# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dfli@mail.ccnu.edu.cn _publ_contact_author_name 'Dongfeng Li' loop_ _publ_author_name 'Feng Wang' 'Xiaohuan Ke' 'Jinbo Zhao' 'Kejian Deng' 'Xiaoke Leng' 'Zhengfang Tian' 'Lili Wen' 'Dongfeng Li' data_1 _database_code_depnum_ccdc_archive 'CCDC 828134' #TrackingRef '- new-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H32 Cu N4 O10' _chemical_formula_weight 864.30 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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 26.9695(15) _cell_length_b 14.7086(8) _cell_length_c 9.9706(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.0810(10) _cell_angle_gamma 90.00 _cell_volume 3915.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description purple _exptl_crystal_colour block _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.888 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40329 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 0.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7685 _reflns_number_gt 3956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _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^)+(0.0511P)^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 7685 _refine_ls_number_parameters 561 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.865 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.5000 1.5000 0.04887(17) Uani 1 2 d S . . Cu2 Cu 0.5000 0.5000 1.0000 0.05282(17) Uani 1 2 d S . . C1 C 0.04429(11) 0.4823(2) 1.2719(4) 0.0556(9) Uani 1 1 d . . . C2 C 0.08486(10) 0.4970(2) 1.1851(3) 0.0496(8) Uani 1 1 d . . . C3 C 0.12879(10) 0.5418(2) 1.2367(3) 0.0547(8) Uani 1 1 d . . . H3 H 0.1323 0.5656 1.3240 0.066 Uiso 1 1 calc R . . C4 C 0.16719(10) 0.5515(2) 1.1605(3) 0.0597(9) Uani 1 1 d . . . H4 H 0.1965 0.5816 1.1956 0.072 Uiso 1 1 calc R . . C5 C 0.16180(10) 0.5162(2) 1.0327(3) 0.0563(9) Uani 1 1 d . . . C6 C 0.11839(10) 0.4735(2) 0.9773(3) 0.0658(10) Uani 1 1 d . . . H6 H 0.1150 0.4508 0.8895 0.079 Uiso 1 1 calc R . . C7 C 0.07973(11) 0.4649(2) 1.0548(4) 0.0645(9) Uani 1 1 d . . . H7 H 0.0500 0.4371 1.0178 0.077 Uiso 1 1 calc R . . C8 C 0.24843(10) 0.5161(2) 1.0000(3) 0.0543(9) Uani 1 1 d . . . C9 C 0.26517(10) 0.4569(2) 1.1028(3) 0.0668(10) Uani 1 1 d . . . H9 H 0.2424 0.4241 1.1456 0.080 Uiso 1 1 calc R . . C10 C 0.31599(10) 0.4460(2) 1.1426(3) 0.0629(9) Uani 1 1 d . . . H10 H 0.3272 0.4063 1.2130 0.075 Uiso 1 1 calc R . . C11 C 0.35006(10) 0.4931(2) 1.0796(3) 0.0474(8) Uani 1 1 d . . . C12 C 0.40521(10) 0.4786(2) 1.1193(3) 0.0528(8) Uani 1 1 d . . . C13 C 0.33272(10) 0.5515(2) 0.9769(3) 0.0542(8) Uani 1 1 d . . . H13 H 0.3556 0.5832 0.9330 0.065 Uiso 1 1 calc R . . C14 C 0.28195(10) 0.5648(2) 0.9364(3) 0.0571(9) Uani 1 1 d . . . H14 H 0.2708 0.6058 0.8677 0.068 Uiso 1 1 calc R . . C15 C 0.43103(10) 0.4161(2) 0.7843(3) 0.0509(8) Uani 1 1 d . . . H15 H 0.4047 0.4494 0.8106 0.061 Uiso 1 1 calc R . . C16 C 0.50280(12) 0.3603(2) 0.7775(4) 0.0762(11) Uani 1 1 d . . . H16 H 0.5367 0.3475 0.7992 0.091 Uiso 1 1 calc R . . C17 C 0.47279(12) 0.3251(2) 0.6713(4) 0.0792(11) Uani 1 1 d . . . H17 H 0.4818 0.2842 0.6076 0.095 Uiso 1 1 calc R . . C18 C 0.38136(11) 0.3423(2) 0.5889(3) 0.0496(8) Uani 1 1 d . . . C19 C 0.37639(13) 0.2654(2) 0.5128(4) 0.0865(12) Uani 1 1 d . . . H19 H 0.4035 0.2263 0.5128 0.104 Uiso 1 1 calc R . . C20 C 0.33116(13) 0.2453(2) 0.4354(4) 0.0838(12) Uani 1 1 d . . . H20 H 0.3287 0.1932 0.3821 0.101 Uiso 1 1 calc R . . C21 C 0.28964(11) 0.2996(2) 0.4343(3) 0.0508(8) Uani 1 1 d . A . C22 C 0.29682(12) 0.3787(2) 0.5076(4) 0.0733(10) Uani 1 1 d . . . H22 H 0.2702 0.4191 0.5061 0.088 Uiso 1 1 calc R . . C23 C 0.34188(12) 0.4003(2) 0.5830(3) 0.0708(10) Uani 1 1 d . . . H23 H 0.3454 0.4549 0.6303 0.085 Uiso 1 1 calc R . . C24 C 0.23989(12) 0.2740(2) 0.3632(3) 0.0527(8) Uani 1 1 d GD . . C25 C 0.23291(17) 0.1860(4) 0.3136(6) 0.0707(16) Uani 0.707(3) 1 d PGD A 1 H25A H 0.2598 0.1461 0.3177 0.085 Uiso 0.707(3) 1 calc PR A 1 C26 C 0.18502(17) 0.1582(4) 0.2576(5) 0.0764(17) Uani 0.707(3) 1 d PD A 1 H26A H 0.1798 0.0987 0.2271 0.092 Uiso 0.707(3) 1 calc PR A 1 C27 C 0.14336(11) 0.2213(2) 0.2466(3) 0.0587(9) Uani 1 1 d D . . C28 C 0.15377(19) 0.3065(3) 0.2927(6) 0.0733(17) Uani 0.707(3) 1 d PD A 1 H28A H 0.1280 0.3490 0.2862 0.088 Uiso 0.707(3) 1 calc PR A 1 C29 C 0.20118(19) 0.3328(3) 0.3492(5) 0.0722(16) Uani 0.707(3) 1 d PD A 1 H29A H 0.2066 0.3925 0.3783 0.087 Uiso 0.707(3) 1 calc PR A 1 C25' C 0.2276(4) 0.2375(7) 0.2377(11) 0.0707(16) Uani 0.293(3) 1 d PD A 2 H25B H 0.2540 0.2260 0.1894 0.085 Uiso 0.293(3) 1 calc PR A 2 C26' C 0.1805(4) 0.2157(8) 0.1742(14) 0.0764(17) Uani 0.293(3) 1 d PD A 2 H26B H 0.1750 0.1977 0.0839 0.092 Uiso 0.293(3) 1 calc PR A 2 C28' C 0.1481(5) 0.2671(8) 0.3641(12) 0.0733(17) Uani 0.293(3) 1 d PD A 2 H28B H 0.1203 0.2820 0.4054 0.088 Uiso 0.293(3) 1 calc PR A 2 C29' C 0.1961(4) 0.2910(8) 0.4210(14) 0.0722(16) Uani 0.293(3) 1 d PD A 2 H29B H 0.1997 0.3208 0.5041 0.087 Uiso 0.293(3) 1 calc PR A 2 C30 C 0.08122(6) 0.12171(11) 0.11122(17) 0.0538(8) Uani 1 1 d . . . H30 H 0.1042 0.0875 0.0713 0.065 Uiso 1 1 calc R A . N4 N 0.03281(6) 0.10713(11) 0.09258(17) 0.0542(7) Uani 1 1 d R . . C32 C 0.04937(6) 0.22415(11) 0.23289(17) 0.0821(12) Uani 1 1 d R . . H32 H 0.0457 0.2724 0.2910 0.099 Uiso 1 1 d R . . C33 C 0.54041(11) 0.3737(2) 0.2837(4) 0.0553(8) Uani 1 1 d . . . C34 C 0.58976(10) 0.3562(2) 0.3676(3) 0.0470(8) Uani 1 1 d . . . C35 C 0.60188(11) 0.3872(2) 0.4978(3) 0.0571(8) Uani 1 1 d . . . H35 H 0.5779 0.4176 0.5394 0.069 Uiso 1 1 calc R . . C36 C 0.64938(11) 0.3739(2) 0.5683(3) 0.0572(8) Uani 1 1 d . . . H36 H 0.6574 0.3953 0.6565 0.069 Uiso 1 1 calc R . . C37 C 0.68456(10) 0.3286(2) 0.5066(3) 0.0499(8) Uani 1 1 d . . . C38 C 0.67284(11) 0.2950(2) 0.3774(3) 0.0579(9) Uani 1 1 d . . . H38 H 0.6965 0.2626 0.3374 0.069 Uiso 1 1 calc R . . C39 C 0.62558(11) 0.3098(2) 0.3076(3) 0.0537(8) Uani 1 1 d . . . H39 H 0.6177 0.2883 0.2194 0.064 Uiso 1 1 calc R . . C40 C 0.77407(10) 0.3193(2) 0.5228(3) 0.0513(8) Uani 1 1 d . . . C41 C 0.81127(11) 0.2582(2) 0.5635(3) 0.0585(9) Uani 1 1 d . . . H41 H 0.8066 0.2136 0.6266 0.070 Uiso 1 1 calc R . . C42 C 0.85606(11) 0.2630(2) 0.5101(3) 0.0567(8) Uani 1 1 d . . . H42 H 0.8812 0.2208 0.5367 0.068 Uiso 1 1 calc R . . C43 C 0.91223(11) 0.3336(3) 0.3633(3) 0.0569(9) Uani 1 1 d . . . C44 C 0.86373(10) 0.3294(2) 0.4186(3) 0.0469(7) Uani 1 1 d . . . C45 C 0.82534(10) 0.3919(2) 0.3792(3) 0.0521(8) Uani 1 1 d . . . H45 H 0.8300 0.4374 0.3175 0.062 Uiso 1 1 calc R . . C46 C 0.78074(10) 0.3865(2) 0.4310(3) 0.0539(8) Uani 1 1 d . . . H46 H 0.7553 0.4280 0.4042 0.065 Uiso 1 1 calc R . . N1 N 0.47667(8) 0.41728(17) 0.8487(2) 0.0521(7) Uani 1 1 d . . . N2 N 0.42650(9) 0.36137(16) 0.6757(3) 0.0517(6) Uani 1 1 d . . . N3 N 0.09371(9) 0.19250(17) 0.1954(3) 0.0605(7) Uani 1 1 d . A . C31 C 0.01285(12) 0.1719(2) 0.1697(4) 0.0734(10) Uani 1 1 d . A . H31 H -0.0210 0.1782 0.1767 0.088 Uiso 1 1 calc R . . O1 O 0.00482(8) 0.44356(16) 1.2206(2) 0.0781(7) Uani 1 1 d . . . O2 O 0.05372(7) 0.50993(15) 1.3932(2) 0.0625(6) Uani 1 1 d . . . O3 O 0.43161(7) 0.51012(15) 1.0357(2) 0.0650(6) Uani 1 1 d . . . O4 O 0.42014(8) 0.4375(2) 1.2244(3) 0.0936(9) Uani 1 1 d . . . O5 O 0.53246(8) 0.36120(15) 0.1633(2) 0.0648(6) Uani 1 1 d . . . O6 O 0.50706(8) 0.40606(16) 0.3561(2) 0.0814(7) Uani 1 1 d . . . H6A H 0.4805 0.4148 0.3067 0.122 Uiso 1 1 calc R . . O7 O 0.91783(7) 0.40788(17) 0.2952(2) 0.0795(7) Uani 1 1 d . . . H7A H 0.9450 0.4066 0.2670 0.119 Uiso 1 1 calc R . . O8 O 0.94326(9) 0.27486(18) 0.3800(3) 0.0941(9) Uani 1 1 d . . . O9 O 0.19830(7) 0.52700(16) 0.9477(2) 0.0706(7) Uani 1 1 d . . . O10 O 0.73093(7) 0.31381(15) 0.5845(2) 0.0664(6) 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 Cu1 0.0268(3) 0.0713(4) 0.0501(3) 0.0152(3) 0.0110(2) 0.0070(3) Cu2 0.0220(2) 0.0859(4) 0.0519(3) -0.0124(3) 0.0097(2) -0.0095(3) C1 0.0349(18) 0.063(2) 0.074(3) 0.0206(19) 0.0243(17) 0.0144(16) C2 0.0288(15) 0.062(2) 0.061(2) 0.0104(17) 0.0164(14) 0.0059(15) C3 0.0356(17) 0.069(2) 0.062(2) 0.0046(17) 0.0169(15) 0.0009(15) C4 0.0319(17) 0.084(2) 0.065(2) 0.000(2) 0.0132(16) -0.0077(16) C5 0.0264(16) 0.084(3) 0.061(2) 0.0181(19) 0.0145(15) 0.0024(16) C6 0.0361(18) 0.110(3) 0.054(2) -0.0012(19) 0.0147(15) -0.0018(18) C7 0.0305(16) 0.091(3) 0.073(2) 0.003(2) 0.0131(16) -0.0107(16) C8 0.0247(15) 0.088(3) 0.0523(19) 0.0103(18) 0.0134(13) 0.0055(16) C9 0.0323(17) 0.096(3) 0.076(2) 0.031(2) 0.0209(16) -0.0050(17) C10 0.0342(17) 0.093(3) 0.064(2) 0.025(2) 0.0170(16) 0.0081(17) C11 0.0291(14) 0.068(2) 0.0461(18) 0.0050(17) 0.0103(13) -0.0011(15) C12 0.0300(16) 0.074(2) 0.055(2) -0.0084(18) 0.0102(16) -0.0019(15) C13 0.0307(16) 0.072(2) 0.064(2) 0.0036(19) 0.0216(15) -0.0081(16) C14 0.0364(17) 0.079(2) 0.060(2) 0.0195(18) 0.0205(15) 0.0043(16) C15 0.0370(18) 0.064(2) 0.052(2) -0.0068(17) 0.0096(15) -0.0031(15) C16 0.044(2) 0.078(3) 0.103(3) -0.029(2) -0.004(2) 0.0133(19) C17 0.051(2) 0.083(3) 0.101(3) -0.038(2) 0.000(2) 0.0140(19) C18 0.052(2) 0.047(2) 0.0480(19) -0.0065(16) 0.0010(15) -0.0055(16) C19 0.061(2) 0.076(3) 0.114(3) -0.037(2) -0.019(2) 0.009(2) C20 0.076(3) 0.071(3) 0.098(3) -0.044(2) -0.010(2) 0.001(2) C21 0.058(2) 0.047(2) 0.0443(19) -0.0025(16) -0.0014(16) -0.0126(17) C22 0.062(2) 0.058(2) 0.093(3) -0.017(2) -0.015(2) 0.0067(18) C23 0.065(2) 0.057(2) 0.082(3) -0.0274(19) -0.0193(19) -0.0035(19) C24 0.058(2) 0.050(2) 0.049(2) -0.0020(16) 0.0026(16) -0.0126(17) C25 0.047(2) 0.063(4) 0.100(5) -0.025(3) -0.001(3) -0.002(3) C26 0.054(3) 0.061(4) 0.113(5) -0.045(3) 0.007(3) -0.010(3) C27 0.051(2) 0.059(2) 0.064(2) -0.0117(18) -0.0008(17) -0.0125(18) C28 0.070(3) 0.044(4) 0.095(5) -0.003(3) -0.028(3) 0.007(3) C29 0.074(3) 0.042(4) 0.089(5) -0.005(3) -0.031(3) -0.010(3) C25' 0.047(2) 0.063(4) 0.100(5) -0.025(3) -0.001(3) -0.002(3) C26' 0.054(3) 0.061(4) 0.113(5) -0.045(3) 0.007(3) -0.010(3) C28' 0.070(3) 0.044(4) 0.095(5) -0.003(3) -0.028(3) 0.007(3) C29' 0.074(3) 0.042(4) 0.089(5) -0.005(3) -0.031(3) -0.010(3) C30 0.0419(18) 0.061(2) 0.060(2) -0.0120(18) 0.0126(16) -0.0069(16) N4 0.0357(14) 0.0642(18) 0.0646(18) -0.0178(14) 0.0136(12) -0.0068(12) C32 0.062(2) 0.073(3) 0.112(3) -0.045(2) 0.016(2) 0.002(2) C33 0.045(2) 0.056(2) 0.065(2) 0.0090(19) 0.0069(19) -0.0068(16) C34 0.0373(17) 0.053(2) 0.051(2) 0.0036(16) 0.0077(15) -0.0044(15) C35 0.0435(19) 0.071(2) 0.058(2) -0.0008(18) 0.0136(16) 0.0029(16) C36 0.050(2) 0.080(2) 0.0428(19) -0.0007(17) 0.0105(16) -0.0074(17) C37 0.0365(17) 0.067(2) 0.0466(19) 0.0094(17) 0.0077(15) -0.0067(15) C38 0.0427(19) 0.069(2) 0.064(2) -0.0005(18) 0.0136(17) 0.0012(16) C39 0.0454(19) 0.063(2) 0.051(2) -0.0036(16) -0.0003(16) -0.0060(16) C40 0.0347(17) 0.072(2) 0.0464(19) 0.0044(17) 0.0025(14) -0.0089(16) C41 0.0398(18) 0.074(2) 0.060(2) 0.0196(18) -0.0002(16) -0.0105(17) C42 0.0400(18) 0.062(2) 0.066(2) 0.0092(18) 0.0001(16) -0.0010(16) C43 0.0353(18) 0.077(3) 0.058(2) -0.001(2) 0.0039(16) -0.0043(18) C44 0.0358(16) 0.057(2) 0.0477(19) -0.0031(16) 0.0045(14) -0.0082(15) C45 0.0452(18) 0.059(2) 0.052(2) 0.0080(16) 0.0080(15) -0.0061(16) C46 0.0391(17) 0.069(2) 0.054(2) 0.0079(17) 0.0070(15) 0.0040(16) N1 0.0289(13) 0.0681(18) 0.0587(17) -0.0066(14) 0.0039(12) -0.0038(12) N2 0.0426(15) 0.0507(17) 0.0597(17) -0.0104(14) -0.0008(13) -0.0026(12) N3 0.0518(17) 0.0573(18) 0.0718(19) -0.0220(15) 0.0066(14) -0.0087(14) C31 0.048(2) 0.073(3) 0.102(3) -0.027(2) 0.018(2) -0.0016(18) O1 0.0453(14) 0.0990(19) 0.0975(19) -0.0061(15) 0.0363(13) -0.0213(13) O2 0.0344(11) 0.0995(18) 0.0562(15) 0.0223(13) 0.0159(10) 0.0115(11) O3 0.0249(10) 0.1122(19) 0.0608(14) -0.0046(13) 0.0157(10) -0.0073(11) O4 0.0359(13) 0.156(3) 0.0885(19) 0.0438(19) 0.0080(13) 0.0136(15) O5 0.0556(14) 0.0761(17) 0.0594(15) 0.0009(13) -0.0036(12) -0.0044(11) O6 0.0444(13) 0.130(2) 0.0694(16) 0.0120(15) 0.0063(12) 0.0207(14) O7 0.0499(14) 0.0947(19) 0.1011(19) 0.0261(16) 0.0364(13) 0.0012(13) O8 0.0537(15) 0.103(2) 0.132(2) 0.0187(18) 0.0340(15) 0.0169(15) O9 0.0256(11) 0.129(2) 0.0599(14) 0.0245(13) 0.0159(10) 0.0030(11) O10 0.0339(12) 0.1143(19) 0.0517(13) 0.0190(12) 0.0087(10) -0.0040(12) _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 O2 1.9205(19) 3_568 ? Cu1 O2 1.9205(19) . ? Cu1 N4 1.9719(17) 4_567 ? Cu1 N4 1.9719(17) 2_556 ? Cu2 O3 1.9328(18) 3_667 ? Cu2 O3 1.9328(18) . ? Cu2 N1 1.971(2) 3_667 ? Cu2 N1 1.971(2) . ? C1 O1 1.251(4) . ? C1 O2 1.267(4) . ? C1 C2 1.503(4) . ? C2 C7 1.371(4) . ? C2 C3 1.390(4) . ? C3 C4 1.375(4) . ? C3 H3 0.9300 . ? C4 C5 1.365(4) . ? C4 H4 0.9300 . ? C5 C6 1.373(4) . ? C5 O9 1.396(3) . ? C6 C7 1.388(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.373(4) . ? C8 C14 1.376(4) . ? C8 O9 1.388(3) . ? C9 C10 1.382(4) . ? C9 H9 0.9300 . ? C10 C11 1.372(4) . ? C10 H10 0.9300 . ? C11 C13 1.368(4) . ? C11 C12 1.500(4) . ? C12 O4 1.228(3) . ? C12 O3 1.258(3) . ? C13 C14 1.386(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N1 1.306(3) . ? C15 N2 1.340(3) . ? C15 H15 0.9300 . ? C16 C17 1.343(4) . ? C16 N1 1.358(4) . ? C16 H16 0.9300 . ? C17 N2 1.364(4) . ? C17 H17 0.9300 . ? C18 C19 1.358(4) . ? C18 C23 1.359(4) . ? C18 N2 1.419(3) . ? C19 C20 1.381(4) . ? C19 H19 0.9300 . ? C20 C21 1.374(4) . ? C20 H20 0.9300 . ? C21 C22 1.373(4) . ? C21 C24 1.476(4) . ? C22 C23 1.373(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.348(5) . ? C24 C25' 1.359(10) . ? C24 C25 1.389(5) . ? C24 C29' 1.409(11) . ? C25 C26 1.395(5) . ? C25 H25A 0.9300 . ? C26 C27 1.450(5) . ? C26 H26A 0.9300 . ? C27 C26' 1.316(10) . ? C27 C28' 1.341(11) . ? C27 C28 1.350(5) . ? C27 N3 1.429(4) . ? C28 C29 1.378(6) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C25' C26' 1.377(11) . ? C25' H25B 0.9300 . ? C26' H26B 0.9300 . ? C28' C29' 1.384(11) . ? C28' H28B 0.9300 . ? C29' H29B 0.9300 . ? C30 N4 1.3102 . ? C30 N3 1.350(3) . ? C30 H30 0.9300 . ? N4 C31 1.380(3) . ? N4 Cu1 1.9719(17) 2_546 ? C32 C31 1.335(3) . ? C32 N3 1.383(3) . ? C32 H32 0.9300 . ? C33 O5 1.204(3) . ? C33 O6 1.319(4) . ? C33 C34 1.491(4) . ? C34 C35 1.372(4) . ? C34 C39 1.386(4) . ? C35 C36 1.386(4) . ? C35 H35 0.9300 . ? C36 C37 1.374(4) . ? C36 H36 0.9300 . ? C37 C38 1.374(4) . ? C37 O10 1.393(3) . ? C38 C39 1.381(4) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.365(4) . ? C40 C46 1.375(4) . ? C40 O10 1.393(3) . ? C41 C42 1.389(4) . ? C41 H41 0.9300 . ? C42 C44 1.372(4) . ? C42 H42 0.9300 . ? C43 O8 1.198(3) . ? C43 O7 1.306(4) . ? C43 C44 1.490(4) . ? C44 C45 1.398(4) . ? C45 C46 1.376(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C31 H31 0.9300 . ? O6 H6A 0.8200 . ? O7 H7A 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 180.000(1) 3_568 . ? O2 Cu1 N4 90.20(8) 3_568 4_567 ? O2 Cu1 N4 89.80(8) . 