# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Jian-Fang Ma' 'Stuart Batte' 'Zhong-Min Su' 'Jin Yang' _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University No. 5268, Renmin Street Changchun 130024 CHINA ; _publ_contact_author_email JIANFANGMA@YAHOO.COM.CN _publ_requested_journal 'Chemical Communications' _publ_section_title ; Unusual parallel and inclined interlocking modes in polyrotaxane-like metal-organic frameworks ; data_compound1 _database_code_depnum_ccdc_archive 'CCDC 674032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 Co2 N8 O8' _chemical_formula_sum 'C60 H48 Co2 N8 O8' _chemical_formula_weight 1126.92 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.039(4) _cell_length_b 13.094(5) _cell_length_c 19.901(7) _cell_angle_alpha 100.224(7) _cell_angle_beta 101.872(7) _cell_angle_gamma 108.184(6) _cell_volume 2582.6(16) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 9922 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 26.10 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_process_details '(SAINT; Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 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 14496 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.1163 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.10 _reflns_number_total 9922 _reflns_number_gt 6176 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'SHELXTL (Bruker, 1998)' _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^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9922 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1248 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.020 _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 C1 C 2.3496(4) 0.9907(4) -0.5020(3) 0.0282(12) Uani 1 1 d . . . H1 H 2.3747 0.9674 -0.4617 0.034 Uiso 1 1 calc R . . C2 C 2.3542(5) 1.0951(4) -0.5021(3) 0.0343(13) Uani 1 1 d . . . H2 H 2.3817 1.1555 -0.4627 0.041 Uiso 1 1 calc R . . C3 C 2.2795(5) 0.9908(4) -0.6114(3) 0.0290(12) Uani 1 1 d . . . H3 H 2.2467 0.9684 -0.6607 0.035 Uiso 1 1 calc R . . C4 C 2.2813(5) 1.1840(4) -0.5986(3) 0.0343(13) Uani 1 1 d . . . H4A H 2.2824 1.1737 -0.6480 0.041 Uiso 1 1 calc R . . H4B H 2.3502 1.2548 -0.5716 0.041 Uiso 1 1 calc R . . C5 C 2.1466(5) 1.1869(4) -0.5930(3) 0.0284(12) Uani 1 1 d . . . C6 C 2.0574(5) 1.1074(4) -0.5723(3) 0.0387(14) Uani 1 1 d . . . H6 H 2.0784 1.0477 -0.5612 0.046 Uiso 1 1 calc R . . C7 C 1.9374(5) 1.1152(5) -0.5679(3) 0.0462(16) Uani 1 1 d . . . H7 H 1.8783 1.0613 -0.5537 0.055 Uiso 1 1 calc R . . C8 C 1.9049(5) 1.2037(5) -0.5847(3) 0.0424(15) Uani 1 1 d . . . H8 H 1.8240 1.2089 -0.5815 0.051 Uiso 1 1 calc R . . C9 C 1.9922(5) 1.2841(4) -0.6062(3) 0.0298(12) Uani 1 1 d . . . C10 C 2.1126(5) 1.2754(4) -0.6101(3) 0.0301(12) Uani 1 1 d . . . H10 H 2.1718 1.3292 -0.6245 0.036 Uiso 1 1 calc R . . C11 C 1.9568(5) 1.3785(4) -0.6278(3) 0.0344(13) Uani 1 1 d . . . H11A H 1.8787 1.3814 -0.6136 0.041 Uiso 1 1 calc R . . H11B H 2.0293 1.4485 -0.6034 0.041 Uiso 1 1 calc R . . C12 C 2.0214(5) 1.3961(4) -0.7424(3) 0.0355(13) Uani 1 1 d . . . H12 H 2.1106 1.4412 -0.7233 0.043 Uiso 1 1 calc R . . C13 C 1.9567(5) 1.3499(4) -0.8114(3) 0.0332(13) Uani 1 1 d . . . H13 H 1.9947 1.3575 -0.8487 0.040 Uiso 1 1 calc R . . C14 C 1.8142(5) 1.3007(4) -0.7536(3) 0.0314(12) Uani 1 1 d . . . H14 H 1.7355 1.2686 -0.7424 0.038 Uiso 1 1 calc R . . C15 C -0.0284(5) 0.6550(4) -0.6216(3) 0.0354(13) Uani 1 1 d . . . H15 H -0.0155 0.6623 -0.5730 0.043 Uiso 1 1 calc R . . C16 C -0.1472(5) 0.6099(4) -0.6710(3) 0.0354(13) Uani 1 1 d . . . H16 H -0.2295 0.5795 -0.6631 0.043 Uiso 1 1 calc R . . C17 C 0.0094(4) 0.6658(4) -0.7219(3) 0.0282(12) Uani 1 1 d . . . H17 H 0.0524 0.6812 -0.7565 0.034 Uiso 1 1 calc R . . C18 C -0.2283(5) 0.5717(5) -0.8038(3) 0.0383(14) Uani 1 1 d . . . H18A H -0.3056 0.5882 -0.7974 0.046 Uiso 1 1 calc R . . H18B H -0.2540 0.4914 -0.8170 0.046 Uiso 1 1 calc R . . C19 C -0.1881(4) 0.6162(4) -0.8640(3) 0.0268(11) Uani 1 1 d . . . C20 C -0.0988(5) 0.5844(4) -0.8950(3) 0.0319(13) Uani 1 1 d . . . H20 H -0.0591 0.5385 -0.8765 0.038 Uiso 1 1 calc R . . C21 C -0.0681(5) 0.6200(4) -0.9532(3) 0.0348(13) Uani 1 1 d . . . H21 H -0.0057 0.6007 -0.9723 0.042 Uiso 1 1 calc R . . C22 C -0.1315(5) 0.6848(4) -0.9826(3) 0.0308(12) Uani 1 1 d . . . H22 H -0.1113 0.7084 -1.0218 0.037 Uiso 1 1 calc R . . C23 C -0.2243(5) 0.7148(4) -0.9548(3) 0.0257(11) Uani 1 1 d . . . C24 C -0.2492(4) 0.6824(4) -0.8945(2) 0.0250(11) Uani 1 1 d . . . H24 H -0.3079 0.7054 -0.8740 0.030 Uiso 1 1 calc R . . C25 C -0.3054(5) 0.7721(4) -0.9931(3) 0.0355(13) Uani 1 1 d . . . H25A H -0.3097 0.7532 -1.0431 0.043 Uiso 1 1 calc R . . H25B H -0.3952 0.7430 -0.9892 0.043 Uiso 1 1 calc R . . C26 C -0.3272(5) 0.9560(4) -0.9522(3) 0.0262(11) Uani 1 1 d . . . H26 H -0.4151 0.9271 -0.9513 0.031 Uiso 1 1 calc R . . N8 N -0.2579(4) 1.0637(3) -0.9390(2) 0.0259(9) Uani 1 1 d . . . C28 C -0.1311(5) 0.9659(4) -0.9627(3) 0.0366(13) Uani 1 1 d . . . H28 H -0.0592 0.9474 -0.9700 0.044 Uiso 1 1 calc R . . C29 C 0.4162(5) 0.7988(4) -0.6877(3) 0.0277(12) Uani 1 1 d . . . C30 C 0.5370(5) 0.8433(4) -0.7121(3) 0.0296(12) Uani 1 1 d . . . C31 C 0.6462(5) 0.8114(4) -0.6939(3) 0.0337(13) Uani 1 1 d . . . H31 H 0.6429 0.7591 -0.6676 0.040 Uiso 1 1 calc R . . C32 C 0.7593(5) 0.8565(4) -0.7145(3) 0.0319(13) Uani 1 1 d . . . H32 H 0.8300 0.8325 -0.7030 0.038 Uiso 1 1 calc R . . C33 C 0.7690(5) 0.9378(4) -0.7525(3) 0.0286(12) Uani 1 1 d . . . C34 C 0.6609(5) 0.9703(5) -0.7695(3) 0.0388(14) Uani 1 1 d . . . H34 H 0.6658 1.0249 -0.7941 0.047 Uiso 1 1 calc R . . C35 C 0.5461(5) 0.9237(5) -0.7507(3) 0.0362(13) Uani 1 1 d . . . H35 H 0.4744 0.9459 -0.7639 0.043 Uiso 1 1 calc R . . C36 C 0.8873(5) 0.9883(4) -0.7753(3) 0.0323(12) Uani 1 1 d . . . H36 H 0.8981 1.0570 -0.7849 0.039 Uiso 1 1 calc R . . C37 C 0.9813(5) 0.9469(4) -0.7838(3) 0.0347(13) Uani 1 1 d . . . H37 H 0.9707 0.8777 -0.7748 0.042 Uiso 1 1 calc R . . C38 C 1.0995(5) 0.9995(4) -0.8058(3) 0.0295(12) Uani 1 1 d . . . C39 C 1.1644(5) 0.9359(4) -0.8360(3) 0.0353(13) Uani 1 1 d . . . H39 H 1.1307 0.8591 -0.8428 0.042 Uiso 1 1 calc R . . C40 C 1.2773(5) 0.9835(4) -0.8559(3) 0.0302(12) Uani 1 1 d . . . H40 H 1.3178 0.9386 -0.8763 0.036 Uiso 1 1 calc R . . C41 C 1.3309(5) 1.0983(4) -0.8458(3) 0.0273(12) Uani 1 1 d . . . C42 C 1.4618(5) 1.1540(4) -0.8596(3) 0.0285(12) Uani 1 1 d . . . C43 C 1.2645(5) 1.1625(4) -0.8175(3) 0.0306(12) Uani 1 1 d . . . H43 H 1.2983 1.2392 -0.8111 0.037 Uiso 1 1 calc R . . C44 C 1.1503(5) 1.1154(4) -0.7987(3) 0.0310(12) Uani 1 1 d . . . H44 H 1.1066 1.1599 -0.7813 0.037 Uiso 1 1 calc R . . C45 C 1.7119(5) 1.3038(4) -1.0039(3) 0.0288(12) Uani 1 1 d . . . C46 C 1.6820(4) 1.3659(4) -1.0586(3) 0.0262(11) Uani 1 1 d . . . C47 C 1.6046(4) 1.4312(4) -1.0493(3) 0.0262(11) Uani 1 1 d . . . H47 H 1.5735 1.4375 -1.0093 0.031 Uiso 1 1 calc R . . C48 C 1.5744(5) 1.4869(4) -1.1003(3) 0.0267(11) Uani 1 1 d . . . H48 H 1.5249 1.5317 -1.0931 0.032 Uiso 1 1 calc R . . C49 C 1.6161(5) 1.4770(4) -1.1612(2) 0.0243(11) Uani 1 1 d . . . C50 C 1.6971(5) 1.4151(4) -1.1689(3) 0.0283(12) Uani 1 1 d . . . H50 H 1.7288 1.4096 -1.2087 0.034 Uiso 1 1 calc R . . C51 C 1.7308(5) 1.3616(4) -1.1177(3) 0.0297(12) Uani 1 1 d . . . H51 H 1.7868 1.3222 -1.1231 0.036 Uiso 1 1 calc R . . C52 C 1.5650(4) 1.5260(4) -1.2173(3) 0.0253(11) Uani 1 1 d . . . H52 H 1.5392 1.5856 -1.2032 0.030 Uiso 1 1 calc R . . C53 C 1.5530(4) 1.4917(4) -1.2865(3) 0.0271(12) Uani 1 1 d . . . H53 H 1.5896 1.4390 -1.3000 0.032 Uiso 1 1 calc R . . C54 C 1.4869(5) 1.5306(4) -1.3429(3) 0.0256(11) Uani 1 1 d . . . C55 C 1.4635(4) 1.6303(4) -1.3311(3) 0.0290(12) Uani 1 1 d . . . H55 H 1.4895 1.6754 -1.2850 0.035 Uiso 1 1 calc R . . C56 C 1.4017(5) 1.6632(4) -1.3874(3) 0.0284(12) Uani 1 1 d . . . H56 H 1.3897 1.7311 -1.3790 0.034 Uiso 1 1 calc R . . C57 C 1.3577(4) 1.5941(4) -1.4564(3) 0.0254(11) Uani 1 1 d . . . C58 C 1.3766(5) 1.4939(4) -1.4679(3) 0.0332(13) Uani 1 1 d . . . H58 H 1.3453 1.4464 -1.5134 0.040 Uiso 1 1 calc R . . C59 C 1.4416(5) 1.4636(4) -1.4121(3) 0.0328(13) Uani 1 1 d . . . H59 H 1.4555 1.3966 -1.4211 0.039 Uiso 1 1 calc R . . C60 C 1.3010(5) 1.6316(4) -1.5194(3) 0.0275(12) Uani 1 1 d . . . N1 N 1.8257(4) 1.2897(3) -0.8190(2) 0.0304(10) Uani 1 1 d . . . N2 N 1.9303(4) 1.3639(3) -0.7052(2) 0.0308(10) Uani 1 1 d . . . N3 N 2.3101(4) 1.0939(3) -0.5720(2) 0.0290(10) Uani 1 1 d . . . N4 N 2.3020(4) 0.9240(3) -0.5709(2) 0.0267(10) Uani 1 1 d . . . N5 N 0.0705(4) 0.6886(3) -0.6537(2) 0.0276(10) Uani 1 1 d . . . N6 N -0.1234(4) 0.6175(3) -0.7351(2) 0.0285(10) Uani 1 1 d . . . N7 N -0.2548(4) 0.8936(3) -0.9669(2) 0.0264(10) Uani 1 1 d . . . C27 C -0.1349(5) 1.0689(4) -0.9458(3) 0.0348(13) Uani 1 1 d . . . H27 H -0.0641 1.1343 -0.9395 0.042 