# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 _journal_name_full CrystEngComm _publ_contact_author_name 'Zhan Shi' _publ_contact_author_email ZSHI@MAIL.JLU.EDU.CN loop_ _publ_author_name 'Zhan Shi' 'Li, Baiyan' 'Zhou, Xiaojing' 'Zhou, Qi' 'Li, Guanghua' 'Hua, Jia' 'Bi, Ye' 'Li, Yijin' 'Feng, Shouhua' data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 806099' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C33.50 H22 Mn2 N6 O17' _chemical_formula_sum 'C33.50 H22 Mn2 N6 O17' _chemical_formula_weight 890.45 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 7.9017(16) _cell_length_b 27.456(6) _cell_length_c 32.408(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.03(3) _cell_angle_gamma 90.00 _cell_volume 7004(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6026 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3608 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24295 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6026 _reflns_number_gt 4752 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+18.5590P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6026 _refine_ls_number_parameters 574 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.020 _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 0.70751(7) 0.87517(2) 0.815714(18) 0.02876(19) Uani 1 1 d . . . Mn2 Mn 0.30348(8) 0.83110(2) 0.846871(19) 0.0337(2) Uani 1 1 d D . . O1 O 0.4524(4) 0.85757(12) 0.90020(9) 0.0420(8) Uani 1 1 d . . . O2 O 0.7146(4) 0.86416(13) 0.88051(9) 0.0446(8) Uani 1 1 d . . . O3 O 0.9013(4) 1.11528(12) 1.15000(10) 0.0462(8) Uani 1 1 d . . . O5 O 1.1647(4) 0.88838(19) 0.99480(14) 0.0810(13) Uani 1 1 d . . . O6 O 1.1321(4) 0.95840(17) 1.02329(11) 0.0681(11) Uani 1 1 d . . . O7 O 0.9665(5) 0.87208(13) 1.07995(12) 0.0673(11) Uani 1 1 d . . . O8 O 1.1500(4) 0.90165(13) 1.12533(12) 0.0636(10) Uani 1 1 d . . . O9 O 0.4988(4) 0.78034(12) 0.83036(12) 0.0577(9) Uani 1 1 d . . . O10 O 0.7354(5) 0.80233(11) 0.80208(10) 0.0521(9) Uani 1 1 d . . . O11 O 0.9388(3) 0.38741(10) 0.81094(8) 0.0335(7) Uani 1 1 d . . . O13 O 1.1660(5) 0.68317(17) 0.79147(14) 0.0784(13) Uani 1 1 d . . . O14 O 1.1289(4) 0.60726(15) 0.80053(13) 0.0630(10) Uani 1 1 d . . . O15 O 1.0790(4) 0.52899(13) 0.89284(10) 0.0554(9) Uani 1 1 d . . . O16 O 0.9391(5) 0.59577(13) 0.88262(10) 0.0567(9) Uani 1 1 d . . . O17 O 0.1666(4) 0.80361(13) 0.78747(10) 0.0537(9) Uani 1 1 d D . . N1 N 1.0754(5) 0.92158(19) 1.00603(12) 0.0501(11) Uani 1 1 d . . . N2 N 1.0284(5) 0.90646(14) 1.09991(11) 0.0393(9) Uani 1 1 d . . . N3 N 1.0775(4) 0.64850(16) 0.79958(11) 0.0400(9) Uani 1 1 d . . . N4 N 0.9817(5) 0.55535(14) 0.87186(11) 0.0373(9) Uani 1 1 d . . . N5 N 0.1769(5) 0.77604(15) 0.88205(13) 0.0482(10) Uani 1 1 d . . . N6 N -0.0130(7) 0.7350(2) 0.91384(16) 0.0744(15) Uani 1 1 d . . . C1 C 0.7798(5) 0.93171(15) 1.02472(12) 0.0307(9) Uani 1 1 d . . . C2 C 0.8918(5) 0.91570(17) 0.99689(13) 0.0355(10) Uani 1 1 d . . . C3 C 0.8401(5) 0.89411(17) 0.95956(12) 0.0350(10) Uani 1 1 d . . . H3 H 0.9196 0.8849 0.9415 0.080 Uiso 1 1 calc . . . C4 C 0.6679(5) 0.88622(16) 0.94908(12) 0.0316(9) Uani 1 1 d . . . C5 C 0.5542(5) 0.89805(16) 0.97745(12) 0.0328(10) Uani 1 1 d . . . H5 H 0.4396 0.8907 0.9717 0.080 Uiso 1 1 calc . . . C6 C 0.6088(5) 0.92092(17) 1.01463(12) 0.0348(10) Uani 1 1 d . . . H6 H 0.5296 0.9291 1.0331 0.080 Uiso 1 1 calc . . . C7 C 0.6059(5) 0.86736(16) 0.90637(13) 0.0334(10) Uani 1 1 d . . . C8 C 0.8261(5) 0.96356(16) 1.06164(12) 0.0317(10) Uani 1 1 d . . . C9 C 0.9477(5) 0.95466(16) 1.09476(12) 0.0319(9) Uani 1 1 d . . . C10 C 0.9976(5) 0.99016(16) 1.12376(12) 0.0334(10) Uani 1 1 d . . . H10 H 1.0819 0.9835 1.1449 0.080 Uiso 1 1 calc . . . C11 C 0.9214(5) 1.03571(16) 1.12118(12) 0.0304(9) Uani 1 1 d . . . C12 C 0.7905(5) 1.04437(17) 1.09050(13) 0.0361(10) Uani 1 1 d . . . H12 H 0.7325 1.0739 1.0896 0.080 Uiso 1 1 calc . . . C13 C 0.7472(5) 1.00858(17) 1.06125(13) 0.0371(10) Uani 1 1 d . . . H13 H 0.6614 1.0151 1.0405 0.080 Uiso 1 1 calc . . . C14 C 0.9838(5) 1.07669(17) 1.14992(12) 0.0324(10) Uani 1 1 d . . . C15 C 0.7829(5) 0.62021(15) 0.80785(13) 0.0313(9) Uani 1 1 d . . . C16 C 0.9006(5) 0.65812(15) 0.80571(12) 0.0307(9) Uani 1 1 d . . . C17 C 0.8543(5) 0.70650(16) 0.80739(13) 0.0360(10) Uani 1 1 d . . . H17 H 0.9348 0.7309 0.8053 0.080 Uiso 1 1 calc . . . C18 C 0.6868(5) 0.71841(16) 0.81227(13) 0.0371(10) Uani 1 1 d . . . C19 C 0.5682(5) 0.68190(18) 0.81440(16) 0.0452(12) Uani 1 1 d . . . H19 H 0.4558 0.6898 0.8177 0.080 Uiso 1 1 calc . . . C20 C 0.6150(5) 0.63385(16) 0.81170(15) 0.0405(11) Uani 1 1 d . . . H20 H 0.5325 0.6098 0.8125 0.080 Uiso 1 1 calc . . . C21 C 0.6341(6) 0.77127(17) 0.81544(14) 0.0434(11) Uani 1 1 d . . . C22 C 0.8145(5) 0.56703(15) 0.80300(13) 0.0300(9) Uani 1 1 d . . . C23 C 0.9039(5) 0.53628(15) 0.83172(12) 0.0300(9) Uani 1 1 d . . . C24 C 0.9214(5) 0.48721(15) 0.82522(12) 0.0301(9) Uani 1 1 d . . . H24 H 0.9843 0.4681 0.8447 0.080 Uiso 1 1 calc . . . C25 C 0.8439(5) 0.46601(14) 0.78899(12) 0.0280(9) Uani 1 1 d . . . C26 C 0.7518(5) 0.49542(16) 0.76032(12) 0.0348(10) Uani 1 1 d . . . H26 H 0.6991 0.4818 0.7362 0.080 Uiso 1 1 calc . . . C27 C 0.7384(5) 0.54473(16) 0.76741(13) 0.0367(10) Uani 1 1 d . . . H27 H 0.6764 0.5638 0.7478 0.080 Uiso 1 1 calc . . . C28 C 0.8589(5) 0.41267(15) 0.78205(12) 0.0300(9) Uani 1 1 d . . . C29 C 0.0238(7) 0.7765(2) 0.89372(16) 0.0579(14) Uani 1 1 d . . . H29 H -0.0518 0.8022 0.8888 0.080 Uiso 1 1 calc . . . C30 C 0.2376(8) 0.7308(2) 0.8939(2) 0.081(2) Uani 1 1 d . . . H30 H 0.3424 0.7186 0.8878 0.080 Uiso 1 1 calc . . . C31 C 0.1286(11) 0.7069(3) 0.9149(2) 0.093(2) Uani 1 1 d . . . H31 H 0.1454 0.6768 0.9278 0.080 Uiso 1 1 calc . . . O12 O 0.7916(4) 0.39456(12) 0.74940(9) 0.0468(8) Uani 1 1 d . . . O4 O 1.1206(4) 1.06894(11) 1.17209(9) 0.0424(8) Uani 1 1 d . . . C32 C -0.177(3) 0.7331(9) 0.9348(7) 0.101(7) Uani 0.50 1 d P . . C32' C -0.172(3) 0.7057(9) 0.9223(7) 0.108(8) Uani 0.50 1 d P . . C33 C -0.135(4) 0.7484(11) 0.9833(8) 0.095(7) Uani 0.40 1 d PU . . C33' C -0.183(6) 0.7189(19) 0.9761(16) 0.110(13) Uani 0.20 1 d PU . . C33" C -0.269(3) 0.7361(8) 0.9467(7) 0.093(6) Uani 0.40 1 d PU . . C34 C -0.218(3) 0.7501(11) 0.9915(8) 0.084(7) Uani 0.35 1 d PU . . C34' C -0.426(10) 0.756(3) 1.003(3) 0.13(2) Uani 0.15 1 d PU . . H1A H 0.179(5) 0.8271(9) 0.7714(5) 0.080 Uiso 1 1 d D . . H1B H 0.0659(16) 0.8021(16) 0.7942(6) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0354(4) 0.0266(4) 0.0231(3) -0.0017(2) -0.0033(2) 0.0003(3) Mn2 0.0365(4) 0.0310(4) 0.0326(4) -0.0023(3) -0.0041(3) 0.0005(3) O1 0.0390(18) 0.058(2) 0.0284(17) -0.0071(14) -0.0031(12) -0.0019(15) O2 0.0394(16) 0.071(2) 0.0222(16) -0.0069(15) -0.0028(13) 0.0067(16) O3 0.0480(18) 0.038(2) 0.052(2) -0.0121(15) -0.0025(15) 0.0036(16) O5 0.0324(19) 0.126(4) 0.085(3) -0.021(3) 0.0072(18) 0.013(2) O6 0.048(2) 0.109(3) 0.047(2) -0.014(2) 0.0024(16) -0.033(2) O7 0.099(3) 0.038(2) 0.059(2) -0.0067(18) -0.024(2) 0.005(2) O8 0.059(2) 0.053(2) 0.074(3) 0.003(2) -0.0247(19) 0.0095(19) O9 0.059(2) 0.039(2) 0.076(3) -0.0060(18) 0.0078(19) 0.0181(18) O10 0.091(3) 0.0280(19) 0.0391(19) 0.0007(15) 0.0152(17) 0.0022(18) O11 0.0421(16) 0.0268(16) 0.0303(16) 0.0008(12) -0.0051(12) 0.0076(13) O13 0.044(2) 0.083(3) 0.110(4) 0.013(3) 0.017(2) -0.015(2) O14 0.0389(19) 0.057(3) 0.095(3) -0.012(2) 0.0144(18) 0.0130(18) O15 0.070(2) 0.053(2) 0.039(2) -0.0049(17) -0.0211(16) 0.0072(18) O16 0.091(3) 0.040(2) 0.0366(19) -0.0110(16) -0.0040(17) 0.0114(19) O17 0.062(2) 0.059(2) 0.0389(19) -0.0009(16) -0.0023(15) -0.0183(18) N1 0.031(2) 0.086(4) 0.033(2) -0.006(2) 0.0030(16) -0.009(2) N2 0.043(2) 0.037(2) 0.036(2) 0.0013(18) -0.0002(17) 0.0018(18) N3 0.033(2) 0.050(3) 0.038(2) -0.0051(18) 0.0026(15) -0.004(2) N4 0.049(2) 0.035(2) 0.027(2) -0.0019(17) -0.0004(16) -0.0043(19) N5 0.045(2) 0.047(3) 0.053(3) 0.006(2) 0.0085(18) 0.002(2) N6 0.086(4) 0.079(4) 0.062(3) 0.007(3) 0.024(3) -0.021(3) C1 0.031(2) 0.033(3) 0.027(2) -0.0006(18) -0.0014(16) -0.0002(18) C2 0.025(2) 0.050(3) 0.031(2) 0.000(2) 0.0003(16) -0.0038(19) C3 0.031(2) 0.050(3) 0.024(2) -0.0018(19) 0.0025(16) -0.001(2) C4 0.030(2) 0.038(3) 0.027(2) -0.0011(18) -0.0009(16) 0.0015(19) C5 0.030(2) 0.038(3) 0.030(2) -0.0021(19) -0.0015(16) -0.0028(19) C6 0.030(2) 0.047(3) 0.027(2) -0.0052(19) 0.0022(16) 0.002(2) C7 0.034(2) 0.031(3) 0.034(2) -0.0020(19) -0.0003(18) 0.0050(19) C8 0.031(2) 0.038(3) 0.025(2) -0.0025(18) 0.0015(16) -0.0073(19) C9 0.030(2) 0.035(3) 0.031(2) 0.0012(18) 0.0022(16) 0.0007(19) C10 0.031(2) 0.040(3) 0.028(2) 0.0020(19) -0.0024(17) -0.006(2) C11 0.027(2) 0.035(3) 0.028(2) -0.0025(18) -0.0004(16) -0.0045(19) C12 0.035(2) 0.040(3) 0.032(2) -0.004(2) -0.0018(17) 0.000(2) C13 0.036(2) 0.042(3) 0.032(2) 0.001(2) -0.0048(18) 0.003(2) C14 0.033(2) 0.040(3) 0.024(2) -0.0038(18) 0.0045(17) -0.009(2) C15 0.036(2) 0.026(2) 0.032(2) 0.0022(18) 0.0035(17) 0.0013(19) C16 0.031(2) 0.032(3) 0.030(2) -0.0022(18) 0.0028(16) 0.0040(19) C17 0.045(2) 0.030(3) 0.033(2) 0.0007(19) 0.0052(18) -0.008(2) C18 0.044(3) 0.028(3) 0.039(3) -0.0019(19) 0.0008(19) 0.007(2) C19 0.034(2) 0.034(3) 0.068(3) -0.009(2) 0.006(2) 0.005(2) C20 0.032(2) 0.029(3) 0.061(3) -0.004(2) 0.007(2) -0.008(2) C21 0.061(3) 0.032(3) 0.036(3) 0.003(2) -0.005(2) 0.005(2) C22 0.030(2) 0.024(2) 0.037(2) 0.0015(18) 0.0071(17) 0.0007(18) C23 0.037(2) 0.029(3) 0.023(2) -0.0037(17) -0.0010(16) -0.0012(19) C24 0.036(2) 0.026(2) 0.027(2) -0.0008(17) -0.0010(16) 0.0028(18) C25 0.037(2) 0.023(2) 0.024(2) 0.0002(17) 0.0038(16) 0.0067(18) C26 0.043(2) 0.034(3) 0.026(2) 0.0002(18) -0.0053(17) 0.009(2) C27 0.043(2) 0.030(3) 0.035(2) 0.0021(19) -0.0059(18) 0.008(2) C28 0.030(2) 0.031(3) 0.028(2) -0.0030(18) 0.0004(16) 0.0064(18) C29 0.066(3) 0.062(4) 0.046(3) 0.004(3) 0.006(2) 0.005(3) C30 0.085(4) 0.067(4) 0.097(5) 0.031(4) 0.042(4) 0.028(4) C31 0.125(6) 0.062(5) 0.099(6) 0.028(4) 0.046(5) 0.019(4) O12 0.065(2) 0.041(2) 0.0310(17) -0.0082(14) -0.0126(14) 0.0153(16) O4 0.0441(17) 0.0389(19) 0.0406(18) 0.0011(14) -0.0164(14) -0.0076(14) C32 0.081(11) 0.12(2) 0.106(18) 0.010(12) 0.041(11) -0.050(14) C32' 0.112(14) 0.13(2) 0.087(14) -0.025(13) 0.032(10) -0.048(15) C33 0.095(7) 0.095(7) 0.095(7) -0.0002(10) 0.0084(12) 0.0001(10) C33' 0.110(13) 0.110(13) 0.110(13) 0.0001(10) 0.0098(16) 0.0000(10) C33" 0.093(6) 0.093(6) 0.093(6) -0.0002(10) 0.0086(12) -0.0002(10) C34 0.084(7) 0.084(7) 0.084(7) -0.0001(10) 0.0073(12) -0.0001(10) C34' 0.13(2) 0.13(2) 0.13(2) 0.0000(10) 0.012(2) 0.0000(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O10 2.064(3) . ? Mn1 O4 2.064(3) 5_777 ? Mn1 O2 2.117(3) . ? Mn1 O11 2.142(3) 3_455 ? Mn1 O12 2.177(3) 4_656 ? Mn2 O1 2.131(3) . ? Mn2 O9 2.180(3) . ? Mn2 N5 2.187(4) . ? Mn2 O3 2.196(3) 5_677 ? Mn2 O17 2.254(3) . ? Mn2 O11 2.260(3) 3_455 ? O1 C7 1.242(5) . ? O2 C7 1.255(5) . ? O3 C14 1.244(5) . ? O3 Mn2 2.196(3) 5_677 ? O5 N1 1.227(6) . ? O6 N1 1.221(5) . ? O7 N2 1.222(5) . ? O8 N2 1.217(5) . ? O9 C21 1.236(6) . ? O10 C21 1.272(6) . ? O11 C28 1.286(5) . ? O11 Mn1 2.142(3) 3_545 ? O11 Mn2 2.260(3) 3_545 ? O13 N3 1.223(5) . ? O14 N3 1.202(5) . ? O15 N4 1.219(5) . ? O16 N4 1.219(5) . ? O17 H1A 0.840(10) . ? O17 H1B 0.844(10) . ? N1 C2 1.464(5) . ? N2 C9 1.472(6) . ? N3 C16 1.453(5) . ? N4 C23 1.485(5) . ? N5 C29 1.299(6) . ? N5 C30 1.374(7) . ? N6 C29 1.356(7) . ? N6 C31 1.359(8) . ? N6 C32 1.52(2) . ? N6 C32' 1.54(2) . ? C1 C2 1.389(6) . ? C1 C6 1.394(6) . ? C1 C8 1.501(5) . ? C2 C3 1.377(6) . ? C3 C4 1.390(6) . ? C3 H3 0.9300 . ? C4 C5 1.380(6) . ? C4 C7 1.518(6) . ? C5 C6 1.393(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.384(6) . ? C8 C9 1.398(6) . ? C9 C10 1.387(6) . ? C10 C11 1.387(6) . ? C10 H10 0.9300 . ? C11 C12 1.391(6) . ? C11 C14 1.515(6) . ? C12 C13 1.387(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O4 1.263(5) . ? C15 C20 1.394(6) . ? C15 C16 1.402(6) . ? C15 C22 1.492(6) . ? C16 C17 1.380(6) . ? C17 C18 1.386(6) . ? C17 H17 0.9300 . ? C18 C19 1.378(6) . ? C18 C21 1.516(6) . ? C19 C20 1.375(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.395(6) . ? C22 C23 1.401(5) . ? C23 C24 1.373(6) . ? C24 C25 1.402(5) . ? C24 H24 0.9300 . ? C25 C26 1.388(5) . ? C25 C28 1.488(6) . ? C26 C27 1.379(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O12 1.246(5) . ? C29 H29 0.9300 . ? C30 C31 1.320(9) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? O12 Mn1 2.177(3) 4_646 ? O4 Mn1 2.064(3) 5_777 ? C32 C33" 0.85(2) . ? C32 C33 1.63(4) . ? C32 C34 1.95(3) . ? C32' C33" 1.42(3) . ? C32' C33' 1.79(6) . ? C33 C34' 0.65(8) 7_467 ? C33 C34 0.73(3) . ? C33 C34 1.48(4) 7_467 ? C33 C33" 1.55(4) . ? C33' C34 1.04(5) . ? C33' C33" 1.22(5) . ? C33' C34' 1.26(9) 7_467 ? C33' C34 1.61(6) 7_467 ? C33" C34 1.52(3) . ? C34 C34 0.78(4) 7_467 ? C34 C34' 1.15(9) 7_467 ? C34 C33 1.48(4) 7_467 ? C34 C33' 1.61(6) 7_467 ? C34 C34' 1.73(9) . ? C34' C33 0.65(8) 7_467 ? C34' C34 1.15(8) 7_467 ? C34' C33' 1.26(9) 7_467 ? 