4_567 ? O2 Cu1 N4 89.80(8) 3_568 2_556 ? O2 Cu1 N4 90.20(8) . 2_556 ? N4 Cu1 N4 180.0 4_567 2_556 ? O3 Cu2 O3 180.0 3_667 . ? O3 Cu2 N1 88.76(9) 3_667 3_667 ? O3 Cu2 N1 91.24(9) . 3_667 ? O3 Cu2 N1 91.24(9) 3_667 . ? O3 Cu2 N1 88.76(9) . . ? N1 Cu2 N1 180.000(1) 3_667 . ? O1 C1 O2 125.5(3) . . ? O1 C1 C2 118.4(3) . . ? O2 C1 C2 116.0(3) . . ? C7 C2 C3 118.8(3) . . ? C7 C2 C1 120.8(3) . . ? C3 C2 C1 120.4(3) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.1(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.4(3) . . ? C4 C5 O9 122.1(3) . . ? C6 C5 O9 116.2(3) . . ? C5 C6 C7 118.9(3) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C2 C7 C6 120.8(3) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C9 C8 C14 120.4(3) . . ? C9 C8 O9 123.7(3) . . ? C14 C8 O9 115.8(3) . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.7(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C13 C11 C10 118.7(3) . . ? C13 C11 C12 120.6(3) . . ? C10 C11 C12 120.7(3) . . ? O4 C12 O3 126.8(3) . . ? O4 C12 C11 119.3(3) . . ? O3 C12 C11 113.9(3) . . ? C11 C13 C14 121.8(3) . . ? C11 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C8 C14 C13 118.6(3) . . ? C8 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? N1 C15 N2 112.2(3) . . ? N1 C15 H15 123.9 . . ? N2 C15 H15 123.9 . . ? C17 C16 N1 110.6(3) . . ? C17 C16 H16 124.7 . . ? N1 C16 H16 124.7 . . ? C16 C17 N2 106.0(3) . . ? C16 C17 H17 127.0 . . ? N2 C17 H17 127.0 . . ? C19 C18 C23 118.9(3) . . ? C19 C18 N2 120.9(3) . . ? C23 C18 N2 120.2(3) . . ? C18 C19 C20 120.1(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 122.3(3) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C22 C21 C20 115.8(3) . . ? C22 C21 C24 121.5(3) . . ? C20 C21 C24 122.7(3) . . ? C23 C22 C21 122.3(3) . . ? C23 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C18 C23 C22 120.4(3) . . ? C18 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C29 C24 C25' 94.2(6) . . ? C29 C24 C25 119.8(4) . . ? C25' C24 C25 45.7(5) . . ? C29 C24 C29' 41.0(5) . . ? C25' C24 C29' 109.7(8) . . ? C25 C24 C29' 103.4(6) . . ? C29 C24 C21 121.6(3) . . ? C25' C24 C21 129.1(6) . . ? C25 C24 C21 118.5(3) . . ? C29' C24 C21 121.1(6) . . ? C24 C25 C26 119.2(4) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C25 C26 C27 120.4(4) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C26' C27 C28' 121.7(8) . . ? C26' C27 C28 96.2(6) . . ? C28' C27 C28 41.2(5) . . ? C26' C27 N3 122.1(6) . . ? C28' C27 N3 115.5(6) . . ? C28 C27 N3 122.5(3) . . ? C26' C27 C26 50.2(5) . . ? C28' C27 C26 106.2(6) . . ? C28 C27 C26 116.6(4) . . ? N3 C27 C26 120.9(3) . . ? C27 C28 C29 122.4(5) . . ? C27 C28 H28A 118.8 . . ? C29 C28 H28A 118.8 . . ? C24 C29 C28 121.5(4) . . ? C24 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C24 C25' C26' 127.2(11) . . ? C24 C25' H25B 116.4 . . ? C26' C25' H25B 116.4 . . ? C27 C26' C25' 117.2(11) . . ? C27 C26' H26B 121.4 . . ? C25' C26' H26B 121.4 . . ? C27 C28' C29' 117.0(12) . . ? C27 C28' H28B 121.5 . . ? C29' C28' H28B 121.5 . . ? C28' C29' C24 125.2(11) . . ? C28' C29' H29B 117.4 . . ? C24 C29' H29B 117.4 . . ? N4 C30 N3 111.77(12) . . ? N4 C30 H30 124.1 . . ? N3 C30 H30 124.1 . . ? C30 N4 C31 105.49(15) . . ? C30 N4 Cu1 124.74(5) . 2_546 ? C31 N4 Cu1 128.88(16) . 2_546 ? C31 C32 N3 106.69(19) . . ? C31 C32 H32 126.6 . . ? N3 C32 H32 126.7 . . ? O5 C33 O6 124.1(3) . . ? O5 C33 C34 123.6(3) . . ? O6 C33 C34 112.3(3) . . ? C35 C34 C39 119.0(3) . . ? C35 C34 C33 123.3(3) . . ? C39 C34 C33 117.7(3) . . ? C34 C35 C36 120.9(3) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C37 C36 C35 119.3(3) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C37 C38 120.8(3) . . ? C36 C37 O10 116.6(3) . . ? C38 C37 O10 122.5(3) . . ? C37 C38 C39 119.4(3) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C38 C39 C34 120.7(3) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? C41 C40 C46 120.7(3) . . ? C41 C40 O10 117.0(3) . . ? C46 C40 O10 122.1(3) . . ? C40 C41 C42 119.7(3) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C44 C42 C41 120.8(3) . . ? C44 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? O8 C43 O7 123.1(3) . . ? O8 C43 C44 123.4(3) . . ? O7 C43 C44 113.5(3) . . ? C42 C44 C45 118.6(3) . . ? C42 C44 C43 119.9(3) . . ? C45 C44 C43 121.5(3) . . ? C46 C45 C44 120.6(3) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C40 C46 C45 119.6(3) . . ? C40 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C15 N1 C16 104.9(3) . . ? C15 N1 Cu2 124.2(2) . . ? C16 N1 Cu2 130.4(2) . . ? C15 N2 C17 106.3(3) . . ? C15 N2 C18 125.7(3) . . ? C17 N2 C18 127.8(3) . . ? C30 N3 C32 106.15(19) . . ? C30 N3 C27 126.2(2) . . ? C32 N3 C27 127.3(2) . . ? C32 C31 N4 109.9(2) . . ? C32 C31 H31 125.1 . . ? N4 C31 H31 125.1 . . ? C1 O2 Cu1 116.03(19) . . ? C12 O3 Cu2 137.5(2) . . ? C33 O6 H6A 109.5 . . ? C43 O7 H7A 109.5 . . ? C8 O9 C5 119.4(2) . . ? C40 O10 C37 119.0(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.462 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.056 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 828135' #TrackingRef '- new-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H22 Cu N4 O5' _chemical_formula_sum 'C32 H22 Cu N4 O5' _chemical_formula_weight 606.08 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 Orthorhombic _symmetry_space_group_name_H-M 'Pnna ' _symmetry_space_group_name_Hall '-P 2a 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 9.8501(12) _cell_length_b 18.1491(18) _cell_length_c 15.1858(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2714.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1818 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 21.18 _exptl_crystal_description green _exptl_crystal_colour block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7958 _exptl_absorpt_correction_T_max 0.8476 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14167 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2675 _reflns_number_gt 1908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _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. Checkcif output: 432_ALERT_2_G Short Inter X...Y Contact C1 .. C6 .. 3.13 Ang. 432_ALERT_2_G Short Inter X...Y Contact C6 .. C7 .. 2.57 Ang. 432_ALERT_2_G Short Inter X...Y Contact C6 .. C8 .. 3.08 Ang. 432_ALERT_2_G Short Inter X...Y Contact C7 .. C7 .. 1.50 Ang. 432_ALERT_2_G Short Inter X...Y Contact C7 .. C8 .. 2.60 Ang. Due to the high degree of the structural symmetry, only a half of the organic ligands are given during the refinement. In fact, all of these carbon atoms referred in PLAT_432 Alerts belong to a single organic ligand. Platon mistakenly judges the contact between the carbons from the symmetry-related half within a single organic ligand as the inter-molecular contact. ; _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^)+(0.06P)^2^+1.99P] 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 2675 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0648(4) 0.8192(2) 0.1447(2) 0.0495(9) Uani 1 1 d . . . H1 H -0.0612 0.8594 0.1826 0.059 Uiso 1 1 calc R . . C2 C -0.0146(3) 0.7196(2) 0.0802(2) 0.0440(8) Uani 1 1 d . . . H2 H 0.0305 0.6765 0.0643 0.053 Uiso 1 1 calc R . . C3 C -0.1262(4) 0.7471(2) 0.0395(2) 0.0507(9) Uani 1 1 d . . . H3 H -0.1748 0.7251 -0.0060 0.061 Uiso 1 1 d R . . C4 C -0.2648(3) 0.8611(2) 0.0570(2) 0.0424(8) Uani 1 1 d . . . C5 C -0.2753(4) 0.8787(2) -0.0296(2) 0.0441(8) Uani 1 1 d . . . H5 H -0.2209 0.8565 -0.0720 0.053 Uiso 1 1 calc R . . C6 C -0.3709(4) 0.9314(2) -0.0514(2) 0.0458(8) Uani 1 1 d . . . H6 H -0.3825 0.9452 -0.1098 0.055 Uiso 1 1 d R . . C7 C -0.4530(3) 0.9691(2) 0.0124(2) 0.0437(8) Uani 1 1 d . . . C8 C -0.4320(4) 0.9438(2) 0.1012(2) 0.0492(9) Uani 1 1 d . . . H8 H -0.4837 0.9659 0.1450 0.059 Uiso 1 1 d R . . C9 C -0.3355(4) 0.8919(2) 0.1235(2) 0.0482(9) Uani 1 1 d . . . H9 H -0.3198 0.8789 0.1818 0.058 Uiso 1 1 calc R . . C10 C 0.3094(3) 0.64888(18) 0.1973(2) 0.0361(7) Uani 1 1 d . . . C11 C 0.4322(3) 0.60939(19) 0.1646(2) 0.0412(8) Uani 1 1 d . . . C12 C 0.5397(3) 0.6483(2) 0.1285(2) 0.0482(9) Uani 1 1 d . . . H12 H 0.5390 0.6995 0.1297 0.058 Uiso 1 1 calc R . . C13 C 0.6490(4) 0.6111(2) 0.0905(2) 0.0512(9) Uani 1 1 d . . . H13 H 0.7207 0.6372 0.0658 0.061 Uiso 1 1 d R . . C14 C 0.6502(4) 0.5366(2) 0.0906(2) 0.0525(9) Uani 1 1 d . . . C15 C 0.5463(3) 0.4962(2) 0.1284(2) 0.0456(8) Uani 1 1 d . . . H15 H 0.5479 0.4449 0.1273 0.055 Uiso 1 1 calc R . . C16 C 0.4392(4) 0.5336(2) 0.1680(2) 0.0494(9) Uani 1 1 d . . . H16 H 0.3718 0.5073 0.1972 0.059 Uiso 1 1 calc R . . Cu1 Cu 0.14662(5) 0.7500 0.2500 0.03380(18) Uani 1 2 d S . . N1 N 0.0206(3) 0.76412(16) 0.14698(18) 0.0421(7) Uani 1 1 d . . . N2 N -0.1581(2) 0.81058(15) 0.08127(17) 0.0359(6) Uani 1 1 d . . . O1 O 0.2441(2) 0.62303(13) 0.26014(13) 0.0401(5) Uani 1 1 d . . . O2 O 0.2805(2) 0.70738(13) 0.16271(15) 0.0466(6) Uani 1 1 d . . . O3 O 0.7500 0.5000 0.0423(2) 0.0565(10) Uani 1 2 d S . . 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 0.059(2) 0.055(2) 0.0342(17) -0.0159(15) -0.0185(15) 0.0134(18) C2 0.047(2) 0.0451(18) 0.0398(17) -0.0133(15) -0.0132(15) 0.0198(16) C3 0.061(2) 0.056(2) 0.0356(17) -0.0151(15) -0.0181(16) 0.0199(19) C4 0.0308(16) 0.062(2) 0.0340(15) -0.0012(15) -0.0036(12) 0.0076(15) C5 0.047(2) 0.052(2) 0.0335(16) -0.0032(14) -0.0015(14) 0.0030(16) C6 0.050(2) 0.053(2) 0.0343(16) -0.0006(15) -0.0069(14) -0.0011(17) C7 0.0370(18) 0.056(2) 0.0383(16) 0.0086(15) -0.0011(14) 0.0010(15) C8 0.050(2) 0.063(2) 0.0343(16) 0.0103(15) 0.0125(15) 0.0139(18) C9 0.055(2) 0.055(2) 0.0345(16) 0.0136(15) -0.0029(15) 0.0148(17) C10 0.0299(15) 0.0384(17) 0.0401(16) 0.0015(14) 0.0018(13) 0.0020(13) C11 0.0354(17) 0.052(2) 0.0366(16) 0.0005(15) -0.0021(14) 0.0123(14) C12 0.0463(19) 0.049(2) 0.0497(19) 0.0202(16) 0.0241(16) 0.0157(16) C13 0.047(2) 0.055(2) 0.052(2) 0.0169(17) 0.0132(16) 0.0152(17) C14 0.055(2) 0.059(2) 0.0437(19) 0.0061(17) -0.0029(17) 0.0169(19) C15 0.0443(19) 0.0477(19) 0.0448(17) -0.0127(16) -0.0124(15) 0.0116(16) C16 0.060(2) 0.0414(18) 0.0466(18) 0.0004(15) 0.0065(17) 0.0080(16) Cu1 0.0316(3) 0.0427(3) 0.0271(3) 0.0019(2) 0.000 0.000 N1 0.0370(15) 0.0509(17) 0.0383(15) -0.0072(12) -0.0077(12) 0.0098(12) N2 0.0312(14) 0.0428(15) 0.0338(13) -0.0033(11) -0.0022(10) 0.0096(11) O1 0.0407(12) 0.0436(12) 0.0358(11) 0.0030(9) 0.0039(9) 0.0012(10) O2 0.0493(15) 0.0477(14) 0.0427(12) 0.0105(11) 0.0148(11) 0.0152(11) O3 0.060(2) 0.065(2) 0.0445(19) 0.000 0.000 0.028(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 N1 1.306(4) . ? C1 N2 1.341(4) . ? C1 H1 0.9300 . ? C2 N1 1.343(4) . ? C2 C3 1.357(5) . ? C2 H2 0.9300 . ? C3 N2 1.352(4) . ? C3 H3 0.9300 . ? C4 C9 1.347(5) . ? C4 C5 1.357(4) . ? C4 N2 1.443(4) . ? C5 C6 1.382(5) . ? C5 H5 0.9300 . ? C6 C7 1.436(5) . ? C6 H6 0.9300 . ? C7 C8 1.438(4) . ? C7 C7 1.503(7) 5_475 ? C8 C9 1.380(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 O2 1.219(4) . ? C10 O1 1.243(4) . ? C10 C11 1.492(4) . ? C11 C16 1.378(5) . ? C11 C12 1.385(5) . ? C12 C13 1.396(5) . ? C12 H12 0.9300 . ? C13 C14 1.352(6) . ? C13 H13 0.9300 . ? C14 C15 1.384(5) . ? C14 O3 1.395(4) . ? C15 C16 1.392(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? Cu1 N1 2.014(3) . ? Cu1 N1 2.014(3) 4_565 ? Cu1 O2 2.023(2) 4_565 ? Cu1 O2 2.023(2) . ? O3 C14 1.395(4) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 111.8(3) . . ? N1 C1 H1 124.1 . . ? N2 C1 H1 124.1 . . ? N1 C2 C3 109.3(3) . . ? N1 C2 H2 125.3 . . ? C3 C2 H2 125.3 . . ? N2 C3 C2 106.8(3) . . ? N2 C3 H3 126.5 . . ? C2 C3 H3 126.6 . . ? C9 C4 C5 126.0(3) . . ? C9 C4 N2 116.7(3) . . ? C5 C4 N2 116.9(3) . . ? C4 C5 C6 116.6(3) . . ? C4 C5 H5 121.7 . . ? C6 C5 H5 121.7 . . ? C5 C6 C7 123.5(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 116.5 . . ? C6 C7 C8 113.5(3) . . ? C6 C7 C7 122.2(4) . 5_475 ? C8 C7 C7 124.2(4) . 5_475 ? C9 C8 C7 123.1(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 117.0 . . ? C4 C9 C8 117.1(3) . . ? C4 C9 H9 121.5 . . ? C8 C9 H9 121.5 . . ? O2 C10 O1 122.6(3) . . ? O2 C10 C11 117.7(3) . . ? O1 C10 C11 119.6(3) . . ? C16 C11 C12 119.1(3) . . ? C16 C11 C10 120.5(3) . . ? C12 C11 C10 120.4(3) . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 121.6(3) . . ? C13 C14 O3 118.8(3) . . ? C15 C14 O3 119.1(3) . . ? C14 C15 C16 118.8(3) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C11 C16 C15 120.6(4) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? N1 Cu1 N1 103.86(17) . 4_565 ? N1 Cu1 O2 149.56(11) . 4_565 ? N1 Cu1 O2 86.64(11) 4_565 4_565 ? N1 Cu1 O2 86.64(11) . . ? N1 Cu1 O2 149.56(11) 4_565 . ? O2 Cu1 O2 98.67(15) 4_565 . ? C1 N1 C2 106.0(3) . . ? C1 N1 Cu1 120.9(2) . . ? C2 N1 Cu1 132.0(2) . . ? C1 N2 C3 106.1(3) . . ? C1 N2 C4 127.5(3) . . ? C3 N2 C4 126.2(3) . . ? C10 O2 Cu1 101.7(2) . . ? C14 O3 C14 116.5(4) 2_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 1.2(5) . . . . ? C9 C4 C5 C6 -2.4(6) . . . . ? N2 C4 C5 C6 -175.2(3) . . . . ? C4 C5 C6 C7 2.5(6) . . . . ? C5 C6 C7 C8 -3.4(5) . . . . ? C5 C6 C7 C7 174.3(4) . . . 5_475 ? C6 C7 C8 C9 4.3(6) . . . . ? C7 C7 C8 C9 -173.4(4) 5_475 . . . ? C5 C4 C9 C8 3.3(6) . . . . ? N2 C4 C9 C8 176.1(3) . . . . ? C7 C8 C9 C4 -4.3(6) . . . . ? O2 C10 C11 C16 -150.2(3) . . . . ? O1 C10 C11 C16 32.6(5) . . . . ? O2 C10 C11 C12 28.5(5) . . . . ? O1 C10 C11 C12 -148.8(3) . . . . ? C16 C11 C12 C13 4.6(6) . . . . ? C10 C11 C12 C13 -174.1(3) . . . . ? C11 C12 C13 C14 -1.2(6) . . . . ? C12 C13 C14 C15 -0.7(6) . . . . ? C12 C13 C14 O3 171.4(3) . . . . ? C13 C14 C15 C16 -0.9(6) . . . . ? O3 C14 C15 C16 -173.0(3) . . . . ? C12 C11 C16 C15 -6.2(5) . . . . ? C10 C11 C16 C15 172.5(3) . . . . ? C14 C15 C16 C11 4.3(5) . . . . ? N2 C1 N1 C2 2.7(4) . . . . ? N2 C1 N1 Cu1 -166.8(2) . . . . ? C3 C2 N1 C1 -2.4(4) . . . . ? C3 C2 N1 Cu1 165.5(3) . . . . ? N1 Cu1 N1 C1 61.1(3) 4_565 . . . ? O2 Cu1 N1 C1 -46.4(4) 4_565 . . . ? O2 Cu1 N1 C1 -147.9(3) . . . . ? N1 Cu1 N1 C2 -105.4(4) 4_565 . . . ? O2 Cu1 N1 C2 147.1(3) 4_565 . . . ? O2 Cu1 N1 C2 45.7(3) . . . . ? N1 C1 N2 C3 -2.0(4) . . . . ? N1 C1 N2 C4 -177.4(3) . . . . ? C2 C3 N2 C1 0.4(4) . . . . ? C2 C3 N2 C4 175.9(3) . . . . ? C9 C4 N2 C1 -44.5(5) . . . . ? C5 C4 N2 C1 129.1(4) . . . . ? C9 C4 N2 C3 141.0(4) . . . . ? C5 C4 N2 C3 -45.5(5) . . . . ? O1 C10 O2 Cu1 12.4(4) . . . . ? C11 C10 O2 Cu1 -164.7(2) . . . . ? N1 Cu1 O2 C10 -128.0(2) . . . . ? N1 Cu1 O2 C10 -16.1(3) 4_565 . . . ? O2 Cu1 O2 C10 82.1(2) 4_565 . . . ? C13 C14 O3 C14 110.0(4) . . . 