# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1' _database_code_depnum_ccdc_archive 'CCDC 884070' #TrackingRef 'web_deposit_cif_file_0_feilonghu_1350638779.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H41 N4 Ni2 O14.50' _chemical_formula_weight 1023.27 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.089(11) _cell_length_b 14.791(13) _cell_length_c 15.760(14) _cell_angle_alpha 87.779(13) _cell_angle_beta 74.046(12) _cell_angle_gamma 70.035(12) _cell_volume 2542(4) _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 Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1058 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7936 _exptl_absorpt_correction_T_max 0.8551 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14498 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.2001 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8847 _reflns_number_gt 3662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0860P)^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 SHELXL _refine_ls_extinction_coef 0.0076(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8847 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2047 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.2224 _refine_ls_wR_factor_gt 0.1637 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _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 Ni1 Ni -0.31572(10) 0.55793(7) 0.97723(7) 0.0403(4) Uani 1 1 d . . . Ni2 Ni 0.66272(11) 0.19528(8) 0.60834(7) 0.0478(4) Uani 1 1 d . . . N1 N 0.4850(7) 0.2623(5) 0.6801(4) 0.053(2) Uani 1 1 d . . . N2 N -0.1394(6) 0.5004(5) 0.8936(4) 0.0445(18) Uani 1 1 d . . . N4 N -0.3869(6) 0.6159(5) 0.8765(4) 0.0463(18) Uani 1 1 d . . . N5 N -0.6041(6) 0.7757(5) 0.5079(4) 0.0441(18) Uani 1 1 d . . . O1 O -0.2508(5) 0.4533(4) 1.0680(3) 0.0435(14) Uani 1 1 d . . . O2 O -0.3322(5) 0.4220(4) 0.9709(3) 0.0416(14) Uani 1 1 d . . . O3 O -0.1386(7) 0.0122(4) 1.1205(6) 0.105(3) Uani 1 1 d . . . O4 O -0.2769(5) -0.3296(4) 1.0111(4) 0.0499(16) Uani 1 1 d . . . O5 O -0.4609(7) -0.2269(5) 1.0766(6) 0.092(3) Uani 1 1 d . . . O6 O 0.8208(5) 0.0750(4) 0.5347(4) 0.0609(18) Uani 1 1 d . . . O7 O 0.6491(7) 0.0621(4) 0.6129(4) 0.0600(18) Uani 1 1 d . . . O8 O 0.7463(6) 0.3527(4) 0.7031(4) 0.0671(19) Uani 1 1 d . . . O9 O 0.7121(5) 0.3098(4) 0.5819(4) 0.0527(16) Uani 1 1 d . . . O10 O 0.8937(6) 0.6456(4) 0.4322(4) 0.072(2) Uani 1 1 d . . . O11 O 0.7296(7) 0.1792(5) 0.7162(5) 0.102(3) Uani 1 1 d . . . H11B H 0.6855 0.1656 0.7634 0.123 Uiso 1 1 d R . . H11 H 0.7562 0.2225 0.7204 0.154 Uiso 1 1 d R . . O12 O -0.4827(4) 0.6076(4) 1.0683(3) 0.0467(15) Uani 1 1 d . . . H12C H -0.5395 0.6028 1.0488 0.056 Uiso 1 1 d R . . H12 H -0.4962 0.6627 1.0862 0.070 Uiso 1 1 d R . . O13 O 0.6390(17) 0.9400(10) 0.7629(9) 0.131(7) Uani 0.50 1 d P . . H13C H 0.6402 0.9670 0.7142 0.157 Uiso 0.50 1 d PR . . H13D H 0.6472 0.9770 0.7988 0.157 Uiso 0.50 1 d PR . . O14 O 0.906(3) 0.773(2) 0.7354(19) 0.265(15) Uani 0.50 1 d P . . H14C H 0.8324 0.8109 0.7469 0.318 Uiso 0.50 1 d PR . . H14D H 0.9524 0.8040 0.7099 0.318 Uiso 0.50 1 d PR . . O15 O 0.6685(10) 0.0883(8) 0.8548(7) 0.188(5) Uani 1 1 d . . . H15C H 0.5993 0.1287 0.8821 0.225 Uiso 1 1 d R . . H15B H 0.7176 0.0783 0.8865 0.225 Uiso 1 1 d R . . O16 O 0.029(3) 0.899(4) 0.6503(17) 0.40(3) Uani 0.50 1 d P . . H16C H 0.0671 0.8941 0.5957 0.478 Uiso 0.50 1 d PR . . H16A H -0.0265 0.9547 0.6641 0.478 Uiso 0.50 1 d PR . . C1 C -0.2777(7) 0.3944(5) 1.0313(5) 0.036(2) Uani 1 1 d . . . C2 C -0.2446(7) 0.2935(6) 1.0541(5) 0.039(2) Uani 1 1 d . . . C3 C -0.1941(8) 0.2651(6) 1.1217(6) 0.055(2) Uani 1 1 d . . . H3 H -0.1813 0.3107 1.1533 0.066 Uiso 1 1 calc R . . C4 C -0.1612(8) 0.1719(6) 1.1452(6) 0.059(3) Uani 1 1 d . . . H4 H -0.1277 0.1541 1.1924 0.071 Uiso 1 1 calc R . . C5 C -0.1789(9) 0.1053(6) 1.0976(8) 0.075(3) Uani 1 1 d . . . C6 C -0.2260(10) 0.1309(6) 1.0263(8) 0.084(4) Uani 1 1 d . . . H6 H -0.2354 0.0850 0.9929 0.100 Uiso 1 1 calc R . . C7 C -0.2581(8) 0.2238(6) 1.0063(7) 0.063(3) Uani 1 1 d . . . H7 H -0.2904 0.2416 0.9585 0.076 Uiso 1 1 calc R . . C8 C -0.1910(11) -0.0503(7) 1.1006(8) 0.075(3) Uani 1 1 d . . . C9 C -0.1169(10) -0.1359(7) 1.0599(7) 0.078(3) Uani 1 1 d . . . H9 H -0.0324 -0.1509 1.0432 0.094 Uiso 1 1 calc R . . C10 C -0.1672(10) -0.2015(7) 1.0429(7) 0.068(3) Uani 1 1 d . . . H10 H -0.1163 -0.2610 1.0145 0.082 Uiso 1 1 calc R . . C11 C -0.2909(10) -0.1799(6) 1.0675(7) 0.061(3) Uani 1 1 d . . . C12 C -0.3651(10) -0.0945(7) 1.1112(9) 0.100(4) Uani 1 1 d . . . H12A H -0.4496 -0.0800 1.1301 0.120 Uiso 1 1 calc R . . C13 C -0.3129(12) -0.0285(8) 1.1273(9) 0.107(4) Uani 1 1 d . . . H13 H -0.3627 0.0308 1.1567 0.128 Uiso 1 1 calc R . . C14 C -0.3475(12) -0.2505(8) 1.0499(7) 0.062(3) Uani 1 1 d . . . C15 C 0.7544(10) 0.0257(7) 0.5596(6) 0.052(2) Uani 1 1 d . . . C16 C 0.7918(8) -0.0749(6) 0.5281(6) 0.048(2) Uani 1 1 d . . . C17 C 0.9074(9) -0.1227(7) 0.4776(7) 0.071(3) Uani 1 1 d . . . H17 H 0.9642 -0.0912 0.4635 0.085 Uiso 1 1 calc R . . C18 C 0.9421(9) 0.7829(7) 0.4468(7) 0.071(3) Uani 1 1 d . . . H18 H 1.0220 0.7504 0.4132 0.085 Uiso 1 1 calc R . . C19 C 0.8569(9) 0.7380(6) 0.4665(6) 0.057(3) Uani 1 1 d . . . C20 C 0.7391(8) -0.2125(6) 0.5153(6) 0.056(3) Uani 1 1 d . . . H20 H 0.6806 -0.2424 0.5272 0.067 Uiso 1 1 calc R . . C21 C 0.7084(8) -0.1226(6) 0.5453(6) 0.056(3) Uani 1 1 d . . . H21 H 0.6284 -0.0905 0.5789 0.067 Uiso 1 1 calc R . . C22 C 0.4446(9) 0.3453(7) 0.7285(6) 0.060(3) Uani 1 1 d . . . H22 H 0.5013 0.3725 0.7343 0.073 Uiso 1 1 calc R . . C23 C 0.3243(9) 0.3914(7) 0.7694(6) 0.064(3) Uani 1 1 d . . . H23 H 0.3002 0.4485 0.8033 0.076 Uiso 1 1 calc R . . C24 C 0.2385(8) 0.3548(6) 0.7612(5) 0.047(2) Uani 1 1 d . . . C25 C 0.2771(10) 0.2687(7) 0.7140(6) 0.063(3) Uani 1 1 d . . . H25 H 0.2219 0.2399 0.7085 0.075 Uiso 1 1 calc R . . C26 C 0.4000(10) 0.2267(7) 0.6751(6) 0.061(3) Uani 1 1 d . . . H26 H 0.4261 0.1685 0.6424 0.073 Uiso 1 1 calc R . . C27 C 0.1068(9) 0.4041(7) 0.8050(6) 0.051(2) Uani 1 1 d . . . C28 C 0.0670(10) 0.4834(7) 0.8658(7) 0.075(3) Uani 1 1 d . . . H28 H 0.1243 0.5058 0.8782 0.091 Uiso 1 1 calc R . . C29 C -0.0531(9) 0.5274(7) 0.9064(7) 0.068(3) Uani 1 1 d . . . H29 H -0.0756 0.5801 0.9458 0.082 Uiso 1 1 calc R . . C30 C -0.1037(10) 0.4290(7) 0.8344(6) 0.065(3) Uani 1 1 d . . . H30 H -0.1635 0.4099 0.8219 0.078 Uiso 1 1 calc R . . C31 C 0.0157(9) 0.3810(7) 0.7898(6) 0.067(3) Uani 1 1 d . . . H31 H 0.0341 0.3313 0.7482 0.080 Uiso 1 1 calc R . . C32 C -0.3886(9) 0.7001(7) 0.8458(6) 0.068(3) Uani 1 1 d . . . H32 H -0.3569 0.7367 0.8725 0.081 Uiso 1 1 calc R . . C33 C -0.4345(9) 0.7367(7) 0.7769(6) 0.064(3) Uani 1 1 d . . . H33 H -0.4349 0.7974 0.7588 0.077 Uiso 1 1 calc R . . C34 C -0.4794(7) 0.6855(6) 0.7347(5) 0.039(2) Uani 1 1 d . . . C35 C -0.4803(7) 0.5985(6) 0.7671(5) 0.047(2) Uani 1 1 d . . . H35 H -0.5125 0.5612 0.7419 0.057 Uiso 1 1 calc R . . C36 C -0.4338(8) 0.5669(6) 0.8365(5) 0.053(2) Uani 1 1 d . . . H36 H -0.4350 0.5074 0.8571 0.063 Uiso 1 1 calc R . . C37 C -0.5239(8) 0.7183(6) 0.6578(5) 0.044(2) Uani 1 1 d . . . C38 C -0.5838(8) 0.8126(6) 0.6454(6) 0.049(2) Uani 1 1 d . . . H38 H -0.5996 0.8599 0.6886 0.059 Uiso 1 1 calc R . . C39 C -0.6207(8) 0.8386(6) 0.5710(6) 0.050(2) Uani 1 1 d . . . H39 H -0.6592 0.9036 0.5646 0.060 Uiso 1 1 calc R . . C40 C -0.5450(8) 0.6858(7) 0.5182(6) 0.050(2) Uani 1 1 d . . . H40 H -0.5301 0.6404 0.4735 0.060 Uiso 1 1 calc R . . C41 C -0.5037(8) 0.6539(6) 0.5892(5) 0.049(2) Uani 1 1 d . . . H41 H -0.4619 0.5886 0.5919 0.059 Uiso 1 1 calc R . . C42 C 0.8464(9) 0.5762(6) 0.5709(7) 0.063(3) Uani 1 1 d . . . H42 H 0.8653 0.6208 0.5991 0.075 Uiso 1 1 calc R . . C45 C 0.7452(7) 0.3615(6) 0.6243(7) 0.047(2) Uani 1 1 d . . . C46 C 0.7826(8) 0.4390(6) 0.5744(6) 0.048(2) Uani 1 1 d . . . C50 C 0.8123(8) 0.5045(6) 0.6158(6) 0.051(2) Uani 1 1 d . . . H50 H 0.8091 0.4998 0.6754 0.061 Uiso 1 1 calc R . . C79 C 0.7892(8) 0.4462(6) 0.4871(6) 0.058(3) Uani 1 1 d . . . H79 H 0.7695 0.4027 0.4582 0.069 Uiso 1 1 calc R . . C80 C 0.8516(8) 0.5800(6) 0.4829(7) 0.058(3) Uani 1 1 d . . . C114 C 0.8243(9) 0.5160(7) 0.4417(7) 0.067(3) Uani 1 1 d . . . H114 H 0.8295 0.5197 0.3818 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0475(8) 0.0373(7) 0.0477(7) 0.0064(5) -0.0222(6) -0.0225(6) Ni2 0.0631(9) 0.0374(7) 0.0501(8) 0.0055(6) -0.0230(6) -0.0210(6) N1 0.063(5) 0.054(5) 0.047(4) -0.003(4) -0.011(4) -0.030(4) N2 0.045(5) 0.048(5) 0.047(4) -0.001(4) -0.015(4) -0.021(4) N4 0.055(5) 0.039(4) 0.053(5) 0.010(4) -0.022(4) -0.021(4) N5 0.049(5) 0.035(4) 0.048(4) 0.000(4) -0.017(4) -0.010(4) O1 0.054(4) 0.032(3) 0.054(4) 0.000(3) -0.024(3) -0.019(3) O2 0.049(4) 0.041(3) 0.046(3) 0.003(3) -0.022(3) -0.022(3) O3 0.135(7) 0.036(4) 0.203(9) 0.034(5) -0.128(7) -0.042(4) O4 0.059(4) 0.036(3) 0.063(4) 0.001(3) -0.020(3) -0.025(3) O5 0.064(5) 0.044(4) 0.178(8) -0.020(5) -0.044(5) -0.017(4) O6 0.057(4) 0.049(4) 0.096(5) 0.022(4) -0.039(4) -0.029(3) O7 0.087(5) 0.042(4) 0.057(4) 0.002(3) -0.017(4) -0.032(4) O8 0.096(5) 0.070(5) 0.056(4) 0.010(4) -0.029(4) -0.049(4) O9 0.071(4) 0.042(4) 0.063(4) 0.011(3) -0.037(3) -0.029(3) O10 0.084(5) 0.036(4) 0.076(5) -0.005(3) 0.011(4) -0.022(4) O11 0.182(8) 0.077(5) 0.107(6) 0.039(4) -0.103(6) -0.071(5) O12 0.043(4) 0.044(3) 0.060(4) -0.006(3) -0.022(3) -0.017(3) O13 0.24(2) 0.065(10) 0.074(10) -0.004(8) 0.037(12) -0.101(12) O14 0.23(3) 0.31(4) 0.32(4) -0.01(3) -0.05(3) -0.19(3) O15 0.149(10) 0.194(12) 0.186(11) -0.003(9) -0.019(8) -0.037(9) O16 0.30(4) 0.92(10) 0.20(3) 0.26(4) -0.20(3) -0.42(5) C1 0.037(5) 0.026(4) 0.049(5) -0.002(4) -0.012(4) -0.012(4) C2 0.037(5) 0.033(5) 0.057(6) 0.003(4) -0.019(4) -0.019(4) C3 0.060(6) 0.041(6) 0.081(7) 0.000(5) -0.037(6) -0.025(5) C4 0.069(7) 0.037(5) 0.087(7) 0.014(5) -0.049(6) -0.019(5) C5 0.082(8) 0.029(5) 0.145(10) 0.020(6) -0.078(8) -0.023(5) C6 0.111(9) 0.026(5) 0.145(10) 0.001(6) -0.088(8) -0.019(6) C7 0.066(7) 0.034(5) 0.105(8) -0.005(5) -0.054(6) -0.012(5) C8 0.090(9) 0.036(6) 0.139(10) 0.025(6) -0.082(8) -0.033(6) C9 0.072(8) 0.052(7) 0.125(10) -0.001(7) -0.038(7) -0.031(6) C10 0.081(8) 0.046(6) 0.094(8) 0.005(6) -0.041(7) -0.029(6) C11 0.079(8) 0.025(5) 0.097(8) 0.014(5) -0.042(6) -0.027(5) C12 0.062(8) 0.039(6) 0.207(14) -0.032(8) -0.050(8) -0.013(6) C13 0.091(10) 0.043(7) 0.191(14) -0.027(8) -0.051(10) -0.016(7) C14 0.082(9) 0.048(7) 0.082(8) 0.022(6) -0.046(7) -0.037(7) C15 0.054(7) 0.058(7) 0.047(6) 0.014(5) -0.022(5) -0.018(6) C16 0.044(6) 0.032(5) 0.072(6) 0.012(5) -0.027(5) -0.011(5) C17 0.055(7) 0.046(6) 0.116(9) 0.016(6) -0.022(7) -0.026(6) C18 0.044(6) 0.046(6) 0.105(8) -0.002(6) 0.003(6) -0.012(5) C19 0.057(7) 0.038(6) 0.065(6) 0.011(5) -0.006(5) -0.013(5) C20 0.041(6) 0.038(5) 0.084(7) -0.010(5) -0.001(5) -0.018(5) C21 0.050(6) 0.033(5) 0.074(7) 0.000(5) -0.004(5) -0.011(5) C22 0.072(7) 0.060(6) 0.057(6) -0.023(5) -0.005(6) -0.039(6) C23 0.055(7) 0.072(7) 0.058(6) -0.023(5) 0.006(5) -0.030(6) C24 0.050(6) 0.057(6) 0.041(5) -0.003(5) -0.003(5) -0.033(5) C25 0.064(7) 0.055(6) 0.076(7) -0.012(6) -0.010(6) -0.035(6) C26 0.077(8) 0.052(6) 0.060(6) -0.018(5) -0.009(6) -0.038(6) C27 0.060(7) 0.063(6) 0.044(5) 0.012(5) -0.013(5) -0.040(5) C28 0.055(7) 0.076(8) 0.115(9) -0.025(7) -0.030(7) -0.038(6) C29 0.050(7) 0.060(7) 0.107(9) -0.020(6) -0.027(6) -0.027(6) C30 0.070(8) 0.081(7) 0.060(7) -0.013(6) -0.008(6) -0.053(6) C31 0.064(7) 0.092(8) 0.052(6) -0.030(6) 0.000(6) -0.045(6) C32 0.100(8) 0.065(7) 0.068(7) 0.018(6) -0.050(6) -0.046(6) C33 0.102(8) 0.054(6) 0.059(6) 0.018(5) -0.040(6) -0.042(6) C34 0.050(6) 0.037(5) 0.033(5) 0.007(4) -0.017(4) -0.015(4) C35 0.057(6) 0.050(6) 0.049(5) 0.012(5) -0.022(5) -0.030(5) C36 0.070(7) 0.051(6) 0.050(6) 0.012(5) -0.020(5) -0.035(5) C37 0.049(6) 0.043(5) 0.044(5) 0.005(4) -0.016(4) -0.019(5) C38 0.063(6) 0.033(5) 0.047(6) -0.008(4) -0.014(5) -0.011(5) C39 0.068(7) 0.035(5) 0.049(6) 0.009(5) -0.023(5) -0.014(5) C40 0.056(6) 0.052(6) 0.048(6) -0.004(5) -0.021(5) -0.020(5) C41 0.059(6) 0.037(5) 0.048(6) 0.001(4) -0.019(5) -0.010(5) C42 0.076(7) 0.047(6) 0.074(7) 0.005(5) -0.018(6) -0.035(5) C45 0.039(6) 0.035(5) 0.068(7) 0.004(5) -0.014(5) -0.014(4) C46 0.047(6) 0.027(5) 0.068(7) -0.003(5) -0.013(5) -0.010(4) C50 0.061(6) 0.049(6) 0.051(6) 0.002(5) -0.016(5) -0.028(5) C79 0.074(7) 0.041(6) 0.057(6) 0.000(5) -0.016(6) -0.021(5) C80 0.056(6) 0.035(5) 0.068(7) 0.007(5) 0.003(5) -0.011(5) C114 0.095(8) 0.048(6) 0.061(6) 0.008(5) -0.007(6) -0.041(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O4 2.003(6) 1_565 ? Ni1 N4 2.034(7) . ? Ni1 O12 2.037(5) . ? Ni1 N2 2.076(7) . ? Ni1 O2 2.096(5) . ? Ni1 O1 2.162(5) . ? Ni1 C1 2.467(8) . ? Ni2 O9 1.975(6) . ? Ni2 O7 2.029(6) . ? Ni2 N1 2.043(7) . ? Ni2 O11 2.048(6) . ? Ni2 N5 2.117(7) 2_566 ? Ni2 O6 2.187(6) . ? Ni2 C15 2.428(10) . ? N1 C26 1.325(10) . ? N1 C22 1.336(10) . ? N2 C29 1.302(10) . ? N2 C30 1.309(10) . ? N4 C32 1.314(10) . ? N4 C36 1.325(10) . ? N5 C40 1.306(10) . ? N5 C39 1.315(9) . ? N5 Ni2 2.117(7) 2_566 ? O1 C1 1.240(8) . ? O2 C1 1.280(8) . ? O3 C5 1.366(10) . ? O3 C8 1.373(10) . ? O4 C14 1.249(11) . ? O4 Ni1 2.003(6) 1_545 ? O5 C14 1.243(11) . ? O6 C15 1.240(10) . ? O7 C15 1.262(10) . ? O8 C45 1.247(10) . ? O9 C45 1.259(9) . ? O10 C19 1.366(10) . ? O10 C80 1.375(10) . ? O11 H11B 0.8501 . ? O11 H11 0.8200 . ? O12 H12C 0.8500 . ? O12 H12 0.8199 . ? O13 H13C 0.8500 . ? O13 H13D 0.8498 . ? O14 H14C 0.8500 . ? O14 H14D 0.8500 . ? O15 H15C 0.8499 . ? O15 H15B 0.8500 . ? O16 H16C 0.8501 . ? O16 H16A 0.8500 . ? C1 C2 1.465(10) . ? C2 C3 1.354(10) . ? C2 C7 1.378(10) . ? C3 C4 1.365(11) . ? C3 H3 0.9300 . ? C4 C5 1.366(12) . ? C4 H4 0.9300 . ? C5 C6 1.378(12) . ? C6 C7 1.345(12) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.339(13) . ? C8 C13 1.340(14) . ? C9 C10 1.376(12) . ? C9 H9 0.9300 . ? C10 C11 1.361(12) . ? C10 H10 0.9300 . ? C11 C12 1.353(12) . ? C11 C14 1.500(12) . ? C12 C13 1.394(13) . ? C12 H12A 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.462(12) . ? C16 C17 1.358(11) . ? C16 C21 1.381(11) . ? C17 C18 1.379(12) 1_545 ? C17 H17 0.9300 . ? C18 C19 1.369(12) . ? C18 C17 1.379(12) 1_565 ? C18 H18 0.9300 . ? C19 C20 1.373(11) 1_565 ? C20 C21 1.322(11) . ? C20 C19 1.373(11) 1_545 ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.356(11) . ? C22 H22 0.9300 . ? C23 C24 1.359(11) . ? C23 H23 0.9300 . ? C24 C25 1.367(11) . ? C24 C27 1.478(11) . ? C25 C26 1.366(12) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C31 1.340(11) . ? C27 C28 1.405(12) . ? C28 C29 1.348(12) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.364(12) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.364(11) . ? C32 H32 0.9300 . ? C33 C34 1.351(11) . ? C33 H33 0.9300 . ? C34 C35 1.369(10) . ? C34 C37 1.459(10) . ? C35 C36 1.359(10) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.369(11) . ? C37 C41 1.384(10) . ? C38 C39 1.363(10) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.352(11) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C50 1.370(11) . ? C42 C80 1.371(12) . ? C42 H42 0.9300 . ? C45 C46 1.492(11) . ? C46 C79 1.357(11) . ? C46 C50 1.382(11) . ? C50 H50 0.9300 . ? C79 C114 1.354(11) . ? C79 H79 0.9300 . ? C80 C114 1.343(12) . ? C114 H114 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ni1 N4 98.4(3) 1_565 . ? O4 Ni1 O12 89.9(2) 1_565 . ? N4 Ni1 O12 92.4(2) . . ? O4 Ni1 N2 90.1(3) 1_565 . ? N4 Ni1 N2 92.8(3) . . ? O12 Ni1 N2 174.7(2) . . ? O4 Ni1 O2 163.1(2) 1_565 . ? N4 Ni1 O2 98.5(2) . . ? O12 Ni1 O2 90.3(2) . . ? N2 Ni1 O2 88.3(2) . . ? O4 Ni1 O1 101.8(2) 1_565 . ? N4 Ni1 O1 159.8(2) . . ? O12 Ni1 O1 89.2(2) . . ? N2 Ni1 O1 85.7(2) . . ? O2 Ni1 O1 61.3(2) . . ? O4 Ni1 C1 131.9(3) 1_565 . ? N4 Ni1 C1 129.6(3) . . ? O12 Ni1 C1 91.2(2) . . ? N2 Ni1 C1 85.0(3) . . ? O2 Ni1 C1 31.3(2) . . ? O1 Ni1 C1 30.2(2) . . ? O9 Ni2 O7 166.5(3) . . ? O9 Ni2 N1 98.9(3) . . ? O7 Ni2 N1 94.2(3) . . ? O9 Ni2 O11 88.7(2) . . ? O7 Ni2 O11 93.7(3) . . ? N1 Ni2 O11 94.1(3) . . ? O9 Ni2 N5 84.5(2) . 2_566 ? O7 Ni2 N5 92.6(3) . 2_566 ? N1 Ni2 N5 88.3(3) . 2_566 ? O11 Ni2 N5 173.1(3) . 2_566 ? O9 Ni2 O6 104.8(2) . . ? O7 Ni2 O6 61.8(2) . . ? N1 Ni2 O6 155.7(3) . . ? O11 Ni2 O6 91.6(3) . . ? N5 Ni2 O6 88.9(2) 2_566 . ? O9 Ni2 C15 135.2(3) . . ? O7 Ni2 C15 31.3(3) . . ? N1 Ni2 C15 125.2(3) . . ? O11 Ni2 C15 94.7(3) . . ? N5 Ni2 C15 89.2(3) 2_566 . ? O6 Ni2 C15 30.6(3) . . ? C26 N1 C22 115.9(8) . . ? C26 N1 Ni2 119.6(6) . . ? C22 N1 Ni2 124.4(7) . . ? C29 N2 C30 115.9(8) . . ? C29 N2 Ni1 119.2(6) . . ? C30 N2 Ni1 124.4(6) . . ? C32 N4 C36 115.9(8) . . ? C32 N4 Ni1 124.4(6) . . ? C36 N4 Ni1 119.7(6) . . ? C40 N5 C39 116.2(7) . . ? C40 N5 Ni2 116.7(6) . 2_566 ? C39 N5 Ni2 127.1(6) . 2_566 ? C1 O1 Ni1 88.7(5) . . ? C1 O2 Ni1 90.6(4) . . ? C5 O3 C8 118.5(8) . . ? C14 O4 Ni1 129.6(6) . 1_545 ? C15 O6 Ni2 85.5(6) . . ? C15 O7 Ni2 92.1(6) . . ? C45 O9 Ni2 134.4(6) . . ? C19 O10 C80 119.0(7) . . ? Ni2 O11 H11B 116.1 . . ? Ni2 O11 H11 110.1 . . ? H11B O11 H11 117.0 . . ? Ni1 O12 H12C 112.3 . . ? Ni1 O12 H12 109.8 . . ? H12C O12 H12 112.8 . . ? H13C O13 H13D 108.0 . . ? H14C O14 H14D 108.1 . . ? H15C O15 H15B 109.6 . . ? H16C O16 H16A 110.8 . . ? O1 C1 O2 119.2(7) . . ? O1 C1 C2 121.0(7) . . ? O2 C1 C2 119.8(7) . . ? O1 C1 Ni1 61.2(4) . . ? O2 C1 Ni1 58.2(4) . . ? C2 C1 Ni1 173.7(6) . . ? C3 C2 C7 117.7(8) . . ? C3 C2 C1 120.1(7) . . ? C7 C2 C1 122.1(8) . . ? C2 C3 C4 122.3(8) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C3 C4 C5 118.3(9) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? O3 C5 C4 116.1(9) . . ? O3 C5 C6 122.6(9) . . ? C4 C5 C6 121.0(9) . . ? C7 C6 C5 118.5(9) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C6 C7 C2 122.2(9) . . ? C6 C7 H7 118.9 . . ? C2 C7 H7 118.9 . . ? C9 C8 C13 121.1(10) . . ? C9 C8 O3 118.2(11) . . ? C13 C8 O3 120.5(11) . . ? C8 C9 C10 119.3(10) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 120.6(10) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.9(9) . . ? C12 C11 C14 118.7(10) . . ? C10 C11 C14 121.4(9) . . ? C11 C12 C13 118.8(10) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C8 C13 C12 120.3(10) . . ? C8 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? O5 C14 O4 124.7(9) . . ? O5 C14 C11 117.8(10) . . ? O4 C14 C11 117.5(10) . . ? O6 C15 O7 120.3(9) . . ? O6 C15 C16 122.4(9) . . ? O7 C15 C16 117.2(9) . . ? O6 C15 Ni2 63.9(5) . . ? O7 C15 Ni2 56.6(5) . . ? C16 C15 Ni2 171.3(7) . . ? C17 C16 C21 118.0(8) . . ? C17 C16 C15 121.2(9) . . ? C21 C16 C15 120.7(9) . . ? C16 C17 C18 121.2(9) . 1_545 ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 1_545 . ? C19 C18 C17 118.8(9) . 1_565 ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 1_565 . ? O10 C19 C18 117.0(9) . . ? O10 C19 C20 123.0(9) . 1_565 ? C18 C19 C20 119.9(9) . 1_565 ? C21 C20 C19 120.3(9) . 1_545 ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 1_545 . ? C20 C21 C16 121.8(9) . . ? C20 C21 H21 119.1 . . ? C16 C21 H21 119.1 . . ? N1 C22 C23 122.6(9) . . ? N1 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C22 C23 C24 120.4(9) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 118.4(9) . . ? C23 C24 C27 121.3(8) . . ? C25 C24 C27 120.2(8) . . ? C26 C25 C24 117.5(9) . . ? C26 C25 H25 121.3 . . ? C24 C25 H25 121.3 . . ? N1 C26 C25 125.2(8) . . ? N1 C26 H26 117.4 . . ? C25 C26 H26 117.4 . . ? C31 C27 C28 114.0(9) . . ? C31 C27 C24 124.9(9) . . ? C28 C27 C24 121.1(8) . . ? C29 C28 C27 120.9(9) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? N2 C29 C28 123.7(9) . . ? N2 C29 H29 118.2 . . ? C28 C29 H29 118.2 . . ? N2 C30 C31 124.2(9) . . ? N2 C30 H30 117.9 . . ? C31 C30 H30 117.9 . . ? C27 C31 C30 121.2(9) . . ? C27 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? N4 C32 C33 123.5(9) . . ? N4 C32 H32 118.3 . . ? C33 C32 H32 118.3 . . ? C34 C33 C32 120.5(9) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 116.5(8) . . ? C33 C34 C37 123.3(8) . . ? C35 C34 C37 120.2(8) . . ? C36 C35 C34 119.6(8) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? N4 C36 C35 123.9(8) . . ? N4 C36 H36 118.1 . . ? C35 C36 H36 118.1 . . ? C38 C37 C41 114.7(8) . . ? C38 C37 C34 124.4(8) . . ? C41 C37 C34 120.9(8) . . ? C39 C38 C37 121.4(8) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? N5 C39 C38 122.9(8) . . ? N5 C39 H39 118.6 . . ? C38 C39 H39 118.6 . . ? N5 C40 C41 124.8(8) . . ? N5 C40 H40 117.6 . . ? C41 C40 H40 117.6 . . ? C40 C41 C37 120.0(8) . . ? C40 C41 H41 120.0 . . ? C37 C41 H41 120.0 . . ? C50 C42 C80 117.6(9) . . ? C50 C42 H42 121.2 . . ? C80 C42 H42 121.2 . . ? O8 C45 O9 124.7(8) . . ? O8 C45 C46 119.8(8) . . ? O9 C45 C46 115.5(9) . . ? C79 C46 C50 118.6(8) . . ? C79 C46 C45 120.7(8) . . ? C50 C46 C45 120.7(9) . . ? C42 C50 C46 121.3(9) . . ? C42 C50 H50 119.3 . . ? C46 C50 H50 119.3 . . ? C114 C79 C46 120.6(9) . . ? C114 C79 H79 119.7 . . ? C46 C79 H79 119.7 . . ? C114 C80 C42 121.5(9) . . ? C114 C80 O10 117.6(9) . . ? C42 C80 O10 120.7(10) . . ? C80 C114 C79 120.3(10) . . ? C80 C114 H114 119.8 . . ? C79 C114 H114 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Ni2 N1 C26 146.0(7) . . . . ? O7 Ni2 N1 C26 -30.7(7) . . . . ? O11 Ni2 N1 C26 -124.7(7) . . . . ? N5 Ni2 N1 C26 61.8(7) 2_566 . . . ? O6 Ni2 N1 C26 -21.7(11) . . . . ? C15 Ni2 N1 C26 -26.0(8) . . . . ? O9 Ni2 N1 C22 -28.9(7) . . . . ? O7 Ni2 N1 C22 154.4(7) . . . . ? O11 Ni2 N1 C22 60.4(7) . . . . ? N5 Ni2 N1 C22 -113.1(7) 2_566 . . . ? O6 Ni2 N1 C22 163.4(6) . . . . ? C15 Ni2 N1 C22 159.0(7) . . . . ? O4 Ni1 N2 C29 21.4(7) 1_565 . . . ? N4 Ni1 N2 C29 119.7(7) . . . . ? O12 Ni1 N2 C29 -68(3) . . . . ? O2 Ni1 N2 C29 -141.8(7) . . . . ? O1 Ni1 N2 C29 -80.4(7) . . . . ? C1 Ni1 N2 C29 -110.7(7) . . . . ? O4 Ni1 N2 C30 -167.5(7) 1_565 . . . ? N4 Ni1 N2 C30 -69.2(7) . . . . ? O12 Ni1 N2 C30 103(3) . . . . ? O2 Ni1 N2 C30 29.3(7) . . . . ? O1 Ni1 N2 C30 90.7(7) . . . . ? C1 Ni1 N2 C30 60.4(7) . . . . ? O4 Ni1 N4 C32 5.5(8) 1_565 . . . ? O12 Ni1 N4 C32 95.7(7) . . . . ? N2 Ni1 N4 C32 -85.0(8) . . . . ? O2 Ni1 N4 C32 -173.6(7) . . . . ? O1 Ni1 N4 C32 -170.1(7) . . . . ? C1 Ni1 N4 C32 -170.7(7) . . . . ? O4 Ni1 N4 C36 -175.6(6) 1_565 . . . ? O12 Ni1 N4 C36 -85.4(6) . . . . ? N2 Ni1 N4 C36 93.9(6) . . . . ? O2 Ni1 N4 C36 5.3(6) . . . . ? O1 Ni1 N4 C36 8.8(11) . . . . ? C1 Ni1 N4 C36 8.2(8) . . . . ? O4 Ni1 O1 C1 -176.5(4) 1_565 . . . ? N4 Ni1 O1 C1 -0.9(9) . . . . ? O12 Ni1 O1 C1 93.8(5) . . . . ? N2 Ni1 O1 C1 -87.4(5) . . . . ? O2 Ni1 O1 C1 3.0(4) . . . . ? O4 Ni1 O2 C1 -1.3(10) 1_565 . . . ? N4 Ni1 O2 C1 175.7(4) . . . . ? O12 Ni1 O2 C1 -91.8(4) . . . . ? N2 Ni1 O2 C1 83.1(5) . . . . ? O1 Ni1 O2 C1 -2.9(4) . . . . ? O9 Ni2 O6 C15 -174.4(5) . . . . ? O7 Ni2 O6 C15 3.3(5) . . . . ? N1 Ni2 O6 C15 -7.0(9) . . . . ? O11 Ni2 O6 C15 96.6(5) . . . . ? N5 Ni2 O6 C15 -90.3(5) 2_566 . . . ? O9 Ni2 O7 C15 6.6(13) . . . . ? N1 Ni2 O7 C15 172.6(5) . . . . ? O11 Ni2 O7 C15 -93.0(5) . . . . ? N5 Ni2 O7 C15 84.2(5) 2_566 . . . ? O6 Ni2 O7 C15 -3.2(5) . . . . ? O7 Ni2 O9 C45 -113.5(11) . . . . ? N1 Ni2 O9 C45 80.6(8) . . . . ? O11 Ni2 O9 C45 -13.3(8) . . . . ? N5 Ni2 O9 C45 168.0(8) 2_566 . . . ? O6 Ni2 O9 C45 -104.6(8) . . . . ? C15 Ni2 O9 C45 -108.6(8) . . . . ? Ni1 O1 C1 O2 -5.0(7) . . . . ? Ni1 O1 C1 C2 173.2(7) . . . . ? Ni1 O2 C1 O1 5.1(7) . . . . ? Ni1 O2 C1 C2 -173.0(6) . . . . ? O4 Ni1 C1 O1 4.6(6) 1_565 . . . ? N4 Ni1 C1 O1 179.6(4) . . . . ? O12 Ni1 C1 O1 -86.3(4) . . . . ? N2 Ni1 C1 O1 90.1(5) . . . . ? O2 Ni1 C1 O1 -174.9(7) . . . . ? O4 Ni1 C1 O2 179.5(4) 1_565 . . . ? N4 Ni1 C1 O2 -5.5(6) . . . . ? O12 Ni1 C1 O2 88.6(4) . . . . ? N2 Ni1 C1 O2 -95.0(4) . . . . ? O1 Ni1 C1 O2 174.9(7) . . . . ? O4 Ni1 C1 C2 -107(6) 1_565 . . . ? N4 Ni1 C1 C2 68(6) . . . . ? O12 Ni1 C1 C2 162(6) . . . . ? N2 Ni1 C1 C2 -22(6) . . . . ? O2 Ni1 C1 C2 73(6) . . . . ? O1 Ni1 C1 C2 -112(6) . . . . ? O1 C1 C2 C3 6.2(12) . . . . ? O2 C1 C2 C3 -175.7(7) . . . . ? Ni1 C1 C2 C3 114(5) . . . . ? O1 C1 C2 C7 -170.9(8) . . . . ? O2 C1 C2 C7 7.3(12) . . . . ? Ni1 C1 C2 C7 -63(6) . . . . ? C7 C2 C3 C4 -2.5(13) . . . . ? C1 C2 C3 C4 -179.7(8) . . . . ? C2 C3 C4 C5 0.9(15) . . . . ? C8 O3 C5 C4 156.1(10) . . . . ? C8 O3 C5 C6 -28.8(17) . . . . ? C3 C4 C5 O3 176.6(9) . . . . ? C3 C4 C5 C6 1.5(16) . . . . ? O3 C5 C6 C7 -176.9(10) . . . . ? C4 C5 C6 C7 -2.1(17) . . . . ? C5 C6 C7 C2 0.4(17) . . . . ? C3 C2 C7 C6 1.9(14) . . . . ? C1 C2 C7 C6 178.9(9) . . . . ? C5 O3 C8 C9 130.8(11) . . . . ? C5 O3 C8 C13 -54.0(16) . . . . ? C13 C8 C9 C10 1.9(18) . . . . ? O3 C8 C9 C10 177.0(9) . . . . ? C8 C9 C10 C11 -0.2(16) . . . . ? C9 C10 C11 C12 -1.9(16) . . . . ? C9 C10 C11 C14 -179.8(9) . . . . ? C10 C11 C12 C13 2.3(17) . . . . ? C14 C11 C12 C13 -179.8(10) . . . . ? C9 C8 C13 C12 -1(2) . . . . ? O3 C8 C13 C12 -176.5(11) . . . . ? C11 C12 C13 C8 -1(2) . . . . ? Ni1 O4 C14 O5 0.7(14) 1_545 . . . ? Ni1 O4 C14 C11 179.3(5) 1_545 . . . ? C12 C11 C14 O5 0.1(14) . . . . ? C10 C11 C14 O5 177.9(10) . . . . ? C12 C11 C14 O4 -178.6(9) . . . . ? C10 C11 C14 O4 -0.7(14) . . . . ? Ni2 O6 C15 O7 -5.4(8) . . . . ? Ni2 O6 C15 C16 173.2(8) . . . . ? Ni2 O7 C15 O6 5.8(8) . . . . ? Ni2 O7 C15 C16 -172.9(6) . . . . ? O9 Ni2 C15 O6 7.7(7) . . . . ? O7 Ni2 C15 O6 -174.5(8) . . . . ? N1 Ni2 C15 O6 176.5(4) . . . . ? O11 Ni2 C15 O6 -85.1(5) . . . . ? N5 Ni2 C15 O6 89.2(5) 2_566 . . . ? O9 Ni2 C15 O7 -177.8(4) . . . . ? N1 Ni2 C15 O7 -9.0(6) . . . . ? O11 Ni2 C15 O7 89.3(5) . . . . ? N5 Ni2 C15 O7 -96.4(5) 2_566 . . . ? O6 Ni2 C15 O7 174.5(8) . . . . ? O9 Ni2 C15 C16 -131(5) . . . . ? O7 Ni2 C15 C16 47(5) . . . . ? N1 Ni2 C15 C16 38(5) . . . . ? O11 Ni2 C15 C16 136(5) . . . . ? N5 Ni2 C15 C16 -50(5) 2_566 . . . ? O6 Ni2 C15 C16 -139(5) . . . . ? O6 C15 C16 C17 7.8(13) . . . . ? O7 C15 C16 C17 -173.6(8) . . . . ? Ni2 C15 C16 C17 143(4) . . . . ? O6 C15 C16 C21 -169.0(8) . . . . ? O7 C15 C16 C21 9.7(12) . . . . ? Ni2 C15 C16 C21 -34(5) . . . . ? C21 C16 C17 C18 -2.2(14) . . . 1_545 ? C15 C16 C17 C18 -179.1(9) . . . 1_545 ? C80 O10 C19 C18 142.0(10) . . . . ? C80 O10 C19 C20 -41.0(13) . . . 1_565 ? C17 C18 C19 O10 177.8(9) 1_565 . . . ? C17 C18 C19 C20 0.7(15) 1_565 . . 1_565 ? C19 C20 C21 C16 0.9(14) 1_545 . . . ? C17 C16 C21 C20 1.1(14) . . . . ? C15 C16 C21 C20 178.0(8) . . . . ? C26 N1 C22 C23 -0.6(13) . . . . ? Ni2 N1 C22 C23 174.5(7) . . . . ? N1 C22 C23 C24 -1.1(15) . . . . ? C22 C23 C24 C25 2.6(14) . . . . ? C22 C23 C24 C27 -179.8(8) . . . . ? C23 C24 C25 C26 -2.4(13) . . . . ? C27 C24 C25 C26 180.0(8) . . . . ? C22 N1 C26 C25 0.9(14) . . . . ? Ni2 N1 C26 C25 -174.5(7) . . . . ? C24 C25 C26 N1 0.7(15) . . . . ? C23 C24 C27 C31 169.5(10) . . . . ? C25 C24 C27 C31 -13.0(14) . . . . ? C23 C24 C27 C28 -8.5(13) . . . . ? C25 C24 C27 C28 169.1(9) . . . . ? C31 C27 C28 C29 2.6(15) . . . . ? C24 C27 C28 C29 -179.2(9) . . . . ? C30 N2 C29 C28 -3.2(14) . . . . ? Ni1 N2 C29 C28 168.6(8) . . . . ? C27 C28 C29 N2 0.6(16) . . . . ? C29 N2 C30 C31 2.7(14) . . . . ? Ni1 N2 C30 C31 -168.7(7) . . . . ? C28 C27 C31 C30 -3.2(14) . . . . ? C24 C27 C31 C30 178.7(9) . . . . ? N2 C30 C31 C27 0.6(16) . . . . ? C36 N4 C32 C33 -0.4(14) . . . . ? Ni1 N4 C32 C33 178.6(7) . . . . ? N4 C32 C33 C34 -1.3(15) . . . . ? C32 C33 C34 C35 2.5(13) . . . . ? C32 C33 C34 C37 -176.8(8) . . . . ? C33 C34 C35 C36 -2.0(12) . . . . ? C37 C34 C35 C36 177.2(7) . . . . ? C32 N4 C36 C35 0.9(13) . . . . ? Ni1 N4 C36 C35 -178.1(6) . . . . ? C34 C35 C36 N4 0.4(13) . . . . ? C33 C34 C37 C38 -35.0(13) . . . . ? C35 C34 C37 C38 145.8(9) . . . . ? C33 C34 C37 C41 142.8(9) . . . . ? C35 C34 C37 C41 -36.4(12) . . . . ? C41 C37 C38 C39 0.6(13) . . . . ? C34 C37 C38 C39 178.5(8) . . . . ? C40 N5 C39 C38 -2.8(13) . . . . ? Ni2 N5 C39 C38 177.3(6) 2_566 . . . ? C37 C38 C39 N5 1.6(14) . . . . ? C39 N5 C40 C41 1.9(13) . . . . ? Ni2 N5 C40 C41 -178.2(7) 2_566 . . . ? N5 C40 C41 C37 0.3(14) . . . . ? C38 C37 C41 C40 -1.5(13) . . . . ? C34 C37 C41 C40 -179.5(8) . . . . ? Ni2 O9 C45 O8 -5.2(13) . . . . ? Ni2 O9 C45 C46 176.1(5) . . . . ? O8 C45 C46 C79 175.9(8) . . . . ? O9 C45 C46 C79 -5.2(12) . . . . ? O8 C45 C46 C50 -3.5(12) . . . . ? O9 C45 C46 C50 175.4(7) . . . . ? C80 C42 C50 C46 -0.8(13) . . . . ? C79 C46 C50 C42 0.8(13) . . . . ? C45 C46 C50 C42 -179.8(8) . . . . ? C50 C46 C79 C114 0.0(13) . . . . ? C45 C46 C79 C114 -179.4(8) . . . . ? C50 C42 C80 C114 0.0(14) . . . . ? C50 C42 C80 O10 -175.2(8) . . . . ? C19 O10 C80 C114 141.9(9) . . . . ? C19 O10 C80 C42 -42.7(13) . . . . ? C42 C80 C114 C79 0.8(15) . . . . ? O10 C80 C114 C79 176.2(8) . . . . ? C46 C79 C114 C80 -0.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.667 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.101 data_1 _database_code_depnum_ccdc_archive 'CCDC 884071' #TrackingRef 'web_deposit_cif_file_0_feilonghu_1350638779.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H47 N5 Ni2 O15' _chemical_formula_weight 1087.36 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.215(3) _cell_length_b 14.940(4) _cell_length_c 15.929(4) _cell_angle_alpha 88.100(3) _cell_angle_beta 73.721(3) _cell_angle_gamma 70.836(3) _cell_volume 2630.1(12) _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 block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8586 _exptl_absorpt_correction_T_max 0.8912 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15921 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9796 _reflns_number_gt 5429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0550P)^2^+2.5000P] 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 9796 _refine_ls_number_parameters 707 _refine_ls_number_restraints 286 _refine_ls_R_factor_all 0.1273 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.021 _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 Ni1 Ni 0.68470(6) 0.55839(4) 0.47676(4) 0.0373(2) Uani 1 1 d . . . Ni2 Ni 0.34239(6) 0.80077(4) -0.10748(4) 0.0426(2) Uani 1 1 d . . . O1 O 0.2545(4) 0.6454(3) -0.2020(3) 0.0644(12) Uani 1 1 d . . . O2 O 0.2911(3) 0.6862(2) -0.0820(2) 0.0509(10) Uani 1 1 d . . . O3 O 0.1012(4) 0.3517(3) 0.0656(3) 0.0688(12) Uani 1 1 d . . . O4 O 0.6686(3) 0.4217(2) 0.4704(2) 0.0374(8) Uani 1 1 d . . . O5 O 0.7484(3) 0.4556(2) 0.5671(2) 0.0395(8) Uani 1 1 d . . . O6 O 0.8605(5) 0.0168(3) 0.6200(4) 0.121(2) Uani 1 1 d . . . O7 O 0.7236(4) -0.3287(3) 0.5118(2) 0.0520(10) Uani 1 1 d . . . O8 O 0.5407(5) -0.2296(3) 0.5819(4) 0.107(2) Uani 1 1 d . . . O9 O 0.1858(3) -0.0801(2) -0.0368(3) 0.0600(11) Uani 1 1 d . . . O10 O 0.3590(4) -0.0661(2) -0.1103(3) 0.0519(10) Uani 1 1 d . . . O11 O 0.2819(5) 0.8150(3) -0.2176(3) 0.0972(18) Uani 1 1 d . . . H11A H 0.2869 0.7618 -0.2388 0.117 Uiso 1 1 d R . . H11B H 0.3205 0.8423 -0.2567 0.117 Uiso 1 1 d R . . O12 O 0.5193(3) 0.6064(2) 0.5680(2) 0.0424(9) Uani 1 1 d . . . H12A H 0.4669 0.5932 0.5500 0.051 Uiso 1 1 d R . . H12B H 0.4969 0.6663 0.5773 0.051 Uiso 1 1 d R . . N1 N 0.6144(4) 0.6164(3) 0.3758(3) 0.0422(11) Uani 1 1 d . . . N2 N 0.3980(4) 0.7732(3) 0.0099(3) 0.0395(10) Uani 1 1 d . . . N3 N 0.5199(4) 0.7346(3) -0.1774(3) 0.0469(11) Uani 1 1 d . . . N4 N 1.1411(4) 0.4976(3) -0.3927(3) 0.0457(11) Uani 1 1 d . . . C1 C 0.5647(5) 0.5688(4) 0.3376(3) 0.0486(14) Uani 1 1 d . . . H1 H 0.5620 0.5104 0.3585 0.058 Uiso 1 1 calc R . . C2 C 0.5171(5) 0.6000(4) 0.2695(3) 0.0490(15) Uani 1 1 d . . . H2 H 0.4822 0.5641 0.2459 0.059 Uiso 1 1 calc R . . C3 C 0.5217(4) 0.6854(3) 0.2364(3) 0.0366(12) Uani 1 1 d . . . C4 C 0.5725(6) 0.7358(4) 0.2751(4) 0.0625(18) Uani 1 1 d . . . H4 H 0.5767 0.7941 0.2551 0.075 Uiso 1 1 calc R . . C5 C 0.6169(6) 0.6992(4) 0.3436(4) 0.0661(19) Uani 1 1 d . . . H5 H 0.6509 0.7345 0.3690 0.079 Uiso 1 1 calc R . . C6 C 0.4775(4) 0.7171(3) 0.1585(3) 0.0371(12) Uani 1 1 d . . . C7 C 0.4942(5) 0.6520(4) 0.0926(3) 0.0444(13) Uani 1 1 d . . . H7 H 0.5326 0.5877 0.0968 0.053 Uiso 1 1 calc R . . C8 C 0.4540(5) 0.6823(4) 0.0209(3) 0.0486(14) Uani 1 1 d . . . H8 H 0.4664 0.6370 -0.0225 0.058 Uiso 1 1 calc R . . C9 C 0.3833(5) 0.8356(4) 0.0731(3) 0.0476(14) Uani 1 1 d . . . H9 H 0.3459 0.8996 0.0668 0.057 Uiso 1 1 calc R . . C10 C 0.4203(5) 0.8111(4) 0.1473(3) 0.0475(14) Uani 1 1 d . . . H10 H 0.4067 0.8579 0.1897 0.057 Uiso 1 1 calc R . . C11 C 0.2575(5) 0.6354(3) -0.1249(4) 0.0430(13) Uani 1 1 d . . . C12 C 0.2193(4) 0.5578(3) -0.0756(3) 0.0399(12) Uani 1 1 d . . . C13 C 0.1877(5) 0.4936(3) -0.1176(4) 0.0493(14) Uani 1 1 d . . . H13 H 0.1911 0.4983 -0.1765 0.059 Uiso 1 1 calc R . . C14 C 0.1511(5) 0.4228(4) -0.0721(4) 0.0551(15) Uani 1 1 d . . . H14 H 0.1313 0.3795 -0.1005 0.066 Uiso 1 1 calc R . . C15 C 0.1446(5) 0.4171(4) 0.0146(4) 0.0521(15) Uani 1 1 d . . . C16 C 0.1754(6) 0.4799(4) 0.0567(4) 0.0608(17) Uani 1 1 d . . . H16 H 0.1703 0.4756 0.1160 0.073 Uiso 1 1 calc R . . C17 C 0.2141(5) 0.5493(4) 0.0109(4) 0.0510(15) Uani 1 1 d . . . H17 H 0.2368 0.5907 0.0393 0.061 Uiso 1 1 calc R . . C18 C 0.1398(5) 0.2592(4) 0.0306(4) 0.0506(15) Uani 1 1 d . . . C19 C 0.2569(5) 0.2139(4) -0.0169(4) 0.0572(16) Uani 1 1 d . . . H19 H 0.3124 0.2462 -0.0295 0.069 Uiso 1 1 calc R . . C20 C 0.2925(5) 0.1205(4) -0.0461(4) 0.0556(16) Uani 1 1 d . . . H20 H 0.3724 0.0895 -0.0779 0.067 Uiso 1 1 calc R . . C21 C 0.2096(5) 0.0719(3) -0.0283(4) 0.0447(14) Uani 1 1 d . . . C22 C 0.0936(5) 0.1182(4) 0.0205(4) 0.0578(17) Uani 1 1 d . . . H22 H 0.0380 0.0859 0.0331 0.069 Uiso 1 1 calc R . . C23 C 0.0570(5) 0.2116(4) 0.0514(4) 0.0616(17) Uani 1 1 d . . . H23 H -0.0218 0.2419 0.0855 0.074 Uiso 1 1 calc R . . C24 C 0.2520(6) -0.0300(4) -0.0603(4) 0.0482(15) Uani 1 1 d . . . C25 C 0.5595(6) 0.6533(4) -0.2267(4) 0.0577(16) Uani 1 1 d . . . H25 H 0.5023 0.6273 -0.2327 0.069 Uiso 1 1 calc R . . C26 C 0.6782(5) 0.6057(4) -0.2689(4) 0.0598(17) Uani 1 1 d . . . H26 H 0.7000 0.5495 -0.3024 0.072 Uiso 1 1 calc R . . C27 C 0.7663(5) 0.6426(4) -0.2611(3) 0.0469(14) Uani 1 1 d . . . C28 C 0.7258(6) 0.7273(4) -0.2111(4) 0.0558(16) Uani 1 1 d . . . H28 H 0.7809 0.7552 -0.2044 0.067 Uiso 1 1 calc R . . C29 C 0.6048(6) 0.7701(4) -0.1713(4) 0.0579(16) Uani 1 1 d . . . H29 H 0.5804 0.8269 -0.1382 0.069 Uiso 1 1 calc R . . C30 C 0.8964(5) 0.5926(4) -0.3050(3) 0.0467(14) Uani 1 1 d . . . C31 C 0.9338(6) 0.5168(5) -0.3651(5) 0.078(2) Uani 1 1 d . . . H31 H 0.8764 0.4956 -0.3779 0.093 Uiso 1 1 calc R . . C32 C 1.0541(6) 0.4718(4) -0.4064(5) 0.073(2) Uani 1 1 d . . . H32 H 1.0751 0.4204 -0.4460 0.087 Uiso 1 1 calc R . . C33 C 1.1073(6) 0.5693(5) -0.3336(4) 0.0665(19) Uani 1 1 d . . . H33 H 1.1669 0.5884 -0.3218 0.080 Uiso 1 1 calc R . . C34 C 0.9891(6) 0.6166(5) -0.2890(4) 0.0701(19) Uani 1 1 d . . . H34 H 0.9710 0.6655 -0.2474 0.084 Uiso 1 1 calc R . . C35 C 0.7219(4) 0.3957(3) 0.5304(3) 0.0351(12) Uani 1 1 d . . . C36 C 0.7366(5) 0.2264(4) 0.5080(4) 0.0589(17) Uani 1 1 d . . . H36 H 0.7022 0.2430 0.4621 0.071 Uiso 1 1 calc R . . C37 C 0.7547(4) 0.2955(3) 0.5530(3) 0.0377(12) Uani 1 1 d . . . C38 C 0.7691(6) 0.1330(4) 0.5303(5) 0.083(2) Uani 1 1 d . . . H38 H 0.7559 0.0872 0.5001 0.099 Uiso 1 1 calc R . . C39 C 0.8204(6) 0.1088(4) 0.5970(5) 0.078(2) Uani 1 1 d . . . C40 C 0.8401(6) 0.1754(4) 0.6423(4) 0.069(2) Uani 1 1 d . . . H40 H 0.8747 0.1580 0.6881 0.082 Uiso 1 1 calc R . . C41 C 0.8084(5) 0.2677(4) 0.6199(4) 0.0527(15) Uani 1 1 d . . . H41 H 0.8232 0.3126 0.6501 0.063 Uiso 1 1 calc R . . C42 C 0.8074(8) -0.0480(4) 0.6016(6) 0.091(3) Uani 1 1 d . . . C43 C 0.6871(9) -0.0294(5) 0.6333(7) 0.121(4) Uani 1 1 d . . . H43 H 0.6384 0.0274 0.6656 0.145 Uiso 1 1 calc R . . C44 C 0.6358(8) -0.0963(5) 0.6172(6) 0.107(3) Uani 1 1 d . . . H44 H 0.5528 -0.0839 0.6386 0.129 Uiso 1 1 calc R . . C45 C 0.7090(7) -0.1801(4) 0.5697(5) 0.0661(19) Uani 1 1 d . . . C46 C 0.8312(7) -0.1985(4) 0.5425(5) 0.081(2) Uani 1 1 d . . . H46 H 0.8814 -0.2565 0.5128 0.097 Uiso 1 1 calc R . . C47 C 0.8818(7) -0.1321(5) 0.5586(5) 0.091(3) Uani 1 1 d . . . H47 H 0.9651 -0.1453 0.5401 0.109 Uiso 1 1 calc R . . C48 C 0.6525(7) -0.2511(4) 0.5537(5) 0.0614(19) Uani 1 1 d . . . O13 O 0.4071(14) 0.0478(7) 0.7439(8) 0.379(10) Uani 1 1 d . . . H13A H 0.3447 0.0580 0.7265 0.568 Uiso 1 1 d R . . H13B H 0.3944 0.0138 0.7869 0.568 Uiso 1 1 d R . . O14 O 0.3352(8) 0.9036(6) 0.6444(5) 0.217(4) Uani 1 1 d . . . H14A H 0.2816 0.9532 0.6356 0.325 Uiso 1 1 d R . . H14B H 0.3918 0.8741 0.5998 0.325 Uiso 1 1 d R . . O15 O 0.8411(17) 0.7827(14) 0.2628(15) 0.207(6) Uani 0.50 1 d PDU A 1 N7 N 0.9655(15) 0.8736(12) 0.2093(13) 0.165(6) Uani 0.50 1 d PDU A 1 C49 C 0.861(2) 0.8575(15) 0.2645(19) 0.192(7) Uani 0.50 1 d PDU A 1 H49A H 0.8052 0.9066 0.3043 0.230 Uiso 0.50 1 calc PR A 1 C50 C 1.052(3) 0.7973(18) 0.149(3) 0.207(9) Uani 0.50 1 d PDU A 1 H50A H 1.0352 0.7395 0.1645 0.311 Uiso 0.50 1 calc PR A 1 H50B H 1.1318 0.7905 0.1515 0.311 Uiso 0.50 1 calc PR A 1 H50C H 1.0464 0.8108 0.0907 0.311 Uiso 0.50 1 calc PR A 1 C51 C 0.9690(15) 0.9651(11) 0.2006(11) 0.111(5) Uani 0.50 1 d PDU A 1 H51A H 0.9431 0.9972 0.2576 0.167 Uiso 0.50 1 calc PR A 1 H51B H 0.9162 0.9987 0.1668 0.167 Uiso 0.50 1 calc PR A 1 H51C H 1.0501 0.9630 0.1714 0.167 Uiso 0.50 1 calc PR A 1 O15B O 0.7971(16) 0.9206(13) 0.3107(12) 0.207(6) Uani 0.50 1 d PDU B 2 N7B N 0.9567(19) 0.8115(15) 0.2073(14) 0.194(7) Uani 0.50 1 d PDU B 2 C49B C 0.897(2) 0.9024(14) 0.250(2) 0.203(7) Uani 0.50 1 d PDU B 2 H49B H 0.9315 0.9500 0.2344 0.244 Uiso 0.50 1 calc PR B 2 C50B C 1.080(3) 0.787(2) 0.151(3) 0.204(9) Uani 0.50 1 d PDU B 2 H50D H 1.0985 0.8446 0.1356 0.306 Uiso 0.50 1 calc PR B 2 H50E H 1.0879 0.7530 0.0983 0.306 Uiso 0.50 1 calc PR B 2 H50F H 1.1349 0.7489 0.1809 0.306 Uiso 0.50 1 calc PR B 2 C51B C 0.934(2) 0.7314(15) 0.2516(18) 0.190(7) Uani 0.50 1 d PDU B 2 H51D H 1.0093 0.6802 0.2433 0.285 Uiso 0.50 1 calc PR B 2 H51E H 0.8810 0.7116 0.2281 0.285 Uiso 0.50 1 calc PR B 2 H51F H 0.8974 0.7488 0.3131 0.285 Uiso 0.50 1 calc PR B 2 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 Ni1 0.0465(4) 0.0323(4) 0.0464(4) 0.0080(3) -0.0243(4) -0.0216(3) Ni2 0.0589(5) 0.0287(4) 0.0493(4) 0.0075(3) -0.0266(4) -0.0174(3) O1 0.104(4) 0.062(3) 0.052(3) 0.011(2) -0.032(3) -0.052(3) O2 0.069(3) 0.038(2) 0.062(2) 0.0118(19) -0.034(2) -0.0272(19) O3 0.074(3) 0.033(2) 0.083(3) -0.001(2) 0.008(2) -0.021(2) O4 0.044(2) 0.0333(19) 0.046(2) 0.0047(16) -0.0228(18) -0.0193(16) O5 0.048(2) 0.0260(18) 0.057(2) 0.0023(16) -0.0284(19) -0.0168(16) O6 0.167(5) 0.035(2) 0.244(7) 0.049(3) -0.168(5) -0.052(3) O7 0.071(3) 0.038(2) 0.065(3) 0.010(2) -0.030(2) -0.033(2) O8 0.076(4) 0.037(3) 0.224(7) -0.022(3) -0.074(4) -0.011(2) O9 0.058(3) 0.034(2) 0.103(3) 0.018(2) -0.039(2) -0.024(2) O10 0.066(3) 0.028(2) 0.065(3) 0.0063(19) -0.023(2) -0.016(2) O11 0.182(5) 0.053(3) 0.116(4) 0.038(3) -0.114(4) -0.059(3) O12 0.046(2) 0.0337(19) 0.057(2) -0.0031(17) -0.0251(19) -0.0156(17) N1 0.052(3) 0.037(2) 0.048(3) 0.010(2) -0.024(2) -0.022(2) N2 0.049(3) 0.027(2) 0.045(3) 0.002(2) -0.021(2) -0.010(2) N3 0.062(3) 0.047(3) 0.038(3) 0.000(2) -0.012(2) -0.027(2) N4 0.054(3) 0.054(3) 0.041(3) 0.004(2) -0.018(2) -0.030(2) C1 0.066(4) 0.045(3) 0.051(3) 0.014(3) -0.029(3) -0.031(3) C2 0.066(4) 0.054(4) 0.048(3) 0.016(3) -0.031(3) -0.037(3) C3 0.038(3) 0.038(3) 0.036(3) 0.004(2) -0.016(2) -0.012(2) C4 0.103(5) 0.047(4) 0.071(4) 0.025(3) -0.058(4) -0.044(4) C5 0.109(6) 0.053(4) 0.074(4) 0.024(3) -0.061(4) -0.050(4) C6 0.039(3) 0.038(3) 0.035(3) 0.005(2) -0.011(2) -0.014(2) C7 0.051(4) 0.032(3) 0.049(3) 0.004(3) -0.024(3) -0.003(3) C8 0.065(4) 0.035(3) 0.045(3) -0.005(3) -0.022(3) -0.009(3) C9 0.063(4) 0.031(3) 0.051(3) 0.001(3) -0.024(3) -0.012(3) C10 0.069(4) 0.036(3) 0.042(3) -0.001(3) -0.025(3) -0.015(3) C11 0.040(3) 0.032(3) 0.058(4) -0.002(3) -0.019(3) -0.009(2) C12 0.036(3) 0.029(3) 0.052(3) 0.002(2) -0.012(3) -0.007(2) C13 0.058(4) 0.038(3) 0.056(4) 0.002(3) -0.020(3) -0.020(3) C14 0.061(4) 0.040(3) 0.069(4) 0.000(3) -0.014(3) -0.026(3) C15 0.050(4) 0.026(3) 0.065(4) 0.000(3) 0.003(3) -0.008(3) C16 0.081(5) 0.045(4) 0.056(4) 0.005(3) -0.012(3) -0.028(3) C17 0.066(4) 0.038(3) 0.050(4) -0.003(3) -0.015(3) -0.020(3) C18 0.052(4) 0.030(3) 0.065(4) 0.007(3) -0.011(3) -0.013(3) C19 0.049(4) 0.034(3) 0.088(5) -0.002(3) -0.007(3) -0.024(3) C20 0.041(3) 0.036(3) 0.086(5) 0.001(3) -0.014(3) -0.011(3) C21 0.046(4) 0.029(3) 0.070(4) 0.012(3) -0.029(3) -0.017(3) C22 0.047(4) 0.035(3) 0.099(5) 0.015(3) -0.023(4) -0.023(3) C23 0.038(4) 0.046(4) 0.095(5) 0.014(3) -0.009(3) -0.016(3) C24 0.059(4) 0.033(3) 0.067(4) 0.015(3) -0.039(4) -0.017(3) C25 0.061(4) 0.071(4) 0.050(4) -0.014(3) -0.006(3) -0.040(4) C26 0.057(4) 0.066(4) 0.055(4) -0.029(3) 0.003(3) -0.031(3) C27 0.062(4) 0.055(4) 0.034(3) 0.004(3) -0.012(3) -0.035(3) C28 0.068(5) 0.054(4) 0.062(4) -0.004(3) -0.025(4) -0.036(3) C29 0.065(5) 0.049(4) 0.066(4) -0.007(3) -0.018(4) -0.027(3) C30 0.057(4) 0.060(4) 0.034(3) 0.004(3) -0.014(3) -0.033(3) C31 0.054(4) 0.074(5) 0.114(6) -0.040(4) -0.023(4) -0.027(4) C32 0.052(4) 0.060(4) 0.111(6) -0.034(4) -0.022(4) -0.022(3) C33 0.060(4) 0.103(5) 0.054(4) -0.015(4) -0.006(3) -0.056(4) C34 0.066(5) 0.094(5) 0.060(4) -0.030(4) -0.004(4) -0.048(4) C35 0.033(3) 0.031(3) 0.046(3) 0.000(2) -0.012(3) -0.015(2) C36 0.077(4) 0.036(3) 0.085(5) 0.007(3) -0.055(4) -0.020(3) C37 0.041(3) 0.026(3) 0.054(3) -0.002(2) -0.019(3) -0.015(2) C38 0.117(6) 0.031(3) 0.140(7) 0.004(4) -0.093(6) -0.028(4) C39 0.105(6) 0.030(3) 0.146(7) 0.029(4) -0.096(5) -0.033(3) C40 0.099(5) 0.036(3) 0.104(5) 0.017(3) -0.072(5) -0.029(3) C41 0.071(4) 0.033(3) 0.073(4) 0.005(3) -0.041(4) -0.024(3) C42 0.125(7) 0.029(4) 0.170(8) 0.027(4) -0.108(7) -0.038(4) C43 0.128(8) 0.039(4) 0.227(11) -0.020(5) -0.096(8) -0.027(5) C44 0.104(6) 0.048(4) 0.191(9) -0.020(5) -0.074(6) -0.023(4) C45 0.092(5) 0.030(3) 0.103(5) 0.014(3) -0.063(5) -0.026(3) C46 0.102(6) 0.046(4) 0.120(6) 0.001(4) -0.055(5) -0.038(4) C47 0.110(6) 0.057(5) 0.148(7) 0.025(5) -0.075(6) -0.053(5) C48 0.088(5) 0.029(3) 0.095(5) 0.016(3) -0.065(5) -0.025(3) O13 0.52(2) 0.195(10) 0.286(14) -0.050(9) 0.148(14) -0.149(12) O14 0.217(10) 0.221(9) 0.169(8) 0.010(7) -0.024(7) -0.042(7) O15 0.147(11) 0.238(14) 0.241(13) 0.026(12) -0.034(11) -0.091(11) N7 0.111(10) 0.263(14) 0.129(11) -0.020(11) -0.080(8) -0.033(11) C49 0.151(12) 0.251(14) 0.176(12) -0.010(13) -0.075(10) -0.043(12) C50 0.165(15) 0.273(15) 0.186(14) -0.014(13) -0.089(13) -0.039(13) C51 0.121(10) 0.111(11) 0.139(11) 0.081(9) -0.074(9) -0.063(9) O15B 0.132(11) 0.262(14) 0.174(12) 0.013(11) -0.014(10) -0.022(11) N7B 0.143(12) 0.264(14) 0.153(12) 0.003(12) -0.055(10) -0.025(12) C49B 0.144(13) 0.273(14) 0.173(13) -0.001(12) -0.075(10) -0.018(12) C50B 0.160(15) 0.258(15) 0.174(14) -0.026(13) -0.073(13) -0.020(13) C51B 0.147(13) 0.246(16) 0.199(14) 0.025(13) -0.060(13) -0.085(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O7 2.030(3) 1_565 ? Ni1 O12 2.045(3) . ? Ni1 N1 2.065(4) . ? Ni1 N4 2.080(5) 2_765 ? Ni1 O4 2.124(3) . ? Ni1 O5 2.175(3) . ? Ni1 C35 2.491(5) . ? Ni2 O2 2.002(3) . ? Ni2 N3 2.057(5) . ? Ni2 O10 2.062(3) 1_565 ? Ni2 O11 2.066(4) . ? Ni2 N2 2.146(4) . ? Ni2 O9 2.187(4) 1_565 ? Ni2 C24 2.450(6) 1_565 ? O1 C11 1.242(6) . ? O2 C11 1.267(6) . ? O3 C18 1.384(6) . ? O3 C15 1.394(6) . ? O4 C35 1.284(5) . ? O5 C35 1.256(5) . ? O6 C39 1.374(6) . ? O6 C42 1.408(7) . ? O7 C48 1.268(7) . ? O7 Ni1 2.030(3) 1_545 ? O8 C48 1.244(8) . ? O9 C24 1.251(6) . ? O9 Ni2 2.187(4) 1_545 ? O10 C24 1.270(6) . ? O10 Ni2 2.062(3) 1_545 ? O11 H11A 0.8501 . ? O11 H11B 0.8500 . ? O12 H12A 0.8499 . ? O12 H12B 0.8500 . ? N1 C1 1.329(6) . ? N1 C5 1.330(6) . ? N2 C9 1.329(6) . ? N2 C8 1.335(6) . ? N3 C29 1.337(6) . ? N3 C25 1.339(7) . ? N4 C32 1.316(6) . ? N4 C33 1.327(7) . ? N4 Ni1 2.080(5) 2_765 ? C1 C2 1.369(6) . ? C1 H1 0.9300 . ? C2 C3 1.375(6) . ? C2 H2 0.9300 . ? C3 C4 1.372(7) . ? C3 C6 1.492(6) . ? C4 C5 1.371(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.379(6) . ? C6 C7 1.381(7) . ? C7 C8 1.374(7) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.377(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.507(7) . ? C12 C17 1.365(7) . ? C12 C13 1.395(7) . ? C13 C14 1.386(7) . ? C13 H13 0.9300 . ? C14 C15 1.361(8) . ? C14 H14 0.9300 . ? C15 C16 1.373(7) . ? C16 C17 1.382(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.367(7) . ? C18 C23 1.381(7) . ? C19 C20 1.372(7) . ? C19 H19 0.9300 . ? C20 C21 1.393(7) . ? C20 H20 0.9300 . ? C21 C22 1.366(7) . ? C21 C24 1.493(7) . ? C22 C23 1.380(7) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 Ni2 2.450(6) 1_545 ? C25 C26 1.367(8) . ? C25 H25 0.9300 . ? C26 C27 1.395(7) . ? C26 H26 0.9300 . ? C27 C28 1.385(7) . ? C27 C30 1.484(7) . ? C28 C29 1.370(8) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.376(7) . ? C30 C34 1.382(7) . ? C31 C32 1.372(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.370(8) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C37 1.477(6) . ? C36 C38 1.384(7) . ? C36 C37 1.384(6) . ? C36 H36 0.9300 . ? C37 C41 1.386(7) . ? C38 C39 1.359(8) . ? C38 H38 0.9300 . ? C39 C40 1.368(7) . ? C40 C41 1.369(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.347(11) . ? C42 C47 1.353(10) . ? C43 C44 1.406(9) . ? C43 H43 0.9300 . ? C44 C45 1.375(9) . ? C44 H44 0.9300 . ? C45 C46 1.365(9) . ? C45 C48 1.505(7) . ? C46 C47 1.393(8) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? O13 H13A 0.8492 . ? O13 H13B 0.8494 . ? O14 H14A 0.8501 . ? O14 H14B 0.8500 . ? O15 C49 1.225(10) . ? N7 C51 1.383(12) . ? N7 C49 1.418(12) . ? N7 C50 1.431(13) . ? C49 H49A 0.9300 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? O15B C49B 1.281(10) . ? N7B C49B 1.405(13) . ? N7B C51B 1.434(13) . ? N7B C50B 1.454(13) . ? C49B H49B 0.9300 . ? C50B H50D 0.9600 . ? C50B H50E 0.9600 . ? C50B H50F 0.9600 . ? C51B H51D 0.9600 . ? C51B H51E 0.9600 . ? C51B H51F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ni1 O12 89.63(15) 1_565 . ? O7 Ni1 N1 98.30(15) 1_565 . ? O12 Ni1 N1 92.64(15) . . ? O7 Ni1 N4 90.49(16) 1_565 2_765 ? O12 Ni1 N4 174.76(14) . 