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 O10 Mn1 O4 132.88(14) . 5_777 ? O10 Mn1 O2 94.58(13) . . ? O4 Mn1 O2 87.50(13) 5_777 . ? O10 Mn1 O11 105.11(13) . 3_455 ? O4 Mn1 O11 121.89(12) 5_777 3_455 ? O2 Mn1 O11 91.95(11) . 3_455 ? O10 Mn1 O12 91.15(13) . 4_656 ? O4 Mn1 O12 86.89(12) 5_777 4_656 ? O2 Mn1 O12 173.81(13) . 4_656 ? O11 Mn1 O12 88.80(12) 3_455 4_656 ? O1 Mn2 O9 93.71(13) . . ? O1 Mn2 N5 93.33(14) . . ? O9 Mn2 N5 92.98(15) . . ? O1 Mn2 O3 95.19(12) . 5_677 ? O9 Mn2 O3 168.46(13) . 5_677 ? N5 Mn2 O3 93.83(14) . 5_677 ? O1 Mn2 O17 174.99(12) . . ? O9 Mn2 O17 82.73(14) . . ? N5 Mn2 O17 90.38(14) . . ? O3 Mn2 O17 87.92(13) 5_677 . ? O1 Mn2 O11 86.10(11) . 3_455 ? O9 Mn2 O11 86.20(13) . 3_455 ? N5 Mn2 O11 178.97(13) . 3_455 ? O3 Mn2 O11 87.08(12) 5_677 3_455 ? O17 Mn2 O11 90.14(11) . 3_455 ? C7 O1 Mn2 131.8(3) . . ? C7 O2 Mn1 133.8(3) . . ? C14 O3 Mn2 163.6(3) . 5_677 ? C21 O9 Mn2 151.6(3) . . ? C21 O10 Mn1 119.6(3) . . ? C28 O11 Mn1 123.9(3) . 3_545 ? C28 O11 Mn2 121.3(2) . 3_545 ? Mn1 O11 Mn2 111.48(12) 3_545 3_545 ? Mn2 O17 H1A 101.4(10) . . ? Mn2 O17 H1B 100.9(9) . . ? H1A O17 H1B 111.3(18) . . ? O6 N1 O5 123.6(4) . . ? O6 N1 C2 120.1(4) . . ? O5 N1 C2 116.3(4) . . ? O8 N2 O7 122.0(4) . . ? O8 N2 C9 118.9(4) . . ? O7 N2 C9 119.0(4) . . ? O14 N3 O13 122.7(4) . . ? O14 N3 C16 119.6(4) . . ? O13 N3 C16 117.6(4) . . ? O15 N4 O16 123.9(4) . . ? O15 N4 C23 118.1(4) . . ? O16 N4 C23 117.9(4) . . ? C29 N5 C30 103.8(5) . . ? C29 N5 Mn2 128.7(4) . . ? C30 N5 Mn2 127.3(3) . . ? C29 N6 C31 106.2(5) . . ? C29 N6 C32 118.2(11) . . ? C31 N6 C32 134.7(11) . . ? C29 N6 C32' 137.6(13) . . ? C31 N6 C32' 112.5(12) . . ? C32 N6 C32' 32.6(9) . . ? C2 C1 C6 116.1(4) . . ? C2 C1 C8 125.2(4) . . ? C6 C1 C8 118.3(4) . . ? C3 C2 C1 123.3(4) . . ? C3 C2 N1 116.0(4) . . ? C1 C2 N1 120.7(4) . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 C7 120.7(4) . . ? C3 C4 C7 120.4(4) . . ? C4 C5 C6 120.8(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 121.3(4) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? O1 C7 O2 126.4(4) . . ? O1 C7 C4 116.9(4) . . ? O2 C7 C4 116.6(4) . . ? C13 C8 C9 116.2(4) . . ? C13 C8 C1 115.8(4) . . ? C9 C8 C1 127.8(4) . . ? C10 C9 C8 122.2(4) . . ? C10 C9 N2 117.4(4) . . ? C8 C9 N2 120.4(4) . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 119.3(4) . . ? C10 C11 C14 121.1(4) . . ? C12 C11 C14 119.6(4) . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C8 C13 C12 122.8(4) . . ? C8 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? O3 C14 O4 124.4(4) . . ? O3 C14 C11 119.4(4) . . ? O4 C14 C11 116.1(4) . . ? C20 C15 C16 116.5(4) . . ? C20 C15 C22 116.2(4) . . ? C16 C15 C22 127.1(4) . . ? C17 C16 C15 122.3(4) . . ? C17 C16 N3 116.2(4) . . ? C15 C16 N3 121.5(4) . . ? C16 C17 C18 119.4(4) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 119.6(4) . . ? C19 C18 C21 120.1(4) . . ? C17 C18 C21 120.3(4) . . ? C20 C19 C18 120.5(4) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C15 121.8(4) . . ? C19 C20 H20 119.1 . . ? C15 C20 H20 119.1 . . ? O9 C21 O10 126.1(5) . . ? O9 C21 C18 118.1(4) . . ? O10 C21 C18 115.7(4) . . ? C27 C22 C23 116.1(4) . . ? C27 C22 C15 116.9(4) . . ? C23 C22 C15 126.8(4) . . ? C24 C23 C22 122.8(4) . . ? C24 C23 N4 116.2(3) . . ? C22 C23 N4 121.0(4) . . ? C23 C24 C25 119.6(4) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 119.0(4) . . ? C26 C25 C28 121.0(4) . . ? C24 C25 C28 120.0(3) . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C22 122.3(4) . . ? C26 C27 H27 118.8 . . ? C22 C27 H27 118.8 . . ? O12 C28 O11 123.3(4) . . ? O12 C28 C25 119.2(4) . . ? O11 C28 C25 117.5(3) . . ? N5 C29 N6 112.1(5) . . ? N5 C29 H29 123.9 . . ? N6 C29 H29 123.9 . . ? C31 C30 N5 111.5(5) . . ? C31 C30 H30 124.2 . . ? N5 C30 H30 124.2 . . ? C30 C31 N6 106.1(6) . . ? C30 C31 H31 127.0 . . ? N6 C31 H31 127.0 . . ? C28 O12 Mn1 152.1(3) . 4_646 ? C14 O4 Mn1 120.0(3) . 5_777 ? C33" C32 N6 173(3) . . ? C33" C32 C33 70(2) . . ? N6 C32 C33 108.2(17) . . ? C33" C32 C34 48(2) . . ? N6 C32 C34 129.2(16) . . ? C33 C32 C34 21.3(12) . . ? C33" C32' N6 106.2(18) . . ? C33" C32' C33' 42.6(18) . . ? N6 C32' C33' 100(2) . . ? C34' C33 C34 113(10) 7_467 . ? C34' C33 C34 101(10) 7_467 7_467 ? C34 C33 C34 12(4) . 7_467 ? C34' C33 C33" 156(10) 7_467 . ? C34 C33 C33" 74(4) . . ? C34 C33 C33" 85(2) 7_467 . ? C34' C33 C32 135(10) 7_467 . ? C34 C33 C32 105(4) . . ? C34 C33 C32 116(2) 7_467 . ? C33" C33 C32 31.0(11) . . ? C34 C33' C33" 84(4) . . ? C34 C33' C34' 59(5) . 7_467 ? C33" C33' C34' 122(7) . 7_467 ? C34 C33' C34 24(3) . 7_467 ? C33" C33' C34 92(3) . 7_467 ? C34' C33' C34 73(5) 7_467 7_467 ? C34 C33' C32' 132(5) . . ? C33" C33' C32' 52(2) . . ? C34' C33' C32' 124(5) 7_467 . ? C34 C33' C32' 144(4) 7_467 . ? C32 C33" C33' 83(3) . . ? C32 C33" C32' 34(2) . . ? C33' C33" C32' 85(3) . . ? C32 C33" C34 107(3) . . ? C33' C33" C34 43(3) . . ? C32' C33" C34 125(2) . . ? C32 C33" C33 79(3) . . ? C33' C33" C33 36(3) . . ? C32' C33" C33 101(2) . . ? C34 C33" C33 27.4(12) . . ? C33 C34 C34 157(7) . 7_467 ? C33 C34 C33' 59(4) . . ? C34 C34 C33' 123(7) 7_467 . ? C33 C34 C34' 31(5) . 7_467 ? C34 C34 C34' 125(7) 7_467 7_467 ? C33' C34 C34' 70(5) . 7_467 ? C33 C34 C33 168(4) . 7_467 ? C34 C34 C33 11(4) 7_467 7_467 ? C33' C34 C33 123(4) . 7_467 ? C34' C34 C33 137(5) 7_467 7_467 ? C33 C34 C33" 79(3) . . ? C34 C34 C33" 122(5) 7_467 . ? C33' C34 C33" 53(3) . . ? C34' C34 C33" 107(5) 7_467 . ? C33 C34 C33" 112(2) 7_467 . ? C33 C34 C33' 141(5) . 7_467 ? C34 C34 C33' 33(4) 7_467 7_467 ? C33' C34 C33' 156(3) . 7_467 ? C34' C34 C33' 120(5) 7_467 7_467 ? C33 C34 C33' 34.2(17) 7_467 7_467 ? C33" C34 C33' 131(3) . 7_467 ? C33 C34 C34' 171(5) . . ? C34 C34 C34' 33(5) 7_467 . ? C33' C34 C34' 118(5) . . ? C34' C34 C34' 158(3) 7_467 . ? C33 C34 C34' 22(3) 7_467 . ? C33" C34 C34' 93(3) . . ? C33' C34 C34' 44(3) 7_467 . ? C33 C34 C32 54(3) . . ? C34 C34 C32 146(5) 7_467 . ? C33' C34 C32 44(3) . . ? C34' C34 C32 83(5) 7_467 . ? C33 C34 C32 137(2) 7_467 . ? C33" C34 C32 24.8(11) . . ? C33' C34 C32 151(3) 7_467 . ? C34' C34 C32 117(3) . . ? C33 C34' C34 36(6) 7_467 7_467 ? C33 C34' C33' 44(7) 7_467 7_467 ? C34 C34' C33' 51(4) 7_467 7_467 ? C33 C34' C34 57(8) 7_467 . ? C34 C34' C34 22(3) 7_467 . ? C33' C34' C34 63(4) 7_467 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O17 H1A O12 0.840(10) 2.200(13) 2.991(5) 157.0(17) 3_455 O17 H1A O10 0.840(10) 2.62(3) 3.069(5) 115(3) 2_656 O17 H1B O10 0.844(10) 2.646(12) 3.481(5) 170(3) 1_455 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.534 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.085 #=========================END data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 806100' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C39 H35 Co2.50 N7 O20' _chemical_formula_sum 'C39 H35 Co2.50 N7 O20' _chemical_formula_weight 1069.06 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' Co Co 0.3494 0.9721 '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 12.803(3) _cell_length_b 12.071(2) _cell_length_c 28.433(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.13(3) _cell_angle_gamma 90.00 _cell_volume 4393.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7657 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2182 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32865 _diffrn_reflns_av_R_equivalents 0.1073 _diffrn_reflns_av_sigmaI/netI 0.0891 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7657 _reflns_number_gt 5306 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1365P)^2^+26.1425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7657 _refine_ls_number_parameters 697 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2759 _refine_ls_wR_factor_gt 0.2576 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.040 _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 Co1 Co -0.5000 0.5000 0.5000 0.0298(4) Uani 1 2 d S . . Co2 Co -0.45915(9) 0.27368(9) 0.54470(3) 0.0344(3) Uani 1 1 d . . . Co3 Co -0.28529(9) 0.59372(10) 0.47559(4) 0.0391(3) Uani 1 1 d . . . O1 O -0.3832(4) 0.4472(5) 0.45580(17) 0.0386(13) Uani 1 1 d . . . O1W O 0.2659(10) 0.0617(9) 0.5436(4) 0.113(3) Uani 1 1 d D . . O2 O -0.3734(5) 0.2685(5) 0.47783(18) 0.0454(15) Uani 1 1 d . . . O3 O -0.2005(5) 0.1678(6) 0.08863(19) 0.0519(16) Uani 1 1 d . . . O4 O -0.0394(5) 0.2318(5) 0.10712(18) 0.0434(14) Uani 1 1 d . . . O5 O -0.2871(8) 0.0440(9) 0.2847(4) 0.106(3) Uani 1 1 d U . . O6 O -0.2652(9) 0.0025(10) 0.3562(4) 0.113(3) Uani 1 1 d U . . O7 O -0.4618(8) 0.2349(9) 0.2608(4) 0.104(3) Uani 1 1 d U . . O8 O -0.4819(9) 0.2657(9) 0.1884(4) 0.109(3) Uani 1 1 d U . . O9 O -0.2608(5) 0.5318(6) 0.5452(2) 0.0536(17) Uani 1 1 d . . . O10 O -0.4146(4) 0.4528(4) 0.56094(17) 0.0372(13) Uani 1 1 d . . . O11 O -0.0333(6) 0.4266(6) 0.9306(2) 0.068(2) Uani 1 1 d . . . O12 O -0.1342(7) 0.2747(7) 0.9307(2) 0.073(2) Uani 1 1 d . . . O13 O -0.5106(8) 0.4960(10) 0.7263(3) 0.103(3) Uani 1 1 d . . . O14 O -0.3977(8) 0.5047(8) 0.7788(4) 0.102(3) Uani 1 1 d U . . O15 O -0.3766(9) 0.2133(9) 0.8046(4) 0.112(4) Uani 1 1 d . . . O16 O -0.3273(8) 0.2437(8) 0.7364(4) 0.095(3) Uani 1 1 d U . . O17 O -0.2152(6) 0.7438(6) 0.5028(2) 0.066(2) Uani 1 1 d . . . O18 O -0.4296(4) 0.6486(4) 0.49433(16) 0.0312(11) Uani 1 1 d D . . O19 O -0.5190(6) 0.1167(5) 0.5245(2) 0.0542(17) Uani 1 1 d . . . N1 N -0.2777(9) 0.0723(8) 0.3261(3) 0.081(3) Uani 1 1 d . . . N2 N -0.4246(8) 0.2478(10) 0.2227(3) 0.079(3) Uani 1 1 d . . . N3 N -0.4210(7) 0.4923(8) 0.7386(2) 0.061(2) Uani 1 1 d . . . N4 N -0.3189(9) 0.2581(8) 0.7782(3) 0.076(3) Uani 1 1 d . . . N5 N -0.1525(6) 0.5047(8) 0.4551(4) 0.068(2) Uani 1 1 d . . . N6 N -0.0579(17) 0.353(2) 0.4409(8) 0.062(6) Uani 0.50 1 d P A 1 N6' N -0.030(2) 0.402(2) 0.4262(11) 0.063(7) Uani 0.50 1 d P A 2 N7 N 0.3245(6) -0.2108(7) 0.4238(2) 0.0498(19) Uani 1 1 d . . . C1 C -0.2772(8) 0.2702(8) 0.3057(3) 0.050(2) Uani 1 1 d . . . C2 C -0.2927(8) 0.1856(7) 0.3388(3) 0.049(2) Uani 1 1 d . . . C3 C -0.3195(8) 0.2080(7) 0.3847(3) 0.046(2) Uani 1 1 d . . . H3 H -0.3272 0.1505 0.4061 0.080 Uiso 1 1 calc . . . C4 C -0.3347(7) 0.3170(7) 0.3987(3) 0.0376(18) Uani 1 1 d . . . C5 C -0.3231(8) 0.4004(7) 0.3656(3) 0.050(2) Uani 1 1 d . . . H5 H -0.3347 0.4735 0.3743 0.080 Uiso 1 1 calc . . . C6 C -0.2953(8) 0.3776(9) 0.3211(3) 0.056(2) Uani 1 1 d . . . H6 H -0.2881 0.4359 0.2999 0.080 Uiso 1 1 calc . . . C7 C -0.3649(6) 0.3448(7) 0.4478(3) 0.040(2) Uani 1 1 d . . . C8 C -0.2434(8) 0.2523(8) 0.2569(3) 0.051(2) Uani 1 1 d . . . C9 C -0.3108(7) 0.2464(9) 0.2175(3) 0.056(3) Uani 1 1 d . . . C10 C -0.2758(8) 0.2357(9) 0.1726(3) 0.057(3) Uani 1 1 d . . . H10 H -0.3231 0.2329 0.1474 0.080 Uiso 1 1 calc . . . C11 C -0.1704(7) 0.2292(7) 0.1648(3) 0.041(2) Uani 1 1 d . . . C12 C -0.1004(7) 0.2468(9) 0.2030(3) 0.053(2) Uani 1 1 d . . . H12 H -0.0288 0.2504 0.1983 0.080 Uiso 1 1 calc . . . C13 C -0.1402(8) 0.2587(10) 0.2474(3) 0.058(3) Uani 1 1 d . . . H13 H -0.0936 0.2719 0.2722 0.080 Uiso 1 1 calc . . . C14 C -0.1312(7) 0.2104(7) 0.1161(3) 0.041(2) Uani 1 1 d . . . C15 C -0.2353(8) 0.4436(7) 0.7183(3) 0.048(2) Uani 1 1 d . . . C16 C -0.3379(8) 0.4752(7) 0.7043(3) 0.049(2) Uani 1 1 d . . . C17 C -0.3678(7) 0.4876(7) 0.6574(3) 0.044(2) Uani 1 1 d . . . H17 H -0.4370 0.5020 0.6490 0.080 Uiso 1 1 calc . . . C18 C -0.2927(7) 0.4781(7) 0.6234(3) 0.044(2) Uani 1 1 d . . . C19 C -0.1913(7) 0.4544(9) 0.6362(3) 0.052(2) Uani 1 1 d . . . H19 H -0.1404 