2_665 ? C15 C14 O3 C14 -77.7(3) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.284 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.064 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 828136' #TrackingRef '- new-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H44 N8 O10 Zn2' _chemical_formula_weight 1215.86 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 18.167(4) _cell_length_b 26.668(5) _cell_length_c 12.453(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6033(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Colorless _exptl_crystal_colour plate _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8747 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10509 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0946 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10509 _reflns_number_gt 8771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+5.3679P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.038(16) _refine_ls_number_reflns 10509 _refine_ls_number_parameters 745 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.54009(4) 0.26960(3) 0.41939(6) 0.03522(18) Uani 1 1 d . . . Zn2 Zn 0.74351(4) 0.46428(3) 0.11658(6) 0.03567(19) Uani 1 1 d . . . C1 C 2.2588(4) 0.4496(3) 0.9520(6) 0.062(2) Uani 1 1 d . . . H1 H 2.3102 0.4512 0.9391 0.075 Uiso 1 1 calc R . . C2 C 2.2125(4) 0.4147(3) 0.9086(7) 0.064(2) Uani 1 1 d . . . H2 H 2.2251 0.3885 0.8605 0.076 Uiso 1 1 calc R . . C3 C 2.1526(4) 0.4656(3) 1.0138(6) 0.0526(19) Uani 1 1 d . . . H3 H 2.1140 0.4808 1.0536 0.063 Uiso 1 1 calc R . . C4 C 2.0749(4) 0.4017(4) 0.9236(9) 0.0858(19) Uani 1 1 d . . . C5 C 2.0704(4) 0.3573(3) 0.8772(7) 0.061(2) Uani 1 1 d . . . H5 H 2.1138 0.3387 0.8622 0.074 Uiso 1 1 calc R . . C6 C 2.0022(4) 0.3381(3) 0.8505(8) 0.068(3) Uani 1 1 d . . . H6 H 2.0002 0.3057 0.8189 0.082 Uiso 1 1 calc R . . C7 C 1.9381(3) 0.3627(3) 0.8669(5) 0.0443(17) Uani 1 1 d . . . C8 C 1.9446(4) 0.4073(3) 0.9229(9) 0.0858(19) Uani 1 1 d . . . H8 H 1.9014 0.4253 0.9419 0.103 Uiso 1 1 calc R . . C9 C 2.0114(4) 0.4261(4) 0.9513(9) 0.0858(19) Uani 1 1 d . . . H9 H 2.0140 0.4566 0.9908 0.103 Uiso 1 1 calc R . . C10 C 1.8639(4) 0.3460(3) 0.8319(6) 0.0447(18) Uani 1 1 d . . . C11 C 1.8579(4) 0.3081(3) 0.7582(7) 0.057(2) Uani 1 1 d . . . H11 H 1.8999 0.2890 0.7382 0.068 Uiso 1 1 calc R . . C12 C 1.7889(4) 0.2978(3) 0.7124(7) 0.062(2) Uani 1 1 d . . . H12 H 1.7854 0.2726 0.6587 0.074 Uiso 1 1 calc R . . C13 C 1.7280(4) 0.3223(3) 0.7422(6) 0.0479(18) Uani 1 1 d . . . C14 C 1.7337(5) 0.3572(4) 0.8207(8) 0.098(4) Uani 1 1 d . . . H14 H 1.6910 0.3740 0.8461 0.118 Uiso 1 1 calc R . . C15 C 1.8009(4) 0.3683(5) 0.8634(8) 0.099(4) Uani 1 1 d . . . H15 H 1.8034 0.3930 0.9182 0.118 Uiso 1 1 calc R . . C16 C 1.6512(3) 0.2971(2) 0.5866(5) 0.0369(15) Uani 1 1 d . . . H16 H 1.6911 0.2863 0.5430 0.044 Uiso 1 1 calc R . . C17 C 1.5425(5) 0.3167(4) 0.6408(6) 0.088(3) Uani 1 1 d . . . H17 H 1.4906 0.3205 0.6429 0.106 Uiso 1 1 calc R . . C18 C 1.5894(4) 0.3291(4) 0.7200(7) 0.085(3) Uani 1 1 d . . . H18 H 1.5771 0.3452 0.7857 0.102 Uiso 1 1 calc R . . C19 C 1.4022(3) 0.3180(2) 0.4038(6) 0.0392(16) Uani 1 1 d . . . C20 C 1.3326(3) 0.3276(3) 0.3398(5) 0.0368(15) Uani 1 1 d . . . C21 C 1.3348(4) 0.3304(3) 0.2287(5) 0.0421(16) Uani 1 1 d . . . H21 H 1.3806 0.3308 0.1920 0.051 Uiso 1 1 calc R . . C22 C 1.2697(4) 0.3324(3) 0.1719(6) 0.0480(18) Uani 1 1 d . . . H22 H 1.2704 0.3360 0.0961 0.058 Uiso 1 1 calc R . . C23 C 1.2032(4) 0.3293(2) 0.2259(6) 0.0439(18) Uani 1 1 d . . . C24 C 1.2001(4) 0.3277(2) 0.3349(6) 0.0448(18) Uani 1 1 d . . . H24 H 1.1541 0.3266 0.3710 0.054 Uiso 1 1 calc R . . C25 C 1.2656(3) 0.3275(2) 0.3924(6) 0.0401(16) Uani 1 1 d . . . H25 H 1.2644 0.3274 0.4687 0.048 Uiso 1 1 calc R . . C26 C 1.0769(4) 0.3507(3) 0.1867(6) 0.0503(19) Uani 1 1 d . . . C27 C 1.0104(4) 0.3282(3) 0.1563(6) 0.0490(19) Uani 1 1 d . . . H27 H 1.0098 0.2948 0.1296 0.059 Uiso 1 1 calc R . . C28 C 0.9462(4) 0.3548(3) 0.1655(6) 0.0523(19) Uani 1 1 d . . . H28 H 0.9011 0.3399 0.1436 0.063 Uiso 1 1 calc R . . C29 C 0.9460(4) 0.4037(2) 0.2066(6) 0.0450(18) Uani 1 1 d . . . C30 C 1.0119(4) 0.4242(3) 0.2392(6) 0.0428(17) Uani 1 1 d . . . H30 H 1.0122 0.4573 0.2673 0.051 Uiso 1 1 calc R . . C31 C 1.0772(4) 0.3985(3) 0.2324(6) 0.0434(17) Uani 1 1 d . . . H31 H 1.1216 0.4129 0.2583 0.052 Uiso 1 1 calc R . . C32 C 0.8772(4) 0.4357(3) 0.2031(7) 0.0475(19) Uani 1 1 d . . . C33 C 0.6118(4) 0.4317(3) 0.0141(5) 0.0379(15) Uani 1 1 d . . . C34 C 0.5558(3) 0.3903(2) -0.0022(5) 0.0354(15) Uani 1 1 d . . . C35 C 0.5724(4) 0.3413(3) 0.0209(6) 0.0467(18) Uani 1 1 d . . . H35 H 0.6205 0.3331 0.0451 0.056 Uiso 1 1 calc R . . C36 C 0.5205(4) 0.3033(3) 0.0098(5) 0.0453(17) Uani 1 1 d . . . H36 H 0.5326 0.2696 0.0274 0.054 Uiso 1 1 calc R . . C37 C 0.4505(4) 0.3155(3) -0.0276(5) 0.0420(16) Uani 1 1 d . . . C38 C 0.4334(3) 0.3645(2) -0.0520(6) 0.0424(17) Uani 1 1 d . . . H38 H 0.3861 0.3729 -0.0791 0.051 Uiso 1 1 calc R . . C39 C 0.4863(4) 0.4018(3) -0.0364(5) 0.0415(16) Uani 1 1 d . . . H39 H 0.4738 0.4358 -0.0499 0.050 Uiso 1 1 calc R . . C40 C 0.3435(3) 0.2768(2) -0.1030(5) 0.0384(15) Uani 1 1 d . . . C41 C 0.3517(4) 0.2931(3) -0.2055(6) 0.056(2) Uani 1 1 d . . . H41 H 0.3977 0.3063 -0.2284 0.067 Uiso 1 1 calc R . . C42 C 0.2938(4) 0.2905(3) -0.2764(6) 0.0509(19) Uani 1 1 d . . . H42 H 0.2999 0.3027 -0.3475 0.061 Uiso 1 1 calc R . . C43 C 0.2258(3) 0.2702(2) -0.2455(5) 0.0372(15) Uani 1 1 d . . . C44 C 0.2195(4) 0.2534(2) -0.1430(5) 0.0425(17) Uani 1 1 d . . . H44 H 0.1738 0.2395 -0.1208 0.051 Uiso 1 1 calc R . . C45 C 0.2770(4) 0.2556(2) -0.0687(5) 0.0421(16) Uani 1 1 d . . . H45 H 0.2712 0.2432 0.0024 0.051 Uiso 1 1 calc R . . C46 C 0.1635(3) 0.2660(3) -0.3255(6) 0.0420(16) Uani 1 1 d . . . C47 C 0.7231(4) 0.5184(2) 0.3325(5) 0.0411(16) Uani 1 1 d . . . H47 H 0.7719 0.5127 0.3571 0.049 Uiso 1 1 calc R . . C48 C 0.6699(4) 0.5426(3) 0.3857(5) 0.0437(16) Uani 1 1 d . . . H48 H 0.6739 0.5565 0.4557 0.052 Uiso 1 1 calc R . . C49 C 0.6264(3) 0.5191(2) 0.2296(5) 0.0339(15) Uani 1 1 d . . . H49 H 0.5942 0.5142 0.1704 0.041 Uiso 1 1 calc R . . C50 C 0.5374(4) 0.5636(2) 0.3448(5) 0.0376(15) Uani 1 1 d . . . C51 C 0.4953(4) 0.5829(2) 0.2647(6) 0.0381(16) Uani 1 1 d . . . H51 H 0.5151 0.5858 0.1943 0.046 Uiso 1 1 calc R . . C52 C 0.4233(4) 0.5985(2) 0.2851(5) 0.0363(15) Uani 1 1 d . . . H52 H 0.3941 0.6116 0.2283 0.044 Uiso 1 1 calc R . . C53 C 0.3939(3) 0.5951(2) 0.3879(6) 0.0378(15) Uani 1 1 d . . . C54 C 0.4402(4) 0.5765(3) 0.4688(6) 0.0453(17) Uani 1 1 d . . . H54 H 0.4218 0.5743 0.5400 0.054 Uiso 1 1 calc R . . C55 C 0.5099(4) 0.5616(3) 0.4493(5) 0.0426(17) Uani 1 1 d . . . H55 H 0.5401 0.5498 0.5063 0.051 Uiso 1 1 calc R . . C56 C 0.3167(4) 0.6101(2) 0.4092(6) 0.0436(17) Uani 1 1 d . . . C57 C 0.2798(4) 0.6437(3) 0.3435(6) 0.0433(17) Uani 1 1 d . . . H57 H 0.3043 0.6571 0.2826 0.052 Uiso 1 1 calc R . . C58 C 0.2072(4) 0.6584(3) 0.3648(7) 0.0504(19) Uani 1 1 d . . . H58 H 0.1826 0.6814 0.3189 0.061 Uiso 1 1 calc R . . C59 C 0.1718(4) 0.6386(3) 0.4545(6) 0.0482(19) Uani 1 1 d . . . C60 C 0.2060(4) 0.6046(3) 0.5176(7) 0.055(2) Uani 1 1 d . . . H60 H 0.1808 0.5906 0.5773 0.066 Uiso 1 1 calc R . . C61 C 0.2780(4) 0.5901(3) 0.4954(6) 0.054(2) Uani 1 1 d . . . H61 H 0.3012 0.5659 0.5401 0.065 Uiso 1 1 calc R . . C62 C 0.0410(4) 0.6263(3) 0.5109(9) 0.077(3) Uani 1 1 d . . . H62 H 0.0397 0.5907 0.5127 0.093 Uiso 1 1 calc R . . C63 C -0.0134(4) 0.6566(3) 0.5365(8) 0.073(3) Uani 1 1 d . . . H63 H -0.0615 0.6462 0.5565 0.087 Uiso 1 1 calc R . . C64 C 0.0775(4) 0.7023(3) 0.4930(6) 0.0500(19) Uani 1 1 d . . . H64 H 0.1074 0.7304 0.4764 0.060 Uiso 1 1 calc R . . N1 N 2.2217(3) 0.4809(2) 1.0149(5) 0.0423(14) Uani 1 1 d . . . N2 N 2.1442(3) 0.4255(2) 0.9488(5) 0.0478(16) Uani 1 1 d . . . N3 N 1.6587(3) 0.3141(2) 0.6878(4) 0.0396(14) Uani 1 1 d . . . N4 N 1.5825(3) 0.2974(2) 0.5557(4) 0.0384(13) Uani 1 1 d . . . N5 N 0.6941(3) 0.50306(18) 0.2350(4) 0.0343(12) Uani 1 1 d . . . N6 N 0.6089(3) 0.54391(18) 0.3215(4) 0.0340(12) Uani 1 1 d . . . N7 N 0.0988(3) 0.65488(19) 0.4817(5) 0.0463(15) Uani 1 1 d . . . N8 N 0.0099(3) 0.7054(2) 0.5299(5) 0.0414(14) Uani 1 1 d . . . O1 O 1.4582(3) 0.30398(17) 0.3504(4) 0.0447(11) Uani 1 1 d . . . O2 O 1.3995(3) 0.3220(2) 0.5051(4) 0.0542(13) Uani 1 1 d . . . O3 O 1.1409(3) 0.3249(2) 0.1606(4) 0.0605(15) Uani 1 1 d . . . O4 O 0.8254(2) 0.41943(17) 0.1422(4) 0.0488(13) Uani 1 1 d . . . O5 O 0.8773(3) 0.47619(19) 0.2451(5) 0.0636(16) Uani 1 1 d . . . O6 O 0.6732(2) 0.41693(17) 0.0545(4) 0.0444(12) Uani 1 1 d . . . O7 O 0.5972(3) 0.47537(18) -0.0073(5) 0.0636(15) Uani 1 1 d . . . O8 O 0.4011(3) 0.27635(17) -0.0294(4) 0.0495(12) Uani 1 1 d . . . O9 O 0.1077(2) 0.23989(18) -0.2976(4) 0.0457(12) Uani 1 1 d . . . O10 O 0.1695(3) 0.2870(2) -0.4120(4) 0.0596(15) 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 Zn1 0.0220(3) 0.0464(4) 0.0373(4) -0.0019(4) -0.0001(3) -0.0007(3) Zn2 0.0229(3) 0.0396(4) 0.0444(4) -0.0045(3) 0.0019(3) -0.0006(3) C1 0.024(3) 0.080(5) 0.083(6) -0.022(5) 0.005(4) -0.004(4) C2 0.031(4) 0.081(5) 0.079(6) -0.047(5) 0.002(4) -0.004(4) C3 0.027(3) 0.065(5) 0.066(5) 0.004(5) -0.004(3) -0.004(4) C4 0.031(2) 0.090(4) 0.136(5) -0.081(4) -0.004(3) -0.001(2) C5 0.039(4) 0.064(5) 0.082(6) -0.016(5) -0.004(4) 0.001(4) C6 0.037(4) 0.069(5) 0.099(7) -0.036(5) -0.017(4) 0.010(4) C7 0.031(3) 0.063(5) 0.039(4) -0.021(3) -0.006(3) -0.004(3) C8 0.031(2) 0.090(4) 0.136(5) -0.081(4) -0.004(3) -0.001(2) C9 0.031(2) 0.090(4) 0.136(5) -0.081(4) -0.004(3) -0.001(2) C10 0.032(4) 0.058(5) 0.044(4) -0.018(4) -0.003(3) -0.006(3) C11 0.040(4) 0.044(4) 0.087(6) -0.022(4) -0.012(4) 0.003(3) C12 0.047(4) 0.051(4) 0.088(6) -0.030(4) -0.027(4) 0.017(4) C13 0.038(4) 0.062(5) 0.044(4) -0.012(4) -0.009(3) -0.010(3) C14 0.031(4) 0.174(11) 0.091(7) -0.067(7) -0.012(5) 0.013(6) C15 0.032(4) 0.175(11) 0.089(7) -0.077(8) -0.011(5) -0.002(6) C16 0.036(3) 0.037(3) 0.037(4) 0.005(3) -0.001(3) 0.000(3) C17 0.033(4) 0.191(11) 0.040(5) -0.025(6) 0.005(4) -0.018(6) C18 0.033(4) 0.177(11) 0.045(5) -0.038(6) 0.010(4) -0.006(6) C19 0.029(3) 0.035(3) 0.053(5) 0.009(3) -0.002(3) -0.006(3) C20 0.029(3) 0.044(4) 0.037(4) 0.000(3) 0.003(3) 0.010(3) C21 0.039(4) 0.050(4) 0.038(4) 0.009(3) 0.005(3) 0.008(3) C22 0.038(4) 0.067(5) 0.040(4) 0.000(4) -0.004(3) 0.016(4) C23 0.035(4) 0.039(4) 0.058(5) -0.007(3) -0.013(3) 0.015(3) C24 0.029(4) 0.046(4) 0.059(5) 0.013(4) 0.012(3) 0.005(3) C25 0.036(3) 0.030(3) 0.054(4) 0.014(3) -0.001(3) 0.003(3) C26 0.036(4) 0.064(5) 0.051(5) -0.005(4) -0.011(3) 0.022(4) C27 0.040(4) 0.047(4) 0.060(5) -0.020(4) -0.012(4) 0.015(3) C28 0.026(4) 0.055(4) 0.075(5) -0.005(4) -0.009(4) 0.001(3) C29 0.034(4) 0.032(3) 0.069(5) -0.005(3) -0.007(4) 0.001(3) C30 0.028(3) 0.037(4) 0.063(5) -0.005(3) -0.002(3) 0.001(3) C31 0.035(4) 0.051(4) 0.044(4) -0.012(3) -0.015(3) 0.006(3) C32 0.028(4) 0.037(4) 0.078(6) 0.002(4) 0.012(4) 0.004(3) C33 0.034(4) 0.050(4) 0.029(4) -0.009(3) -0.001(3) 0.000(3) C34 0.035(4) 0.035(3) 0.036(4) -0.003(3) 0.004(3) -0.004(3) C35 0.031(4) 0.058(4) 0.052(4) -0.005(4) -0.011(3) -0.002(3) C36 0.053(4) 0.040(4) 0.043(4) -0.003(3) -0.007(3) -0.008(3) C37 0.030(3) 0.051(4) 0.045(4) -0.009(3) -0.006(3) -0.017(3) C38 0.023(3) 0.050(4) 0.054(4) -0.004(3) -0.010(3) 0.003(3) C39 0.042(4) 0.037(4) 0.045(4) -0.007(3) -0.004(3) 0.012(3) C40 0.021(3) 0.050(4) 0.045(4) -0.003(3) -0.012(3) -0.005(3) C41 0.036(4) 0.080(6) 0.051(5) 0.000(4) 0.001(4) -0.012(4) C42 0.035(4) 0.083(5) 0.035(4) 0.005(4) 0.001(3) -0.011(4) C43 0.024(3) 0.047(4) 0.040(4) -0.021(3) 0.003(3) 0.000(3) C44 0.036(3) 0.055(4) 0.037(4) -0.012(3) 0.004(3) -0.002(3) C45 0.045(4) 0.043(4) 0.038(4) -0.002(3) -0.003(3) -0.009(3) C46 0.023(3) 0.055(4) 0.048(4) -0.009(4) 0.002(3) 0.006(3) C47 0.038(4) 0.042(4) 0.043(4) -0.007(3) -0.008(3) 0.005(3) C48 0.043(4) 0.059(4) 0.030(3) -0.007(3) -0.012(3) 0.002(3) C49 0.028(3) 0.031(3) 0.042(4) -0.003(3) -0.001(3) -0.010(3) C50 0.031(3) 0.031(3) 0.051(4) -0.011(3) 0.001(3) 0.007(3) C51 0.036(4) 0.042(4) 0.037(4) 0.004(3) 0.000(3) -0.002(3) C52 0.038(4) 0.034(3) 0.036(4) 0.005(3) 0.005(3) -0.001(3) C53 0.035(3) 0.031(3) 0.047(4) 0.000(3) 0.006(3) 0.005(3) C54 0.046(4) 0.050(4) 0.039(4) 0.000(3) 0.016(3) 0.005(3) C55 0.038(4) 0.063(4) 0.027(4) 0.009(3) 0.006(3) 0.016(3) C56 0.045(4) 0.033(3) 0.053(4) -0.003(3) 0.017(4) 0.000(3) C57 0.035(4) 0.044(4) 0.051(4) -0.008(3) 0.012(3) 0.001(3) C58 0.041(4) 0.043(4) 0.067(5) -0.005(4) 0.007(4) 0.007(3) C59 0.035(4) 0.044(4) 0.066(5) -0.008(4) 0.014(4) -0.003(3) C60 0.044(4) 0.045(4) 0.076(6) 0.001(4) 0.020(4) 0.010(4) C61 0.049(5) 0.054(4) 0.059(5) 0.005(4) 0.015(4) 0.015(4) C62 0.042(4) 0.036(4) 0.153(9) -0.026(5) 0.012(6) -0.017(4) C63 0.036(4) 0.053(5) 0.130(8) -0.011(5) 0.012(5) -0.005(4) C64 0.037(4) 0.054(4) 0.060(5) -0.002(4) 0.008(4) -0.005(3) N1 0.031(3) 0.047(3) 0.049(3) -0.007(3) -0.003(3) -0.002(2) N2 0.033(3) 0.061(4) 0.050(4) -0.023(3) -0.003(3) -0.002(3) N3 0.027(3) 0.060(4) 0.031(3) -0.010(3) -0.007(2) -0.003(3) N4 0.022(3) 0.061(4) 0.032(3) -0.002(3) 0.003(2) -0.005(2) N5 0.029(3) 0.025(3) 0.049(3) -0.012(3) -0.001(3) -0.001(2) N6 0.039(3) 0.029(3) 0.033(3) -0.011(2) 0.006(2) -0.001(2) N7 0.040(3) 0.031(3) 0.068(4) -0.011(3) 0.013(3) 0.007(3) N8 0.028(3) 0.045(3) 0.051(4) 0.000(3) 0.005(3) 0.002(2) O1 0.032(2) 0.052(3) 0.051(3) 0.002(2) -0.005(2) 0.006(2) O2 0.038(3) 0.074(4) 0.050(3) 0.002(3) -0.001(2) 0.007(3) O3 0.036(3) 0.077(4) 0.069(4) -0.033(3) -0.020(3) 0.017(3) O4 0.025(2) 0.051(3) 0.071(4) -0.002(3) 0.000(2) 0.001(2) O5 0.032(3) 0.047(3) 0.111(5) -0.020(3) -0.002(3) 0.012(2) O6 0.034(2) 0.044(3) 0.056(3) -0.010(2) -0.003(2) -0.001(2) O7 0.046(3) 0.046(3) 0.099(5) 0.001(3) -0.013(3) -0.006(2) O8 0.045(3) 0.052(3) 0.052(3) 0.007(2) -0.020(2) -0.012(2) O9 0.020(2) 0.057(3) 0.060(3) -0.002(2) -0.005(2) -0.004(2) O10 0.033(3) 0.103(4) 0.043(3) 0.005(3) -0.002(2) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.947(4) . ? Zn1 O9 1.968(5) 4_655 ? Zn1 N4 2.005(5) . ? Zn1 N8 2.038(5) 3_646 ? Zn2 O4 1.936(4) . ? Zn2 