Uiso 1 1 calc R . . O1 O 1.5126(3) 1.2574(3) -0.8432(2) 0.0375(9) Uani 1 1 d . . . O2 O 1.5171(3) 1.0914(3) -0.88775(18) 0.0323(8) Uani 1 1 d . . . O3 O 1.6165(3) 1.2644(3) -0.97726(19) 0.0383(9) Uani 1 1 d . . . O4 O 1.8203(3) 1.2935(3) -0.9865(2) 0.0400(10) Uani 1 1 d . . . O5 O 1.2558(3) 1.5683(3) -1.58034(19) 0.0355(9) Uani 1 1 d . . . O6 O 1.3046(3) 1.7325(3) -1.50613(17) 0.0328(9) Uani 1 1 d . . . O7 O 0.4253(3) 0.7502(3) -0.63691(18) 0.0308(8) Uani 1 1 d . . . O8 O 0.3106(3) 0.8118(3) -0.71386(18) 0.0348(9) Uani 1 1 d . . . Co1 Co 1.67850(6) 1.18913(5) -0.90798(4) 0.02580(19) Uani 1 1 d . . . Co2 Co 0.26824(6) 0.75857(5) -0.60402(3) 0.02405(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(3) 0.037(3) 0.023(3) 0.011(2) 0.005(2) 0.014(2) C2 0.032(3) 0.038(3) 0.031(3) 0.003(3) 0.006(2) 0.014(3) C3 0.034(3) 0.028(3) 0.027(3) 0.012(2) 0.004(2) 0.016(2) C4 0.042(3) 0.028(3) 0.046(4) 0.023(3) 0.020(3) 0.019(3) C5 0.031(3) 0.028(3) 0.027(3) 0.009(2) 0.007(2) 0.012(2) C6 0.038(3) 0.036(3) 0.050(4) 0.024(3) 0.016(3) 0.013(3) C7 0.038(3) 0.056(4) 0.055(4) 0.034(3) 0.025(3) 0.013(3) C8 0.034(3) 0.062(4) 0.038(4) 0.018(3) 0.015(3) 0.021(3) C9 0.029(3) 0.037(3) 0.025(3) 0.009(2) 0.002(2) 0.016(3) C10 0.033(3) 0.029(3) 0.026(3) 0.010(2) 0.006(2) 0.008(2) C11 0.037(3) 0.036(3) 0.028(3) 0.007(2) 0.004(2) 0.014(3) C12 0.030(3) 0.036(3) 0.041(4) 0.020(3) 0.005(3) 0.011(3) C13 0.035(3) 0.033(3) 0.037(4) 0.020(3) 0.013(3) 0.012(3) C14 0.028(3) 0.034(3) 0.032(3) 0.012(2) 0.006(2) 0.011(2) C15 0.040(3) 0.043(3) 0.026(3) 0.019(3) 0.010(3) 0.014(3) C16 0.031(3) 0.049(4) 0.034(3) 0.023(3) 0.015(3) 0.015(3) C17 0.027(3) 0.027(3) 0.030(3) 0.014(2) 0.010(2) 0.004(2) C18 0.031(3) 0.041(3) 0.037(4) 0.021(3) 0.002(3) 0.004(3) C19 0.020(2) 0.030(3) 0.027(3) 0.014(2) 0.002(2) 0.004(2) C20 0.029(3) 0.031(3) 0.037(3) 0.015(2) 0.001(2) 0.013(2) C21 0.026(3) 0.037(3) 0.040(4) 0.009(3) 0.007(2) 0.012(3) C22 0.033(3) 0.032(3) 0.029(3) 0.016(2) 0.011(2) 0.007(2) C23 0.029(3) 0.017(3) 0.022(3) 0.003(2) -0.002(2) 0.003(2) C24 0.023(3) 0.026(3) 0.020(3) 0.002(2) -0.001(2) 0.009(2) C25 0.042(3) 0.030(3) 0.033(3) 0.014(2) -0.002(3) 0.015(3) C26 0.023(3) 0.031(3) 0.026(3) 0.016(2) 0.006(2) 0.008(2) N8 0.033(2) 0.027(2) 0.025(2) 0.0147(18) 0.0120(19) 0.013(2) C28 0.037(3) 0.041(3) 0.046(4) 0.023(3) 0.023(3) 0.021(3) C29 0.036(3) 0.027(3) 0.021(3) 0.004(2) 0.012(2) 0.011(2) C30 0.030(3) 0.026(3) 0.032(3) 0.009(2) 0.010(2) 0.008(2) C31 0.039(3) 0.033(3) 0.033(3) 0.015(2) 0.015(3) 0.012(3) C32 0.029(3) 0.039(3) 0.039(3) 0.021(3) 0.014(2) 0.018(3) C33 0.028(3) 0.031(3) 0.028(3) 0.012(2) 0.011(2) 0.008(2) C34 0.043(3) 0.047(4) 0.038(4) 0.029(3) 0.017(3) 0.018(3) C35 0.032(3) 0.055(4) 0.031(3) 0.025(3) 0.009(2) 0.022(3) C36 0.034(3) 0.036(3) 0.027(3) 0.017(2) 0.007(2) 0.011(3) C37 0.036(3) 0.031(3) 0.035(3) 0.016(2) 0.008(2) 0.007(3) C38 0.028(3) 0.036(3) 0.025(3) 0.012(2) 0.006(2) 0.009(2) C39 0.038(3) 0.030(3) 0.040(3) 0.016(3) 0.008(3) 0.013(3) C40 0.029(3) 0.037(3) 0.032(3) 0.015(2) 0.010(2) 0.017(3) C41 0.027(3) 0.030(3) 0.024(3) 0.009(2) 0.006(2) 0.007(2) C42 0.037(3) 0.034(3) 0.023(3) 0.017(2) 0.010(2) 0.018(3) C43 0.032(3) 0.033(3) 0.028(3) 0.012(2) 0.012(2) 0.008(2) C44 0.025(3) 0.029(3) 0.038(3) 0.008(2) 0.011(2) 0.008(2) C45 0.032(3) 0.026(3) 0.027(3) 0.015(2) 0.008(2) 0.006(2) C46 0.026(3) 0.028(3) 0.024(3) 0.018(2) 0.004(2) 0.006(2) C47 0.030(3) 0.033(3) 0.019(3) 0.012(2) 0.013(2) 0.009(2) C48 0.031(3) 0.026(3) 0.028(3) 0.013(2) 0.011(2) 0.012(2) C49 0.031(3) 0.026(3) 0.015(3) 0.010(2) 0.004(2) 0.007(2) C50 0.032(3) 0.040(3) 0.019(3) 0.016(2) 0.011(2) 0.014(3) C51 0.031(3) 0.036(3) 0.029(3) 0.014(2) 0.008(2) 0.018(3) C52 0.028(3) 0.024(3) 0.025(3) 0.012(2) 0.006(2) 0.008(2) C53 0.029(3) 0.029(3) 0.030(3) 0.018(2) 0.010(2) 0.012(2) C54 0.028(3) 0.028(3) 0.027(3) 0.019(2) 0.011(2) 0.011(2) C55 0.028(3) 0.030(3) 0.029(3) 0.012(2) 0.009(2) 0.009(2) C56 0.033(3) 0.028(3) 0.032(3) 0.018(2) 0.014(2) 0.014(2) C57 0.022(3) 0.034(3) 0.026(3) 0.019(2) 0.012(2) 0.009(2) C58 0.043(3) 0.038(3) 0.019(3) 0.009(2) 0.004(2) 0.017(3) C59 0.042(3) 0.029(3) 0.033(3) 0.012(2) 0.009(2) 0.018(3) C60 0.025(3) 0.039(3) 0.028(3) 0.021(3) 0.012(2) 0.013(2) N1 0.030(2) 0.028(2) 0.035(3) 0.015(2) 0.007(2) 0.011(2) N2 0.029(2) 0.028(2) 0.034(3) 0.011(2) 0.001(2) 0.012(2) N3 0.030(2) 0.030(3) 0.033(3) 0.016(2) 0.010(2) 0.013(2) N4 0.028(2) 0.029(2) 0.026(3) 0.0131(19) 0.0080(18) 0.0102(19) N5 0.029(2) 0.031(2) 0.024(3) 0.0152(19) 0.0054(19) 0.011(2) N6 0.027(2) 0.032(3) 0.030(3) 0.017(2) 0.0042(19) 0.011(2) N7 0.031(2) 0.028(2) 0.022(2) 0.0138(18) 0.0040(18) 0.011(2) C27 0.028(3) 0.030(3) 0.052(4) 0.021(3) 0.020(3) 0.007(2) O1 0.037(2) 0.033(2) 0.048(3) 0.0163(18) 0.0199(18) 0.0113(18) O2 0.0319(19) 0.038(2) 0.037(2) 0.0204(17) 0.0156(17) 0.0166(18) O3 0.035(2) 0.051(2) 0.042(2) 0.0355(19) 0.0154(18) 0.0171(19) O4 0.034(2) 0.051(2) 0.050(3) 0.035(2) 0.0170(18) 0.0215(19) O5 0.042(2) 0.041(2) 0.023(2) 0.0161(17) 0.0035(17) 0.0150(18) O6 0.041(2) 0.040(2) 0.027(2) 0.0208(17) 0.0095(16) 0.0204(18) O7 0.039(2) 0.029(2) 0.030(2) 0.0161(16) 0.0168(17) 0.0105(17) O8 0.0293(19) 0.048(2) 0.030(2) 0.0127(17) 0.0104(16) 0.0146(18) Co1 0.0298(4) 0.0276(4) 0.0246(4) 0.0152(3) 0.0074(3) 0.0122(3) Co2 0.0259(4) 0.0283(4) 0.0212(4) 0.0132(3) 0.0061(3) 0.0107(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.352(7) . ? C1 N4 1.382(6) . ? C1 H1 0.9300 . ? C2 N3 1.371(6) . ? C2 H2 0.9300 . ? C3 N4 1.334(6) . ? C3 N3 1.336(6) . ? C3 H3 0.9300 . ? C4 N3 1.470(6) . ? C4 C5 1.526(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.379(7) . ? C5 C10 1.400(6) . ? C6 C7 1.379(7) . ? C6 H6 0.9300 . ? C7 C8 1.390(7) . ? C7 H7 0.9300 . ? C8 C9 1.384(7) . ? C8 H8 0.9300 . ? C9 C10 1.386(6) . ? C9 C11 1.513(7) . ? C10 H10 0.9300 . ? C11 N2 1.473(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.340(7) . ? C12 N2 1.374(7) . ? C12 H12 0.9300 . ? C13 N1 1.376(6) . ? C13 H13 0.9300 . ? C14 N1 1.321(6) . ? C14 N2 1.342(6) . ? C14 H14 0.9300 . ? C15 C16 1.347(7) . ? C15 N5 1.372(6) . ? C15 H15 0.9300 . ? C16 N6 1.369(6) . ? C16 H16 0.9300 . ? C17 N5 1.319(6) . ? C17 N6 1.349(6) . ? C17 H17 0.9300 . ? C18 N6 1.480(6) . ? C18 C19 1.509(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.394(7) . ? C19 C24 1.399(6) . ? C20 C21 1.387(7) . ? C20 H20 0.9300 . ? C21 C22 1.390(7) . ? C21 H21 0.9300 . ? C22 C23 1.385(7) . ? C22 H22 0.9300 . ? C23 C24 1.392(7) . ? C23 C25 1.512(6) . ? C24 H24 0.9300 . ? C25 N7 1.464(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N8 1.325(6) . ? C26 N7 1.346(6) . ? C26 H26 0.9300 . ? N8 C27 1.375(6) . ? N8 Co1 2.027(4) 1_355 ? C28 C27 1.346(7) . ? C28 N7 1.373(6) . ? C28 H28 0.9300 . ? C29 O8 1.251(5) . ? C29 O7 1.290(6) . ? C29 C30 1.495(7) . ? C30 C31 1.395(6) . ? C30 C35 1.401(7) . ? C31 C32 1.383(7) . ? C31 H31 0.9300 . ? C32 C33 1.401(7) . ? C32 H32 0.9300 . ? C33 C34 1.386(7) . ? C33 C36 1.469(7) . ? C34 C35 1.382(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.338(7) . ? C36 H36 0.9300 . ? C37 C38 1.467(7) . ? C37 H37 0.9300 . ? C38 C39 1.392(7) . ? C38 C44 1.413(7) . ? C39 C40 1.381(7) . ? C39 H39 0.9300 . ? C40 C41 1.393(7) . ? C40 H40 0.9300 . ? C41 C43 1.395(6) . ? C41 C42 1.507(7) . ? C42 O1 1.243(6) . ? C42 O2 1.284(5) . ? C43 C44 1.379(7) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 O4 1.232(5) . ? C45 O3 1.282(6) . ? C45 C46 1.512(6) . ? C46 C51 1.391(7) . ? C46 C47 1.401(6) . ? C47 C48 1.396(6) . ? C47 H47 0.9300 . ? C48 C49 1.382(7) . ? C48 H48 0.9300 . ? C49 C50 1.394(6) . ? C49 C52 1.483(6) . ? C50 C51 1.388(6) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.335(7) . ? C52 H52 0.9300 . ? C53 C54 1.467(6) . ? C53 H53 0.9300 . ? C54 C59 1.388(7) . ? C54 C55 1.399(6) . ? C55 C56 1.395(6) . ? C55 H55 0.9300 . ? C56 C57 1.396(7) . ? C56 H56 0.9300 . ? C57 C58 1.379(6) . ? C57 C60 1.515(6) . ? C58 C59 1.383(7) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 O5 1.242(6) . ? C60 O6 1.286(6) . ? N1 Co1 2.040(4) . ? N4 Co2 2.038(4) 1_755 ? N5 Co2 2.030(4) . ? C27 H27 0.9300 . ? O2 Co1 2.007(3) . ? O3 Co1 1.964(3) . ? O6 Co2 2.018(3) 1_664 ? O7 Co2 2.002(3) . ? Co1 N8 2.027(4) 1_755 ? Co2 O6 2.018(3) 1_446 ? Co2 N4 2.038(4) 1_355 ? 