0.4500 0.6134 0.080 Uiso 1 1 calc . . . C20 C -0.1646(7) 0.4368(9) 0.6838(3) 0.056(3) Uani 1 1 d . . . H20 H -0.0956 0.4198 0.6918 0.080 Uiso 1 1 calc . . . C21 C -0.3232(7) 0.4887(7) 0.5722(3) 0.0383(19) Uani 1 1 d . . . C22 C -0.1991(7) 0.4185(7) 0.7676(3) 0.042(2) Uani 1 1 d . . . C23 C -0.2372(8) 0.3324(8) 0.7956(3) 0.053(2) Uani 1 1 d . . . C24 C -0.2000(8) 0.3124(8) 0.8407(3) 0.051(2) Uani 1 1 d . . . H24 H -0.2254 0.2524 0.8574 0.080 Uiso 1 1 calc . . . C25 C -0.1273(7) 0.3789(7) 0.8606(3) 0.042(2) Uani 1 1 d . . . C26 C -0.0839(8) 0.4628(8) 0.8337(3) 0.050(2) Uani 1 1 d . . . H26 H -0.0299 0.5057 0.8462 0.080 Uiso 1 1 calc . . . C27 C -0.1209(8) 0.4832(7) 0.7879(3) 0.052(2) Uani 1 1 d . . . H27 H -0.0925 0.5411 0.7707 0.080 Uiso 1 1 calc . . . C28 C -0.0944(8) 0.3583(8) 0.9117(3) 0.051(2) Uani 1 1 d . . . C29 C -0.125(2) 0.4051(19) 0.4673(7) 0.061(7) Uani 0.50 1 d P A 1 C31 C -0.049(2) 0.420(2) 0.3971(11) 0.069(8) Uani 0.50 1 d P A 1 C32 C 0.002(2) 0.250(2) 0.4484(10) 0.095(10) Uani 0.50 1 d P A 1 C35 C 0.001(2) -0.047(2) 0.4054(10) 0.089(7) Uani 0.50 1 d PU B 1 C36 C 0.0445(16) -0.143(2) 0.4195(8) 0.082(8) Uani 0.50 1 d P B 1 C37 C 0.2310(19) -0.202(2) 0.4421(9) 0.067(3) Uani 0.50 1 d PU B 1 N8 N 0.1570(15) -0.1713(15) 0.4097(7) 0.048(5) Uani 0.50 1 d P B 1 C30' C -0.096(3) 0.446(3) 0.4930(12) 0.104(10) Uani 0.50 1 d P A 2 C31' C -0.0148(19) 0.391(2) 0.4738(10) 0.080(7) Uani 0.50 1 d P A 2 C32' C 0.019(3) 0.347(3) 0.3914(12) 0.122(12) Uani 0.50 1 d P A 2 C33 C -0.0172(15) 0.1519(18) 0.4181(7) 0.131(7) Uani 1 1 d . A 2 C33' C -0.037(2) 0.226(2) 0.3826(10) 0.086(8) Uani 0.50 1 d P A 2 C36' C 0.0897(18) -0.040(2) 0.4325(8) 0.067(3) Uani 0.50 1 d PU B 2 C37' C 0.2561(19) -0.147(2) 0.4472(8) 0.067(3) Uani 0.50 1 d PU B 2 N8' N 0.1828(19) -0.106(2) 0.4171(7) 0.076(7) Uani 0.50 1 d P B 2 C30 C -0.1094(10) 0.4960(15) 0.4119(6) 0.106(5) Uani 1 1 d . A . C34 C 0.0664(19) 0.062(2) 0.4182(8) 0.166(8) Uani 1 1 d U . . C38 C 0.3036(8) -0.1968(8) 0.3768(3) 0.053(2) Uani 1 1 d . B . C39 C 0.2046(10) -0.1556(11) 0.3702(4) 0.077(4) Uani 1 1 d . . . H1A H -0.438(9) 0.694(7) 0.517(3) 0.080 Uiso 1 1 d D . . H1B H 0.280(10) 0.001(5) 0.529(3) 0.080 Uiso 1 1 d D . . H2B H 0.233(8) 0.104(6) 0.525(3) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0413(9) 0.0307(7) 0.0172(7) -0.0004(6) -0.0028(6) 0.0015(6) Co2 0.0499(7) 0.0340(6) 0.0193(5) 0.0021(4) -0.0020(4) 0.0046(5) Co3 0.0414(7) 0.0506(7) 0.0251(6) 0.0077(5) -0.0008(4) 0.0007(5) O1 0.046(3) 0.044(3) 0.026(3) -0.004(3) 0.008(2) 0.005(3) O1W 0.123(9) 0.097(7) 0.120(8) 0.044(7) -0.015(7) 0.001(7) O2 0.072(4) 0.042(3) 0.022(3) 0.010(3) 0.004(3) 0.015(3) O3 0.057(4) 0.070(4) 0.029(3) -0.018(3) 0.003(3) 0.001(3) O4 0.046(4) 0.057(4) 0.027(3) -0.002(3) 0.006(2) -0.002(3) O5 0.107(3) 0.105(3) 0.105(3) -0.0005(10) 0.0028(10) 0.0000(10) O6 0.114(3) 0.112(3) 0.112(3) -0.0004(10) 0.0026(10) 0.0009(10) O7 0.103(3) 0.105(3) 0.103(3) -0.0005(10) 0.0027(10) -0.0007(10) O8 0.109(3) 0.111(3) 0.109(3) -0.0004(10) 0.0021(10) 0.0001(10) O9 0.045(4) 0.081(5) 0.034(3) 0.021(3) -0.010(3) -0.012(3) O10 0.053(4) 0.037(3) 0.021(3) 0.003(2) -0.010(2) -0.001(3) O11 0.100(6) 0.058(4) 0.043(4) -0.006(3) -0.032(4) 0.002(4) O12 0.101(6) 0.079(5) 0.037(4) 0.022(4) -0.018(4) -0.019(4) O13 0.083(6) 0.172(10) 0.052(5) -0.008(6) -0.001(5) 0.004(6) O14 0.102(3) 0.104(3) 0.101(3) -0.0003(10) 0.0019(10) 0.0012(10) O15 0.115(8) 0.118(8) 0.103(7) 0.026(6) -0.031(6) -0.057(7) O16 0.096(3) 0.095(3) 0.095(3) 0.0002(10) 0.0004(10) -0.0016(10) O17 0.064(5) 0.076(5) 0.058(4) 0.004(4) -0.011(3) -0.027(4) O18 0.043(3) 0.031(3) 0.019(2) -0.003(2) -0.003(2) 0.002(2) O19 0.089(5) 0.040(3) 0.034(3) -0.003(3) -0.013(3) 0.001(3) N1 0.153(10) 0.057(5) 0.034(4) -0.007(4) 0.032(5) 0.000(6) N2 0.068(6) 0.139(10) 0.031(4) -0.009(5) 0.008(4) -0.016(6) N3 0.079(6) 0.088(6) 0.015(3) -0.005(4) -0.015(4) 0.019(5) N4 0.112(8) 0.070(6) 0.046(5) 0.015(5) -0.038(5) -0.026(6) N5 0.043(5) 0.081(7) 0.081(6) 0.008(5) 0.011(4) 0.006(4) N6 0.041(12) 0.11(2) 0.039(12) -0.008(13) 0.011(9) 0.017(12) N6' 0.052(14) 0.078(18) 0.060(18) -0.005(15) 0.021(13) 0.004(11) N7 0.059(5) 0.062(5) 0.028(3) 0.006(3) -0.001(3) 0.016(4) C1 0.065(6) 0.057(6) 0.027(4) -0.013(4) 0.012(4) 0.000(5) C2 0.072(6) 0.043(5) 0.030(4) -0.007(4) 0.004(4) -0.004(4) C3 0.069(6) 0.040(5) 0.031(4) 0.002(4) 0.009(4) 0.003(4) C4 0.049(5) 0.040(4) 0.024(4) -0.001(4) -0.003(3) 0.001(4) C5 0.079(7) 0.044(5) 0.027(4) 0.002(4) 0.008(4) 0.005(5) C6 0.072(7) 0.064(6) 0.032(5) 0.003(5) 0.014(4) -0.001(5) C7 0.037(5) 0.053(5) 0.030(4) -0.014(4) 0.005(3) 0.008(4) C8 0.066(6) 0.052(5) 0.035(5) -0.007(4) 0.007(4) -0.002(5) C9 0.049(6) 0.084(7) 0.034(5) -0.020(5) 0.007(4) -0.008(5) C10 0.060(6) 0.070(7) 0.041(5) -0.009(5) -0.002(4) -0.010(5) C11 0.056(6) 0.044(5) 0.025(4) -0.011(4) 0.006(4) 0.001(4) C12 0.051(5) 0.086(7) 0.022(4) -0.002(4) -0.001(4) 0.001(5) C13 0.057(6) 0.088(8) 0.029(4) -0.009(5) -0.003(4) 0.006(5) C14 0.059(6) 0.045(5) 0.020(4) -0.011(4) -0.006(4) 0.004(4) C15 0.075(7) 0.045(5) 0.024(4) 0.008(4) -0.012(4) 0.000(4) C16 0.072(6) 0.044(5) 0.029(4) 0.007(4) -0.003(4) -0.002(4) C17 0.061(6) 0.041(5) 0.029(4) 0.006(4) -0.013(4) 0.003(4) C18 0.061(6) 0.039(5) 0.031(4) 0.009(4) -0.016(4) -0.012(4) C19 0.052(6) 0.075(7) 0.027(4) 0.009(4) -0.013(4) -0.012(5) C20 0.052(6) 0.079(7) 0.035(5) 0.010(5) -0.017(4) -0.002(5) C21 0.051(5) 0.040(4) 0.024(4) 0.006(4) -0.007(4) -0.006(4) C22 0.056(5) 0.048(5) 0.022(4) 0.002(4) -0.011(3) -0.003(4) C23 0.075(7) 0.048(5) 0.035(4) 0.006(4) -0.021(4) 0.001(5) C24 0.069(6) 0.052(5) 0.031(4) 0.010(4) -0.006(4) -0.006(5) C25 0.063(6) 0.044(5) 0.020(4) 0.002(4) -0.007(4) 0.002(4) C26 0.064(6) 0.043(5) 0.041(5) -0.006(4) -0.020(4) 0.000(4) C27 0.074(7) 0.045(5) 0.035(5) 0.013(4) -0.010(4) -0.005(5) C28 0.073(7) 0.045(5) 0.036(5) -0.005(4) -0.007(4) 0.013(5) C29 0.103(19) 0.051(13) 0.029(10) 0.010(10) -0.023(12) 0.015(12) C31 0.057(15) 0.091(19) 0.061(15) 0.015(16) 0.034(14) 0.026(13) C32 0.11(2) 0.082(17) 0.097(19) -0.018(15) -0.025(16) 0.076(16) C35 0.089(7) 0.089(7) 0.089(7) 0.0000(10) 0.0018(11) 0.0001(10) C36 0.040(12) 0.13(2) 0.077(15) 0.025(15) -0.007(10) 0.031(13) C37 0.067(3) 0.067(3) 0.067(3) 0.0003(6) 0.0012(6) 0.0002(6) N8 0.052(10) 0.044(10) 0.047(10) -0.001(9) -0.009(8) 0.001(9) C30' 0.11(2) 0.12(3) 0.08(2) 0.02(2) 0.007(18) 0.05(2) C31' 0.066(15) 0.087(18) 0.086(18) -0.028(15) 0.000(14) 0.017(13) C32' 0.12(3) 0.13(3) 0.12(3) -0.02(2) 0.07(2) 0.00(2) C33 0.125(14) 0.144(16) 0.125(14) 0.008(13) 0.030(11) 0.052(13) C33' 0.10(2) 0.085(18) 0.078(17) -0.001(15) -0.018(14) 0.005(15) C36' 0.067(3) 0.067(3) 0.067(3) 0.0003(6) 0.0012(6) 0.0002(6) C37' 0.067(3) 0.067(3) 0.067(3) 0.0003(6) 0.0012(6) 0.0002(6) N8' 0.075(16) 0.108(19) 0.046(11) 0.010(14) 0.004(10) 0.048(15) C30 0.059(8) 0.142(14) 0.118(12) -0.052(11) 0.007(8) 0.012(8) C34 0.166(8) 0.166(8) 0.166(8) -0.0001(10) 0.0028(11) 0.0004(10) C38 0.077(7) 0.043(5) 0.037(5) 0.001(4) -0.021(4) 0.000(5) C39 0.085(8) 0.101(10) 0.045(6) 0.032(6) -0.009(6) 0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O18 2.016(5) 3_466 ? Co1 O18 2.016(5) . ? Co1 O1 2.073(5) 3_466 ? Co1 O1 2.073(5) . ? Co1 O10 2.109(5) . ? Co1 O10 2.109(5) 3_466 ? Co2 O18 2.020(5) 3_466 ? Co2 O4 2.070(6) 4_566 ? Co2 N7 2.070(7) 3_556 ? Co2 O19 2.119(6) . ? Co2 O2 2.215(6) . ? Co2 O10 2.281(5) . ? Co3 O3 2.038(5) 2_455 ? Co3 O18 2.043(5) . ? Co3 N5 2.103(9) . ? Co3 O9 2.134(6) . ? Co3 O17 2.159(7) . ? Co3 O1 2.234(6) . ? O1 C7 1.278(10) . ? O1W H1B 0.86(2) . ? O1W H2B 0.85(2) . ? O2 C7 1.262(10) . ? O3 C14 1.278(10) . ? O3 Co3 2.038(5) 2_445 ? O4 C14 1.235(10) . ? O4 Co2 2.070(6) 4_665 ? O5 N1 1.227(12) . ? O6 N1 1.210(13) . ? O7 N2 1.201(13) . ? O8 N2 1.229(13) . ? O9 C21 1.233(10) . ? O10 C21 1.283(10) . ? O11 C28 1.251(12) . ? O12 C28 1.257(12) . ? O13 N3 1.193(11) . ? O14 N3 1.185(11) . ? O15 N4 1.194(13) . ? O16 N4 1.203(12) . ? O18 Co2 2.020(5) 3_466 ? O18 H1A 0.84(2) . ? N1 C2 1.429(13) . ? N2 C9 1.468(13) . ? N3 C16 1.472(13) . ? N4 C23 1.456(13) . ? N5 C29 1.30(2) . ? N5 C30 1.361(18) . ? N5 C30' 1.47(3) . ? N6 C29 1.31(3) . ? N6 C32 1.47(3) . ? N6 C31 1.49(3) . ? N6' C32' 1.36(4) . ? N6' C31' 1.37(4) . ? N6' C30 1.57(3) . ? N7 C37 1.32(3) . ? N7 C37' 1.35(3) . ? N7 C38 1.367(11) . ? N7 Co2 2.070(7) 3_556 ? C1 C6 1.390(14) . ? C1 C2 1.406(13) . ? C1 C8 1.476(12) . ? C2 C3 1.382(12) . ? C3 C4 1.389(12) . ? C3 H3 0.9300 . ? C4 C5 1.386(12) . ? C4 C7 1.495(10) . ? C5 C6 1.351(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.356(14) . ? C8 C9 1.404(13) . ? C9 C10 1.366(13) . ? C10 C11 1.374(13) . ? C10 H10 0.9300 . ? C11 C12 1.409(12) . ? C11 C14 1.500(11) . ? C12 C13 1.378(12) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C20 1.352(14) . ? C15 C16 1.417(13) . ? C15 C22 1.500(10) . ? C16 C17 1.388(11) . ? C17 C18 1.381(13) . ? C17 H17 0.9300 . ? C18 C19 1.371(13) . ? C18 C21 1.507(10) . ? C19 C20 1.406(11) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.386(12) . ? C22 C23 1.403(13) . ? C23 C24 1.379(11) . ? C24 C25 1.346(13) . ? C24 H24 0.9300 . ? C25 C26 1.393(13) . ? C25 C28 1.523(11) . ? C26 C27 1.398(12) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 C30 1.93(3) . ? C31 C30 1.28(3) . ? C35 C36 1.34(4) . ? C35 C34 1.60(4) . ? C36 N8 1.51(3) . ? C37 N8 1.36(3) . ? N8 C39 1.30(2) . ? C30' C31' 1.35(4) . ? C32' C33' 1.64(4) . ? C33 C33' 1.37(3) . ? C33 C34 1.52(3) . ? C36' C34 1.33(3) . ? C36' N8' 1.51(3) . ? C37' N8' 1.35(3) . ? N8' C39 1.49(2) . ? C38 C39 1.371(15) . ? 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 O18 Co1 O18 180.0(3) 3_466 . ? O18 Co1 O1 84.0(2) 3_466 3_466 ? O18 Co1 O1 96.0(2) . 3_466 ? O18 Co1 O1 96.0(2) 3_466 . ? O18 Co1 O1 84.0(2) . . ? O1 Co1 O1 180.0(2) 3_466 . ? O18 Co1 O10 85.4(2) 3_466 . ? O18 Co1 O10 94.6(2) . . ? O1 Co1 O10 87.4(2) 3_466 . ? O1 Co1 O10 92.6(2) . . ? O18 Co1 O10 94.6(2) 3_466 3_466 ? O18 Co1 O10 85.4(2) . 3_466 ? O1 Co1 O10 92.6(2) 3_466 3_466 ? O1 Co1 O10 87.4(2) . 3_466 ? O10 Co1 O10 180.000(1) . 3_466 ? O18 Co2 O4 97.4(2) 3_466 4_566 ? O18 Co2 N7 168.5(3) 3_466 3_556 ? O4 Co2 N7 92.3(3) 4_566 3_556 ? O18 Co2 O19 91.1(2) 3_466 . ? O4 Co2 O19 91.2(3) 4_566 . ? N7 Co2 O19 94.8(3) 3_556 . ? O18 Co2 O2 84.1(2) 3_466 . ? O4 Co2 O2 176.6(2) 4_566 . ? N7 Co2 O2 86.5(3) 3_556 . ? O19 Co2 O2 85.7(2) . . ? O18 Co2 O10 80.91(19) 3_466 . ? O4 Co2 O10 89.0(2) 4_566 . ? N7 Co2 O10 93.3(3) 3_556 . ? O19 Co2 O10 171.9(2) . . ? O2 Co2 O10 94.2(2) . . ? O3 Co3 O18 91.5(2) 2_455 . ? O3 Co3 N5 92.0(3) 2_455 . ? O18 Co3 N5 167.9(3) . . ? O3 Co3 O9 173.7(3) 2_455 . ? O18 Co3 O9 89.4(2) . . ? N5 Co3 O9 88.4(3) . . ? O3 Co3 O17 89.0(3) 2_455 . ? O18 Co3 O17 90.3(3) . . ? N5 Co3 O17 101.3(3) . . ? O9 Co3 O17 84.7(3) . . ? O3 Co3 O1 94.7(2) 2_455 . ? O18 Co3 O1 79.5(2) . . ? N5 Co3 O1 88.7(3) . . ? O9 Co3 O1 91.6(2) . . ? O17 Co3 O1 169.2(3) . . ? C7 O1 Co1 122.8(5) . . ? C7 O1 Co3 134.9(5) . . ? Co1 O1 Co3 90.7(2) . . ? H1B O1W H2B 109(4) . . ? C7 O2 Co2 127.7(5) . . ? C14 O3 Co3 140.6(6) . 2_445 ? C14 O4 Co2 131.4(5) . 4_665 ? C21 O9 Co3 129.7(5) . . ? C21 O10 Co1 124.7(5) . . ? C21 O10 Co2 126.5(5) . . ? Co1 O10 Co2 88.07(18) . . ? Co1 O18 Co2 98.4(2) . 3_466 ? Co1 O18 Co3 98.1(2) . . ? Co2 O18 Co3 129.7(2) 3_466 . ? Co1 O18 H1A 117(8) . . ? Co2 O18 H1A 91(8) 3_466 . ? Co3 O18 H1A 122(8) . . ? O6 N1 O5 119.5(11) . . ? O6 N1 C2 120.2(9) . . ? O5 N1 C2 119.9(10) . . ? O7 N2 O8 119.8(11) . . ? O7 N2 C9 120.3(9) . . ? O8 N2 C9 119.9(9) . . ? O14 N3 O13 120.0(10) . . ? O14 N3 C16 119.0(9) . . ? O13 N3 C16 121.0(7) . . ? O15 N4 O16 120.7(11) . . ? O15 N4 C23 121.0(9) . . ? O16 N4 C23 118.3(10) . . ? C29 N5 C30 93.1(14) . . ? C29 N5 C30' 39.6(16) . . ? C30 N5 C30' 114.9(15) . . ? C29 N5 Co3 128.3(13) . . ? C30 N5 Co3 129.4(9) . . ? C30' N5 Co3 115.8(14) . . ? C29 N6 C32 132(2) . . ? C29 N6 C31 107(2) . . ? C32 N6 C31 122(2) . . ? C32' N6' C31' 128(3) . . ? C32' N6' C30 118(3) . . ? C31' N6' C30 114(2) . . ? C37 N7 C37' 32.7(12) . . ? C37 N7 C38 102.3(13) . . ? C37' N7 C38 107.1(12) . . ? C37 N7 Co2 127.8(11) . 3_556 ? C37' N7 Co2 122.5(11) . 3_556 ? C38 N7 Co2 127.8(7) . 