O6 1.955(4) . ? Zn2 N5 2.013(5) . ? Zn2 N1 2.035(5) 2_864 ? C1 N1 1.328(8) . ? C1 C2 1.365(9) . ? C1 H1 0.9500 . ? C2 N2 1.369(9) . ? C2 H2 0.9500 . ? C3 N1 1.320(8) . ? C3 N2 1.349(9) . ? C3 H3 0.9500 . ? C4 C5 1.321(10) . ? C4 C9 1.370(10) . ? C4 N2 1.443(9) . ? C5 C6 1.381(10) . ? C5 H5 0.9500 . ? C6 C7 1.353(10) . ? C6 H6 0.9500 . ? C7 C8 1.384(9) . ? C7 C10 1.485(9) . ? C8 C9 1.359(10) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.349(11) . ? C10 C11 1.370(10) . ? C11 C12 1.403(10) . ? C11 H11 0.9500 . ? C12 C13 1.338(10) . ? C12 H12 0.9500 . ? C13 C14 1.354(11) . ? C13 N3 1.446(8) . ? C14 C15 1.362(11) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N4 1.308(8) . ? C16 N3 1.346(8) . ? C16 H16 0.9500 . ? C17 C18 1.345(11) . ? C17 N4 1.383(9) . ? C17 H17 0.9500 . ? C18 N3 1.381(9) . ? C18 H18 0.9500 . ? C19 O2 1.267(8) . ? C19 O1 1.272(8) . ? C19 C20 1.516(9) . ? C20 C25 1.382(8) . ? C20 C21 1.387(9) . ? C21 C22 1.379(9) . ? C21 H21 0.9500 . ? C22 C23 1.384(10) . ? C22 H22 0.9500 . ? C23 C24 1.359(10) . ? C23 O3 1.399(8) . ? C24 C25 1.389(9) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O3 1.389(8) . ? C26 C31 1.395(10) . ? C26 C27 1.401(10) . ? C27 C28 1.371(9) . ? C27 H27 0.9500 . ? C28 C29 1.401(9) . ? C28 H28 0.9500 . ? C29 C30 1.377(9) . ? C29 C32 1.514(9) . ? C30 C31 1.373(9) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 O5 1.200(8) . ? C32 O4 1.283(8) . ? C33 O7 1.223(8) . ? C33 O6 1.285(8) . ? C33 C34 1.517(9) . ? C34 C39 1.366(9) . ? C34 C35 1.372(9) . ? C35 C36 1.391(9) . ? C35 H35 0.9500 . ? C36 C37 1.393(9) . ? C36 H36 0.9500 . ? C37 O8 1.377(7) . ? C37 C38 1.377(9) . ? C38 C39 1.396(9) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.356(10) . ? C40 O8 1.390(7) . ? C40 C45 1.402(8) . ? C41 C42 1.375(10) . ? C41 H41 0.9500 . ? C42 C43 1.403(9) . ? C42 H42 0.9500 . ? C43 C44 1.358(9) . ? C43 C46 1.511(9) . ? C44 C45 1.397(9) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 O10 1.219(8) . ? C46 O9 1.278(8) . ? C47 C48 1.338(9) . ? C47 N5 1.385(8) . ? C47 H47 0.9500 . ? C48 N6 1.367(8) . ? C48 H48 0.9500 . ? C49 N5 1.304(8) . ? C49 N6 1.360(8) . ? C49 H49 0.9500 . ? C50 C51 1.358(9) . ? C50 C55 1.394(9) . ? C50 N6 1.431(8) . ? C51 C52 1.397(9) . ? C51 H51 0.9500 . ? C52 C53 1.390(9) . ? C52 H52 0.9500 . ? C53 C54 1.403(9) . ? C53 C56 1.482(9) . ? C54 C55 1.349(9) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.387(10) . ? C56 C61 1.389(10) . ? C57 C58 1.400(9) . ? C57 H57 0.9500 . ? C58 C59 1.392(10) . ? C58 H58 0.9500 . ? C59 C60 1.351(10) . ? C59 N7 1.436(8) . ? C60 C61 1.392(9) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.314(10) . ? C62 N7 1.348(9) . ? C62 H62 0.9500 . ? C63 N8 1.371(9) . ? C63 H63 0.9500 . ? C64 N8 1.314(8) . ? C64 N7 1.329(9) . ? C64 H64 0.9500 . ? N1 Zn2 2.035(5) 2_866 ? N8 Zn1 2.038(5) 3_656 ? O9 Zn1 1.969(5) 4_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 O1 Zn1 O9 101.38(19) . 4_655 ? O1 Zn1 N4 119.5(2) . . ? O9 Zn1 N4 117.41(19) 4_655 . ? O1 Zn1 N8 101.1(2) . 3_646 ? O9 Zn1 N8 114.1(2) 4_655 3_646 ? N4 Zn1 N8 102.6(2) . 3_646 ? O4 Zn2 O6 99.69(19) . . ? O4 Zn2 N5 122.7(2) . . ? O6 Zn2 N5 109.26(19) . . ? O4 Zn2 N1 107.9(2) . 2_864 ? O6 Zn2 N1 114.9(2) . 2_864 ? N5 Zn2 N1 103.0(2) . 2_864 ? N1 C1 C2 110.4(6) . . ? N1 C1 H1 124.8 . . ? C2 C1 H1 124.8 . . ? C1 C2 N2 105.7(6) . . ? C1 C2 H2 127.1 . . ? N2 C2 H2 127.1 . . ? N1 C3 N2 111.0(7) . . ? N1 C3 H3 124.5 . . ? N2 C3 H3 124.5 . . ? C5 C4 C9 118.9(7) . . ? C5 C4 N2 123.0(7) . . ? C9 C4 N2 118.1(7) . . ? C4 C5 C6 119.6(8) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 123.8(7) . . ? C7 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? C6 C7 C8 114.8(6) . . ? C6 C7 C10 126.2(6) . . ? C8 C7 C10 119.0(6) . . ? C9 C8 C7 121.7(7) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C4 120.7(7) . . ? C8 C9 H9 119.6 . . ? C4 C9 H9 119.6 . . ? C15 C10 C11 116.9(7) . . ? C15 C10 C7 123.6(6) . . ? C11 C10 C7 119.4(6) . . ? C10 C11 C12 119.2(7) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 122.0(7) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 118.2(7) . . ? C12 C13 N3 121.1(6) . . ? C14 C13 N3 120.5(7) . . ? C13 C14 C15 119.9(8) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C10 C15 C14 123.5(8) . . ? C10 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? N4 C16 N3 111.8(6) . . ? N4 C16 H16 124.1 . . ? N3 C16 H16 124.1 . . ? C18 C17 N4 108.8(7) . . ? C18 C17 H17 125.6 . . ? N4 C17 H17 125.6 . . ? C17 C18 N3 107.0(7) . . ? C17 C18 H18 126.5 . . ? N3 C18 H18 126.5 . . ? O2 C19 O1 125.2(6) . . ? O2 C19 C20 118.5(6) . . ? O1 C19 C20 116.2(6) . . ? C25 C20 C21 119.9(6) . . ? C25 C20 C19 119.0(6) . . ? C21 C20 C19 120.7(6) . . ? C22 C21 C20 119.3(6) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 119.8(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 121.5(6) . . ? C24 C23 O3 123.0(7) . . ? C22 C23 O3 115.4(6) . . ? C23 C24 C25 118.7(6) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? C20 C25 C24 120.7(6) . . ? C20 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? O3 C26 C31 123.0(7) . . ? O3 C26 C27 116.5(6) . . ? C31 C26 C27 120.3(6) . . ? C28 C27 C26 119.3(6) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 121.0(7) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C28 118.3(6) . . ? C30 C29 C32 120.2(6) . . ? C28 C29 C32 121.1(6) . . ? C31 C30 C29 122.4(6) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C30 C31 C26 118.5(6) . . ? C30 C31 H31 120.7 . . ? C26 C31 H31 120.7 . . ? O5 C32 O4 124.3(7) . . ? O5 C32 C29 119.5(7) . . ? O4 C32 C29 115.5(6) . . ? O7 C33 O6 124.4(6) . . ? O7 C33 C34 121.2(6) . . ? O6 C33 C34 114.3(6) . . ? C39 C34 C35 118.9(6) . . ? C39 C34 C33 119.9(6) . . ? C35 C34 C33 121.2(6) . . ? C34 C35 C36 121.6(6) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C37 118.8(6) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? O8 C37 C38 124.7(6) . . ? O8 C37 C36 115.1(6) . . ? C38 C37 C36 120.1(6) . . ? C37 C38 C39 119.4(6) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C34 C39 C38 121.2(6) . . ? C34 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C41 C40 O8 122.7(6) . . ? C41 C40 C45 120.7(6) . . ? O8 C40 C45 116.4(6) . . ? C40 C41 C42 120.3(7) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C43 121.1(7) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 117.4(6) . . ? C44 C43 C46 122.1(6) . . ? C42 C43 C46 120.5(6) . . ? C43 C44 C45 123.1(6) . . ? C43 C44 H44 118.5 . . ? C45 C44 H44 118.5 . . ? C44 C45 C40 117.4(6) . . ? C44 C45 H45 121.3 . . ? C40 C45 H45 121.3 . . ? O10 C46 O9 124.1(6) . . ? O10 C46 C43 118.8(6) . . ? O9 C46 C43 117.1(6) . . ? C48 C47 N5 107.5(6) . . ? C48 C47 H47 126.2 . . ? N5 C47 H47 126.2 . . ? C47 C48 N6 108.0(6) . . ? C47 C48 H48 126.0 . . ? N6 C48 H48 126.0 . . ? N5 C49 N6 109.6(6) . . ? N5 C49 H49 125.2 . . ? N6 C49 H49 125.2 . . ? C51 C50 C55 120.0(6) . . ? C51 C50 N6 120.0(6) . . ? C55 C50 N6 120.0(6) . . ? C50 C51 C52 120.4(7) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C53 C52 C51 120.5(6) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C54 117.0(6) . . ? C52 C53 C56 120.7(6) . . ? C54 C53 C56 122.3(6) . . ? C55 C54 C53 122.6(6) . . ? C55 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? C54 C55 C50 119.4(6) . . ? C54 C55 H55 120.3 . . ? C50 C55 H55 120.3 . . ? C57 C56 C61 117.3(6) . . ? C57 C56 C53 121.7(6) . . ? C61 C56 C53 120.9(7) . . ? C56 C57 C58 121.6(7) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? C59 C58 C57 118.7(7) . . ? C59 C58 H58 120.6 . . ? C57 C58 H58 120.6 . . ? C60 C59 C58 120.6(7) . . ? C60 C59 N7 119.3(7) . . ? C58 C59 N7 120.1(7) . . ? C59 C60 C61 120.2(8) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C56 C61 C60 121.5(7) . . ? C56 C61 H61 119.3 . . ? C60 C61 H61 119.3 . . ? C63 C62 N7 107.8(7) . . ? C63 C62 H62 126.1 . . ? N7 C62 H62 126.1 . . ? C62 C63 N8 109.7(7) . . ? C62 C63 H63 125.2 . . ? N8 C63 H63 125.2 . . ? N8 C64 N7 111.8(6) . . ? N8 C64 H64 124.1 . . ? N7 C64 H64 124.1 . . ? C3 N1 C1 106.4(6) . . ? C3 N1 Zn2 121.6(5) . 2_866 ? C1 N1 Zn2 131.4(5) . 2_866 ? C3 N2 C2 106.4(6) . . ? C3 N2 C4 125.3(6) . . ? C2 N2 C4 128.2(6) . . ? C16 N3 C18 106.1(6) . . ? C16 N3 C13 125.2(6) . . ? C18 N3 C13 127.9(6) . . ? C16 N4 C17 106.1(6) . . ? C16 N4 Zn1 127.9(5) . . ? C17 N4 Zn1 125.8(4) . . ? C49 N5 C47 107.9(5) . . ? C49 N5 Zn2 123.5(5) . . ? C47 N5 Zn2 128.6(4) . . ? C49 N6 C48 106.9(5) . . ? C49 N6 C50 124.1(5) . . ? C48 N6 C50 128.8(5) . . ? C64 N7 C62 106.3(6) . . ? C64 N7 C59 125.6(6) . . ? C62 N7 C59 127.8(6) . . ? C64 N8 C63 104.4(6) . . ? C64 N8 Zn1 125.3(5) . 3_656 ? C63 N8 Zn1 129.9(5) . 3_656 ? C19 O1 Zn1 121.3(4) . . ? C26 O3 C23 120.0(5) . . ? C32 O4 Zn2 116.8(4) . . ? C33 O6 Zn2 121.5(4) . . ? C37 O8 C40 119.7(5) . . ? C46 O9 Zn1 110.8(4) . 4_355 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -0.7(10) . . . . ? C9 C4 C5 C6 4.6(17) . . . . ? N2 C4 C5 C6 -176.7(10) . . . . ? C4 C5 C6 C7 1.6(16) . . . . ? C5 C6 C7 C8 -6.1(14) . . . . ? C5 C6 C7 C10 174.5(8) . . . . ? C6 C7 C8 C9 4.7(16) . . . . ? C10 C7 C8 C9 -175.9(10) . . . . ? C7 C8 C9 C4 1.1(19) . . . . ? C5 C4 C9 C8 -6.0(19) . . . . ? N2 C4 C9 C8 175.3(11) . . . . ? C6 C7 C10 C15 170.2(10) . . . . ? C8 C7 C10 C15 -9.1(14) . . . . ? C6 C7 C10 C11 -14.2(13) . . . . ? C8 C7 C10 C11 166.4(9) . . . . ? C15 C10 C11 C12 5.9(13) . . . . ? C7 C10 C11 C12 -169.9(8) . . . . ? C10 C11 C12 C13 -3.1(14) . . . . ? C11 C12 C13 C14 -1.6(14) . . . . ? C11 C12 C13 N3 174.7(8) . . . . ? C12 C13 C14 C15 3.3(16) . . . . ? N3 C13 C14 C15 -173.1(10) . . . . ? C11 C10 C15 C14 -4.4(17) . . . . ? C7 C10 C15 C14 171.2(10) . . . . ? C13 C14 C15 C10 0(2) . . . . ? N4 C17 C18 N3 -4.4(12) . . . . ? O2 C19 C20 C25 -16.4(9) . . . . ? O1 C19 C20 C25 160.1(6) . . . . ? O2 C19 C20 C21 171.3(6) . . . . ? O1 C19 C20 C21 -12.3(9) . . . . ? C25 C20 C21 C22 -0.8(11) . . . . ? C19 C20 C21 C22 171.5(6) . . . . ? C20 C21 C22 C23 -3.1(11) . . . . ? C21 C22 C23 C24 4.6(11) . . . . ? C21 C22 C23 O3 -171.6(6) . . . . ? C22 C23 C24 C25 -2.1(11) . . . . ? O3 C23 C24 C25 173.9(6) . . . . ? C21 C20 C25 C24 3.3(10) . . . . ? C19 C20 C25 C24 -169.1(6) . . . . ? C23 C24 C25 C20 -1.9(10) . . . . ? O3 C26 C27 C28 -170.6(7) . . . . ? C31 C26 C27 C28 4.2(12) . . . . ? C26 C27 C28 C29 -1.2(12) . . . . ? C27 C28 C29 C30 -0.9(12) . . . . ? C27 C28 C29 C32 171.7(8) . . . . ? C28 C29 C30 C31 0.1(12) . . . . ? C32 C29 C30 C31 -172.5(7) . . . . ? C29 C30 C31 C26 2.8(12) . . . . ? O3 C26 C31 C30 169.5(7) . . . . ? C27 C26 C31 C30 -4.9(11) . . . . ? C30 C29 C32 O5 -12.3(12) . . . . ? C28 C29 C32 O5 175.2(8) . . . . ? C30 C29 C32 O4 159.0(7) . . . . ? C28 C29 C32 O4 -13.4(11) . . . . ? O7 C33 C34 C39 -3.1(10) . . . . ? O6 C33 C34 C39 174.7(6) . . . . ? O7 C33 C34 C35 179.4(7) . . . . ? O6 C33 C34 C35 -2.7(9) . . . . ? C39 C34 C35 C36 0.3(11) . . . . ? C33 C34 C35 C36 177.8(6) . . . . ? C34 C35 C36 C37 1.1(11) . . . . ? C35 C36 C37 O8 -175.9(6) . . . . ? C35 C36 C37 C38 -0.5(11) . . . . ? O8 C37 C38 C39 173.4(6) . . . . ? C36 C37 C38 C39 -1.5(10) . . . . ? C35 C34 C39 C38 -2.4(10) . . . . ? C33 C34 C39 C38 -179.9(6) . . . . ? C37 C38 C39 C34 3.1(10) . . . . ? O8 C40 C41 C42 177.0(7) . . . . ? C45 C40 C41 C42 2.3(12) . . . . ? C40 C41 C42 C43 -1.4(13) . . . . ? C41 C42 C43 C44 0.3(11) . . . . ? C41 C42 C43 C46 -177.8(7) . . . . ? C42 C43 C44 C45 0.1(10) . . . . ? C46 C43 C44 C45 178.1(6) . . . . ? C43 C44 C45 C40 0.7(10) . . . . ? C41 C40 C45 C44 -1.9(10) . . . . ? O8 C40 C45 C44 -176.9(6) . . . . ? C44 C43 C46 O10 171.4(7) . . . . ? C42 C43 C46 O10 -10.7(10) . . . . ? C44 C43 C46 O9 -9.1(10) . . . . ? C42 C43 C46 O9 168.8(6) . . . . ? N5 C47 C48 N6 -1.8(8) . . . . ? C55 C50 C51 C52 -3.3(10) . . . . ? N6 C50 C51 C52 174.9(6) . . . . ? C50 C51 C52 C53 0.9(10) . . . . ? C51 C52 C53 C54 1.3(9) . . . . ? C51 C52 C53 C56 -178.0(6) . . . . ? C52 C53 C54 C55 -1.1(10) . . . . ? C56 C53 C54 C55 178.2(7) . . . . ? C53 C54 C55 C50 -1.3(11) . . . . ? C51 C50 C55 C54 3.5(11) . . . . ? N6 C50 C55 C54 -174.7(6) . . . . ? C52 C53 C56 C57 -23.9(10) . . . . ? C54 C53 C56 C57 156.8(7) . . . . ? C52 C53 C56 C61 155.0(7) . . . . ? C54 C53 C56 C61 -24.3(10) . . . . ? C61 C56 C57 C58 2.1(10) . . . . ? C53 C56 C57 C58 -179.0(6) . . . . ? C56 C57 C58 C59 0.2(10) . . . . ? C57 C58 C59 C60 -2.2(11) . . . . ? C57 C58 C59 N7 176.7(6) . . . . ? C58 C59 C60 C61 2.0(12) . . . . ? N7 C59 C60 C61 -177.0(7) . . . . ? C57 C56 C61 C60 -2.4(11) . . . . ? C53 C56 C61 C60 178.6(7) . . . . ? C59 C60 C61 C56 0.4(12) . . . . ? N7 C62 C63 N8 -3.4(12) . . . . ? N2 C3 N1 C1 -1.5(9) . . . . ? N2 C3 N1 Zn2 -173.3(5) . . . 2_866 ? C2 C1 N1 C3 1.4(10) . . . . ? C2 C1 N1 Zn2 172.0(6) . . . 2_866 ? N1 C3 N2 C2 1.1(9) . . . . ? N1 C3 N2 C4 -175.5(8) . . . . ? C1 C2 N2 C3 -0.3(10) . . . . ? C1 C2 N2 C4 176.2(9) . . . . ? C5 C4 N2 C3 -166.4(9) . . . . ? C9 C4 N2 C3 12.3(16) . . . . ? C5 C4 N2 C2 17.7(17) . . . . ? C9 C4 N2 C2 -163.6(10) . . . . ? N4 C16 N3 C18 -4.0(9) . . . . ? N4 C16 N3 C13 -174.7(6) . . . . ? C17 C18 N3 C16 5.0(11) . . . . ? C17 C18 N3 C13 175.4(8) . . . . ? C12 C13 N3 C16 -24.1(12) . . . . ? C14 C13 N3 C16 152.2(8) . . . . ? C12 C13 N3 C18 167.3(9) . . . . ? C14 C13 N3 C18 -16.5(13) . . . . ? N3 C16 N4 C17 1.4(9) . . . . ? N3 C16 N4 Zn1 -173.2(4) . . . . ? C18 C17 N4 C16 1.9(11) . . . . ? C18 C17 N4 Zn1 176.7(7) . . . . ? O1 Zn1 N4 C16 -144.6(5) . . . . ? O9 Zn1 N4 C16 -21.3(7) 4_655 . . . ? N8 Zn1 N4 C16 104.8(6) 3_646 . . . ? O1 Zn1 N4 C17 41.8(8) . . . . ? O9 Zn1 N4 C17 165.2(7) 4_655 . . . ? N8 Zn1 N4 C17 -68.8(7) 3_646 . . . ? N6 C49 N5 C47 -1.2(7) . . . . ? N6 C49 N5 Zn2 -180.0(4) . . . . ? C48 C47 N5 C49 1.8(8) . . . . ? C48 C47 N5 Zn2 -179.4(5) . . . . ? O4 Zn2 N5 C49 -155.5(5) . . . . ? O6 Zn2 N5 C49 -39.6(5) . . . . ? N1 Zn2 N5 C49 83.0(5) 2_864 . . . ? O4 Zn2 N5 C47 26.0(6) . . . . ? O6 Zn2 N5 C47 141.8(5) . . . . ? N1 Zn2 N5 C47 -95.6(5) 2_864 . . . ? N5 C49 N6 C48 0.1(7) . . . . ? N5 C49 N6 C50 -175.9(5) . . . . ? C47 C48 N6 C49 1.1(7) . . . . ? C47 C48 N6 C50 176.8(6) . . . . ? C51 C50 N6 C49 -35.5(9) . . . . ? C55 C50 N6 C49 142.7(6) . . . . ? C51 C50 N6 C48 149.5(7) . . . . ? C55 C50 N6 C48 -32.4(10) . . . . ? N8 C64 N7 C62 1.3(10) . . . . ? N8 C64 N7 C59 -172.8(7) . . . . ? C63 C62 N7 C64 1.3(11) . . . . ? C63 C62 N7 C59 175.3(8) . . . . ? C60 C59 N7 C64 126.9(8) . . . . ? C58 C59 N7 C64 -52.1(11) . . . . ? C60 C59 N7 C62 -46.0(12) . . . . ? C58 C59 N7 C62 135.0(9) . . . . ? N7 C64 N8 C63 -3.3(9) . . . . ? N7 C64 N8 Zn1 170.4(5) . . . 