2_765 ? N1 Ni1 N4 92.53(17) . 2_765 ? O7 Ni1 O4 162.49(13) 1_565 . ? O12 Ni1 O4 90.39(12) . . ? N1 Ni1 O4 99.19(14) . . ? N4 Ni1 O4 87.92(15) 2_765 . ? O7 Ni1 O5 101.27(13) 1_565 . ? O12 Ni1 O5 88.94(13) . . ? N1 Ni1 O5 160.38(14) . . ? N4 Ni1 O5 85.90(15) 2_765 . ? O4 Ni1 O5 61.23(11) . . ? O7 Ni1 C35 131.47(15) 1_565 . ? O12 Ni1 C35 91.07(14) . . ? N1 Ni1 C35 130.11(16) . . ? N4 Ni1 C35 84.93(16) 2_765 . ? O4 Ni1 C35 31.03(13) . . ? O5 Ni1 C35 30.27(13) . . ? O2 Ni2 N3 98.97(16) . . ? O2 Ni2 O10 166.53(17) . 1_565 ? N3 Ni2 O10 93.92(17) . 1_565 ? O2 Ni2 O11 88.81(15) . . ? N3 Ni2 O11 93.4(2) . . ? O10 Ni2 O11 94.34(15) 1_565 . ? O2 Ni2 N2 84.93(14) . . ? N3 Ni2 N2 87.90(16) . . ? O10 Ni2 N2 91.68(14) 1_565 . ? O11 Ni2 N2 173.73(15) . . ? O2 Ni2 O9 105.05(15) . 1_565 ? N3 Ni2 O9 155.52(15) . 1_565 ? O10 Ni2 O9 61.82(15) 1_565 1_565 ? O11 Ni2 O9 91.75(17) . 1_565 ? N2 Ni2 O9 89.56(15) . 1_565 ? O2 Ni2 C24 135.51(19) . 1_565 ? N3 Ni2 C24 124.96(19) . 1_565 ? O10 Ni2 C24 31.21(15) 1_565 1_565 ? O11 Ni2 C24 94.65(17) . 1_565 ? N2 Ni2 C24 89.60(16) . 1_565 ? O9 Ni2 C24 30.64(16) 1_565 1_565 ? C11 O2 Ni2 134.1(3) . . ? C18 O3 C15 118.1(4) . . ? C35 O4 Ni1 90.5(3) . . ? C35 O5 Ni1 88.9(3) . . ? C39 O6 C42 119.0(5) . . ? C48 O7 Ni1 129.2(4) . 1_545 ? C24 O9 Ni2 86.4(4) . 1_545 ? C24 O10 Ni2 91.5(3) . 1_545 ? Ni2 O11 H11A 112.0 . . ? Ni2 O11 H11B 111.2 . . ? H11A O11 H11B 109.7 . . ? Ni1 O12 H12A 110.2 . . ? Ni1 O12 H12B 110.3 . . ? H12A O12 H12B 108.5 . . ? C1 N1 C5 115.8(4) . . ? C1 N1 Ni1 119.5(3) . . ? C5 N1 Ni1 124.7(3) . . ? C9 N2 C8 116.1(4) . . ? C9 N2 Ni2 127.8(3) . . ? C8 N2 Ni2 116.1(3) . . ? C29 N3 C25 115.9(5) . . ? C29 N3 Ni2 119.9(4) . . ? C25 N3 Ni2 124.1(4) . . ? C32 N4 C33 116.3(5) . . ? C32 N4 Ni1 119.2(4) . 2_765 ? C33 N4 Ni1 123.7(4) . 2_765 ? N1 C1 C2 124.2(5) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C1 C2 C3 119.0(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 117.7(4) . . ? C4 C3 C6 122.8(4) . . ? C2 C3 C6 119.5(4) . . ? C5 C4 C3 119.2(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 124.0(5) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? C10 C6 C7 116.5(5) . . ? C10 C6 C3 122.9(5) . . ? C7 C6 C3 120.5(4) . . ? C8 C7 C6 119.9(5) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? N2 C8 C7 123.7(5) . . ? N2 C8 H8 118.1 . . ? C7 C8 H8 118.1 . . ? N2 C9 C10 123.8(5) . . ? N2 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C9 C10 C6 119.9(5) . . ? C9 C10 H10 120.1 . . ? C6 C10 H10 120.1 . . ? O1 C11 O2 125.2(5) . . ? O1 C11 C12 119.6(5) . . ? O2 C11 C12 115.1(5) . . ? C17 C12 C13 118.8(5) . . ? C17 C12 C11 120.8(5) . . ? C13 C12 C11 120.4(5) . . ? C14 C13 C12 120.5(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 119.4(5) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.7(5) . . ? C14 C15 O3 122.4(5) . . ? C16 C15 O3 116.9(5) . . ? C15 C16 C17 119.9(6) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C12 C17 C16 120.7(5) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C23 120.8(5) . . ? C19 C18 O3 122.0(5) . . ? C23 C18 O3 117.1(5) . . ? C18 C19 C20 119.9(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 120.4(5) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 118.8(5) . . ? C22 C21 C24 122.4(5) . . ? C20 C21 C24 118.8(5) . . ? C21 C22 C23 121.5(5) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.7(6) . . ? C22 C23 H23 120.7 . . ? C18 C23 H23 120.7 . . ? O9 C24 O10 120.1(5) . . ? O9 C24 C21 121.3(6) . . ? O10 C24 C21 118.6(5) . . ? O9 C24 Ni2 63.0(3) . 1_545 ? O10 C24 Ni2 57.3(3) . 1_545 ? C21 C24 Ni2 173.4(4) . 1_545 ? N3 C25 C26 124.5(5) . . ? N3 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? C25 C26 C27 119.2(5) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C28 C27 C26 116.6(6) . . ? C28 C27 C30 122.5(5) . . ? C26 C27 C30 120.9(5) . . ? C29 C28 C27 120.2(5) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? N3 C29 C28 123.7(5) . . ? N3 C29 H29 118.2 . . ? C28 C29 H29 118.2 . . ? C31 C30 C34 114.6(6) . . ? C31 C30 C27 121.7(5) . . ? C34 C30 C27 123.7(5) . . ? C32 C31 C30 121.4(5) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? N4 C32 C31 123.3(6) . . ? N4 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? N4 C33 C34 123.5(5) . . ? N4 C33 H33 118.2 . . ? C34 C33 H33 118.2 . . ? C33 C34 C30 120.8(6) . . ? C33 C34 H34 119.6 . . ? C30 C34 H34 119.6 . . ? O5 C35 O4 119.1(4) . . ? O5 C35 C37 121.2(4) . . ? O4 C35 C37 119.6(4) . . ? O5 C35 Ni1 60.8(2) . . ? O4 C35 Ni1 58.5(2) . . ? C37 C35 Ni1 173.6(4) . . ? C38 C36 C37 120.9(5) . . ? C38 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C41 117.9(4) . . ? C36 C37 C35 122.2(5) . . ? C41 C37 C35 119.9(4) . . ? C39 C38 C36 119.4(5) . . ? C39 C38 H38 120.3 . . ? C36 C38 H38 120.3 . . ? C38 C39 C40 121.0(5) . . ? C38 C39 O6 122.7(5) . . ? C40 C39 O6 116.2(5) . . ? C39 C40 C41 119.5(5) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C40 C41 C37 121.3(5) . . ? C40 C41 H41 119.4 . . ? C37 C41 H41 119.4 . . ? C43 C42 C47 121.7(6) . . ? C43 C42 O6 120.1(8) . . ? C47 C42 O6 117.9(7) . . ? C42 C43 C44 119.6(8) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C45 C44 C43 119.6(8) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 119.1(6) . . ? C46 C45 C48 122.0(6) . . ? C44 C45 C48 118.8(7) . . ? C45 C46 C47 121.2(7) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C42 C47 C46 118.7(7) . . ? C42 C47 H47 120.7 . . ? C46 C47 H47 120.7 . . ? O8 C48 O7 125.1(5) . . ? O8 C48 C45 118.1(6) . . ? O7 C48 C45 116.8(6) . . ? H13A O13 H13B 102.4 . . ? H14A O14 H14B 117.1 . . ? C51 N7 C49 119.9(12) . . ? C51 N7 C50 120.8(12) . . ? C49 N7 C50 117.7(11) . . ? O15 C49 N7 123.6(15) . . ? O15 C49 H49A 118.2 . . ? N7 C49 H49A 118.2 . . ? C49B N7B C51B 118.9(13) . . ? C49B N7B C50B 119.8(15) . . ? C51B N7B C50B 112.1(13) . . ? O15B C49B N7B 120.9(15) . . ? O15B C49B H49B 119.6 . . ? N7B C49B H49B 119.6 . . ? N7B C50B H50D 109.5 . . ? N7B C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? N7B C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? N7B C51B H51D 109.5 . . ? N7B C51B H51E 109.5 . . ? H51D C51B H51E 109.5 . . ? N7B C51B H51F 109.5 . . ? H51D C51B H51F 109.5 . . ? H51E C51B H51F 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 N3 Ni2 O2 C11 -81.8(5) . . . . ? O10 Ni2 O2 C11 115.2(7) 1_565 . . . ? O11 Ni2 O2 C11 11.4(5) . . . . ? N2 Ni2 O2 C11 -168.9(5) . . . . ? O9 Ni2 O2 C11 102.9(5) 1_565 . . . ? C24 Ni2 O2 C11 106.9(5) 1_565 . . . ? O7 Ni1 O4 C35 -1.4(6) 1_565 . . . ? O12 Ni1 O4 C35 -91.4(3) . . . . ? N1 Ni1 O4 C35 175.8(3) . . . . ? N4 Ni1 O4 C35 83.6(3) 2_765 . . . ? O5 Ni1 O4 C35 -2.9(3) . . . . ? O7 Ni1 O5 C35 -176.6(3) 1_565 . . . ? O12 Ni1 O5 C35 93.9(3) . . . . ? N1 Ni1 O5 C35 -0.9(6) . . . . ? N4 Ni1 O5 C35 -87.0(3) 2_765 . . . ? O4 Ni1 O5 C35 2.9(3) . . . . ? O7 Ni1 N1 C1 -173.4(4) 1_565 . . . ? O12 Ni1 N1 C1 -83.4(4) . . . . ? N4 Ni1 N1 C1 95.7(4) 2_765 . . . ? O4 Ni1 N1 C1 7.4(4) . . . . ? O5 Ni1 N1 C1 10.8(7) . . . . ? C35 Ni1 N1 C1 10.2(5) . . . . ? O7 Ni1 N1 C5 8.0(5) 1_565 . . . ? O12 Ni1 N1 C5 98.0(5) . . . . ? N4 Ni1 N1 C5 -82.8(5) 2_765 . . . ? O4 Ni1 N1 C5 -171.1(5) . . . . ? O5 Ni1 N1 C5 -167.7(5) . . . . ? C35 Ni1 N1 C5 -168.3(5) . . . . ? O2 Ni2 N2 C9 -137.9(4) . . . . ? N3 Ni2 N2 C9 122.9(4) . . . . ? O10 Ni2 N2 C9 29.0(4) 1_565 . . . ? O11 Ni2 N2 C9 -134.9(17) . . . . ? O9 Ni2 N2 C9 -32.8(4) 1_565 . . . ? C24 Ni2 N2 C9 -2.1(5) 1_565 . . . ? O2 Ni2 N2 C8 42.0(4) . . . . ? N3 Ni2 N2 C8 -57.2(4) . . . . ? O10 Ni2 N2 C8 -151.1(4) 1_565 . . . ? O11 Ni2 N2 C8 45.0(19) . . . . ? O9 Ni2 N2 C8 147.1(4) 1_565 . . . ? C24 Ni2 N2 C8 177.8(4) 1_565 . . . ? O2 Ni2 N3 C29 -146.0(4) . . . . ? O10 Ni2 N3 C29 30.1(4) 1_565 . . . ? O11 Ni2 N3 C29 124.7(4) . . . . ? N2 Ni2 N3 C29 -61.5(4) . . . . ? O9 Ni2 N3 C29 22.9(6) 1_565 . . . ? C24 Ni2 N3 C29 26.6(5) 1_565 . . . ? O2 Ni2 N3 C25 30.2(4) . . . . ? O10 Ni2 N3 C25 -153.7(4) 1_565 . . . ? O11 Ni2 N3 C25 -59.1(4) . . . . ? N2 Ni2 N3 C25 114.8(4) . . . . ? O9 Ni2 N3 C25 -160.9(4) 1_565 . . . ? C24 Ni2 N3 C25 -157.2(4) 1_565 . . . ? C5 N1 C1 C2 -0.4(9) . . . . ? Ni1 N1 C1 C2 -179.0(4) . . . . ? N1 C1 C2 C3 1.1(9) . . . . ? C1 C2 C3 C4 -1.1(8) . . . . ? C1 C2 C3 C6 176.0(5) . . . . ? C2 C3 C4 C5 0.6(9) . . . . ? C6 C3 C4 C5 -176.5(6) . . . . ? C1 N1 C5 C4 -0.2(9) . . . . ? Ni1 N1 C5 C4 178.4(5) . . . . ? C3 C4 C5 N1 0.1(10) . . . . ? C4 C3 C6 C10 -37.7(8) . . . . ? C2 C3 C6 C10 145.3(5) . . . . ? C4 C3 C6 C7 141.4(6) . . . . ? C2 C3 C6 C7 -35.6(7) . . . . ? C10 C6 C7 C8 -0.3(8) . . . . ? C3 C6 C7 C8 -179.5(5) . . . . ? C9 N2 C8 C7 0.7(8) . . . . ? Ni2 N2 C8 C7 -179.2(4) . . . . ? C6 C7 C8 N2 0.0(9) . . . . ? C8 N2 C9 C10 -1.1(8) . . . . ? Ni2 N2 C9 C10 178.8(4) . . . . ? N2 C9 C10 C6 0.8(9) . . . . ? C7 C6 C10 C9 -0.1(8) . . . . ? C3 C6 C10 C9 179.1(5) . . . . ? Ni2 O2 C11 O1 3.8(9) . . . . ? Ni2 O2 C11 C12 -176.3(3) . . . . ? O1 C11 C12 C17 -175.6(5) . . . . ? O2 C11 C12 C17 4.4(7) . . . . ? O1 C11 C12 C13 3.9(8) . . . . ? O2 C11 C12 C13 -176.0(5) . . . . ? C17 C12 C13 C14 0.3(8) . . . . ? C11 C12 C13 C14 -179.3(5) . . . . ? C12 C13 C14 C15 1.0(9) . . . . ? C13 C14 C15 C16 -1.0(9) . . . . ? C13 C14 C15 O3 175.8(5) . . . . ? C18 O3 C15 C14 44.1(8) . . . . ? C18 O3 C15 C16 -139.0(5) . . . . ? C14 C15 C16 C17 -0.3(9) . . . . ? O3 C15 C16 C17 -177.2(5) . . . . ? C13 C12 C17 C16 -1.5(8) . . . . ? C11 C12 C17 C16 178.0(5) . . . . ? C15 C16 C17 C12 1.6(9) . . . . ? C15 O3 C18 C19 40.6(8) . . . . ? C15 O3 C18 C23 -144.2(6) . . . . ? C23 C18 C19 C20 1.4(9) . . . . ? O3 C18 C19 C20 176.4(5) . . . . ? C18 C19 C20 C21 0.7(9) . . . . ? C19 C20 C21 C22 -1.7(9) . . . . ? C19 C20 C21 C24 -179.4(5) . . . . ? C20 C21 C22 C23 0.7(9) . . . . ? C24 C21 C22 C23 178.3(5) . . . . ? C21 C22 C23 C18 1.3(9) . . . . ? C19 C18 C23 C22 -2.4(9) . . . . ? O3 C18 C23 C22 -177.6(5) . . . . ? Ni2 O9 C24 O10 3.6(5) 1_545 . . . ? Ni2 O9 C24 C21 -174.2(4) 1_545 . . . ? Ni2 O10 C24 O9 -3.8(5) 1_545 . . . ? Ni2 O10 C24 C21 174.1(4) 1_545 . . . ? C22 C21 C24 O9 -6.9(8) . . . . ? C20 C21 C24 O9 170.7(5) . . . . ? C22 C21 C24 O10 175.2(5) . . . . ? C20 C21 C24 O10 -7.2(7) . . . . ? C22 C21 C24 Ni2 -136(4) . . . 1_545 ? C20 C21 C24 Ni2 42(4) . . . 1_545 ? C29 N3 C25 C26 0.7(8) . . . . ? Ni2 N3 C25 C26 -175.7(5) . . . . ? N3 C25 C26 C27 0.2(9) . . . . ? C25 C26 C27 C28 -0.9(8) . . . . ? C25 C26 C27 C30 179.3(5) . . . . ? C26 C27 C28 C29 0.8(8) . . . . ? C30 C27 C28 C29 -179.4(5) . . . . ? C25 N3 C29 C28 -0.8(8) . . . . ? Ni2 N3 C29 C28 175.7(4) . . . . ? C27 C28 C29 N3 0.1(9) . . . . ? C28 C27 C30 C31 -169.9(6) . . . . ? C26 C27 C30 C31 9.9(8) . . . . ? C28 C27 C30 C34 10.9(8) . . . . ? C26 C27 C30 C34 -169.3(6) . . . . ? C34 C30 C31 C32 -1.7(10) . . . . ? C27 C30 C31 C32 179.0(6) . . . . ? C33 N4 C32 C31 2.1(10) . . . . ? Ni1 N4 C32 C31 -167.9(6) 2_765 . . . ? C30 C31 C32 N4 -0.7(11) . . . . ? C32 N4 C33 C34 -1.1(9) . . . . ? Ni1 N4 C33 C34 168.4(5) 2_765 . . . ? N4 C33 C34 C30 -1.3(10) . . . . ? C31 C30 C34 C33 2.6(9) . . . . ? C27 C30 C34 C33 -178.1(6) . . . . ? Ni1 O5 C35 O4 -4.8(4) . . . . ? Ni1 O5 C35 C37 173.0(4) . . . . ? Ni1 O4 C35 O5 5.0(5) . . . . ? Ni1 O4 C35 C37 -172.9(4) . . . . ? O7 Ni1 C35 O5 4.4(4) 1_565 . . . ? O12 Ni1 C35 O5 -86.1(3) . . . . ? N1 Ni1 C35 O5 179.6(3) . . . . ? N4 Ni1 C35 O5 90.6(3) 2_765 . . . ? O4 Ni1 C35 O5 -175.0(5) . . . . ? O7 Ni1 C35 O4 179.4(3) 1_565 . . . ? O12 Ni1 C35 O4 89.0(3) . . . . ? N1 Ni1 C35 O4 -5.4(4) . . . . ? N4 Ni1 C35 O4 -94.4(3) 2_765 . . . ? O5 Ni1 C35 O4 175.0(5) . . . . ? O7 Ni1 C35 C37 -106(3) 1_565 . . . ? O12 Ni1 C35 C37 164(3) . . . . ? N1 Ni1 C35 C37 69(3) . . . . ? N4 Ni1 C35 C37 -20(3) 2_765 . . . ? O4 Ni1 C35 C37 75(3) . . . . ? O5 Ni1 C35 C37 -110(3) . . . . ? C38 C36 C37 C41 1.2(9) . . . . ? C38 C36 C37 C35 179.6(6) . . . . ? O5 C35 C37 C36 -173.9(5) . . . . ? O4 C35 C37 C36 4.0(8) . . . . ? Ni1 C35 C37 C36 -67(3) . . . . ? O5 C35 C37 C41 4.4(8) . . . . ? O4 C35 C37 C41 -177.7(5) . . . . ? Ni1 C35 C37 C41 111(3) . . . . ? C37 C36 C38 C39 -0.6(11) . . . . ? C36 C38 C39 C40 0.2(12) . . . . ? C36 C38 C39 O6 -176.7(7) . . . . ? C42 O6 C39 C38 -26.0(12) . . . . ? C42 O6 C39 C40 157.0(8) . . . . ? C38 C39 C40 C41 -0.5(11) . . . . ? O6 C39 C40 C41 176.6(7) . . . . ? C39 C40 C41 C37 1.2(10) . . . . ? C36 C37 C41 C40 -1.5(9) . . . . ? C35 C37 C41 C40 -179.9(6) . . . . ? C39 O6 C42 C43 -57.1(11) . . . . ? C39 O6 C42 C47 128.8(8) . . . . ? C47 C42 C43 C44 -3.8(14) . . . . ? O6 C42 C43 C44 -177.6(7) . . . . ? C42 C43 C44 C45 0.3(13) . . . . ? C43 C44 C45 C46 3.1(12) . . . . ? C43 C44 C45 C48 179.6(7) . . . . ? C44 C45 C46 C47 -3.1(11) . . . . ? C48 C45 C46 C47 -179.5(6) . . . . ? C43 C42 C47 C46 3.8(12) . . . . ? O6 C42 C47 C46 177.7(6) . . . . ? C45 C46 C47 C42 -0.3(11) . . . . ? Ni1 O7 C48 O8 0.0(9) 1_545 . . . ? Ni1 O7 C48 C45 -179.9(3) 1_545 . . . ? C46 C45 C48 O8 178.6(7) . . . . ? C44 C45 C48 O8 2.2(9) . . . . ? C46 C45 C48 O7 -1.5(9) . . . . ? C44 C45 C48 O7 -177.9(6) . . . . ? C51 N7 C49 O15 165(3) . . . . ? C50 N7 C49 O15 -1(5) . . . . ? C51B N7B C49B O15B -25(5) . . . . ? C50B N7B C49B O15B -169(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.612 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.075 data_2 _database_code_depnum_ccdc_archive 'CCDC 884072' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H49 N4 Ni2 O19' _chemical_formula_weight 1187.40 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.275(5) _cell_length_b 13.288(6) _cell_length_c 18.774(8) _cell_angle_alpha 92.211(6) _cell_angle_beta 100.988(5) _cell_angle_gamma 104.960(5) _cell_volume 2656(2) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1230 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8579 _exptl_absorpt_correction_T_max 0.8579 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 14970 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9205 _reflns_number_gt 6486 _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^)+(0.0698P)^2^+1.2495P] 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 9205 _refine_ls_number_parameters 750 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Ni1 Ni 0.950719(8) 1.390532(8) 0.071731(5) 0.02648(3) Uani 1 1 d . . . Ni2 Ni 0.5000 0.5000 0.5000 0.03257(5) Uani 1 2 d S . . Ni3 Ni 0.5000 0.0000 0.0000 0.03744(5) Uani 1 2 d S . . O1 O 0.21979(6) 0.77547(7) -0.40412(4) 0.0750(3) Uani 1 1 d . . . H1 H 0.1526 0.7357 -0.4251 0.113 Uiso 1 1 d R . . O2 O 0.28448(7) 0.72678(6) -0.50092(4) 0.0706(3) Uani 1 1 d . . . O3 O 0.76034(8) 1.08404(8) -0.34477(4) 0.1242(4) Uani 1 1 d . . . O4 O 0.89722(5) 1.33574(5) -0.03366(3) 0.03895(19) Uani 1 1 d . . . O5 O 0.99055(5) 1.45436(4) -0.10021(3) 0.0424(2) Uani 1 1 d . . . O6 O 0.97708(5) 1.36398(5) 0.18274(3) 0.0421(2) Uani 1 1 d . . . O7 O 0.90300(6) 1.22651(5) 0.10431(3) 0.0467(2) Uani 1 1 d . . . O8 O 1.03000(6) 1.02497(5) 0.40340(3) 0.0547(2) Uani 1 1 d . . . O9 O 0.80552(6) 0.58991(5) 0.51094(4) 0.0609(2) Uani 1 1 d . . . O10 O 0.62552(5) 0.62746(5) 0.46989(3) 0.0411(2) Uani 1 1 d . . . O11 O 0.46078(8) -0.26726(8) 0.22658(5) 0.0632(3) Uani 0.7417(11) 1 d P A 1 C46 C 0.57573(10) -0.25679(8) 0.21720(6) 0.0571(5) Uani 0.7417(11) 1 d P A 1 C50 C 0.74359(9) -0.19055(8) 0.15513(5) 0.0498(5) Uani 0.7417(11) 1 d P A 1 H50 H 0.7746 -0.1505 0.1198 0.060 Uiso 0.7417(11) 1 calc PR A 1 O11' O 0.7855(2) -0.1432(2) 0.11306(15) 0.0632(3) Uani 0.2583(11) 1 d P A 2 C50' C 0.57573(10) -0.25679(8) 0.21720(6) 0.0571(15) Uani 0.2583(11) 1 d P A 2 C46' C 0.74359(9) -0.19055(8) 0.15513(5) 0.0498(11) Uani 0.2583(11) 1 d P A 2 H46 H 0.5022 -0.2590 0.2217 0.060 Uiso 0.2583(11) 1 d PR A 2 O12 O 0.90829(11) 0.47654(9) 0.29428(6) 0.1411(5) Uani 1 1 d . . . H12C H 0.9306 0.4408 0.2633 0.169 Uiso 1 1 d R . . H12D H 0.9251 0.4541 0.3358 0.169 Uiso 1 1 d R . . C47 C 0.65258(11) -0.30948(9) 0.25942(6) 0.0689(4) Uani 1 1 d . . . H47 H 0.6227 -0.3505 0.2946 0.083 Uiso 1 1 d R A . C48 C 0.77128(11) -0.30100(9) 0.24926(7) 0.0782(4) Uani 1 1 d . A . H48 H 0.8213 -0.3356 0.2784 0.094 Uiso 1 1 calc R . . C49 C 0.81978(11) -0.24212(9) 0.19654(6) 0.0699(4) Uani 1 1 d . . . H49 H 0.9003 -0.2377 0.1895 0.084 Uiso 1 1 calc R A 1 O13 O 0.95647(7) 0.41083(6) 0.43472(4) 0.0755(3) Uani 1 1 d . . . H13D H 0.9328 0.4506 0.4623 0.091 Uiso 1 1 d R . . H13C H 1.0297 0.4051 0.4515 0.091 Uiso 1 1 d R . . O14 O 0.34814(19) 0.54918(13) 0.29219(9) 0.2387(11) Uani 1 1 d . . . H14C H 0.3544 0.5584 0.3380 0.286 Uiso 1 1 d R . . H14D H 0.3828 0.6069 0.2772 0.286 Uiso 1 1 d R . . O15 O 0.58789(5) -0.08746(5) 0.06941(3) 0.0445(2) Uani 1 1 d . . . O16 O 0.43217(6) -0.15289(6) 0.12630(4) 0.0619(2) Uani 1 1 d . . . O17 O 0.68128(6) 0.08883(5) -0.00687(3) 0.0506(2) Uani 1 1 d . . . H17B H 0.6723 0.1397 0.0184 0.061 Uiso 1 1 d R . . H17 H 0.6768 0.1213 -0.0431 0.076 Uiso 1 1 d R . . O18 O 0.35739(5) 0.55757(5) 0.44441(3) 0.0428(2) Uani 1 1 d . . . H18C H 0.3728 0.6211 0.4610 0.051 Uiso 1 1 d R . . H18 H 0.2902 0.5262 0.4538 0.051 Uiso 1 1 d R . . O19 O 0.01759(18) 0.04533(18) 0.04268(13) 0.2437(14) Uani 0.7206(13) 1 d P B 1 H19A H -0.0436 -0.0063 0.0457 0.292 Uiso 0.7206(13) 1 d PR B 1 H19B H 0.0695 0.1043 0.0583 0.292 Uiso 0.7206(13) 1 d PR B 1 O19' O -0.1079(3) 0.0560(3) 0.02740(17) 0.0999(14) Uani 0.2794(13) 1 d P B 2 H19D H -0.0823 0.1107 0.0572 0.120 Uiso 0.2794(13) 1 d PR B 2 H19E H -0.1839 0.0504 0.0075 0.120 Uiso 0.2794(13) 1 d PR B 2 C1 C 0.30266(8) 0.78430(8) -0.44670(6) 0.0520(3) Uani 1 1 d . . . C2 C 0.41953(8) 0.86842(7) -0.41838(5) 0.0467(3) Uani 1 1 d . . . C3 C 0.43261(9) 0.93829(8) -0.35942(6) 0.0526(3) Uani 1 1 d . . . H3 H 0.3647 0.9360 -0.3375 0.063 Uiso 1 1 calc R . . C4 C 0.54531(10) 1.01148(9) -0.33257(6) 0.0719(4) Uani 1 1 d . . . H4 H 0.5538 1.0585 -0.2927 0.086 Uiso 1 1 calc R . . C5 C 0.64570(10) 1.01436(10) -0.36538(6) 0.0730(4) Uani 1 1 d . . . C6 C 0.63332(10) 0.94512(9) -0.42465(6) 0.0698(4) Uani 1 1 d . . . H6 H 0.7012 0.9474 -0.4466 0.084 Uiso 1 1 calc R . . C7 C 0.52062(10) 0.87305(8) -0.45105(6) 0.0596(4) Uani 1 1 d . . . H7 H 0.5119 0.8268 -0.4913 0.072 Uiso 1 1 calc R . . C8 C 0.79291(10) 1.15120(10) -0.28129(6) 0.0818(4) Uani 1 1 d . . . C9 C 0.80210(11) 1.11319(9) -0.21452(6) 0.0824(4) Uani 1 1 d . . . H9 H 0.7813 1.0415 -0.2105 0.099 Uiso 1 1 calc R . . C10 C 0.84336(9) 1.18407(8) -0.15246(6) 0.0560(3) Uani 1 1 d . . . H10 H 0.8472 1.1593 -0.1066 0.067 Uiso 1 1 calc R . . C11 C 0.87831(7) 1.28960(7) -0.15799(5) 0.0356(3) Uani 1 1 d . . . C12 C 0.87172(9) 1.32573(9) -0.22682(5) 0.0553(4) Uani 1 1 d . . . H12 H 0.8974 1.3972 -0.2312 0.066 Uiso 1 1 calc R . . C13 C 0.82722(10) 1.25626(10) -0.28885(6) 0.0722(5) Uani 1 1 d . . . H13 H 0.8207 1.2805 -0.3349 0.087 Uiso 1 1 calc R . . C14 C 0.92462(7) 1.36636(6) -0.09199(5) 0.0304(2) Uani 1 1 d . . . C15 C 1.17016(7) 1.34062(7) 0.02099(5) 0.0426(3) Uani 1 1 d . . . H15 H 1.1069 1.3005 -0.0162 0.051 Uiso 1 1 calc R . . C16 C 0.29172(8) 1.34578(7) 0.01797(5) 0.0465(3) Uani 1 1 d . . . H16 H 0.3087 1.3102 -0.0209 0.056 Uiso 1 1 calc R . . C17 C 0.38942(7) 1.40299(6) 0.07177(4) 0.0272(2) Uani 1 1 d . . . C18 C 0.35520(7) 1.45240(7) 0.12760(5) 0.0459(3) Uani 1 1 d . . . H18A H 0.4165 1.4916 0.1660 0.055 Uiso 1 1 calc R . . C19 C 1.23003(7) 1.44365(8) 0.12634(5) 0.0451(3) Uani 1 1 d . . . H19 H 1.2098 1.4778 0.1646 0.054 Uiso 1 1 calc R . . C20 C 0.94517(7) 1.26534(7) 0.16887(5) 0.0378(3) Uani 1 1 d . . . C21 C 0.96194(7) 1.19826(7) 0.22926(5) 0.0365(3) Uani 1 1 d . . . C22 C 0.91099(9) 1.09213(7) 0.22050(5) 0.0477(3) Uani 1 1 d . . . H22 H 0.8633 1.0604 0.1754 0.057 Uiso 1 1 calc R . . C23 C 0.92953(10) 1.03081(7) 0.27819(5) 0.0525(4) Uani 1 1 d . . . H23 H 0.8949 0.9587 0.2717 0.063 Uiso 1 1 calc R . . C24 C 0.99929(8) 1.07815(7) 0.34437(5) 0.0410(3) Uani 1 1 d . . . C25 C 1.05038(8) 1.18459(7) 0.35418(5) 0.0440(3) Uani 1 1 d . . . H25 H 1.0976 1.2159 0.3994 0.053 Uiso 1 1 calc R . . C26 C 1.03212(9) 1.24516(7) 0.29748(5) 0.0444(3) Uani 1 1 d . . . H26 H 1.0665 1.3173 0.3045 0.053 Uiso 1 1 calc R . . C27 C 0.95146(8) 0.92955(7) 0.41305(5) 0.0427(3) Uani 1 1 d . . . C28 C 0.82682(9) 0.91664(7) 0.41237(5) 0.0467(3) Uani 1 1 d . . . H28 H 0.7890 0.9696 0.3994 0.056 Uiso 1 1 calc R . . C29 C 0.75804(8) 0.82270(7) 0.43147(5) 0.0434(3) Uani 1 1 d . . . H29 H 0.6730 0.8126 0.4307 0.052 Uiso 1 1 calc R . . C30 C 0.81371(8) 0.74384(7) 0.45163(4) 0.0355(3) Uani 1 1 d . . . C31 C 0.93830(8) 0.75811(7) 0.44859(5) 0.0447(3) Uani 1 1 d . . . H31 H 0.9761 0.7045 0.4595 0.054 Uiso 1 1 calc R . . C32 C 1.00728(9) 0.85106(7) 0.42953(5) 0.0487(3) Uani 1 1 d . . . H32 H 1.0913 0.8603 0.4279 0.058 Uiso 1 1 calc R . . C33 C 0.74269(8) 