3_556 ? C6 C1 C2 116.1(7) . . ? C6 C1 C8 119.0(8) . . ? C2 C1 C8 124.8(8) . . ? C3 C2 C1 122.1(8) . . ? C3 C2 N1 117.6(8) . . ? C1 C2 N1 120.2(8) . . ? C2 C3 C4 119.6(8) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.5(7) . . ? C5 C4 C7 120.2(8) . . ? C3 C4 C7 121.3(7) . . ? C6 C5 C4 121.5(9) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 122.2(9) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? O2 C7 O1 124.5(7) . . ? O2 C7 C4 119.7(7) . . ? O1 C7 C4 115.8(7) . . ? C13 C8 C9 115.3(8) . . ? C13 C8 C1 119.0(8) . . ? C9 C8 C1 124.8(9) . . ? C10 C9 C8 122.9(9) . . ? C10 C9 N2 116.2(8) . . ? C8 C9 N2 120.9(8) . . ? C9 C10 C11 119.8(8) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 118.6(8) . . ? C10 C11 C14 120.3(8) . . ? C12 C11 C14 121.0(8) . . ? C13 C12 C11 118.7(9) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C8 C13 C12 123.9(9) . . ? C8 C13 H13 118.1 . . ? C12 C13 H13 118.1 . . ? O4 C14 O3 127.6(7) . . ? O4 C14 C11 119.7(7) . . ? O3 C14 C11 112.6(8) . . ? C20 C15 C16 116.3(8) . . ? C20 C15 C22 117.9(8) . . ? C16 C15 C22 125.8(8) . . ? C17 C16 C15 122.4(9) . . ? C17 C16 N3 115.6(8) . . ? C15 C16 N3 122.0(7) . . ? C18 C17 C16 118.7(8) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 120.1(8) . . ? C19 C18 C21 119.9(8) . . ? C17 C18 C21 119.9(8) . . ? C18 C19 C20 119.8(9) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C15 C20 C19 122.4(9) . . ? C15 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? O9 C21 O10 126.0(7) . . ? O9 C21 C18 118.6(7) . . ? O10 C21 C18 115.5(7) . . ? C27 C22 C23 116.0(7) . . ? C27 C22 C15 118.8(8) . . ? C23 C22 C15 125.1(8) . . ? C24 C23 C22 122.6(9) . . ? C24 C23 N4 116.1(8) . . ? C22 C23 N4 121.3(7) . . ? C25 C24 C23 120.8(8) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 118.7(7) . . ? C24 C25 C28 118.7(8) . . ? C26 C25 C28 122.5(8) . . ? C25 C26 C27 120.7(8) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C22 C27 C26 121.0(8) . . ? C22 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? O11 C28 O12 126.8(9) . . ? O11 C28 C25 117.5(9) . . ? O12 C28 C25 115.7(8) . . ? N5 C29 N6 118(2) . . ? N5 C29 C30 44.7(9) . . ? N6 C29 C30 74.2(16) . . ? C30 C31 N6 93(2) . . ? C36 C35 C34 115(2) . . ? C35 C36 N8 122(2) . . ? N7 C37 N8 112(2) . . ? C39 N8 C37 106.9(18) . . ? C39 N8 C36 126.2(17) . . ? C37 N8 C36 126(2) . . ? C31' C30' N5 108(3) . . ? C30' C31' N6' 105(2) . . ? N6' C32' C33' 110(2) . . ? C33' C33 C34 126(2) . . ? C33 C33' C32' 113(2) . . ? C34 C36' N8' 125(2) . . ? N7 C37' N8' 110.2(19) . . ? C37' N8' C39 106.3(17) . . ? C37' N8' C36' 124(2) . . ? C39 N8' C36' 129.2(18) . . ? C31 C30 N5 128(2) . . ? C31 C30 N6' 34.2(13) . . ? N5 C30 N6' 95.4(16) . . ? C31 C30 C29 86.0(18) . . ? N5 C30 C29 42.2(10) . . ? N6' C30 C29 56.8(14) . . ? C36' C34 C33 144(2) . . ? C36' C34 C35 54.4(17) . . ? C33 C34 C35 103(2) . . ? N7 C38 C39 110.1(9) . . ? N8 C39 C38 106.0(11) . . ? N8 C39 N8' 35.7(11) . . ? C38 C39 N8' 102.1(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2B O17 0.85(2) 2.00(6) 2.764(12) 148(10) 3_566 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.271 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.135 #=========================END data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 806101' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C39 H31 Cu2.50 N8 O18' _chemical_formula_sum 'C39 H31 Cu2.50 N8 O18' _chemical_formula_weight 1058.57 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 11.6736(4) _cell_length_b 28.3206(8) _cell_length_c 13.2080(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.597(2) _cell_angle_gamma 90.00 _cell_volume 4184.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7745 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 25.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2150 _exptl_absorpt_coefficient_mu 1.353 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24473 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.48 _reflns_number_total 7745 _reflns_number_gt 5206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7745 _refine_ls_number_parameters 619 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.003 _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 0.78172(4) 0.020570(13) 2.03783(3) 0.02306(12) Uani 1 1 d . . . Cu2 Cu 0.63657(4) -0.009724(14) 1.80027(3) 0.02499(12) Uani 1 1 d . . . Cu3 Cu 0.5000 0.0000 2.0000 0.01971(15) Uani 1 2 d S . . O1 O 0.6056(2) 0.05843(8) 1.80399(18) 0.0331(6) Uani 1 1 d . . . O2 O 0.7556(2) 0.07791(8) 1.94719(19) 0.0286(6) Uani 1 1 d . . . O3 O 0.5774(2) 0.46269(8) 1.7296(2) 0.0367(7) Uani 1 1 d . . . O4 O 0.5781(2) 0.44321(8) 1.5653(2) 0.0343(7) Uani 1 1 d . . . O5 O 0.3872(3) 0.17823(11) 1.5790(3) 0.0695(11) Uani 1 1 d . . . O6 O 0.4154(3) 0.25164(10) 1.6146(2) 0.0582(9) Uani 1 1 d . . . O7 O 0.5937(4) 0.33460(13) 1.9789(3) 0.0861(13) Uani 1 1 d . . . O8 O 0.5307(3) 0.26673(11) 1.9152(3) 0.0627(10) Uani 1 1 d . . . O9 O 0.9798(3) -0.05892(11) 2.1106(3) 0.0746(11) Uani 1 1 d . . . O10 O 0.8057(2) -0.03486(8) 2.13259(18) 0.0290(6) Uani 1 1 d . . . O11 O 0.7079(3) -0.39866(9) 2.4479(2) 0.0503(9) Uani 1 1 d . . . O12 O 0.6676(2) -0.42256(8) 2.28127(18) 0.0287(6) Uani 1 1 d . . . O13 O 1.1557(3) -0.18962(13) 2.3561(4) 0.0958(14) Uani 1 1 d . . . O14 O 1.0645(3) -0.25472(10) 2.3123(3) 0.0742(11) Uani 1 1 d . . . O15 O 0.9685(4) -0.26342(12) 2.5518(3) 0.0917(14) Uani 1 1 d . . . O16 O 0.9053(4) -0.20114(11) 2.4653(2) 0.0796(13) Uani 1 1 d . . . O17 O 0.8661(3) -0.00799(10) 1.9047(3) 0.0447(7) Uani 1 1 d D . . O18 O 0.6398(2) -0.01347(7) 1.95016(17) 0.0193(5) Uani 1 1 d D . . N1 N 0.4440(3) 0.21071(12) 1.6302(3) 0.0386(8) Uani 1 1 d . . . N2 N 0.5721(3) 0.30555(13) 1.9082(3) 0.0452(9) Uani 1 1 d . . . N3 N 1.0663(3) -0.21201(12) 2.3140(3) 0.0478(9) Uani 1 1 d . . . N4 N 0.9117(3) -0.24350(11) 2.4725(3) 0.0414(9) Uani 1 1 d . . . N5 N 0.6444(3) -0.00070(10) 1.6537(2) 0.0326(8) Uani 1 1 d . . . N6 N 0.6569(3) -0.01942(11) 1.4954(2) 0.0378(8) Uani 1 1 d . . . N7 N 1.1143(3) -0.06133(10) 1.8527(2) 0.0319(8) Uani 1 1 d . . . N8 N 1.0749(3) -0.10210(12) 1.7049(3) 0.0469(9) Uani 1 1 d . . . C1 C 0.6338(3) 0.23373(12) 1.7680(3) 0.0310(9) Uani 1 1 d . . . C2 C 0.5529(3) 0.19906(12) 1.7166(3) 0.0276(8) Uani 1 1 d . . . C3 C 0.5678(3) 0.15213(12) 1.7461(3) 0.0276(8) Uani 1 1 d . . . H3 H 0.5131 0.1298 1.7098 0.080 Uiso 1 1 calc . . . C4 C 0.6635(3) 0.13832(11) 1.8291(3) 0.0258(8) Uani 1 1 d . . . C5 C 0.7467(4) 0.17186(13) 1.8803(3) 0.0356(10) Uani 1 1 d . . . H5 H 0.8124 0.1629 1.9354 0.080 Uiso 1 1 calc . . . C6 C 0.7316(4) 0.21842(13) 1.8492(3) 0.0415(11) Uani 1 1 d . . . H6 H 0.7888 0.2404 1.8835 0.080 Uiso 1 1 calc . . . C7 C 0.6760(3) 0.08699(12) 1.8634(3) 0.0246(8) Uani 1 1 d . . . C8 C 0.6225(3) 0.28537(12) 1.7417(3) 0.0296(9) Uani 1 1 d . . . C9 C 0.5969(3) 0.31919(12) 1.8086(3) 0.0276(8) Uani 1 1 d . . . C10 C 0.5883(3) 0.36687(12) 1.7843(3) 0.0273(8) Uani 1 1 d . . . H10 H 0.5704 0.3885 1.8305 0.080 Uiso 1 1 calc . . . C11 C 0.6066(3) 0.38210(11) 1.6908(3) 0.0254(8) Uani 1 1 d . . . C12 C 0.6380(4) 0.34948(13) 1.6250(3) 0.0352(10) Uani 1 1 d . . . H12 H 0.6526 0.3596 1.5629 0.080 Uiso 1 1 calc . . . C13 C 0.6476(4) 0.30192(13) 1.6509(3) 0.0375(10) Uani 1 1 d . . . H13 H 0.6712 0.2807 1.6070 0.080 Uiso 1 1 calc . . . C14 C 0.5867(3) 0.43386(12) 1.6625(3) 0.0260(8) Uani 1 1 d . . . C15 C 0.8444(3) -0.20583(11) 2.2484(3) 0.0254(8) Uani 1 1 d . . . C16 C 0.9565(3) -0.18568(12) 2.2619(3) 0.0285(8) Uani 1 1 d . . . C17 C 0.9711(3) -0.14046(12) 2.2270(3) 0.0294(9) Uani 1 1 d . . . H17 H 1.0474 -0.1287 2.2344 0.080 Uiso 1 1 calc . . . C18 C 0.8714(3) -0.11292(12) 2.1812(3) 0.0249(8) Uani 1 1 d . . . C19 C 0.7589(3) -0.13144(12) 2.1698(3) 0.0280(8) Uani 1 1 d . . . H19 H 0.6916 -0.1130 2.1409 0.080 Uiso 1 1 calc . . . C20 C 0.7457(3) -0.17750(12) 2.2014(3) 0.0292(9) Uani 1 1 d . . . H20 H 0.6692 -0.1897 2.1908 0.080 Uiso 1 1 calc . . . C21 C 0.8885(4) -0.06475(12) 2.1389(3) 0.0328(9) Uani 1 1 d . . . C22 C 0.8185(3) -0.25496(11) 2.2793(3) 0.0260(8) Uani 1 1 d . . . C23 C 0.8464(3) -0.27258(12) 2.3823(3) 0.0262(8) Uani 1 1 d . . . C24 C 0.8103(3) -0.31634(12) 2.4062(3) 0.0276(8) Uani 1 1 d . . . H24 H 0.8292 -0.3264 2.4760 0.080 Uiso 1 1 calc . . . C25 C 0.7452(3) -0.34556(11) 2.3252(3) 0.0242(8) Uani 1 1 d . . . C26 C 0.7204(3) -0.32975(12) 2.2215(3) 0.0279(8) Uani 1 1 d . . . H26 H 0.6800 -0.3494 2.1665 0.080 Uiso 1 1 calc . . . C27 C 0.7552(3) -0.28513(12) 2.1993(3) 0.0313(9) Uani 1 1 d . . . H27 H 0.7359 -0.2750 2.1294 0.080 Uiso 1 1 calc . . . C28 C 0.7048(3) -0.39273(11) 2.3553(3) 0.0247(8) Uani 1 1 d . . . C29 C 0.6438(4) -0.03529(13) 1.5865(3) 0.0404(11) Uani 1 1 d . . . H29 H 0.6352 -0.0670 1.6009 0.080 Uiso 1 1 calc . . . C30 C 0.6591(5) 0.03967(14) 1.6010(3) 0.0488(12) Uani 1 1 d . . . H30 H 0.6631 0.0701 1.6282 0.080 Uiso 1 1 calc . . . C31 C 0.6670(4) 0.02847(15) 1.5038(3) 0.0490(12) Uani 1 1 d . . . H31 H 0.6772 0.0493 1.4526 0.080 Uiso 1 1 calc . . . C32 C 0.6721(5) -0.04884(15) 1.4080(3) 0.0488(12) Uani 1 1 d . . . H32A H 0.6292 -0.0346 1.3411 0.080 Uiso 1 1 calc . . . H32B H 0.6382 -0.0798 1.4116 0.080 Uiso 1 1 calc . . . C33 C 0.8017(5) -0.05393(18) 1.4129(3) 0.0620(14) Uani 1 1 d . . . H33A H 0.8365 -0.0227 1.4151 0.080 Uiso 1 1 calc . . . H33B H 0.8072 -0.0693 1.3488 0.080 Uiso 1 1 calc . . . C34 C 0.8747(5) -0.08219(17) 1.5081(4) 0.0582(13) Uani 1 1 d . . . H34A H 0.8689 -0.0670 1.5722 0.080 Uiso 1 1 calc . . . H34B H 0.8404 -0.1135 1.5056 0.080 Uiso 1 1 calc . . . C35 C 1.0039(5) -0.0868(2) 1.5129(4) 0.0730(17) Uani 1 1 d . . . H35A H 1.0089 -0.0991 1.4458 0.080 Uiso 1 1 calc . . . H35B H 1.0392 -0.0555 1.5213 0.080 Uiso 1 1 calc . . . C36 C 1.0768(5) -0.1176(2) 1.5990(4) 0.0742(17) Uani 1 1 d . . . H36A H 1.0468 -0.1496 1.5874 0.080 Uiso 1 1 calc . . . H36B H 1.1588 -0.1178 1.5958 0.080 Uiso 1 1 calc . . . C37 C 1.1252(3) -0.06302(13) 1.7558(3) 0.0358(10) Uani 1 1 d . . . H37 H 1.1630 -0.0400 1.7267 0.080 Uiso 1 1 calc . . . C38 C 1.0532(4) -0.10158(14) 1.8646(4) 0.0451(11) Uani 1 1 d . . . H38 H 1.0327 -0.1101 1.9251 0.080 Uiso 1 1 calc . . . C39 C 1.0280(4) -0.12661(15) 1.7740(4) 0.0577(14) Uani 1 1 d . . . H39 H 0.9866 -0.1551 1.7606 0.080 Uiso 1 1 calc . . . H1A H 0.665(4) -0.0411(9) 1.960(4) 0.080 Uiso 1 1 d D . . H2A H 0.912(4) 0.0091(13) 1.878(3) 0.080 Uiso 1 1 d D . . H2B H 0.910(4) -0.0295(12) 1.940(3) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0290(3) 0.0105(2) 0.0273(2) 0.00339(17) 0.00428(19) -0.00249(17) Cu2 0.0410(3) 0.0107(2) 0.0243(2) -0.00023(17) 0.0111(2) 0.00280(18) Cu3 0.0247(3) 0.0113(3) 0.0254(3) -0.0066(2) 0.0109(3) -0.0037(2) O1 0.0512(18) 0.0118(12) 0.0303(15) 0.0005(11) 0.0019(13) 0.0006(12) O2 0.0352(16) 0.0135(12) 0.0345(15) 0.0071(10) 0.0061(12) -0.0003(11) O3 0.0480(18) 0.0145(13) 0.0434(16) -0.0006(12) 0.0064(13) 0.0030(12) O4 0.0450(18) 0.0220(14) 0.0462(17) 0.0195(12) 0.0294(14) 0.0152(12) O5 0.064(2) 0.047(2) 0.072(2) 0.0095(17) -0.0219(18) -0.0075(17) O6 0.054(2) 0.0353(19) 0.076(2) 0.0168(16) 0.0041(17) 0.0193(15) O7 0.155(4) 0.073(3) 0.039(2) 0.0006(19) 0.040(2) -0.011(3) O8 0.087(3) 0.041(2) 0.077(2) 0.0290(17) 0.050(2) 0.0078(18) O9 0.059(2) 0.0410(19) 0.142(3) 0.047(2) 0.056(2) 0.0048(17) O10 0.0425(17) 0.0143(12) 0.0283(14) 0.0035(10) 0.0072(12) -0.0031(11) O11 0.104(3) 0.0206(14) 0.0277(16) 0.0007(12) 0.0205(16) -0.0235(15) O12 0.0448(17) 0.0147(12) 0.0277(14) -0.0013(10) 0.0121(12) -0.0068(11) O13 0.044(2) 0.054(2) 0.157(4) 0.022(2) -0.021(2) -0.0049(18) O14 0.047(2) 0.0278(18) 0.148(3) 0.0281(19) 0.027(2) 0.0112(15) O15 0.131(4) 0.063(2) 0.048(2) 0.0119(19) -0.029(2) -0.040(2) O16 0.148(4) 0.0298(19) 0.050(2) -0.0087(15) 0.010(2) -0.031(2) O17 0.0396(18) 0.0316(17) 0.071(2) 0.0018(14) 0.0297(16) -0.0017(13) O18 0.0250(14) 0.0106(11) 0.0242(12) -0.0019(10) 0.0098(10) 0.0003(10) N1 0.037(2) 0.036(2) 0.041(2) 0.0113(16) 0.0092(17) 0.0066(17) N2 0.060(3) 0.038(2) 0.044(2) 0.0181(18) 0.0256(19) 0.0108(19) N3 0.039(2) 0.029(2) 0.075(3) 0.0164(18) 0.015(2) 0.0037(17) N4 0.060(3) 0.027(2) 0.035(2) -0.0004(15) 0.0104(18) -0.0176(17) N5 0.048(2) 0.0204(17) 0.0300(17) 0.0025(13) 0.0117(15) 0.0028(14) N6 0.053(2) 0.034(2) 0.0260(18) -0.0005(15) 0.0117(16) 0.0058(16) N7 0.035(2) 0.0187(16) 