3_656 ? C62 C63 N8 C64 4.1(11) . . . . ? C62 C63 N8 Zn1 -169.2(7) . . . 3_656 ? O2 C19 O1 Zn1 16.6(9) . . . . ? C20 C19 O1 Zn1 -159.6(4) . . . . ? O9 Zn1 O1 C19 -178.5(5) 4_655 . . . ? N4 Zn1 O1 C19 -47.7(5) . . . . ? N8 Zn1 O1 C19 63.8(5) 3_646 . . . ? C31 C26 O3 C23 35.8(11) . . . . ? C27 C26 O3 C23 -149.5(7) . . . . ? C24 C23 O3 C26 43.9(10) . . . . ? C22 C23 O3 C26 -139.9(7) . . . . ? O5 C32 O4 Zn2 0.8(10) . . . . ? C29 C32 O4 Zn2 -170.1(5) . . . . ? O6 Zn2 O4 C32 -166.3(5) . . . . ? N5 Zn2 O4 C32 -45.8(6) . . . . ? N1 Zn2 O4 C32 73.4(6) 2_864 . . . ? O7 C33 O6 Zn2 13.7(10) . . . . ? C34 C33 O6 Zn2 -164.1(4) . . . . ? O4 Zn2 O6 C33 -172.5(5) . . . . ? N5 Zn2 O6 C33 57.7(5) . . . . ? N1 Zn2 O6 C33 -57.5(5) 2_864 . . . ? C38 C37 O8 C40 32.2(10) . . . . ? C36 C37 O8 C40 -152.7(6) . . . . ? C41 C40 O8 C37 39.4(10) . . . . ? C45 C40 O8 C37 -145.7(6) . . . . ? O10 C46 O9 Zn1 8.1(9) . . . 4_355 ? C43 C46 O9 Zn1 -171.3(4) . . . 4_355 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.741 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.074 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.001 0.000 0.336 474 231 ' ' 2 0.068 0.500 0.664 474 231 ' ' _platon_squeeze_details ; In the refinement, the solvent molecules were found to be seriouly disordered. We have tried to refine these atoms coordinates many times, but failed each time. So in the final refinement, the contribution of these unsolved solvent to the whole structure were treated by using PLATON/SQUEEZE programm. Further analysis using PLATON indicates that he void in the unit cell has a volume of 948.1 Ang^3 (consisting of about 15.7% of the crystal volume, equally distributed across two cavities). The residual electron density count amounted to 462 e per unit cell, corresponding to nearly 8 molecules of DMF and 14 molecules of H2O (the content of each of the two cavities per unit cell being equivalent about 4 molecules of DMF and 7 molecules of H2O, i.e. every molecule is distributed with 2 molecules of DMF and 3.5 molecules of H2O). W: Number of unusual anisotropic displacement parameters ................. 2 N: Total Potential Solvent Accessible Void Vol .................. 948.1 Ang^3 N: Electron Count / Cell = 461 - To be included in D(calc), F000 & Mol.Wght. ; #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 828137' #TrackingRef '- new-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H46 N8 Ni3 O18, 1.2(H2 O), 2(H0.80 O0.40)' _chemical_formula_sum 'C68 H50 N8 Ni3 O20' _chemical_formula_weight 1475.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Fddd ' _symmetry_space_group_name_Hall '-F 2uv 2vw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 16.292(4) _cell_length_b 30.712(8) _cell_length_c 51.727(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25881(12) _cell_formula_units_Z 16 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5813 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 23.57 _exptl_crystal_description green _exptl_crystal_colour block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12128 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7773 _exptl_absorpt_correction_T_max 0.8186 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49638 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 63 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6374 _reflns_number_gt 5019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _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^)+(0.09P)^2^+1.99P] 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 6374 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1369 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.17698(19) -0.04537(10) 0.52636(6) 0.0371(7) Uani 1 1 d . . . C2 C 1.15867(18) -0.08469(10) 0.51381(6) 0.0377(7) Uani 1 1 d . . . C3 C 1.2168(2) -0.10269(11) 0.49700(7) 0.0431(8) Uani 1 1 d . . . H3 H 1.2047 -0.1286 0.4885 0.052 Uiso 1 1 calc R . . C4 C 1.2930(2) -0.08254(11) 0.49264(6) 0.0414(7) Uani 1 1 d . . . H4 H 1.3308 -0.0944 0.4811 0.050 Uiso 1 1 calc R . . C5 C 1.3102(2) -0.04405(10) 0.50619(6) 0.0390(7) Uani 1 1 d . . . C6 C 1.2545(2) -0.02594(11) 0.52341(7) 0.0431(8) Uani 1 1 d . . . H6 H 1.2683 -0.0013 0.5329 0.052 Uiso 1 1 calc R . . C7 C 1.11875(19) -0.02241(10) 0.54395(6) 0.0387(7) Uani 1 1 d . . . C8 C 1.3922(2) -0.02256(11) 0.50310(6) 0.0400(7) Uani 1 1 d . . . C9 C 1.08371(19) -0.11159(10) 0.51780(6) 0.0379(7) Uani 1 1 d . . . C10 C 1.0794(2) -0.13705(10) 0.53957(6) 0.0414(7) Uani 1 1 d . . . H10 H 1.1189 -0.1338 0.5524 0.050 Uiso 1 1 calc R . . C11 C 1.01656(19) -0.16797(11) 0.54286(7) 0.0414(7) Uani 1 1 d . . . H11 H 1.0135 -0.1842 0.5580 0.050 Uiso 1 1 calc R . . C12 C 0.95929(19) -0.17407(11) 0.52340(6) 0.0395(7) Uani 1 1 d . . . C13 C 0.96374(19) -0.14871(11) 0.50135(6) 0.0381(7) Uani 1 1 d . . . H13 H 0.9260 -0.1531 0.4881 0.046 Uiso 1 1 calc R . . C14 C 1.0238(2) -0.11675(10) 0.49862(6) 0.0384(7) Uani 1 1 d . . . C15 C 1.0190(2) -0.08888(12) 0.47527(6) 0.0438(8) Uani 1 1 d . . . C16 C 0.8592(2) -0.04344(10) 0.52598(6) 0.0405(7) Uani 1 1 d . . . C17 C 0.8718(2) 0.09692(11) 0.57983(6) 0.0422(8) Uani 1 1 d . A . H17 H 0.9216 0.1105 0.5833 0.051 Uiso 1 1 calc R . . C18 C 0.7809(2) 0.04905(11) 0.56918(6) 0.0432(8) Uani 1 1 d . . . H18 H 0.7562 0.0232 0.5639 0.052 Uiso 1 1 calc R . . C19 C 0.7413(2) 0.08710(11) 0.57468(7) 0.0451(8) Uani 1 1 d . A . H19 H 0.6849 0.0917 0.5739 0.054 Uiso 1 1 calc R . . C20 C 0.7855(2) 0.16164(12) 0.58701(7) 0.0426(8) Uani 0.50 1 d P A 1 C21 C 0.7254(4) 0.1731(2) 0.60717(13) 0.0436(15) Uani 0.50 1 d P A 1 H21A H 0.6952 0.1518 0.6157 0.052 Uiso 0.50 1 calc PR A 1 C22 C 0.7159(4) 0.2161(2) 0.61280(14) 0.0459(16) Uani 0.50 1 d P A 1 H22A H 0.6783 0.2240 0.6255 0.055 Uiso 0.50 1 calc PR A 1 C23 C 0.7655(2) 0.25291(11) 0.59875(7) 0.0426(7) Uani 0.50 1 d P A 1 C24 C 0.8208(4) 0.2367(2) 0.58086(13) 0.0451(16) Uani 0.50 1 d P A 1 H24A H 0.8541 0.2567 0.5723 0.054 Uiso 0.50 1 calc PR A 1 C25 C 0.8309(4) 0.1911(2) 0.57445(13) 0.0409(14) Uani 0.50 1 d P A 1 H25A H 0.8683 0.1825 0.5619 0.049 Uiso 0.50 1 calc PR A 1 C26 C 0.7573(2) 0.29587(11) 0.60605(6) 0.0402(7) Uani 1 1 d . . . C27 C 0.7535(2) 0.30780(12) 0.63229(7) 0.0463(8) Uani 1 1 d . A . H27 H 0.7537 0.2863 0.6450 0.056 Uiso 1 1 calc R . . C28 C 0.7495(2) 0.35090(12) 0.63942(7) 0.0469(8) Uani 1 1 d . . . H28 H 0.7425 0.3577 0.6568 0.056 Uiso 1 1 calc R A . C29 C 0.75530(19) 0.38391(11) 0.62211(6) 0.0415(7) Uani 1 1 d . A . C30 C 0.7615(2) 0.37384(11) 0.59621(6) 0.0415(7) Uani 1 1 d . . . H30 H 0.7648 0.3961 0.5841 0.050 Uiso 1 1 calc R A . C31 C 0.7629(2) 0.33112(11) 0.58819(7) 0.0423(7) Uani 1 1 d . A . H31 H 0.7676 0.3251 0.5706 0.051 Uiso 1 1 calc R . . C32 C 0.7792(2) 0.43958(11) 0.65524(6) 0.0423(7) Uani 1 1 d . A . H32 H 0.7939 0.4206 0.6685 0.051 Uiso 1 1 calc R . . C33 C 0.7512(2) 0.49803(12) 0.63332(7) 0.0490(9) Uani 1 1 d . A . H33 H 0.7434 0.5272 0.6291 0.059 Uiso 1 1 calc R . . C34 C 0.73937(19) 0.46412(11) 0.61698(7) 0.0423(8) Uani 1 1 d . A . H34 H 0.7225 0.4656 0.5998 0.051 Uiso 1 1 calc R . . C20' C 0.7855(2) 0.16164(12) 0.58701(7) 0.0426(8) Uani 0.50 1 d P A 2 C21' C 0.8205(4) 0.1810(2) 0.60927(13) 0.0441(16) Uani 0.50 1 d P A 2 H21B H 0.8491 0.1640 0.6211 0.053 Uiso 0.50 1 calc PR A 2 C22' C 0.8119(4) 0.2272(2) 0.61347(13) 0.0428(15) Uani 0.50 1 d P A 2 H22B H 0.8402 0.2397 0.6272 0.051 Uiso 0.50 1 calc PR A 2 C23' C 0.7655(2) 0.25291(11) 0.59875(7) 0.0426(7) Uani 0.50 1 d P A 2 C24' C 0.7247(4) 0.2369(2) 0.57915(12) 0.0438(16) Uani 0.50 1 d P A 2 H24B H 0.6906 0.2549 0.5695 0.053 Uiso 0.50 1 calc PR A 2 C25' C 0.7330(4) 0.1864(2) 0.57155(13) 0.0421(15) Uani 0.50 1 d P A 2 H25B H 0.7046 0.1743 0.5577 0.050 Uiso 0.50 1 calc PR A 2 N1 N 0.86362(18) 0.05542(9) 0.57272(5) 0.0450(6) Uani 1 1 d . . . N2 N 0.79766(17) 0.11650(10) 0.58130(5) 0.0442(7) Uani 1 1 d . . . N3 N 0.75736(16) 0.42682(9) 0.63093(5) 0.0417(6) Uani 1 1 d . . . N4 N 0.77674(15) 0.48299(8) 0.65748(5) 0.0362(6) Uani 1 1 d . . . Ni1 Ni 1.0000 0.0000 0.5000 0.04242(18) Uani 1 2 d S . . Ni2 Ni 0.95561(3) 0.016044(14) 0.559138(8) 0.04079(15) Uani 1 1 d . . . O1 O 1.04339(13) -0.01892(7) 0.53694(4) 0.0392(5) Uani 1 1 d . . . O2 O 1.14623(14) -0.00872(7) 0.56460(4) 0.0417(5) Uani 1 1 d . . . O3 O 1.40734(15) 0.01055(8) 0.51566(5) 0.0464(6) Uani 1 1 d . . . O4 O 1.44172(14) -0.03984(7) 0.48740(4) 0.0439(6) Uani 1 1 d . . . H4B H 1.4845 -0.0441 0.4964 0.053 Uiso 1 1 d R . . O5 O 1.04671(14) -0.05014(8) 0.47606(4) 0.0433(5) Uani 1 1 d . . . O6 O 0.98654(14) -0.10436(8) 0.45566(4) 0.0449(6) Uani 1 1 d . . . O7 O 0.89900(14) -0.03499(8) 0.50584(4) 0.0422(5) Uani 1 1 d . . . O8 O 0.86989(13) -0.02759(7) 0.54808(4) 0.0403(5) Uani 1 1 d . . . O1W O 1.04491(14) 0.05635(8) 0.57823(4) 0.0439(6) Uani 1 1 d . . . H1WB H 1.0780 0.0403 0.5867 0.053 Uiso 1 1 d R . . H1WC H 1.0714 0.0709 0.5670 0.053 Uiso 1 1 d R . . O2W O 0.9702(2) 0.82367(13) 0.42587(7) 0.0482(10) Uani 0.60 1 d P . . H2WA H 0.9891 0.8438 0.4354 0.058 Uiso 0.60 1 d PR . . H2WD H 0.9733 0.7966 0.4291 0.058 Uiso 0.60 1 d PR . . O3W O 0.0143(3) 0.1250 0.6250 0.0485(10) Uani 0.80 2 d SP . . H3WF H 0.0629 0.1179 0.6209 0.058 Uiso 0.40 1 d PR . . H3WE H 0.0102 0.1526 0.6252 0.058 Uiso 0.40 1 d PR . . 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 0.0360(16) 0.0346(16) 0.0407(17) 0.0063(13) -0.0035(13) -0.0118(13) C2 0.0318(15) 0.0359(16) 0.0454(18) 0.0087(13) -0.0041(13) -0.0076(12) C3 0.0401(17) 0.0417(18) 0.0475(18) -0.0070(15) 0.0056(14) -0.0178(15) C4 0.0358(16) 0.0430(18) 0.0454(18) -0.0085(14) 0.0072(13) -0.0164(14) C5 0.0430(17) 0.0361(16) 0.0378(16) 0.0043(13) 0.0083(13) -0.0137(14) C6 0.0371(16) 0.0427(18) 0.0496(19) -0.0034(15) 0.0019(14) -0.0154(14) C7 0.0389(17) 0.0416(18) 0.0358(16) 0.0059(13) -0.0073(13) -0.0105(13) C8 0.0358(16) 0.0389(17) 0.0452(18) -0.0109(14) 0.0073(14) -0.0131(13) C9 0.0349(15) 0.0389(17) 0.0400(17) -0.0047(13) 0.0033(13) -0.0102(13) C10 0.0398(17) 0.0422(18) 0.0421(17) 0.0043(14) -0.0145(13) -0.0213(14) C11 0.0358(16) 0.0422(18) 0.0462(19) 0.0063(14) -0.0122(14) -0.0125(13) C12 0.0363(16) 0.0419(17) 0.0403(17) 0.0008(14) -0.0065(13) -0.0198(13) C13 0.0345(16) 0.0400(17) 0.0398(17) -0.0021(13) -0.0005(13) -0.0141(14) C14 0.0371(16) 0.0383(17) 0.0398(17) -0.0041(13) 0.0003(13) -0.0093(14) C15 0.0432(18) 0.0491(19) 0.0391(18) 0.0103(15) -0.0037(14) -0.0143(15) C16 0.0434(18) 0.0317(16) 0.0465(19) 0.0032(14) -0.0012(14) -0.0125(13) C17 0.0400(17) 0.0444(18) 0.0423(18) -0.0112(14) -0.0049(14) -0.0029(14) C18 0.0428(18) 0.0458(19) 0.0409(18) -0.0103(15) 0.0139(14) -0.0144(14) C19 0.0403(18) 0.049(2) 0.0462(19) -0.0102(15) 0.0003(14) -0.0032(15) C20 0.0390(17) 0.0502(19) 0.0386(17) -0.0143(15) -0.0088(14) 0.0019(15) C21 0.052(4) 0.034(3) 0.044(4) -0.015(3) 0.003(3) 0.001(3) C22 0.043(4) 0.040(4) 0.054(4) -0.019(3) 0.012(3) -0.010(3) C23 0.0423(18) 0.0425(18) 0.0430(18) -0.0077(15) -0.0062(14) 0.0019(14) C24 0.043(4) 0.056(4) 0.037(3) -0.006(3) -0.005(3) 0.009(3) C25 0.038(3) 0.042(3) 0.043(4) -0.013(3) -0.009(3) 0.011(3) C26 0.0425(17) 0.0426(18) 0.0355(17) 0.0018(13) -0.0036(13) 0.0006(14) C27 0.051(2) 0.0477(19) 0.0400(18) -0.0009(15) 0.0124(15) 0.0035(16) C28 0.050(2) 0.048(2) 0.0433(18) -0.0128(15) 0.0121(15) -0.0154(16) C29 0.0382(17) 0.0471(19) 0.0392(17) -0.0072(14) -0.0086(13) -0.0085(14) C30 0.0415(17) 0.0424(18) 0.0407(17) -0.0104(14) -0.0127(14) 0.0049(14) C31 0.0413(18) 0.0453(18) 0.0402(18) 0.0044(14) -0.0050(14) -0.0068(14) C32 0.0444(18) 0.0407(17) 0.0419(17) -0.0040(14) -0.0107(14) 0.0088(14) C33 0.052(2) 0.048(2) 0.047(2) 0.0187(16) -0.0150(16) -0.0157(16) C34 0.0368(17) 0.0447(18) 0.0454(18) 0.0107(15) -0.0084(13) -0.0084(14) C20' 0.0390(17) 0.0502(19) 0.0386(17) -0.0143(15) -0.0088(14) 0.0019(15) C21' 0.047(4) 0.044(4) 0.042(3) -0.021(3) -0.012(3) 0.016(3) C22' 0.044(4) 0.038(3) 0.047(4) -0.004(3) 0.000(3) -0.011(3) C23' 0.0423(18) 0.0425(18) 0.0430(18) -0.0077(15) -0.0062(14) 0.0019(14) C24' 0.044(4) 0.057(4) 0.030(3) -0.015(3) 0.016(3) 0.013(3) C25' 0.051(4) 0.035(3) 0.040(3) 0.012(3) 0.004(3) -0.009(3) N1 0.0474(16) 0.0464(15) 0.0412(15) -0.0010(12) 0.0086(12) -0.0029(13) N2 0.0454(16) 0.0516(17) 0.0355(15) -0.0215(12) -0.0071(12) 0.0034(13) N3 0.0398(15) 0.0447(16) 0.0406(15) 0.0002(12) -0.0022(12) 0.0084(12) N4 0.0305(13) 0.0360(13) 0.0420(15) 0.0095(11) 0.0012(11) -0.0165(11) Ni1 0.0433(3) 0.0476(4) 0.0363(3) -0.0159(3) -0.0046(2) 0.0010(3) Ni2 0.0371(2) 0.0442(3) 0.0411(3) -0.00654(18) -0.00798(17) -0.00993(18) O1 0.0387(12) 0.0414(12) 0.0373(12) -0.0058(9) -0.0076(9) -0.0060(9) O2 0.0423(12) 0.0358(12) 0.0470(13) -0.0136(10) -0.0096(10) -0.0062(9) O3 0.0464(13) 0.0450(13) 0.0480(13) -0.0145(11) 0.0145(11) -0.0164(10) O4 0.0413(12) 0.0444(13) 0.0461(13) -0.0148(10) 0.0144(10) -0.0126(10) O5 0.0433(12) 0.0504(14) 0.0362(12) -0.0145(10) -0.0063(9) 0.0024(10) O6 0.0406(12) 0.0499(14) 0.0441(13) 0.0116(11) -0.0113(10) -0.0096(10) O7 0.0440(12) 0.0481(13) 0.0347(11) -0.0162(10) -0.0042(10) 0.0008(10) O8 0.0392(12) 0.0372(12) 0.0444(13) -0.0029(10) 0.0044(10) -0.0159(9) O1W 0.0418(12) 0.0494(14) 0.0406(12) 0.0006(10) -0.0166(10) -0.0166(10) O2W 0.057(2) 0.044(2) 0.043(2) -0.0065(17) 0.0149(18) -0.0225(19) O3W 0.054(2) 0.048(2) 0.043(2) -0.0158(19) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.403(4) . ? C1 C6 1.405(4) . ? C1 C7 1.492(5) . ? C2 C3 1.399(5) . ? C2 C9 1.489(4) . ? C3 C4 1.406(4) . ? C3 H3 0.9300 . ? C4 C5 1.403(5) . ? C4 H4 0.9300 . ? C5 C6 1.388(5) . ? C5 C8 1.498(4) . ? C6 H6 0.9300 . ? C7 O2 1.233(4) . ? C7 O1 1.284(4) . ? C8 O3 1.232(4) . ? C8 O4 1.262(4) . ? C9 C10 1.373(4) . ? C9 C14 1.400(4) . ? C10 C11 1.407(4) . ? C10 H10 0.9300 . ? C11 C12 1.385(4) . ? C11 H11 0.9300 . ? C12 C13 1.383(5) . ? C12 C16 1.503(4) 2_645 ? C13 C14 1.393(4) . ? C13 H13 0.9300 . ? C14 C15 1.483(5) . ? C15 O6 1.239(4) . ? C15 O5 1.274(4) . ? C16 O7 1.254(4) . ? C16 O8 1.255(4) . ? C16 C12 1.503(4) 2_645 ? C17 N1 1.333(4) . ? C17 N2 1.351(4) . ? C17 H17 0.9300 . ? C18 C19 1.365(5) . ? C18 N1 1.373(4) . ? C18 H18 0.9300 . ? C19 N2 1.333(4) . ? C19 H19 0.9300 . ? C20 C25 1.338(8) . ? C20 N2 1.431(4) . ? C20 C21 1.473(7) . ? C21 C22 1.362(9) . ? C21 H21A 0.9300 . ? C22 C23 1.569(8) . ? C22 H22A 0.9300 . ? C23 C26 1.379(5) . ? C23 C24 1.384(8) . ? C24 C25 1.448(9) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.407(5) . ? C26 C31 1.426(5) . ? C27 C28 1.376(5) . ? C27 H27 0.9300 . ? C28 C29 1.356(5) . ? C28 H28 0.9300 . ? C29 C30 1.379(5) . ? C29 N3 1.395(4) . ? C30 C31 1.376(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 N4 1.339(4) . ? C32 N3 1.365(4) . ? C32 H32 0.9300 . ? C33 C34 1.355(5) . ? C33 N4 1.395(4) . ? C33 H33 0.9300 . ? C34 N3 1.386(4) . ? C34 H34 0.9300 . ? C21' C22' 1.442(9) . ? C21' H21B 0.9300 . ? C22' H22B 0.9300 . ? C24' C25' 1.606(9) . ? C24' H24B 0.9300 . ? C25' H25B 0.9300 . ? N1 Ni2 2.050(3) . ? N4 Ni2 2.024(3) 7_655 ? Ni1 O7 1.988(2) 17_756 ? Ni1 O7 1.988(2) . ? Ni1 O5 2.117(2) . ? Ni1 O5 2.117(2) 17_756 ? Ni1 O1 2.119(2) 17_756 ? Ni1 O1 2.119(2) . ? Ni2 O8 2.018(2) . ? Ni2 N4 2.024(3) 7_645 ? Ni2 O5 2.101(2) 17_756 ? Ni2 O1 2.125(2) . ? Ni2 O1W 2.150(2) . ? O4 H4B 0.8500 . ? O5 Ni2 2.101(2) 17_756 ? O1W H1WB 0.8501 . ? O1W H1WC 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WD 0.8502 . ? O3W H3WF 0.8498 . ? O3W H3WE 0.8501 . ? 