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 C2 C1 N4 109.8(5) . . ? C2 C1 H1 125.1 . . ? N4 C1 H1 125.1 . . ? C1 C2 N3 106.2(4) . . ? C1 C2 H2 126.9 . . ? N3 C2 H2 126.9 . . ? N4 C3 N3 111.3(4) . . ? N4 C3 H3 124.4 . . ? N3 C3 H3 124.4 . . ? N3 C4 C5 111.8(4) . . ? N3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C10 118.8(5) . . ? C6 C5 C4 123.7(4) . . ? C10 C5 C4 117.6(5) . . ? C7 C6 C5 120.7(5) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 120.1(6) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.3(5) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.1(5) . . ? C8 C9 C11 121.4(5) . . ? C10 C9 C11 119.5(5) . . ? C9 C10 C5 121.1(5) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? N2 C11 C9 111.1(4) . . ? N2 C11 H11A 109.4 . . ? C9 C11 H11A 109.4 . . ? N2 C11 H11B 109.4 . . ? C9 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 N2 106.6(5) . . ? C13 C12 H12 126.7 . . ? N2 C12 H12 126.7 . . ? C12 C13 N1 110.0(5) . . ? C12 C13 H13 125.0 . . ? N1 C13 H13 125.0 . . ? N1 C14 N2 111.5(5) . . ? N1 C14 H14 124.2 . . ? N2 C14 H14 124.2 . . ? C16 C15 N5 109.7(5) . . ? C16 C15 H15 125.1 . . ? N5 C15 H15 125.1 . . ? C15 C16 N6 106.8(5) . . ? C15 C16 H16 126.6 . . ? N6 C16 H16 126.6 . . ? N5 C17 N6 111.6(4) . . ? N5 C17 H17 124.2 . . ? N6 C17 H17 124.2 . . ? N6 C18 C19 114.4(4) . . ? N6 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? N6 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C24 118.1(5) . . ? C20 C19 C18 121.1(5) . . ? C24 C19 C18 120.5(5) . . ? C21 C20 C19 121.0(5) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.4(5) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 121.2(5) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 118.5(5) . . ? C22 C23 C25 120.4(5) . . ? C24 C23 C25 120.9(5) . . ? C23 C24 C19 121.8(5) . . ? C23 C24 H24 119.1 . . ? C19 C24 H24 119.1 . . ? N7 C25 C23 115.1(4) . . ? N7 C25 H25A 108.5 . . ? C23 C25 H25A 108.5 . . ? N7 C25 H25B 108.5 . . ? C23 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? N8 C26 N7 111.7(4) . . ? N8 C26 H26 124.1 . . ? N7 C26 H26 124.1 . . ? C26 N8 C27 104.7(4) . . ? C26 N8 Co1 125.7(3) . 1_355 ? C27 N8 Co1 129.4(3) . 1_355 ? C27 C28 N7 106.2(4) . . ? C27 C28 H28 126.9 . . ? N7 C28 H28 126.9 . . ? O8 C29 O7 120.8(5) . . ? O8 C29 C30 121.1(5) . . ? O7 C29 C30 118.1(4) . . ? C31 C30 C35 118.1(5) . . ? C31 C30 C29 121.6(5) . . ? C35 C30 C29 120.3(4) . . ? C32 C31 C30 121.0(5) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 121.0(5) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C34 C33 C32 117.8(5) . . ? C34 C33 C36 119.3(5) . . ? C32 C33 C36 122.9(4) . . ? C35 C34 C33 121.7(5) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 C35 C30 120.5(5) . . ? C34 C35 H35 119.8 . . ? C30 C35 H35 119.8 . . ? C37 C36 C33 127.6(5) . . ? C37 C36 H36 116.2 . . ? C33 C36 H36 116.2 . . ? C36 C37 C38 126.6(5) . . ? C36 C37 H37 116.7 . . ? C38 C37 H37 116.7 . . ? C39 C38 C44 117.5(5) . . ? C39 C38 C37 120.7(5) . . ? C44 C38 C37 121.7(5) . . ? C40 C39 C38 121.9(5) . . ? C40 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? C39 C40 C41 120.5(5) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C43 118.0(5) . . ? C40 C41 C42 121.7(4) . . ? C43 C41 C42 120.1(4) . . ? O1 C42 O2 122.5(5) . . ? O1 C42 C41 119.7(4) . . ? O2 C42 C41 117.8(5) . . ? C44 C43 C41 121.8(5) . . ? C44 C43 H43 119.1 . . ? C41 C43 H43 119.1 . . ? C43 C44 C38 120.1(5) . . ? C43 C44 H44 120.0 . . ? C38 C44 H44 120.0 . . ? O4 C45 O3 123.3(5) . . ? O4 C45 C46 122.0(5) . . ? O3 C45 C46 114.7(4) . . ? C51 C46 C47 118.6(4) . . ? C51 C46 C45 122.0(4) . . ? C47 C46 C45 119.4(4) . . ? C48 C47 C46 119.7(5) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C49 C48 C47 121.6(4) . . ? C49 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? C48 C49 C50 118.3(4) . . ? C48 C49 C52 118.4(4) . . ? C50 C49 C52 123.1(4) . . ? C51 C50 C49 120.6(5) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C46 120.9(4) . . ? C50 C51 H51 119.5 . . ? C46 C51 H51 119.5 . . ? C53 C52 C49 125.5(5) . . ? C53 C52 H52 117.2 . . ? C49 C52 H52 117.2 . . ? C52 C53 C54 125.3(5) . . ? C52 C53 H53 117.4 . . ? C54 C53 H53 117.4 . . ? C59 C54 C55 117.7(4) . . ? C59 C54 C53 118.5(4) . . ? C55 C54 C53 123.8(5) . . ? C56 C55 C54 120.9(5) . . ? C56 C55 H55 119.6 . . ? C54 C55 H55 119.6 . . ? C55 C56 C57 120.0(5) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 119.2(4) . . ? C58 C57 C60 119.3(4) . . ? C56 C57 C60 121.2(4) . . ? C57 C58 C59 120.4(5) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? C58 C59 C54 121.8(5) . . ? C58 C59 H59 119.1 . . ? C54 C59 H59 119.1 . . ? O5 C60 O6 122.6(5) . . ? O5 C60 C57 121.3(5) . . ? O6 C60 C57 116.1(4) . . ? C14 N1 C13 105.2(4) . . ? C14 N1 Co1 124.6(3) . . ? C13 N1 Co1 129.9(4) . . ? C14 N2 C12 106.7(5) . . ? C14 N2 C11 125.2(5) . . ? C12 N2 C11 127.3(4) . . ? C3 N3 C2 107.7(4) . . ? C3 N3 C4 125.2(4) . . ? C2 N3 C4 126.5(4) . . ? C3 N4 C1 105.0(4) . . ? C3 N4 Co2 127.1(3) . 1_755 ? C1 N4 Co2 127.9(3) . 1_755 ? C17 N5 C15 105.4(4) . . ? C17 N5 Co2 128.6(3) . . ? C15 N5 Co2 126.0(3) . . ? C17 N6 C16 106.4(4) . . ? C17 N6 C18 129.8(4) . . ? C16 N6 C18 123.6(4) . . ? C26 N7 C28 106.8(4) . . ? C26 N7 C25 125.8(4) . . ? C28 N7 C25 126.7(4) . . ? C28 C27 N8 110.5(5) . . ? C28 C27 H27 124.7 . . ? N8 C27 H27 124.7 . . ? C42 O2 Co1 108.1(3) . . ? C45 O3 Co1 107.3(3) . . ? C60 O6 Co2 102.4(3) . 1_664 ? C29 O7 Co2 100.5(3) . . ? O3 Co1 O2 107.03(14) . . ? O3 Co1 N8 120.08(16) . 1_755 ? O2 Co1 N8 94.78(15) . 1_755 ? O3 Co1 N1 115.92(16) . . ? O2 Co1 N1 113.96(16) . . ? N8 Co1 N1 103.44(16) 1_755 . ? O7 Co2 O6 104.12(14) . 1_446 ? O7 Co2 N5 131.31(15) . . ? O6 Co2 N5 109.86(15) 1_446 . ? O7 Co2 N4 105.70(15) . 1_355 ? O6 Co2 N4 96.30(15) 1_446 1_355 ? N5 Co2 N4 104.10(15) . 1_355 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.713 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.093 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 674033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C120 H88 Cd4 N16 O16, 4(O)' _chemical_formula_sum 'C120 H96 Cd4 N16 O20' _chemical_formula_weight 2531.73 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 'P 21/n' _symmetry_space_group_name_Hall '-p 2yn' 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 15.0358(10) _cell_length_b 34.679(2) _cell_length_c 21.8823(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.8230(10) _cell_angle_gamma 90.00 _cell_volume 11369.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 22406 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 26.05 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5120 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.856 _exptl_absorpt_process_details '(SAINT; Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 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 63711 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.05 _reflns_number_total 22406 _reflns_number_gt 12590 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'SHELXTL (Bruker, 1998)' _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^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22406 _refine_ls_number_parameters 1441 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1648 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.034 _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 C1 C 0.3488(4) 0.2332(2) 0.6855(3) 0.0363(18) Uani 1 1 d . . . H1 H 0.3653 0.2574 0.7008 0.044 Uiso 1 1 calc R . . C2 C 0.3502(5) 0.1729(2) 0.6638(4) 0.057(2) Uani 1 1 d . . . H2 H 0.3686 0.1474 0.6613 0.068 Uiso 1 1 calc R . . C3 C 0.2008(4) 0.2533(2) 0.6345(3) 0.049(2) Uani 1 1 d . . . H3 H 0.1548 0.2589 0.6589 0.059 Uiso 1 1 calc R . . C4 C 0.2087(4) 0.2723(2) 0.5724(3) 0.0388(19) Uani 1 1 d . . . C5 C 0.2802(5) 0.2959(3) 0.5626(4) 0.064(3) Uani 1 1 d . . . H5 H 0.3258 0.2990 0.5936 0.077 Uiso 1 1 calc R . . C6 C 0.2850(5) 0.3148(3) 0.5083(4) 0.060(3) Uani 1 1 d . . . H6 H 0.3339 0.3307 0.5037 0.072 Uiso 1 1 calc R . . C7 C 0.2724(5) 0.1871(3) 0.6392(4) 0.057(2) Uani 1 1 d . . . H7 H 0.2272 0.1734 0.6171 0.069 Uiso 1 1 calc R . . C8 C 0.1417(5) 0.2690(3) 0.5259(4) 0.061(3) Uani 1 1 d . . . H8 H 0.0920 0.2539 0.5317 0.074 Uiso 1 1 calc R . . C9 C 0.3772(4) 0.3604(2) 0.3953(3) 0.044(2) Uani 1 1 d . . . H9 H 0.3737 0.3808 0.4226 0.053 Uiso 1 1 calc R . . C10 C 0.4487(5) 0.3506(2) 0.3655(3) 0.0398(19) Uani 1 1 d . . . H10 H 0.5037 0.3631 0.3693 0.048 Uiso 1 1 calc R . . C11 C 0.3441(4) 0.3105(2) 0.3381(3) 0.0314(17) Uani 1 1 d . . . H11 H 0.3129 0.2899 0.3193 0.038 Uiso 1 1 calc R . . C12 C 0.2215(4) 0.3322(2) 0.4011(3) 0.045(2) Uani 1 1 d D . . H12 H 0.1706 0.3428 0.3805 0.054 Uiso 1 1 calc R . . C13 C 0.2198(4) 0.3114(2) 0.4595(3) 0.0379(19) Uani 1 1 d D . . C14 C 0.1471(5) 0.2880(3) 0.4706(4) 0.059(3) Uani 1 1 d . . . H14 H 0.1009 0.2851 0.4399 0.070 Uiso 1 1 calc R . . C15 C 0.6024(5) 0.1470(2) 0.6349(3) 0.048(2) Uani 1 1 d . . . H15 H 0.5499 0.1327 0.6329 0.057 Uiso 1 1 calc R . . C16 C 0.6740(5) 0.1391(2) 0.6053(3) 0.050(2) Uani 1 1 d . . . H16 H 0.6803 0.1184 0.5791 0.060 Uiso 1 1 calc R . . C17 C 0.7011(4) 0.1906(2) 0.6588(3) 0.0331(17) Uani 1 1 d . . . H17 H 0.7305 0.2120 0.6764 0.040 Uiso 1 1 calc R . . C18 C 0.8241(5) 0.1702(2) 0.5961(3) 0.048(2) Uani 1 1 d D . . H18 H 0.8757 0.1605 0.6170 0.058 Uiso 1 1 