0.64581(7) 0.47877(4) 0.0404(3) Uani 1 1 d . . . C34 C 0.38814(8) 0.34293(7) 0.36611(5) 0.0422(3) Uani 1 1 d . . . H34 H 0.3152 0.3371 0.3837 0.051 Uiso 1 1 calc R . . C35 C 0.38096(8) 0.27988(7) 0.30432(5) 0.0449(3) Uani 1 1 d . . . H35 H 0.3059 0.2316 0.2823 0.054 Uiso 1 1 calc R . . C36 C 0.48771(8) 0.28982(6) 0.27565(4) 0.0341(3) Uani 1 1 d . . . C37 C 0.59578(8) 0.36398(7) 0.31127(5) 0.0418(3) Uani 1 1 d . . . H37 H 0.6690 0.3750 0.2932 0.050 Uiso 1 1 calc R . . C38 C 0.59395(8) 0.42120(7) 0.37345(5) 0.0418(3) Uani 1 1 d . . . H38 H 0.6680 0.4696 0.3969 0.050 Uiso 1 1 calc R . . C39 C 0.48833(7) 0.22218(6) 0.21089(4) 0.0326(3) Uani 1 1 d . . . C40 C 0.38249(8) 0.18166(7) 0.15715(4) 0.0379(3) Uani 1 1 d . . . H40 H 0.3072 0.1956 0.1611 0.045 Uiso 1 1 calc R . . C41 C 0.38792(8) 0.12009(7) 0.09713(5) 0.0396(3) Uani 1 1 d . . . H41 H 0.3158 0.0947 0.0610 0.048 Uiso 1 1 calc R . . C42 C 0.59469(8) 0.13456(7) 0.14113(5) 0.0441(3) Uani 1 1 d . . . H42 H 0.6685 0.1185 0.1363 0.053 Uiso 1 1 calc R . . C43 C 0.59661(8) 0.19751(7) 0.20201(5) 0.0432(3) Uani 1 1 d . . . H43 H 0.6705 0.2231 0.2368 0.052 Uiso 1 1 calc R . . C44 C 0.54211(8) -0.14052(7) 0.11655(5) 0.0427(3) Uani 1 1 d . A . C45 C 0.62387(9) -0.19561(7) 0.16371(5) 0.0444(3) Uani 1 1 d . . . C51 C 0.52160(7) 1.40634(6) 0.07108(4) 0.0295(2) Uani 1 1 d . . . C66 C 0.62264(7) 1.46474(8) 0.12289(5) 0.0444(3) Uani 1 1 d . . . H66 H 0.6097 1.5075 0.1594 0.053 Uiso 1 1 calc R . . C69 C 0.55057(7) 1.34912(7) 0.01760(5) 0.0493(3) Uani 1 1 d . . . H69 H 0.4868 1.3105 -0.0199 0.059 Uiso 1 1 calc R . . C88 C 0.74166(8) 1.45988(8) 0.12062(5) 0.0461(3) Uani 1 1 d . . . H88 H 0.8074 1.4994 0.1567 0.055 Uiso 1 1 calc R . . C91 C 0.67276(7) 1.34821(7) 0.01887(5) 0.0469(3) Uani 1 1 d . . . H91 H 0.6886 1.3078 -0.0179 0.056 Uiso 1 1 calc R . . N1 N 0.49318(6) 0.41170(5) 0.40213(4) 0.0369(2) Uani 1 1 d . . . N2 N 0.49284(7) 0.09591(5) 0.08918(4) 0.0390(2) Uani 1 1 d . . . N3 N 1.13735(5) 1.38935(5) 0.07369(4) 0.0315(2) Uani 1 1 d . . . N4 N 0.76903(5) 1.40205(5) 0.06990(4) 0.0303(2) 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 Ni1 0.01723(4) 0.03262(5) 0.03046(5) 0.00208(4) 0.00616(4) 0.00752(4) Ni2 0.03403(7) 0.03129(7) 0.02611(7) -0.00637(6) 0.01200(6) -0.00507(6) Ni3 0.04866(8) 0.03734(8) 0.03123(8) -0.00314(7) 0.01693(6) 0.01494(6) O1 0.0395(4) 0.0958(6) 0.0802(5) -0.0105(5) 0.0110(4) 0.0052(4) O2 0.0529(4) 0.0663(4) 0.0790(5) -0.0258(4) 0.0024(4) 0.0054(4) O3 0.0945(5) 0.1420(7) 0.0898(5) -0.0788(4) 0.0608(4) -0.0669(5) O4 0.0249(3) 0.0572(3) 0.0327(3) 0.0005(3) 0.0086(2) 0.0062(3) O5 0.0363(3) 0.0339(3) 0.0538(4) -0.0007(3) 0.0085(3) 0.0052(2) O6 0.0359(3) 0.0492(3) 0.0455(3) 0.0151(3) 0.0124(3) 0.0148(2) O7 0.0503(3) 0.0550(3) 0.0373(3) 0.0100(3) 0.0104(3) 0.0166(3) O8 0.0539(4) 0.0454(3) 0.0460(4) 0.0222(3) -0.0050(3) -0.0109(3) O9 0.0409(3) 0.0563(4) 0.0698(4) 0.0288(3) 0.0006(3) -0.0100(3) O10 0.0361(3) 0.0403(3) 0.0378(3) -0.0035(3) 0.0132(2) -0.0085(3) O11 0.0567(5) 0.0793(6) 0.0613(5) 0.0152(5) 0.0195(4) 0.0252(4) C46 0.0726(8) 0.0556(7) 0.0406(8) -0.0042(6) -0.0007(7) 0.0234(6) C50 0.0479(7) 0.0486(7) 0.0431(7) -0.0089(6) 0.0009(6) 0.0040(6) O11' 0.0567(5) 0.0793(6) 0.0613(5) 0.0152(5) 0.0195(4) 0.0252(4) C50' 0.073(2) 0.056(2) 0.041(2) -0.0042(19) -0.001(2) 0.0234(19) C46' 0.0479(17) 0.0486(17) 0.0431(15) -0.0089(18) 0.0010(18) 0.0040(18) O12 0.2098(9) 0.1507(8) 0.1001(7) 0.0282(7) 0.0558(7) 0.0946(7) C47 0.0922(8) 0.0656(6) 0.0430(6) 0.0017(5) -0.0039(6) 0.0246(6) C48 0.0889(7) 0.0706(6) 0.0664(7) -0.0173(6) -0.0256(6) 0.0400(5) C49 0.0623(6) 0.0707(6) 0.0671(7) -0.0207(6) -0.0146(6) 0.0255(5) O13 0.0577(4) 0.0807(5) 0.0889(5) 0.0161(4) 0.0182(4) 0.0164(4) O14 0.355(2) 0.1724(13) 0.1506(13) 0.0209(11) 0.0041(15) 0.0392(15) O15 0.0524(3) 0.0481(3) 0.0394(3) 0.0031(3) 0.0176(3) 0.0195(3) O16 0.0512(3) 0.0847(4) 0.0634(4) 0.0262(4) 0.0250(3) 0.0303(3) O17 0.0663(4) 0.0437(3) 0.0417(3) -0.0018(3) 0.0194(3) 0.0096(3) O18 0.0427(3) 0.0376(3) 0.0422(3) 0.0011(3) 0.0147(3) -0.0033(3) O19 0.1929(14) 0.288(2) 0.319(3) 0.027(2) 0.1081(16) 0.1457(13) O19' 0.0712(18) 0.127(2) 0.085(2) -0.0397(19) -0.0081(17) 0.0230(18) C1 0.0370(5) 0.0545(5) 0.0624(6) -0.0005(5) 0.0022(5) 0.0153(4) C2 0.0416(5) 0.0469(5) 0.0498(6) 0.0018(4) 0.0061(4) 0.0117(4) C3 0.0495(5) 0.0567(6) 0.0515(6) -0.0022(5) 0.0129(4) 0.0138(4) C4 0.0703(7) 0.0685(7) 0.0659(7) -0.0249(6) 0.0276(5) -0.0057(6) C5 0.0655(6) 0.0782(7) 0.0537(6) -0.0243(6) 0.0272(5) -0.0248(6) C6 0.0633(6) 0.0722(7) 0.0606(6) -0.0232(6) 0.0279(5) -0.0115(6) C7 0.0583(6) 0.0603(6) 0.0513(6) -0.0171(5) 0.0126(5) 0.0027(5) C8 0.0566(6) 0.1010(8) 0.0633(6) -0.0432(6) 0.0358(4) -0.0316(6) C9 0.0907(7) 0.0516(6) 0.0890(7) -0.0273(6) 0.0544(5) -0.0297(6) C10 0.0595(5) 0.0461(5) 0.0562(5) -0.0068(5) 0.0328(4) -0.0098(5) C11 0.0238(4) 0.0437(5) 0.0370(4) -0.0016(4) 0.0111(3) 0.0021(3) C12 0.0557(5) 0.0646(6) 0.0420(5) -0.0069(5) 0.0116(4) 0.0107(5) C13 0.0650(7) 0.0954(9) 0.0426(6) -0.0144(6) 0.0115(5) 0.0004(6) C14 0.0159(3) 0.0377(4) 0.0379(4) 0.0010(4) 0.0055(3) 0.0084(3) C15 0.0228(4) 0.0535(5) 0.0470(5) -0.0157(4) -0.0035(4) 0.0131(3) C16 0.0310(4) 0.0664(5) 0.0425(5) -0.0200(4) 0.0037(4) 0.0205(4) C17 0.0221(3) 0.0302(4) 0.0305(4) 0.0008(3) 0.0043(3) 0.0101(3) C18 0.0245(4) 0.0605(5) 0.0469(5) -0.0215(4) 0.0004(4) 0.0101(4) C19 0.0258(4) 0.0683(6) 0.0384(5) -0.0197(4) 0.0033(4) 0.0135(4) C20 0.0286(4) 0.0485(5) 0.0415(5) 0.0089(4) 0.0125(3) 0.0151(3) C21 0.0334(4) 0.0452(4) 0.0340(4) 0.0089(4) 0.0105(3) 0.0130(3) C22 0.0542(5) 0.0423(5) 0.0354(5) 0.0027(4) -0.0038(4) 0.0033(4) C23 0.0650(6) 0.0355(5) 0.0464(6) 0.0055(4) -0.0006(5) 0.0034(5) C24 0.0343(4) 0.0412(5) 0.0406(5) 0.0139(4) 0.0069(4) -0.0024(4) C25 0.0443(5) 0.0422(5) 0.0367(5) 0.0039(4) 0.0021(4) 0.0008(4) C26 0.0496(5) 0.0333(4) 0.0441(5) 0.0070(4) 0.0105(4) -0.0006(4) C27 0.0446(5) 0.0391(5) 0.0334(5) 0.0109(4) 0.0030(4) -0.0055(4) C28 0.0440(5) 0.0434(5) 0.0502(5) 0.0137(4) 0.0079(4) 0.0073(4) C29 0.0329(4) 0.0519(5) 0.0412(5) 0.0021(4) 0.0101(4) 0.0026(4) C30 0.0349(4) 0.0385(4) 0.0251(4) 0.0017(4) 0.0088(3) -0.0059(4) C31 0.0440(5) 0.0430(5) 0.0453(5) 0.0141(4) 0.0137(4) 0.0042(4) C32 0.0350(4) 0.0563(5) 0.0517(5) 0.0194(4) 0.0153(4) 0.0000(4) C33 0.0419(5) 0.0422(5) 0.0259(4) -0.0040(4) 0.0101(4) -0.0096(4) C34 0.0384(4) 0.0500(5) 0.0340(4) -0.0143(4) 0.0157(3) 0.0009(4) C35 0.0389(5) 0.0499(5) 0.0376(5) -0.0147(4) 0.0086(4) -0.0003(4) C36 0.0384(4) 0.0369(4) 0.0269(4) -0.0019(4) 0.0094(3) 0.0089(3) C37 0.0385(4) 0.0462(5) 0.0373(5) -0.0115(4) 0.0161(4) 0.0017(4) C38 0.0369(4) 0.0405(5) 0.0411(5) -0.0096(4) 0.0137(4) -0.0040(4) C39 0.0366(4) 0.0346(4) 0.0264(4) -0.0031(4) 0.0104(3) 0.0074(3) C40 0.0416(4) 0.0432(4) 0.0302(4) -0.0072(4) 0.0082(4) 0.0150(4) C41 0.0427(4) 0.0469(5) 0.0302(4) -0.0070(4) 0.0048(4) 0.0176(4) C42 0.0405(4) 0.0506(5) 0.0433(5) -0.0091(4) 0.0146(4) 0.0136(4) C43 0.0366(4) 0.0564(5) 0.0338(5) -0.0122(4) 0.0067(4) 0.0106(4) C44 0.0518(5) 0.0449(5) 0.0335(5) -0.0047(4) 0.0100(4) 0.0170(4) C45 0.0557(5) 0.0386(4) 0.0350(5) -0.0082(4) -0.0006(4) 0.0150(4) C51 0.0220(3) 0.0315(4) 0.0334(4) -0.0007(4) 0.0039(3) 0.0066(3) C66 0.0234(4) 0.0684(5) 0.0405(5) -0.0201(4) 0.0058(3) 0.0152(4) C69 0.0183(4) 0.0620(5) 0.0595(6) -0.0290(5) 0.0015(4) 0.0065(4) C88 0.0260(4) 0.0703(6) 0.0364(5) -0.0164(5) 0.0011(4) 0.0103(4) C91 0.0256(4) 0.0534(5) 0.0599(6) -0.0250(4) 0.0099(4) 0.0110(4) N1 0.0395(4) 0.0372(4) 0.0290(4) -0.0084(3) 0.0127(3) -0.0008(3) N2 0.0481(4) 0.0419(4) 0.0308(4) -0.0043(3) 0.0118(3) 0.0173(3) N3 0.0210(3) 0.0414(4) 0.0334(4) -0.0004(3) 0.0052(3) 0.0113(3) N4 0.0195(3) 0.0368(3) 0.0348(4) -0.0004(3) 0.0050(3) 0.0089(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 Ni1 O4 2.0040(10) . ? Ni1 O5 2.0119(10) 2_785 ? Ni1 N4 2.0872(11) . ? Ni1 N3 2.1017(12) . ? Ni1 O6 2.1050(10) . ? Ni1 O7 2.2443(11) . ? Ni1 C20 2.5141(12) . ? Ni2 O18 2.0777(9) . ? Ni2 O18 2.0777(9) 2_666 ? Ni2 O10 2.0815(8) . ? Ni2 O10 2.0815(8) 2_666 ? Ni2 N1 2.1195(10) . ? Ni2 N1 2.1195(10) 2_666 ? Ni3 O15 2.0615(8) . ? Ni3 O15 2.0615(8) 2_655 ? Ni3 N2 2.0914(10) . ? Ni3 N2 2.0914(10) 2_655 ? Ni3 O17 2.1105(10) . ? Ni3 O17 2.1105(10) 2_655 ? O1 C1 1.3272(14) . ? O2 C1 1.2007(13) . ? O3 C5 1.3570(13) . ? O3 C8 1.3904(15) . ? O4 C14 1.2486(11) . ? O5 C14 1.2460(10) . ? O5 Ni1 2.0119(10) 2_785 ? O6 C20 1.2688(12) . ? O7 C20 1.2517(11) . ? O8 C24 1.3741(12) . ? O8 C27 1.3870(11) . ? O9 C33 1.2497(13) . ? O10 C33 1.2566(12) . ? O11 C46 1.3137(16) . ? C46 C47 1.4013(17) . ? C46 C45 1.4165(15) . ? C50 C45 1.3745(16) . ? C50 C49 1.3792(16) . ? C47 C48 1.3643(19) . ? C48 C49 1.3915(18) . ? O15 C44 1.2574(12) . ? O16 C44 1.2573(13) . ? C1 C2 1.4815(12) . ? C2 C3 1.3773(15) . ? C2 C7 1.3828(16) . ? C3 C4 1.3764(14) . ? C4 C5 1.3812(18) . ? C5 C6 1.3782(17) . ? C6 C7 1.3684(14) . ? C8 C9 1.3651(17) . ? C8 C13 1.3698(19) . ? C9 C10 1.3942(15) . ? C10 C11 1.3689(14) . ? C11 C12 1.3912(14) . ? C11 C14 1.4931(12) . ? C12 C13 1.3839(15) . ? C15 N3 1.3224(13) . ? C15 C16 1.3668(14) 1_655 ? C16 C15 1.3668(14) 1_455 ? C16 C17 1.3769(11) . ? C17 C18 1.3821(14) . ? C17 C51 1.4820(13) . ? C18 C19 1.3814(14) 1_455 ? C19 N3 1.3234(10) . ? C19 C18 1.3814(14) 1_655 ? C20 C21 1.4830(14) . ? C21 C22 1.3687(13) . ? C21 C26 1.3972(12) . ? C22 C23 1.3966(15) . ? C23 C24 1.3674(13) . ? C24 C25 1.3730(13) . ? C25 C26 1.3753(14) . ? C27 C32 1.3671(15) . ? C27 C28 1.3686(15) . ? C28 C29 1.3888(14) . ? C29 C30 1.3838(15) . ? C30 C31 1.3807(14) . ? C30 C33 1.5053(13) . ? C31 C32 1.3793(14) . ? C34 N1 1.3353(10) . ? C34 C35 1.3815(14) . ? C35 C36 1.3879(14) . ? C36 C37 1.3862(11) . ? C36 C39 1.4860(13) . ? C37 C38 1.3747(14) . ? C38 N1 1.3271(13) . ? C39 C40 1.3781(11) . ? C39 C43 1.3805(15) . ? C40 C41 1.3871(13) . ? C41 N2 1.3360(14) . ? C42 N2 1.3280(11) . ? C42 C43 1.3834(14) . ? C44 C45 1.5024(14) . ? C51 C69 1.3738(14) . ? C51 C66 1.3816(11) . ? C66 C88 1.3686(14) . ? C69 C91 1.3766(14) . ? C88 N4 1.3306(13) . ? C91 N4 1.3257(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 O4 Ni1 O5 120.22(3) . 2_785 ? O4 Ni1 N4 89.10(3) . . ? O5 Ni1 N4 87.04(3) 2_785 . ? O4 Ni1 N3 91.91(3) . . ? O5 Ni1 N3 89.43(3) 2_785 . ? N4 Ni1 N3 176.36(3) . . ? O4 Ni1 O6 150.23(3) . . ? O5 Ni1 O6 89.53(3) 2_785 . ? N4 Ni1 O6 91.69(3) . . ? N3 Ni1 O6 89.17(3) . . ? O4 Ni1 O7 90.27(3) . . ? O5 Ni1 O7 149.45(3) 2_785 . ? N4 Ni1 O7 91.89(3) . . ? N3 Ni1 O7 91.60(3) . . ? O6 Ni1 O7 59.97(2) . . ? O4 Ni1 C20 120.01(4) . . ? O5 Ni1 C20 119.77(4) 2_785 . ? N4 Ni1 C20 94.02(3) . . ? N3 Ni1 C20 88.51(3) . . ? O6 Ni1 C20 30.26(3) . . ? O7 Ni1 C20 29.82(2) . . ? O18 Ni2 O18 180.000(1) . 2_666 ? O18 Ni2 O10 87.00(4) . . ? O18 Ni2 O10 93.00(4) 2_666 . ? O18 Ni2 O10 93.00(4) . 2_666 ? O18 Ni2 O10 87.00(4) 2_666 2_666 ? O10 Ni2 O10 180.0 . 2_666 ? O18 Ni2 N1 88.69(3) . . ? O18 Ni2 N1 91.31(3) 2_666 . ? O10 Ni2 N1 90.17(4) . . ? O10 Ni2 N1 89.83(4) 2_666 . ? O18 Ni2 N1 91.31(3) . 2_666 ? O18 Ni2 N1 88.69(3) 2_666 2_666 ? O10 Ni2 N1 89.83(4) . 2_666 ? O10 Ni2 N1 90.17(4) 2_666 2_666 ? N1 Ni2 N1 180.0 . 2_666 ? O15 Ni3 O15 180.00(5) . 2_655 ? O15 Ni3 N2 90.20(4) . . ? O15 Ni3 N2 89.80(4) 2_655 . ? O15 Ni3 N2 89.80(4) . 2_655 ? O15 Ni3 N2 90.20(4) 2_655 2_655 ? N2 Ni3 N2 180.00(5) . 2_655 ? O15 Ni3 O17 86.73(4) . . ? O15 Ni3 O17 93.27(4) 2_655 . ? N2 Ni3 O17 93.23(3) . . ? N2 Ni3 O17 86.77(3) 2_655 . ? O15 Ni3 O17 93.27(4) . 2_655 ? O15 Ni3 O17 86.73(4) 2_655 2_655 ? N2 Ni3 O17 86.77(3) . 2_655 ? N2 Ni3 O17 93.23(3) 2_655 2_655 ? O17 Ni3 O17 180.00(5) . 2_655 ? C5 O3 C8 122.01(10) . . ? C14 O4 Ni1 135.89(5) . . ? C14 O5 Ni1 149.33(7) . 2_785 ? C20 O6 Ni1 93.00(5) . . ? C20 O7 Ni1 87.12(6) . . ? C24 O8 C27 120.81(7) . . ? C33 O10 Ni2 128.09(6) . . ? O11 C46 C47 119.75(11) . . ? O11 C46 C45 121.75(10) . . ? C47 C46 C45 118.48(11) . . ? C45 C50 C49 122.99(10) . . ? C48 C47 C46 120.38(11) . . ? C47 C48 C49 121.97(12) . . ? C50 C49 C48 117.33(12) . . ? C44 O15 Ni3 125.98(7) . . ? O2 C1 O1 122.41(8) . . ? O2 C1 C2 124.61(10) . . ? O1 C1 C2 112.93(9) . . ? C3 C2 C7 119.33(8) . . ? C3 C2 C1 122.71(10) . . ? C7 C2 C1 117.89(9) . . ? C4 C3 C2 120.60(11) . . ? C3 C4 C5 119.32(11) . . ? O3 C5 C6 114.81(11) . . ? O3 C5 C4 124.68(11) . . ? C6 C5 C4 120.49(10) . . ? C7 C6 C5 119.62(11) . . ? C6 C7 C2 120.62(10) . . ? C9 C8 C13 121.96(10) . . ? C9 C8 O3 120.87(12) . . ? C13 C8 O3 116.85(11) . . ? C8 C9 C10 118.61(11) . . ? C11 C10 C9 120.94(10) . . ? C10 C11 C12 119.01(8) . . ? C10 C11 C14 121.53(8) . . ? C12 C11 C14 119.45(9) . . ? C13 C12 C11 120.56(11) . . ? C8 C13 C12 118.85(11) . . ? O5 C14 O4 126.22(7) . . ? O5 C14 C11 116.37(8) . . ? O4 C14 C11 117.37(7) . . ? N3 C15 C16 123.78(7) . 1_655 ? C15 C16 C17 120.78(9) 1_455 . ? C16 C17 C18 115.52(8) . . ? C16 C17 C51 121.68(8) . . ? C18 C17 C51 122.73(6) . . ? C19 C18 C17 120.06(7) 1_455 . ? N3 C19 C18 123.62(9) . 1_655 ? O7 C20 O6 119.46(8) . . ? O7 C20 C21 121.18(8) . . ? O6 C20 C21 119.33(8) . . ? O7 C20 Ni1 63.07(6) . . ? O6 C20 Ni1 56.74(5) . . ? C21 C20 Ni1 171.65(5) . . ? C22 C21 C26 118.92(8) . . ? C22 C21 C20 122.30(8) . . ? C26 C21 C20 118.78(8) . . ? C21 C22 C23 121.02(8) . . ? C24 C23 C22 119.13(9) . . ? C23 C24 C25 120.57(9) . . ? C23 C24 O8 124.00(8) . . ? C25 C24 O8 115.31(7) . . ? C24 C25 C26 120.40(8) . . ? C25 C26 C21 119.95(8) . . ? C32 C27 C28 121.37(9) . . ? C32 C27 O8 116.35(9) . . ? C28 C27 O8 122.06(9) . . ? C27 C28 C29 118.55(10) . . ? C30 C29 C28 121.18(9) . . ? C31 C30 C29 118.48(8) . . ? C31 C30 C33 120.07(9) . . ? C29 C30 C33 121.42(9) . . ? C32 C31 C30 120.65(10) . . ? C27 C32 C31 119.65(10) . . ? O9 C33 O10 124.47(8) . . ? O9 C33 C30 117.24(8) . . ? O10 C33 C30 118.25(8) . . ? N1 C34 C35 124.15(9) . . ? C34 C35 C36 118.87(7) . . ? C37 C36 C35 117.15(8) . . ? C37 C36 C39 120.92(8) . . ? C35 C36 C39 121.91(7) . . ? C38 C37 C36 119.50(9) . . ? N1 C38 C37 124.11(7) . . ? C40 C39 C43 116.97(8) . . ? C40 C39 C36 122.19(9) . . ? C43 C39 C36 120.84(7) . . ? C39 C40 C41 120.18(9) . . ? N2 C41 C40 122.49(7) . . ? N2 C42 C43 123.36(9) . . ? C39 C43 C42 119.67(7) . . ? O16 C44 O15 125.05(9) . . ? O16 C44 C45 117.34(9) . . ? O15 C44 C45 117.59(9) . . ? C50 C45 C46 118.84(9) . . ? C50 C45 C44 121.70(9) . . ? C46 C45 C44 119.44(10) . . ? C69 C51 C66 115.61(8) . . ? C69 C51 C17 120.78(6) . . ? C66 C51 C17 123.61(8) . . ? C88 C66 C51 120.22(9) . . ? C51 C69 C91 120.82(8) . . ? N4 C88 C66 123.99(7) . . ? N4 C91 C69 123.30(9) . . ? C38 N1 C34 116.15(8) . . ? C38 N1 Ni2 121.63(5) . . ? C34 N1 Ni2 122.21(7) . . ? C42 N2 C41 117.31(8) . . ? C42 N2 Ni3 120.15(7) . . ? C41 N2 Ni3 122.53(5) . . ? C15 N3 C19 116.22(8) . . ? C15 N3 Ni1 122.66(5) . . ? C19 N3 Ni1 120.99(7) . . ? C91 N4 C88 116.00(8) . . ? C91 N4 Ni1 121.24(7) . . ? C88 N4 Ni1 122.71(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 O5 Ni1 O4 C14 29.35(9) 2_785 . . . ? N4 Ni1 O4 C14 115.40(9) . . . . ? N3 Ni1 O4 C14 -61.10(9) . . . . ? O6 Ni1 O4 C14 -152.76(8) . . . . ? O7 Ni1 O4 C14 -152.71(9) . . . . ? C20 Ni1 O4 C14 -150.48(8) . . . . ? O4 Ni1 O6 C20 3.91(8) . . . . ? O5 Ni1 O6 C20 -177.91(5) 2_785 . . . ? N4 Ni1 O6 C20 95.07(5) . . . . ? N3 Ni1 O6 C20 -88.47(5) . . . . ? O7 Ni1 O6 C20 3.86(5) . . . . ? O4 Ni1 O7 C20 176.11(5) . . . . ? O5 Ni1 O7 C20 -7.40(8) 2_785 . . . ? N4 Ni1 O7 C20 -94.78(6) . . . . ? N3 Ni1 O7 C20 84.20(6) . . . . ? O6 Ni1 O7 C20 -3.92(5) . . . . ? O18 Ni2 O10 C33 -173.05(7) . . . . ? O18 Ni2 O10 C33 6.95(7) 2_666 . . . ? O10 Ni2 O10 C33 135(100) 2_666 . . . ? N1 Ni2 O10 C33 -84.37(7) . . . . ? N1 Ni2 O10 C33 95.63(7) 2_666 . . . ? O11 C46 C47 C48 178.69(10) . . . . ? C45 C46 C47 C48 0.48(15) . . . . ? C46 C47 C48 C49 -1.13(17) . . . . ? C45 C50 C49 C48 -0.33(15) . . . . ? C47 C48 C49 C50 1.04(16) . . . . ? O15 Ni3 O15 C44 -3.28(7) 2_655 . . . ? N2 Ni3 O15 C44 63.02(7) . . . . ? N2 Ni3 O15 C44 -116.98(7) 2_655 . . . ? O17 Ni3 O15 C44 156.24(7) . . . . ? O17 Ni3 O15 C44 -23.76(7) 2_655 . . . ? O2 C1 C2 C3 174.41(11) . . . . ? O1 C1 C2 C3 -8.10(15) . . . . ? O2 C1 C2 C7 -8.52(16) . . . . ? O1 C1 C2 C7 168.97(10) . . . . ? C7 C2 C3 C4 -0.66(16) . . . . ? C1 C2 C3 C4 176.38(10) . . . . ? C2 C3 C4 C5 0.01(18) . . . . ? C8 O3 C5 C6 -172.53(11) . . . . ? C8 O3 C5 C4 9.07(19) . . . . ? C3 C4 C5 O3 178.64(11) . . . . ? C3 C4 C5 C6 0.33(19) . . . . ? O3 C5 C6 C7 -178.49(11) . . . . ? C4 C5 C6 C7 -0.01(19) . . . . ? C5 C6 C7 C2 -0.64(18) . . . . ? C3 C2 C7 C6 0.98(17) . . . . ? C1 C2 C7 C6 -176.20(10) . . . . ? C5 O3 C8 C9 65.36(17) . . . . ? C5 O3 C8 C13 -121.04(13) . . . . ? C13 C8 C9 C10 2.40(19) . . . . ? O3 C8 C9 C10 175.67(10) . . . . ? C8 C9 C10 C11 -2.30(17) . . . . ? C9 C10 C11 C12 0.24(15) . . . . ? C9 C10 C11 C14 -179.01(10) . . . . ? C10 C11 C12 C13 1.78(15) . . . . ? C14 C11 C12 C13 -178.95(10) . . . . ? C9 C8 C13 C12 -0.43(19) . . . . ? O3 C8 C13 C12 -173.96(11) . . . . ? C11 C12 C13 C8 -1.71(17) . . . . ? Ni1 O5 C14 O4 -32.95(16) 2_785 . . . ? Ni1 O5 C14 C11 149.40(8) 2_785 . . . ? Ni1 O4 C14 O5 -9.09(14) . . . . ? Ni1 O4 C14 C11 168.53(6) . . . . ? C10 C11 C14 O5 157.53(9) . . . . ? C12 C11 C14 O5 -21.71(12) . . . . ? C10 C11 C14 O4 -20.33(13) . . . . ? C12 C11 C14 O4 160.43(9) . . . . ? C15 C16 C17 C18 0.52(14) 1_455 . . . ? C15 C16 C17 C51 177.59(8) 1_455 . . . ? C16 C17 C18 C19 -0.87(13) . . . 1_455 ? C51 C17 C18 C19 -177.90(9) . . . 1_455 ? Ni1 O7 C20 O6 6.47(8) . . . . ? Ni1 O7 C20 C21 -171.77(8) . . . . ? Ni1 O6 C20 O7 -6.90(9) . . . . ? Ni1 O6 C20 C21 171.37(7) . . . . ? O4 Ni1 C20 O7 -4.49(6) . . . . ? O5 Ni1 C20 O7 175.68(5) 2_785 . . . ? N4 Ni1 C20 O7 86.79(6) . . . . ? N3 Ni1 C20 O7 -95.83(5) . . . . ? O6 Ni1 C20 O7 173.26(8) . . . . ? O4 Ni1 C20 O6 -177.76(4) . . . . ? O5 Ni1 C20 O6 2.41(6) 2_785 . . . ? N4 Ni1 C20 O6 -86.47(5) . . . . ? N3 Ni1 C20 O6 90.90(5) . . . . ? O7 Ni1 C20 O6 -173.26(8) . . . . ? O4 Ni1 C20 C21 118.0(5) . . . . ? O5 Ni1 C20 C21 -61.8(5) 2_785 . . . ? N4 Ni1 C20 C21 -150.7(5) . . . . ? N3 Ni1 C20 C21 26.7(5) . . . . ? O6 Ni1 C20 C21 -64.2(5) . . . . ? O7 Ni1 C20 C21 122.5(5) . . . . ? O7 C20 C21 C22 -12.88(14) . . . . ? O6 C20 C21 C22 168.88(9) . . . . ? Ni1 C20 C21 C22 -131.4(4) . . . . ? O7 C20 C21 C26 167.19(9) . . . . ? O6 C20 C21 C26 -11.06(13) . . . . ? Ni1 C20 C21 C26 48.7(5) . . . . ? C26 C21 C22 C23 -0.77(16) . . . . ? C20 C21 C22 C23 179.29(10) . . . . ? C21 C22 C23 C24 0.30(17) . . . . ? C22 C23 C24 C25 0.12(16) . . . . ? C22 C23 C24 O8 -175.75(10) . . . . ? C27 O8 C24 C23 -29.77(15) . . . . ? C27 O8 C24 C25 154.17(9) . . . . ? C23 C24 C25 C26 -0.03(16) . . . . ? O8 C24 C25 C26 176.18(9) . . . . ? C24 C25 C26 C21 -0.46(16) . . . . ? C22 C21 C26 C25 0.85(15) . . . . ? C20 C21 C26 C25 -179.22(9) . . . . ? C24 O8 C27 C32 132.60(9) . . . . ? C24 O8 C27 C28 -52.83(13) . . . . ? C32 C27 C28 C29 2.30(14) . . . . ? O8 C27 C28 C29 -172.01(8) . . . . ? C27 C28 C29 C30 0.73(14) . . . . ? C28 C29 C30 C31 -3.49(13) . . . . ? C28 C29 C30 C33 174.47(8) . . . . ? C29 C30 C31 C32 3.32(13) . . . . ? C33 C30 C31 C32 -174.67(8) . . . . ? C28 C27 C32 C31 -2.47(14) . . . . ? O8 C27 C32 C31 172.14(8) . . . . ? C30 C31 C32 C27 -0.41(13) . . . . ? Ni2 O10 C33 O9 -2.94(13) . . . . ? Ni2 O10 C33 C30 179.59(5) . . . . ? C31 C30 C33 O9 13.66(12) . . . . ? C29 C30 C33 O9 -164.27(8) . . . . ? C31 C30 C33 O10 -168.68(8) . . . . ? C29 C30 C33 O10 13.38(12) . . . . ? N1 C34 C35 C36 -2.17(15) . . . . ? C34 C35 C36 C37 -0.41(14) . . . . ? C34 C35 C36 C39 177.82(9) . . . . ? C35 C36 C37 C38 1.94(14) . . . . ? C39 C36 C37 C38 -176.30(8) . . . . ? C36 C37 C38 N1 -1.14(15) . . . . ? C37 C36 C39 C40 -152.02(9) . . . . ? C35 C36 C39 C40 29.82(13) . . . . ? C37 C36 C39 C43 27.74(13) . . . . ? C35 C36 C39 C43 -150.42(9) . . . . ? C43 C39 C40 C41 -0.70(13) . . . . ? C36 C39 C40 C41 179.07(8) . . . . ? C39 C40 C41 N2 1.24(13) . . . . ? C40 C39 C43 C42 -0.08(13) . . . . ? C36 C39 C43 C42 -179.85(8) . . . . ? N2 C42 C43 C39 0.41(14) . . . . ? Ni3 O15 C44 O16 3.84(12) . . . . ? Ni3 O15 C44 C45 -177.74(5) . . . . ? C49 C50 C45 C46 -0.28(14) . . . . ? C49 C50 C45 C44 -178.55(9) . . . . ? O11 C46 C45 C50 -177.96(9) . . . . ? C47 C46 C45 C50 0.21(13) . . . . ? O11 C46 C45 C44 0.35(14) . . . . ? C47 C46 C45 C44 178.52(8) . . . . ? O16 C44 C45 C50 177.22(8) . . . . ? O15 C44 C45 C50 -1.33(12) . . . . ? O16 C44 C45 C46 -1.04(12) . . . . ? O15 C44 C45 C46 -179.59(8) . . . . ? C16 C17 C51 C69 -2.24(13) . . . . ? C18 C17 C51 C69 174.61(9) . . . . ? C16 C17 C51 C66 178.31(9) . . . . ? C18 C17 C51 C66 -4.84(13) . . . . ? C69 C51 C66 C88 -2.67(14) . . . . ? C17 C51 C66 C88 176.81(9) . . . . ? C66 C51 C69 C91 2.65(14) . . . . ? C17 C51 C69 C91 -176.85(9) . . . . ? C51 C66 C88 N4 0.90(15) . . . . ? C51 C69 C91 N4 -0.85(15) . . . . ? C37 C38 N1 C34 -1.29(14) . . . . ? C37 C38 N1 Ni2 178.18(7) . . . . ? C35 C34 N1 C38 2.98(14) . . . . ? C35 C34 N1 Ni2 -176.49(7) . . . . ? O18 Ni2 N1 C38 123.38(8) . . . . ? O18 Ni2 N1 C38 -56.62(8) 2_666 . . . ? O10 Ni2 N1 C38 36.39(7) . . . . ? O10 Ni2 N1 C38 -143.61(7) 2_666 . . . ? N1 Ni2 N1 C38 118(100) 2_666 . . . ? O18 Ni2 N1 C34 -57.18(8) . . . . ? O18 Ni2 N1 C34 122.82(8) 2_666 . . . ? O10 Ni2 N1 C34 -144.17(7) . . . . ? O10 Ni2 N1 C34 35.83(7) 2_666 . . . ? N1 Ni2 N1 C34 -62(100) 2_666 . . . ? C43 C42 N2 C41 0.08(13) . . . . ? C43 C42 N2 Ni3 -179.26(7) . . . . ? C40 C41 N2 C42 -0.90(13) . . . . ? C40 C41 N2 Ni3 178.42(6) . . . . ? O15 Ni3 N2 C42 48.18(7) . . . . ? O15 Ni3 N2 C42 -131.82(7) 2_655 . . . ? N2 Ni3 N2 C42 0.00(3) 2_655 . . . ? O17 Ni3 N2 C42 -38.55(7) . . . . ? O17 Ni3 N2 C42 141.45(7) 2_655 . . . ? O15 Ni3 N2 C41 -131.12(7) . . . . ? O15 Ni3 N2 C41 48.88(7) 2_655 . . . ? N2 Ni3 N2 C41 0.00(7) 2_655 . . . ? O17 Ni3 N2 C41 142.15(7) . . . . ? O17 Ni3 N2 C41 -37.85(7) 2_655 . . . ? C16 C15 N3 C19 -1.46(14) 1_655 . . . ? C16 C15 N3 Ni1 174.40(7) 1_655 . . . ? C18 C19 N3 C15 1.08(14) 1_655 . . . ? C18 C19 N3 Ni1 -174.85(8) 1_655 . . . ? O4 Ni1 N3 C15 -13.22(7) . . . . ? O5 Ni1 N3 C15 -133.43(7) 2_785 . . . ? N4 Ni1 N3 C15 -119.3(4) . . . . ? O6 Ni1 N3 C15 137.03(7) . . . . ? O7 Ni1 N3 C15 77.11(7) . . . . ? C20 Ni1 N3 C15 106.76(8) . . . . ? O4 Ni1 N3 C19 162.45(7) . . . . ? O5 Ni1 N3 C19 42.23(7) 2_785 . . . ? N4 Ni1 N3 C19 56.4(4) . . . . ? O6 Ni1 N3 C19 -47.31(7) . . . . ? O7 Ni1 N3 C19 -107.23(8) . . . . ? C20 Ni1 N3 C19 -77.57(8) . . . . ? C69 C91 N4 C88 -1.03(14) . . . . ? C69 C91 N4 Ni1 176.55(8) . . . . ? C66 C88 N4 C91 1.00(14) . . . . ? C66 C88 N4 Ni1 -176.54(8) . . . . ? O4 Ni1 N4 C91 20.07(7) . . . . ? O5 Ni1 N4 C91 140.39(7) 2_785 . . . ? N3 Ni1 N4 C91 126.2(4) . . . . ? O6 Ni1 N4 C91 -130.16(7) . . . . ? O7 Ni1 N4 C91 -70.16(8) . . . . ? C20 Ni1 N4 C91 -99.95(8) . . . . ? O4 Ni1 N4 C88 -162.51(7) . . . . ? O5 Ni1 N4 C88 -42.19(7) 2_785 . . . ? N3 Ni1 N4 C88 -56.4(4) . . . . ? O6 Ni1 N4 C88 47.25(8) . . . . ? O7 Ni1 N4 C88 107.25(8) . . . . ? C20 Ni1 N4 C88 77.47(8) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.577 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.070 data_3 _database_code_depnum_ccdc_archive 'CCDC 884073' #TrackingRef 'web_deposit_cif_file_0_feilonghu_1350638779.