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 C6 120.4(3) . . ? C2 C1 C7 123.6(3) . . ? C6 C1 C7 115.9(3) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C9 114.9(3) . . ? C1 C2 C9 126.0(3) . . ? C2 C3 C4 121.6(3) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 117.9(3) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C6 C5 C4 121.8(3) . . ? C6 C5 C8 118.4(3) . . ? C4 C5 C8 119.8(3) . . ? C5 C6 C1 119.2(3) . . ? C5 C6 H6 120.4 . . ? C1 C6 H6 120.4 . . ? O2 C7 O1 124.3(3) . . ? O2 C7 C1 117.3(3) . . ? O1 C7 C1 118.4(3) . . ? O3 C8 O4 123.9(3) . . ? O3 C8 C5 119.1(3) . . ? O4 C8 C5 117.0(3) . . ? C10 C9 C14 118.8(3) . . ? C10 C9 C2 118.1(3) . . ? C14 C9 C2 122.4(3) . . ? C9 C10 C11 121.4(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 119.2(3) . . ? C13 C12 C16 119.1(3) . 2_645 ? C11 C12 C16 121.7(3) . 2_645 ? C12 C13 C14 121.1(3) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C9 119.8(3) . . ? C13 C14 C15 116.9(3) . . ? C9 C14 C15 123.3(3) . . ? O6 C15 O5 122.4(3) . . ? O6 C15 C14 117.9(3) . . ? O5 C15 C14 119.6(3) . . ? O7 C16 O8 127.2(3) . . ? O7 C16 C12 116.6(3) . 2_645 ? O8 C16 C12 116.2(3) . 2_645 ? N1 C17 N2 110.6(3) . . ? N1 C17 H17 124.7 . . ? N2 C17 H17 124.7 . . ? C19 C18 N1 108.3(3) . . ? C19 C18 H18 125.8 . . ? N1 C18 H18 125.8 . . ? N2 C19 C18 107.9(3) . . ? N2 C19 H19 126.0 . . ? C18 C19 H19 126.0 . . ? C25 C20 N2 118.6(4) . . ? C25 C20 C21 123.4(5) . . ? N2 C20 C21 118.0(4) . . ? C22 C21 C20 117.3(6) . . ? C22 C21 H21A 121.4 . . ? C20 C21 H21A 121.4 . . ? C21 C22 C23 122.8(6) . . ? C21 C22 H22A 118.6 . . ? C23 C22 H22A 118.6 . . ? C26 C23 C24 126.2(5) . . ? C26 C23 C22 120.8(4) . . ? C24 C23 C22 112.8(5) . . ? C23 C24 C25 125.0(7) . . ? C23 C24 H24A 117.5 . . ? C25 C24 H24A 117.5 . . ? C20 C25 C24 118.7(6) . . ? C20 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C23 C26 C27 121.2(3) . . ? C23 C26 C31 122.9(3) . . ? C27 C26 C31 115.5(3) . . ? C28 C27 C26 120.7(3) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 122.6(3) . . ? C29 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? C28 C29 C30 118.6(3) . . ? C28 C29 N3 119.5(3) . . ? C30 C29 N3 121.9(3) . . ? C31 C30 C29 120.5(3) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C26 121.8(3) . . ? C30 C31 H31 119.1 . . ? C26 C31 H31 119.1 . . ? N4 C32 N3 111.0(3) . . ? N4 C32 H32 124.5 . . ? N3 C32 H32 124.5 . . ? C34 C33 N4 110.3(3) . . ? C34 C33 H33 124.9 . . ? N4 C33 H33 124.9 . . ? C33 C34 N3 106.3(3) . . ? C33 C34 H34 126.9 . . ? N3 C34 H34 126.9 . . ? C22' C21' H21B 120.1 . . ? C21' C22' H22B 118.2 . . ? C25' C24' H24B 119.7 . . ? C24' C25' H25B 122.0 . . ? C17 N1 C18 105.7(3) . . ? C17 N1 Ni2 125.8(2) . . ? C18 N1 Ni2 126.0(2) . . ? C19 N2 C17 107.5(3) . . ? C19 N2 C20 127.9(3) . . ? C17 N2 C20 124.5(3) . . ? C32 N3 C34 107.3(3) . . ? C32 N3 C29 125.4(3) . . ? C34 N3 C29 127.3(3) . . ? C32 N4 C33 105.1(3) . . ? C32 N4 Ni2 124.7(2) . 7_655 ? C33 N4 Ni2 129.8(2) . 7_655 ? O7 Ni1 O7 180.00(11) 17_756 . ? O7 Ni1 O5 90.39(9) 17_756 . ? O7 Ni1 O5 89.61(9) . . ? O7 Ni1 O5 89.61(9) 17_756 17_756 ? O7 Ni1 O5 90.39(9) . 17_756 ? O5 Ni1 O5 180.00(10) . 17_756 ? O7 Ni1 O1 89.48(9) 17_756 17_756 ? O7 Ni1 O1 90.52(9) . 17_756 ? O5 Ni1 O1 77.99(9) . 17_756 ? O5 Ni1 O1 102.01(9) 17_756 17_756 ? O7 Ni1 O1 90.52(9) 17_756 . ? O7 Ni1 O1 89.48(9) . . ? O5 Ni1 O1 102.01(9) . . ? O5 Ni1 O1 77.99(9) 17_756 . ? O1 Ni1 O1 180.00(5) 17_756 . ? O8 Ni2 N4 90.40(10) . 7_645 ? O8 Ni2 N1 89.01(11) . . ? N4 Ni2 N1 96.17(10) 7_645 . ? O8 Ni2 O5 94.18(9) . 17_756 ? N4 Ni2 O5 172.84(10) 7_645 17_756 ? N1 Ni2 O5 89.41(10) . 17_756 ? O8 Ni2 O1 88.69(9) . . ? N4 Ni2 O1 96.42(9) 7_645 . ? N1 Ni2 O1 167.22(10) . . ? O5 Ni2 O1 78.21(9) 17_756 . ? O8 Ni2 O1W 168.66(9) . . ? N4 Ni2 O1W 78.50(10) 7_645 . ? N1 Ni2 O1W 89.87(11) . . ? O5 Ni2 O1W 97.09(9) 17_756 . ? O1 Ni2 O1W 94.80(9) . . ? C7 O1 Ni1 126.6(2) . . ? C7 O1 Ni2 122.2(2) . . ? Ni1 O1 Ni2 97.13(9) . . ? C8 O4 H4B 103.6 . . ? C15 O5 Ni2 115.5(2) . 17_756 ? C15 O5 Ni1 124.8(2) . . ? Ni2 O5 Ni1 97.93(10) 17_756 . ? C16 O7 Ni1 131.7(2) . . ? C16 O8 Ni2 127.7(2) . . ? Ni2 O1W H1WB 109.4 . . ? Ni2 O1W H1WC 109.5 . . ? H1WB O1W H1WC 109.5 . . ? H2WA O2W H2WD 125.3 . . ? H3WF O3W H3WE 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -4.2(5) . . . . ? C7 C1 C2 C3 177.8(3) . . . . ? C6 C1 C2 C9 171.7(3) . . . . ? C7 C1 C2 C9 -6.3(5) . . . . ? C1 C2 C3 C4 0.6(5) . . . . ? C9 C2 C3 C4 -175.7(3) . . . . ? C2 C3 C4 C5 1.5(5) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C3 C4 C5 C8 177.2(3) . . . . ? C4 C5 C6 C1 -3.4(5) . . . . ? C8 C5 C6 C1 179.3(3) . . . . ? C2 C1 C6 C5 5.6(5) . . . . ? C7 C1 C6 C5 -176.3(3) . . . . ? C2 C1 C7 O2 134.4(3) . . . . ? C6 C1 C7 O2 -43.7(4) . . . . ? C2 C1 C7 O1 -44.2(4) . . . . ? C6 C1 C7 O1 137.7(3) . . . . ? C6 C5 C8 O3 -0.7(5) . . . . ? C4 C5 C8 O3 -178.0(3) . . . . ? C6 C5 C8 O4 179.7(3) . . . . ? C4 C5 C8 O4 2.4(5) . . . . ? C3 C2 C9 C10 98.7(4) . . . . ? C1 C2 C9 C10 -77.4(4) . . . . ? C3 C2 C9 C14 -71.8(4) . . . . ? C1 C2 C9 C14 112.2(4) . . . . ? C14 C9 C10 C11 0.2(5) . . . . ? C2 C9 C10 C11 -170.6(3) . . . . ? C9 C10 C11 C12 2.3(5) . . . . ? C10 C11 C12 C13 -1.7(5) . . . . ? C10 C11 C12 C16 -179.8(3) . . . 2_645 ? C11 C12 C13 C14 -1.2(5) . . . . ? C16 C12 C13 C14 177.0(3) 2_645 . . . ? C12 C13 C14 C9 3.6(5) . . . . ? C12 C13 C14 C15 -175.0(3) . . . . ? C10 C9 C14 C13 -3.1(5) . . . . ? C2 C9 C14 C13 167.3(3) . . . . ? C10 C9 C14 C15 175.4(3) . . . . ? C2 C9 C14 C15 -14.2(5) . . . . ? C13 C14 C15 O6 -27.5(5) . . . . ? C9 C14 C15 O6 154.0(3) . . . . ? C13 C14 C15 O5 151.4(3) . . . . ? C9 C14 C15 O5 -27.1(5) . . . . ? N1 C18 C19 N2 0.4(4) . . . . ? C25 C20 C21 C22 0.8(9) . . . . ? N2 C20 C21 C22 178.5(5) . . . . ? C20 C21 C22 C23 0.2(10) . . . . ? C21 C22 C23 C26 -176.3(6) . . . . ? C21 C22 C23 C24 -1.8(9) . . . . ? C26 C23 C24 C25 176.8(5) . . . . ? C22 C23 C24 C25 2.6(8) . . . . ? N2 C20 C25 C24 -177.8(4) . . . . ? C21 C20 C25 C24 -0.1(8) . . . . ? C23 C24 C25 C20 -1.9(9) . . . . ? C24 C23 C26 C27 -131.9(5) . . . . ? C22 C23 C26 C27 41.8(6) . . . . ? C24 C23 C26 C31 39.6(6) . . . . ? C22 C23 C26 C31 -146.6(4) . . . . ? C23 C26 C27 C28 176.7(3) . . . . ? C31 C26 C27 C28 4.6(5) . . . . ? C26 C27 C28 C29 -5.2(6) . . . . ? C27 C28 C29 C30 3.2(5) . . . . ? C27 C28 C29 N3 -174.8(3) . . . . ? C28 C29 C30 C31 -0.9(5) . . . . ? N3 C29 C30 C31 177.1(3) . . . . ? C29 C30 C31 C26 0.6(5) . . . . ? C23 C26 C31 C30 -174.3(3) . . . . ? C27 C26 C31 C30 -2.4(5) . . . . ? N4 C33 C34 N3 0.2(4) . . . . ? N2 C17 N1 C18 1.0(4) . . . . ? N2 C17 N1 Ni2 164.0(2) . . . . ? C19 C18 N1 C17 -0.9(4) . . . . ? C19 C18 N1 Ni2 -163.8(2) . . . . ? C18 C19 N2 C17 0.2(4) . . . . ? C18 C19 N2 C20 175.6(3) . . . . ? N1 C17 N2 C19 -0.8(4) . . . . ? N1 C17 N2 C20 -176.3(3) . . . . ? C25 C20 N2 C19 -127.4(5) . . . . ? C21 C20 N2 C19 54.8(5) . . . . ? C25 C20 N2 C17 47.2(5) . . . . ? C21 C20 N2 C17 -130.7(4) . . . . ? N4 C32 N3 C34 -0.5(4) . . . . ? N4 C32 N3 C29 178.6(3) . . . . ? C33 C34 N3 C32 0.2(4) . . . . ? C33 C34 N3 C29 -178.9(3) . . . . ? C28 C29 N3 C32 21.5(5) . . . . ? C30 C29 N3 C32 -156.5(3) . . . . ? C28 C29 N3 C34 -159.6(3) . . . . ? C30 C29 N3 C34 22.3(5) . . . . ? N3 C32 N4 C33 0.6(4) . . . . ? N3 C32 N4 Ni2 174.2(2) . . . 7_655 ? C34 C33 N4 C32 -0.5(4) . . . . ? C34 C33 N4 Ni2 -173.7(2) . . . 7_655 ? C17 N1 Ni2 O8 -167.7(3) . . . . ? C18 N1 Ni2 O8 -8.2(3) . . . . ? C17 N1 Ni2 N4 102.0(3) . . . 7_645 ? C18 N1 Ni2 N4 -98.5(3) . . . 7_645 ? C17 N1 Ni2 O5 -73.6(3) . . . 17_756 ? C18 N1 Ni2 O5 86.0(3) . . . 17_756 ? C17 N1 Ni2 O1 -88.1(5) . . . . ? C18 N1 Ni2 O1 71.5(6) . . . . ? C17 N1 Ni2 O1W 23.5(3) . . . . ? C18 N1 Ni2 O1W -176.9(3) . . . . ? O2 C7 O1 Ni1 135.6(3) . . . . ? C1 C7 O1 Ni1 -45.9(4) . . . . ? O2 C7 O1 Ni2 5.0(4) . . . . ? C1 C7 O1 Ni2 -176.47(19) . . . . ? O7 Ni1 O1 C7 -28.1(3) 17_756 . . . ? O7 Ni1 O1 C7 151.9(3) . . . . ? O5 Ni1 O1 C7 62.5(3) . . . . ? O5 Ni1 O1 C7 -117.5(3) 17_756 . . . ? O7 Ni1 O1 Ni2 111.56(9) 17_756 . . . ? O7 Ni1 O1 Ni2 -68.44(9) . . . . ? O5 Ni1 O1 Ni2 -157.93(9) . . . . ? O5 Ni1 O1 Ni2 22.07(9) 17_756 . . . ? O8 Ni2 O1 C7 -145.6(2) . . . . ? N4 Ni2 O1 C7 -55.4(2) 7_645 . . . ? N1 Ni2 O1 C7 134.7(4) . . . . ? O5 Ni2 O1 C7 119.8(2) 17_756 . . . ? O1W Ni2 O1 C7 23.6(2) . . . . ? O8 Ni2 O1 Ni1 72.31(9) . . . . ? N4 Ni2 O1 Ni1 162.56(10) 7_645 . . . ? N1 Ni2 O1 Ni1 -7.4(5) . . . . ? O5 Ni2 O1 Ni1 -22.24(9) 17_756 . . . ? O1W Ni2 O1 Ni1 -118.49(9) . . . . ? O6 C15 O5 Ni2 -5.7(4) . . . 17_756 ? C14 C15 O5 Ni2 175.4(2) . . . 17_756 ? O6 C15 O5 Ni1 115.5(3) . . . . ? C14 C15 O5 Ni1 -63.4(4) . . . . ? O7 Ni1 O5 C15 164.2(3) 17_756 . . . ? O7 Ni1 O5 C15 -15.8(3) . . . . ? O1 Ni1 O5 C15 -106.5(3) 17_756 . . . ? O1 Ni1 O5 C15 73.5(3) . . . . ? O7 Ni1 O5 Ni2 -67.00(10) 17_756 . . 17_756 ? O7 Ni1 O5 Ni2 113.00(10) . . . 17_756 ? O1 Ni1 O5 Ni2 22.39(9) 17_756 . . 17_756 ? O1 Ni1 O5 Ni2 -157.61(9) . . . 17_756 ? O8 C16 O7 Ni1 7.7(5) . . . . ? C12 C16 O7 Ni1 -172.7(2) 2_645 . . . ? O5 Ni1 O7 C16 134.8(3) . . . . ? O5 Ni1 O7 C16 -45.2(3) 17_756 . . . ? O1 Ni1 O7 C16 -147.2(3) 17_756 . . . ? O1 Ni1 O7 C16 32.8(3) . . . . ? O7 C16 O8 Ni2 -1.1(5) . . . . ? C12 C16 O8 Ni2 179.2(2) 2_645 . . . ? N4 Ni2 O8 C16 -139.2(3) 7_645 . . . ? N1 Ni2 O8 C16 124.7(3) . . . . ? O5 Ni2 O8 C16 35.3(3) 17_756 . . . ? O1 Ni2 O8 C16 -42.7(3) . . . . ? O1W Ni2 O8 C16 -150.9(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.414 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.059 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 828138' #TrackingRef '- new-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H78 N16 Ni2 O19' _chemical_formula_weight 1636.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 8.9784(18) _cell_length_b 15.352(3) _cell_length_c 27.656(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.26(3) _cell_angle_gamma 90.00 _cell_volume 3781.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description green _exptl_crystal_colour plate _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27433 _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7345 _reflns_number_gt 6072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _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^)+(0.0017P)^2^+14.0113P] 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 7345 _refine_ls_number_parameters 546 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1561 _refine_ls_R_factor_gt 0.1312 _refine_ls_wR_factor_ref 0.1974 _refine_ls_wR_factor_gt 0.1891 _refine_ls_goodness_of_fit_ref 1.384 _refine_ls_restrained_S_all 1.383 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N3 N 1.3289(6) 1.4663(3) 0.64382(19) 0.0295(13) Uani 1 1 d . . . C10 C 1.3204(8) 1.3870(4) 0.6609(2) 0.0311(16) Uani 1 1 d G . . N4 N 1.1777(6) 1.3570(4) 0.6569(2) 0.0338(14) Uani 1 1 d . . . C13 C 1.1320(8) 1.2705(5) 0.6667(3) 0.0377(18) Uani 1 1 d . A . C14 C 1.2274(10) 1.2127(5) 0.6909(4) 0.070(3) Uani 1 1 d . . . C15 C 1.1840(9) 1.1271(5) 0.6966(4) 0.064(3) Uani 1 1 d . A . C16 C 1.0438(8) 1.0989(5) 0.6793(3) 0.0431(19) Uani 1 1 d D . . C4 C 0.9003(11) 0.8337(5) 0.6805(4) 0.041(4) Uani 0.823(7) 1 d PD A 1 C5 C 1.0149(11) 0.8616(6) 0.7136(4) 0.042(3) Uani 0.823(7) 1 d PD A 1 H5A H 1.0624 0.8228 0.7364 0.050 Uiso 0.823(7) 1 calc PR A 1 C6 C 1.0612(11) 0.9480(6) 0.7136(4) 0.046(3) Uani 0.823(7) 1 d PD A 1 H6A H 1.1388 0.9671 0.7366 0.055 Uiso 0.823(7) 1 calc PR A 1 C7 C 0.9924(12) 1.0055(5) 0.6794(5) 0.041(4) Uani 0.823(7) 1 d PD A 1 C8 C 0.8730(11) 0.9762(6) 0.6466(4) 0.049(3) Uani 0.823(7) 1 d PD A 1 H8A H 0.8221 1.0148 0.6244 0.059 Uiso 0.823(7) 1 calc PR A 1 C9 C 0.8298(11) 0.8900(6) 0.6467(3) 0.046(3) Uani 0.823(7) 1 d PD A 1 H9F H 0.7525 0.8702 0.6238 0.055 Uiso 0.823(7) 1 calc PR A 1 C4' C 0.916(5) 0.828(2) 0.696(3) 0.041(4) Uani 0.177(7) 1 d PGD A 2 C5' C 1.057(4) 0.850(3) 0.6886(19) 0.042(3) Uani 0.177(7) 1 d PGD A 2 H5B H 1.1262 0.8071 0.6830 0.050 Uiso 0.177(7) 1 calc PR A 2 C6' C 1.101(5) 0.938(2) 0.6895(18) 0.046(3) Uani 0.177(7) 1 d PD A 2 H6B H 1.2007 0.9506 0.6867 0.055 Uiso 0.177(7) 1 calc PR A 2 C7' C 1.006(6) 1.0077(18) 0.694(3) 0.041(4) Uani 0.177(7) 1 d PD A 2 C8' C 0.874(4) 0.977(2) 0.7102(16) 0.049(3) Uani 0.177(7) 1 d PD A 2 H8B H 0.8094 1.0189 0.7202 0.059 Uiso 0.177(7) 1 calc PR A 2 C9' C 0.829(5) 0.891(2) 0.7127(15) 0.046(3) Uani 0.177(7) 1 d PD A 2 H9G H 0.7420 0.8769 0.7257 0.055 Uiso 0.177(7) 1 calc PR A 2 Ni1 Ni 0.51843(10) 0.54857(5) 0.65102(3) 0.0252(2) Uani 1 1 d . . . C1 C 0.7107(8) 0.7156(4) 0.6692(3) 0.0357(17) Uani 1 1 d . A . H1 H 0.6273 0.7518 0.6636 0.043 Uiso 1 1 calc R . . C2 C 0.8512(8) 0.6014(5) 0.6775(3) 0.0402(18) Uani 1 1 d . . . H2 H 0.8816 0.5435 0.6784 0.048 Uiso 1 1 calc R . . C3 C 0.9443(9) 0.6711(5) 0.6863(3) 0.046(2) Uani 1 1 d . A . H3 H 1.0480 0.6699 0.6945 0.055 Uiso 1 1 calc R . . H10 H 1.4030 1.3551 0.6741 0.055 Uiso 1 1 d R . . C11 C 1.1824(8) 1.4893(5) 0.6281(3) 0.048(2) Uani 1 1 d . . . H11 H 1.1523 1.5427 0.6143 0.057 Uiso 1 1 calc R . . C12 C 1.0891(9) 1.4232(5) 0.6356(3) 0.053(2) Uani 1 1 d . . . H12 H 0.9853 1.4225 0.6280 0.063 Uiso 1 1 calc R . . H14 H 1.3215 1.2308 0.7045 0.063 Uiso 1 1 d R . . H15 H 1.2520 1.0879 0.7126 0.063 Uiso 1 1 d R . . C17 C 0.9473(11) 1.1608(6) 0.6605(5) 0.110(5) Uani 1 1 d . A . H17 H 0.8472 1.1456 0.6518 0.132 Uiso 1 1 calc R . . C18 C 0.9900(10) 1.2457(6) 0.6536(5) 0.104(5) Uani 1 1 d . . . H18 H 0.9196 1.2859 0.6397 0.124 Uiso 1 1 calc R A . C19 C 0.3098(10) 