calc R . . C19 C 0.8255(4) 0.1900(2) 0.5372(3) 0.0395(19) Uani 1 1 d D . . C20 C 0.7527(5) 0.1910(3) 0.4928(4) 0.058(3) Uani 1 1 d . . . H20 H 0.6992 0.1797 0.5016 0.070 Uiso 1 1 calc R . . C21 C 0.7576(5) 0.2080(3) 0.4372(4) 0.060(3) Uani 1 1 d . . . H21 H 0.7075 0.2084 0.4092 0.072 Uiso 1 1 calc R . . C22 C 0.8356(4) 0.2248(2) 0.4216(3) 0.045(2) Uani 1 1 d . . . C23 C 0.9077(4) 0.2244(2) 0.4645(4) 0.052(2) Uani 1 1 d . . . H23 H 0.9608 0.2360 0.4553 0.062 Uiso 1 1 calc R . . C24 C 0.9029(4) 0.2072(2) 0.5206(4) 0.049(2) Uani 1 1 d . . . H24 H 0.9534 0.2070 0.5483 0.059 Uiso 1 1 calc R . . C25 C 0.8448(4) 0.2407(3) 0.3582(3) 0.058(3) Uani 1 1 d . . . H25 H 0.8894 0.2331 0.3338 0.070 Uiso 1 1 calc R . . C26 C 0.6957(4) 0.2621(2) 0.3103(3) 0.0359(18) Uani 1 1 d . . . H26 H 0.6755 0.2377 0.2983 0.043 Uiso 1 1 calc R . . C27 C 0.7803(5) 0.3081(3) 0.3477(4) 0.065(3) Uani 1 1 d . . . H27 H 0.8284 0.3217 0.3666 0.078 Uiso 1 1 calc R . . C28 C 0.7032(5) 0.3232(2) 0.3245(4) 0.060(3) Uani 1 1 d . . . H28 H 0.6883 0.3493 0.3241 0.072 Uiso 1 1 calc R . . C29 C 0.9216(5) 0.6023(2) 1.3681(3) 0.0413(19) Uani 1 1 d . . . H29 H 0.9753 0.6158 1.3713 0.050 Uiso 1 1 calc R . . C30 C 0.8503(5) 0.6115(2) 1.3976(3) 0.0417(19) Uani 1 1 d . . . H30 H 0.8449 0.6321 1.4243 0.050 Uiso 1 1 calc R . . C31 C 0.8220(4) 0.5605(2) 1.3414(3) 0.0346(18) Uani 1 1 d . . . H31 H 0.7921 0.5395 1.3228 0.042 Uiso 1 1 calc R . . C32 C 0.6957(4) 0.5817(2) 1.4021(3) 0.047(2) Uani 1 1 d D . . H32 H 0.6451 0.5920 1.3807 0.057 Uiso 1 1 calc R . . C33 C 0.7609(5) 0.5655(3) 1.5101(4) 0.064(3) Uani 1 1 d . . . H33 H 0.8098 0.5812 1.5050 0.077 Uiso 1 1 calc R . . C34 C 0.7558(5) 0.5469(3) 1.5652(4) 0.069(3) Uani 1 1 d . . . H34 H 0.8017 0.5503 1.5959 0.083 Uiso 1 1 calc R . . C35 C 0.6941(4) 0.5614(2) 1.4609(3) 0.042(2) Uani 1 1 d D . . C36 C 0.6219(5) 0.5393(2) 1.4738(4) 0.052(2) Uani 1 1 d . . . H36 H 0.5742 0.5369 1.4441 0.062 Uiso 1 1 calc R . . C37 C 0.2671(9) 0.1175(3) -0.0253(5) 0.106(4) Uani 1 1 d DU . . H37 H 0.3256 0.1195 -0.0358 0.128 Uiso 1 1 calc R . . C38 C 0.2171(7) 0.0931(3) -0.0661(5) 0.073(3) Uani 1 1 d D . . C39 C 0.2631(6) 0.0745(3) -0.1095(5) 0.074(3) Uani 1 1 d . . . H39 H 0.3236 0.0797 -0.1110 0.089 Uiso 1 1 calc R . . C40 C 0.2236(5) 0.0491(2) -0.1499(4) 0.053(2) Uani 1 1 d . . . H40 H 0.2576 0.0365 -0.1774 0.064 Uiso 1 1 calc R . . C41 C 0.1329(4) 0.0415(2) -0.1508(3) 0.0351(17) Uani 1 1 d . . . C42 C 0.0827(5) 0.0602(2) -0.1102(4) 0.048(2) Uani 1 1 d . . . H42 H 0.0215 0.0562 -0.1110 0.058 Uiso 1 1 calc R . . C43 C 0.1261(7) 0.0854(3) -0.0677(4) 0.068(3) Uani 1 1 d . . . H43 H 0.0927 0.0976 -0.0394 0.082 Uiso 1 1 calc R . . C44 C 0.0895(4) 0.0116(2) -0.1935(3) 0.0306(16) Uani 1 1 d . . . C45 C 0.6176(5) 0.5205(3) 1.5296(4) 0.057(2) Uani 1 1 d . . . H45 H 0.5675 0.5057 1.5353 0.068 Uiso 1 1 calc R . . C46 C 0.6839(4) 0.5229(2) 1.5768(3) 0.041(2) Uani 1 1 d D . . C47 C 0.5328(4) 0.3603(2) 0.1763(3) 0.0326(17) Uani 1 1 d . . . C48 C 0.5354(4) 0.39519(19) 0.1368(3) 0.0286(16) Uani 1 1 d . . . C49 C 0.5182(4) 0.3927(2) 0.0732(3) 0.0326(17) Uani 1 1 d . . . H49 H 0.5103 0.3687 0.0546 0.039 Uiso 1 1 calc R . . C50 C 0.5127(4) 0.4259(2) 0.0376(3) 0.0323(17) Uani 1 1 d . . . H50 H 0.5017 0.4238 -0.0048 0.039 Uiso 1 1 calc R . . C51 C 0.5234(4) 0.4625(2) 0.0639(3) 0.0313(17) Uani 1 1 d . . . C52 C 0.5437(4) 0.4643(2) 0.1270(3) 0.0374(18) Uani 1 1 d . . . H52 H 0.5537 0.4882 0.1455 0.045 Uiso 1 1 calc R . . C53 C 0.5496(4) 0.4315(2) 0.1631(4) 0.0389(19) Uani 1 1 d . . . H53 H 0.5632 0.4337 0.2052 0.047 Uiso 1 1 calc R . . C54 C 0.5132(4) 0.4982(2) 0.0294(3) 0.040(2) Uani 1 1 d . . . H54 H 0.5266 0.5208 0.0509 0.048 Uiso 1 1 calc R . . C55 C 0.4369(4) 0.2398(2) 0.1918(3) 0.0285(16) Uani 1 1 d . . . C56 C 0.3946(4) 0.21108(19) 0.1479(3) 0.0340(17) Uani 1 1 d . . . C57 C 0.3039(5) 0.2030(2) 0.1467(4) 0.057(2) Uani 1 1 d . . . H57 H 0.2701 0.2144 0.1755 0.068 Uiso 1 1 calc R . . C58 C 0.2640(6) 0.1789(3) 0.1042(5) 0.080(3) Uani 1 1 d . . . H58 H 0.2032 0.1740 0.1048 0.097 Uiso 1 1 calc R . . C59 C 0.2558(8) 0.1372(3) 0.0205(5) 0.102(4) Uani 1 1 d DU . . H59 H 0.1974 0.1358 0.0315 0.122 Uiso 1 1 calc R . . C60 C 0.3100(8) 0.1611(3) 0.0601(5) 0.078(4) Uani 1 1 d D . . C61 C 0.3996(7) 0.1684(3) 0.0620(4) 0.067(3) Uani 1 1 d . . . H61 H 0.4325 0.1567 0.0331 0.080 Uiso 1 1 calc R . . C62 C 0.4440(5) 0.1929(2) 0.1056(3) 0.047(2) Uani 1 1 d . . . H62 H 0.5053 0.1968 0.1062 0.056 Uiso 1 1 calc R . . C63 C 0.5160(4) 0.1372(2) 0.8205(3) 0.0376(18) Uani 1 1 d . . . C64 C 0.5076(4) 0.1023(2) 0.8599(3) 0.0330(17) Uani 1 1 d . . . C65 C 0.4960(6) 0.0660(2) 0.8343(4) 0.055(2) Uani 1 1 d . . . H65 H 0.4931 0.0630 0.7919 0.066 Uiso 1 1 calc R . . C66 C 0.4946(4) 0.0375(2) 0.9344(4) 0.0381(19) Uani 1 1 d . . . C67 C 0.4887(5) 0.0339(2) 0.8715(4) 0.051(2) Uani 1 1 d . . . H67 H 0.4796 0.0097 0.8538 0.061 Uiso 1 1 calc R . . C68 C 0.4921(5) 0.0015(2) 0.9707(3) 0.048(2) Uani 1 1 d . . . H68 H 0.4778 -0.0211 0.9491 0.057 Uiso 1 1 calc R . . C69 C 0.5063(4) 0.0744(2) 0.9603(3) 0.0376(19) Uani 1 1 d . . . H69 H 0.5105 0.0772 1.0027 0.045 Uiso 1 1 calc R . . C70 C 0.5118(4) 0.1067(2) 0.9231(3) 0.0325(17) Uani 1 1 d . . . H70 H 0.5182 0.1311 0.9405 0.039 Uiso 1 1 calc R . . C71 C 0.6081(4) 0.25881(19) 0.8037(3) 0.0288(16) Uani 1 1 d . . . C72 C 0.6396(4) 0.29015(19) 0.8472(3) 0.0323(17) Uani 1 1 d . . . C73 C 0.7297(4) 0.2962(2) 0.8640(4) 0.055(2) Uani 1 1 d . . . H73 H 0.7719 0.2819 0.8450 0.066 Uiso 1 1 calc R . . C74 C 0.7580(5) 0.3229(3) 0.9082(4) 0.059(3) Uani 1 1 d . . . H74 H 0.8188 0.3264 0.9181 0.071 Uiso 1 1 calc R . . C75 C 0.6973(4) 0.3445(2) 0.9382(3) 0.0336(17) Uani 1 1 d . . . C76 C 0.6068(4) 0.3386(2) 0.9215(3) 0.043(2) Uani 1 1 d . . . H76 H 0.5647 0.3526 0.9410 0.051 Uiso 1 1 calc R . . C77 C 0.5784(4) 0.3122(2) 0.8763(3) 0.0371(18) Uani 1 1 d . . . H77 H 0.5177 0.3092 0.8653 0.045 Uiso 1 1 calc R . . C78 C 0.7240(4) 0.3724(2) 0.9849(3) 0.044(2) Uani 1 1 d . . . H78 H 0.6774 0.3859 1.0006 0.053 Uiso 1 1 calc R . . C79 C 0.8040(4) 0.3816(2) 1.0086(3) 0.045(2) Uani 1 1 d . . . H79 H 0.8508 0.3685 0.9927 0.054 Uiso 1 1 calc R . . C80 C 0.8291(4) 0.4094(2) 1.0560(3) 0.0355(18) Uani 1 1 d . . . C81 C 0.9184(4) 0.4147(2) 1.0747(4) 0.043(2) Uani 1 1 d . . . H81 H 0.9606 0.4005 1.0555 0.051 Uiso 1 1 calc R . . C82 C 0.8867(4) 0.46239(19) 1.1482(3) 0.0288(16) Uani 1 1 d . . . C83 C 0.9473(4) 0.4400(2) 1.1204(3) 0.0376(18) Uani 1 1 d . . . H83 H 1.0079 0.4420 1.1326 0.045 Uiso 1 1 calc R . . C84 C 0.7969(4) 0.4571(2) 1.1319(4) 0.057(3) Uani 1 1 d . . . H84 H 0.7550 0.4713 1.1512 0.068 Uiso 1 1 calc R . . C85 C 0.7691(5) 0.4306(2) 1.0869(4) 0.058(3) Uani 1 1 d . . . H85 H 0.7082 0.4270 1.0771 0.069 Uiso 1 1 calc R . . C86 C 0.9174(4) 0.4923(2) 1.1949(3) 0.0319(17) Uani 1 1 d . . . C87 C 1.0059(4) 0.6125(2) 1.1769(3) 0.0302(16) Uani 1 1 d . . . C88 C 1.0071(4) 0.64706(19) 1.1364(3) 0.0290(16) Uani 1 1 d . . . C89 C 0.9921(4) 0.6445(2) 1.0733(3) 0.0293(16) Uani 1 1 d . . . H89 H 0.9848 0.6203 1.0551 0.035 Uiso 1 1 calc R . . C90 C 0.9879(4) 0.67642(19) 1.0372(3) 0.0316(17) Uani 1 1 d . . . H90 H 0.9762 0.6741 0.9950 0.038 Uiso 1 1 calc R . . C91 C 1.0012(4) 0.7133(2) 1.0641(3) 0.0352(18) Uani 1 1 d . . . C92 C 1.0180(4) 0.7159(2) 1.1265(3) 0.0373(18) Uani 1 1 d . . . H92 H 1.0270 0.7401 1.1445 0.045 Uiso 1 1 calc R . . C93 C 1.0218(4) 0.6833(2) 1.1633(3) 0.0368(18) Uani 1 1 d . . . H93 H 1.0340 0.6856 1.2055 0.044 Uiso 1 1 calc R . . C94 C 0.9954(4) 0.7491(2) 1.0275(3) 0.0408(19) Uani 1 1 d . . . H94 H 1.0086 0.7719 1.0488 0.049 Uiso 1 1 calc R . . C95 C 0.9741(4) 0.7525(2) 0.9691(3) 0.0365(18) Uani 1 1 d . . . H95 H 0.9592 0.7300 0.9477 0.044 Uiso 1 1 calc R . . C96 C 0.9711(4) 0.7883(2) 0.9331(3) 0.0342(18) Uani 1 1 d . . . C97 C 0.9621(5) 0.7860(2) 0.8700(4) 0.046(2) Uani 1 1 d . . . H97 H 0.9528 0.7620 0.8513 0.055 Uiso 1 1 calc R . . C98 C 0.9669(5) 0.8187(2) 0.8338(3) 0.046(2) Uani 1 1 d . . . H98 H 0.9616 0.8166 0.7913 0.055 Uiso 1 1 calc R . . C99 C 0.9796(4) 0.85489(19) 0.8611(3) 0.0313(16) Uani 1 1 d . . . C100 C 0.9854(4) 0.8579(2) 0.9241(3) 0.0281(15) Uani 1 1 d . . . H100 H 0.9916 0.8820 0.9427 0.034 Uiso 1 1 calc R . . C101 C 0.9820(4) 0.8250(2) 0.9597(3) 0.0353(18) Uani 1 1 d . . . H101 H 0.9870 0.8272 1.0022 0.042 Uiso 1 1 calc R . . C102 C 0.9882(4) 0.8897(2) 0.8207(4) 0.0386(19) Uani 1 1 d . . . C103 C 0.8544(5) 1.1112(2) 0.3933(3) 0.044(2) Uani 1 1 d . . . H103 H 0.8504 1.1319 0.4198 0.052 Uiso 1 1 calc R . . C104 C 0.8210(4) 1.0597(2) 0.3377(3) 0.0310(16) Uani 1 1 d . . . H104 H 0.7894 1.0389 0.3199 0.037 Uiso 1 1 calc R . . C105 C 0.7003(4) 1.0818(2) 0.4005(3) 0.045(2) Uani 1 1 d . . . H105 H 0.6496 1.0929 0.3804 0.054 Uiso 1 1 calc R . . C106 C 0.6997(4) 1.0603(2) 0.4602(3) 