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C118 H103 Cu5 N12 O37' _chemical_formula_weight 2598.82 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.858(18) _cell_length_b 15.017(18) _cell_length_c 15.900(18) _cell_angle_alpha 64.059(15) _cell_angle_beta 71.167(15) _cell_angle_gamma 76.371(15) _cell_volume 3001(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8241 _exptl_absorpt_correction_T_max 0.8314 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16864 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10361 _reflns_number_gt 6285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.1230P)^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 10361 _refine_ls_number_parameters 901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.2146 _refine_ls_wR_factor_gt 0.1803 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.60243(6) 1.14895(5) -0.06917(5) 0.0451(2) Uani 1 1 d . . . Cu2 Cu 0.67990(4) 0.68132(5) 0.67635(5) 0.0368(2) Uani 1 1 d . A . Cu3 Cu 0.99024(12) -0.01223(13) 0.53444(11) 0.0478(5) Uani 0.50 1 d P . . N1 N 0.5622(3) 1.2788(3) -0.0439(3) 0.0371(11) Uani 1 1 d . . . N2 N 0.6150(4) 1.0761(3) 0.0709(3) 0.0444(12) Uani 1 1 d . . . N3 N 0.6586(3) 0.7780(3) 0.5445(3) 0.0373(11) Uani 1 1 d . . . N4 N 0.7271(3) 0.5619(3) 0.6289(3) 0.0368(11) Uani 1 1 d . A . O1 O 0.7427(2) 0.5963(3) 0.7920(3) 0.0399(9) Uani 1 1 d . A . O2 O 0.8261(2) 0.6936(3) 0.6554(3) 0.0368(9) Uani 1 1 d . A . O3 O 1.1465(2) 0.4730(3) 0.8904(3) 0.0529(12) Uani 1 1 d . . . O4 O 0.5497(2) 0.6322(3) 0.7369(3) 0.0380(9) Uani 1 1 d . . . O5 O 0.4561(3) 0.7685(3) 0.7498(4) 0.0656(13) Uani 1 1 d . . . O6 O 1.4554(3) 1.1377(3) -0.0514(3) 0.0476(10) Uani 1 1 d . . . O7 O 1.5457(3) 1.2188(3) -0.1936(3) 0.0514(11) Uani 1 1 d . . . O8 O 1.1486(3) 1.3321(4) -0.3059(3) 0.0729(15) Uani 1 1 d . . . O9 O 0.8244(4) 1.0442(4) -0.1357(5) 0.0898(18) Uani 1 1 d . . . O10 O 0.7379(3) 1.1841(3) -0.1326(3) 0.0500(10) Uani 1 1 d . . . O11 O 0.6423(3) 1.0162(3) -0.0913(3) 0.0523(11) Uani 1 1 d . . . H11B H 0.7008 1.0050 -0.1049 0.063 Uiso 1 1 d R . . H11C H 0.6311 0.9580 -0.0412 0.063 Uiso 1 1 d R . . O18 O 0.6547(4) 0.1389(4) 0.3959(4) 0.105(2) Uani 1 1 d . . . H18B H 0.6206 0.0911 0.4213 0.126 Uiso 1 1 d R . . H18A H 0.7150 0.1294 0.3750 0.126 Uiso 1 1 d R . . O20 O 0.3326(4) -0.0003(4) 0.4150(3) 0.0775(15) Uani 1 1 d . . . H20B H 0.3882 0.0154 0.4029 0.093 Uiso 1 1 d R . . H20A H 0.2764 0.0168 0.4432 0.093 Uiso 1 1 d R . . O19 O 0.3380(7) 0.8859(7) 0.3064(7) 0.198(4) Uani 1 1 d . . . H19A H 0.3388 0.9313 0.3244 0.238 Uiso 1 1 d R . . H19B H 0.3464 0.9065 0.2457 0.238 Uiso 1 1 d R . . O21 O 0.6328(3) 0.8017(3) 0.7236(3) 0.0429(9) Uani 1 1 d . . . H21B H 0.5601 0.8097 0.7184 0.052 Uiso 1 1 d R . . H21C H 0.6389 0.8548 0.6766 0.052 Uiso 1 1 d R . . C1 C 0.8212(3) 0.6295(4) 0.7394(4) 0.0327(12) Uani 1 1 d . . . C2 C 0.9081(3) 0.5902(4) 0.7781(4) 0.0346(12) Uani 1 1 d . . . C3 C 0.9029(4) 0.5167(4) 0.8692(4) 0.0420(14) Uani 1 1 d . . . H3 H 0.8450 0.4916 0.9072 0.050 Uiso 1 1 calc R . . C4 C 0.9841(4) 0.4800(5) 0.9043(4) 0.0451(15) Uani 1 1 d . . . H4 H 0.9803 0.4303 0.9659 0.054 Uiso 1 1 calc R . . C5 C 1.0688(4) 0.5156(4) 0.8498(4) 0.0417(14) Uani 1 1 d . . . C6 C 1.0752(4) 0.5883(5) 0.7589(5) 0.0521(17) Uani 1 1 d . . . H6 H 1.1333 0.6128 0.7210 0.063 Uiso 1 1 calc R . . C7 C 0.9947(4) 0.6245(5) 0.7241(4) 0.0471(15) Uani 1 1 d . . . H7 H 0.9992 0.6737 0.6621 0.056 Uiso 1 1 calc R . . C8 C 1.2230(4) 0.5259(5) 0.8581(4) 0.0430(14) Uani 1 1 d . . . C9 C 1.3130(4) 0.4808(5) 0.8303(5) 0.0519(16) Uani 1 1 d . . . H9 H 1.3202 0.4171 0.8315 0.062 Uiso 1 1 calc R . . C10 C 1.3916(4) 0.5291(5) 0.8010(5) 0.0488(16) Uani 1 1 d . . . H10 H 1.4520 0.4972 0.7833 0.059 Uiso 1 1 calc R . . C11 C 1.3835(3) 0.6235(4) 0.7970(4) 0.0368(13) Uani 1 1 d . . . C12 C 1.2935(4) 0.6680(5) 0.8273(4) 0.0475(15) Uani 1 1 d . . . H12 H 1.2865 0.7310 0.8277 0.057 Uiso 1 1 calc R . . C13 C 1.2139(4) 0.6188(5) 0.8569(5) 0.0539(17) Uani 1 1 d . . . H13 H 1.1535 0.6496 0.8762 0.065 Uiso 1 1 calc R . . C14 C 0.7184(4) 0.8446(4) 0.4844(4) 0.0439(14) Uani 1 1 d . . . H14 H 0.7700 0.8467 0.5043 0.053 Uiso 1 1 calc R . . C15 C 0.7093(4) 0.9102(4) 0.3953(4) 0.0461(15) Uani 1 1 d . . . H15 H 0.7536 0.9559 0.3563 0.055 Uiso 1 1 calc R . . C16 C 0.6348(4) 0.9092(4) 0.3626(4) 0.0393(13) Uani 1 1 d . . . C17 C 0.5717(4) 0.8403(5) 0.4253(4) 0.0502(16) Uani 1 1 d . . . H17 H 0.5196 0.8368 0.4069 0.060 Uiso 1 1 calc R . . C18 C 0.5852(4) 0.7776(5) 0.5136(4) 0.0470(15) Uani 1 1 d . . . H18 H 0.5413 0.7321 0.5547 0.056 Uiso 1 1 calc R . . C19 C 0.6263(4) 0.9747(4) 0.2620(4) 0.0412(14) Uani 1 1 d . . . C20 C 0.7011(5) 1.0190(5) 0.1913(4) 0.0553(17) Uani 1 1 d . . . H20 H 0.7577 1.0166 0.2058 0.066 Uiso 1 1 calc R . . C21 C 0.6929(5) 1.0674(5) 0.0978(5) 0.0598(18) Uani 1 1 d . . . H21A H 0.7457 1.0961 0.0502 0.072 Uiso 1 1 calc R . . C22 C 0.5422(5) 0.9851(5) 0.2362(4) 0.0532(16) Uani 1 1 d . . . H22 H 0.4882 0.9581 0.2830 0.064 Uiso 1 1 calc R . . C23 C 0.5396(5) 1.0358(5) 0.1406(5) 0.0552(17) Uani 1 1 d . . . H23 H 0.4831 1.0421 0.1240 0.066 Uiso 1 1 calc R . . C24 C 0.6228(4) 1.3456(5) -0.0762(5) 0.0598(19) Uani 1 1 d . . . H24 H 0.6840 1.3331 -0.1120 0.072 Uiso 1 1 calc R . . C25 C 0.6018(4) 1.4300(4) -0.0609(5) 0.0570(18) Uani 1 1 d . . . H25 H 0.6482 1.4734 -0.0862 0.068 Uiso 1 1 calc R . . C26 C 0.5123(3) 1.4536(4) -0.0079(4) 0.0288(11) Uani 1 1 d . . . C27 C 0.4499(4) 1.3828(5) 0.0289(5) 0.0507(16) Uani 1 1 d . . . H27 H 0.3891 1.3921 0.0672 0.061 Uiso 1 1 calc R . . C28 C 0.4773(4) 1.2989(5) 0.0090(5) 0.0521(16) Uani 1 1 d . . . H28 H 0.4333 1.2530 0.0345 0.063 Uiso 1 1 calc R . . C29 C 0.8155(5) 1.1343(5) -0.1517(4) 0.0522(16) Uani 1 1 d . . . C30 C 0.9045(5) 1.1861(5) -0.1938(4) 0.0540(17) Uani 1 1 d . . . C31 C 0.9934(5) 1.1378(5) -0.2226(5) 0.0638(19) Uani 1 1 d . . . H31 H 0.9979 1.0730 -0.2178 0.077 Uiso 1 1 calc R . . C32 C 1.0741(5) 1.1843(6) -0.2580(5) 0.071(2) Uani 1 1 d . . . H32 H 1.1333 1.1510 -0.2764 0.085 Uiso 1 1 calc R . . C33 C 1.0679(5) 1.2797(6) -0.2663(5) 0.0595(18) Uani 1 1 d . . . C34 C 0.9817(5) 1.3317(6) -0.2419(5) 0.0645(19) Uani 1 1 d . . . H34 H 0.9777 1.3975 -0.2497 0.077 Uiso 1 1 calc R . . C35 C 0.9017(5) 1.2833(5) -0.2054(5) 0.0602(18) Uani 1 1 d . . . H35 H 0.8427 1.3174 -0.1877 0.072 Uiso 1 1 calc R . . C36 C 1.2231(5) 1.2931(5) -0.2600(5) 0.0589(18) Uani 1 1 d . . . C37 C 1.2126(5) 1.2326(5) -0.1651(5) 0.0633(19) Uani 1 1 d . . . H37 H 1.1528 1.2132 -0.1262 0.076 Uiso 1 1 calc R . . C38 C 1.2906(5) 1.2003(5) -0.1267(5) 0.0555(17) Uani 1 1 d . . . H38 H 1.2828 1.1592 -0.0616 0.067 Uiso 1 1 calc R . . C39 C 1.3792(5) 1.2270(4) -0.1818(4) 0.0476(15) Uani 1 1 d . . . C40 C 1.3899(5) 1.2895(5) -0.2790(5) 0.0550(17) Uani 1 1 d . . . H40 H 1.4498 1.3083 -0.3180 0.066 Uiso 1 1 calc R . . C41 C 1.3109(5) 1.3236(5) -0.3174(5) 0.0597(18) Uani 1 1 d . . . H41 H 1.3172 1.3670 -0.3818 0.072 Uiso 1 1 calc R . . C42 C 1.4654(5) 1.1920(4) -0.1412(5) 0.0479(15) Uani 1 1 d . . . C43 C 0.8061(4) 0.5624(5) 0.5583(4) 0.0509(16) Uani 1 1 d . . . H43 H 0.8347 0.6212 0.5227 0.061 Uiso 1 1 calc R . . C44 C 0.8476(5) 0.4818(5) 0.5350(5) 0.0552(17) Uani 1 1 d . . . H44 H 0.9035 0.4866 0.4858 0.066 Uiso 1 1 calc R . . C45 C 0.8065(4) 0.3931(4) 0.5843(5) 0.0489(16) Uani 1 1 d . . . C46 C 0.7226(4) 0.3948(5) 0.6531(6) 0.066(2) Uani 1 1 d . . . H46 H 0.6895 0.3388 0.6868 0.079 Uiso 1 1 calc R . . N5 N 0.9446(8) 0.1430(9) 0.4970(9) 0.047(3) Uani 0.50 1 d P . 1 C51 C 0.8078(8) 0.2601(9) 0.5225(10) 0.050(3) Uani 0.50 1 d P A 1 H51 H 0.7439 0.2823 0.5222 0.060 Uiso 0.50 1 calc PR A 1 C48 C 0.858(4) 0.308(5) 0.548(3) 0.046(8) Uani 0.50 1 d P A 1 C52 C 0.8528(8) 0.1792(9) 0.4971(10) 0.053(3) Uani 0.50 1 d P A 1 H52 H 0.8178 0.1492 0.4795 0.063 Uiso 0.50 1 calc PR A 1 N5' N 0.9297(9) 0.1207(9) 0.5594(10) 0.048(3) Uani 0.50 1 d P . 2 C52' C 0.8342(9) 0.1352(10) 0.6056(11) 0.059(4) Uani 0.50 1 d P . 2 H52' H 0.7967 0.0834 0.6304 0.070 Uiso 0.50 1 calc PR . 2 C51' C 0.7933(9) 0.2214(10) 0.6161(11) 0.056(3) Uani 0.50 1 d P . 2 H51' H 0.7289 0.2267 0.6481 0.067 Uiso 0.50 1 calc PR . 2 C48' C 0.843(4) 0.301(5) 0.581(3) 0.047(8) Uani 0.50 1 d P . 2 C49 C 0.9475(4) 0.2778(4) 0.5428(4) 0.0464(15) Uani 1 1 d . . . H49 H 0.9858 0.3133 0.5502 0.056 Uiso 1 1 calc R A 1 C50 C 0.9855(4) 0.1931(5) 0.5260(5) 0.0502(16) Uani 1 1 d . . . H50 H 1.0464 0.1668 0.5355 0.060 Uiso 1 1 calc R B 1 C47 C 0.6869(4) 0.4794(5) 0.6726(5) 0.0548(17) Uani 1 1 d . . . H47 H 0.6301 0.4774 0.7202 0.066 Uiso 1 1 calc R A . C59 C 0.4698(4) 0.6796(4) 0.7588(4) 0.0372(13) Uani 1 1 d . . 1 O13 O 1.1469(10) -0.1013(10) 0.7291(10) 0.074(4) Uani 0.50 1 d P . 1 O12 O 1.099(3) -0.0226(17) 0.587(3) 0.053(7) Uani 0.50 1 d P . 1 C61 C 1.0887(13) -0.0768(12) 0.6768(15) 0.051(4) Uani 0.50 1 d P . 1 C62 C 0.994(7) -0.118(5) 0.727(4) 0.054(12) Uani 0.50 1 d P . 1 C63 C 0.9691(15) -0.1795(14) 0.8291(14) 0.060(5) Uani 0.50 1 d P . 1 C64 C 0.8809(13) -0.2189(13) 0.8741(13) 0.066(4) Uani 0.50 1 d P . 1 C65 C 0.8204(13) -0.1962(13) 0.8159(15) 0.059(4) Uani 0.50 1 d P . 1 C66 C 0.850(4) -0.136(4) 0.715(3) 0.060(12) Uani 0.50 1 d P . 1 H66 H 0.8956 -0.1910 0.7175 0.072 Uiso 0.50 1 calc PR . 1 N6 N 0.9329(10) -0.0999(9) 0.6778(11) 0.046(3) Uani 0.50 1 d P . 1 O22 O 0.0450(11) 0.0709(9) 0.0085(9) 0.135(5) Uani 0.50 1 d P . . H22A H 0.0305 0.0850 -0.0438 0.161 Uiso 1 1 d R . . H22B H -0.0123 0.0694 0.0430 0.161 Uiso 1 1 d R . . O14 O 0.8763(8) 0.0065(9) 0.4771(9) 0.051(3) Uani 0.50 1 d P . 1 O15 O 0.8345(10) 0.0864(11) 0.3348(11) 0.078(4) Uani 0.50 1 d P . 1 C67 C 0.893(5) 0.056(3) 0.388(5) 0.049(8) Uani 0.50 1 d P . 1 C72 C 1.1366(13) 0.0944(13) 0.3481(14) 0.056(4) Uani 0.50 1 d P . 1 N7 N 1.0517(9) 0.0725(9) 0.3862(12) 0.046(3) Uani 0.50 1 d P . 1 C68 C 0.9880(16) 0.0927(15) 0.3363(15) 0.055(5) Uani 0.50 1 d P . 1 C69 C 1.018(7) 0.138(5) 0.237(4) 0.056(14) Uani 0.50 1 d P . 1 H69 H 1.0824 0.1210 0.2383 0.067 Uiso 0.50 1 calc PR . 1 C70 C 1.1099(13) 0.1674(14) 0.1898(15) 0.070(4) Uani 0.50 1 d P . 1 C71 C 1.170(4) 0.146(4) 0.248(3) 0.059(12) Uani 0.50 1 d P . 1 H71 H 1.2138 0.0909 0.2458 0.071 Uiso 0.50 1 calc PR . 1 O23 O 0.3711(9) 0.6952(10) 0.5418(9) 0.270(6) Uani 1 1 d . . . H23C H 0.3966 0.7351 0.4854 0.324 Uiso 1 1 d R . . H23A H 0.3145 0.6931 0.5779 0.324 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0680(5) 0.0295(4) 0.0388(4) -0.0120(3) -0.0211(4) 0.0008(3) Cu2 0.0260(4) 0.0439(4) 0.0383(4) -0.0116(3) -0.0098(3) -0.0065(3) Cu3 0.0359(9) 0.0374(10) 0.0698(15) -0.0249(14) -0.0093(12) -0.0016(8) N1 0.044(3) 0.029(3) 0.039(3) -0.016(2) -0.006(2) -0.005(2) N2 0.063(3) 0.033(3) 0.038(3) -0.010(2) -0.019(3) -0.005(2) N3 0.035(3) 0.038(3) 0.037(3) -0.009(2) -0.014(2) -0.005(2) N4 0.028(2) 0.034(3) 0.044(3) -0.008(2) -0.011(2) -0.005(2) O1 0.0213(19) 0.054(3) 0.039(2) -0.0098(19) -0.0077(16) -0.0113(17) O2 0.0277(19) 0.043(2) 0.035(2) -0.0063(18) -0.0105(16) -0.0099(17) O3 0.025(2) 0.048(3) 0.072(3) -0.002(2) -0.022(2) -0.0118(18) O4 0.0219(19) 0.039(2) 0.048(2) -0.0125(19) -0.0093(17) -0.0033(16) O5 0.033(2) 0.047(3) 0.110(4) -0.029(3) -0.012(2) -0.006(2) O6 0.072(3) 0.032(2) 0.042(2) -0.0100(19) -0.026(2) -0.006(2) O7 0.067(3) 0.042(3) 0.043(2) -0.013(2) -0.023(2) 0.004(2) O8 0.057(3) 0.073(3) 0.060(3) 0.002(3) -0.025(3) 0.000(3) O9 0.074(3) 0.045(3) 0.137(5) -0.045(3) -0.006(3) 0.009(3) O10 0.059(3) 0.035(2) 0.050(3) -0.018(2) -0.010(2) 0.004(2) O11 0.077(3) 0.034(2) 0.053(3) -0.019(2) -0.031(2) 0.005(2) O18 0.106(5) 0.076(4) 0.091(4) -0.012(3) -0.022(4) 0.018(3) O20 0.085(4) 0.069(3) 0.070(3) -0.013(3) -0.015(3) -0.028(3) O19 0.203(10) 0.200(10) 0.165(8) -0.064(8) -0.014(7) -0.034(8) O21 0.036(2) 0.050(2) 0.047(2) -0.020(2) -0.0111(18) -0.0084(18) C1 0.024(3) 0.040(3) 0.033(3) -0.013(3) -0.007(2) -0.007(2) C2 0.024(3) 0.040(3) 0.039(3) -0.013(3) -0.008(2) -0.008(2) C3 0.026(3) 0.052(4) 0.041(3) -0.007(3) -0.009(2) -0.013(3) C4 0.028(3) 0.054(4) 0.043(3) -0.002(3) -0.011(3) -0.016(3) C5 0.024(3) 0.048(4) 0.051(4) -0.012(3) -0.014(3) -0.007(3) C6 0.022(3) 0.060(4) 0.056(4) -0.005(3) -0.005(3) -0.014(3) C7 0.031(3) 0.055(4) 0.040(3) -0.001(3) -0.011(3) -0.010(3) C8 0.026(3) 0.047(4) 0.051(4) -0.009(3) -0.015(3) -0.007(3) C9 0.034(3) 0.045(4) 0.074(5) -0.023(3) -0.012(3) -0.002(3) C10 0.020(3) 0.046(4) 0.076(4) -0.022(3) -0.011(3) 0.000(3) C11 0.022(3) 0.046(4) 0.043(3) -0.014(3) -0.016(2) 0.000(2) C12 0.029(3) 0.047(4) 0.065(4) -0.022(3) -0.005(3) -0.009(3) C13 0.024(3) 0.055(4) 0.068(4) -0.020(4) -0.004(3) 0.002(3) C14 0.039(3) 0.052(4) 0.043(3) -0.011(3) -0.021(3) -0.009(3) C15 0.051(4) 0.047(4) 0.043(4) -0.013(3) -0.016(3) -0.015(3) C16 0.043(3) 0.040(3) 0.039(3) -0.017(3) -0.016(3) -0.002(3) C17 0.052(4) 0.056(4) 0.049(4) -0.012(3) -0.027(3) -0.013(3) C18 0.046(4) 0.051(4) 0.045(4) -0.009(3) -0.020(3) -0.015(3) C19 0.053(4) 0.036(3) 0.037(3) -0.011(3) -0.021(3) -0.005(3) C20 0.064(4) 0.057(4) 0.042(4) -0.002(3) -0.023(3) -0.022(3) C21 0.066(4) 0.059(4) 0.046(4) -0.005(3) -0.017(3) -0.017(4) C22 0.064(4) 0.057(4) 0.039(4) -0.014(3) -0.018(3) -0.009(3) C23 0.067(4) 0.056(4) 0.046(4) -0.017(3) -0.026(4) -0.001(3) C24 0.043(4) 0.040(4) 0.075(5) -0.027(4) 0.020(3) -0.008(3) C25 0.041(4) 0.034(4) 0.080(5) -0.027(3) 0.020(3) -0.018(3) C26 0.025(3) 0.030(3) 0.031(3) -0.012(2) -0.005(2) -0.004(2) C27 0.030(3) 0.049(4) 0.077(5) -0.038(4) 0.005(3) -0.010(3) C28 0.045(4) 0.045(4) 0.073(5) -0.031(4) -0.004(3) -0.015(3) C29 0.063(4) 0.042(4) 0.045(4) -0.020(3) -0.012(3) 0.007(3) C30 0.064(4) 0.048(4) 0.049(4) -0.023(3) -0.019(3) 0.013(3) C31 0.065(5) 0.052(4) 0.070(5) -0.032(4) -0.011(4) 0.011(4) C32 0.059(5) 0.066(5) 0.071(5) -0.025(4) -0.010(4) 0.011(4) C33 0.062(5) 0.062(5) 0.047(4) -0.012(4) -0.023(3) 0.001(4) C34 0.067(5) 0.061(5) 0.063(5) -0.028(4) -0.014(4) 0.003(4) C35 0.057(4) 0.051(4) 0.065(5) -0.026(4) -0.011(4) 0.009(3) C36 0.065(5) 0.054(4) 0.054(4) -0.015(4) -0.028(4) 0.003(4) C37 0.063(4) 0.060(5) 0.053(4) -0.009(4) -0.019(4) -0.003(4) C38 0.069(5) 0.045(4) 0.043(4) -0.006(3) -0.023(4) -0.001(3) C39 0.070(4) 0.032(3) 0.047(4) -0.018(3) -0.026(3) 0.003(3) C40 0.064(4) 0.053(4) 0.046(4) -0.015(3) -0.023(3) 0.000(3) C41 0.070(5) 0.058(4) 0.043(4) -0.010(3) -0.021(4) -0.001(4) C42 0.072(5) 0.032(3) 0.049(4) -0.020(3) -0.029(4) 0.006(3) C43 0.053(4) 0.037(4) 0.054(4) -0.016(3) 0.000(3) -0.012(3) C44 0.054(4) 0.045(4) 0.057(4) -0.021(3) -0.003(3) -0.004(3) C45 0.042(4) 0.038(4) 0.072(4) -0.018(3) -0.026(3) -0.004(3) C46 0.037(4) 0.039(4) 0.098(6) -0.006(4) -0.009(4) -0.015(3) N5 0.033(6) 0.037(7) 0.064(8) -0.020(7) -0.009(7) 0.003(5) C51 0.031(6) 0.037(7) 0.078(10) -0.026(7) -0.009(6) 0.003(5) C48 0.037(16) 0.036(13) 0.07(2) -0.03(2) -0.008(17) -0.003(10) C52 0.035(7) 0.044(8) 0.080(10) -0.025(7) -0.015(7) -0.004(6) N5' 0.037(7) 0.037(7) 0.068(8) -0.022(7) -0.013(7) 0.002(5) C52' 0.041(7) 0.041(8) 0.085(11) -0.020(8) -0.008(7) -0.007(6) C51' 0.034(7) 0.041(8) 0.082(11) -0.024(8) -0.002(7) -0.002(6) C48' 0.036(19) 0.039(12) 0.07(2) -0.02(2) -0.016(18) -0.003(12) C49 0.045(4) 0.040(4) 0.059(4) -0.021(3) -0.015(3) -0.008(3) C50 0.038(3) 0.043(4) 0.068(4) -0.018(3) -0.019(3) -0.004(3) C47 0.032(3) 0.044(4) 0.073(5) -0.014(4) -0.003(3) -0.009(3) C59 0.026(3) 0.042(4) 0.038(3) -0.007(3) -0.011(2) -0.008(3) O13 0.049(7) 0.072(8) 0.090(9) -0.010(9) -0.031(8) -0.014(6) O12 0.032(10) 0.042(14) 0.08(3) -0.020(18) -0.009(10) -0.007(12) C61 0.035(10) 0.035(9) 0.079(13) -0.021(10) -0.012(10) -0.007(6) C62 0.05(3) 0.04(3) 0.07(4) -0.03(3) -0.01(4) -0.01(2) C63 0.052(10) 0.051(12) 0.072(13) -0.024(10) -0.008(12) -0.006(9) C64 0.064(11) 0.060(11) 0.063(11) -0.016(9) -0.014(10) -0.009(9) C65 0.055(10) 0.052(11) 0.067(13) -0.020(9) -0.005(10) -0.019(9) C66 0.05(2) 0.052(16) 0.07(3) -0.02(2) -0.01(2) -0.011(15) N6 0.034(8) 0.040(7) 0.064(9) -0.022(7) -0.010(9) -0.005(6) O22 0.163(13) 0.096(10) 0.082(9) 0.015(8) -0.040(9) 0.010(9) O14 0.039(6) 0.041(6) 0.068(8) -0.022(7) -0.008(5) -0.003(5) O15 0.049(9) 0.069(8) 0.096(10) -0.006(9) -0.024(9) -0.018(6) C67 0.037(14) 0.04(2) 0.07(3) -0.02(2) -0.021(15) -0.003(18) C72 0.047(10) 0.046(10) 0.074(13) -0.026(9) -0.011(11) -0.006(8) N7 0.031(7) 0.035(7) 0.067(9) -0.017(8) -0.003(8) -0.014(5) C68 0.047(12) 0.042(10) 0.069(14) -0.019(12) -0.010(13) -0.003(8) C69 0.05(3) 0.05(3) 0.07(4) -0.02(3) -0.02(4) -0.01(2) C70 0.061(13) 0.063(12) 0.083(14) -0.030(10) -0.012(12) -0.007(11) C71 0.05(2) 0.056(18) 0.08(4) -0.03(2) -0.01(2) -0.013(15) O23 0.233(13) 0.277(15) 0.246(14) -0.051(12) -0.062(11) -0.036(11) _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 O10 2.018(5) . ? Cu1 N2 2.057(5) . ? Cu1 N1 2.074(5) . ? Cu1 O11 2.090(4) . ? Cu1 O7 2.138(4) 1_455 ? Cu1 O6 2.149(5) 1_455 ? Cu1 C42 2.472(7) 1_455 ? Cu2 O4 2.016(4) . ? Cu2 N3 2.037(5) . ? Cu2 O1 2.091(4) . ? Cu2 N4 2.128(5) . ? Cu2 O2 2.129(4) . ? Cu2 O21 2.138(4) . ? Cu2 C1 2.435(5) . ? Cu3 Cu3 0.955(3) 2_756 ? Cu3 N7 1.249(15) 2_756 ? Cu3 O14 1.950(11) 2_756 ? Cu3 C68 1.96(2) 2_756 ? Cu3 O12 2.00(3) . ? Cu3 N6 2.075(15) . ? Cu3 O14 2.079(11) . ? Cu3 N7 2.131(16) . ? Cu3 N5 2.133(12) . ? Cu3 N5' 2.137(12) . ? Cu3 N5 2.167(12) 2_756 ? Cu3 C67 2.26(5) 2_756 ? N1 C28 1.322(7) . ? N1 C24 1.326(7) . ? N2 C21 1.319(8) . ? N2 C23 1.334(8) . ? N3 C14 1.319(7) . ? N3 C18 1.334(7) . ? N4 C47 1.305(7) . ? N4 C43 1.335(7) . ? O1 C1 1.260(6) . ? O2 C1 1.250(6) . ? O3 C8 1.371(6) . ? O3 C5 1.389(6) . ? O4 C59 1.260(6) . ? O5 C59 1.252(7) . ? O6 C42 1.275(7) . ? O6 Cu1 2.149(5) 1_655 ? O7 C42 1.253(8) . ? O7 Cu1 2.138(4) 1_655 ? O8 C36 1.393(7) . ? O8 C33 1.406(8) . ? O9 C29 1.244(8) . ? O10 C29 1.244(7) . ? O11 H11B 0.8199 . ? O11 H11C 0.8944 . ? O18 H18B 0.8499 . ? O18 H18A 0.8501 . ? O20 H20B 0.8500 . ? O20 H20A 0.8500 . ? O19 H19A 0.8500 . ? O19 H19B 0.8500 . ? O21 H21B 1.0843 . ? O21 H21C 0.8200 . ? C1 C2 1.493(7) . ? C2 C7 1.367(7) . ? C2 C3 1.376(7) . ? C3 C4 1.387(7) . ? C3 H3 0.9300 . ? C4 C5 1.351(7) . ? C4 H4 0.9300 . ? C5 C6 1.367(8) . ? C6 C7 1.375(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.362(9) . ? C8 C9 1.377(8) . ? C9 C10 1.363(8) . ? C9 H9 0.9300 . ? C10 C11 1.370(8) . ? C10 H10 0.9300 . ? C11 C12 1.383(8) . ? C11 C59 1.511(7) 1_655 ? C12 C13 1.383(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.354(7) . ? C14 H14 0.9300 . ? C15 C16 1.373(7) . ? C15 H15 0.9300 . ? C16 C17 1.376(8) . ? C16 C19 1.495(8) . ? C17 C18 1.356(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.353(8) . ? C19 C22 1.391(8) . ? C20 C21 1.373(8) . ? C20 H20 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.380(8) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.340(8) . ? C24 H24 0.9300 . ? C25 C26 1.386(7) . ? C25 H25 0.9300 . ? C26 C27 1.379(7) . ? C26 C26 1.464(10) 2_685 ? C27 C28 1.370(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.504(10) . ? C30 C35 1.380(9) . ? C30 C31 1.389(9) . ? C31 C32 1.362(10) . ? C31 H31 0.9300 . ? C32 C33 1.363(10) . ? C32 H32 0.9300 . ? C33 C34 1.369(9) . ? C34 C35 1.369(9) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.358(9) . ? C36 C41 1.376(9) . ? C37 C38 1.372(9) . ? C37 H37 0.9300 . ? C38 C39 1.363(9) . ? C38 H38 0.9300 . ? C39 C40 1.393(8) . ? C39 C42 1.501(8) . ? C40 C41 1.384(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 Cu1 2.472(7) 1_655 ? C43 C44 1.370(8) . ? C43 H43 0.9300 . ? C44 C45 1.386(8) . ? C44 H44 0.9300 . ? C45 C46 1.373(9) . ? C45 C48' 1.38(6) . ? C45 C48 1.57(6) . ? C46 C47 1.382(9) . ? C46 H46 0.9300 . ? N5 C52 1.344(16) . ? N5 C50 1.359(14) . ? N5 Cu3 2.167(12) 2_756 ? C51 C48 1.39(7) . ? C51 C52 1.400(16) . ? C51 H51 0.9300 . ? C48 C49 1.28(6) . ? C52 H52 0.9300 . ? N5' C50 1.338(13) . ? N5' C52' 1.386(17) . ? C52' C51' 1.351(17) . ? C52' H52' 0.9300 . ? C51' C48' 1.36(6) . ? C51' H51' 0.9300 . ? C48' C49 1.49(5) . ? C49 C50 1.366(8) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C47 H47 0.9300 . ? C59 C11 1.511(7) 1_455 ? O13 O15 0.900(14) 2_756 ? O13 C61 1.27(3) . ? O13 C67 1.93(6) 2_756 ? O12 C67 0.50(5) 2_756 ? O12 O14 0.91(5) 2_756 ? O12 C61 1.27(4) . ? O12 O15 1.65(3) 2_756 ? O12 C68 1.66(4) 2_756 ? C61 C67 0.90(8) 2_756 ? C61 O15 1.081(19) 2_756 ? C61 C68 1.31(3) 2_756 ? C61 C62 1.50(8) . ? C61 C69 1.85(8) 2_756 ? C62 C69 0.51(9) 2_756 ? C62 C68 0.88(5) 2_756 ? C62 N6 1.30(10) . ? C62 C63 1.44(5) . ? C62 C70 1.75(8) 2_756 ? C62 N7 1.92(8) 2_756 ? C63 C69 0.94(5) 2_756 ? C63 C70 1.26(3) 2_756 ? C63 C64 1.40(3) . ? C64 C70 0.96(2) 2_756 ? C64 C65 1.38(3) . ? C64 C69 2.03(7) 2_756 ? C65 C71 0.96(5) 2_756 ? C65 C70 1.18(2) 2_756 ? C65 C66 1.43(5) . ? C66 C71 0.53(7) 2_756 ? C66 C72 0.91(4) 2_756 ? C66 N6 1.31(6) . ? C66 C70 1.64(6) 2_756 ? C66 N7 1.85(5) 2_756 ? C66 H66 0.9300 . ? N6 N7 0.886(14) 2_756 ? N6 C68 1.15(3) 2_756 ? N6 C72 1.20(2) 2_756 ? N6 C69 1.56(9) 2_756 ? N6 C71 1.68(5) 2_756 ? N6 C70 1.85(3) 2_756 ? O22 H22A 0.8500 . ? O22 H22B 0.8500 . ? O14 O12 0.91(5) 2_756 ? O14 C67 1.25(7) . ? O14 Cu3 1.950(11) 2_756 ? O15 O13 0.900(14) 2_756 ? O15 C61 1.081(19) 2_756 ? O15 C67 1.28(5) . ? O15 O12 1.65(3) 2_756 ? C67 O12 0.50(5) 2_756 ? C67 C61 0.90(8) 2_756 ? C67 C68 1.48(7) . ? C67 O13 1.93(6) 2_756 ? C67 Cu3 2.26(5) 2_756 ? C72 C66 0.91(4) 2_756 ? C72 N6 1.20(2) 2_756 ? C72 N7 1.26(2) . ? C72 C71 1.40(5) . ? C72 Cu3 2.318(19) 2_756 ? N7 N6 0.886(14) 2_756 ? N7 Cu3 1.249(15) 2_756 ? N7 C68 1.33(3) . ? N7 C66 1.85(5) 2_756 ? N7 C62 1.92(8) 2_756 ? C68 C62 0.88(5) 2_756 ? C68 N6 1.15(3) 2_756 ? C68 C61 1.31(3) 2_756 ? C68 C69 1.38(5) . ? C68 O12 1.66(4) 2_756 ? C68 Cu3 1.96(2) 2_756 ? C69 C62 0.51(9) 2_756 ? C69 C63 0.94(5) 2_756 ? C69 C70 1.39(9) . ? C69 N6 1.56(9) 2_756 ? C69 C61 1.85(8) 2_756 ? C69 C64 2.03(7) 2_756 ? C69 H69 0.9300 . ? C70 C64 0.96(2) 2_756 ? C70 C65 1.18(2) 2_756 ? C70 C63 1.26(3) 2_756 ? C70 C71 1.38(6) . ? C70 C66 1.64(6) 2_756 ? C70 C62 1.75(8) 2_756 ? C70 N6 1.85(3) 2_756 ? C71 C66 0.53(7) 2_756 ? C71 C65 0.96(5) 2_756 ? C71 N6 1.68(5) 2_756 ? C71 H71 0.9300 . ? O23 H23C 0.8501 . ? O23 H23A 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Cu1 N2 97.8(2) . . ? O10 Cu1 N1 90.56(17) . . ? N2 Cu1 N1 87.45(19) . . ? O10 Cu1 O11 90.01(17) . . ? N2 Cu1 O11 91.33(18) . . ? N1 Cu1 O11 178.71(17) . . ? O10 Cu1 O7 99.13(19) . 