0.0357(19) 0.0014(13) -0.0006(15) -0.0039(13) N8 0.040(2) 0.035(2) 0.054(2) -0.0190(18) -0.0052(18) 0.0005(17) C1 0.039(2) 0.0144(19) 0.041(2) 0.0097(16) 0.0141(19) 0.0040(16) C2 0.034(2) 0.0200(19) 0.029(2) 0.0065(15) 0.0101(17) 0.0076(16) C3 0.036(2) 0.0173(18) 0.029(2) 0.0023(15) 0.0084(17) 0.0002(16) C4 0.037(2) 0.0123(17) 0.030(2) 0.0010(14) 0.0129(17) 0.0017(15) C5 0.036(2) 0.021(2) 0.042(2) 0.0084(17) -0.0003(19) 0.0031(17) C6 0.044(3) 0.017(2) 0.054(3) 0.0094(18) -0.001(2) -0.0050(18) C7 0.034(2) 0.0156(18) 0.029(2) 0.0040(15) 0.0171(18) 0.0050(16) C8 0.035(2) 0.0150(18) 0.039(2) 0.0077(16) 0.0103(18) 0.0045(16) C9 0.030(2) 0.0234(19) 0.029(2) 0.0115(15) 0.0080(17) 0.0047(16) C10 0.032(2) 0.0187(19) 0.029(2) 0.0048(15) 0.0057(17) 0.0035(15) C11 0.028(2) 0.0160(18) 0.033(2) 0.0093(15) 0.0096(17) 0.0053(15) C12 0.050(3) 0.022(2) 0.041(2) 0.0107(17) 0.024(2) 0.0071(18) C13 0.054(3) 0.022(2) 0.041(2) 0.0053(17) 0.021(2) 0.0093(18) C14 0.020(2) 0.0196(19) 0.039(2) 0.0106(17) 0.0104(16) 0.0045(15) C15 0.036(2) 0.0153(17) 0.026(2) 0.0003(14) 0.0107(17) -0.0034(16) C16 0.032(2) 0.0191(19) 0.035(2) 0.0048(15) 0.0102(17) 0.0031(16) C17 0.033(2) 0.0204(19) 0.036(2) 0.0039(16) 0.0119(18) -0.0042(16) C18 0.037(2) 0.0158(18) 0.024(2) 0.0033(14) 0.0127(17) -0.0026(16) C19 0.035(2) 0.0186(19) 0.032(2) 0.0023(15) 0.0112(17) -0.0007(16) C20 0.030(2) 0.024(2) 0.033(2) 0.0052(16) 0.0086(17) -0.0044(16) C21 0.042(3) 0.018(2) 0.039(2) 0.0075(16) 0.012(2) -0.0050(18) C22 0.035(2) 0.0132(17) 0.032(2) 0.0057(15) 0.0123(17) -0.0004(15) C23 0.032(2) 0.0186(18) 0.027(2) -0.0008(15) 0.0065(16) -0.0055(16) C24 0.035(2) 0.0170(18) 0.029(2) 0.0058(15) 0.0062(17) -0.0038(16) C25 0.032(2) 0.0126(17) 0.029(2) 0.0041(14) 0.0105(16) 0.0011(15) C26 0.039(2) 0.0158(18) 0.028(2) 0.0014(15) 0.0079(17) -0.0044(16) C27 0.043(3) 0.022(2) 0.027(2) 0.0056(16) 0.0088(18) -0.0045(17) C28 0.033(2) 0.0130(17) 0.029(2) 0.0031(15) 0.0115(17) -0.0021(15) C29 0.065(3) 0.030(2) 0.027(2) -0.0001(17) 0.015(2) 0.002(2) C30 0.088(4) 0.023(2) 0.040(3) 0.0086(18) 0.027(3) 0.008(2) C31 0.075(4) 0.033(2) 0.045(3) 0.015(2) 0.027(2) 0.010(2) C32 0.073(4) 0.050(3) 0.020(2) -0.0029(19) 0.006(2) 0.012(2) C33 0.080(4) 0.073(4) 0.038(3) -0.016(2) 0.025(3) 0.005(3) C34 0.061(4) 0.056(3) 0.056(3) -0.008(2) 0.014(3) 0.004(3) C35 0.063(4) 0.105(5) 0.050(3) -0.037(3) 0.014(3) 0.003(3) C36 0.051(3) 0.083(4) 0.074(4) -0.049(3) -0.004(3) 0.008(3) C37 0.030(2) 0.025(2) 0.043(3) -0.0060(18) -0.0043(19) -0.0006(17) C38 0.037(3) 0.024(2) 0.066(3) 0.005(2) 0.001(2) -0.0123(18) C39 0.043(3) 0.022(2) 0.092(4) -0.007(2) -0.007(3) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N7 1.973(3) 3_759 ? Cu1 O10 1.977(2) . ? Cu1 O18 1.980(2) . ? Cu1 O2 1.989(2) . ? Cu1 O17 2.389(3) . ? Cu2 O1 1.967(2) . ? Cu2 O18 1.972(2) . ? Cu2 N5 1.980(3) . ? Cu2 O12 1.981(2) 4 ? Cu3 O4 1.927(2) 2_648 ? Cu3 O4 1.927(2) 4_566 ? Cu3 O18 1.963(2) . ? Cu3 O18 1.963(2) 3_659 ? O1 C7 1.256(4) . ? O2 C7 1.252(4) . ? O3 C14 1.232(4) . ? O4 C14 1.286(4) . ? O4 Cu3 1.927(2) 2_658 ? O5 N1 1.219(4) . ? O6 N1 1.208(4) . ? O7 N2 1.216(4) . ? O8 N2 1.215(4) . ? O9 C21 1.237(5) . ? O10 C21 1.269(4) . ? O11 C28 1.225(4) . ? O12 C28 1.271(4) . ? O12 Cu2 1.981(2) 4_556 ? O13 N3 1.212(5) . ? O14 N3 1.210(4) . ? O15 N4 1.208(4) . ? O16 N4 1.204(4) . ? O17 H2A 0.865(19) . ? O17 H2B 0.846(19) . ? O18 H1A 0.831(19) . ? N1 C2 1.482(5) . ? N2 C9 1.477(5) . ? N3 C16 1.473(5) . ? N4 C23 1.470(5) . ? N5 C29 1.321(5) . ? N5 C30 1.375(5) . ? N6 C29 1.334(5) . ? N6 C31 1.363(5) . ? N6 C32 1.475(5) . ? N7 C37 1.323(5) . ? N7 C38 1.377(5) . ? N7 Cu1 1.973(3) 3_759 ? N8 C37 1.340(5) . ? N8 C39 1.379(6) . ? N8 C36 1.473(6) . ? C1 C6 1.393(5) . ? C1 C2 1.397(5) . ? C1 C8 1.500(4) . ? C2 C3 1.382(5) . ? C3 C4 1.380(5) . ? C3 H3 0.9300 . ? C4 C5 1.388(5) . ? C4 C7 1.517(4) . ? C5 C6 1.378(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.392(5) . ? C8 C13 1.395(5) . ? C9 C10 1.385(5) . ? C10 C11 1.381(5) . ? C10 H10 0.9300 . ? C11 C12 1.387(5) . ? C11 C14 1.514(4) . ? C12 C13 1.387(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.392(5) . ? C15 C20 1.396(5) . ? C15 C22 1.504(4) . ? C16 C17 1.388(5) . ? C17 C18 1.388(5) . ? C17 H17 0.9300 . ? C18 C19 1.382(5) . ? C18 C21 1.509(5) . ? C19 C20 1.391(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.395(5) . ? C22 C23 1.397(5) . ? C23 C24 1.374(5) . ? C24 C25 1.393(5) . ? C24 H24 0.9300 . ? C25 C26 1.390(5) . ? C25 C28 1.508(4) . ? C26 C27 1.384(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.351(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.502(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.528(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.497(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.492(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37 0.9300 . ? C38 C39 1.349(6) . ? C38 H38 0.9300 . ? 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 N7 Cu1 O10 93.12(11) 3_759 . ? N7 Cu1 O18 161.86(12) 3_759 . ? O10 Cu1 O18 85.82(10) . . ? N7 Cu1 O2 85.40(11) 3_759 . ? O10 Cu1 O2 177.56(10) . . ? O18 Cu1 O2 94.98(9) . . ? N7 Cu1 O17 116.15(12) 3_759 . ? O10 Cu1 O17 100.57(10) . . ? O18 Cu1 O17 81.78(10) . . ? O2 Cu1 O17 81.83(10) . . ? O1 Cu2 O18 88.78(9) . . ? O1 Cu2 N5 87.59(11) . . ? O18 Cu2 N5 174.39(12) . . ? O1 Cu2 O12 174.13(10) . 4 ? O18 Cu2 O12 97.09(9) . 4 ? N5 Cu2 O12 86.55(11) . 4 ? O4 Cu3 O4 180.00(8) 2_648 4_566 ? O4 Cu3 O18 91.13(10) 2_648 . ? O4 Cu3 O18 88.87(10) 4_566 . ? O4 Cu3 O18 88.87(10) 2_648 3_659 ? O4 Cu3 O18 91.13(10) 4_566 3_659 ? O18 Cu3 O18 180.000(1) . 3_659 ? C7 O1 Cu2 123.7(2) . . ? C7 O2 Cu1 130.3(2) . . ? C14 O4 Cu3 120.7(2) . 2_658 ? C21 O10 Cu1 122.6(2) . . ? C28 O12 Cu2 125.5(2) . 4_556 ? Cu1 O17 H2A 123(3) . . ? Cu1 O17 H2B 98(3) . . ? H2A O17 H2B 107(3) . . ? Cu3 O18 Cu2 123.15(12) . . ? Cu3 O18 Cu1 110.25(10) . . ? Cu2 O18 Cu1 109.49(10) . . ? Cu3 O18 H1A 115(4) . . ? Cu2 O18 H1A 96(3) . . ? Cu1 O18 H1A 100(4) . . ? O6 N1 O5 123.3(4) . . ? O6 N1 C2 118.7(3) . . ? O5 N1 C2 118.0(3) . . ? O8 N2 O7 123.5(4) . . ? O8 N2 C9 119.2(4) . . ? O7 N2 C9 117.2(4) . . ? O14 N3 O13 122.7(4) . . ? O14 N3 C16 119.3(4) . . ? O13 N3 C16 118.0(3) . . ? O16 N4 O15 122.7(4) . . ? O16 N4 C23 119.3(3) . . ? O15 N4 C23 118.1(3) . . ? C29 N5 C30 104.7(3) . . ? C29 N5 Cu2 124.7(3) . . ? C30 N5 Cu2 130.5(3) . . ? C29 N6 C31 106.9(3) . . ? C29 N6 C32 125.9(3) . . ? C31 N6 C32 126.8(3) . . ? C37 N7 C38 106.0(3) . . ? C37 N7 Cu1 121.4(3) . 3_759 ? C38 N7 Cu1 129.1(3) . 3_759 ? C37 N8 C39 106.5(4) . . ? C37 N8 C36 126.8(4) . . ? C39 N8 C36 126.6(4) . . ? C6 C1 C2 116.6(3) . . ? C6 C1 C8 118.7(3) . . ? C2 C1 C8 124.8(3) . . ? C3 C2 C1 121.7(3) . . ? C3 C2 N1 116.2(3) . . ? C1 C2 N1 122.0(3) . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.2(3) . . ? C3 C4 C7 119.7(3) . . ? C5 C4 C7 121.1(3) . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 122.3(4) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? O2 C7 O1 127.5(3) . . ? O2 C7 C4 116.4(3) . . ? O1 C7 C4 116.1(3) . . ? C9 C8 C13 116.8(3) . . ? C9 C8 C1 123.0(3) . . ? C13 C8 C1 120.0(3) . . ? C10 C9 C8 122.5(3) . . ? C10 C9 N2 116.3(3) . . ? C8 C9 N2 121.2(3) . . ? C11 C10 C9 119.5(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 119.2(3) . . ? C10 C11 C14 118.1(3) . . ? C12 C11 C14 122.7(3) . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C8 121.1(3) . . ? C12 C13 H13 119.5 . . ? C8 C13 H13 119.5 . . ? O3 C14 O4 125.7(3) . . ? O3 C14 C11 120.2(3) . . ? O4 C14 C11 114.1(3) . . ? C16 C15 C20 116.6(3) . . ? C16 C15 C22 126.8(3) . . ? C20 C15 C22 116.6(3) . . ? C17 C16 C15 122.4(3) . . ? C17 C16 N3 116.7(3) . . ? C15 C16 N3 120.9(3) . . ? C16 C17 C18 119.8(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 119.1(3) . . ? C19 C18 C21 121.6(3) . . ? C17 C18 C21 119.1(3) . . ? C18 C19 C20 120.5(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 121.6(3) . . ? C19 C20 H20 119.2 . . ? C15 C20 H20 119.2 . . ? O9 C21 O10 126.6(3) . . ? O9 C21 C18 116.7(3) . . ? O10 C21 C18 116.7(3) . . ? C27 C22 C23 116.4(3) . . ? C27 C22 C15 117.7(3) . . ? C23 C22 C15 125.8(3) . . ? C24 C23 C22 123.0(3) . . ? C24 C23 N4 116.2(3) . . ? C22 C23 N4 120.8(3) . . ? C23 C24 C25 119.7(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 118.6(3) . . ? C26 C25 C28 123.5(3) . . ? C24 C25 C28 117.8(3) . . ? C27 C26 C25 120.8(3) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C22 121.5(3) . . ? C26 C27 H27 119.3 . . ? C22 C27 H27 119.3 . . ? O11 C28 O12 125.7(3) . . ? O11 C28 C25 117.6(3) . . ? O12 C28 C25 116.7(3) . . ? N5 C29 N6 112.1(3) . . ? N5 C29 H29 123.9 . . ? N6 C29 H29 123.9 . . ? C31 C30 N5 109.8(3) . . ? C31 C30 H30 125.1 . . ? N5 C30 H30 125.1 . . ? C30 C31 N6 106.5(3) . . ? C30 C31 H31 126.8 . . ? N6 C31 H31 126.8 . . ? N6 C32 C33 111.4(4) . . ? N6 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? N6 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C32 C33 C34 113.8(4) . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33B 108.8 . . ? C34 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C35 C34 C33 113.5(4) . . ? C35 C34 H34A 108.9 . . ? C33 C34 H34A 108.9 . . ? C35 C34 H34B 108.9 . . ? C33 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C34 115.6(5) . . ? C36 C35 H35A 108.4 . . ? C34 C35 H35A 108.4 . . ? C36 C35 H35B 108.4 . . ? C34 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? N8 C36 C35 113.0(4) . . ? N8 C36 H36A 109.0 . . ? C35 C36 H36A 109.0 . . ? N8 C36 H36B 109.0 . . ? C35 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? N7 C37 N8 111.4(4) . . ? N7 C37 H37 124.3 . . ? N8 C37 H37 124.3 . . ? C39 C38 N7 108.9(4) . . ? C39 C38 H38 125.6 . . ? N7 C38 H38 125.6 . . ? C38 C39 N8 107.1(4) . . ? C38 C39 H39 126.4 . . ? N8 C39 H39 126.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.473 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.100 #=========================END data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 806102' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C39 H29 N8 O17 Zn2.50' _chemical_formula_sum 'C39 H29 N8 O17 Zn2.50' _chemical_formula_weight 1045.13 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' Zn Zn 0.2839 1.4301 '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 10.821(2) _cell_length_b 13.850(3) _cell_length_c 14.788(3) _cell_angle_alpha 70.17(3) _cell_angle_beta 82.92(3) _cell_angle_gamma 85.58(3) _cell_volume 2067.