0.6611(5) 0.5208(3) 0.058(3) Uani 1 1 d . . . H19 H 0.2809 0.6576 0.4874 0.069 Uiso 1 1 calc R . . C20 C 0.3925(10) 0.6029(5) 0.5485(3) 0.049(2) Uani 1 1 d . . . H20 H 0.4317 0.5520 0.5369 0.058 Uiso 1 1 calc R . . C21 C 0.3408(8) 0.7037(4) 0.5963(2) 0.0353(17) Uani 1 1 d . . . H21 H 0.3357 0.7371 0.6242 0.042 Uiso 1 1 calc R . . C22 C 0.1933(8) 0.8045(4) 0.5374(3) 0.0361(17) Uani 1 1 d . . . C23 C 0.1810(10) 0.8703(5) 0.5698(3) 0.052(2) Uani 1 1 d . . . H23 H 0.2232 0.8642 0.6021 0.062 Uiso 1 1 calc R . . C24 C 0.1059(9) 0.9459(5) 0.5546(3) 0.049(2) Uani 1 1 d . . . H24 H 0.1005 0.9902 0.5773 0.059 Uiso 1 1 calc R . . C25 C 0.0388(9) 0.9588(5) 0.5079(3) 0.046(2) Uani 1 1 d . . . C26 C 0.0517(13) 0.8904(6) 0.4758(4) 0.086(4) Uani 1 1 d . . . H26 H 0.0073 0.8959 0.4437 0.103 Uiso 1 1 calc R . . C27 C 0.1281(12) 0.8141(6) 0.4899(3) 0.082(4) Uani 1 1 d . . . H27 H 0.1354 0.7698 0.4674 0.099 Uiso 1 1 calc R . . C28 C 0.5117(10) 0.4594(5) 0.8198(3) 0.045(2) Uani 1 1 d . . . C29 C 0.4883(9) 0.5259(4) 0.8587(2) 0.0371(18) Uani 1 1 d . . . C30 C 0.5060(9) 0.4997(4) 0.9070(2) 0.0404(19) Uani 1 1 d . . . H30 H 0.5302 0.4422 0.9151 0.049 Uiso 1 1 calc R . . C31 C 0.4876(9) 0.5592(5) 0.9432(2) 0.0394(18) Uani 1 1 d . . . C32 C 0.4526(9) 0.6449(5) 0.9317(2) 0.0380(18) Uani 1 1 d . . . H32 H 0.4441 0.6848 0.9565 0.046 Uiso 1 1 calc R . . C33 C 0.3816(8) 0.7648(4) 0.8715(3) 0.0356(17) Uani 1 1 d . . . C34 C 0.4300(8) 0.6717(4) 0.8834(2) 0.0319(16) Uani 1 1 d . . . C35 C 0.4493(9) 0.6115(4) 0.8473(2) 0.0387(19) Uani 1 1 d . . . H35 H 0.4359 0.6289 0.8148 0.046 Uiso 1 1 calc R . . C36 C 0.2233(14) 0.2097(7) 0.9517(4) 0.095(4) Uani 1 1 d . . . H36A H 0.1684 0.1866 0.9225 0.142 Uiso 1 1 calc R . . H36B H 0.3285 0.2107 0.9484 0.142 Uiso 1 1 calc R . . H36C H 0.1894 0.2678 0.9570 0.142 Uiso 1 1 calc R . . C37 C 0.2448(14) 0.1921(8) 1.0391(3) 0.101(4) Uani 1 1 d . . . H37A H 0.2106 0.1547 1.0633 0.151 Uiso 1 1 calc R . . H37B H 0.2020 0.2491 1.0414 0.151 Uiso 1 1 calc R . . H37C H 0.3523 0.1962 1.0446 0.151 Uiso 1 1 calc R . . C38 C 0.1517(10) 0.0749(6) 0.9852(4) 0.060(2) Uani 1 1 d . . . H38 H 0.1365 0.0437 1.0130 0.072 Uiso 1 1 calc R . . N1 N 0.7055(7) 0.6297(3) 0.6669(2) 0.0333(14) Uani 1 1 d . . . N2 N 0.8535(7) 0.7438(4) 0.6807(2) 0.0393(15) Uani 1 1 d D . . N5 N 0.4111(6) 0.6291(3) 0.59629(19) 0.0294(13) Uani 1 1 d . . . N6 N 0.2759(7) 0.7269(4) 0.5510(2) 0.0366(15) Uani 1 1 d . . . N7 N 0.5090(8) 0.5386(4) 0.9943(2) 0.0440(16) Uani 1 1 d . . . N8 N 0.1993(9) 0.1569(5) 0.9915(3) 0.058(2) Uani 1 1 d . . . O1 O 0.4130(6) 0.6023(3) 0.70634(16) 0.0426(13) Uani 1 1 d . . . H1A H 0.4656 0.6442 0.7194 0.064 Uiso 1 1 d R . . H1B H 0.3275 0.6214 0.6942 0.064 Uiso 1 1 d R . . O2 O 0.6324(5) 0.4597(3) 0.69994(16) 0.0337(11) Uani 1 1 d . . . H2B H 0.5843 0.4539 0.7243 0.051 Uiso 1 1 d R . . H2C H 0.6385 0.4107 0.6861 0.051 Uiso 1 1 d R . . O3 O 0.6233(5) 0.4838(3) 0.59772(16) 0.0361(12) Uani 1 1 d . . . H3A H 0.7064 0.5087 0.5952 0.054 Uiso 1 1 d R . . H3B H 0.6391 0.4309 0.6060 0.054 Uiso 1 1 d R . . O4 O 0.4909(7) 0.4846(3) 0.77608(18) 0.0556(17) Uani 1 1 d . . . O5 O 0.5494(7) 0.3834(3) 0.83314(17) 0.0492(15) Uani 1 1 d . . . O6 O 0.3683(6) 0.7879(3) 0.82733(16) 0.0354(12) Uani 1 1 d . . . O7 O 0.3564(6) 0.8124(3) 0.90607(17) 0.0413(13) Uani 1 1 d . . . O8 O 0.1263(7) 0.0370(5) 0.9463(2) 0.0710(19) Uani 1 1 d . . . O9 O 0.6037(14) 0.2641(4) 0.7690(3) 0.127(4) Uani 1 1 d D . . H9A H 0.637(17) 0.273(8) 0.743(3) 0.190 Uiso 1 1 d D . . H9B H 0.612(17) 0.310(5) 0.784(4) 0.190 Uiso 1 1 d D . . O10 O 0.5748(18) 0.6074(8) 1.0221(4) 0.083(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N3 0.037(3) 0.020(3) 0.031(3) 0.002(2) 0.003(2) -0.001(2) C10 0.031(4) 0.028(4) 0.035(4) 0.004(3) 0.003(3) -0.001(3) N4 0.026(3) 0.024(3) 0.051(4) 0.003(3) 0.002(3) -0.001(2) C13 0.032(4) 0.031(4) 0.050(5) -0.004(4) 0.007(3) 0.000(3) C14 0.041(5) 0.029(4) 0.133(9) 0.017(5) -0.017(5) -0.017(4) C15 0.039(5) 0.030(4) 0.119(8) 0.019(5) -0.003(5) -0.005(4) C16 0.032(4) 0.035(4) 0.062(5) -0.006(4) 0.006(4) -0.015(3) C4 0.045(5) 0.022(4) 0.055(10) 0.000(5) 0.006(5) -0.017(4) C5 0.043(6) 0.032(5) 0.048(7) 0.010(5) -0.008(5) -0.011(4) C6 0.047(6) 0.039(5) 0.047(7) 0.006(5) -0.011(5) -0.021(5) C7 0.038(5) 0.019(4) 0.067(11) -0.005(5) 0.009(6) -0.013(3) C8 0.050(6) 0.030(5) 0.064(6) 0.015(5) -0.013(5) -0.015(4) C9 0.051(6) 0.028(5) 0.053(6) 0.011(4) -0.011(5) -0.017(4) C4' 0.045(5) 0.022(4) 0.055(10) 0.000(5) 0.006(5) -0.017(4) C5' 0.043(6) 0.032(5) 0.048(7) 0.010(5) -0.008(5) -0.011(4) C6' 0.047(6) 0.039(5) 0.047(7) 0.006(5) -0.011(5) -0.021(5) C7' 0.038(5) 0.019(4) 0.067(11) -0.005(5) 0.009(6) -0.013(3) C8' 0.050(6) 0.030(5) 0.064(6) 0.015(5) -0.013(5) -0.015(4) C9' 0.051(6) 0.028(5) 0.053(6) 0.011(4) -0.011(5) -0.017(4) Ni1 0.0324(5) 0.0161(4) 0.0261(4) 0.0027(4) 0.0004(3) -0.0009(4) C1 0.038(4) 0.027(4) 0.042(4) 0.004(3) 0.006(3) -0.005(3) C2 0.042(5) 0.027(4) 0.052(5) 0.003(4) 0.005(4) -0.003(3) C3 0.035(5) 0.036(4) 0.065(6) 0.001(4) 0.002(4) -0.013(4) C11 0.036(5) 0.030(4) 0.074(6) 0.007(4) -0.005(4) 0.004(3) C12 0.034(5) 0.039(5) 0.082(6) 0.007(4) -0.005(4) 0.004(4) C17 0.033(6) 0.051(6) 0.229(15) 0.020(8) -0.049(7) -0.021(5) C18 0.038(6) 0.039(5) 0.220(14) 0.032(7) -0.037(7) -0.011(4) C19 0.091(7) 0.043(5) 0.036(5) 0.001(4) -0.006(4) 0.031(5) C20 0.079(6) 0.038(4) 0.026(4) -0.003(3) -0.006(4) 0.026(4) C21 0.047(5) 0.025(4) 0.031(4) -0.006(3) -0.003(3) 0.009(3) C22 0.033(4) 0.024(4) 0.048(5) 0.005(3) -0.004(3) 0.000(3) C23 0.070(6) 0.038(5) 0.047(5) 0.016(4) 0.004(4) 0.026(4) C24 0.068(6) 0.033(4) 0.046(5) 0.006(4) 0.007(4) 0.020(4) C25 0.042(5) 0.030(4) 0.062(5) 0.012(4) -0.009(4) 0.009(4) C26 0.127(10) 0.046(6) 0.070(7) -0.004(5) -0.048(6) 0.037(6) C27 0.126(10) 0.043(5) 0.064(6) -0.012(5) -0.044(6) 0.039(6) C28 0.080(6) 0.024(4) 0.030(4) 0.004(3) 0.009(4) 0.000(4) C29 0.064(5) 0.022(4) 0.025(4) -0.003(3) 0.008(4) -0.002(3) C30 0.069(6) 0.023(4) 0.029(4) 0.006(3) 0.005(4) 0.004(4) C31 0.058(5) 0.037(4) 0.021(4) -0.001(3) -0.002(3) 0.006(4) C32 0.059(5) 0.033(4) 0.021(4) -0.005(3) 0.002(3) -0.005(4) C33 0.049(5) 0.020(4) 0.037(4) 0.004(3) 0.002(3) -0.003(3) C34 0.048(5) 0.018(3) 0.030(4) -0.001(3) 0.004(3) -0.003(3) C35 0.066(6) 0.027(4) 0.022(4) 0.000(3) 0.003(4) -0.004(4) C36 0.128(11) 0.088(9) 0.073(8) -0.007(7) 0.034(7) 0.009(8) C37 0.142(12) 0.104(9) 0.049(6) 0.005(6) -0.012(7) 0.044(8) C38 0.058(6) 0.064(7) 0.058(6) 0.002(5) 0.003(5) 0.008(5) N1 0.042(4) 0.021(3) 0.036(3) 0.000(3) 0.004(3) -0.004(3) N2 0.040(4) 0.023(3) 0.054(4) -0.001(3) 0.002(3) -0.008(3) N5 0.041(4) 0.020(3) 0.026(3) 0.003(2) 0.000(2) 0.000(2) N6 0.042(4) 0.024(3) 0.042(4) 0.005(3) -0.004(3) 0.008(3) N7 0.069(5) 0.036(4) 0.026(3) 0.005(3) 0.003(3) 0.016(4) N8 0.070(5) 0.058(5) 0.045(4) 0.005(4) 0.010(4) 0.005(4) O1 0.060(4) 0.031(3) 0.037(3) -0.005(2) 0.008(3) 0.000(3) O2 0.047(3) 0.020(2) 0.033(3) 0.001(2) -0.001(2) -0.002(2) O3 0.050(3) 0.020(2) 0.041(3) 0.002(2) 0.013(2) 0.004(2) O4 0.115(5) 0.026(3) 0.026(3) -0.001(2) 0.012(3) 0.009(3) O5 0.092(5) 0.024(3) 0.031(3) -0.002(2) 0.002(3) 0.013(3) O6 0.053(3) 0.022(2) 0.031(3) 0.001(2) 0.003(2) -0.003(2) O7 0.071(4) 0.020(2) 0.035(3) -0.006(2) 0.014(3) 0.000(2) O8 0.069(4) 0.084(5) 0.061(4) 0.032(4) 0.015(4) 0.007(4) O9 0.311(13) 0.019(3) 0.068(5) -0.009(3) 0.091(7) -0.023(5) O10 0.149(14) 0.047(8) 0.051(8) -0.007(6) 0.001(8) -0.014(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N3 C10 1.311(8) . ? N3 C11 1.378(9) . ? N3 Ni1 2.108(5) 1_665 ? C10 N4 1.353(8) . ? C10 H10 0.9251 . ? N4 C12 1.376(9) . ? N4 C13 1.426(8) . ? C13 C18 1.336(11) . ? C13 C14 1.352(11) . ? C14 C15 1.384(10) . ? C14 H14 0.9229 . ? C15 C16 1.360(10) . ? C15 H15 0.9295 . ? C16 C17 1.345(12) . ? C16 C7 1.507(10) . ? C16 C7' 1.51(2) . ? C4 C5 1.357(12) . ? C4 C9 1.369(13) . ? C4 N2 1.442(9) . ? C5 C6 1.391(11) . ? C5 H5A 0.9300 . ? C6 C7 1.381(13) . ? C6 H6A 0.9300 . ? C7 C8 1.389(14) . ? C8 C9 1.379(11) . ? C8 H8A 0.9300 . ? C9 H9F 0.9300 . ? C4' C5' 1.36(2) . ? C4' C9' 1.37(2) . ? C4' N2 1.443(19) . ? C5' C6' 1.41(2) . ? C5' H5B 0.9300 . ? C6' C7' 1.38(2) . ? C6' H6B 0.9300 . ? C7' C8' 1.39(2) . ? C8' C9' 1.38(2) . ? C8' H8B 0.9300 . ? C9' H9G 0.9300 . ? Ni1 O1 2.070(5) . ? Ni1 N1 2.093(6) . ? Ni1 N5 2.093(5) . ? Ni1 O2 2.095(4) . ? Ni1 O3 2.097(4) . ? Ni1 N3 2.108(5) 1_445 ? C1 N1 1.321(8) . ? C1 N2 1.353(9) . ? C1 H1 0.9300 . ? C2 C3 1.360(9) . ? C2 N1 1.375(9) . ? C2 H2 0.9300 . ? C3 N2 1.379(9) . ? C3 H3 0.9300 . ? C11 C12 1.349(10) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C17 C18 1.380(12) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.338(10) . ? C19 N6 1.370(9) . ? C19 H19 0.9300 . ? C20 N5 1.372(8) . ? C20 H20 0.9300 . ? C21 N5 1.308(8) . ? C21 N6 1.360(8) . ? C21 H21 0.9300 . ? C22 C23 1.363(10) . ? C22 C27 1.378(10) . ? C22 N6 1.429(8) . ? C23 C24 1.380(9) . ? C23 H23 0.9300 . ? C24 C25 1.369(10) . ? C24 H24 0.9300 . ? C25 C26 1.389(12) . ? C25 C25 1.484(13) 3_576 ? C26 C27 1.388(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O5 1.258(8) . ? C28 O4 1.259(8) . ? C28 C29 1.518(9) . ? C29 C30 1.385(9) . ? C29 C35 1.386(9) . ? C30 C31 1.378(9) . ? C30 H30 0.9300 . ? C31 C32 1.379(9) . ? C31 N7 1.438(8) . ? C32 C34 1.388(9) . ? C32 H32 0.9300 . ? C33 O7 1.246(8) . ? C33 O6 1.263(8) . ? C33 C34 1.518(9) . ? C34 C35 1.389(9) . ? C35 H35 0.9300 . ? C36 N8 1.406(11) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N8 1.434(11) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 O8 1.219(10) . ? C38 N8 1.335(11) . ? C38 H38 0.9300 . ? N7 N7 1.241(11) 3_667 ? N7 O10 1.394(13) . ? O1 H1A 0.8500 . ? O1 H1B 0.8499 . ? O2 H2B 0.8498 . ? O2 H2C 0.8500 . ? O3 H3A 0.8500 . ? O3 H3B 0.8499 . ? O9 H9A 0.82(11) . ? O9 H9B 0.82(9) . ? 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 C10 N3 C11 104.8(6) . . ? C10 N3 Ni1 127.2(5) . 1_665 ? C11 N3 Ni1 127.1(5) . 1_665 ? N3 C10 N4 112.6(6) . . ? N3 C10 H10 123.7 . . ? N4 C10 H10 123.7 . . ? C10 N4 C12 105.8(6) . . ? C10 N4 C13 126.5(6) . . ? C12 N4 C13 127.2(6) . . ? C18 C13 C14 118.1(8) . . ? C18 C13 N4 120.1(7) . . ? C14 C13 N4 121.7(7) . . ? C13 C14 C15 120.6(8) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 121.5(8) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.5 . . ? C17 C16 C15 115.8(7) . . ? C17 C16 C7 119.4(8) . . ? C15 C16 C7 124.9(8) . . ? C17 C16 C7' 127(2) . . ? C15 C16 C7' 115(3) . . ? C7 C16 C7' 16(4) . . ? C5 C4 C9 120.4(8) . . ? C5 C4 N2 119.7(9) . . ? C9 C4 N2 119.9(8) . . ? C4 C5 C6 120.1(9) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C7 C6 C5 120.2(9) . . ? C7 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? C6 C7 C8 118.8(8) . . ? C6 C7 C16 120.0(9) . . ? C8 C7 C16 121.2(9) . . ? C9 C8 C7 120.2(9) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C4 C9 C8 120.2(9) . . ? C4 C9 H9F 119.9 . . ? C8 C9 H9F 119.9 . . ? C5' C4' C9' 117(3) . . ? C5' C4' N2 121(3) . . ? C9' C4' N2 121(3) . . ? C4' C5' C6' 120(4) . . ? C4' C5' H5B 119.8 . . ? C6' C5' H5B 119.8 . . ? C7' C6' C5' 125(4) . . ? C7' C6' H6B 117.6 . . ? C5' C6' H6B 117.6 . . ? C6' C7' C8' 109(3) . . ? C6' C7' C16 122(3) . . ? C8' C7' C16 129(3) . . ? C9' C8' C7' 127(4) . . ? C9' C8' H8B 116.6 . . ? C7' C8' H8B 116.6 . . ? C4' C9' C8' 119(4) . . ? C4' C9' H9G 120.6 . . ? C8' C9' H9G 120.6 . . ? O1 Ni1 N1 92.1(2) . . ? O1 Ni1 N5 95.0(2) . . ? N1 Ni1 N5 94.9(2) . . ? O1 Ni1 O2 90.79(19) . . ? N1 Ni1 O2 86.5(2) . . ? N5 Ni1 O2 174.0(2) . . ? O1 Ni1 O3 175.15(18) . . ? N1 Ni1 O3 90.6(2) . . ? N5 Ni1 O3 88.77(19) . . ? O2 Ni1 O3 85.37(18) . . ? O1 Ni1 N3 82.5(2) . 1_445 ? N1 Ni1 N3 173.3(2) . 1_445 ? N5 Ni1 N3 89.6(2) . 1_445 ? O2 Ni1 N3 89.62(19) . 1_445 ? O3 Ni1 N3 94.5(2) . 1_445 ? N1 C1 N2 110.9(7) . . ? N1 C1 H1 124.5 . . ? N2 C1 H1 124.5 . . ? C3 C2 N1 109.7(7) . . ? C3 C2 H2 125.2 . . ? N1 C2 H2 125.2 . . ? C2 C3 N2 106.0(7) . . ? C2 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? C12 C11 N3 110.2(7) . . ? C12 C11 H11 124.9 . . ? N3 C11 H11 124.9 . . ? C11 C12 N4 106.6(7) . . ? C11 C12 H12 126.7 . . ? N4 C12 H12 126.7 . . ? C16 C17 C18 123.0(8) . . ? C16 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C13 C18 C17 120.2(9) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 N6 107.1(7) . . ? C20 C19 H19 126.5 . . ? N6 C19 H19 126.5 . . ? C19 C20 N5 110.2(7) . . ? C19 C20 H20 124.9 . . ? N5 C20 H20 124.9 . . ? N5 C21 N6 112.2(6) . . ? N5 C21 H21 123.9 . . ? N6 C21 H21 123.9 . . ? C23 C22 C27 119.2(7) . . ? C23 C22 N6 121.8(7) . . ? C27 C22 N6 118.9(7) . . ? C22 C23 C24 120.0(8) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 123.2(8) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C24 C25 C26 115.5(7) . . ? C24 C25 C25 122.4(10) . 3_576 ? C26 C25 C25 122.0(9) . 3_576 ? C27 C26 C25 122.5(8) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C22 C27 C26 119.5(8) . . ? C22 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? O5 C28 O4 124.6(7) . . ? O5 C28 C29 118.1(6) . . ? O4 C28 C29 117.2(6) . . ? C30 C29 C35 119.3(6) . . ? C30 C29 C28 118.8(6) . . ? C35 C29 C28 121.9(6) . . ? C31 C30 C29 119.9(6) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.7(6) . . ? C30 C31 N7 123.6(6) . . ? C32 C31 N7 115.7(6) . . ? C31 C32 C34 120.3(6) . . ? C31 C32 H32 119.8 . . ? C34 C32 H32 119.8 . . ? O7 C33 O6 124.9(6) . . ? O7 C33 C34 117.4(6) . . ? O6 C33 C34 117.7(6) . . ? C32 C34 C35 118.6(6) . . ? C32 C34 C33 119.5(6) . . ? C35 C34 C33 121.9(6) . . ? C29 C35 C34 121.2(6) . . ? C29 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? N8 C36 H36A 109.5 . . ? N8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N8 C37 H37A 109.5 . . ? N8 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N8 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O8 C38 N8 126.0(10) . . ? O8 C38 H38 117.0 . . ? N8 C38 H38 117.0 . . ? C1 N1 C2 106.1(6) . . ? C1 N1 Ni1 128.8(5) . . ? C2 N1 Ni1 125.0(4) . . ? C1 N2 C3 107.2(6) . . ? C1 N2 C4 124.9(7) . . ? C3 N2 C4 127.3(7) . . ? C1 N2 C4' 132(2) . . ? C3 N2 C4' 119(2) . . ? C4 N2 C4' 17(3) . . ? C21 N5 C20 105.0(6) . . ? C21 N5 Ni1 134.0(5) . . ? C20 N5 Ni1 120.8(4) . . ? C21 N6 C19 105.5(6) . . ? C21 N6 C22 127.5(6) . . ? C19 N6 C22 127.0(6) . . ? N7 N7 O10 130.0(9) 3_667 . ? N7 N7 C31 117.0(8) 3_667 . ? O10 N7 C31 111.8(7) . . ? C38 N8 C36 121.3(9) . . ? C38 N8 C37 121.8(9) . . ? C36 N8 C37 116.6(9) . . ? Ni1 O1 H1A 109.5 . . ? Ni1 O1 H1B 108.7 . . ? H1A O1 H1B 109.5 . . ? Ni1 O2 H2B 109.0 . . ? Ni1 O2 H2C 109.9 . . ? H2B O2 H2C 109.5 . . ? Ni1 O3 H3A 108.8 . . ? Ni1 O3 H3B 109.8 . . ? H3A O3 H3B 109.5 . . ? H9A O9 H9B 106(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.723 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.086 #TrackingRef '- new-1.cif' data_081204bm _database_code_depnum_ccdc_archive 'CCDC 840687' #TrackingRef '- new-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H18 Cd O17, C18 H16 N4' _chemical_formula_sum 'C50 H34 Cd N4 O17' _chemical_formula_weight 1075.21 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.498(3) _cell_length_b 11.7312(11) _cell_length_c 12.4676(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.487(2) _cell_angle_gamma 90.00 _cell_volume 4149.