1_455 ? N2 Cu1 O7 162.9(2) . 1_455 ? N1 Cu1 O7 90.12(17) . 1_455 ? O11 Cu1 O7 90.93(16) . 1_455 ? O10 Cu1 O6 160.59(16) . 1_455 ? N2 Cu1 O6 101.63(18) . 1_455 ? N1 Cu1 O6 90.21(17) . 1_455 ? O11 Cu1 O6 89.64(16) . 1_455 ? O7 Cu1 O6 61.46(17) 1_455 1_455 ? O10 Cu1 C42 129.6(2) . 1_455 ? N2 Cu1 C42 132.5(2) . 1_455 ? N1 Cu1 C42 89.03(18) . 1_455 ? O11 Cu1 C42 91.50(17) . 1_455 ? O7 Cu1 C42 30.46(18) 1_455 1_455 ? O6 Cu1 C42 31.05(19) 1_455 1_455 ? O4 Cu2 N3 98.19(17) . . ? O4 Cu2 O1 99.06(15) . . ? N3 Cu2 O1 162.74(16) . . ? O4 Cu2 N4 88.52(17) . . ? N3 Cu2 N4 91.37(19) . . ? O1 Cu2 N4 88.46(17) . . ? O4 Cu2 O2 160.83(15) . . ? N3 Cu2 O2 100.75(16) . . ? O1 Cu2 O2 61.99(14) . . ? N4 Cu2 O2 88.08(16) . . ? O4 Cu2 O21 91.64(15) . . ? N3 Cu2 O21 88.49(18) . . ? O1 Cu2 O21 91.63(16) . . ? N4 Cu2 O21 179.80(18) . . ? O2 Cu2 O21 91.80(14) . . ? O4 Cu2 C1 130.07(18) . . ? N3 Cu2 C1 131.59(18) . . ? O1 Cu2 C1 31.16(15) . . ? N4 Cu2 C1 86.88(17) . . ? O2 Cu2 C1 30.86(15) . . ? O21 Cu2 C1 93.11(16) . . ? Cu3 Cu3 N7 150.3(7) 2_756 2_756 ? Cu3 Cu3 O14 83.9(4) 2_756 2_756 ? N7 Cu3 O14 114.7(7) 2_756 2_756 ? Cu3 Cu3 C68 152.8(7) 2_756 2_756 ? N7 Cu3 C68 41.7(10) 2_756 2_756 ? O14 Cu3 C68 73.8(8) 2_756 2_756 ? Cu3 Cu3 O12 110.4(14) 2_756 . ? N7 Cu3 O12 91.3(13) 2_756 . ? O14 Cu3 O12 26.6(14) 2_756 . ? C68 Cu3 O12 49.6(13) 2_756 . ? Cu3 Cu3 N6 161.6(4) 2_756 . ? N7 Cu3 N6 11.4(8) 2_756 . ? O14 Cu3 N6 106.6(6) 2_756 . ? C68 Cu3 N6 32.8(7) 2_756 . ? O12 Cu3 N6 81.8(13) . . ? Cu3 Cu3 O14 68.9(4) 2_756 . ? N7 Cu3 O14 90.4(8) 2_756 . ? O14 Cu3 O14 152.82(17) 2_756 . ? C68 Cu3 O14 132.1(8) 2_756 . ? O12 Cu3 O14 177.1(9) . . ? N6 Cu3 O14 99.7(5) . . ? Cu3 Cu3 N7 16.9(4) 2_756 . ? N7 Cu3 N7 167.2(3) 2_756 . ? O14 Cu3 N7 73.0(5) 2_756 . ? C68 Cu3 N7 146.7(8) 2_756 . ? O12 Cu3 N7 98.2(13) . . ? N6 Cu3 N7 177.7(5) . . ? O14 Cu3 N7 80.5(5) . . ? Cu3 Cu3 N5 79.2(4) 2_756 . ? N7 Cu3 N5 118.5(7) 2_756 . ? O14 Cu3 N5 97.0(5) 2_756 . ? C68 Cu3 N5 118.3(7) 2_756 . ? O12 Cu3 N5 98.7(9) . . ? N6 Cu3 N5 113.6(5) . . ? O14 Cu3 N5 78.4(5) . . ? N7 Cu3 N5 68.7(5) . . ? Cu3 Cu3 N5' 102.5(4) 2_756 . ? N7 Cu3 N5' 97.5(7) 2_756 . ? O14 Cu3 N5' 98.4(5) 2_756 . ? C68 Cu3 N5' 96.2(7) 2_756 . ? O12 Cu3 N5' 89.6(12) . . ? N6 Cu3 N5' 91.1(5) . . ? O14 Cu3 N5' 87.8(5) . . ? N7 Cu3 N5' 91.1(5) . . ? N5 Cu3 N5' 23.3(3) . . ? Cu3 Cu3 N5 75.2(4) 2_756 2_756 ? N7 Cu3 N5 85.0(7) 2_756 2_756 ? O14 Cu3 N5 80.4(5) 2_756 2_756 ? C68 Cu3 N5 85.7(7) 2_756 2_756 ? O12 Cu3 N5 90.3(12) . 2_756 ? N6 Cu3 N5 91.4(5) . 2_756 ? O14 Cu3 N5 92.2(5) . 2_756 ? N7 Cu3 N5 86.4(5) . 2_756 ? N5 Cu3 N5 154.36(17) . 2_756 ? N5' Cu3 N5 177.5(4) . 2_756 ? Cu3 Cu3 C67 117(2) 2_756 2_756 ? N7 Cu3 C67 81.8(18) 2_756 2_756 ? O14 Cu3 C67 34(2) 2_756 2_756 ? C68 Cu3 C67 40.3(19) 2_756 2_756 ? O12 Cu3 C67 11.6(15) . 2_756 ? N6 Cu3 C67 73.1(18) . 2_756 ? O14 Cu3 C67 171.1(13) . 2_756 ? N7 Cu3 C67 106.5(19) . 2_756 ? N5 Cu3 C67 109.0(12) . 2_756 ? N5' Cu3 C67 97.4(16) . 2_756 ? N5 Cu3 C67 82.9(16) 2_756 2_756 ? C28 N1 C24 115.1(5) . . ? C28 N1 Cu1 123.3(4) . . ? C24 N1 Cu1 121.5(4) . . ? C21 N2 C23 116.8(5) . . ? C21 N2 Cu1 124.4(4) . . ? C23 N2 Cu1 118.9(4) . . ? C14 N3 C18 116.3(5) . . ? C14 N3 Cu2 120.8(4) . . ? C18 N3 Cu2 122.8(4) . . ? C47 N4 C43 115.3(5) . . ? C47 N4 Cu2 122.5(4) . . ? C43 N4 Cu2 121.9(4) . . ? C1 O1 Cu2 89.6(3) . . ? C1 O2 Cu2 88.2(3) . . ? C8 O3 C5 119.3(4) . . ? C59 O4 Cu2 128.7(4) . . ? C42 O6 Cu1 88.6(4) . 1_655 ? C42 O7 Cu1 89.7(4) . 1_655 ? C36 O8 C33 117.9(5) . . ? C29 O10 Cu1 132.8(4) . . ? Cu1 O11 H11B 109.5 . . ? Cu1 O11 H11C 119.9 . . ? H11B O11 H11C 96.5 . . ? H18B O18 H18A 120.8 . . ? H20B O20 H20A 135.6 . . ? H19A O19 H19B 113.1 . . ? Cu2 O21 H21B 94.0 . . ? Cu2 O21 H21C 109.6 . . ? H21B O21 H21C 86.8 . . ? O2 C1 O1 120.0(5) . . ? O2 C1 C2 120.7(4) . . ? O1 C1 C2 119.3(5) . . ? O2 C1 Cu2 60.9(2) . . ? O1 C1 Cu2 59.2(3) . . ? C2 C1 Cu2 175.7(4) . . ? C7 C2 C3 118.3(5) . . ? C7 C2 C1 121.4(5) . . ? C3 C2 C1 120.3(5) . . ? C2 C3 C4 119.9(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.7(6) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.0(5) . . ? C4 C5 O3 116.6(5) . . ? C6 C5 O3 123.4(5) . . ? C5 C6 C7 119.2(5) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C2 C7 C6 121.8(5) . . ? C2 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C13 C8 O3 122.7(5) . . ? C13 C8 C9 119.0(5) . . ? O3 C8 C9 118.2(6) . . ? C10 C9 C8 120.4(6) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 121.3(5) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 118.5(5) . . ? C10 C11 C59 121.5(5) . 1_655 ? C12 C11 C59 120.0(5) . 1_655 ? C11 C12 C13 120.0(6) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 120.9(5) . . ? C8 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? N3 C14 C15 123.9(5) . . ? N3 C14 H14 118.0 . . ? C15 C14 H14 118.0 . . ? C14 C15 C16 120.0(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 116.3(5) . . ? C15 C16 C19 121.8(5) . . ? C17 C16 C19 121.8(5) . . ? C18 C17 C16 120.2(5) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? N3 C18 C17 123.2(6) . . ? N3 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C20 C19 C22 117.5(5) . . ? C20 C19 C16 122.0(5) . . ? C22 C19 C16 120.3(5) . . ? C19 C20 C21 119.4(6) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? N2 C21 C20 124.3(6) . . ? N2 C21 H21A 117.8 . . ? C20 C21 H21A 117.8 . . ? C23 C22 C19 119.4(6) . . ? C23 C22 H22 120.3 . . ? C19 C22 H22 120.3 . . ? N2 C23 C22 122.5(6) . . ? N2 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? N1 C24 C25 124.5(6) . . ? N1 C24 H24 117.8 . . ? C25 C24 H24 117.8 . . ? C24 C25 C26 121.1(5) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 114.8(5) . . ? C27 C26 C26 123.4(6) . 2_685 ? C25 C26 C26 121.8(6) . 2_685 ? C28 C27 C26 120.0(5) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? N1 C28 C27 124.4(5) . . ? N1 C28 H28 117.8 . . ? C27 C28 H28 117.8 . . ? O9 C29 O10 124.5(7) . . ? O9 C29 C30 118.1(6) . . ? O10 C29 C30 117.4(6) . . ? C35 C30 C31 117.2(7) . . ? C35 C30 C29 121.7(6) . . ? C31 C30 C29 121.1(6) . . ? C32 C31 C30 120.7(7) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 120.0(7) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 121.6(7) . . ? C32 C33 O8 122.0(7) . . ? C34 C33 O8 116.3(7) . . ? C33 C34 C35 117.5(7) . . ? C33 C34 H34 121.2 . . ? C35 C34 H34 121.2 . . ? C34 C35 C30 123.0(6) . . ? C34 C35 H35 118.5 . . ? C30 C35 H35 118.5 . . ? C37 C36 C41 120.4(6) . . ? C37 C36 O8 124.5(7) . . ? C41 C36 O8 115.1(6) . . ? C36 C37 C38 119.6(7) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 121.7(6) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C40 118.7(6) . . ? C38 C39 C42 122.4(6) . . ? C40 C39 C42 118.9(6) . . ? C41 C40 C39 119.7(6) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C36 C41 C40 119.8(6) . . ? C36 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? O7 C42 O6 120.1(6) . . ? O7 C42 C39 120.8(6) . . ? O6 C42 C39 119.1(6) . . ? O7 C42 Cu1 59.9(3) . 1_655 ? O6 C42 Cu1 60.4(3) . 1_655 ? C39 C42 Cu1 174.1(4) . 1_655 ? N4 C43 C44 124.1(6) . . ? N4 C43 H43 118.0 . . ? C44 C43 H43 118.0 . . ? C43 C44 C45 120.3(6) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C48' 115(2) . . ? C46 C45 C44 115.2(6) . . ? C48' C45 C44 129(2) . . ? C46 C45 C48 129(2) . . ? C48' C45 C48 17(3) . . ? C44 C45 C48 115(2) . . ? C45 C46 C47 120.3(6) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C52 N5 C50 111.8(11) . . ? C52 N5 Cu3 120.9(9) . . ? C50 N5 Cu3 117.5(8) . . ? C52 N5 Cu3 121.7(10) . 2_756 ? C50 N5 Cu3 126.3(8) . 2_756 ? Cu3 N5 Cu3 25.64(17) . 2_756 ? C48 C51 C52 120(3) . . ? C48 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C49 C48 C51 118(4) . . ? C49 C48 C45 122(5) . . ? C51 C48 C45 121(4) . . ? N5 C52 C51 122.6(12) . . ? N5 C52 H52 118.7 . . ? C51 C52 H52 118.7 . . ? C50 N5' C52' 119.5(11) . . ? C50 N5' Cu3 118.4(8) . . ? C52' N5' Cu3 122.1(9) . . ? C51' C52' N5' 122.8(12) . . ? C51' C52' H52' 118.6 . . ? N5' C52' H52' 118.6 . . ? C52' C51' C48' 122(2) . . ? C52' C51' H51' 119.0 . . ? C48' C51' H51' 119.0 . . ? C51' C48' C45 126(4) . . ? C51' C48' C49 113(4) . . ? C45 C48' C49 121(4) . . ? C48 C49 C50 119(3) . . ? C48 C49 C48' 18(3) . . ? C50 C49 C48' 123(3) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? C48' C49 H49 113.7 . . ? N5' C50 N5 37.3(6) . . ? N5' C50 C49 118.6(7) . . ? N5 C50 C49 127.5(7) . . ? N5' C50 H50 110.9 . . ? N5 C50 H50 116.3 . . ? C49 C50 H50 116.3 . . ? N4 C47 C46 124.7(6) . . ? N4 C47 H47 117.7 . . ? C46 C47 H47 117.7 . . ? O5 C59 O4 125.9(5) . . ? O5 C59 C11 118.0(5) . 1_455 ? O4 C59 C11 116.1(5) . 1_455 ? O15 O13 C61 56.5(15) 2_756 . ? O15 O13 C67 34(3) 2_756 2_756 ? C61 O13 C67 23(2) . 2_756 ? C67 O12 O14 122(10) 2_756 2_756 ? C67 O12 C61 35(10) 2_756 . ? O14 O12 C61 156(4) 2_756 . ? C67 O12 O15 36(9) 2_756 2_756 ? O14 O12 O15 122(4) 2_756 2_756 ? C61 O12 O15 41.0(13) . 2_756 ? C67 O12 C68 60(10) 2_756 2_756 ? O14 O12 C68 129(4) 2_756 2_756 ? C61 O12 C68 51.0(18) . 2_756 ? O15 O12 C68 88.6(19) 2_756 2_756 ? C67 O12 Cu3 114(10) 2_756 . ? O14 O12 Cu3 73(2) 2_756 . ? C61 O12 Cu3 115(3) . . ? O15 O12 Cu3 150.1(18) 2_756 . ? C68 O12 Cu3 64.0(14) 2_756 . ? C67 C61 O15 80(4) 2_756 2_756 ? C67 C61 O12 18(5) 2_756 . ? O15 C61 O12 89(2) 2_756 . ? C67 C61 O13 123(4) 2_756 . ? O15 C61 O13 44.0(12) 2_756 . ? O12 C61 O13 129(2) . . ? C67 C61 C68 81(4) 2_756 2_756 ? O15 C61 C68 150(2) 2_756 2_756 ? O12 C61 C68 80(2) . 2_756 ? O13 C61 C68 149.4(19) . 2_756 ? C67 C61 C62 117(5) 2_756 . ? O15 C61 C62 150(3) 2_756 . ? O12 C61 C62 115(4) . . ? O13 C61 C62 116(3) . . ? C68 C61 C62 36(3) 2_756 . ? C67 C61 C69 129(5) 2_756 2_756 ? O15 C61 C69 140(3) 2_756 2_756 ? O12 C61 C69 127(4) . 2_756 ? O13 C61 C69 103(3) . 2_756 ? C68 C61 C69 48(3) 2_756 2_756 ? C62 C61 C69 12(6) . 2_756 ? C69 C62 C68 167(10) 2_756 2_756 ? C69 C62 N6 112(10) 2_756 . ? C68 C62 N6 60(5) 2_756 . ? C69 C62 C63 6(10) 2_756 . ? C68 C62 C63 167(8) 2_756 . ? N6 C62 C63 118(7) . . ? C69 C62 C61 129(10) 2_756 . ? C68 C62 C61 61(4) 2_756 . ? N6 C62 C61 119(4) . . ? C63 C62 C61 123(7) . . ? C69 C62 C70 39(10) 2_756 2_756 ? C68 C62 C70 132(9) 2_756 2_756 ? N6 C62 C70 73(5) . 2_756 ? C63 C62 C70 45(3) . 2_756 ? C61 C62 C70 167(6) . 2_756 ? C69 C62 N7 135(10) 2_756 2_756 ? C68 C62 N7 37(4) 2_756 2_756 ? N6 C62 N7 23.0(14) . 2_756 ? C63 C62 N7 140(7) . 2_756 ? C61 C62 N7 97(3) . 2_756 ? C70 C62 N7 96(5) 2_756 2_756 ? C69 C63 C70 77(6) 2_756 2_756 ? C69 C63 C64 118(6) 2_756 . ? C70 C63 C64 41.8(11) 2_756 . ? C69 C63 C62 3(10) 2_756 . ? C70 C63 C62 80(5) 2_756 . ? C64 C63 C62 121(5) . . ? C70 C64 C65 57.1(17) 2_756 . ? C70 C64 C63 61.0(18) 2_756 . ? C65 C64 C63 116.6(18) . . ? C70 C64 C69 38(3) 2_756 2_756 ? C65 C64 C69 93(3) . 2_756 ? C63 C64 C69 24(3) . 2_756 ? C71 C65 C70 80(4) 2_756 2_756 ? C71 C65 C64 123(4) 2_756 . ? C70 C65 C64 43.3(13) 2_756 . ? C71 C65 C66 12(5) 2_756 . ? C70 C65 C66 77(3) 2_756 . ? C64 C65 C66 119(3) . . ? C71 C66 C72 153(10) 2_756 2_756 ? C71 C66 N6 126(10) 2_756 . ? C72 C66 N6 62(3) 2_756 . ? C71 C66 C65 22(10) 2_756 . ? C72 C66 C65 175(5) 2_756 . ? N6 C66 C65 121(5) . . ? C71 C66 C70 52(10) 2_756 2_756 ? C72 C66 C70 138(5) 2_756 2_756 ? N6 C66 C70 77(3) . 2_756 ? C65 C66 C70 44.5(19) . 2_756 ? C71 C66 N7 150(10) 2_756 2_756 ? C72 C66 N7 38(2) 2_756 2_756 ? N6 C66 N7 26.0(11) . 2_756 ? C65 C66 N7 147(4) . 2_756 ? C70 C66 N7 103(3) 2_756 2_756 ? C71 C66 H66 103.7 2_756 . ? C72 C66 H66 103.7 2_756 . ? N6 C66 H66 74.9 . . ? C65 C66 H66 81.6 . . ? C70 C66 H66 73.4 2_756 . ? N7 C66 H66 80.8 2_756 . ? N7 N6 C68 80.3(19) 2_756 2_756 ? N7 N6 C72 72.6(18) 2_756 2_756 ? C68 N6 C72 153(2) 2_756 2_756 ? N7 N6 C62 122(3) 2_756 . ? C68 N6 C62 42(3) 2_756 . ? C72 N6 C62 165(3) 2_756 . ? N7 N6 C66 113(3) 2_756 . ? C68 N6 C66 161(3) 2_756 . ? C72 N6 C66 42(2) 2_756 . ? C62 N6 C66 123(4) . . ? N7 N6 C69 139(3) 2_756 2_756 ? C68 N6 C69 59(3) 2_756 2_756 ? C72 N6 C69 148(3) 2_756 2_756 ? C62 N6 C69 17(5) . 2_756 ? C66 N6 C69 106(4) . 2_756 ? N7 N6 C71 128(3) 2_756 2_756 ? C68 N6 C71 151(3) 2_756 2_756 ? C72 N6 C71 55(2) 2_756 2_756 ? C62 N6 C71 110(3) . 2_756 ? C66 N6 C71 15(4) . 2_756 ? C69 N6 C71 93(3) 2_756 2_756 ? N7 N6 C70 172.0(18) 2_756 2_756 ? C68 N6 C70 105.9(15) 2_756 2_756 ? C72 N6 C70 100.8(14) 2_756 2_756 ? C62 N6 C70 65(3) . 2_756 ? C66 N6 C70 59(2) . 2_756 ? C69 N6 C70 47(3) 2_756 2_756 ? C71 N6 C70 46(2) 2_756 2_756 ? N7 N6 Cu3 16.2(11) 2_756 . ? C68 N6 Cu3 68.3(13) 2_756 . ? C72 N6 Cu3 85.6(13) 2_756 . ? C62 N6 Cu3 109(3) . . ? C66 N6 Cu3 128(2) . . ? C69 N6 Cu3 126(3) 2_756 . ? C71 N6 Cu3 140(2) 2_756 . ? C70 N6 Cu3 171.7(10) 2_756 . ? H22A O22 H22B 95.5 . . ? O12 O14 C67 20(4) 2_756 . ? O12 O14 Cu3 80(2) 2_756 2_756 ? C67 O14 Cu3 87(3) . 2_756 ? O12 O14 Cu3 107(2) 2_756 . ? C67 O14 Cu3 113(3) . . ? Cu3 O14 Cu3 27.18(17) 2_756 . ? O13 O15 C61 80(2) 2_756 2_756 ? O13 O15 C67 123(4) 2_756 . ? C61 O15 C67 44(4) 2_756 . ? O13 O15 O12 126(3) 2_756 2_756 ? C61 O15 O12 50.3(19) 2_756 2_756 ? C67 O15 O12 13(3) . 2_756 ? O12 C67 C61 127(10) 2_756 2_756 ? O12 C67 O14 38(10) 2_756 . ? C61 C67 O14 165(6) 2_756 . ? O12 C67 O15 131(10) 2_756 . ? C61 C67 O15 56(3) 2_756 . ? O14 C67 O15 127(5) . . ? O12 C67 C68 103(10) 2_756 . ? C61 C67 C68 61(4) 2_756 . ? O14 C67 C68 119(4) . . ? O15 C67 C68 114(5) . . ? O12 C67 O13 133(10) 2_756 2_756 ? C61 C67 O13 33(2) 2_756 2_756 ? O14 C67 O13 147(4) . 2_756 ? O15 C67 O13 22.9(19) . 2_756 ? C68 C67 O13 93(4) . 2_756 ? O12 C67 Cu3 54(9) 2_756 2_756 ? C61 C67 Cu3 117(5) 2_756 2_756 ? O14 C67 Cu3 59.7(19) . 2_756 ? O15 C67 Cu3 173(5) . 2_756 ? C68 C67 Cu3 59.2(18) . 2_756 ? O13 C67 Cu3 150(4) 2_756 2_756 ? C66 C72 N6 75(4) 2_756 2_756 ? C66 C72 N7 116(4) 2_756 . ? N6 C72 N7 42.0(9) 2_756 . ? C66 C72 C71 10(5) 2_756 . ? N6 C72 C71 80(3) 2_756 . ? N7 C72 C71 122(3) . . ? C66 C72 Cu3 138(4) 2_756 2_756 ? N6 C72 Cu3 63.2(11) 2_756 2_756 ? N7 C72 Cu3 22.5(9) . 2_756 ? C71 C72 Cu3 143(3) . 2_756 ? N6 N7 Cu3 152.3(19) 2_756 2_756 ? N6 N7 C72 65.4(16) 2_756 . ? Cu3 N7 C72 134.7(16) 2_756 . ? N6 N7 C68 58.4(16) 2_756 . ? Cu3 N7 C68 99.5(13) 2_756 . ? C72 N7 C68 123.7(19) . . ? N6 N7 C66 41(2) 2_756 2_756 ? Cu3 N7 C66 160(2) 2_756 2_756 ? C72 N7 C66 26.1(19) . 2_756 ? C68 N7 C66 98(2) . 2_756 ? N6 N7 C62 35(3) 2_756 2_756 ? Cu3 N7 C62 121(2) 2_756 2_756 ? C72 N7 C62 100(3) . 2_756 ? C68 N7 C62 23(2) . 2_756 ? C66 N7 C62 75(3) 2_756 2_756 ? N6 N7 Cu3 164.9(17) 2_756 . ? Cu3 N7 Cu3 12.8(3) 2_756 . ? C72 N7 Cu3 127.4(14) . . ? C68 N7 Cu3 108.7(12) . . ? C66 N7 Cu3 153.3(19) 2_756 . ? C62 N7 Cu3 132(2) 2_756 . ? C62 C68 N6 79(6) 2_756 2_756 ? C62 C68 C61 83(6) 2_756 2_756 ? N6 C68 C61 158(2) 2_756 2_756 ? C62 C68 N7 120(6) 2_756 . ? N6 C68 N7 41.2(11) 2_756 . ? C61 C68 N7 153(2) 2_756 . ? C62 C68 C69 5(9) 2_756 . ? N6 C68 C69 76(5) 2_756 . ? C61 C68 C69 87(5) 2_756 . ? N7 C68 C69 117(6) . . ? C62 C68 C67 120(6) 2_756 . ? N6 C68 C67 159(3) 2_756 . ? C61 C68 C67 37(3) 2_756 . ? N7 C68 C67 119(3) . . ? C69 C68 C67 124(6) . . ? C62 C68 O12 130(6) 2_756 2_756 ? N6 C68 O12 143(2) 2_756 2_756 ? C61 C68 O12 48.7(17) 2_756 2_756 ? N7 C68 O12 105.2(18) . 2_756 ? C69 C68 O12 135(6) . 2_756 ? C67 C68 O12 17.0(17) . 2_756 ? C62 C68 Cu3 154(6) 2_756 2_756 ? N6 C68 Cu3 78.9(14) 2_756 2_756 ? C61 C68 Cu3 114.9(15) 2_756 2_756 ? N7 C68 Cu3 38.8(8) . 2_756 ? C69 C68 Cu3 153(6) . 2_756 ? C67 C68 Cu3 80(2) . 2_756 ? O12 C68 Cu3 66.4(14) 2_756 2_756 ? C62 C69 C63 170(10) 2_756 2_756 ? C62 C69 C68 8(10) 2_756 . ? C63 C69 C68 169(9) 2_756 . ? C62 C69 C70 128(10) 2_756 . ? C63 C69 C70 62(4) 2_756 . ? C68 C69 C70 123(8) . . ? C62 C69 N6 50(10) 2_756 2_756 ? C63 C69 N6 138(8) 2_756 2_756 ? C68 C69 N6 45(3) . 2_756 ? C70 C69 N6 77(5) . 2_756 ? C62 C69 C61 39(10) 2_756 2_756 ? C63 C69 C61 132(9) 2_756 2_756 ? C68 C69 C61 45(3) . 2_756 ? C70 C69 C61 166(6) . 2_756 ? N6 C69 C61 90(2) 2_756 2_756 ? C62 C69 C64 151(10) 2_756 2_756 ? C63 C69 C64 38(3) 2_756 2_756 ? C68 C69 C64 145(8) . 2_756 ? C70 C69 C64 24.8(13) . 2_756 ? N6 C69 C64 101(5) 2_756 2_756 ? C61 C69 C64 169(6) 2_756 2_756 ? C62 C69 H69 94.8 2_756 . ? C63 C69 H69 94.8 2_756 . ? C68 C69 H69 92.2 . . ? C70 C69 H69 36.0 . . ? N6 C69 H69 49.0 2_756 . ? C61 C69 H69 130.0 2_756 . ? C64 C69 H69 60.3 2_756 . ? C64 C70 C65 80(2) 2_756 2_756 ? C64 C70 C63 77(2) 2_756 2_756 ? C65 C70 C63 153(2) 2_756 2_756 ? C64 C70 C71 123(3) 2_756 . ? C65 C70 C71 43(2) 2_756 . ? C63 C70 C71 156(3) 2_756 . ? C64 C70 C69 118(4) 2_756 . ? C65 C70 C69 153(4) 2_756 . ? C63 C70 C69 41(3) 2_756 . ? C71 C70 C69 116(4) . . ? C64 C70 C66 136(3) 2_756 2_756 ? C65 C70 C66 58(2) 2_756 2_756 ? C63 C70 C66 138(2) 2_756 2_756 ? C71 C70 C66 18(3) . 2_756 ? C69 C70 C66 99(4) . 2_756 ? C64 C70 C62 130(4) 2_756 2_756 ? C65 C70 C62 142(3) 2_756 2_756 ? C63 C70 C62 54(3) 2_756 2_756 ? C71 C70 C62 103(4) . 2_756 ? C69 C70 C62 13(6) . 2_756 ? C66 C70 C62 86(3) 2_756 2_756 ? C64 C70 N6 162(2) 2_756 2_756 ? C65 C70 N6 101.6(17) 2_756 2_756 ? C63 C70 N6 96.2(15) 2_756 2_756 ? C71 C70 N6 60(2) . 2_756 ? C69 C70 N6 55(3) . 2_756 ? C66 C70 N6 43.7(18) 2_756 2_756 ? C62 C70 N6 42(3) 2_756 2_756 ? C66 C71 C65 146(10) 2_756 2_756 ? C66 C71 C70 110(10) 2_756 . ? C65 C71 C70 57(3) 2_756 . ? C66 C71 C72 17(10) 2_756 . ? C65 C71 C72 163(5) 2_756 . ? C70 C71 C72 119(4) . . ? C66 C71 N6 39(10) 2_756 2_756 ? C65 C71 N6 128(5) 2_756 2_756 ? C70 C71 N6 74(3) . 2_756 ? C72 C71 N6 44.9(17) . 2_756 ? C66 C71 H71 107.1 2_756 . ? C65 C71 H71 107.1 2_756 . ? C70 C71 H71 110.1 . . ? C72 C71 H71 89.7 . . ? N6 C71 H71 106.0 2_756 . ? H23C O23 H23A 133.4 . . ? 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 O10 Cu1 N1 C28 -172.0(5) . . . . ? N2 Cu1 N1 C28 -74.2(5) . . . . ? O11 Cu1 N1 C28 -56(8) . . . . ? O7 Cu1 N1 C28 88.9(5) 1_455 . . . ? O6 Cu1 N1 C28 27.4(5) 1_455 . . . ? C42 Cu1 N1 C28 58.4(5) 1_455 . . . ? O10 Cu1 N1 C24 4.3(5) . . . . ? N2 Cu1 N1 C24 102.1(5) . . . . ? O11 Cu1 N1 C24 121(8) . . . . ? O7 Cu1 N1 C24 -94.8(5) 1_455 . . . ? O6 Cu1 N1 C24 -156.3(5) 1_455 . . . ? C42 Cu1 N1 C24 -125.3(5) 1_455 . . . ? O10 Cu1 N2 C21 3.2(5) . . . . ? N1 Cu1 N2 C21 -87.0(5) . . . . ? O11 Cu1 N2 C21 93.4(5) . . . . ? O7 Cu1 N2 C21 -169.1(6) 1_455 . . . ? O6 Cu1 N2 C21 -176.7(5) 1_455 . . . ? C42 Cu1 N2 C21 -173.4(5) 1_455 . . . ? O10 Cu1 N2 C23 -178.0(4) . . . . ? N1 Cu1 N2 C23 91.8(5) . . . . ? O11 Cu1 N2 C23 -87.8(5) . . . . ? O7 Cu1 N2 C23 9.7(9) 1_455 . . . ? O6 Cu1 N2 C23 2.1(5) 1_455 . . . ? C42 Cu1 N2 C23 5.4(6) 1_455 . . . ? O4 Cu2 N3 C14 166.0(4) . . . . ? O1 Cu2 N3 C14 -16.1(9) . . . . ? N4 Cu2 N3 C14 -105.3(5) . . . . ? O2 Cu2 N3 C14 -17.0(5) . . . . ? O21 Cu2 N3 C14 74.5(5) . . . . ? C1 Cu2 N3 C14 -18.3(6) . . . . ? O4 Cu2 N3 C18 -14.7(5) . . . . ? O1 Cu2 N3 C18 163.3(5) . . . . ? N4 Cu2 N3 C18 74.1(5) . . . . ? O2 Cu2 N3 C18 162.4(4) . . . . ? O21 Cu2 N3 C18 -106.1(5) . . . . ? C1 Cu2 N3 C18 161.1(4) . . . . ? O4 Cu2 N4 C47 -25.2(5) . . . . ? N3 Cu2 N4 C47 -123.4(5) . . . . ? O1 Cu2 N4 C47 73.9(5) . . . . ? O2 Cu2 N4 C47 135.9(5) . . . . ? O21 Cu2 N4 C47 -170(100) . . . . ? C1 Cu2 N4 C47 105.0(5) . . . . ? O4 Cu2 N4 C43 161.7(4) . . . . ? N3 Cu2 N4 C43 63.6(5) . . . . ? O1 Cu2 N4 C43 -99.2(4) . . . . ? O2 Cu2 N4 C43 -37.2(4) . . . . ? O21 Cu2 N4 C43 17(50) . . . . ? C1 Cu2 N4 C43 -68.0(5) . . . . ? O4 Cu2 O1 C1 174.8(3) . . . . ? N3 Cu2 O1 C1 -3.2(7) . . . . ? N4 Cu2 O1 C1 86.5(3) . . . . ? O2 Cu2 O1 C1 -2.1(3) . . . . ? O21 Cu2 O1 C1 -93.3(3) . . . . ? O4 Cu2 O2 C1 -7.2(6) . . . . ? N3 Cu2 O2 C1 -178.2(3) . . . . ? O1 Cu2 O2 C1 2.2(3) . . . . ? N4 Cu2 O2 C1 -87.1(3) . . . . ? O21 Cu2 O2 C1 93.0(3) . . . . ? N3 Cu2 O4 C59 -66.7(5) . . . . ? O1 Cu2 O4 C59 113.9(4) . . . . ? N4 Cu2 O4 C59 -157.9(5) . . . . ? O2 Cu2 O4 C59 122.3(5) . . . . ? O21 Cu2 O4 C59 22.0(4) . . . . ? C1 Cu2 O4 C59 117.5(4) . . . . ? N2 Cu1 O10 C29 74.7(6) . . . . ? N1 Cu1 O10 C29 162.2(6) . . . . ? O11 Cu1 O10 C29 -16.6(6) . . . . ? O7 Cu1 O10 C29 -107.6(5) 1_455 . . . ? O6 Cu1 O10 C29 -105.6(6) 1_455 . . . ? C42 Cu1 O10 C29 -108.6(6) 1_455 . . . ? Cu2 O2 C1 O1 -3.7(5) . . . . ? Cu2 O2 C1 C2 175.4(5) . . . . ? Cu2 O1 C1 O2 3.7(5) . . . . ? Cu2 O1 C1 C2 -175.4(4) . . . . ? O4 Cu2 C1 O2 176.9(3) . . . . ? N3 Cu2 C1 O2 2.4(4) . . . . ? O1 Cu2 C1 O2 -176.3(5) . . . . ? N4 Cu2 C1 O2 91.5(3) . . . . ? O21 Cu2 C1 O2 -88.3(3) . . . . ? O4 Cu2 C1 O1 -6.8(4) . . . . ? N3 Cu2 C1 O1 178.7(3) . . . . ? N4 Cu2 C1 O1 -92.2(3) . . . . ? O2 Cu2 C1 O1 176.3(5) . . . . ? O21 Cu2 C1 O1 88.0(3) . . . . ? O4 Cu2 C1 C2 64(5) . . . . ? N3 Cu2 C1 C2 -111(5) . . . . ? O1 Cu2 C1 C2 71(5) . . . . ? N4 Cu2 C1 C2 -22(5) . . . . ? O2 Cu2 C1 C2 -113(5) . . . . ? O21 Cu2 C1 C2 159(5) . . . . ? O2 C1 C2 C7 1.5(8) . . . . ? O1 C1 C2 C7 -179.5(5) . . . . ? Cu2 C1 C2 C7 112(5) . . . . ? O2 C1 C2 C3 -177.3(5) . . . . ? O1 C1 C2 C3 1.7(8) . . . . ? Cu2 C1 C2 C3 -66(5) . . . . ? C7 C2 C3 C4 0.6(9) . . . . ? C1 C2 C3 C4 179.4(5) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C3 C4 C5 C6 -0.4(10) . . . . ? C3 C4 C5 O3 -178.9(5) . . . . ? C8 O3 C5 C4 -156.6(6) . . . . ? C8 O3 C5 C6 25.0(9) . . . . ? C4 C5 C6 C7 0.3(10) . . . . ? O3 C5 C6 C7 178.7(6) . . . . ? C3 C2 C7 C6 -0.7(9) . . . . ? C1 C2 C7 C6 -179.5(6) . . . . ? C5 C6 C7 C2 0.3(10) . . . . ? C5 O3 C8 C13 55.0(8) . . . . ? C5 O3 C8 C9 -128.2(6) . . . . ? C13 C8 C9 C10 -0.7(10) . . . . ? O3 C8 C9 C10 -177.6(6) . . . . ? C8 C9 C10 C11 -1.0(10) . . . . ? C9 C10 C11 C12 2.6(9) . . . . ? C9 C10 C11 C59 -176.2(6) . . . 