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9345 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20515 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9345 _reflns_number_gt 8289 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+2.4351P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9345 _refine_ls_number_parameters 609 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Zn1 Zn 1.0000 1.0000 0.0000 0.01781(9) Uani 1 2 d S . . Zn2 Zn 1.15185(3) 0.98457(2) 0.208727(19) 0.02240(8) Uani 1 1 d . . . Zn3 Zn 1.30704(3) 0.98160(2) -0.007480(19) 0.02279(8) Uani 1 1 d . . . O1 O 1.10383(19) 1.11524(15) -0.11337(15) 0.0393(5) Uani 1 1 d . . . O2 O 1.30023(19) 1.06329(15) -0.14370(13) 0.0345(4) Uani 1 1 d . . . O3 O 1.1813(2) 1.76108(14) -0.82699(13) 0.0349(4) Uani 1 1 d . . . O4 O 1.2404(2) 1.84028(14) -0.73141(14) 0.0384(5) Uani 1 1 d . . . O5 O 1.4730(3) 1.3801(3) -0.5394(3) 0.0958(13) Uani 1 1 d . . . O6 O 1.5066(3) 1.2213(2) -0.4677(2) 0.0848(11) Uani 1 1 d . . . O7 O 1.2430(4) 1.3046(2) -0.5950(2) 0.0919(13) Uani 1 1 d . . . O8 O 1.1441(3) 1.3942(3) -0.7123(3) 0.0826(9) Uiso 1 1 d . . . O9 O 1.05009(18) 1.12955(14) 0.15139(14) 0.0314(4) Uani 1 1 d . . . O10 O 0.92200(19) 1.11325(15) 0.05055(15) 0.0360(5) Uani 1 1 d . . . O11 O 0.58970(18) 1.92771(13) -0.02936(14) 0.0312(4) Uani 1 1 d . . . O12 O 0.40720(17) 1.85286(13) 0.01453(15) 0.0318(4) Uani 1 1 d . . . O13 O 0.8263(7) 1.5092(3) 0.2436(4) 0.173(3) Uani 1 1 d . . . O14 O 0.8594(4) 1.3573(3) 0.3275(3) 0.1054(15) Uani 1 1 d . . . O15 O 0.5712(3) 1.40054(19) 0.2218(3) 0.0759(10) Uani 1 1 d . . . O16 O 0.4032(11) 1.4788(9) 0.1779(9) 0.054(3) Uani 0.50 1 d P . . O16' O 0.4101(13) 1.4750(12) 0.1575(14) 0.128(7) Uani 0.50 1 d P . . O17 O 1.15598(15) 0.96044(12) 0.08171(11) 0.0180(3) Uani 1 1 d D . . N1 N 1.4425(3) 1.2985(2) -0.4791(2) 0.0610(9) Uani 1 1 d . . . N2 N 1.1915(4) 1.3861(2) -0.6406(2) 0.0572(9) Uani 1 1 d . . . N3 N 0.8441(5) 1.4232(3) 0.2506(3) 0.0885(15) Uani 1 1 d . . . N4 N 0.5161(3) 1.47410(18) 0.1708(2) 0.0483(7) Uani 1 1 d . . . N5 N 1.2819(2) 1.06590(16) 0.23711(16) 0.0278(4) Uani 1 1 d . . . N6 N 1.4603(2) 1.13363(19) 0.23148(18) 0.0333(5) Uani 1 1 d . . . N7 N 2.0207(2) 0.9524(2) 0.32637(18) 0.0386(6) Uani 1 1 d . . . N8 N 1.8924(2) 0.9842(3) 0.44076(19) 0.0471(7) Uani 1 1 d . . . C1 C 1.2352(3) 1.3716(2) -0.43731(19) 0.0345(6) Uani 1 1 d . . . C2 C 1.3293(3) 1.2958(2) -0.4130(2) 0.0377(7) Uani 1 1 d . . . C3 C 1.3216(3) 1.2151(2) -0.3258(2) 0.0357(6) Uani 1 1 d . . . H3 H 1.3868 1.1664 -0.3112 0.080 Uiso 1 1 calc . . . C4 C 1.2157(3) 1.20758(18) -0.26053(18) 0.0269(5) Uani 1 1 d . . . C5 C 1.1202(3) 1.2814(2) -0.28370(19) 0.0316(6) Uani 1 1 d . . . H5 H 1.0488 1.2769 -0.2408 0.080 Uiso 1 1 calc . . . C6 C 1.1306(3) 1.3622(2) -0.3706(2) 0.0346(6) Uani 1 1 d . . . H6 H 1.0658 1.4114 -0.3846 0.080 Uiso 1 1 calc . . . C7 C 1.2043(2) 1.12168(18) -0.16490(17) 0.0263(5) Uani 1 1 d . . . C8 C 1.2409(3) 1.4676(2) -0.52428(19) 0.0347(6) Uani 1 1 d . . . C9 C 1.2147(3) 1.4768(2) -0.6165(2) 0.0348(6) Uani 1 1 d . . . C10 C 1.2083(3) 1.57048(19) -0.68994(18) 0.0307(6) Uani 1 1 d . . . H10 H 1.1876 1.5740 -0.7502 0.080 Uiso 1 1 calc . . . C11 C 1.2330(3) 1.65895(19) -0.67270(18) 0.0290(5) Uani 1 1 d . . . C12 C 1.2613(3) 1.6516(2) -0.5819(2) 0.0417(7) Uani 1 1 d . . . H12 H 1.2785 1.7106 -0.5697 0.080 Uiso 1 1 calc . . . C13 C 1.2642(4) 1.5570(2) -0.5088(2) 0.0436(8) Uani 1 1 d . . . H13 H 1.2823 1.5538 -0.4480 0.080 Uiso 1 1 calc . . . C14 C 1.2182(2) 1.76164(18) -0.75139(18) 0.0273(5) Uani 1 1 d . . . C15 C 0.7782(3) 1.4506(2) 0.0884(2) 0.0329(6) Uani 1 1 d . . . C16 C 0.8458(3) 1.3932(2) 0.1640(2) 0.0430(7) Uani 1 1 d . . . C17 C 0.9087(3) 1.3026(2) 0.1660(2) 0.0358(6) Uani 1 1 d . . . H17 H 0.9568 1.2683 0.2161 0.080 Uiso 1 1 calc . . . C18 C 0.9003(2) 1.26231(18) 0.09333(18) 0.0249(5) Uani 1 1 d . . . C19 C 0.8309(3) 1.3151(2) 0.0190(2) 0.0397(7) Uani 1 1 d . . . H19 H 0.8225 1.2879 -0.0293 0.080 Uiso 1 1 calc . . . C20 C 0.7728(3) 1.4095(2) 0.0159(2) 0.0446(8) Uani 1 1 d . . . H20 H 0.7292 1.4459 -0.0365 0.080 Uiso 1 1 calc . . . C21 C 0.9636(2) 1.15970(17) 0.09841(17) 0.0217(5) Uani 1 1 d . . . C22 C 0.7126(3) 1.5525(2) 0.0785(2) 0.0335(6) Uani 1 1 d . . . C23 C 0.5876(3) 1.56465(19) 0.1102(2) 0.0325(6) Uani 1 1 d . . . C24 C 0.5245(2) 1.65900(19) 0.0881(2) 0.0311(6) Uani 1 1 d . . . H24 H 0.4401 1.6639 0.1084 0.080 Uiso 1 1 calc . . . C25 C 0.5896(2) 1.74648(18) 0.03490(19) 0.0258(5) Uani 1 1 d . . . C26 C 0.7153(3) 1.7370(2) 0.0049(2) 0.0376(7) Uani 1 1 d . . . H26 H 0.7599 1.7955 -0.0290 0.080 Uiso 1 1 calc . . . C27 C 0.7747(3) 1.6408(2) 0.0253(3) 0.0431(7) Uani 1 1 d . . . H27 H 0.8582 1.6356 0.0026 0.080 Uiso 1 1 calc . . . C28 C 0.5242(2) 1.85033(17) 0.00594(17) 0.0232(5) Uani 1 1 d . . . C29 C 1.4040(3) 1.0527(2) 0.2278(2) 0.0300(5) Uani 1 1 d . . . H29 H 1.4458 0.9944 0.2196 0.080 Uiso 1 1 calc . . . C30 C 1.2598(3) 1.1602(2) 0.2500(2) 0.0360(6) Uani 1 1 d . . . H30 H 1.1815 1.1900 0.2598 0.080 Uiso 1 1 calc . . . C31 C 1.3692(3) 1.2023(2) 0.2461(3) 0.0410(7) Uani 1 1 d . . . H31 H 1.3806 1.2657 0.2522 0.080 Uiso 1 1 calc . . . C32 C 1.5945(3) 1.1502(3) 0.2207(2) 0.0423(7) Uani 1 1 d . . . H32A H 1.6113 1.2189 0.1766 0.080 Uiso 1 1 calc . . . H32B H 1.6395 1.1016 0.1933 0.080 Uiso 1 1 calc . . . C33 C 1.6402(3) 1.1372(3) 0.3168(3) 0.0472(8) Uani 1 1 d . . . H33A H 1.7245 1.1611 0.3059 0.080 Uiso 1 1 calc . . . H33B H 1.5878 1.1793 0.3480 0.080 Uiso 1 1 calc . . . C34 C 1.6391(3) 1.0276(3) 0.3827(3) 0.0526(9) Uani 1 1 d . . . H34A H 1.6991 0.9876 0.3542 0.080 Uiso 1 1 calc . . . H34B H 1.5574 1.0015 0.3861 0.080 Uiso 1 1 calc . . . C35 C 1.6688(3) 1.0105(4) 0.4846(3) 0.0706(13) Uani 1 1 d . . . H35A H 1.6583 0.9388 0.5229 0.080 Uiso 1 1 calc . . . H35B H 1.6098 1.0511 0.5132 0.080 Uiso 1 1 calc . . . C36 C 1.8006(3) 1.0392(4) 0.4886(3) 0.0654(12) Uani 1 1 d . . . H36A H 1.8087 1.1126 0.4572 0.080 Uiso 1 1 calc . . . H36B H 1.8164 1.0223 0.5555 0.080 Uiso 1 1 calc . . . C37 C 1.9534(3) 1.0233(3) 0.3531(2) 0.0409(7) Uani 1 1 d . . . H37 H 1.9489 1.0923 0.3153 0.080 Uiso 1 1 calc . . . C38 C 2.0009(4) 0.8618(3) 0.4022(3) 0.0548(9) Uani 1 1 d . . . H38 H 2.0362 0.7976 0.4050 0.080 Uiso 1 1 calc . . . C39 C 1.9205(4) 0.8828(4) 0.4720(3) 0.0607(11) Uani 1 1 d . . . H39 H 1.8905 0.8356 0.5308 0.080 Uiso 1 1 calc . . . H1A H 1.153(4) 0.8964(15) 0.104(3) 0.058(12) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01958(18) 0.01376(16) 0.01870(17) -0.00396(13) -0.00321(14) 0.00296(13) Zn2 0.02778(15) 0.01958(14) 0.01972(14) -0.00556(10) -0.00504(11) -0.00058(10) Zn3 0.02348(14) 0.01740(13) 0.02151(14) -0.00096(10) -0.00030(11) 0.00644(10) O1 0.0366(11) 0.0297(10) 0.0325(10) 0.0110(8) 0.0047(9) 0.0016(8) O2 0.0378(10) 0.0289(9) 0.0237(9) 0.0058(7) -0.0017(8) 0.0079(8) O3 0.0561(13) 0.0183(8) 0.0260(9) 0.0008(7) -0.0125(9) -0.0016(8) O4 0.0632(14) 0.0175(8) 0.0329(10) -0.0019(7) -0.0203(10) 0.0015(8) O5 0.077(2) 0.074(2) 0.080(2) 0.0298(17) 0.0360(18) 0.0117(17) O6 0.075(2) 0.0611(18) 0.081(2) 0.0036(15) 0.0363(17) 0.0252(15) O7 0.186(4) 0.0284(13) 0.0562(17) -0.0093(12) -0.011(2) 0.0033(18) O9 0.0357(10) 0.0253(9) 0.0376(10) -0.0150(8) -0.0165(8) 0.0138(8) O10 0.0395(11) 0.0308(10) 0.0478(11) -0.0245(9) -0.0208(9) 0.0169(8) O11 0.0372(10) 0.0185(8) 0.0350(10) -0.0070(7) 0.0022(8) -0.0020(7) O12 0.0272(9) 0.0192(8) 0.0447(11) -0.0073(8) -0.0029(8) 0.0085(7) O13 0.343(8) 0.081(3) 0.152(4) -0.093(3) -0.154(5) 0.105(4) O14 0.148(4) 0.122(3) 0.068(2) -0.062(2) -0.043(2) 0.062(3) O15 0.0622(17) 0.0318(13) 0.102(2) 0.0136(14) 0.0012(16) 0.0083(12) O16 0.042(5) 0.030(4) 0.070(4) 0.000(3) 0.020(4) -0.003(3) O16' 0.069(8) 0.069(8) 0.202(16) 0.040(8) -0.078(9) -0.034(6) O17 0.0219(8) 0.0129(7) 0.0166(7) -0.0018(6) -0.0030(6) 0.0023(6) N1 0.0591(19) 0.0463(17) 0.0467(16) 0.0118(13) 0.0229(15) 0.0118(14) N2 0.104(3) 0.0211(12) 0.0401(15) -0.0024(11) -0.0044(16) -0.0077(14) N3 0.129(4) 0.074(2) 0.094(3) -0.066(2) -0.066(3) 0.066(3) N4 0.0423(15) 0.0187(11) 0.073(2) -0.0034(12) -0.0020(14) 0.0017(10) N5 0.0302(11) 0.0224(10) 0.0328(11) -0.0099(9) -0.0096(9) 0.0012(8) N6 0.0283(11) 0.0394(13) 0.0361(12) -0.0165(10) -0.0059(10) -0.0032(10) N7 0.0380(13) 0.0473(15) 0.0300(12) -0.0105(11) -0.0019(10) -0.0113(11) N8 0.0318(13) 0.079(2) 0.0319(13) -0.0196(14) -0.0005(11) -0.0102(13) C1 0.0495(17) 0.0207(12) 0.0225(12) 0.0037(10) 0.0009(12) 0.0042(11) C2 0.0448(16) 0.0254(13) 0.0290(13) 0.0027(11) 0.0109(12) 0.0044(11) C3 0.0395(15) 0.0258(13) 0.0296(13) 0.0036(11) 0.0007(12) 0.0060(11) C4 0.0340(13) 0.0185(11) 0.0230(11) 0.0002(9) -0.0046(10) 0.0004(9) C5 0.0343(14) 0.0253(12) 0.0263(12) 0.0011(10) 0.0011(11) 0.0008(10) C6 0.0404(15) 0.0247(13) 0.0287(13) 0.0016(10) -0.0023(12) 0.0079(11) C7 0.0343(13) 0.0186(11) 0.0208(11) 0.0010(9) -0.0044(10) -0.0016(9) C8 0.0473(16) 0.0208(12) 0.0246(12) 0.0044(10) 0.0017(12) 0.0041(11) C9 0.0500(17) 0.0171(11) 0.0312(13) -0.0020(10) 0.0008(12) -0.0001(11) C10 0.0437(15) 0.0202(12) 0.0231(12) -0.0016(9) -0.0028(11) 0.0018(10) C11 0.0384(14) 0.0188(11) 0.0240(12) 0.0002(9) -0.0044(11) 0.0018(10) C12 0.071(2) 0.0212(13) 0.0307(14) -0.0025(11) -0.0136(14) -0.0017(13) C13 0.074(2) 0.0272(14) 0.0245(13) -0.0005(11) -0.0118(14) 0.0023(14) C14 0.0341(13) 0.0170(11) 0.0244(12) 0.0011(9) -0.0038(10) 0.0011(9) C15 0.0326(13) 0.0209(12) 0.0456(15) -0.0127(11) -0.0066(12) 0.0092(10) C16 0.0506(18) 0.0382(16) 0.0517(18) -0.0294(14) -0.0203(15) 0.0191(14) C17 0.0427(16) 0.0301(13) 0.0422(15) -0.0201(12) -0.0210(13) 0.0178(12) C18 0.0261(12) 0.0195(11) 0.0306(12) -0.0107(9) -0.0065(10) 0.0068(9) C19 0.0567(19) 0.0297(14) 0.0400(15) -0.0197(12) -0.0229(14) 0.0214(13) C20 0.060(2) 0.0315(15) 0.0458(17) -0.0163(13) -0.0261(15) 0.0258(14) C21 0.0239(11) 0.0171(10) 0.0242(11) -0.0078(9) -0.0033(9) 0.0052(8) C22 0.0332(14) 0.0203(12) 0.0474(16) -0.0135(11) -0.0056(12) 0.0103(10) C23 0.0324(13) 0.0169(11) 0.0453(15) -0.0073(11) -0.0040(12) 0.0024(10) C24 0.0263(12) 0.0196(11) 0.0430(15) -0.0066(11) -0.0013(11) 0.0039(10) C25 0.0260(12) 0.0174(11) 0.0317(12) -0.0071(9) -0.0024(10) 0.0064(9) C26 0.0297(14) 0.0221(12) 0.0522(17) -0.0058(12) 0.0061(13) 0.0041(10) C27 0.0281(14) 0.0283(14) 0.064(2) -0.0109(14) 0.0070(14) 0.0100(11) C28 0.0287(12) 0.0156(10) 0.0234(11) -0.0060(9) -0.0012(9) 0.0056(9) C29 0.0310(13) 0.0304(13) 0.0318(13) -0.0130(11) -0.0102(11) 0.0029(10) C30 0.0336(14) 0.0305(14) 0.0499(17) -0.0199(13) -0.0102(13) 0.0030(11) C31 0.0384(16) 0.0326(15) 0.0599(19) -0.0240(14) -0.0092(14) -0.0020(12) C32 0.0288(14) 0.0555(19) 0.0439(17) -0.0175(15) -0.0019(13) -0.0084(13) C33 0.0318(15) 0.065(2) 0.0531(19) -0.0280(17) -0.0074(14) -0.0072(14) C34 0.0303(15) 0.074(2) 0.0499(19) -0.0131(18) -0.0045(14) -0.0120(15) C35 0.0346(18) 0.125(4) 0.0422(19) -0.017(2) 0.0038(16) -0.002(2) C36 0.0368(17) 0.130(4) 0.0363(17) -0.039(2) -0.0020(15) 0.004(2) C37 0.0284(14) 0.061(2) 0.0306(14) -0.0129(14) -0.0020(12) 0.0004(13) C38 0.075(3) 0.049(2) 0.0386(17) -0.0106(15) 0.0070(17) -0.0280(18) C39 0.065(2) 0.081(3) 0.0335(17) -0.0142(18) 0.0103(16) -0.039(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O10 2.0413(19) 2_775 ? Zn1 O10 2.0413(19) . ? Zn1 O17 2.1262(17) 2_775 ? Zn1 O17 2.1262(17) . ? Zn1 O1 2.149(2) . ? Zn1 O1 2.149(2) 2_775 ? Zn2 O17 2.0112(16) . ? Zn2 N5 2.034(2) . ? Zn2 N7 2.050(3) 1_455 ? Zn2 O4 2.100(2) 1_546 ? Zn2 O9 2.1675(19) . ? Zn3 O17 1.9436(17) . ? Zn3 O2 1.9548(19) . ? Zn3 O12 1.9636(18) 1_645 ? Zn3 O11 1.988(2) 2_785 ? O1 C7 1.239(3) . ? O2 C7 1.269(3) . ? O3 C14 1.235(3) . ? O4 C14 1.268(3) . ? O4 Zn2 2.100(2) 1_564 ? O5 N1 1.217(4) . ? O6 N1 1.202(4) . ? O7 N2 1.232(4) . ? O8 N2 1.201(5) . ? O9 C21 1.250(3) . ? O10 C21 1.245(3) . ? O11 C28 1.253(3) . ? O11 Zn3 1.988(2) 2_785 ? O12 C28 1.255(3) . ? O12 Zn3 1.9636(18) 1_465 ? O13 N3 1.162(5) . ? O14 N3 1.213(5) . ? O15 N4 1.208(4) . ? O16 N4 1.211(12) . ? O16' N4 1.186(14) . ? O17 H1A 0.836(19) . ? N1 C2 1.464(4) . ? N2 C9 1.464(4) . ? N3 C16 1.473(5) . ? N4 C23 1.481(4) . ? N5 C29 1.317(3) . ? N5 C30 1.382(3) . ? N6 C29 1.337(4) . ? N6 C31 1.366(4) . ? N6 C32 1.469(4) . ? N7 C37 1.316(4) . ? N7 C38 1.380(4) . ? N7 Zn2 2.050(3) 1_655 ? N8 C37 1.333(4) . ? N8 C39 1.344(6) . ? N8 C36 1.464(5) . ? C1 C6 1.390(4) . ? C1 C2 1.392(4) . ? C1 C8 1.503(3) . ? C2 C3 1.390(4) . ? C3 C4 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.385(4) . ? C4 C7 1.506(3) . ? C5 C6 1.387(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.380(4) . ? C8 C9 1.389(4) . ? C9 C10 1.384(3) . ? C10 C11 1.385(4) . ? C10 H10 0.9300 . ? C11 C12 1.383(4) . ? C11 C14 1.514(3) . ? C12 C13 1.388(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C20 1.382(4) . ? C15 C16 1.388(4) . ? C15 C22 1.499(3) . ? C16 C17 1.375(4) . ? C17 C18 1.383(4) . ? C17 H17 0.9300 . ? C18 C19 1.371(4) . ? C18 C21 1.512(3) . ? C19 C20 1.396(4) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.383(4) . ? C22 C23 1.392(4) . ? C23 C24 1.382(4) . ? C24 C25 1.390(4) . ? C24 H24 0.9300 . ? C25 C26 1.388(4) . ? C25 C28 1.501(3) . ? C26 C27 1.387(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.347(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.511(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.499(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.516(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.524(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37 0.9300 . ? C38 C39 1.361(6) . ? C38 H38 0.9300 . ? 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 O10 Zn1 O10 180.000(1) 2_775 . ? O10 Zn1 O17 98.04(7) 2_775 2_775 ? O10 Zn1 O17 81.96(7) . 2_775 ? O10 Zn1 O17 81.96(7) 2_775 . ? O10 Zn1 O17 98.04(7) . . ? O17 Zn1 O17 180.00(7) 2_775 . ? O10 Zn1 O1 91.63(9) 2_775 . ? O10 Zn1 O1 88.37(9) . . ? O17 Zn1 O1 89.25(8) 2_775 . ? O17 Zn1 O1 90.75(8) . . ? O10 Zn1 O1 88.37(9) 2_775 2_775 ? O10 Zn1 O1 91.63(9) . 2_775 ? O17 Zn1 O1 90.75(8) 2_775 2_775 ? O17 Zn1 O1 89.25(8) . 