0.0377(18) Uani 1 1 d . . . C107 C 0.6212(4) 1.0426(2) 0.4745(3) 0.044(2) Uani 1 1 d . . . H107 H 0.5715 1.0428 0.4461 0.052 Uiso 1 1 calc R . . C108 C 0.6161(5) 1.0246(3) 0.5308(4) 0.052(2) Uani 1 1 d . . . H108 H 0.5630 1.0127 0.5393 0.063 Uiso 1 1 calc R . . C109 C 0.6881(4) 1.0238(2) 0.5746(3) 0.045(2) Uani 1 1 d . . . C111 C 0.8276(4) 0.9877(2) 0.6872(3) 0.0404(19) Uani 1 1 d . . . H111 H 0.8464 1.0125 0.6980 0.048 Uiso 1 1 calc R . . C112 C 0.7464(5) 0.9404(3) 0.6492(4) 0.057(2) Uani 1 1 d . . . H112 H 0.7001 0.9261 0.6294 0.069 Uiso 1 1 calc R . . C113 C 0.8246(5) 0.9267(3) 0.6747(4) 0.056(2) Uani 1 1 d . . . H113 H 0.8415 0.9009 0.6757 0.067 Uiso 1 1 calc R . . C114 C 0.6788(4) 1.0076(3) 0.6377(4) 0.063(3) Uani 1 1 d . . . H114 H 0.6331 1.0147 0.6615 0.075 Uiso 1 1 calc R . . C115 C 0.7664(4) 1.0413(3) 0.5590(4) 0.056(3) Uani 1 1 d . . . H115 H 0.8162 1.0409 0.5873 0.068 Uiso 1 1 calc R . . C116 C 0.7728(4) 1.0591(3) 0.5037(4) 0.050(2) Uani 1 1 d . . . H116 H 0.8264 1.0704 0.4952 0.059 Uiso 1 1 calc R . . C117 C 0.8251(5) 0.4236(2) 1.6638(4) 0.060(3) Uani 1 1 d . . . H117 H 0.8429 0.3980 1.6609 0.072 Uiso 1 1 calc R . . C118 C 0.7472(5) 0.4381(3) 1.6394(5) 0.068(3) Uani 1 1 d . . . H118 H 0.7020 0.4247 1.6168 0.082 Uiso 1 1 calc R . . C119 C 0.8246(4) 0.4829(2) 1.6869(3) 0.0300(16) Uani 1 1 d . . . H119 H 0.8412 0.5068 1.7033 0.036 Uiso 1 1 calc R . . C120 C 0.6769(4) 0.5050(2) 1.6376(3) 0.050(2) Uani 1 1 d D . . H120 H 0.6322 0.5111 1.6628 0.060 Uiso 1 1 calc R . . C121 C 0.9248(5) 1.1012(2) 0.3621(3) 0.045(2) Uani 1 1 d . . . H121 H 0.9791 1.1142 0.3642 0.055 Uiso 1 1 calc R . . N1 N 0.4275(3) 0.31955(16) 0.3291(3) 0.0309(14) Uani 1 1 d . . . N2 N 0.3977(3) 0.20174(18) 0.6930(3) 0.0367(14) Uani 1 1 d . . . N3 N 0.2721(4) 0.22528(18) 0.6525(3) 0.0396(15) Uani 1 1 d . . . N4 N 0.3108(3) 0.33484(17) 0.3778(3) 0.0334(14) Uani 1 1 d . . . N5 N 0.6190(4) 0.18001(17) 0.6690(3) 0.0339(14) Uani 1 1 d . . . N6 N 0.7358(4) 0.16640(19) 0.6201(3) 0.0378(15) Uani 1 1 d . . . N7 N 0.7762(3) 0.2695(2) 0.3390(3) 0.0423(16) Uani 1 1 d . . . N8 N 0.6495(3) 0.29370(17) 0.3014(3) 0.0345(14) Uani 1 1 d . . . N9 N 0.7476(3) 0.47627(19) 1.6545(3) 0.0386(15) Uani 1 1 d . . . N10 N 0.8741(3) 0.45218(16) 1.6933(3) 0.0329(14) Uani 1 1 d . . . N11 N 0.9045(3) 0.57010(16) 1.3323(3) 0.0328(14) Uani 1 1 d . . . N12 N 0.7862(3) 0.58418(18) 1.3804(3) 0.0340(14) Uani 1 1 d . . . N13 N 0.9043(3) 1.06885(16) 0.3264(3) 0.0348(15) Uani 1 1 d . . . N14 N 0.7890(4) 1.08365(17) 0.3773(3) 0.0350(14) Uani 1 1 d . . . N15 N 0.8757(3) 0.95673(18) 0.6988(3) 0.0367(15) Uani 1 1 d . . . N16 N 0.7484(4) 0.9796(2) 0.6582(3) 0.0442(17) Uani 1 1 d . . . O1 O 0.5057(3) 0.17023(14) 0.8412(2) 0.0353(12) Uani 1 1 d . . . O2 O 0.5356(4) 0.13171(16) 0.7664(3) 0.0696(19) Uani 1 1 d . . . O1W O 0.8653(3) 0.67450(15) 1.2624(3) 0.0626(17) Uani 1 1 d . . . O3 O 0.5260(3) 0.25799(13) 0.7867(2) 0.0356(12) Uani 1 1 d . . . O2W O 0.8920(4) 1.07705(15) 0.7608(3) 0.0681(17) Uani 1 1 d . . . O4 O 0.6616(3) 0.23447(14) 0.7878(2) 0.0427(13) Uani 1 1 d . . . O3W O 0.6730(5) 0.6739(2) 1.2714(4) 0.124(3) Uani 1 1 d . . . O5 O 0.9992(3) 0.49273(13) 1.2133(2) 0.0329(11) Uani 1 1 d . . . O4W O 0.6966(5) 1.0743(2) 0.7643(4) 0.110(3) Uani 1 1 d . . . O6 O 0.8636(3) 0.51719(14) 1.2113(2) 0.0419(13) Uani 1 1 d . . . O7 O 1.0162(3) 0.57942(14) 1.1556(2) 0.0375(12) Uani 1 1 d . . . O8 O 0.9925(3) 0.61761(14) 1.2326(2) 0.0461(14) Uani 1 1 d . . . O9 O 0.5223(3) 0.36571(13) 0.2321(2) 0.0446(13) Uani 1 1 d . . . O10 O 0.5382(3) 0.32724(14) 0.1541(2) 0.0382(12) Uani 1 1 d . . . O11 O 0.5200(3) 0.23857(13) 0.2052(2) 0.0367(12) Uani 1 1 d . . . O12 O 0.3884(3) 0.26549(14) 0.2122(2) 0.0396(13) Uani 1 1 d . . . O13 O 0.9828(3) 0.92271(14) 0.8435(2) 0.0351(12) Uani 1 1 d . . . O14 O 1.0022(4) 0.88419(15) 0.7658(3) 0.0675(19) Uani 1 1 d . . . O15 O 0.1371(3) -0.01416(15) -0.2135(2) 0.0450(14) Uani 1 1 d . . . O16 O 0.0056(3) 0.01252(13) -0.2061(2) 0.0361(12) Uani 1 1 d . . . Cd1 Cd 0.99020(3) 0.552830(14) 1.25694(2) 0.02626(13) Uani 1 1 d . . . Cd2 Cd 1.01078(3) 0.950654(14) 0.74775(2) 0.02724(13) Uani 1 1 d . . . Cd3 Cd 0.53327(3) 0.197558(14) 0.74445(2) 0.02756(13) Uani 1 1 d . . . Cd4 Cd 0.51250(3) 0.300304(14) 0.25348(2) 0.02643(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(4) 0.039(5) 0.027(4) -0.003(4) 0.000(3) -0.004(3) C2 0.052(5) 0.041(5) 0.074(7) -0.026(5) -0.008(4) -0.007(4) C3 0.033(4) 0.074(6) 0.044(5) 0.021(4) 0.019(3) 0.018(4) C4 0.026(4) 0.053(5) 0.038(5) 0.003(4) 0.006(3) 0.005(3) C5 0.041(4) 0.097(8) 0.053(6) 0.021(6) -0.007(4) -0.010(5) C6 0.034(4) 0.081(7) 0.063(6) 0.023(5) -0.006(4) -0.015(4) C7 0.042(5) 0.064(7) 0.063(6) -0.022(5) -0.016(4) -0.004(4) C8 0.047(5) 0.088(7) 0.050(6) 0.006(5) 0.012(4) -0.028(5) C9 0.044(4) 0.049(5) 0.039(5) -0.007(4) 0.006(3) 0.000(4) C10 0.049(4) 0.042(5) 0.027(4) -0.001(4) -0.001(3) -0.015(3) C11 0.036(4) 0.030(5) 0.028(4) 0.002(3) -0.001(3) 0.002(3) C12 0.029(4) 0.066(6) 0.040(5) 0.006(4) -0.003(3) 0.008(4) C13 0.027(3) 0.057(5) 0.030(4) 0.001(4) 0.002(3) 0.010(3) C14 0.045(5) 0.088(8) 0.041(5) -0.006(5) -0.009(4) -0.026(4) C15 0.063(5) 0.048(5) 0.034(5) -0.012(4) 0.015(4) -0.024(4) C16 0.065(5) 0.048(6) 0.038(5) -0.012(4) 0.016(4) -0.005(4) C17 0.036(4) 0.036(5) 0.027(4) 0.002(3) 0.002(3) -0.005(3) C18 0.035(4) 0.072(6) 0.038(5) 0.011(4) 0.006(3) 0.007(4) C19 0.041(4) 0.046(5) 0.031(4) 0.004(4) 0.001(3) 0.018(3) C20 0.030(4) 0.095(7) 0.049(6) 0.021(5) 0.000(3) -0.001(4) C21 0.033(4) 0.105(8) 0.041(5) 0.018(5) -0.006(3) 0.008(4) C22 0.031(4) 0.064(6) 0.039(5) 0.015(4) 0.001(3) 0.014(4) C23 0.031(4) 0.071(6) 0.054(6) 0.025(5) -0.001(4) -0.004(4) C24 0.032(4) 0.063(6) 0.049(5) 0.001(5) -0.010(3) -0.005(4) C25 0.034(4) 0.096(7) 0.045(5) 0.035(5) 0.010(3) 0.027(4) C26 0.036(4) 0.038(5) 0.033(5) 0.004(4) 0.000(3) -0.003(3) C27 0.048(5) 0.079(8) 0.063(6) 0.007(6) -0.025(4) -0.026(5) C28 0.063(6) 0.040(6) 0.072(7) 0.003(5) -0.016(5) -0.013(4) C29 0.043(4) 0.045(5) 0.036(5) -0.009(4) 0.005(3) -0.013(3) C30 0.053(5) 0.043(5) 0.030(5) -0.012(4) 0.013(3) -0.003(4) C31 0.033(4) 0.029(4) 0.041(5) 0.005(4) -0.005(3) -0.008(3) C32 0.027(4) 0.085(7) 0.028(5) 0.016(4) 0.001(3) 0.011(4) C33 0.037(4) 0.102(8) 0.053(6) 0.014(6) 0.001(4) -0.022(4) C34 0.045(5) 0.109(9) 0.050(6) 0.020(6) -0.008(4) -0.019(5) C35 0.014(3) 0.066(6) 0.045(5) -0.006(4) 0.000(3) 0.006(3) C36 0.046(5) 0.073(7) 0.033(5) 0.007(5) -0.014(3) -0.015(4) C37 0.158(8) 0.064(7) 0.095(7) 0.014(6) -0.006(7) 0.015(6) C38 0.114(8) 0.028(5) 0.067(7) -0.013(5) -0.056(6) -0.009(5) C39 0.061(6) 0.047(6) 0.106(9) -0.018(6) -0.043(6) -0.012(4) C40 0.037(4) 0.038(5) 0.082(7) -0.018(5) -0.011(4) 0.000(3) C41 0.042(4) 0.023(4) 0.039(5) 0.005(4) -0.007(3) 0.003(3) C42 0.067(5) 0.035(5) 0.041(5) -0.004(4) 0.004(4) 0.003(4) C43 0.125(9) 0.038(6) 0.040(6) -0.017(5) -0.005(5) 0.015(5) C44 0.040(4) 0.023(4) 0.030(4) -0.005(3) 0.006(3) -0.007(3) C45 0.039(4) 0.077(7) 0.053(6) 0.017(5) -0.003(4) -0.018(4) C46 0.023(3) 0.069(6) 0.033(5) 0.003(4) 0.009(3) 0.007(3) C47 0.023(3) 0.034(5) 0.041(5) 0.008(4) 0.002(3) -0.004(3) C48 0.029(3) 0.023(4) 0.034(4) 0.008(3) 0.003(3) -0.002(3) C49 0.027(3) 0.033(4) 0.038(5) -0.001(4) 0.001(3) 0.000(3) C50 0.031(4) 0.038(5) 0.028(4) 0.006(4) 0.002(3) 0.001(3) C51 0.028(3) 0.024(4) 0.042(5) 0.005(4) 0.004(3) -0.001(3) C52 0.046(4) 0.021(4) 0.046(5) 0.000(4) 0.010(3) 0.000(3) C53 0.038(4) 0.041(5) 0.038(5) 0.009(4) 0.005(3) 0.001(3) C54 0.039(4) 0.031(4) 0.052(5) 0.008(5) 0.008(4) -0.006(3) C55 0.032(4) 0.029(4) 0.025(4) 0.000(3) 0.002(3) -0.007(3) C56 0.040(4) 0.021(4) 0.039(5) -0.001(3) -0.009(3) -0.001(3) C57 0.043(4) 0.034(5) 0.093(7) -0.015(5) 0.000(4) -0.005(4) C58 0.062(6) 0.046(6) 0.124(10) -0.025(7) -0.040(6) -0.005(5) C59 0.143(8) 0.070(7) 0.090(7) 0.021(6) -0.005(6) 0.004(6) C60 0.108(8) 0.034(6) 0.080(8) 0.004(6) -0.066(7) -0.018(5) C61 0.129(9) 0.038(6) 0.032(5) -0.019(4) -0.004(5) -0.001(5) C62 0.066(5) 0.032(5) 0.042(5) -0.003(4) 0.005(4) -0.001(4) C63 0.041(4) 0.033(5) 0.039(5) 0.010(4) 0.007(3) -0.005(3) C64 0.042(4) 0.030(4) 0.028(4) 0.003(3) 0.010(3) 0.000(3) C65 0.096(7) 0.030(5) 0.041(6) -0.005(4) 0.018(4) -0.007(4) C66 0.040(4) 0.030(5) 0.044(5) 0.012(4) 0.004(3) 0.000(3) C67 0.079(6) 0.029(5) 0.045(6) 0.000(4) 0.012(4) -0.003(4) C68 0.047(4) 0.040(5) 0.057(6) 0.006(5) 0.008(4) -0.006(3) C69 0.032(4) 0.048(5) 0.033(5) 0.006(4) -0.001(3) -0.005(3) C70 0.037(4) 0.026(4) 0.035(5) 0.004(3) 0.006(3) -0.001(3) C71 0.032(4) 0.020(4) 0.034(4) 0.000(3) 0.002(3) -0.001(3) C72 0.033(4) 0.023(4) 0.040(5) -0.003(3) -0.002(3) 0.001(3) C73 0.031(4) 0.047(5) 0.088(7) -0.037(5) 0.008(4) -0.003(3) C74 0.030(4) 0.072(7) 0.074(7) -0.031(5) -0.006(4) -0.009(4) C75 0.037(4) 0.029(4) 0.035(5) -0.007(4) 0.000(3) 