1_655 ? C10 C11 C12 C13 -2.6(9) . . . . ? C59 C11 C12 C13 176.3(5) 1_655 . . . ? O3 C8 C13 C12 177.4(6) . . . . ? C9 C8 C13 C12 0.7(10) . . . . ? C11 C12 C13 C8 1.0(10) . . . . ? C18 N3 C14 C15 -0.3(9) . . . . ? Cu2 N3 C14 C15 179.1(5) . . . . ? N3 C14 C15 C16 -0.6(9) . . . . ? C14 C15 C16 C17 0.9(9) . . . . ? C14 C15 C16 C19 -175.1(5) . . . . ? C15 C16 C17 C18 -0.5(9) . . . . ? C19 C16 C17 C18 175.6(5) . . . . ? C14 N3 C18 C17 0.8(9) . . . . ? Cu2 N3 C18 C17 -178.6(5) . . . . ? C16 C17 C18 N3 -0.5(10) . . . . ? C15 C16 C19 C20 16.9(9) . . . . ? C17 C16 C19 C20 -158.9(6) . . . . ? C15 C16 C19 C22 -168.7(6) . . . . ? C17 C16 C19 C22 15.5(9) . . . . ? C22 C19 C20 C21 -3.1(10) . . . . ? C16 C19 C20 C21 171.5(6) . . . . ? C23 N2 C21 C20 1.0(10) . . . . ? Cu1 N2 C21 C20 179.9(5) . . . . ? C19 C20 C21 N2 1.3(11) . . . . ? C20 C19 C22 C23 2.6(9) . . . . ? C16 C19 C22 C23 -172.1(5) . . . . ? C21 N2 C23 C22 -1.5(9) . . . . ? Cu1 N2 C23 C22 179.6(5) . . . . ? C19 C22 C23 N2 -0.3(10) . . . . ? C28 N1 C24 C25 -2.1(10) . . . . ? Cu1 N1 C24 C25 -178.7(6) . . . . ? N1 C24 C25 C26 0.3(12) . . . . ? C24 C25 C26 C27 1.9(10) . . . . ? C24 C25 C26 C26 -178.7(7) . . . 2_685 ? C25 C26 C27 C28 -2.2(9) . . . . ? C26 C26 C27 C28 178.3(6) 2_685 . . . ? C24 N1 C28 C27 1.7(9) . . . . ? Cu1 N1 C28 C27 178.2(5) . . . . ? C26 C27 C28 N1 0.5(10) . . . . ? Cu1 O10 C29 O9 2.2(10) . . . . ? Cu1 O10 C29 C30 -175.5(4) . . . . ? O9 C29 C30 C35 -174.0(6) . . . . ? O10 C29 C30 C35 4.0(9) . . . . ? O9 C29 C30 C31 6.0(10) . . . . ? O10 C29 C30 C31 -176.0(6) . . . . ? C35 C30 C31 C32 2.0(10) . . . . ? C29 C30 C31 C32 -178.0(6) . . . . ? C30 C31 C32 C33 -0.7(11) . . . . ? C31 C32 C33 C34 -1.5(11) . . . . ? C31 C32 C33 O8 -177.4(6) . . . . ? C36 O8 C33 C32 -60.6(9) . . . . ? C36 O8 C33 C34 123.3(7) . . . . ? C32 C33 C34 C35 2.2(10) . . . . ? O8 C33 C34 C35 178.4(6) . . . . ? C33 C34 C35 C30 -0.8(11) . . . . ? C31 C30 C35 C34 -1.2(10) . . . . ? C29 C30 C35 C34 178.8(6) . . . . ? C33 O8 C36 C37 -25.3(10) . . . . ? C33 O8 C36 C41 157.4(6) . . . . ? C41 C36 C37 C38 -1.3(11) . . . . ? O8 C36 C37 C38 -178.4(6) . . . . ? C36 C37 C38 C39 -0.3(11) . . . . ? C37 C38 C39 C40 0.7(10) . . . . ? C37 C38 C39 C42 -179.7(6) . . . . ? C38 C39 C40 C41 0.4(9) . . . . ? C42 C39 C40 C41 -179.1(5) . . . . ? C37 C36 C41 C40 2.4(11) . . . . ? O8 C36 C41 C40 179.9(6) . . . . ? C39 C40 C41 C36 -2.0(10) . . . . ? Cu1 O7 C42 O6 -3.9(5) 1_655 . . . ? Cu1 O7 C42 C39 173.2(5) 1_655 . . . ? Cu1 O6 C42 O7 3.9(5) 1_655 . . . ? Cu1 O6 C42 C39 -173.3(5) 1_655 . . . ? C38 C39 C42 O7 -179.2(6) . . . . ? C40 C39 C42 O7 0.3(8) . . . . ? C38 C39 C42 O6 -2.1(9) . . . . ? C40 C39 C42 O6 177.5(5) . . . . ? C38 C39 C42 Cu1 -85(5) . . . 1_655 ? C40 C39 C42 Cu1 95(5) . . . 1_655 ? C47 N4 C43 C44 -3.9(9) . . . . ? Cu2 N4 C43 C44 169.7(5) . . . . ? N4 C43 C44 C45 1.5(10) . . . . ? C43 C44 C45 C46 2.1(9) . . . . ? C43 C44 C45 C48' -170(3) . . . . ? C43 C44 C45 C48 178(3) . . . . ? C48' C45 C46 C47 170(3) . . . . ? C44 C45 C46 C47 -3.1(10) . . . . ? C48 C45 C46 C47 -178(3) . . . . ? Cu3 Cu3 N5 C52 99.6(12) 2_756 . . . ? N7 Cu3 N5 C52 -54.9(15) 2_756 . . . ? O14 Cu3 N5 C52 -178.0(12) 2_756 . . . ? C68 Cu3 N5 C52 -102.7(14) 2_756 . . . ? O12 Cu3 N5 C52 -151.2(19) . . . . ? N6 Cu3 N5 C52 -66.5(13) . . . . ? O14 Cu3 N5 C52 29.1(12) . . . . ? N7 Cu3 N5 C52 113.3(13) . . . . ? N5' Cu3 N5 C52 -83.0(17) . . . . ? N5 Cu3 N5 C52 99.6(12) 2_756 . . . ? C67 Cu3 N5 C52 -146(2) 2_756 . . . ? Cu3 Cu3 N5 C50 -117.3(9) 2_756 . . . ? N7 Cu3 N5 C50 88.2(11) 2_756 . . . ? O14 Cu3 N5 C50 -34.9(10) 2_756 . . . ? C68 Cu3 N5 C50 40.4(12) 2_756 . . . ? O12 Cu3 N5 C50 -8.1(17) . . . . ? N6 Cu3 N5 C50 76.7(10) . . . . ? O14 Cu3 N5 C50 172.3(10) . . . . ? N7 Cu3 N5 C50 -103.6(10) . . . . ? N5' Cu3 N5 C50 60.1(13) . . . . ? N5 Cu3 N5 C50 -117.3(9) 2_756 . . . ? C67 Cu3 N5 C50 -3(2) 2_756 . . . ? N7 Cu3 N5 Cu3 -154.5(8) 2_756 . . 2_756 ? O14 Cu3 N5 Cu3 82.4(4) 2_756 . . 2_756 ? C68 Cu3 N5 Cu3 157.7(8) 2_756 . . 2_756 ? O12 Cu3 N5 Cu3 109.2(15) . . . 2_756 ? N6 Cu3 N5 Cu3 -166.0(5) . . . 2_756 ? O14 Cu3 N5 Cu3 -70.4(4) . . . 2_756 ? N7 Cu3 N5 Cu3 13.8(4) . . . 2_756 ? N5' Cu3 N5 Cu3 177.4(14) . . . 2_756 ? N5 Cu3 N5 Cu3 0.000(3) 2_756 . . 2_756 ? C67 Cu3 N5 Cu3 115(2) 2_756 . . 2_756 ? C52 C51 C48 C49 3(5) . . . . ? C52 C51 C48 C45 -175(2) . . . . ? C46 C45 C48 C49 -130(3) . . . . ? C48' C45 C48 C49 -90(18) . . . . ? C44 C45 C48 C49 55(4) . . . . ? C46 C45 C48 C51 49(5) . . . . ? C48' C45 C48 C51 88(17) . . . . ? C44 C45 C48 C51 -126(3) . . . . ? C50 N5 C52 C51 1.2(19) . . . . ? Cu3 N5 C52 C51 146.2(11) . . . . ? Cu3 N5 C52 C51 176.3(10) 2_756 . . . ? C48 C51 C52 N5 1(3) . . . . ? Cu3 Cu3 N5' C50 -60.0(10) 2_756 . . . ? N7 Cu3 N5' C50 142.1(11) 2_756 . . . ? O14 Cu3 N5' C50 25.6(10) 2_756 . . . ? C68 Cu3 N5' C50 100.1(11) 2_756 . . . ? O12 Cu3 N5' C50 50.8(15) . . . . ? N6 Cu3 N5' C50 132.5(10) . . . . ? O14 Cu3 N5' C50 -127.8(10) . . . . ? N7 Cu3 N5' C50 -47.4(10) . . . . ? N5 Cu3 N5' C50 -62.6(14) . . . . ? N5 Cu3 N5' C50 -37(13) 2_756 . . . ? C67 Cu3 N5' C50 59(2) 2_756 . . . ? Cu3 Cu3 N5' C52' 117.7(11) 2_756 . . . ? N7 Cu3 N5' C52' -40.3(14) 2_756 . . . ? O14 Cu3 N5' C52' -156.7(12) 2_756 . . . ? C68 Cu3 N5' C52' -82.3(13) 2_756 . . . ? O12 Cu3 N5' C52' -131.6(17) . . . . ? N6 Cu3 N5' C52' -49.8(12) . . . . ? O14 Cu3 N5' C52' 49.9(12) . . . . ? N7 Cu3 N5' C52' 130.3(12) . . . . ? N5 Cu3 N5' C52' 115(2) . . . . ? N5 Cu3 N5' C52' 141(12) 2_756 . . . ? C67 Cu3 N5' C52' -123(2) 2_756 . . . ? C50 N5' C52' C51' 2(2) . . . . ? Cu3 N5' C52' C51' -175.4(11) . . . . ? N5' C52' C51' C48' 0(3) . . . . ? C52' C51' C48' C45 176(3) . . . . ? C52' C51' C48' C49 -7(5) . . . . ? C46 C45 C48' C51' 22(5) . . . . ? C44 C45 C48' C51' -166(3) . . . . ? C48 C45 C48' C51' -125(21) . . . . ? C46 C45 C48' C49 -155(2) . . . . ? C44 C45 C48' C49 18(5) . . . . ? C48 C45 C48' C49 59(15) . . . . ? C51 C48 C49 C50 -9(4) . . . . ? C45 C48 C49 C50 170(2) . . . . ? C51 C48 C49 C48' -117(19) . . . . ? C45 C48 C49 C48' 62(15) . . . . ? C51' C48' C49 C48 96(18) . . . . ? C45 C48' C49 C48 -88(17) . . . . ? C51' C48' C49 C50 13(4) . . . . ? C45 C48' C49 C50 -171(2) . . . . ? C52' N5' C50 N5 -112.2(19) . . . . ? Cu3 N5' C50 N5 65.5(13) . . . . ? C52' N5' C50 C49 3.1(17) . . . . ? Cu3 N5' C50 C49 -179.2(6) . . . . ? C52 N5 C50 N5' 81.6(16) . . . . ? Cu3 N5 C50 N5' -64.7(13) . . . . ? Cu3 N5 C50 N5' -93.2(16) 2_756 . . . ? C52 N5 C50 C49 -7.8(16) . . . . ? Cu3 N5 C50 C49 -154.2(6) . . . . ? Cu3 N5 C50 C49 177.3(6) 2_756 . . . ? C48 C49 C50 N5' -31(2) . . . . ? C48' C49 C50 N5' -11(3) . . . . ? C48 C49 C50 N5 12(3) . . . . ? C48' C49 C50 N5 33(3) . . . . ? C43 N4 C47 C46 2.8(9) . . . . ? Cu2 N4 C47 C46 -170.7(5) . . . . ? C45 C46 C47 N4 0.7(11) . . . . ? Cu2 O4 C59 O5 -2.6(8) . . . . ? Cu2 O4 C59 C11 175.7(3) . . . 1_455 ? Cu3 Cu3 O12 C67 -125(17) 2_756 . . 2_756 ? N7 Cu3 O12 C67 35(18) 2_756 . . 2_756 ? O14 Cu3 O12 C67 -118(19) 2_756 . . 2_756 ? C68 Cu3 O12 C67 34(17) 2_756 . . 2_756 ? N6 Cu3 O12 C67 41(17) . . . 2_756 ? O14 Cu3 O12 C67 161(12) . . . 2_756 ? N7 Cu3 O12 C67 -137(17) . . . 2_756 ? N5 Cu3 O12 C67 154(17) . . . 2_756 ? N5' Cu3 O12 C67 132(18) . . . 2_756 ? N5 Cu3 O12 C67 -50(18) 2_756 . . 2_756 ? Cu3 Cu3 O12 O14 -7(2) 2_756 . . 2_756 ? N7 Cu3 O12 O14 153(2) 2_756 . . 2_756 ? C68 Cu3 O12 O14 152(3) 2_756 . . 2_756 ? N6 Cu3 O12 O14 159(2) . . . 2_756 ? O14 Cu3 O12 O14 -81(30) . . . 2_756 ? N7 Cu3 O12 O14 -19(2) . . . 2_756 ? N5 Cu3 O12 O14 -88(2) . . . 2_756 ? N5' Cu3 O12 O14 -110(2) . . . 2_756 ? N5 Cu3 O12 O14 68(2) 2_756 . . 2_756 ? C67 Cu3 O12 O14 118(19) 2_756 . . 2_756 ? Cu3 Cu3 O12 C61 -163(2) 2_756 . . . ? N7 Cu3 O12 C61 -4(3) 2_756 . . . ? O14 Cu3 O12 C61 -156(4) 2_756 . . . ? C68 Cu3 O12 C61 -4.7(17) 2_756 . . . ? N6 Cu3 O12 C61 3(2) . . . . ? O14 Cu3 O12 C61 122(27) . . . . ? N7 Cu3 O12 C61 -175(2) . . . . ? N5 Cu3 O12 C61 115(2) . . . . ? N5' Cu3 O12 C61 94(3) . . . . ? N5 Cu3 O12 C61 -89(3) 2_756 . . . ? C67 Cu3 O12 C61 -38(15) 2_756 . . . ? Cu3 Cu3 O12 O15 -133(6) 2_756 . . 2_756 ? N7 Cu3 O12 O15 27(6) 2_756 . . 2_756 ? O14 Cu3 O12 O15 -126(8) 2_756 . . 2_756 ? C68 Cu3 O12 O15 26(5) 2_756 . . 2_756 ? N6 Cu3 O12 O15 33(6) . . . 2_756 ? O14 Cu3 O12 O15 153(23) . . . 2_756 ? N7 Cu3 O12 O15 -145(6) . . . 2_756 ? N5 Cu3 O12 O15 146(6) . . . 2_756 ? N5' Cu3 O12 O15 124(6) . . . 2_756 ? N5 Cu3 O12 O15 -58(6) 2_756 . . 2_756 ? C67 Cu3 O12 O15 -8(12) 2_756 . . 2_756 ? Cu3 Cu3 O12 C68 -158.4(11) 2_756 . . 2_756 ? N7 Cu3 O12 C68 1.0(14) 2_756 . . 2_756 ? O14 Cu3 O12 C68 -152(3) 2_756 . . 2_756 ? N6 Cu3 O12 C68 7.3(12) . . . 2_756 ? O14 Cu3 O12 C68 127(28) . . . 2_756 ? N7 Cu3 O12 C68 -170.4(12) . . . 2_756 ? N5 Cu3 O12 C68 120.1(12) . . . 2_756 ? N5' Cu3 O12 C68 98.5(14) . . . 2_756 ? N5 Cu3 O12 C68 -84.1(13) 2_756 . . 2_756 ? C67 Cu3 O12 C68 -34(17) 2_756 . . 2_756 ? O14 O12 C61 C67 -8(9) 2_756 . . 2_756 ? O15 O12 C61 C67 -60(15) 2_756 . . 2_756 ? C68 O12 C61 C67 92(15) 2_756 . . 2_756 ? Cu3 O12 C61 C67 98(15) . . . 2_756 ? C67 O12 C61 O15 60(15) 2_756 . . 2_756 ? O14 O12 C61 O15 51(10) 2_756 . . 2_756 ? C68 O12 C61 O15 152(2) 2_756 . . 2_756 ? Cu3 O12 C61 O15 157(2) . . . 2_756 ? C67 O12 C61 O13 79(15) 2_756 . . . ? O14 O12 C61 O13 70(11) 2_756 . . . ? O15 O12 C61 O13 19(2) 2_756 . . . ? C68 O12 C61 O13 171(2) 2_756 . . . ? Cu3 O12 C61 O13 176.2(18) . . . . ? C67 O12 C61 C68 -92(15) 2_756 . . 2_756 ? O14 O12 C61 C68 -101(10) 2_756 . . 2_756 ? O15 O12 C61 C68 -152(2) 2_756 . . 2_756 ? Cu3 O12 C61 C68 5(2) . . . 2_756 ? C67 O12 C61 C62 -101(15) 2_756 . . . ? O14 O12 C61 C62 -110(10) 2_756 . . . ? O15 O12 C61 C62 -161(4) 2_756 . . . ? C68 O12 C61 C62 -9(3) 2_756 . . . ? Cu3 O12 C61 C62 -4(5) . . . . ? C67 O12 C61 C69 -102(15) 2_756 . . 2_756 ? O14 O12 C61 C69 -111(10) 2_756 . . 2_756 ? O15 O12 C61 C69 -162(4) 2_756 . . 2_756 ? C68 O12 C61 C69 -10(4) 2_756 . . 2_756 ? Cu3 O12 C61 C69 -5(5) . . . 2_756 ? O15 O13 C61 C67 -6(4) 2_756 . . 2_756 ? C67 O13 C61 O15 6(4) 2_756 . . 2_756 ? O15 O13 C61 O12 -28(3) 2_756 . . . ? C67 O13 C61 O12 -22(5) 2_756 . . . ? O15 O13 C61 C68 134(4) 2_756 . . 2_756 ? C67 O13 C61 C68 140(7) 2_756 . . 2_756 ? O15 O13 C61 C62 152(4) 2_756 . . . ? C67 O13 C61 C62 158(6) 2_756 . . . ? O15 O13 C61 C69 153(3) 2_756 . . 2_756 ? C67 O13 C61 C69 159(5) 2_756 . . 2_756 ? C67 C61 C62 C69 164(25) 2_756 . . 2_756 ? O15 C61 C62 C69 44(31) 2_756 . . 2_756 ? O12 C61 C62 C69 -176(25) . . . 2_756 ? O13 C61 C62 C69 4(28) . . . 2_756 ? C68 C61 C62 C69 169(30) 2_756 . . 2_756 ? C67 C61 C62 C68 -5(7) 2_756 . . 2_756 ? O15 C61 C62 C68 -124(6) 2_756 . . 2_756 ? O12 C61 C62 C68 15(6) . . . 2_756 ? O13 C61 C62 C68 -165(3) . . . 2_756 ? C69 C61 C62 C68 -169(30) 2_756 . . 2_756 ? C67 C61 C62 N6 -17(9) 2_756 . . . ? O15 C61 C62 N6 -137(5) 2_756 . . . ? O12 C61 C62 N6 3(8) . . . . ? O13 C61 C62 N6 -177(5) . . . . ? C68 C61 C62 N6 -12(3) 2_756 . . . ? C69 C61 C62 N6 179(32) 2_756 . . . ? C67 C61 C62 C63 161(6) 2_756 . . . ? O15 C61 C62 C63 41(12) 2_756 . . . ? O12 C61 C62 C63 -179(5) . . . . ? O13 C61 C62 C63 1(8) . . . . ? C68 C61 C62 C63 166(10) 2_756 . . . ? C69 C61 C62 C63 -3(20) 2_756 . . . ? C67 C61 C62 C70 -177(23) 2_756 . . 2_756 ? O15 C61 C62 C70 64(28) 2_756 . . 2_756 ? O12 C61 C62 C70 -156(24) . . . 2_756 ? O13 C61 C62 C70 24(27) . . . 2_756 ? C68 C61 C62 C70 -172(29) 2_756 . . 2_756 ? C69 C61 C62 C70 20(10) 2_756 . . 2_756 ? C67 C61 C62 N7 -13(6) 2_756 . . 2_756 ? O15 C61 C62 N7 -133(6) 2_756 . . 2_756 ? O12 C61 C62 N7 7(5) . . . 2_756 ? O13 C61 C62 N7 -172.9(19) . . . 2_756 ? C68 C61 C62 N7 -8.4(17) 2_756 . . 2_756 ? C69 C61 C62 N7 -177(29) 2_756 . . 2_756 ? C68 C62 C63 C69 -99(100) 2_756 . . 2_756 ? N6 C62 C63 C69 -23(100) . . . 2_756 ? C61 C62 C63 C69 158(100) . . . 2_756 ? C70 C62 C63 C69 -14(100) 2_756 . . 2_756 ? N7 C62 C63 C69 -31(100) 2_756 . . 2_756 ? C69 C62 C63 C70 14(100) 2_756 . . 2_756 ? C68 C62 C63 C70 -85(47) 2_756 . . 2_756 ? N6 C62 C63 C70 -9(6) . . . 2_756 ? C61 C62 C63 C70 173(6) . . . 2_756 ? N7 C62 C63 C70 -16(9) 2_756 . . 2_756 ? C69 C62 C63 C64 23(100) 2_756 . . . ? C68 C62 C63 C64 -76(48) 2_756 . . . ? N6 C62 C63 C64 0(9) . . . . ? C61 C62 C63 C64 -178(4) . . . . ? C70 C62 C63 C64 9(3) 2_756 . . . ? N7 C62 C63 C64 -8(11) 2_756 . . . ? C69 C63 C64 C70 -12(6) 2_756 . . 2_756 ? C62 C63 C64 C70 -13(5) . . . 2_756 ? C69 C63 C64 C65 2(6) 2_756 . . . ? C70 C63 C64 C65 13.5(17) 2_756 . . . ? C62 C63 C64 C65 0(5) . . . . ? C70 C63 C64 C69 12(6) 2_756 . . 2_756 ? C62 C63 C64 C69 -2(9) . . . 2_756 ? C70 C64 C65 C71 1(4) 2_756 . . 2_756 ? C63 C64 C65 C71 -13(4) . . . 2_756 ? C69 C64 C65 C71 -12(5) 2_756 . . 2_756 ? C63 C64 C65 C70 -14.1(18) . . . 2_756 ? C69 C64 C65 C70 -13(3) 2_756 . . 2_756 ? C70 C64 C65 C66 15(3) 2_756 . . . ? C63 C64 C65 C66 1(4) . . . . ? C69 C64 C65 C66 1(4) 2_756 . . . ? C70 C65 C66 C71 -101(28) 2_756 . . 2_756 ? C64 C65 C66 C71 -111(27) . . . 2_756 ? C71 C65 C66 C72 -21(48) 2_756 . . 2_756 ? C70 C65 C66 C72 -122(70) 2_756 . . 2_756 ? C64 C65 C66 C72 -132(69) . . . 2_756 ? C71 C65 C66 N6 109(29) 2_756 . . . ? C70 C65 C66 N6 8(4) 2_756 . . . ? C64 C65 C66 N6 -2(6) . . . . ? C71 C65 C66 C70 101(28) 2_756 . . 2_756 ? C64 C65 C66 C70 -10(2) . . . 2_756 ? C71 C65 C66 N7 117(31) 2_756 . . 2_756 ? C70 C65 C66 N7 16(6) 2_756 . . 2_756 ? C64 C65 C66 N7 6(8) . . . 2_756 ? C69 C62 N6 N7 -171(20) 2_756 . . 2_756 ? C68 C62 N6 N7 -2(6) 2_756 . . 2_756 ? C63 C62 N6 N7 -168(4) . . . 2_756 ? C61 C62 N6 N7 10(8) . . . 2_756 ? C70 C62 N6 N7 -175(2) 2_756 . . 2_756 ? C69 C62 N6 C68 -168(25) 2_756 . . 2_756 ? C63 C62 N6 C68 -166(9) . . . 2_756 ? C61 C62 N6 C68 12(3) . . . 2_756 ? C70 C62 N6 C68 -172(5) 2_756 . . 2_756 ? N7 C62 N6 C68 2(6) 2_756 . . 2_756 ? C69 C62 N6 C72 3(36) 2_756 . . 2_756 ? C68 C62 N6 C72 172(12) 2_756 . . 2_756 ? C63 C62 N6 C72 6(21) . . . 2_756 ? C61 C62 N6 C72 -176(10) . . . 2_756 ? C70 C62 N6 C72 -1(16) 2_756 . . 2_756 ? N7 C62 N6 C72 174(17) 2_756 . . 2_756 ? C69 C62 N6 C66 -4(24) 2_756 . . . ? C68 C62 N6 C66 165(3) 2_756 . . . ? C63 C62 N6 C66 -1(9) . . . . ? C61 C62 N6 C66 177(4) . . . . ? C70 C62 N6 C66 -8(5) 2_756 . . . ? N7 C62 N6 C66 167(6) 2_756 . . . ? C68 C62 N6 C69 168(25) 2_756 . . 2_756 ? C63 C62 N6 C69 3(16) . . . 2_756 ? C61 C62 N6 C69 -179(27) . . . 2_756 ? C70 C62 N6 C69 -4(20) 2_756 . . 2_756 ? N7 C62 N6 C69 171(20) 2_756 . . 2_756 ? C69 C62 N6 C71 4(23) 2_756 . . 2_756 ? C68 C62 N6 C71 172(3) 2_756 . . 2_756 ? C63 C62 N6 C71 6(8) . . . 2_756 ? C61 C62 N6 C71 -176(5) . . . 2_756 ? C70 C62 N6 C71 0(4) 2_756 . . 2_756 ? N7 C62 N6 C71 174(5) 2_756 . . 2_756 ? C69 C62 N6 C70 4(20) 2_756 . . 2_756 ? C68 C62 N6 C70 172(5) 2_756 . . 2_756 ? C63 C62 N6 C70 7(5) . . . 2_756 ? C61 C62 N6 C70 -175(7) . . . 2_756 ? N7 C62 N6 C70 175(2) 2_756 . . 2_756 ? C69 C62 N6 Cu3 178(20) 2_756 . . . ? C68 C62 N6 Cu3 -13(5) 2_756 . . . ? C63 C62 N6 Cu3 -179(5) . . . . ? C61 C62 N6 Cu3 -1(7) . . . . ? C70 C62 N6 Cu3 174.4(10) 2_756 . . . ? N7 C62 N6 Cu3 -10.8(16) 2_756 . . . ? C71 C66 N6 N7 -164(15) 2_756 . . 2_756 ? C72 C66 N6 N7 -15(4) 2_756 . . 2_756 ? C65 C66 N6 N7 170(3) . . . 2_756 ? C70 C66 N6 N7 176.2(18) 2_756 . . 2_756 ? C71 C66 N6 C68 61(20) 2_756 . . 2_756 ? C72 C66 N6 C68 -150(7) 2_756 . . 2_756 ? C65 C66 N6 C68 35(11) . . . 2_756 ? C70 C66 N6 C68 41(9) 2_756 . . 2_756 ? N7 C66 N6 C68 -135(9) 2_756 . . 2_756 ? C71 C66 N6 C72 -149(18) 2_756 . . 2_756 ? C65 C66 N6 C72 -175(6) . . . 2_756 ? C70 C66 N6 C72 -169(4) 2_756 . . 2_756 ? N7 C66 N6 C72 15(4) 2_756 . . 2_756 ? C71 C66 N6 C62 28(18) 2_756 . . . ? C72 C66 N6 C62 177(5) 2_756 . . . ? C65 C66 N6 C62 2(7) . . . . ? C70 C66 N6 C62 8(5) 2_756 . . . ? N7 C66 N6 C62 -168(6) 2_756 . . . ? C71 C66 N6 C69 27(17) 2_756 . . 2_756 ? C72 C66 N6 C69 176(4) 2_756 . . 2_756 ? C65 C66 N6 C69 1(6) . . . 2_756 ? C70 C66 N6 C69 7(4) 2_756 . . 2_756 ? N7 C66 N6 C69 -169(4) 2_756 . . 2_756 ? C72 C66 N6 C71 149(18) 2_756 . . 2_756 ? C65 C66 N6 C71 -26(13) . . . 2_756 ? C70 C66 N6 C71 -20(15) 2_756 . . 2_756 ? N7 C66 N6 C71 164(15) 2_756 . . 2_756 ? C71 C66 N6 C70 20(15) 2_756 . . 2_756 ? C72 C66 N6 C70 169(4) 2_756 . . 2_756 ? C65 C66 N6 C70 -6(3) . . . 2_756 ? N7 C66 N6 C70 -176.2(18) 2_756 . . 2_756 ? C71 C66 N6 Cu3 -154(14) 2_756 . . . ? C72 C66 N6 Cu3 -5(4) 2_756 . . . ? C65 C66 N6 Cu3 180(2) . . . . ? C70 C66 N6 Cu3 -174.4(12) 2_756 . . . ? N7 C66 N6 Cu3 9.4(12) 2_756 . . . ? Cu3 Cu3 N6 N7 -14(5) 2_756 . . 2_756 ? O14 Cu3 N6 N7 -137(4) 2_756 . . 2_756 ? C68 Cu3 N6 N7 -136(4) 2_756 . . 2_756 ? O12 Cu3 N6 N7 -146(4) . . . 2_756 ? O14 Cu3 N6 N7 36(4) . . . 2_756 ? N7 Cu3 N6 N7 -57(18) . . . 2_756 ? N5 Cu3 N6 N7 118(4) . . . 2_756 ? N5' Cu3 N6 N7 124(4) . . . 2_756 ? N5 Cu3 N6 N7 -56(4) 2_756 . . 2_756 ? C67 Cu3 N6 N7 -138(4) 2_756 . . 2_756 ? Cu3 Cu3 N6 C68 122.4(16) 2_756 . . 2_756 ? N7 Cu3 N6 C68 136(4) 2_756 . . 2_756 ? O14 Cu3 N6 C68 -0.6(13) 2_756 . . 2_756 ? O12 Cu3 N6 C68 -10.2(17) . . . 2_756 ? O14 Cu3 N6 C68 172.3(12) . . . 2_756 ? N7 Cu3 N6 C68 79(16) . . . 2_756 ? N5 Cu3 N6 C68 -106.1(12) . . . 2_756 ? N5' Cu3 N6 C68 -99.7(12) . . . 2_756 ? N5 Cu3 N6 C68 79.8(12) 2_756 . . 2_756 ? C67 Cu3 N6 C68 -2.3(19) 2_756 . . 2_756 ? Cu3 Cu3 N6 C72 -49.4(18) 2_756 . . 2_756 ? N7 Cu3 N6 C72 -36(4) 2_756 . . 2_756 ? O14 Cu3 N6 C72 -172.4(10) 2_756 . . 2_756 ? C68 Cu3 N6 C72 -171.8(17) 2_756 . . 2_756 ? O12 Cu3 N6 C72 178.0(15) . . . 2_756 ? O14 Cu3 N6 C72 0.5(10) . . . 2_756 ? N7 Cu3 N6 C72 -93(16) . . . 2_756 ? N5 Cu3 N6 C72 82.1(11) . . . 2_756 ? N5' Cu3 N6 C72 88.5(10) . . . 2_756 ? N5 Cu3 N6 C72 -92.0(10) 2_756 . . 2_756 ? C67 Cu3 N6 C72 -174.1(19) 2_756 . . 2_756 ? Cu3 Cu3 N6 C62 132(4) 2_756 . . . ? N7 Cu3 N6 C62 145(6) 2_756 . . . ? O14 Cu3 N6 C62 9(4) 2_756 . . . ? C68 Cu3 N6 C62 9(4) 2_756 . . . ? O12 Cu3 N6 C62 -1(4) . . . . ? O14 Cu3 N6 C62 -178(4) . . . . ? N7 Cu3 N6 C62 88(16) . . . . ? N5 Cu3 N6 C62 -97(4) . . . . ? N5' Cu3 N6 C62 -90(4) . . . . ? N5 Cu3 N6 C62 89(4) 2_756 . . . ? C67 Cu3 N6 C62 7(4) 2_756 . . . ? Cu3 Cu3 N6 C66 -46(3) 2_756 . . . ? N7 Cu3 N6 C66 -32(4) 2_756 . . . ? O14 Cu3 N6 C66 -169(3) 2_756 . . . ? C68 Cu3 N6 C66 -168(3) 2_756 . . . ? O12 Cu3 N6 C66 -179(3) . . . . ? O14 Cu3 N6 C66 4(3) . . . . ? N7 Cu3 N6 C66 -90(16) . . . . ? N5 Cu3 N6 C66 86(3) . . . . ? N5' Cu3 N6 C66 92(3) . . . . ? N5 Cu3 N6 C66 -88(3) 2_756 . . . ? C67 Cu3 N6 C66 -171(3) 2_756 . . . ? Cu3 Cu3 N6 C69 132(4) 2_756 . . 2_756 ? N7 Cu3 N6 C69 146(6) 2_756 . . 2_756 ? O14 Cu3 N6 C69 9(4) 2_756 . . 2_756 ? C68 Cu3 N6 C69 10(5) 2_756 . . 2_756 ? O12 Cu3 N6 C69 0(4) . . . 2_756 ? O14 Cu3 N6 C69 -178(4) . . . 2_756 ? N7 Cu3 N6 C69 89(16) . . . 2_756 ? N5 Cu3 N6 C69 -96(4) . . . 2_756 ? N5' Cu3 N6 C69 -90(4) . . . 2_756 ? N5 Cu3 N6 C69 90(4) 2_756 . . 2_756 ? C67 Cu3 N6 C69 8(4) 2_756 . . 2_756 ? Cu3 Cu3 N6 C71 -56(3) 2_756 . . 2_756 ? N7 Cu3 N6 C71 -42(5) 2_756 . . 2_756 ? O14 Cu3 N6 C71 -179(3) 2_756 . . 2_756 ? C68 Cu3 N6 C71 -178(3) 2_756 . . 2_756 ? O12 Cu3 N6 C71 171(3) . . . 2_756 ? O14 Cu3 N6 C71 -6(3) . . . 2_756 ? N7 Cu3 N6 C71 -100(16) . . . 2_756 ? N5 Cu3 N6 C71 76(3) . . . 2_756 ? N5' Cu3 N6 C71 82(3) . . . 2_756 ? N5 Cu3 N6 C71 -98(3) 2_756 . . 2_756 ? C67 Cu3 N6 C71 179(3) 2_756 . . 2_756 ? Cu3 Cu3 N6 C70 169(6) 2_756 . . 2_756 ? N7 Cu3 N6 C70 -177(9) 2_756 . . 2_756 ? O14 Cu3 N6 C70 47(6) 2_756 . . 2_756 ? C68 Cu3 N6 C70 47(6) 2_756 . . 2_756 ? O12 Cu3 N6 C70 37(6) . . . 2_756 ? O14 Cu3 N6 C70 -141(6) . . . 2_756 ? N7 Cu3 N6 C70 126(14) . . . 2_756 ? N5 Cu3 N6 C70 -59(6) . . . 2_756 ? N5' Cu3 N6 C70 -53(6) . . . 2_756 ? N5 Cu3 N6 C70 127(6) 2_756 . . 2_756 ? C67 Cu3 N6 C70 45(7) 2_756 . . 2_756 ? Cu3 Cu3 O14 O12 7(2) 2_756 . . 2_756 ? N7 Cu3 O14 O12 -152(2) 2_756 . . 2_756 ? O14 Cu3 O14 O12 7(2) 2_756 . . 2_756 ? C68 Cu3 O14 O12 -153(2) 2_756 . . 2_756 ? O12 Cu3 O14 O12 82(30) . . . 2_756 ? N6 Cu3 O14 O12 -158(2) . . . 2_756 ? N7 Cu3 O14 O12 19(2) . . . 2_756 ? N5 Cu3 O14 O12 89(2) . . . 2_756 ? N5' Cu3 O14 O12 111(2) . . . 2_756 ? N5 Cu3 O14 O12 -67(2) 2_756 . . 2_756 ? C67 Cu3 O14 O12 -123(15) 2_756 . . 2_756 ? Cu3 Cu3 O14 C67 -14(3) 2_756 . . . ? N7 Cu3 O14 C67 -172(3) 2_756 . . . ? O14 Cu3 O14 C67 -14(3) 2_756 . . . ? C68 Cu3 O14 C67 -173(3) 2_756 . . . ? O12 Cu3 O14 C67 62(27) . . . . ? N6 Cu3 O14 C67 -178(3) . . . . ? N7 Cu3 O14 C67 -1(3) . . . . ? N5 Cu3 O14 C67 69(3) . . . . ? N5' Cu3 O14 C67 91(3) . . . . ? N5 Cu3 O14 C67 -87(3) 2_756 . . . ? C67 Cu3 O14 C67 -143(11) 2_756 . . . ? N7 Cu3 O14 Cu3 -158.2(6) 2_756 . . 2_756 ? O14 Cu3 O14 Cu3 0.0 2_756 . . 2_756 ? C68 Cu3 O14 Cu3 -159.4(8) 2_756 . . 2_756 ? O12 Cu3 O14 Cu3 76(29) . . . 2_756 ? N6 Cu3 O14 Cu3 -165.0(4) . . . 2_756 ? N7 Cu3 O14 Cu3 12.7(4) . . . 2_756 ? N5 Cu3 O14 Cu3 82.7(4) . . . 2_756 ? N5' Cu3 O14 Cu3 104.3(4) . . . 2_756 ? N5 Cu3 O14 Cu3 -73.2(4) 2_756 . . 2_756 ? C67 Cu3 O14 Cu3 -130(13) 2_756 . . 2_756 ? Cu3 O14 C67 O12 69(13) 2_756 . . 2_756 ? Cu3 O14 C67 O12 75(13) . . . 2_756 ? O12 O14 C67 C61 12(13) 2_756 . . 2_756 ? Cu3 O14 C67 C61 81(23) 2_756 . . 2_756 ? Cu3 O14 C67 C61 87(23) . . . 2_756 ? O12 O14 C67 O15 111(15) 2_756 . . . ? Cu3 O14 C67 O15 180(5) 2_756 . . . ? Cu3 O14 C67 O15 -174(4) . . . . ? O12 O14 C67 C68 -74(12) 2_756 . . . ? Cu3 O14 C67 C68 -5(4) 2_756 . . . ? Cu3 O14 C67 C68 1(5) . . . . ? O12 O14 C67 O13 94(15) 2_756 . . 2_756 ? Cu3 O14 C67 O13 163(7) 2_756 . . 2_756 ? Cu3 O14 C67 O13 169(6) . . . 2_756 ? O12 O14 C67 Cu3 -69(13) 2_756 . . 2_756 ? Cu3 O14 C67 Cu3 6.1(12) . . . 2_756 ? O13 O15 C67 O12 -106(23) 2_756 . . 2_756 ? C61 O15 C67 O12 -112(25) 2_756 . . 2_756 ? O13 O15 C67 C61 6(4) 2_756 . . 2_756 ? O12 O15 C67 C61 112(25) 2_756 . . 2_756 ? O13 O15 C67 O14 -156(4) 2_756 . . . ? C61 O15 C67 O14 -162(7) 2_756 . . . ? O12 O15 C67 O14 -50(19) 2_756 . . . ? O13 O15 C67 C68 28(5) 2_756 . . . ? C61 O15 C67 C68 22(2) 2_756 . . . ? O12 O15 C67 C68 135(27) 2_756 . . . ? C61 O15 C67 O13 -6(4) 2_756 . . 