2_775 ? O1 Zn1 O1 180.00(10) . 2_775 ? O17 Zn2 N5 122.92(8) . . ? O17 Zn2 N7 131.32(9) . 1_455 ? N5 Zn2 N7 105.46(10) . 1_455 ? O17 Zn2 O4 90.38(8) . 1_546 ? N5 Zn2 O4 95.47(9) . 1_546 ? N7 Zn2 O4 90.07(11) 1_455 1_546 ? O17 Zn2 O9 90.33(7) . . ? N5 Zn2 O9 86.93(8) . . ? N7 Zn2 O9 86.95(10) 1_455 . ? O4 Zn2 O9 176.59(8) 1_546 . ? O17 Zn3 O2 120.15(8) . . ? O17 Zn3 O12 110.54(8) . 1_645 ? O2 Zn3 O12 114.26(9) . 1_645 ? O17 Zn3 O11 106.23(8) . 2_785 ? O2 Zn3 O11 98.88(9) . 2_785 ? O12 Zn3 O11 104.43(8) 1_645 2_785 ? C7 O1 Zn1 138.35(18) . . ? C7 O2 Zn3 116.73(17) . . ? C14 O4 Zn2 123.08(17) . 1_564 ? C21 O9 Zn2 134.63(16) . . ? C21 O10 Zn1 131.34(17) . . ? C28 O11 Zn3 142.11(18) . 2_785 ? C28 O12 Zn3 122.46(16) . 1_465 ? Zn3 O17 Zn2 120.57(8) . . ? Zn3 O17 Zn1 108.46(7) . . ? Zn2 O17 Zn1 121.41(8) . . ? Zn3 O17 H1A 103(3) . . ? Zn2 O17 H1A 97(3) . . ? Zn1 O17 H1A 102(3) . . ? O6 N1 O5 122.1(3) . . ? O6 N1 C2 118.7(3) . . ? O5 N1 C2 119.0(3) . . ? O8 N2 O7 121.0(3) . . ? O8 N2 C9 121.0(3) . . ? O7 N2 C9 116.6(3) . . ? O13 N3 O14 122.0(4) . . ? O13 N3 C16 119.0(4) . . ? O14 N3 C16 119.0(3) . . ? O16' N4 O15 124.2(8) . . ? O16' N4 O16 15.4(14) . . ? O15 N4 O16 120.5(6) . . ? O16' N4 C23 116.6(8) . . ? O15 N4 C23 118.7(3) . . ? O16 N4 C23 120.2(6) . . ? C29 N5 C30 105.4(2) . . ? C29 N5 Zn2 128.18(18) . . ? C30 N5 Zn2 125.06(18) . . ? C29 N6 C31 107.4(2) . . ? C29 N6 C32 128.1(3) . . ? C31 N6 C32 124.4(3) . . ? C37 N7 C38 105.5(3) . . ? C37 N7 Zn2 123.7(2) . 1_655 ? C38 N7 Zn2 129.7(3) . 1_655 ? C37 N8 C39 107.1(3) . . ? C37 N8 C36 126.2(4) . . ? C39 N8 C36 126.4(3) . . ? C6 C1 C2 116.8(2) . . ? C6 C1 C8 116.8(2) . . ? C2 C1 C8 126.1(3) . . ? C3 C2 C1 122.3(3) . . ? C3 C2 N1 116.8(3) . . ? C1 C2 N1 120.9(2) . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.1(2) . . ? C5 C4 C7 119.7(2) . . ? C3 C4 C7 121.1(2) . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 121.8(3) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? O1 C7 O2 125.8(2) . . ? O1 C7 C4 117.7(2) . . ? O2 C7 C4 116.5(2) . . ? C13 C8 C9 116.8(2) . . ? C13 C8 C1 116.5(3) . . ? C9 C8 C1 126.5(3) . . ? C10 C9 C8 122.7(3) . . ? C10 C9 N2 116.4(3) . . ? C8 C9 N2 120.9(2) . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 119.1(2) . . ? C12 C11 C14 121.8(2) . . ? C10 C11 C14 118.9(2) . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C8 C13 C12 121.6(3) . . ? C8 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? O3 C14 O4 126.4(2) . . ? O3 C14 C11 117.2(2) . . ? O4 C14 C11 116.4(2) . . ? C20 C15 C16 116.3(2) . . ? C20 C15 C22 117.9(3) . . ? C16 C15 C22 125.8(3) . . ? C17 C16 C15 122.6(3) . . ? C17 C16 N3 116.6(3) . . ? C15 C16 N3 120.6(3) . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 119.1(2) . . ? C19 C18 C21 121.0(2) . . ? C17 C18 C21 119.9(2) . . ? C18 C19 C20 120.1(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C15 C20 C19 121.9(3) . . ? C15 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? O10 C21 O9 126.9(2) . . ? O10 C21 C18 116.1(2) . . ? O9 C21 C18 116.9(2) . . ? C27 C22 C23 116.9(2) . . ? C27 C22 C15 118.5(2) . . ? C23 C22 C15 124.2(2) . . ? C24 C23 C22 123.1(2) . . ? C24 C23 N4 116.8(2) . . ? C22 C23 N4 120.1(2) . . ? C23 C24 C25 118.7(2) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? C26 C25 C24 119.5(2) . . ? C26 C25 C28 119.8(2) . . ? C24 C25 C28 120.7(2) . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C22 C27 C26 121.4(3) . . ? C22 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? O11 C28 O12 124.7(2) . . ? O11 C28 C25 117.9(2) . . ? O12 C28 C25 117.2(2) . . ? N5 C29 N6 111.3(2) . . ? N5 C29 H29 124.3 . . ? N6 C29 H29 124.3 . . ? C31 C30 N5 109.4(3) . . ? C31 C30 H30 125.3 . . ? N5 C30 H30 125.3 . . ? C30 C31 N6 106.4(3) . . ? C30 C31 H31 126.8 . . ? N6 C31 H31 126.8 . . ? N6 C32 C33 111.3(3) . . ? N6 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? N6 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 112.3(3) . . ? C34 C33 H33A 109.1 . . ? C32 C33 H33A 109.1 . . ? C34 C33 H33B 109.1 . . ? C32 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? C33 C34 C35 115.2(4) . . ? C33 C34 H34A 108.5 . . ? C35 C34 H34A 108.5 . . ? C33 C34 H34B 108.5 . . ? C35 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? C34 C35 C36 113.0(3) . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? N8 C36 C35 110.8(4) . . ? N8 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? N8 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? N7 C37 N8 111.8(3) . . ? N7 C37 H37 124.1 . . ? N8 C37 H37 124.1 . . ? C39 C38 N7 108.0(4) . . ? C39 C38 H38 126.0 . . ? N7 C38 H38 126.0 . . ? N8 C39 C38 107.6(3) . . ? N8 C39 H39 126.2 . . ? C38 C39 H39 126.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O17 H1A O3 0.836(19) 1.83(2) 2.640(2) 163(4) 1_546 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.147 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.083 #=========================END data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 806103' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C39 H28 Cd2 N8 O16' _chemical_formula_sum 'C39 H28 Cd2 N8 O16' _chemical_formula_weight 1089.49 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 26.082(5) _cell_length_b 10.575(2) _cell_length_c 14.788(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.53(3) _cell_angle_gamma 90.00 _cell_volume 3965.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9011 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.44 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37974 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.44 _reflns_number_total 9011 _reflns_number_gt 7804 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+4.8566P] 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 9011 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.005 _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 0.730628(5) 1.305278(13) 0.221567(9) 0.00872(4) Uani 1 1 d . . . Cd2 Cd 0.769148(5) 1.197466(13) 0.478698(9) 0.00895(4) Uani 1 1 d . . . O1 O 0.70061(5) 1.19237(14) 0.32989(10) 0.0146(3) Uani 1 1 d . . . O2 O 0.68563(5) 1.08976(13) 0.45103(9) 0.0127(3) Uani 1 1 d . . . O3 O 0.32971(5) 0.77059(14) -0.10199(9) 0.0147(3) Uani 1 1 d . . . O4 O 0.27907(5) 0.85899(13) -0.01507(10) 0.0132(3) Uani 1 1 d . . . O5 O 0.52945(7) 0.83650(18) 0.42820(12) 0.0344(4) Uani 1 1 d . . . O6 O 0.45710(6) 0.89741(16) 0.33376(11) 0.0242(4) Uani 1 1 d . . . O7 O 0.37299(6) 1.22189(15) 0.15741(13) 0.0273(4) Uani 1 1 d . . . O8 O 0.44587(6) 1.18329(15) 0.25862(11) 0.0251(4) Uani 1 1 d . . . O9 O 0.78622(5) 1.41234(13) 0.34583(9) 0.0124(3) Uani 1 1 d . . . O10 O 0.83992(5) 1.28859(13) 0.44846(10) 0.0150(3) Uani 1 1 d . . . O11 O 1.20022(5) 1.66639(13) 0.24888(10) 0.0140(3) Uani 1 1 d . . . O12 O 1.19422(5) 1.80552(13) 0.35806(9) 0.0123(3) Uani 1 1 d . . . O13 O 1.03505(6) 1.34648(18) 0.48562(11) 0.0289(4) Uani 1 1 d . . . O14 O 1.04959(6) 1.33274(15) 0.34725(11) 0.0229(3) Uani 1 1 d . . . O15 O 1.05280(7) 1.38254(19) 0.12050(15) 0.0422(5) Uani 1 1 d . . . O16 O 0.97531(6) 1.46228(17) 0.11403(12) 0.0291(4) Uani 1 1 d . . . N1 N 0.50537(7) 0.89753(18) 0.36076(13) 0.0191(4) Uani 1 1 d . . . N2 N 0.41123(7) 1.15416(17) 0.19046(13) 0.0185(4) Uani 1 1 d . . . N3 N 1.02234(7) 1.36261(17) 0.40132(13) 0.0161(4) Uani 1 1 d . . . N4 N 1.02310(8) 1.45607(19) 0.14723(14) 0.0239(4) Uani 1 1 d . . . N5 N 0.69410(7) 1.49564(16) 0.19468(12) 0.0149(4) Uani 1 1 d . . . N6 N 0.68695(8) 1.70301(16) 0.19719(13) 0.0187(4) Uani 1 1 d . . . N7 N 0.79957(7) 1.50160(16) -0.01806(12) 0.0146(3) Uani 1 1 d . . . N8 N 0.80373(7) 1.70953(16) -0.01096(12) 0.0168(4) Uani 1 1 d . . . C1 C 0.51469(8) 1.01351(19) 0.21837(14) 0.0134(4) Uani 1 1 d . . . C2 C 0.53624(8) 0.97567(19) 0.30971(14) 0.0138(4) Uani 1 1 d . . . C3 C 0.58656(8) 1.00922(19) 0.35743(14) 0.0128(4) Uani 1 1 d . . . H3 H 0.6000 0.9801 0.4177 0.080 Uiso 1 1 calc . . . C4 C 0.61706(7) 1.08706(18) 0.31458(14) 0.0117(4) Uani 1 1 d . . . C5 C 0.59623(8) 1.1278(2) 0.22426(14) 0.0150(4) Uani 1 1 d . . . H5 H 0.6159 1.1810 0.1953 0.080 Uiso 1 1 calc . . . C6 C 0.54609(8) 1.0895(2) 0.17678(15) 0.0178(4) Uani 1 1 d . . . H6 H 0.5333 1.1154 0.1156 0.080 Uiso 1 1 calc . . . C7 C 0.67111(7) 1.12513(18) 0.36826(13) 0.0100(4) Uani 1 1 d . . . C8 C 0.46338(8) 0.96829(19) 0.15863(14) 0.0124(4) Uani 1 1 d . . . C9 C 0.41523(8) 1.03257(19) 0.14417(14) 0.0143(4) Uani 1 1 d . . . C10 C 0.36979(8) 0.9881(2) 0.08503(14) 0.0146(4) Uani 1 1 d . . . H10 H 0.3380 1.0303 0.0802 0.080 Uiso 1 1 calc . . . C11 C 0.37185(8) 0.88008(19) 0.03283(13) 0.0117(4) Uani 1 1 d . . . C12 C 0.42003(8) 0.81753(19) 0.04196(14) 0.0139(4) Uani 1 1 d . . . H12 H 0.4221 0.7471 0.0054 0.080 Uiso 1 1 calc . . . C13 C 0.46475(8) 0.85998(19) 0.10535(14) 0.0140(4) Uani 1 1 d . . . H13 H 0.4962 0.8154 0.1124 0.080 Uiso 1 1 calc . . . C14 C 0.32250(8) 0.83282(18) -0.03334(13) 0.0114(4) Uani 1 1 d . . . C15 C 0.96719(8) 1.52113(19) 0.29953(14) 0.0141(4) Uani 1 1 d . . . C16 C 0.97049(7) 1.42098(19) 0.36213(14) 0.0124(4) Uani 1 1 d . . . C17 C 0.92811(8) 1.37381(18) 0.39252(14) 0.0126(4) Uani 1 1 d . . . H17 H 0.9327 1.3095 0.4365 0.080 Uiso 1 1 calc . . . C18 C 0.87846(7) 1.42471(18) 0.35579(14) 0.0117(4) Uani 1 1 d . . . C19 C 0.87330(8) 1.5220(2) 0.29076(15) 0.0173(4) Uani 1 1 d . . . H19 H 0.8400 1.5547 0.2647 0.080 Uiso 1 1 calc . . . C20 C 0.91708(8) 1.5713(2) 0.26413(15) 0.0192(5) Uani 1 1 d . . . H20 H 0.9128 1.6383 0.2223 0.080 Uiso 1 1 calc . . . C21 C 0.83104(8) 1.37131(18) 0.38527(13) 0.0110(4) Uani 1 1 d . . . C22 C 1.01681(8) 1.58205(19) 0.28582(14) 0.0139(4) Uani 1 1 d . . . C23 C 1.04609(8) 1.54436(19) 0.22243(15) 0.0152(4) Uani 1 1 d . . . C24 C 1.09701(8) 1.5857(2) 0.22727(14) 0.0153(4) Uani 1 1 d . . . H24 H 1.1161 1.5547 0.1862 0.080 Uiso 1 1 calc . . . C25 C 1.11927(8) 1.67461(18) 0.29481(14) 0.0120(4) Uani 1 1 d . . . C26 C 1.08955(8) 1.72210(19) 0.35348(14) 0.0144(4) Uani 1 1 d . . . H26 H 1.1031 1.7862 0.3953 0.080 Uiso 1 1 calc . . . C27 C 1.03936(8) 1.6739(2) 0.34996(14) 0.0149(4) Uani 1 1 d . . . H27 H 1.0205 1.7040 0.3917 0.080 Uiso 1 1 calc . . . C28 C 1.17498(8) 1.71732(18) 0.30182(13) 0.0111(4) Uani 1 1 d . . . C29 C 0.71374(9) 1.6015(2) 0.23704(15) 0.0179(4) Uani 1 1 d . . . H29 H 0.7425 1.6049 0.2879 0.080 Uiso 1 1 calc . . . C30 C 0.65237(9) 1.5325(2) 0.12385(15) 0.0182(4) Uani 1 1 d . . . H30 H 0.6308 1.4782 0.0821 0.080 Uiso 1 1 calc . . . C31 C 0.64762(9) 1.6602(2) 0.12444(16) 0.0221(5) Uani 1 1 d . . . H31 H 0.6228 1.7091 0.0839 0.080 Uiso 1 1 calc . . . C32 C 0.69930(10) 1.8358(2) 0.22365(17) 0.0249(5) Uani 1 1 d . . . H32A H 0.7203 1.8391 0.2871 0.080 Uiso 1 1 calc . . . H32B H 0.6668 1.8815 0.2212 0.080 Uiso 1 1 calc . . . C33 C 0.72929(10) 1.8994(2) 0.15974(17) 0.0235(5) Uani 1 1 d . . . H33A H 0.7323 1.9889 0.1743 0.080 Uiso 1 1 calc . . . H33B H 0.7090 1.8910 0.0961 0.080 Uiso 1 1 calc . . . C34 C 0.78450(10) 1.8461(2) 0.16637(16) 0.0238(5) Uani 1 1 d . . . H34A H 0.7823 1.7548 0.1606 0.080 Uiso 1 1 calc . . . H34B H 0.8066 1.8659 0.2271 0.080 Uiso 1 1 calc . . . C35 C 0.81013(9) 1.8990(2) 0.09128(16) 0.0228(5) Uani 1 1 d . . . H35A H 0.8049 1.9899 0.0876 0.080 Uiso 1 1 calc . . . H35B H 0.8478 1.8835 0.1094 0.080 Uiso 1 1 calc . . . C36 C 0.78838(10) 1.8419(2) -0.00461(17) 0.0226(5) Uani 1 1 d . . . H36A H 0.7502 1.8476 -0.0195 0.080 Uiso 1 1 calc . . . H36B H 0.8009 1.8911 -0.0505 0.080 Uiso 1 1 calc . . . C37 C 0.77296(8) 1.60648(19) -0.01331(14) 0.0150(4) Uani 1 1 d . . . H37 H 0.7375 1.6091 -0.0118 0.080 Uiso 1 1 calc . . . C38 C 0.85023(8) 1.5390(2) -0.01796(16) 0.0196(5) Uani 1 1 d . . . H38 H 0.8780 1.4849 -0.0202 0.080 Uiso 1 1 calc . . . C39 C 0.85322(9) 1.6671(2) -0.01417(16) 0.0212(5) Uani 1 1 d . . . H39 H 0.8828 1.7165 -0.0138 0.080 Uiso 1 1 calc . . . 