0.003(3) C76 0.037(4) 0.043(5) 0.048(5) -0.015(4) 0.004(3) 0.010(3) C77 0.032(4) 0.032(4) 0.046(5) -0.006(4) -0.006(3) 0.002(3) C78 0.037(4) 0.046(5) 0.048(5) -0.003(4) -0.001(3) 0.002(3) C79 0.035(4) 0.045(5) 0.054(5) -0.021(4) -0.001(3) 0.005(3) C80 0.042(4) 0.028(4) 0.037(5) -0.011(4) 0.000(3) 0.005(3) C81 0.031(4) 0.042(5) 0.054(5) -0.017(4) -0.002(3) 0.003(3) C82 0.029(3) 0.022(4) 0.035(4) -0.007(3) 0.002(3) -0.002(3) C83 0.028(4) 0.041(5) 0.043(5) -0.011(4) -0.004(3) 0.001(3) C84 0.027(4) 0.065(6) 0.077(7) -0.038(5) 0.006(4) 0.005(4) C85 0.032(4) 0.066(6) 0.074(7) -0.037(5) -0.004(4) 0.001(4) C86 0.032(4) 0.032(4) 0.031(4) -0.002(3) 0.000(3) -0.002(3) C87 0.023(3) 0.026(4) 0.042(5) 0.006(4) 0.001(3) -0.003(3) C88 0.026(3) 0.021(4) 0.041(5) 0.006(3) 0.005(3) -0.002(3) C89 0.030(3) 0.026(4) 0.032(4) 0.000(3) 0.005(3) -0.005(3) C90 0.030(4) 0.031(4) 0.033(5) 0.006(3) 0.000(3) -0.001(3) C91 0.034(4) 0.028(4) 0.045(5) 0.008(4) 0.009(3) 0.000(3) C92 0.058(5) 0.018(4) 0.037(5) -0.003(4) 0.013(4) -0.001(3) C93 0.051(4) 0.030(4) 0.031(4) 0.000(4) 0.012(3) -0.008(3) C94 0.050(4) 0.033(5) 0.040(5) -0.002(4) 0.006(3) -0.004(3) C95 0.051(4) 0.020(4) 0.040(5) 0.002(4) 0.007(3) -0.006(3) C96 0.035(4) 0.030(4) 0.038(5) 0.006(4) 0.005(3) 0.004(3) C97 0.080(6) 0.017(4) 0.041(5) 0.005(4) 0.013(4) -0.004(3) C98 0.091(6) 0.028(5) 0.018(4) -0.005(4) 0.007(4) -0.010(4) C99 0.040(4) 0.022(4) 0.034(4) 0.005(3) 0.008(3) -0.003(3) C100 0.035(4) 0.027(4) 0.022(4) -0.001(3) 0.002(3) -0.002(3) C101 0.036(4) 0.039(5) 0.030(5) 0.000(4) -0.001(3) 0.002(3) C102 0.041(4) 0.034(5) 0.042(5) 0.009(4) 0.010(3) -0.012(3) C103 0.067(5) 0.031(5) 0.035(5) -0.010(4) 0.014(4) -0.014(4) C104 0.036(4) 0.031(4) 0.025(4) 0.001(3) -0.002(3) -0.004(3) C105 0.030(4) 0.073(6) 0.031(5) 0.011(4) 0.001(3) 0.014(4) C106 0.031(4) 0.045(5) 0.037(5) -0.004(4) 0.005(3) 0.009(3) C107 0.034(4) 0.061(6) 0.034(5) 0.000(4) -0.010(3) -0.007(4) C108 0.033(4) 0.073(6) 0.051(6) 0.009(5) 0.003(4) -0.012(4) C109 0.030(4) 0.065(6) 0.040(5) 0.006(4) 0.009(3) 0.005(4) C111 0.035(4) 0.052(6) 0.034(5) 0.000(4) 0.003(3) -0.010(3) C112 0.041(5) 0.065(7) 0.062(6) 0.000(5) -0.019(4) -0.019(4) C113 0.057(5) 0.053(6) 0.055(6) -0.006(5) -0.010(4) -0.014(4) C114 0.028(4) 0.109(8) 0.052(6) 0.031(5) 0.013(4) 0.018(4) C115 0.023(4) 0.100(8) 0.046(5) 0.012(5) -0.003(3) 0.004(4) C116 0.024(4) 0.081(6) 0.044(5) 0.012(5) 0.005(3) 0.002(4) C117 0.058(5) 0.036(5) 0.081(7) -0.024(5) -0.025(5) -0.002(4) C118 0.047(5) 0.058(6) 0.093(8) -0.017(6) -0.033(5) -0.008(4) C119 0.031(4) 0.032(4) 0.027(4) -0.003(3) 0.002(3) -0.004(3) C120 0.027(4) 0.082(7) 0.044(5) 0.024(5) 0.014(3) 0.018(4) C121 0.051(5) 0.044(5) 0.042(5) -0.009(4) 0.008(4) -0.021(4) N1 0.032(3) 0.030(4) 0.032(4) -0.001(3) 0.004(2) -0.004(2) N2 0.040(3) 0.038(4) 0.032(4) -0.006(3) 0.002(2) 0.000(3) N3 0.036(3) 0.045(4) 0.038(4) -0.008(3) 0.003(3) -0.002(3) N4 0.030(3) 0.044(4) 0.026(4) -0.001(3) 0.002(2) -0.005(3) N5 0.042(3) 0.033(4) 0.026(4) 0.000(3) 0.001(3) -0.006(3) N6 0.039(3) 0.047(4) 0.028(4) -0.001(3) 0.004(3) 0.001(3) N7 0.032(3) 0.058(5) 0.036(4) 0.014(3) -0.004(3) -0.008(3) N8 0.031(3) 0.033(4) 0.037(4) -0.002(3) -0.009(2) -0.008(2) N9 0.033(3) 0.047(4) 0.035(4) 0.001(3) -0.002(3) 0.001(3) N10 0.029(3) 0.028(4) 0.041(4) 0.001(3) -0.004(2) 0.002(2) N11 0.034(3) 0.027(4) 0.037(4) 0.007(3) 0.002(3) -0.007(2) N12 0.032(3) 0.044(4) 0.027(4) 0.001(3) 0.005(2) -0.002(3) N13 0.038(3) 0.033(4) 0.035(4) -0.006(3) 0.007(3) -0.008(2) N14 0.041(3) 0.033(4) 0.031(4) 0.001(3) 0.003(3) 0.002(3) N15 0.033(3) 0.037(4) 0.039(4) 0.001(3) -0.004(3) -0.002(3) N16 0.031(3) 0.064(5) 0.038(4) 0.010(4) 0.003(3) -0.005(3) O1 0.039(3) 0.025(3) 0.041(3) 0.000(2) 0.000(2) -0.001(2) O2 0.138(6) 0.034(4) 0.042(4) 0.008(3) 0.035(4) -0.001(3) O1W 0.058(3) 0.044(4) 0.089(5) 0.006(3) 0.028(3) 0.009(3) O3 0.034(3) 0.028(3) 0.044(3) -0.002(2) 0.000(2) -0.004(2) O2W 0.065(4) 0.045(4) 0.099(5) 0.006(3) 0.035(3) -0.001(3) O4 0.038(3) 0.036(3) 0.053(4) -0.019(3) -0.003(2) 0.004(2) O3W 0.113(6) 0.079(6) 0.186(9) -0.037(6) 0.048(6) -0.013(4) O5 0.030(2) 0.031(3) 0.038(3) -0.003(2) -0.003(2) -0.0010(19) O4W 0.117(6) 0.065(5) 0.152(8) 0.030(5) 0.044(5) 0.009(4) O6 0.035(3) 0.039(3) 0.051(4) -0.016(3) 0.000(2) 0.002(2) O7 0.049(3) 0.022(3) 0.041(3) 0.003(2) -0.003(2) -0.001(2) O8 0.072(3) 0.029(3) 0.041(4) 0.010(3) 0.025(3) 0.005(2) O9 0.074(4) 0.027(3) 0.035(3) 0.012(3) 0.020(3) 0.006(2) O10 0.048(3) 0.024(3) 0.041(3) 0.001(2) -0.005(2) -0.006(2) O11 0.032(3) 0.036(3) 0.041(3) -0.003(2) -0.002(2) -0.007(2) O12 0.034(3) 0.037(3) 0.047(3) -0.011(3) 0.000(2) 0.004(2) O13 0.043(3) 0.030(3) 0.031(3) 0.006(2) -0.002(2) -0.005(2) O14 0.144(6) 0.028(3) 0.036(4) 0.006(3) 0.042(4) -0.003(3) O15 0.041(3) 0.043(3) 0.051(4) -0.016(3) 0.002(2) 0.002(2) O16 0.032(3) 0.030(3) 0.046(3) -0.003(2) 0.001(2) -0.003(2) Cd1 0.0299(3) 0.0216(3) 0.0267(3) 0.0014(2) -0.0009(2) -0.00140(19) Cd2 0.0320(3) 0.0240(3) 0.0255(3) 0.0015(2) 0.0011(2) -0.00511(19) Cd3 0.0353(3) 0.0221(3) 0.0250(3) 0.0008(2) 0.00124(19) -0.0044(2) Cd4 0.0295(2) 0.0225(3) 0.0268(3) 0.0026(2) -0.00038(19) -0.0031(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 C1 N2 1.320(9) . ? C1 N3 1.336(8) . ? C1 H1 0.9300 . ? C2 C7 1.339(10) . ? C2 N2 1.357(9) . ? C2 H2 0.9300 . ? C3 N3 1.477(9) . ? C3 C4 1.522(10) . ? C3 H3 0.9300 . ? C4 C8 1.375(10) . ? C4 C5 1.383(10) . ? C5 C6 1.364(11) . ? C5 H5 0.9300 . ? C6 C13 1.392(10) . ? C6 H6 0.9300 . ? C7 N3 1.357(10) . ? C7 H7 0.9300 . ? C8 C14 1.386(10) . ? C8 H8 0.9300 . ? C9 C10 1.346(9) . ? C9 N4 1.367(9) . ? C9 H9 0.9300 . ? C10 N1 1.363(8) . ? C10 H10 0.9300 . ? C11 N1 1.322(8) . ? C11 N4 1.340(8) . ? C11 H11 0.9300 . ? C12 C13 1.470(9) . ? C12 N4 1.478(8) . ? C12 H12 0.9300 . ? C13 C14 1.399(10) . ? C14 H14 0.9300 . ? C15 C16 1.332(10) . ? C15 N5 1.377(9) . ? C15 H15 0.9300 . ? C16 N6 1.347(9) . ? C16 H16 0.9300 . ? C17 N5 1.324(8) . ? C17 N6 1.330(8) . ? C17 H17 0.9300 . ? C18 C19 1.462(9) . ? C18 N6 1.474(8) . ? C18 H18 0.9300 . ? C19 C24 1.383(10) . ? C19 C20 1.402(9) . ? C20 C21 1.360(10) . ? C20 H20 0.9300 . ? C21 C22 1.378(10) . ? C21 H21 0.9300 . ? C22 C23 1.373(9) . ? C22 C25 1.509(10) . ? C23 C24 1.372(10) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N7 1.471(9) . ? C25 H25 0.9300 . ? C26 N8 1.302(8) . ? C26 N7 1.339(8) . ? C26 H26 0.9300 . ? C27 C28 1.333(11) . ? C27 N7 1.356(10) . ? C27 H27 0.9300 . ? C28 N8 1.374(9) . ? C28 H28 0.9300 . ? C29 C30 1.338(9) . ? C29 N11 1.376(8) . ? C29 H29 0.9300 . ? C30 N12 1.382(9) . ? C30 H30 0.9300 . ? C31 N11 1.316(8) . ? C31 N12 1.330(9) . ? C31 H31 0.9300 . ? C32 C35 1.469(9) . ? C32 N12 1.480(8) . ? C32 H32 0.9300 . ? C33 C34 1.375(11) . ? C33 C35 1.416(10) . ? C33 H33 0.9300 . ? C34 C46 1.403(10) . ? C34 H34 0.9300 . ? C35 C36 1.378(10) . ? C36 C45 1.389(10) . ? C36 H36 0.9300 . ? C37 C59 1.236(11) . ? C37 C38 1.403(11) . ? C37 H37 0.9300 . ? C38 C39 1.381(13) . ? C38 C43 1.391(13) . ? C39 C40 1.350(10) . ? C39 H39 0.9300 . ? C40 C41 1.387(9) . ? C40 H40 0.9300 . ? C41 C42 1.376(10) . ? C41 C44 1.507(9) . ? C42 C43 1.396(11) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 O15 1.247(8) . ? C44 O16 1.269(7) . ? C44 Cd2 2.695(7) 1_444 ? C45 C46 1.378(10) . ? C45 H45 0.9300 . ? C46 C120 1.480(9) . ? C47 O10 1.251(8) . ? C47 O9 1.258(8) . ? C47 C48 1.489(9) . ? C47 Cd4 2.713(7) . ? C48 C53 1.393(9) . ? C48 C49 1.397(9) . ? C49 C50 1.389(9) . ? C49 H49 0.9300 . ? C50 C51 1.398(9) . ? C50 H50 0.9300 . ? C51 C52 1.390(9) . ? C51 C54 1.450(9) . ? C52 C53 1.383(9) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 C54 1.319(13) 3_665 ? C54 H54 0.9300 . ? C55 O12 1.258(8) . ? C55 O11 1.260(7) . ? C55 C56 1.487(9) . ? C55 Cd4 2.696(7) . ? C56 C62 1.386(10) . ? C56 C57 1.391(9) . ? C57 C58 1.353(11) . ? C57 H57 0.9300 . ? C58 C60 1.379(15) . ? C58 H58 0.9300 . ? C59 C60 1.409(12) . ? C59 H59 0.9300 . ? C60 C61 1.368(13) . ? C61 C62 1.403(10) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 O1 1.246(8) . ? C63 O2 1.258(8) . ? C63 C64 1.497(9) . ? C63 Cd3 2.699(7) . ? C64 C65 1.386(10) . ? C64 C70 1.388(9) . ? C65 C67 1.387(10) . ? C65 H65 0.9300 . ? C66 C67 1.376(10) . ? C66 C69 1.405(10) . ? C66 C68 1.480(10) . ? C67 H67 0.9300 . ? C68 C68 1.290(14) 3_657 ? C68 H68 0.9300 . ? C69 C70 1.394(9) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 O4 1.236(7) . ? C71 O3 1.259(7) . ? C71 C72 1.496(9) . ? C71 Cd3 2.685(7) . ? C72 C77 1.389(9) . ? C72 C73 1.390(9) . ? C73 C74 1.380(10) . ? C73 H73 0.9300 . ? C74 C75 1.387(10) . ? C74 H74 0.9300 . ? C75 C76 1.395(9) . ? C75 C78 1.440(9) . ? C76 C77 1.389(9) . ? C76 H76 0.9300 . ? C77 H77 0.9300 . ? C78 C79 1.308(9) . ? C78 H78 0.9300 . ? C79 C80 1.442(9) . ? C79 H79 0.9300 . ? C80 C81 1.382(9) . ? C80 C85 