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9196 _exptl_absorpt_correction_T_max 0.9408 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16659 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4306 _reflns_number_gt 3536 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0412P)^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 4306 _refine_ls_number_parameters 338 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.09019(3) -0.2500 0.02539(11) Uani 1 2 d S . . C1 C 0.07636(10) 0.1320(3) -0.0530(2) 0.0234(6) Uani 1 1 d . . . C2 C 0.12101(10) 0.1001(2) 0.0162(2) 0.0206(6) Uani 1 1 d . . . C3 C 0.07614(10) -0.0115(2) 0.1491(2) 0.0214(6) Uani 1 1 d . . . C4 C 0.12092(10) 0.0306(2) 0.1069(2) 0.0197(6) Uani 1 1 d . . . C5 C 0.16348(10) 0.0023(2) 0.1643(2) 0.0214(6) Uani 1 1 d . . . H5 H 0.1633 -0.0437 0.2250 0.026 Uiso 1 1 calc R . . C6 C 0.20629(10) 0.0405(2) 0.1337(2) 0.0202(6) Uani 1 1 d . . . C7 C 0.20588(10) 0.1085(2) 0.0427(2) 0.0246(7) Uani 1 1 d . . . H7 H 0.2342 0.1345 0.0203 0.030 Uiso 1 1 calc R . . C8 C 0.16378(10) 0.1382(2) -0.0151(2) 0.0226(6) Uani 1 1 d . . . H8 H 0.1641 0.1843 -0.0757 0.027 Uiso 1 1 calc R . . C9 C 0.25115(9) 0.0032(2) 0.1945(2) 0.0204(6) Uani 1 1 d . . . C10 C 0.25506(10) -0.1074(2) 0.2349(2) 0.0272(7) Uani 1 1 d . . . H10 H 0.2291 -0.1557 0.2273 0.033 Uiso 1 1 calc R . . C11 C 0.29716(10) -0.1459(3) 0.2859(2) 0.0282(7) Uani 1 1 d . . . H11 H 0.2992 -0.2205 0.3111 0.034 Uiso 1 1 calc R . . C12 C 0.37944(10) -0.1323(2) 0.3573(3) 0.0258(7) Uani 1 1 d . . . C13 C 0.33639(10) -0.0762(2) 0.3007(2) 0.0233(6) Uani 1 1 d . . . C14 C 0.37409(11) 0.1149(3) 0.2841(2) 0.0268(7) Uani 1 1 d . . . C15 C 0.33298(10) 0.0355(2) 0.2629(2) 0.0215(6) Uani 1 1 d . . . C16 C 0.29042(10) 0.0733(2) 0.2100(2) 0.0227(6) Uani 1 1 d . . . H16 H 0.2883 0.1478 0.1844 0.027 Uiso 1 1 calc R . . C17 C 0.15417(11) 0.6270(3) 0.9811(2) 0.0303(7) Uani 1 1 d . . . H17 H 0.1402 0.5571 0.9935 0.036 Uiso 1 1 calc R . . C18 C 0.20162(10) 0.6405(3) 1.0050(2) 0.0290(7) Uani 1 1 d . . . H18 H 0.2194 0.5795 1.0342 0.035 Uiso 1 1 calc R . . C19 C 0.22417(10) 0.7430(2) 0.9868(2) 0.0251(7) Uani 1 1 d . . . C20 C 0.19585(11) 0.8303(3) 0.9394(3) 0.0330(8) Uani 1 1 d . . . H20 H 0.2098 0.8990 0.9231 0.040 Uiso 1 1 calc R . . C21 C 0.14775(11) 0.8175(3) 0.9161(3) 0.0326(8) Uani 1 1 d . . . H21 H 0.1297 0.8772 0.8853 0.039 Uiso 1 1 calc R . . C22 C 0.12673(10) 0.7160(2) 0.9387(2) 0.0249(7) Uani 1 1 d . . . C23 C 0.05344(12) 0.5974(3) 0.9072(3) 0.0396(8) Uani 1 1 d . . . H23 H 0.0673 0.5256 0.9134 0.048 Uiso 1 1 calc R . . C24 C 0.04432(11) 0.7828(3) 0.9035(3) 0.0317(7) Uani 1 1 d . . . H24 H 0.0502 0.8607 0.9069 0.038 Uiso 1 1 calc R . . C25 C 0.00753(12) 0.6197(3) 0.8860(3) 0.0397(9) Uani 1 1 d . . . H25 H -0.0166 0.5664 0.8751 0.048 Uiso 1 1 calc R . . N1 N 0.07660(8) 0.7009(2) 0.9182(2) 0.0258(6) Uani 1 1 d . . . N2 N 0.00280(9) 0.7351(2) 0.8834(2) 0.0347(6) Uani 1 1 d D . . H2 H -0.0237(6) 0.770(2) 0.874(3) 0.042 Uiso 1 1 d D . . O1 O 0.05263(7) 0.05354(17) -0.09813(17) 0.0320(5) Uani 1 1 d . . . O2 O 0.06715(7) 0.23645(17) -0.06575(17) 0.0344(5) Uani 1 1 d . . . O3 O 0.07353(7) -0.11558(16) 0.17460(18) 0.0328(5) Uani 1 1 d . . . O4 O 0.04388(7) 0.05747(16) 0.16208(17) 0.0283(5) Uani 1 1 d . . . O5 O 0.40530(8) -0.1916(2) 0.31014(18) 0.0394(6) Uani 1 1 d . . . O6 O 0.38211(8) -0.12071(18) 0.46177(19) 0.0377(6) Uani 1 1 d D . . H6 H 0.3999(10) -0.169(2) 0.491(3) 0.045 Uiso 1 1 d D . . O7 O 0.41301(8) 0.08249(19) 0.3159(2) 0.0471(7) Uani 1 1 d . . . O8 O 0.36252(8) 0.22333(18) 0.26807(19) 0.0369(6) Uani 1 1 d D . . H8A H 0.3849(8) 0.265(2) 0.286(3) 0.044 Uiso 1 1 d D . . O9 O 0.0000 0.2821(3) -0.2500 0.0655(13) Uani 1 2 d SD . . H9B H -0.0257(7) 0.312(3) -0.254(4) 0.079 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 Cd1 0.01695(18) 0.02622(19) 0.03346(19) 0.000 0.00476(13) 0.000 C1 0.0188(16) 0.0308(17) 0.0200(15) 0.0024(12) -0.0013(12) -0.0013(13) C2 0.0157(15) 0.0200(15) 0.0249(15) -0.0009(12) -0.0045(11) -0.0007(12) C3 0.0173(15) 0.0242(16) 0.0219(15) 0.0009(12) -0.0026(12) 0.0008(12) C4 0.0175(15) 0.0173(14) 0.0238(15) -0.0010(12) -0.0014(12) 0.0002(12) C5 0.0196(16) 0.0222(15) 0.0219(15) 0.0041(12) 0.0005(12) 0.0025(12) C6 0.0170(15) 0.0195(14) 0.0234(15) -0.0034(12) -0.0013(12) 0.0016(12) C7 0.0187(16) 0.0227(16) 0.0322(16) 0.0005(13) 0.0020(12) -0.0044(12) C8 0.0214(16) 0.0223(15) 0.0234(15) 0.0052(12) -0.0017(12) -0.0014(12) C9 0.0134(15) 0.0242(16) 0.0232(15) 0.0000(12) -0.0006(11) 0.0018(12) C10 0.0196(16) 0.0236(16) 0.0375(18) 0.0041(13) -0.0010(13) -0.0043(13) C11 0.0240(17) 0.0219(16) 0.0374(18) 0.0071(13) -0.0039(14) 0.0015(13) C12 0.0184(16) 0.0212(15) 0.0362(18) 0.0010(13) -0.0054(13) -0.0028(13) C13 0.0162(15) 0.0263(16) 0.0268(15) -0.0018(12) -0.0005(12) 0.0022(12) C14 0.0240(17) 0.0287(17) 0.0272(16) 0.0011(13) -0.0010(13) -0.0039(13) C15 0.0150(15) 0.0231(15) 0.0259(15) -0.0002(12) 0.0001(12) -0.0001(12) C16 0.0215(16) 0.0196(15) 0.0260(15) 0.0014(12) -0.0021(12) 0.0033(12) C17 0.0254(18) 0.0290(17) 0.0367(18) 0.0080(14) 0.0033(14) -0.0003(14) C18 0.0231(17) 0.0292(17) 0.0346(18) 0.0073(14) 0.0017(13) 0.0052(14) C19 0.0251(16) 0.0266(16) 0.0237(15) -0.0025(12) 0.0017(13) 0.0018(13) C20 0.0308(19) 0.0199(16) 0.047(2) -0.0007(14) -0.0035(15) -0.0021(14) C21 0.0279(18) 0.0225(17) 0.045(2) 0.0007(14) -0.0072(15) 0.0029(14) C22 0.0228(16) 0.0282(17) 0.0234(15) -0.0018(12) 0.0006(12) 0.0009(13) C23 0.0285(19) 0.0259(17) 0.063(2) 0.0066(16) -0.0028(16) 0.0028(15) C24 0.0288(18) 0.0284(17) 0.0378(18) -0.0010(14) 0.0030(14) 0.0051(14) C25 0.0242(18) 0.0334(19) 0.060(2) 0.0085(16) -0.0027(16) -0.0008(15) N1 0.0192(13) 0.0248(13) 0.0328(14) 0.0017(11) -0.0008(11) 0.0009(11) N2 0.0197(15) 0.0384(17) 0.0452(17) 0.0047(13) -0.0013(13) 0.0075(13) O1 0.0262(12) 0.0291(12) 0.0376(13) -0.0027(10) -0.0126(10) -0.0071(9) O2 0.0323(13) 0.0245(12) 0.0421(13) 0.0007(10) -0.0186(10) 0.0019(10) O3 0.0247(12) 0.0224(12) 0.0531(14) 0.0106(10) 0.0123(10) 0.0018(9) O4 0.0172(11) 0.0251(11) 0.0429(13) 0.0047(9) 0.0045(9) 0.0033(9) O5 0.0262(13) 0.0495(15) 0.0418(14) -0.0028(11) -0.0014(11) 0.0146(11) O6 0.0419(15) 0.0307(13) 0.0372(13) -0.0023(10) -0.0135(11) 0.0146(11) O7 0.0172(12) 0.0414(14) 0.0795(19) 0.0010(13) -0.0111(12) -0.0009(11) O8 0.0274(13) 0.0249(12) 0.0555(15) 0.0056(11) -0.0110(11) -0.0094(10) O9 0.019(2) 0.033(2) 0.142(4) 0.000 -0.006(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O9 2.251(4) . ? Cd1 O1 2.340(2) . ? Cd1 O1 2.340(2) 2_554 ? Cd1 O3 2.396(2) 6 ? Cd1 O3 2.396(2) 5 ? Cd1 O4 2.455(2) 5 ? Cd1 O4 2.455(2) 6 ? C1 O1 1.245(3) . ? C1 O2 1.259(3) . ? C1 C2 1.515(4) . ? C2 C8 1.389(4) . ? C2 C4 1.394(4) . ? C3 O4 1.247(3) . ? C3 O3 1.265(3) . ? C3 C4 1.510(4) . ? C4 C5 1.388(4) . ? C5 C6 1.387(4) . ? C5 H5 0.9300 . ? C6 C7 1.385(4) . ? C6 C9 1.489(4) . ? C7 C8 1.383(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C16 1.387(4) . ? C9 C10 1.392(4) . ? C10 C11 1.379(4) . ? C10 H10 0.9300 . ? C11 C13 1.383(4) . ? C11 H11 0.9300 . ? C12 O5 1.206(3) . ? C12 O6 1.304(4) . ? C12 C13 1.507(4) . ? C13 C15 1.393(4) . ? C14 O7 1.203(3) . ? C14 O8 1.325(3) . ? C14 C15 1.500(4) . ? C15 C16 1.396(4) . ? C16 H16 0.9300 . ? C17 C18 1.366(4) . ? C17 C22 1.380(4) . ? C17 H17 0.9300 . ? C18 C19 1.393(4) . ? C18 H18 0.9300 . ? C19 C20 1.399(4) . ? C19 C19 1.486(6) 7_567 ? C20 C21 1.382(4) . ? C20 H20 0.9300 . ? C21 C22 1.374(4) . ? C21 H21 0.9300 . ? C22 N1 1.438(4) . ? C23 C25 1.335(4) . ? C23 N1 1.382(4) . ? C23 H23 0.9300 . ? C24 N2 1.311(4) . ? C24 N1 1.331(4) . ? C24 H24 0.9300 . ? C25 N2 1.361(4) . ? C25 H25 0.9300 . ? N2 H2 0.858(10) . ? O3 Cd1 2.396(2) 5 ? O4 Cd1 2.455(2) 5 ? O6 H6 0.824(10) . ? O8 H8A 0.820(10) . ? O9 H9B 0.810(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Cd1 O1 100.59(5) . . ? O9 Cd1 O1 100.59(5) . 2_554 ? O1 Cd1 O1 158.83(10) . 2_554 ? O9 Cd1 O3 82.86(5) . 6 ? O1 Cd1 O3 79.83(8) . 6 ? O1 Cd1 O3 102.84(8) 2_554 6 ? O9 Cd1 O3 82.86(5) . 5 ? O1 Cd1 O3 102.84(8) . 5 ? O1 Cd1 O3 79.83(8) 2_554 5 ? O3 Cd1 O3 165.72(9) 6 5 ? O9 Cd1 O4 134.87(5) . 5 ? O1 Cd1 O4 79.83(7) . 5 ? O1 Cd1 O4 85.26(7) 2_554 5 ? O3 Cd1 O4 139.89(7) 6 5 ? O3 Cd1 O4 53.89(6) 5 5 ? O9 Cd1 O4 134.87(5) . 6 ? O1 Cd1 O4 85.26(7) . 6 ? O1 Cd1 O4 79.83(7) 2_554 6 ? O3 Cd1 O4 53.89(6) 6 6 ? O3 Cd1 O4 139.89(7) 5 6 ? O4 Cd1 O4 90.25(9) 5 6 ? O1 C1 O2 124.4(3) . . ? O1 C1 C2 117.7(3) . . ? O2 C1 C2 117.8(2) . . ? C8 C2 C4 119.0(2) . . ? C8 C2 C1 118.2(2) . . ? C4 C2 C1 122.7(2) . . ? O4 C3 O3 122.1(3) . . ? O4 C3 C4 119.4(2) . . ? O3 C3 C4 118.4(2) . . ? C5 C4 C2 119.3(3) . . ? C5 C4 C3 117.9(2) . . ? C2 C4 C3 122.8(2) . . ? C6 C5 C4 121.9(3) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C7 C6 C5 118.2(3) . . ? C7 C6 C9 121.7(3) . . ? C5 C6 C9 120.0(2) . . ? C8 C7 C6 120.7(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C2 120.9(3) . . ? C7 C8 H8 119.5 . . ? C2 C8 H8 119.5 . . ? C16 C9 C10 117.8(3) . . ? C16 C9 C6 122.6(2) . . ? C10 C9 C6 119.6(2) . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C13 121.6(3) . . ? C10 C11 H11 119.2 . . ? C13 C11 H11 119.2 . . ? O5 C12 O6 124.5(3) . . ? O5 C12 C13 122.1(3) . . ? O6 C12 C13 112.9(3) . . ? C11 C13 C15 118.8(3) . . ? C11 C13 C12 114.6(2) . . ? C15 C13 C12 126.6(3) . . ? O7 C14 O8 124.1(3) . . ? O7 C14 C15 122.8(3) . . ? O8 C14 C15 113.0(2) . . ? C13 C15 C16 119.2(3) . . ? C13 C15 C14 119.8(3) . . ? C16 C15 C14 121.0(3) . . ? C9 C16 C15 122.0(3) . . ? C9 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C18 C17 C22 120.6(3) . . ? C18 C17 H17 119.7 . . ? C22 C17 H17 119.7 . . ? C17 C18 C19 121.8(3) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C18 C19 C20 116.4(3) . . ? C18 C19 C19 121.4(3) . 7_567 ? C20 C19 C19 122.2(3) . 7_567 ? C21 C20 C19 122.0(3) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C22 C21 C20 119.6(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C17 119.5(3) . . ? C21 C22 N1 121.1(3) . . ? C17 C22 N1 119.4(3) . . ? C25 C23 N1 107.3(3) . . ? C25 C23 H23 126.3 . . ? N1 C23 H23 126.3 . . ? N2 C24 N1 108.5(3) . . ? N2 C24 H24 125.7 . . ? N1 C24 H24 125.7 . . ? C23 C25 N2 107.0(3) . . ? C23 C25 H25 126.5 . . ? N2 C25 H25 126.5 . . ? C24 N1 C23 107.6(3) . . ? C24 N1 C22 126.7(3) . . ? C23 N1 C22 125.7(2) . . ? C24 N2 C25 109.5(3) . . ? C24 N2 H2 126(2) . . ? C25 N2 H2 124(2) . . ? C1 O1 Cd1 120.53(18) . . ? C3 O3 Cd1 93.05(16) . 5 ? C3 O4 Cd1 90.75(17) . 5 ? C12 O6 H6 110(2) . . ? C14 O8 H8A 111(2) . . ? Cd1 O9 H9B 116(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C8 116.3(3) . . . . ? O2 C1 C2 C8 -59.9(4) . . . . ? O1 C1 C2 C4 -61.1(4) . . . . ? O2 C1 C2 C4 122.7(3) . . . . ? C8 C2 C4 C5 0.6(4) . . . . ? C1 C2 C4 C5 178.0(3) . . . . ? C8 C2 C4 C3 177.9(3) . . . . ? C1 C2 C4 C3 -4.8(4) . . . . ? O4 C3 C4 C5 128.4(3) . . . . ? O3 C3 C4 C5 -48.7(4) . . . . ? O4 C3 C4 C2 -48.9(4) . . . . ? O3 C3 C4 C2 134.1(3) . . . . ? C2 C4 C5 C6 -0.4(4) . . . . ? C3 C4 C5 C6 -177.7(2) . . . . ? C4 C5 C6 C7 -0.3(4) . . . . ? C4 C5 C6 C9 -176.9(3) . . . . ? C5 C6 C7 C8 0.7(4) . . . . ? C9 C6 C7 C8 177.3(3) . . . . ? C6 C7 C8 C2 -0.4(4) . . . . ? C4 C2 C8 C7 -0.3(4) . . . . ? C1 C2 C8 C7 -177.7(3) . . . . ? C7 C6 C9 C16 37.7(4) . . . . ? C5 C6 C9 C16 -145.7(3) . . . . ? C7 C6 C9 C10 -140.0(3) . . . . ? C5 C6 C9 C10 36.5(4) . . . . ? C16 C9 C10 C11 -1.7(4) . . . . ? C6 C9 C10 C11 176.2(3) . . . . ? C9 C10 C11 C13 1.2(5) . . . . ? C10 C11 C13 C15 0.1(5) . . . . ? C10 C11 C13 C12 -179.6(3) . . . . ? O5 C12 C13 C11 82.3(4) . . . . ? O6 C12 C13 C11 -90.1(3) . . . . ? O5 C12 C13 C15 -97.4(4) . . . . ? O6 C12 C13 C15 90.2(4) . . . . ? C11 C13 C15 C16 -1.0(4) . . . . ? C12 C13 C15 C16 178.7(3) . . . . ? C11 C13 C15 C14 176.2(3) . . . . ? C12 C13 C15 C14 -4.1(4) . . . . ? O7 C14 C15 C13 13.3(5) . . . . ? O8 C14 C15 C13 -164.3(3) . . . . ? O7 C14 C15 C16 -169.6(3) . . . . ? O8 C14 C15 C16 12.8(4) . . . . ? C10 C9 C16 C15 0.8(4) . . . . ? C6 C9 C16 C15 -177.0(3) . . . . ? C13 C15 C16 C9 0.5(4) . . . . ? C14 C15 C16 C9 -176.6(3) . . . . ? C22 C17 C18 C19 -0.7(5) . . . . ? C17 C18 C19 C20 -2.1(5) . . . . ? C17 C18 C19 C19 179.9(3) . . . 7_567 ? C18 C19 C20 C21 2.7(5) . . . . ? C19 C19 C20 C21 -179.2(3) 7_567 . . . ? C19 C20 C21 C22 -0.7(5) . . . . ? C20 C21 C22 C17 -2.2(5) . . . . ? C20 C21 C22 N1 178.3(3) . . . . ? C18 C17 C22 C21 2.9(5) . . . . ? C18 C17 C22 N1 -177.6(3) . . . . ? N1 C23 C25 N2 0.4(4) . . . . ? N2 C24 N1 C23 -0.4(4) . . . . ? N2 C24 N1 C22 177.8(3) . . . . ? C25 C23 N1 C24 0.0(4) . . . . ? C25 C23 N1 C22 -178.3(3) . . . . ? C21 C22 N1 C24 -18.2(5) . . . . ? C17 C22 N1 C24 162.2(3) . . . . ? C21 C22 N1 C23 159.8(3) . . . . ? C17 C22 N1 C23 -19.8(4) . . . . ? N1 C24 N2 C25 0.7(4) . . . . ? C23 C25 N2 C24 -0.7(4) . . . . ? O2 C1 O1 Cd1 17.6(4) . . . . ? C2 C1 O1 Cd1 -158.34(18) . . . . ? O9 Cd1 O1 C1 -10.2(2) . . . . ? O1 Cd1 O1 C1 169.8(2) 2_554 . . . ? O3 Cd1 O1 C1 70.5(2) 6 . . . ? O3 Cd1 O1 C1 -95.2(2) 5 . . . ? O4 Cd1 O1 C1 -144.3(2) 5 . . . ? O4 Cd1 O1 C1 124.6(2) 6 . . . ? O4 C3 O3 Cd1 -4.3(3) . . . 5 ? C4 C3 O3 Cd1 172.6(2) . . . 5 ? O3 C3 O4 Cd1 4.2(3) . . . 5 ? C4 C3 O4 Cd1 -172.7(2) . . . 5 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C24 H24 O1 0.93 2.26 3.185(4) 170.7 1_566 C17 H17 O6 0.93 2.27 3.187(4) 170.6 4_556 O9 H9B O7 0.810(10) 2.37(2) 3.120(3) 154(4) 8_455 O9 H9B O2 0.810(10) 2.60(4) 2.896(2) 103(3) 2_554 O8 H8A O3 0.820(10) 1.867(13) 2.675(3) 168(3) 4 O6 H6 O2 0.824(10) 1.676(12) 2.494(3) 172(4) 4_545 N2 H2 O5 0.858(10) 2.29(3) 2.886(3) 126(3) 8_456 N2 H2 O4 0.858(10) 2.14(2) 2.805(3) 134(3) 5_566 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.642 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.101 #===END