? O5 Cd1 N3 C28 111.7(5) 4_666 . . . ? O1 Cd1 N3 C28 -157.6(5) . . . . ? C10 C1 C2 C3 -2.3(9) . . . . ? C10 C1 C2 C11 -178.3(5) . . . . ? C1 C2 C3 O3 179.3(5) . . . . ? C11 C2 C3 O3 -4.7(8) . . . . ? C1 C2 C3 C4 -1.0(9) . . . . ? C11 C2 C3 C4 175.0(5) . . . . ? O3 C3 C4 C5 -176.0(5) . . . . ? C2 C3 C4 C5 4.3(9) . . . . ? O3 C3 C4 C12 3.5(8) . . . . ? C2 C3 C4 C12 -176.2(5) . . . . ? C3 C4 C5 C6 174.1(6) . . . . ? C12 C4 C5 C6 -5.4(9) . . . . ? C3 C4 C5 C10 -4.2(9) . . . . ? C12 C4 C5 C10 176.2(5) . . . . ? C4 C5 C6 C7 -178.8(7) . . . . ? C10 C5 C6 C7 -0.5(10) . . . . ? C5 C6 C7 C8 0.9(12) . . . . ? C6 C7 C8 C9 -3.2(13) . . . . ? C7 C8 C9 C10 5.0(13) . . . . ? C2 C1 C10 C9 -177.3(6) . . . . ? C2 C1 C10 C5 2.2(9) . . . . ? C8 C9 C10 C1 175.0(7) . . . . ? C8 C9 C10 C5 -4.4(10) . . . . ? C4 C5 C10 C1 1.1(9) . . . . ? C6 C5 C10 C1 -177.3(6) . . . . ? C4 C5 C10 C9 -179.4(6) . . . . ? C6 C5 C10 C9 2.2(9) . . . . ? Cd1 O1 C11 O2 -14.4(5) . . . . ? Cd1 O1 C11 C2 159.7(5) . . . . ? Cd1 O2 C11 O1 16.2(6) . . . . ? Cd1 O2 C11 C2 -158.2(4) . . . . ? C1 C2 C11 O1 0.6(9) . . . . ? C3 C2 C11 O1 -175.4(5) . . . . ? C1 C2 C11 O2 174.8(5) . . . . ? C3 C2 C11 O2 -1.2(8) . . . . ? C3 C4 C12 C13 118.6(6) . . . . ? C5 C4 C12 C13 -61.9(8) . . . . ? C4 C12 C13 C14 119.7(6) . . . . ? C4 C12 C13 C22 -61.5(7) . . . . ? C22 C13 C14 O4 -178.1(5) . . . . ? C12 C13 C14 O4 0.7(8) . . . . ? C22 C13 C14 C15 4.3(8) . . . . ? C12 C13 C14 C15 -176.9(5) . . . . ? O4 C14 C15 C16 178.5(5) . . . . ? C13 C14 C15 C16 -3.9(8) . . . . ? O4 C14 C15 C23 -3.4(8) . . . . ? C13 C14 C15 C23 174.1(5) . . . . ? C14 C15 C16 C17 1.3(9) . . . . ? C23 C15 C16 C17 -176.8(5) . . . . ? C15 C16 C17 C18 -178.2(6) . . . . ? C15 C16 C17 C22 0.7(9) . . . . ? C16 C17 C18 C19 -179.9(7) . . . . ? C22 C17 C18 C19 1.3(11) . . . . ? C17 C18 C19 C20 -2.6(12) . . . . ? C18 C19 C20 C21 2.4(11) . . . . ? C19 C20 C21 C22 -0.9(10) . . . . ? C14 C13 C22 C17 -2.2(8) . . . . ? C12 C13 C22 C17 179.0(5) . . . . ? C14 C13 C22 C21 176.1(5) . . . . ? C12 C13 C22 C21 -2.7(8) . . . . ? C18 C17 C22 C13 178.6(6) . . . . ? C16 C17 C22 C13 -0.3(8) . . . . ? C18 C17 C22 C21 0.2(9) . . . . ? C16 C17 C22 C21 -178.6(5) . . . . ? C20 C21 C22 C13 -178.7(6) . . . . ? C20 C21 C22 C17 -0.4(9) . . . . ? Cd1 O6 C23 O5 -8.7(7) 4_465 . . . ? Cd1 O6 C23 C15 169.9(5) 4_465 . . . ? Cd1 O5 C23 O6 8.0(6) 4_465 . . . ? Cd1 O5 C23 C15 -170.6(5) 4_465 . . . ? C16 C15 C23 O6 7.2(9) . . . . ? C14 C15 C23 O6 -170.9(5) . . . . ? C16 C15 C23 O5 -174.1(5) . . . . ? C14 C15 C23 O5 7.8(8) . . . . ? C28 N3 C24 C25 -2.1(10) . . . . ? Cd1 N3 C24 C25 172.1(6) . . . . ? N3 C24 C25 C26 2.2(12) . . . . ? C24 C25 C26 C27 -0.9(10) . . . . ? C24 C25 C26 C29 179.6(6) . . . . ? C25 C26 C27 C28 -0.3(10) . . . . ? C29 C26 C27 C28 179.3(6) . . . . ? C24 N3 C28 C27 0.8(10) . . . . ? Cd1 N3 C28 C27 -173.4(6) . . . . ? C26 C27 C28 N3 0.3(12) . . . . ? C27 C26 C29 C30 -167.3(6) . . . . ? C25 C26 C29 C30 12.2(9) . . . . ? C27 C26 C29 C33 13.6(9) . . . . ? C25 C26 C29 C33 -166.9(7) . . . . ? C33 C29 C30 C31 0.4(10) . . . . ? C26 C29 C30 C31 -178.9(6) . . . . ? C32 N4 C31 C30 3.4(12) . . . . ? C29 C30 C31 N4 -1.8(11) . . . . ? C31 N4 C32 C33 -3.9(15) . . . . ? C30 C29 C33 C32 -0.7(12) . . . . ? C26 C29 C33 C32 178.5(8) . . . . ? N4 C32 C33 C29 2.7(16) . . . . ? C38 N2 C34 C35 3.2(11) . . . . ? Cd1 N2 C34 C35 -176.7(6) . . . . ? N2 C34 C35 C36 1.1(13) . . . . ? C34 C35 C36 C37 -4.4(11) . . . . ? C34 C35 C36 C39 174.1(7) . . . . ? C35 C36 C37 C38 3.5(11) . . . . ? C39 C36 C37 C38 -175.0(6) . . . . ? C34 N2 C38 C37 -4.0(11) . . . . ? Cd1 N2 C38 C37 175.8(6) . . . . ? C36 C37 C38 N2 0.7(12) . . . . ? C37 C36 C39 C43 33.0(9) . . . . ? C35 C36 C39 C43 -145.3(7) . . . . ? C37 C36 C39 C40 -148.9(7) . . . . ? C35 C36 C39 C40 32.8(9) . . . . ? C43 C39 C40 C41 2.3(9) . . . . ? C36 C39 C40 C41 -175.9(6) . . . . ? C42 N1 C41 C40 -3.6(9) . . . . ? Cd1 N1 C41 C40 169.7(5) 2 . . . ? C39 C40 C41 N1 1.2(10) . . . . ? C41 N1 C42 C43 2.5(9) . . . . ? Cd1 N1 C42 C43 -171.2(5) 2 . . . ? C40 C39 C43 C42 -3.3(9) . . . . ? C36 C39 C43 C42 174.9(5) . . . . ? N1 C42 C43 C39 0.9(10) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.979 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.115 #===END