1.385(9) . ? C81 C83 1.374(9) . ? C81 H81 0.9300 . ? C82 C83 1.378(9) . ? C82 C84 1.378(9) . ? C82 C86 1.501(9) . ? C83 H83 0.9300 . ? C84 C85 1.384(10) . ? C84 H84 0.9300 . ? C85 H85 0.9300 . ? C86 O6 1.256(8) . ? C86 O5 1.262(7) . ? C86 Cd1 2.684(7) . ? C87 O7 1.252(8) . ? C87 O8 1.264(8) . ? C87 C88 1.492(9) . ? C87 Cd1 2.734(7) . ? C88 C89 1.384(9) . ? C88 C93 1.398(9) . ? C89 C90 1.358(9) . ? C89 H89 0.9300 . ? C90 C91 1.414(9) . ? C90 H90 0.9300 . ? C91 C92 1.371(9) . ? C91 C94 1.477(9) . ? C92 C93 1.386(9) . ? C92 H92 0.9300 . ? C93 H93 0.9300 . ? C94 C95 1.296(10) . ? C94 H94 0.9300 . ? C95 C96 1.467(9) . ? C95 H95 0.9300 . ? C96 C97 1.378(9) . ? C96 C101 1.404(9) . ? C97 C98 1.392(9) . ? C97 H97 0.9300 . ? C98 C99 1.395(9) . ? C98 H98 0.9300 . ? C99 C100 1.378(9) . ? C99 C102 1.508(9) . ? C100 C101 1.386(9) . ? C100 H100 0.9300 . ? C101 H101 0.9300 . ? C102 O14 1.251(9) . ? C102 O13 1.255(8) . ? C102 Cd2 2.688(7) . ? C103 C121 1.353(10) . ? C103 N14 1.394(9) . ? C103 H103 0.9300 . ? C104 N14 1.319(8) . ? C104 N13 1.336(8) . ? C104 H104 0.9300 . ? C105 N14 1.469(8) . ? C105 C106 1.504(10) . ? C105 H105 0.9300 . ? C106 C107 1.391(9) . ? C106 C116 1.393(9) . ? C107 C108 1.388(10) . ? C107 H107 0.9300 . ? C108 C109 1.385(10) . ? C108 H108 0.9300 . ? C109 C115 1.392(10) . ? C109 C114 1.507(10) . ? C111 N15 1.308(9) . ? C111 N16 1.332(8) . ? C111 H111 0.9300 . ? C112 C113 1.345(11) . ? C112 N16 1.373(10) . ? C112 H112 0.9300 . ? C113 N15 1.373(9) . ? C113 H113 0.9300 . ? C114 N16 1.471(10) . ? C114 H114 0.9300 . ? C115 C116 1.368(10) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C117 C118 1.343(10) . ? C117 N10 1.365(9) . ? C117 H117 0.9300 . ? C118 N9 1.365(10) . ? C118 H118 0.9300 . ? C119 N10 1.300(8) . ? C119 N9 1.325(8) . ? C119 H119 0.9300 . ? C120 N9 1.480(9) . ? C120 H120 0.9300 . ? C121 N13 1.387(9) . ? C121 H121 0.9300 . ? N1 Cd4 2.274(5) . ? N2 Cd3 2.249(5) . ? N5 Cd3 2.262(6) . ? N8 Cd4 2.244(5) . ? N10 Cd1 2.237(5) 3_768 ? N11 Cd1 2.257(6) . ? N13 Cd2 2.251(5) 3_776 ? N15 Cd2 2.225(5) . ? O1 Cd3 2.387(5) . ? O2 Cd3 2.333(5) . ? O3 Cd3 2.297(5) . ? O4 Cd3 2.440(4) . ? O5 Cd1 2.301(4) . ? O6 Cd1 2.414(4) . ? O7 Cd1 2.462(5) . ? O8 Cd1 2.310(5) . ? O9 Cd4 2.323(5) . ? O10 Cd4 2.428(5) . ? O11 Cd4 2.394(5) . ? O12 Cd4 2.340(4) . ? O13 Cd2 2.378(4) . ? O14 Cd2 2.344(5) . ? O15 Cd2 2.355(5) 1_444 ? O16 Cd2 2.375(5) 1_444 ? Cd1 N10 2.237(5) 3_768 ? Cd2 N13 2.251(5) 3_776 ? Cd2 O15 2.355(5) 1_666 ? Cd2 O16 2.375(5) 1_666 ? Cd2 C44 2.695(7) 1_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N3 110.0(7) . . ? N2 C1 H1 125.0 . . ? N3 C1 H1 125.0 . . ? C7 C2 N2 109.1(7) . . ? C7 C2 H2 125.4 . . ? N2 C2 H2 125.4 . . ? N3 C3 C4 114.4(5) . . ? N3 C3 H3 122.8 . . ? C4 C3 H3 122.8 . . ? C8 C4 C5 117.7(7) . . ? C8 C4 C3 121.1(6) . . ? C5 C4 C3 121.0(7) . . ? C6 C5 C4 121.3(7) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C13 122.7(7) . . ? C5 C6 H6 118.7 . . ? C13 C6 H6 118.7 . . ? C2 C7 N3 106.8(7) . . ? C2 C7 H7 126.6 . . ? N3 C7 H7 126.6 . . ? C4 C8 C14 120.9(7) . . ? C4 C8 H8 119.5 . . ? C14 C8 H8 119.5 . . ? C10 C9 N4 107.2(7) . . ? C10 C9 H9 126.4 . . ? N4 C9 H9 126.4 . . ? C9 C10 N1 109.0(6) . . ? C9 C10 H10 125.5 . . ? N1 C10 H10 125.5 . . ? N1 C11 N4 111.0(6) . . ? N1 C11 H11 124.5 . . ? N4 C11 H11 124.5 . . ? C13 C12 N4 114.4(5) . . ? C13 C12 H12 122.8 . . ? N4 C12 H12 122.8 . . ? C6 C13 C14 115.3(7) . . ? C6 C13 C12 124.2(7) . . ? C14 C13 C12 120.4(6) . . ? C8 C14 C13 122.0(7) . . ? C8 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C16 C15 N5 108.5(7) . . ? C16 C15 H15 125.8 . . ? N5 C15 H15 125.8 . . ? C15 C16 N6 108.0(7) . . ? C15 C16 H16 126.0 . . ? N6 C16 H16 126.0 . . ? N5 C17 N6 110.7(6) . . ? N5 C17 H17 124.7 . . ? N6 C17 H17 124.7 . . ? C19 C18 N6 115.9(6) . . ? C19 C18 H18 122.1 . . ? N6 C18 H18 122.1 . . ? C24 C19 C20 115.6(7) . . ? C24 C19 C18 120.6(6) . . ? C20 C19 C18 123.6(7) . . ? C21 C20 C19 122.2(7) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 121.1(7) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C23 C22 C21 117.8(7) . . ? C23 C22 C25 120.2(7) . . ? C21 C22 C25 121.8(7) . . ? C24 C23 C22 121.2(7) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C19 122.1(7) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? N7 C25 C22 113.3(6) . . ? N7 C25 H25 123.4 . . ? C22 C25 H25 123.4 . . ? N8 C26 N7 111.1(7) . . ? N8 C26 H26 124.4 . . ? N7 C26 H26 124.4 . . ? C28 C27 N7 107.8(7) . . ? C28 C27 H27 126.1 . . ? N7 C27 H27 126.1 . . ? C27 C28 N8 108.2(8) . . ? C27 C28 H28 125.9 . . ? N8 C28 H28 125.9 . . ? C30 C29 N11 110.5(6) . . ? C30 C29 H29 124.8 . . ? N11 C29 H29 124.8 . . ? C29 C30 N12 105.8(7) . . ? C29 C30 H30 127.1 . . ? N12 C30 H30 127.1 . . ? N11 C31 N12 112.2(6) . . ? N11 C31 H31 123.9 . . ? N12 C31 H31 123.9 . . ? C35 C32 N12 113.1(5) . . ? C35 C32 H32 123.5 . . ? N12 C32 H32 123.5 . . ? C34 C33 C35 122.1(8) . . ? C34 C33 H33 118.9 . . ? C35 C33 H33 118.9 . . ? C33 C34 C46 122.5(8) . . ? C33 C34 H34 118.8 . . ? C46 C34 H34 118.8 . . ? C36 C35 C33 114.9(7) . . ? C36 C35 C32 121.1(6) . . ? C33 C35 C32 123.7(7) . . ? C35 C36 C45 122.4(7) . . ? C35 C36 H36 118.8 . . ? C45 C36 H36 118.8 . . ? C59 C37 C38 138.2(14) . . ? C59 C37 H37 110.9 . . ? C38 C37 H37 110.9 . . ? C39 C38 C43 116.2(8) . . ? C39 C38 C37 116.5(11) . . ? C43 C38 C37 127.3(11) . . ? C40 C39 C38 122.4(9) . . ? C40 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C39 C40 C41 120.8(8) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 119.5(7) . . ? C42 C41 C44 119.5(6) . . ? C40 C41 C44 120.9(6) . . ? C41 C42 C43 118.3(8) . . ? C41 C42 H42 120.8 . . ? C43 C42 H42 120.8 . . ? C38 C43 C42 122.6(9) . . ? C38 C43 H43 118.7 . . ? C42 C43 H43 118.7 . . ? O15 C44 O16 122.1(6) . . ? O15 C44 C41 118.6(6) . . ? O16 C44 C41 119.2(6) . . ? O15 C44 Cd2 60.9(4) . 1_444 ? O16 C44 Cd2 61.8(3) . 1_444 ? C41 C44 Cd2 170.1(5) . 1_444 ? C46 C45 C36 123.2(7) . . ? C46 C45 H45 118.4 . . ? C36 C45 H45 118.4 . . ? C45 C46 C34 114.8(7) . . ? C45 C46 C120 123.2(7) . . ? C34 C46 C120 121.7(7) . . ? O10 C47 O9 122.1(6) . . ? O10 C47 C48 120.9(7) . . ? O9 C47 C48 116.9(7) . . ? O10 C47 Cd4 63.5(4) . . ? O9 C47 Cd4 58.7(3) . . ? C48 C47 Cd4 173.7(5) . . ? C53 C48 C49 118.4(6) . . ? C53 C48 C47 120.4(6) . . ? C49 C48 C47 121.1(6) . . ? C50 C49 C48 120.4(7) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 121.4(7) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C52 C51 C50 117.2(6) . . ? C52 C51 C54 119.0(7) . . ? C50 C51 C54 123.7(7) . . ? C53 C52 C51 122.0(7) . . ? C53 C52 H52 119.0 . . ? C51 C52 H52 119.0 . . ? C52 C53 C48 120.5(7) . . ? C52 C53 H53 119.8 . . ? C48 C53 H53 119.8 . . ? C54 C54 C51 126.9(10) 3_665 . ? C54 C54 H54 116.6 3_665 . ? C51 C54 H54 116.6 . . ? O12 C55 O11 122.2(6) . . ? O12 C55 C56 118.3(6) . . ? O11 C55 C56 119.4(6) . . ? O12 C55 Cd4 60.2(4) . . ? O11 C55 Cd4 62.6(3) . . ? C56 C55 Cd4 169.6(5) . . ? C62 C56 C57 118.4(7) . . ? C62 C56 C55 120.8(6) . . ? C57 C56 C55 120.8(7) . . ? C58 C57 C56 120.9(8) . . ? C58 C57 H57 119.5 . . ? C56 C57 H57 119.5 . . ? C57 C58 C60 122.6(9) . . ? C57 C58 H58 118.7 . . ? C60 C58 H58 118.7 . . ? C37 C59 C60 135.4(14) . . ? C37 C59 H59 112.3 . . ? C60 C59 H59 112.3 . . ? C61 C60 C58 116.5(8) . . ? C61 C60 C59 130.2(12) . . ? C58 C60 C59 113.3(11) . . ? C60 C61 C62 123.0(9) . . ? C60 C61 H61 118.5 . . ? C62 C61 H61 118.5 . . ? C56 C62 C61 118.6(8) . . ? C56 C62 H62 120.7 . . ? C61 C62 H62 120.7 . . ? O1 C63 O2 121.9(7) . . ? O1 C63 C64 120.9(7) . . ? O2 C63 C64 117.2(7) . . ? O1 C63 Cd3 62.2(4) . . ? O2 C63 Cd3 59.7(4) . . ? C64 C63 Cd3 176.9(5) . . ? C65 C64 C70 119.8(7) . . ? C65 C64 C63 121.1(7) . . ? C70 C64 C63 119.1(7) . . ? C64 C65 C67 120.3(8) . . ? C64 C65 H65 119.8 . . ? C67 C65 H65 119.8 . . ? C67 C66 C69 118.7(7) . . ? C67 C66 C68 117.3(7) . . ? C69 C66 C68 123.9(7) . . ? C66 C67 C65 121.0(8) . . ? C66 C67 H67 119.5 . . ? C65 C67 H67 119.5 . . ? C68 C68 C66 126.3(11) 3_657 . ? C68 C68 H68 116.9 3_657 . ? C66 C68 H68 116.9 . . ? C70 C69 C66 120.6(7) . . ? C70 C69 H69 119.7 . . ? C66 C69 H69 119.7 . . ? C64 C70 C69 119.6(7) . . ? C64 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? O4 C71 O3 123.2(6) . . ? O4 C71 C72 119.8(6) . . ? O3 C71 C72 117.0(6) . . ? O4 C71 Cd3 65.2(4) . . ? O3 C71 Cd3 58.6(3) . . ? C72 C71 Cd3 168.4(5) . . ? C77 C72 C73 117.6(7) . . ? C77 C72 C71 120.3(6) . . ? C73 C72 C71 121.8(6) . . ? C74 C73 C72 121.5(7) . . ? C74 C73 H73 119.2 . . ? C72 C73 H73 119.2 . . ? C73 C74 C75 121.2(7) . . ? C73 C74 H74 119.4 . . ? C75 C74 H74 119.4 . . ? C74 C75 C76 117.6(7) . . ? C74 C75 C78 123.0(6) . . ? C76 C75 C78 119.5(6) . . ? C77 C76 C75 121.2(6) . . ? C77 C76 H76 119.4 . . ? C75 C76 H76 119.4 . . ? C76 C77 C72 120.9(6) . . ? C76 C77 H77 119.6 . . ? C72 