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 0.00654(7) 0.00952(7) 0.00969(7) -0.00039(5) 0.00106(5) 0.00017(5) Cd2 0.00577(7) 0.01025(7) 0.01055(7) -0.00006(5) 0.00135(5) -0.00060(5) O1 0.0105(7) 0.0210(7) 0.0123(7) 0.0014(6) 0.0027(6) -0.0044(6) O2 0.0098(6) 0.0154(7) 0.0120(7) 0.0012(6) 0.0010(5) -0.0021(6) O3 0.0125(7) 0.0205(7) 0.0104(7) -0.0010(6) 0.0013(6) -0.0046(6) O4 0.0088(6) 0.0138(7) 0.0165(7) 0.0020(6) 0.0021(6) -0.0017(5) O5 0.0242(9) 0.0466(11) 0.0281(9) 0.0209(9) -0.0026(8) -0.0130(8) O6 0.0129(7) 0.0319(9) 0.0270(9) 0.0039(7) 0.0031(7) -0.0076(7) O7 0.0186(8) 0.0209(8) 0.0408(10) -0.0092(7) 0.0040(8) 0.0037(7) O8 0.0203(8) 0.0275(9) 0.0254(8) -0.0132(7) 0.0013(7) -0.0062(7) O9 0.0089(6) 0.0135(7) 0.0145(7) -0.0030(6) 0.0023(6) -0.0011(5) O10 0.0109(7) 0.0187(7) 0.0154(7) 0.0041(6) 0.0032(6) -0.0031(6) O11 0.0105(7) 0.0143(7) 0.0179(7) -0.0004(6) 0.0048(6) -0.0015(6) O12 0.0095(6) 0.0150(7) 0.0115(7) 0.0016(6) 0.0005(5) -0.0010(6) O13 0.0201(8) 0.0446(11) 0.0217(9) 0.0129(8) 0.0046(7) 0.0107(8) O14 0.0175(8) 0.0242(8) 0.0307(9) 0.0019(7) 0.0130(7) 0.0046(6) O15 0.0287(10) 0.0459(12) 0.0600(13) -0.0369(10) 0.0265(10) -0.0185(9) O16 0.0210(9) 0.0356(10) 0.0291(9) -0.0078(8) 0.0025(7) -0.0126(7) N1 0.0161(9) 0.0232(10) 0.0175(9) 0.0013(8) 0.0029(8) -0.0073(8) N2 0.0146(9) 0.0193(9) 0.0227(10) -0.0071(8) 0.0067(8) -0.0055(7) N3 0.0109(8) 0.0162(9) 0.0219(9) 0.0033(7) 0.0051(7) 0.0002(7) N4 0.0209(10) 0.0270(10) 0.0273(10) -0.0096(9) 0.0126(9) -0.0128(8) N5 0.0149(8) 0.0145(8) 0.0152(8) 0.0001(7) 0.0035(7) 0.0032(7) N6 0.0255(10) 0.0128(8) 0.0186(9) 0.0011(7) 0.0068(8) 0.0050(8) N7 0.0121(8) 0.0150(8) 0.0162(8) 0.0002(7) 0.0026(7) -0.0021(7) N8 0.0188(9) 0.0123(8) 0.0189(9) -0.0006(7) 0.0038(8) -0.0033(7) C1 0.0080(9) 0.0172(10) 0.0150(10) -0.0014(8) 0.0026(8) -0.0007(8) C2 0.0137(10) 0.0132(9) 0.0147(10) 0.0012(8) 0.0039(8) -0.0037(8) C3 0.0117(9) 0.0139(9) 0.0124(9) -0.0015(8) 0.0020(8) -0.0021(8) C4 0.0086(9) 0.0115(9) 0.0149(10) -0.0031(8) 0.0024(8) -0.0010(7) C5 0.0110(9) 0.0187(10) 0.0153(10) 0.0023(8) 0.0030(8) -0.0029(8) C6 0.0130(10) 0.0237(11) 0.0154(10) 0.0019(9) 0.0009(8) -0.0044(9) C7 0.0081(9) 0.0090(9) 0.0129(9) -0.0026(7) 0.0026(8) 0.0000(7) C8 0.0090(9) 0.0163(10) 0.0116(9) -0.0002(8) 0.0018(8) -0.0047(8) C9 0.0134(10) 0.0143(10) 0.0155(10) -0.0035(8) 0.0038(8) -0.0022(8) C10 0.0101(9) 0.0180(10) 0.0154(10) 0.0002(8) 0.0024(8) -0.0012(8) C11 0.0095(9) 0.0141(9) 0.0110(9) 0.0027(8) 0.0015(8) -0.0028(8) C12 0.0129(9) 0.0133(9) 0.0153(10) -0.0004(8) 0.0025(8) -0.0026(8) C13 0.0104(9) 0.0144(10) 0.0172(10) 0.0008(8) 0.0028(8) -0.0004(8) C14 0.0114(9) 0.0112(9) 0.0106(9) 0.0045(7) 0.0003(8) -0.0030(7) C15 0.0107(9) 0.0183(10) 0.0144(10) -0.0017(8) 0.0048(8) -0.0034(8) C16 0.0081(9) 0.0136(9) 0.0145(9) -0.0012(8) 0.0006(8) 0.0004(8) C17 0.0127(9) 0.0126(9) 0.0123(9) -0.0009(8) 0.0025(8) -0.0013(8) C18 0.0095(9) 0.0129(9) 0.0127(9) -0.0028(8) 0.0025(8) -0.0040(8) C19 0.0092(9) 0.0209(11) 0.0213(11) 0.0050(9) 0.0026(8) 0.0008(8) C20 0.0139(10) 0.0216(11) 0.0220(11) 0.0090(9) 0.0043(9) -0.0011(9) C21 0.0111(9) 0.0121(9) 0.0100(9) -0.0055(7) 0.0028(8) -0.0037(7) C22 0.0100(9) 0.0156(10) 0.0159(10) 0.0039(8) 0.0027(8) -0.0005(8) C23 0.0136(10) 0.0146(10) 0.0178(10) -0.0017(8) 0.0046(8) -0.0044(8) C24 0.0134(10) 0.0157(10) 0.0180(10) 0.0008(8) 0.0062(8) -0.0008(8) C25 0.0093(9) 0.0122(9) 0.0140(9) 0.0061(8) 0.0015(8) -0.0001(7) C26 0.0116(10) 0.0170(10) 0.0137(10) 0.0015(8) 0.0013(8) -0.0005(8) C27 0.0108(9) 0.0189(10) 0.0150(10) 0.0023(8) 0.0031(8) 0.0008(8) C28 0.0089(9) 0.0122(9) 0.0114(9) 0.0062(8) 0.0006(8) 0.0001(7) C29 0.0228(11) 0.0139(10) 0.0167(10) 0.0012(8) 0.0041(9) 0.0015(9) C30 0.0177(11) 0.0205(11) 0.0150(10) -0.0001(9) 0.0010(9) 0.0037(9) C31 0.0240(12) 0.0218(11) 0.0202(11) 0.0021(9) 0.0047(10) 0.0079(9) C32 0.0398(14) 0.0105(10) 0.0263(12) -0.0014(9) 0.0117(11) 0.0026(10) C33 0.0286(12) 0.0145(10) 0.0278(12) 0.0020(9) 0.0075(10) 0.0028(9) C34 0.0291(13) 0.0170(11) 0.0228(12) -0.0007(9) 0.0011(10) 0.0032(9) C35 0.0231(11) 0.0158(10) 0.0278(12) -0.0039(9) 0.0022(10) -0.0035(9) C36 0.0294(13) 0.0107(10) 0.0266(12) 0.0026(9) 0.0040(10) -0.0016(9) C37 0.0139(10) 0.0135(10) 0.0172(10) 0.0004(8) 0.0027(8) -0.0021(8) C38 0.0130(10) 0.0212(11) 0.0254(12) -0.0041(9) 0.0063(9) -0.0030(9) C39 0.0172(11) 0.0207(11) 0.0266(12) -0.0020(9) 0.0071(10) -0.0062(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 N5 2.2228(17) . ? Cd1 O3 2.2237(15) 3_675 ? Cd1 O1 2.2783(14) . ? Cd1 O11 2.2875(14) 2_745 ? Cd1 O9 2.3482(15) . ? Cd1 O12 2.5118(15) 2_745 ? Cd1 C28 2.729(2) 2_745 ? Cd2 O10 2.2185(14) . ? Cd2 N7 2.2462(17) 4_586 ? Cd2 O4 2.2594(14) 2_655 ? Cd2 O12 2.3794(15) 3_786 ? Cd2 O2 2.4067(14) . ? Cd2 O1 2.4899(16) . ? O1 C7 1.275(2) . ? O2 C7 1.251(2) . ? O3 C14 1.260(2) . ? O3 Cd1 2.2237(15) 3_675 ? O4 C14 1.255(2) . ? O4 Cd2 2.2594(14) 2_645 ? O5 N1 1.230(2) . ? O6 N1 1.229(2) . ? O7 N2 1.232(2) . ? O8 N2 1.225(2) . ? O9 C21 1.255(2) . ? O10 C21 1.261(2) . ? O11 C28 1.256(2) . ? O11 Cd1 2.2875(14) 2_755 ? O12 C28 1.272(2) . ? O12 Cd2 2.3794(15) 3_786 ? O12 Cd1 2.5118(15) 2_755 ? O13 N3 1.225(2) . ? O14 N3 1.229(2) . ? O15 N4 1.226(3) . ? O16 N4 1.230(2) . ? N1 C2 1.478(3) . ? N2 C9 1.472(3) . ? N3 C16 1.476(3) . ? N4 C23 1.468(3) . ? N5 C29 1.326(3) . ? N5 C30 1.379(3) . ? N6 C29 1.340(3) . ? N6 C31 1.378(3) . ? N6 C32 1.473(3) . ? N7 C37 1.319(3) . ? N7 C38 1.379(3) . ? N7 Cd2 2.2462(17) 4_585 ? N8 C37 1.349(3) . ? N8 C39 1.378(3) . ? N8 C36 1.465(3) . ? C1 C6 1.389(3) . ? C1 C2 1.395(3) . ? C1 C8 1.499(3) . ? C2 C3 1.383(3) . ? C3 C4 1.395(3) . ? C3 H3 0.9300 . ? C4 C5 1.387(3) . ? C4 C7 1.502(3) . ? C5 C6 1.392(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.395(3) . ? C8 C9 1.400(3) . ? C9 C10 1.380(3) . ? C10 C11 1.387(3) . ? C10 H10 0.9300 . ? C11 C12 1.398(3) . ? C11 C14 1.508(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C20 1.394(3) . ? C15 C16 1.396(3) . ? C15 C22 1.501(3) . ? C16 C17 1.380(3) . ? C17 C18 1.390(3) . ? C17 H17 0.9300 . ? C18 C19 1.393(3) . ? C18 C21 1.514(3) . ? C19 C20 1.393(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.388(3) . ? C22 C23 1.399(3) . ? C23 C24 1.384(3) . ? C24 C25 1.396(3) . ? C24 H24 0.9300 . ? C25 C26 1.386(3) . ? C25 C28 1.502(3) . ? C26 C27 1.395(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 Cd1 2.729(2) 2_755 ? C29 H29 0.9300 . ? C30 C31 1.356(3) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.518(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.528(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.530(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.523(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37 0.9300 . ? C38 C39 1.357(3) . ? C38 H38 0.9300 . ? 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 N5 Cd1 O3 89.46(6) . 3_675 ? N5 Cd1 O1 113.39(6) . . ? O3 Cd1 O1 94.26(5) 3_675 . ? N5 Cd1 O11 154.35(6) . 2_745 ? O3 Cd1 O11 107.45(6) 3_675 2_745 ? O1 Cd1 O11 85.10(5) . 2_745 ? N5 Cd1 O9 82.16(6) . . ? O3 Cd1 O9 171.40(5) 3_675 . ? O1 Cd1 O9 87.33(5) . . ? O11 Cd1 O9 81.09(5) 2_745 . ? N5 Cd1 O12 105.31(6) . 2_745 ? O3 Cd1 O12 96.45(5) 3_675 2_745 ? O1 Cd1 O12 139.85(5) . 2_745 ? O11 Cd1 O12 54.78(5) 2_745 2_745 ? O9 Cd1 O12 87.68(5) . 2_745 ? N5 Cd1 C28 130.37(6) . 2_745 ? O3 Cd1 C28 105.54(6) 3_675 2_745 ? O1 Cd1 C28 112.28(6) . 2_745 ? O11 Cd1 C28 27.23(5) 2_745 2_745 ? O9 Cd1 C28 81.56(6) . 2_745 ? O12 Cd1 C28 27.70(5) 2_745 2_745 ? O10 Cd2 N7 96.02(6) . 4_586 ? O10 Cd2 O4 104.79(5) . 2_655 ? N7 Cd2 O4 156.48(6) 4_586 2_655 ? O10 Cd2 O12 93.13(5) . 3_786 ? N7 Cd2 O12 84.83(6) 4_586 3_786 ? O4 Cd2 O12 83.24(5) 2_655 3_786 ? O10 Cd2 O2 159.05(5) . . ? N7 Cd2 O2 82.03(6) 4_586 . ? O4 Cd2 O2 82.31(5) 2_655 . ? O12 Cd2 O2 107.39(5) 3_786 . ? O10 Cd2 O1 106.88(5) . . ? N7 Cd2 O1 100.11(6) 4_586 . ? O4 Cd2 O1 84.39(5) 2_655 . ? O12 Cd2 O1 158.61(5) 3_786 . ? O2 Cd2 O1 53.52(5) . . ? C7 O1 Cd1 161.45(13) . . ? C7 O1 Cd2 90.11(11) . . ? Cd1 O1 Cd2 108.44(5) . . ? C7 O2 Cd2 94.57(12) . . ? C14 O3 Cd1 128.15(13) . 3_675 ? C14 O4 Cd2 117.72(12) . 2_645 ? C21 O9 Cd1 122.30(12) . . ? C21 O10 Cd2 115.69(12) . . ? C28 O11 Cd1 96.34(12) . 2_755 ? C28 O12 Cd2 131.06(12) . 3_786 ? C28 O12 Cd1 85.68(11) . 2_755 ? Cd2 O12 Cd1 107.66(6) 3_786 2_755 ? O6 N1 O5 123.57(18) . . ? O6 N1 C2 118.29(18) . . ? O5 N1 C2 118.14(18) . . ? O8 N2 O7 123.55(19) . . ? O8 N2 C9 118.91(18) . . ? O7 N2 C9 117.54(18) . . ? O13 N3 O14 124.52(18) . . ? O13 N3 C16 117.56(17) . . ? O14 N3 C16 117.92(17) . . ? O15 N4 O16 124.2(2) . . ? O15 N4 C23 118.06(19) . . ? O16 N4 C23 117.68(19) . . ? C29 N5 C30 105.61(18) . . ? C29 N5 Cd1 125.33(14) . . ? C30 N5 Cd1 128.41(14) . . ? C29 N6 C31 107.26(18) . . ? C29 N6 C32 125.99(19) . . ? C31 N6 C32 126.68(19) . . ? C37 N7 C38 105.94(17) . . ? C37 N7 Cd2 126.98(14) . 4_585 ? C38 N7 Cd2 127.06(14) . 4_585 ? C37 N8 C39 107.03(17) . . ? C37 N8 C36 127.14(19) . . ? C39 N8 C36 125.82(18) . . ? C6 C1 C2 116.66(18) . . ? C6 C1 C8 117.46(18) . . ? C2 C1 C8 125.54(18) . . ? C3 C2 C1 122.68(18) . . ? C3 C2 N1 116.61(18) . . ? C1 C2 N1 120.70(18) . . ? C2 C3 C4 119.55(18) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.94(18) . . ? C5 C4 C7 122.22(18) . . ? C3 C4 C7 118.83(18) . . ? C4 C5 C6 120.34(19) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 121.78(19) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? O2 C7 O1 121.76(18) . . ? O2 C7 C4 117.97(17) . . ? O1 C7 C4 120.27(17) . . ? C13 C8 C9 116.94(18) . . ? C13 C8 C1 117.21(18) . . ? C9 C8 C1 125.48(18) . . ? C10 C9 C8 122.53(19) . . ? C10 C9 N2 116.65(18) . . ? C8 C9 N2 120.80(18) . . ? C9 C10 C11 119.61(19) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 119.14(18) . . ? C10 C11 C14 119.71(18) . . ? C12 C11 C14 121.14(18) . . ? C13 C12 C11 120.40(19) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 121.19(19) . . ? C12 C13 H13 119.4 . . ? C8 C13 H13 119.4 . . ? O4 C14 O3 126.91(18) . . ? O4 C14 C11 117.62(17) . . ? O3 C14 C11 115.47(17) . . ? C20 C15 C16 116.39(18) . . ? C20 C15 C22 123.25(18) . . ? C16 C15 C22 119.59(18) . . ? C17 C16 C15 124.07(18) . . ? C17 C16 N3 116.81(17) . . ? C15 C16 N3 119.10(17) . . ? C16 C17 C18 118.47(18) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C17 C18 C19 119.11(18) . . ? C17 C18 C21 119.49(17) . . ? C19 C18 C21 121.38(17) . . ? C20 C19 C18 121.19(19) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C15 120.69(19) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? O9 C21 O10 124.99(18) . . ? O9 C21 C18 118.17(17) . . ? O10 C21 C18 116.84(17) . . ? C27 C22 C23 116.54(18) . . ? C27 C22 C15 116.65(18) . . ? C23 C22 C15 126.26(19) . . ? C24 C23 C22 122.90(19) . . ? C24 C23 N4 117.19(18) . . ? C22 C23 N4 119.90(18) . . ? C23 C24 C25 118.90(19) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 119.49(18) . . ? C26 C25 C28 121.45(18) . . ? C24 C25 C28 119.06(18) . . ? C25 C26 C27 120.12(19) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C22 C27 C26 121.68(19) . . ? C22 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? O11 C28 O12 122.53(18) . . ? O11 C28 C25 117.89(18) . . ? O12 C28 C25 119.53(18) . . ? O11 C28 Cd1 56.43(10) . 2_755 ? O12 C28 Cd1 66.62(10) . 2_755 ? C25 C28 Cd1 168.78(14) . 2_755 ? N5 C29 N6 111.38(19) . . ? N5 C29 H29 124.3 . . ? N6 C29 H29 124.3 . . ? C31 C30 N5 109.5(2) . . ? C31 C30 H30 125.2 . . ? N5 C30 H30 125.2 . . ? C30 C31 N6 106.2(2) . . ? C30 C31 H31 126.9 . . ? N6 C31 H31 126.9 . . ? N6 C32 C33 111.69(19) . . ? N6 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? N6 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 114.3(2) . . ? C32 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? C32 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C33 C34 C35 112.57(19) . . ? C33 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? C33 C34 H34B 109.1 . . ? C35 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? C36 C35 C34 113.57(19) . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C34 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? N8 C36 C35 112.99(19) . . ? N8 C36 H36A 109.0 . . ? C35 C36 H36A 109.0 . . ? N8 C36 H36B 109.0 . . ? C35 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? N7 C37 N8 111.30(18) . . ? N7 C37 H37 124.3 . . ? N8 C37 H37 124.3 . . ? C39 C38 N7 109.4(2) . . ? C39 C38 H38 125.3 . . ? N7 C38 H38 125.3 . . ? C38 C39 N8 106.31(19) . . ? C38 C39 H39 126.8 . . ? N8 C39 H39 126.8 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.527 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.073 #=========================END