C77 H77 119.6 . . ? C79 C78 C75 129.5(7) . . ? C79 C78 H78 115.2 . . ? C75 C78 H78 115.2 . . ? C78 C79 C80 128.6(7) . . ? C78 C79 H79 115.7 . . ? C80 C79 H79 115.7 . . ? C81 C80 C85 116.2(7) . . ? C81 C80 C79 119.4(6) . . ? C85 C80 C79 124.3(6) . . ? C83 C81 C80 122.7(6) . . ? C83 C81 H81 118.6 . . ? C80 C81 H81 118.6 . . ? C83 C82 C84 118.7(7) . . ? C83 C82 C86 120.8(6) . . ? C84 C82 C86 120.5(6) . . ? C81 C83 C82 120.1(6) . . ? C81 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C82 C84 C85 120.3(7) . . ? C82 C84 H84 119.9 . . ? C85 C84 H84 119.9 . . ? C84 C85 C80 121.9(7) . . ? C84 C85 H85 119.0 . . ? C80 C85 H85 119.0 . . ? O6 C86 O5 122.2(6) . . ? O6 C86 C82 120.1(6) . . ? O5 C86 C82 117.5(6) . . ? O6 C86 Cd1 64.0(4) . . ? O5 C86 Cd1 58.9(3) . . ? C82 C86 Cd1 166.9(5) . . ? O7 C87 O8 121.4(6) . . ? O7 C87 C88 120.5(7) . . ? O8 C87 C88 118.1(6) . . ? O7 C87 Cd1 64.2(4) . . ? O8 C87 Cd1 57.3(3) . . ? C88 C87 Cd1 174.1(5) . . ? C89 C88 C93 119.0(6) . . ? C89 C88 C87 122.1(6) . . ? C93 C88 C87 118.8(7) . . ? C90 C89 C88 121.5(7) . . ? C90 C89 H89 119.3 . . ? C88 C89 H89 119.3 . . ? C89 C90 C91 119.8(7) . . ? C89 C90 H90 120.1 . . ? C91 C90 H90 120.1 . . ? C92 C91 C90 118.9(7) . . ? C92 C91 C94 118.8(7) . . ? C90 C91 C94 122.3(7) . . ? C91 C92 C93 121.2(7) . . ? C91 C92 H92 119.4 . . ? C93 C92 H92 119.4 . . ? C92 C93 C88 119.5(7) . . ? C92 C93 H93 120.2 . . ? C88 C93 H93 120.2 . . ? C95 C94 C91 127.7(8) . . ? C95 C94 H94 116.2 . . ? C91 C94 H94 116.2 . . ? C94 C95 C96 126.9(8) . . ? C94 C95 H95 116.5 . . ? C96 C95 H95 116.5 . . ? C97 C96 C101 117.8(7) . . ? C97 C96 C95 119.0(7) . . ? C101 C96 C95 123.1(7) . . ? C96 C97 C98 121.2(7) . . ? C96 C97 H97 119.4 . . ? C98 C97 H97 119.4 . . ? C97 C98 C99 120.1(7) . . ? C97 C98 H98 120.0 . . ? C99 C98 H98 120.0 . . ? C100 C99 C98 119.6(6) . . ? C100 C99 C102 121.6(6) . . ? C98 C99 C102 118.8(7) . . ? C99 C100 C101 119.8(7) . . ? C99 C100 H100 120.1 . . ? C101 C100 H100 120.1 . . ? C100 C101 C96 121.5(7) . . ? C100 C101 H101 119.2 . . ? C96 C101 H101 119.2 . . ? O14 C102 O13 122.8(7) . . ? O14 C102 C99 118.1(7) . . ? O13 C102 C99 119.0(7) . . ? O14 C102 Cd2 60.6(4) . . ? O13 C102 Cd2 62.2(4) . . ? C99 C102 Cd2 177.5(5) . . ? C121 C103 N14 105.3(7) . . ? C121 C103 H103 127.4 . . ? N14 C103 H103 127.4 . . ? N14 C104 N13 111.8(6) . . ? N14 C104 H104 124.1 . . ? N13 C104 H104 124.1 . . ? N14 C105 C106 113.2(5) . . ? N14 C105 H105 123.4 . . ? C106 C105 H105 123.4 . . ? C107 C106 C116 117.9(7) . . ? C107 C106 C105 118.8(6) . . ? C116 C106 C105 123.2(7) . . ? C108 C107 C106 120.7(6) . . ? C108 C107 H107 119.7 . . ? C106 C107 H107 119.7 . . ? C109 C108 C107 121.6(7) . . ? C109 C108 H108 119.2 . . ? C107 C108 H108 119.2 . . ? C108 C109 C115 116.7(7) . . ? C108 C109 C114 120.9(6) . . ? C115 C109 C114 122.2(7) . . ? N15 C111 N16 112.1(7) . . ? N15 C111 H111 124.0 . . ? N16 C111 H111 124.0 . . ? C113 C112 N16 106.4(7) . . ? C113 C112 H112 126.8 . . ? N16 C112 H112 126.8 . . ? C112 C113 N15 109.4(8) . . ? C112 C113 H113 125.3 . . ? N15 C113 H113 125.3 . . ? N16 C114 C109 114.0(6) . . ? N16 C114 H114 123.0 . . ? C109 C114 H114 123.0 . . ? C116 C115 C109 122.5(7) . . ? C116 C115 H115 118.8 . . ? C109 C115 H115 118.8 . . ? C115 C116 C106 120.6(7) . . ? C115 C116 H116 119.7 . . ? C106 C116 H116 119.7 . . ? C118 C117 N10 109.6(7) . . ? C118 C117 H117 125.2 . . ? N10 C117 H117 125.2 . . ? C117 C118 N9 106.3(7) . . ? C117 C118 H118 126.9 . . ? N9 C118 H118 126.9 . . ? N10 C119 N9 112.5(6) . . ? N10 C119 H119 123.7 . . ? N9 C119 H119 123.7 . . ? C46 C120 N9 113.8(6) . . ? C46 C120 H120 123.1 . . ? N9 C120 H120 123.1 . . ? C103 C121 N13 110.2(6) . . ? C103 C121 H121 124.9 . . ? N13 C121 H121 124.9 . . ? C11 N1 C10 106.2(5) . . ? C11 N1 Cd4 129.5(5) . . ? C10 N1 Cd4 122.7(4) . . ? C1 N2 C2 106.5(6) . . ? C1 N2 Cd3 126.0(5) . . ? C2 N2 Cd3 127.4(5) . . ? C1 N3 C7 107.5(6) . . ? C1 N3 C3 125.6(7) . . ? C7 N3 C3 126.9(6) . . ? C11 N4 C9 106.6(6) . . ? C11 N4 C12 125.8(6) . . ? C9 N4 C12 127.5(6) . . ? C17 N5 C15 105.6(6) . . ? C17 N5 Cd3 130.1(5) . . ? C15 N5 Cd3 122.0(4) . . ? C17 N6 C16 107.3(6) . . ? C17 N6 C18 125.8(6) . . ? C16 N6 C18 126.9(6) . . ? C26 N7 C27 106.4(6) . . ? C26 N7 C25 126.2(7) . . ? C27 N7 C25 127.4(7) . . ? C26 N8 C28 106.4(6) . . ? C26 N8 Cd4 127.8(5) . . ? C28 N8 Cd4 125.7(5) . . ? C119 N9 C118 106.4(6) . . ? C119 N9 C120 126.5(7) . . ? C118 N9 C120 127.1(6) . . ? C119 N10 C117 105.1(6) . . ? C119 N10 Cd1 127.4(5) . 3_768 ? C117 N10 Cd1 127.5(5) . 3_768 ? C31 N11 C29 104.7(6) . . ? C31 N11 Cd1 130.3(5) . . ? C29 N11 Cd1 122.7(4) . . ? C31 N12 C30 106.8(5) . . ? C31 N12 C32 127.0(6) . . ? C30 N12 C32 126.2(6) . . ? C104 N13 C121 104.8(6) . . ? C104 N13 Cd2 131.3(5) . 3_776 ? C121 N13 Cd2 122.4(4) . 3_776 ? C104 N14 C103 108.0(6) . . ? C104 N14 C105 126.3(6) . . ? C103 N14 C105 125.7(6) . . ? C111 N15 C113 105.4(6) . . ? C111 N15 Cd2 129.7(5) . . ? C113 N15 Cd2 124.9(5) . . ? C111 N16 C112 106.6(7) . . ? C111 N16 C114 126.1(8) . . ? C112 N16 C114 127.2(7) . . ? C63 O1 Cd3 90.4(4) . . ? C63 O2 Cd3 92.5(5) . . ? C71 O3 Cd3 93.5(4) . . ? C71 O4 Cd3 87.4(4) . . ? C86 O5 Cd1 93.1(4) . . ? C86 O6 Cd1 88.1(4) . . ? C87 O7 Cd1 88.5(4) . . ? C87 O8 Cd1 95.3(4) . . ? C47 O9 Cd4 93.8(4) . . ? C47 O10 Cd4 89.1(4) . . ? C55 O11 Cd4 89.5(4) . . ? C55 O12 Cd4 92.0(4) . . ? C102 O13 Cd2 90.0(4) . . ? C102 O14 Cd2 91.6(5) . . ? C44 O15 Cd2 91.6(4) . 1_444 ? C44 O16 Cd2 90.1(4) . 1_444 ? N10 Cd1 N11 102.6(2) 3_768 . ? N10 Cd1 O5 92.77(18) 3_768 . ? N11 Cd1 O5 126.90(17) . . ? N10 Cd1 O8 99.0(2) 3_768 . ? N11 Cd1 O8 86.06(18) . . ? O5 Cd1 O8 141.49(17) . . ? N10 Cd1 O6 144.74(19) 3_768 . ? N11 Cd1 O6 87.65(18) . . ? O5 Cd1 O6 55.71(15) . . ? O8 Cd1 O6 115.42(18) . . ? N10 Cd1 O7 105.05(18) 3_768 . ? N11 Cd1 O7 134.57(18) . . ? O5 Cd1 O7 86.93(16) . . ? O8 Cd1 O7 54.64(17) . . ? O6 Cd1 O7 89.94(16) . . ? N10 Cd1 C86 120.1(2) 3_768 . ? N11 Cd1 C86 110.1(2) . . ? O5 Cd1 C86 28.01(16) . . ? O8 Cd1 C86 131.1(2) . . ? O6 Cd1 C86 27.89(16) . . ? O7 Cd1 C86 85.79(18) . . ? N10 Cd1 C87 104.24(19) 3_768 . ? N11 Cd1 C87 110.6(2) . . ? O5 Cd1 C87 114.11(19) . . ? O8 Cd1 C87 27.40(18) . . ? O6 Cd1 C87 103.32(18) . . ? O7 Cd1 C87 27.25(17) . . ? C86 Cd1 C87 108.8(2) . . ? N15 Cd2 N13 103.4(2) . 3_776 ? N15 Cd2 O14 96.5(2) . . ? N13 Cd2 O14 82.45(19) 3_776 . ? N15 Cd2 O15 143.2(2) . 1_666 ? N13 Cd2 O15 85.76(18) 3_776 1_666 ? O14 Cd2 O15 120.2(2) . 1_666 ? N15 Cd2 O16 93.33(19) . 1_666 ? N13 Cd2 O16 128.21(18) 3_776 1_666 ? O14 Cd2 O16 144.32(18) . 1_666 ? O15 Cd2 O16 55.47(15) 1_666 1_666 ? N15 Cd2 O13 103.93(18) . . ? N13 Cd2 O13 131.74(19) 3_776 . ? O14 Cd2 O13 55.55(17) . . ? O15 Cd2 O13 95.23(17) 1_666 . ? O16 Cd2 O13 88.80(17) 1_666 . ? N15 Cd2 C102 101.8(2) . . ? N13 Cd2 C102 107.4(2) 3_776 . ? O14 Cd2 C102 27.7(2) . . ? O15 Cd2 C102 109.4(2) 1_666 . ? O16 Cd2 C102 116.6(2) 1_666 . ? O13 Cd2 C102 27.83(19) . . ? N15 Cd2 C44 120.1(2) . 1_666 ? N13 Cd2 C44 109.1(2) 3_776 1_666 ? O14 Cd2 C44 135.9(2) . 1_666 ? O15 Cd2 C44 27.54(17) 1_666 1_666 ? O16 Cd2 C44 28.09(16) 1_666 1_666 ? O13 Cd2 C44 90.14(18) . 1_666 ? C102 Cd2 C44 113.9(2) . 1_666 ? N2 Cd3 N5 101.5(2) . . ? N2 Cd3 O3 94.07(19) . . ? N5 Cd3 O3 126.07(18) . . ? N2 Cd3 O2 99.4(2) . . ? N5 Cd3 O2 83.5(2) . . ? O3 Cd3 O2 144.16(18) . . ? N2 Cd3 O1 104.61(18) . . ? N5 Cd3 O1 133.84(19) . . ? O3 Cd3 O1 89.29(16) . . ? O2 Cd3 O1 55.23(17) . . ? N2 Cd3 O4 144.54(19) . . ? N5 Cd3 O4 86.80(18) . . ? O3 Cd3 O4 55.10(15) . . ? O2 Cd3 O4 115.8(2) . . ? O1 Cd3 O4 93.13(16) . . ? N2 Cd3 C71 121.1(2) . . ? N5 Cd3 C71 108.9(2) . . ? O3 Cd3 C71 27.90(16) . . ? O2 Cd3 C71 132.6(2) . . ? O1 Cd3 C71 89.03(18) . . ? O4 Cd3 C71 27.38(16) . . ? N2 Cd3 C63 103.2(2) . . ? N5 Cd3 C63 109.4(2) . . ? O3 Cd3 C63 116.7(2) . . ? O2 Cd3 C63 27.8(2) . . ? O1 Cd3 C63 27.48(18) . . ? O4 Cd3 C63 106.3(2) . . ? C71 Cd3 C63 112.0(2) . . ? N8 Cd4 N1 103.9(2) . . ? N8 Cd4 O9 97.05(19) . . ? N1 Cd4 O9 84.79(18) . . ? N8 Cd4 O12 143.06(19) . . ? N1 Cd4 O12 87.32(17) . . ? O9 Cd4 O12 119.19(18) . . ? N8 Cd4 O11 92.25(18) . . ? N1 Cd4 O11 129.30(17) . . ? O9 Cd4 O11 141.07(17) . . ? O12 Cd4 O11 55.52(15) . . ? N8 Cd4 O10 104.42(18) . . ? N1 Cd4 O10 132.86(18) . . ? O9 Cd4 O10 54.98(16) . . ? O12 Cd4 O10 91.96(16) . . ? O11 Cd4 O10 86.10(16) . . ? N8 Cd4 C55 119.1(2) . . ? N1 Cd4 C55 110.71(19) . . ? O9 Cd4 C55 133.68(19) . . ? O12 Cd4 C55 27.80(16) . . ? O11 Cd4 C55 27.87(16) . . ? O10 Cd4 C55 86.74(18) . . ? N8 Cd4 C47 102.82(19) . . ? N1 Cd4 C47 109.1(2) . . ? O9 Cd4 C47 27.55(18) . . ? O12 Cd4 C47 106.45(19) . . ? O11 Cd4 C47 113.5(2) . . ? O10 Cd4 C47 27.44(18) . . ? C55 Cd4 C47 110.5(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.419 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.124 #===END