2_756 ? O12 O15 C67 O13 106(23) 2_756 . . 2_756 ? O13 O15 C67 Cu3 22(34) 2_756 . . 2_756 ? C61 O15 C67 Cu3 16(30) 2_756 . . 2_756 ? O12 O15 C67 Cu3 128(53) 2_756 . . 2_756 ? C66 C72 N7 N6 15(4) 2_756 . . 2_756 ? C71 C72 N7 N6 6(3) . . . 2_756 ? Cu3 C72 N7 N6 -157(2) 2_756 . . 2_756 ? C66 C72 N7 Cu3 172(4) 2_756 . . 2_756 ? N6 C72 N7 Cu3 157(2) 2_756 . . 2_756 ? C71 C72 N7 Cu3 162(3) . . . 2_756 ? C66 C72 N7 C68 12(4) 2_756 . . . ? N6 C72 N7 C68 -3.3(15) 2_756 . . . ? C71 C72 N7 C68 2(4) . . . . ? Cu3 C72 N7 C68 -160(3) 2_756 . . . ? N6 C72 N7 C66 -15(4) 2_756 . . 2_756 ? C71 C72 N7 C66 -9(6) . . . 2_756 ? Cu3 C72 N7 C66 -172(4) 2_756 . . 2_756 ? C66 C72 N7 C62 14(5) 2_756 . . 2_756 ? N6 C72 N7 C62 -1(3) 2_756 . . 2_756 ? C71 C72 N7 C62 5(4) . . . 2_756 ? Cu3 C72 N7 C62 -157(3) 2_756 . . 2_756 ? C66 C72 N7 Cu3 -174(4) 2_756 . . . ? N6 C72 N7 Cu3 170.5(19) 2_756 . . . ? C71 C72 N7 Cu3 176(3) . . . . ? Cu3 C72 N7 Cu3 14.0(7) 2_756 . . . ? Cu3 Cu3 N7 N6 16(5) 2_756 . . 2_756 ? N7 Cu3 N7 N6 16(5) 2_756 . . 2_756 ? O14 Cu3 N7 N6 144(6) 2_756 . . 2_756 ? C68 Cu3 N7 N6 140(6) 2_756 . . 2_756 ? O12 Cu3 N7 N6 153(6) . . . 2_756 ? N6 Cu3 N7 N6 65(20) . . . 2_756 ? O14 Cu3 N7 N6 -30(6) . . . 2_756 ? N5 Cu3 N7 N6 -111(6) . . . 2_756 ? N5' Cu3 N7 N6 -117(6) . . . 2_756 ? N5 Cu3 N7 N6 63(6) 2_756 . . 2_756 ? C67 Cu3 N7 N6 145(6) 2_756 . . 2_756 ? N7 Cu3 N7 Cu3 0.00(2) 2_756 . . 2_756 ? O14 Cu3 N7 Cu3 128.8(13) 2_756 . . 2_756 ? C68 Cu3 N7 Cu3 124.2(16) 2_756 . . 2_756 ? O12 Cu3 N7 Cu3 137.5(17) . . . 2_756 ? N6 Cu3 N7 Cu3 49(17) . . . 2_756 ? O14 Cu3 N7 Cu3 -45.1(12) . . . 2_756 ? N5 Cu3 N7 Cu3 -126.3(14) . . . 2_756 ? N5' Cu3 N7 Cu3 -132.7(13) . . . 2_756 ? N5 Cu3 N7 Cu3 47.7(13) 2_756 . . 2_756 ? C67 Cu3 N7 Cu3 129.2(19) 2_756 . . 2_756 ? Cu3 Cu3 N7 C72 -129(2) 2_756 . . . ? N7 Cu3 N7 C72 -129(2) 2_756 . . . ? O14 Cu3 N7 C72 -0.4(13) 2_756 . . . ? C68 Cu3 N7 C72 -5(2) 2_756 . . . ? O12 Cu3 N7 C72 8.3(17) . . . . ? N6 Cu3 N7 C72 -80(16) . . . . ? O14 Cu3 N7 C72 -174.4(14) . . . . ? N5 Cu3 N7 C72 104.4(14) . . . . ? N5' Cu3 N7 C72 98.0(13) . . . . ? N5 Cu3 N7 C72 -81.5(13) 2_756 . . . ? C67 Cu3 N7 C72 0(2) 2_756 . . . ? Cu3 Cu3 N7 C68 45.3(14) 2_756 . . . ? N7 Cu3 N7 C68 45.3(14) 2_756 . . . ? O14 Cu3 N7 C68 174.1(12) 2_756 . . . ? C68 Cu3 N7 C68 169.5(4) 2_756 . . . ? O12 Cu3 N7 C68 -177.2(15) . . . . ? N6 Cu3 N7 C68 94(16) . . . . ? O14 Cu3 N7 C68 0.2(11) . . . . ? N5 Cu3 N7 C68 -81.0(12) . . . . ? N5' Cu3 N7 C68 -87.4(11) . . . . ? N5 Cu3 N7 C68 93.1(12) 2_756 . . . ? C67 Cu3 N7 C68 174.5(18) 2_756 . . . ? Cu3 Cu3 N7 C66 -135(4) 2_756 . . 2_756 ? N7 Cu3 N7 C66 -135(4) 2_756 . . 2_756 ? O14 Cu3 N7 C66 -6(4) 2_756 . . 2_756 ? C68 Cu3 N7 C66 -11(4) 2_756 . . 2_756 ? O12 Cu3 N7 C66 3(4) . . . 2_756 ? N6 Cu3 N7 C66 -86(16) . . . 2_756 ? O14 Cu3 N7 C66 -180(4) . . . 2_756 ? N5 Cu3 N7 C66 99(4) . . . 2_756 ? N5' Cu3 N7 C66 93(4) . . . 2_756 ? N5 Cu3 N7 C66 -87(4) 2_756 . . 2_756 ? C67 Cu3 N7 C66 -5(4) 2_756 . . 2_756 ? Cu3 Cu3 N7 C62 39(3) 2_756 . . 2_756 ? N7 Cu3 N7 C62 39(3) 2_756 . . 2_756 ? O14 Cu3 N7 C62 168(3) 2_756 . . 2_756 ? C68 Cu3 N7 C62 164(3) 2_756 . . 2_756 ? O12 Cu3 N7 C62 177(4) . . . 2_756 ? N6 Cu3 N7 C62 88(16) . . . 2_756 ? O14 Cu3 N7 C62 -6(3) . . . 2_756 ? N5 Cu3 N7 C62 -87(3) . . . 2_756 ? N5' Cu3 N7 C62 -93(3) . . . 2_756 ? N5 Cu3 N7 C62 87(3) 2_756 . . 2_756 ? C67 Cu3 N7 C62 169(4) 2_756 . . 2_756 ? N6 N7 C68 C62 2(6) 2_756 . . 2_756 ? Cu3 N7 C68 C62 -160(5) 2_756 . . 2_756 ? C72 N7 C68 C62 6(6) . . . 2_756 ? C66 N7 C68 C62 11(6) 2_756 . . 2_756 ? Cu3 N7 C68 C62 -169(5) . . . 2_756 ? Cu3 N7 C68 N6 -162.1(18) 2_756 . . 2_756 ? C72 N7 C68 N6 3.5(16) . . . 2_756 ? C66 N7 C68 N6 9(2) 2_756 . . 2_756 ? C62 N7 C68 N6 -2(6) 2_756 . . 2_756 ? Cu3 N7 C68 N6 -171.3(16) . . . 2_756 ? N6 N7 C68 C61 150(5) 2_756 . . 2_756 ? Cu3 N7 C68 C61 -12(4) 2_756 . . 2_756 ? C72 N7 C68 C61 154(4) . . . 2_756 ? C66 N7 C68 C61 159(4) 2_756 . . 2_756 ? C62 N7 C68 C61 148(7) 2_756 . . 2_756 ? Cu3 N7 C68 C61 -21(5) . . . 2_756 ? N6 N7 C68 C69 -2(5) 2_756 . . . ? Cu3 N7 C68 C69 -164(5) 2_756 . . . ? C72 N7 C68 C69 1(5) . . . . ? C66 N7 C68 C69 7(5) 2_756 . . . ? C62 N7 C68 C69 -5(9) 2_756 . . . ? Cu3 N7 C68 C69 -173(5) . . . . ? N6 N7 C68 C67 172(3) 2_756 . . . ? Cu3 N7 C68 C67 10(3) 2_756 . . . ? C72 N7 C68 C67 175(3) . . . . ? C66 N7 C68 C67 -180(3) 2_756 . . . ? C62 N7 C68 C67 169(6) 2_756 . . . ? Cu3 N7 C68 C67 0(3) . . . . ? N6 N7 C68 O12 161(2) 2_756 . . 2_756 ? Cu3 N7 C68 O12 -1(2) 2_756 . . 2_756 ? C72 N7 C68 O12 164(2) . . . 2_756 ? C66 N7 C68 O12 169(2) 2_756 . . 2_756 ? C62 N7 C68 O12 158(6) 2_756 . . 2_756 ? Cu3 N7 C68 O12 -11(2) . . . 2_756 ? N6 N7 C68 Cu3 162.1(18) 2_756 . . 2_756 ? C72 N7 C68 Cu3 165.6(19) . . . 2_756 ? C66 N7 C68 Cu3 171(2) 2_756 . . 2_756 ? C62 N7 C68 Cu3 160(5) 2_756 . . 2_756 ? Cu3 N7 C68 Cu3 -9.2(3) . . . 2_756 ? O12 C67 C68 C62 130(15) 2_756 . . 2_756 ? C61 C67 C68 C62 5(7) 2_756 . . 2_756 ? O14 C67 C68 C62 168(6) . . . 2_756 ? O15 C67 C68 C62 -16(7) . . . 2_756 ? O13 C67 C68 C62 -5(6) 2_756 . . 2_756 ? Cu3 C67 C68 C62 163(6) 2_756 . . 2_756 ? O12 C67 C68 N6 -23(22) 2_756 . . 2_756 ? C61 C67 C68 N6 -149(7) 2_756 . . 2_756 ? O14 C67 C68 N6 14(12) . . . 2_756 ? O15 C67 C68 N6 -170(6) . . . 2_756 ? O13 C67 C68 N6 -159(7) 2_756 . . 2_756 ? Cu3 C67 C68 N6 9(9) 2_756 . . 2_756 ? O12 C67 C68 C61 125(17) 2_756 . . 2_756 ? O14 C67 C68 C61 163(7) . . . 2_756 ? O15 C67 C68 C61 -21(2) . . . 2_756 ? O13 C67 C68 C61 -10.5(16) 2_756 . . 2_756 ? Cu3 C67 C68 C61 158(3) 2_756 . . 2_756 ? O12 C67 C68 N7 -39(16) 2_756 . . . ? C61 C67 C68 N7 -164(3) 2_756 . . . ? O14 C67 C68 N7 -1(6) . . . . ? O15 C67 C68 N7 175(3) . . . . ? O13 C67 C68 N7 -174.5(16) 2_756 . . . ? Cu3 C67 C68 N7 -6.1(19) 2_756 . . . ? O12 C67 C68 C69 135(15) 2_756 . . . ? C61 C67 C68 C69 9(6) 2_756 . . . ? O14 C67 C68 C69 172(6) . . . . ? O15 C67 C68 C69 -12(8) . . . . ? O13 C67 C68 C69 -1(6) 2_756 . . . ? Cu3 C67 C68 C69 167(6) 2_756 . . . ? C61 C67 C68 O12 -125(17) 2_756 . . 2_756 ? O14 C67 C68 O12 38(11) . . . 2_756 ? O15 C67 C68 O12 -146(19) . . . 2_756 ? O13 C67 C68 O12 -136(16) 2_756 . . 2_756 ? Cu3 C67 C68 O12 33(15) 2_756 . . 2_756 ? O12 C67 C68 Cu3 -33(15) 2_756 . . 2_756 ? C61 C67 C68 Cu3 -158(3) 2_756 . . 2_756 ? O14 C67 C68 Cu3 5(4) . . . 2_756 ? O15 C67 C68 Cu3 -179(4) . . . 2_756 ? O13 C67 C68 Cu3 -168(2) 2_756 . . 2_756 ? N6 C68 C69 C62 124(100) 2_756 . . 2_756 ? C61 C68 C69 C62 -42(100) 2_756 . . 2_756 ? N7 C68 C69 C62 126(100) . . . 2_756 ? C67 C68 C69 C62 -48(100) . . . 2_756 ? O12 C68 C69 C62 -31(100) 2_756 . . 2_756 ? Cu3 C68 C69 C62 104(100) 2_756 . . 2_756 ? C62 C68 C69 C63 120(100) 2_756 . . 2_756 ? N6 C68 C69 C63 -115(57) 2_756 . . 2_756 ? C61 C68 C69 C63 78(57) 2_756 . . 2_756 ? N7 C68 C69 C63 -114(57) . . . 2_756 ? C67 C68 C69 C63 73(58) . . . 2_756 ? O12 C68 C69 C63 90(57) 2_756 . . 2_756 ? Cu3 C68 C69 C63 -136(51) 2_756 . . 2_756 ? C62 C68 C69 C70 -129(100) 2_756 . . . ? N6 C68 C69 C70 -5(7) 2_756 . . . ? C61 C68 C69 C70 -171(7) 2_756 . . . ? N7 C68 C69 C70 -3(10) . . . . ? C67 C68 C69 C70 -177(4) . . . . ? O12 C68 C69 C70 -160(4) 2_756 . . . ? Cu3 C68 C69 C70 -25(15) 2_756 . . . ? C62 C68 C69 N6 -124(100) 2_756 . . 2_756 ? C61 C68 C69 N6 -166.4(16) 2_756 . . 2_756 ? N7 C68 C69 N6 1(3) . . . 2_756 ? C67 C68 C69 N6 -172(4) . . . 2_756 ? O12 C68 C69 N6 -155(5) 2_756 . . 2_756 ? Cu3 C68 C69 N6 -21(9) 2_756 . . 2_756 ? C62 C68 C69 C61 42(100) 2_756 . . 2_756 ? N6 C68 C69 C61 166.4(16) 2_756 . . 2_756 ? N7 C68 C69 C61 168(4) . . . 2_756 ? C67 C68 C69 C61 -6(4) . . . 2_756 ? O12 C68 C69 C61 11(5) 2_756 . . 2_756 ? Cu3 C68 C69 C61 146(10) 2_756 . . 2_756 ? C62 C68 C69 C64 -145(100) 2_756 . . 2_756 ? N6 C68 C69 C64 -21(10) 2_756 . . 2_756 ? C61 C68 C69 C64 173(10) 2_756 . . 2_756 ? N7 C68 C69 C64 -19(13) . . . 2_756 ? C67 C68 C69 C64 167(8) . . . 2_756 ? O12 C68 C69 C64 -176(6) 2_756 . . 2_756 ? Cu3 C68 C69 C64 -42(17) 2_756 . . 2_756 ? C62 C69 C70 C64 -166(24) 2_756 . . 2_756 ? C63 C69 C70 C64 11(6) 2_756 . . 2_756 ? C68 C69 C70 C64 -157(6) . . . 2_756 ? N6 C69 C70 C64 -161(2) 2_756 . . 2_756 ? C61 C69 C70 C64 176(23) 2_756 . . 2_756 ? C62 C69 C70 C65 -40(32) 2_756 . . 2_756 ? C63 C69 C70 C65 137(6) 2_756 . . 2_756 ? C68 C69 C70 C65 -32(14) . . . 2_756 ? N6 C69 C70 C65 -35(10) 2_756 . . 2_756 ? C61 C69 C70 C65 -59(30) 2_756 . . 2_756 ? C64 C69 C70 C65 125(10) 2_756 . . 2_756 ? C62 C69 C70 C63 -177(30) 2_756 . . 2_756 ? C68 C69 C70 C63 -169(10) . . . 2_756 ? N6 C69 C70 C63 -172(6) 2_756 . . 2_756 ? C61 C69 C70 C63 165(29) 2_756 . . 2_756 ? C64 C69 C70 C63 -11(6) 2_756 . . 2_756 ? C62 C69 C70 C71 -7(28) 2_756 . . . ? C63 C69 C70 C71 170(3) 2_756 . . . ? C68 C69 C70 C71 1(9) . . . . ? N6 C69 C70 C71 -2(5) 2_756 . . . ? C61 C69 C70 C71 -25(27) 2_756 . . . ? C64 C69 C70 C71 159(5) 2_756 . . . ? C62 C69 C70 C66 -11(27) 2_756 . . 2_756 ? C63 C69 C70 C66 166(4) 2_756 . . 2_756 ? C68 C69 C70 C66 -3(8) . . . 2_756 ? N6 C69 C70 C66 -6(4) 2_756 . . 2_756 ? C61 C69 C70 C66 -30(26) 2_756 . . 2_756 ? C64 C69 C70 C66 154(4) 2_756 . . 2_756 ? C63 C69 C70 C62 177(30) 2_756 . . 2_756 ? C68 C69 C70 C62 8(20) . . . 2_756 ? N6 C69 C70 C62 5(24) 2_756 . . 2_756 ? C61 C69 C70 C62 -18(8) 2_756 . . 2_756 ? C64 C69 C70 C62 166(24) 2_756 . . 2_756 ? C62 C69 C70 N6 -5(24) 2_756 . . 2_756 ? C63 C69 C70 N6 172(6) 2_756 . . 2_756 ? C68 C69 C70 N6 3(5) . . . 2_756 ? C61 C69 C70 N6 -23(23) 2_756 . . 2_756 ? C64 C69 C70 N6 161(2) 2_756 . . 2_756 ? C64 C70 C71 C66 143(13) 2_756 . . 2_756 ? C65 C70 C71 C66 145(15) 2_756 . . 2_756 ? C63 C70 C71 C66 2(19) 2_756 . . 2_756 ? C69 C70 C71 C66 -14(15) . . . 2_756 ? C62 C70 C71 C66 -16(14) 2_756 . . 2_756 ? N6 C70 C71 C66 -16(12) 2_756 . . 2_756 ? C64 C70 C71 C65 -1(4) 2_756 . . 2_756 ? C63 C70 C71 C65 -143(6) 2_756 . . 2_756 ? C69 C70 C71 C65 -159(5) . . . 2_756 ? C66 C70 C71 C65 -145(15) 2_756 . . 2_756 ? C62 C70 C71 C65 -160(3) 2_756 . . 2_756 ? N6 C70 C71 C65 -161(4) 2_756 . . 2_756 ? C64 C70 C71 C72 160(3) 2_756 . . . ? C65 C70 C71 C72 161(6) 2_756 . . . ? C63 C70 C71 C72 18(10) 2_756 . . . ? C69 C70 C71 C72 2(7) . . . . ? C66 C70 C71 C72 16(10) 2_756 . . . ? C62 C70 C71 C72 1(5) 2_756 . . . ? N6 C70 C71 C72 0(3) 2_756 . . . ? C64 C70 C71 N6 159(2) 2_756 . . 2_756 ? C65 C70 C71 N6 161(4) 2_756 . . 2_756 ? C63 C70 C71 N6 18(7) 2_756 . . 2_756 ? C69 C70 C71 N6 2(5) . . . 2_756 ? C66 C70 C71 N6 16(12) 2_756 . . 2_756 ? C62 C70 C71 N6 0(3) 2_756 . . 2_756 ? N6 C72 C71 C66 63(35) 2_756 . . 2_756 ? N7 C72 C71 C66 59(36) . . . 2_756 ? Cu3 C72 C71 C66 70(36) 2_756 . . 2_756 ? C66 C72 C71 C65 8(19) 2_756 . . 2_756 ? N6 C72 C71 C65 71(21) 2_756 . . 2_756 ? N7 C72 C71 C65 67(22) . . . 2_756 ? Cu3 C72 C71 C65 78(22) 2_756 . . 2_756 ? C66 C72 C71 C70 -63(33) 2_756 . . . ? N6 C72 C71 C70 0(4) 2_756 . . . ? N7 C72 C71 C70 -4(6) . . . . ? Cu3 C72 C71 C70 7(7) 2_756 . . . ? C66 C72 C71 N6 -63(35) 2_756 . . 2_756 ? N7 C72 C71 N6 -4(2) . . . 2_756 ? Cu3 C72 C71 N6 7(4) 2_756 . . 2_756 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.783 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.091 data_4 _database_code_depnum_ccdc_archive 'CCDC 884074' #TrackingRef 'web_deposit_cif_file_0_feilonghu_1350638779.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H54 Co3 N4 O20' _chemical_formula_weight 1520.02 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.682(7) _cell_length_b 15.358(10) _cell_length_c 20.449(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.388(8) _cell_angle_gamma 90.00 _cell_volume 3349(4) _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 Flake _exptl_crystal_colour Pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1558 _exptl_absorpt_coefficient_mu 0.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8473 _exptl_absorpt_correction_T_max 0.9839 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18232 _diffrn_reflns_av_R_equivalents 0.1333 _diffrn_reflns_av_sigmaI/netI 0.1703 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5821 _reflns_number_gt 2586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.1072P)^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 5821 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1921 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2355 _refine_ls_wR_factor_gt 0.1955 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Co1 Co 0.25402(10) -0.03945(8) 0.41144(6) 0.0341(4) Uani 1 1 d . . . Co2 Co 0.5000 0.0000 0.5000 0.0318(5) Uani 1 2 d S . . N1 N 0.1774(7) -0.1528(5) 0.3611(4) 0.045(2) Uani 1 1 d . . . N2 N 0.1432(7) 0.0445(5) 0.3487(3) 0.0407(18) Uani 1 1 d . . . O1 O 0.3320(5) 0.0692(4) 0.4679(3) 0.0358(14) Uani 1 1 d . . . O2 O 0.1706(6) 0.1026(4) 0.5277(3) 0.0513(17) Uani 1 1 d . . . O3 O 0.3913(5) -0.0360(4) 0.3465(2) 0.0378(14) Uani 1 1 d . . . O4 O 0.5630(5) -0.0133(4) 0.4113(3) 0.0387(15) Uani 1 1 d . . . O5 O 0.8272(8) -0.0707(5) 0.1489(4) 0.082(3) Uani 1 1 d . . . O6 O 0.8092(10) 0.1760(5) -0.1077(4) 0.088(3) Uani 1 1 d . . . H6A H 0.7952 0.2007 -0.0734 0.132 Uiso 1 1 calc R . . O7 O 0.8091(12) 0.0427(6) -0.1468(4) 0.122(4) Uani 1 1 d . . . O8 O 0.3726(5) -0.1086(4) 0.4846(3) 0.0369(15) Uani 1 1 d . . . O9 O 0.2286(6) -0.1913(4) 0.5281(3) 0.0566(18) Uani 1 1 d . . . O10 O 0.1090(5) -0.0480(4) 0.4751(3) 0.0426(15) Uani 1 1 d . . . H10B H 0.1278 -0.0895 0.5013 0.051 Uiso 1 1 d R . . H10A H 0.1064 -0.0033 0.4969 0.064 Uiso 1 1 d R . . C1 C 0.0615(10) -0.1821(7) 0.3711(5) 0.063(3) Uani 1 1 d . . . H1 H 0.0196 -0.1587 0.4056 0.076 Uiso 1 1 calc R . . C2 C 0.0023(9) -0.2445(7) 0.3332(5) 0.060(3) Uani 1 1 d . . . H2 H -0.0761 -0.2645 0.3440 0.072 Uiso 1 1 calc R . . C3 C 0.0554(8) -0.2781(6) 0.2802(4) 0.043(2) Uani 1 1 d . . . C4 C 0.1742(9) -0.2487(7) 0.2704(5) 0.060(3) Uani 1 1 d . . . H4 H 0.2166 -0.2707 0.2355 0.073 Uiso 1 1 calc R . . C5 C 0.2316(9) -0.1879(7) 0.3107(5) 0.061(3) Uani 1 1 d . . . H5 H 0.3125 -0.1703 0.3025 0.073 Uiso 1 1 calc R . . C6 C 0.0642(10) 0.1026(7) 0.3708(4) 0.056(3) Uani 1 1 d . . . H6 H 0.0537 0.1046 0.4156 0.067 Uiso 1 1 calc R . . C7 C -0.0036(10) 0.1605(6) 0.3305(5) 0.055(3) Uani 1 1 d . . . H7 H -0.0585 0.1998 0.3481 0.066 Uiso 1 1 calc R . . C8 C 0.0112(8) 0.1593(6) 0.2641(4) 0.044(2) Uani 1 1 d . . . C9 C 0.0908(9) 0.0985(7) 0.2403(5) 0.053(3) Uani 1 1 d . . . H9 H 0.1028 0.0951 0.1957 0.064 Uiso 1 1 calc R . . C10 C 0.1525(9) 0.0426(7) 0.2837(5) 0.053(3) Uani 1 1 d . . . H10 H 0.2043 0.0006 0.2668 0.063 Uiso 1 1 calc R . . C11 C 0.5682(8) 0.1881(6) 0.4172(4) 0.039(2) Uani 1 1 d . . . C12 C 0.5987(9) 0.1751(6) 0.3529(4) 0.046(2) Uani 1 1 d . . . H12 H 0.6774 0.1532 0.3446 0.055 Uiso 1 1 calc R . . C13 C 0.5149(10) 0.1938(7) 0.3012(5) 0.058(3) Uani 1 1 d . . . H13 H 0.5361 0.1848 0.2583 0.070 Uiso 1 1 calc R . . C14 C 0.3995(10) 0.2259(7) 0.3144(5) 0.064(3) Uani 1 1 d . . . H14 H 0.3410 0.2378 0.2800 0.077 Uiso 1 1 calc R . . C15 C 0.3690(9) 0.2408(6) 0.3777(5) 0.051(3) Uani 1 1 d . . . H15 H 0.2911 0.2640 0.3859 0.061 Uiso 1 1 calc R . . C16 C 0.4533(9) 0.2215(6) 0.4291(5) 0.044(2) Uani 1 1 d . . . C17 C 0.4241(9) 0.2451(6) 0.4979(5) 0.045(2) Uani 1 1 d . . . C18 C 0.4789(10) 0.3194(7) 0.5265(5) 0.061(3) Uani 1 1 d . . . H18 H 0.5362 0.3505 0.5032 0.073 Uiso 1 1 calc R . . C19 C 0.4530(10) 0.3478(8) 0.5856(6) 0.071(3) Uani 1 1 d . . . H19 H 0.4897 0.3986 0.6025 0.085 Uiso 1 1 calc R . . C20 C 0.3702(11) 0.3006(7) 0.6221(5) 0.067(3) Uani 1 1 d . . . H20 H 0.3519 0.3191 0.6638 0.081 Uiso 1 1 calc R . . C21 C 0.3162(9) 0.2269(7) 0.5960(5) 0.053(3) Uani 1 1 d . . . H21 H 0.2617 0.1952 0.6206 0.064 Uiso 1 1 calc R . . C22 C 0.3405(9) 0.1979(6) 0.5334(5) 0.044(2) Uani 1 1 d . . . C23 C 0.2764(9) 0.1177(6) 0.5081(4) 0.037(2) Uani 1 1 d . . . C24 C 0.3378(9) -0.1613(6) 0.5284(5) 0.042(2) Uani 1 1 d . . . C25 C 0.5088(8) -0.0270(5) 0.3565(4) 0.033(2) Uani 1 1 d . . . C26 C 0.5913(8) -0.0341(6) 0.2993(4) 0.038(2) Uani 1 1 d . . . C27 C 0.7204(8) -0.0349(6) 0.3106(4) 0.048(3) Uani 1 1 d . . . H27 H 0.7558 -0.0284 0.3530 0.058 Uiso 1 1 calc R . . C28 C 0.7953(9) -0.0452(7) 0.2599(5) 0.057(3) Uani 1 1 d . . . H28 H 0.8816 -0.0492 0.2683 0.068 Uiso 1 1 calc R . . C29 C 0.7461(10) -0.0500(7) 0.1969(5) 0.055(3) Uani 1 1 d . . . C30 C 0.6201(9) -0.0467(7) 0.1849(4) 0.053(3) Uani 1 1 d . . . H30 H 0.5867 -0.0494 0.1420 0.063 Uiso 1 1 calc R . . C31 C 0.5402(9) -0.0394(6) 0.2355(4) 0.045(2) Uani 1 1 d . . . H31 H 0.4537 -0.0381 0.2269 0.054 Uiso 1 1 calc R . . C32 C 0.8171(11) -0.0284(8) 0.0883(6) 0.062(3) Uani 1 1 d . . . C33 C 0.8002(11) 0.0588(8) 0.0836(5) 0.070(3) Uani 1 1 d . . . H33 H 0.7885 0.0907 0.1214 0.084 Uiso 1 1 calc R . . C34 C 0.7998(11) 0.1009(7) 0.0247(6) 0.070(3) Uani 1 1 d . . . H34 H 0.7910 0.1611 0.0223 0.084 Uiso 1 1 calc R . . C35 C 0.8129(11) 0.0519(8) -0.0311(5) 0.063(3) Uani 1 1 d . . . C36 C 0.8331(13) -0.0384(8) -0.0248(6) 0.079(4) Uani 1 1 d . . . H36 H 0.8421 -0.0725 -0.0619 0.095 Uiso 1 1 calc R . . C37 C 0.8395(10) -0.0765(8) 0.0369(6) 0.067(3) Uani 1 1 d . . . H37 H 0.8593 -0.1352 0.0419 0.080 Uiso 1 1 calc R . . C38 C 0.8104(12) 0.0897(9) -0.0983(6) 0.072(3) 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 Co1 0.0270(6) 0.0513(8) 0.0232(6) -0.0021(6) -0.0054(5) -0.0014(6) Co2 0.0222(8) 0.0554(12) 0.0169(8) -0.0006(7) -0.0074(7) -0.0024(8) N1 0.029(4) 0.065(6) 0.040(5) -0.007(4) 0.003(4) -0.010(4) N2 0.040(4) 0.054(5) 0.027(4) -0.004(4) 0.000(3) 0.004(4) O1 0.035(3) 0.052(4) 0.021(3) -0.003(3) 0.001(3) -0.001(3) O2 0.037(4) 0.075(5) 0.043(4) -0.015(3) 0.005(3) -0.006(3) O3 0.031(3) 0.064(4) 0.017(3) -0.002(3) -0.011(3) -0.002(3) O4 0.025(3) 0.069(5) 0.021(3) 0.002(3) -0.002(3) -0.005(3) O5 0.095(6) 0.093(6) 0.063(5) 0.023(4) 0.043(5) 0.029(5) O6 0.139(8) 0.070(6) 0.058(6) 0.008(4) 0.032(5) 0.030(5) O7 0.230(13) 0.093(7) 0.043(5) -0.014(5) 0.014(6) 0.037(7) O8 0.027(3) 0.055(4) 0.028(3) 0.001(3) -0.001(3) -0.004(3) O9 0.047(4) 0.066(5) 0.056(5) 0.014(4) -0.003(3) -0.016(4) O10 0.033(3) 0.055(4) 0.040(4) -0.003(3) -0.004(3) -0.002(3) C1 0.059(7) 0.083(9) 0.048(7) -0.025(6) 0.014(6) -0.013(6) C2 0.041(6) 0.085(9) 0.055(7) -0.032(6) 0.009(5) -0.020(6) C3 0.032(5) 0.062(7) 0.034(6) -0.006(5) -0.001(4) -0.008(5) C4 0.054(6) 0.078(8) 0.051(7) -0.032(6) 0.019(5) -0.020(6) C5 0.038(6) 0.077(8) 0.067(8) -0.035(6) 0.011(5) -0.020(5) C6 0.074(7) 0.075(8) 0.018(5) 0.000(5) 0.001(5) 0.023(6) C7 0.064(7) 0.062(7) 0.038(6) 0.004(5) 0.002(5) 0.024(6) C8 0.043(6) 0.054(7) 0.034(6) 0.011(5) 0.000(5) 0.008(5) C9 0.058(7) 0.064(8) 0.037(6) 0.002(5) -0.006(5) 0.015(6) C10 0.058(7) 0.066(7) 0.033(6) 0.000(5) -0.009(5) 0.018(5) C11 0.036(5) 0.044(6) 0.036(5) 0.005(4) 0.005(4) 0.002(4) C12 0.048(6) 0.052(7) 0.038(6) 0.003(5) -0.003(5) 0.003(5) C13 0.064(7) 0.072(8) 0.039(6) 0.003(5) 0.002(5) -0.004(6) C14 0.062(8) 0.079(9) 0.049(7) 0.008(6) -0.011(6) -0.002(6) C15 0.044(6) 0.063(7) 0.045(7) 0.007(5) -0.006(5) 0.011(5) C16 0.059(7) 0.036(6) 0.039(6) -0.004(4) 0.018(5) -0.006(5) C17 0.047(6) 0.042(6) 0.045(6) 0.000(5) 0.007(5) 0.001(5) C18 0.056(7) 0.068(8) 0.059(8) -0.013(6) 0.007(6) -0.013(6) C19 0.060(8) 0.081(9) 0.071(9) -0.027(7) -0.001(7) -0.015(6) C20 0.086(9) 0.072(9) 0.044(7) -0.025(6) 0.005(6) 0.002(7) C21 0.048(6) 0.056(7) 0.057(7) -0.017(5) 0.004(5) 0.006(5) C22 0.050(6) 0.043(6) 0.040(6) -0.006(5) 0.007(5) 0.010(5) C23 0.042(6) 0.042(6) 0.027(5) -0.002(4) -0.003(4) 0.002(5) C24 0.049(6) 0.037(6) 0.040(6) 0.001(4) 0.006(5) -0.009(5) C25 0.036(5) 0.038(6) 0.025(5) -0.002(4) -0.002(4) 0.000(4) C26 0.043(5) 0.049(6) 0.023(5) 0.001(4) -0.001(4) -0.007(4) C27 0.032(5) 0.085(8) 0.027(5) 0.000(5) -0.005(4) -0.003(5) C28 0.032(5) 0.088(9) 0.052(7) 0.008(6) 0.003(5) -0.004(5) C29 0.064(7) 0.066(8) 0.038(6) 0.007(5) 0.024(6) 0.008(6) C30 0.055(7) 0.082(8) 0.021(5) -0.002(5) 0.003(5) 0.006(6) C31 0.045(6) 0.062(7) 0.026(5) -0.002(4) -0.014(4) 0.000(5) C32 0.067(8) 0.069(9) 0.052(7) 0.010(6) 0.021(6) 0.004(6) C33 0.096(9) 0.079(10) 0.036(7) 0.003(6) 0.005(6) 0.015(7) C34 0.095(9) 0.054(8) 0.064(8) -0.006(6) 0.024(7) 0.006(6) C35 0.078(8) 0.073(9) 0.041(7) -0.009(6) 0.021(6) -0.007(6) C36 0.137(12) 0.049(8) 0.054(8) -0.008(6) 0.026(8) -0.005(8) C37 0.077(8) 0.071(8) 0.053(8) 0.003(6) 0.019(6) 0.001(6) C38 0.100(10) 0.066(9) 0.052(8) -0.001(7) 0.016(7) 0.024(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.035(5) . ? Co1 O10 2.085(5) . ? Co1 N2 2.129(7) . ? Co1 N1 2.159(7) . ? Co1 O1 2.167(6) . ? Co1 O8 2.179(6) . ? Co2 O4 1.981(5) 3_656 ? Co2 O4 1.981(5) . ? Co2 O1 2.154(6) 3_656 ? Co2 O1 2.154(6) . ? Co2 O8 2.164(6) . ? Co2 O8 2.164(6) 3_656 ? N1 C5 1.326(11) . ? N1 C1 1.344(11) . ? N2 C6 1.326(11) . ? N2 C10 1.338(11) . ? O1 C23 1.280(9) . ? O2 C23 1.244(9) . ? O3 C25 1.268(9) . ? O4 C25 1.249(10) . ? O5 C29 1.383(10) . ? O5 C32 1.398(12) . ? O6 C38 1.340(12) . ? O6 H6A 0.8200 . ? O7 C38 1.226(13) . ? O8 C24 1.279(10) . ? O9 C24 1.254(10) . ? O10 H10B 0.8501 . ? O10 H10A 0.8201 . ? C1 C2 1.365(13) . ? C1 H1 0.9300 . ? C2 C3 1.355(12) . ? C2 H2 0.9300 . ? C3 C4 1.373(11) . ? C3 C8 1.473(12) 2_545 ? C4 C5 1.367(13) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.388(13) . ? C6 H6 0.9300 . ? C7 C8 1.375(12) . ? C7 H7 0.9300 . ? C8 C9 1.372(12) . ? C8 C3 1.473(12) 2 ? C9 C10 1.374(13) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.365(12) . ? C11 C12 1.387(12) . ? C11 C24 1.510(12) 3_656 ? C12 C13 1.375(13) . ? C12 H12 0.9300 . ? C13 C14 1.370(13) . ? C13 H13 0.9300 . ? C14 C15 1.373(13) . ? C14 H14 0.9300 . ? C15 C16 1.375(13) . ? C15 H15 0.9300 . ? C16 C17 1.503(12) . ? C17 C22 1.388(12) . ? C17 C18 1.396(13) . ? C18 C19 1.330(14) . ? C18 H18 0.9300 . ? C19 C20 1.393(14) . ? C19 H19 0.9300 . ? C20 C21 1.365(13) . ? C20 H20 0.9300 . ? C21 C22 1.394(12) . ? C21 H21 0.9300 . ? C22 C23 1.487(12) . ? C24 C11 1.510(12) 3_656 ? C25 C26 1.509(11) . ? C26 C27 1.385(12) . ? C26 C31 1.387(12) . ? C27 C28 1.355(12) . ? C27 H27 0.9300 . ? C28 C29 1.366(14) . ? C28 H28 0.9300 . ? C29 C30 1.355(13) . ? C30 C31 1.384(12) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C37 1.317(14) . ? C32 C33 1.354(14) . ? C33 C34 1.367(14) . ? C33 H33 0.9300 . ? C34 C35 1.381(14) . ? C34 H34 0.9300 . ? C35 C36 1.409(14) . ? C35 C38 1.489(15) . ? C36 C37 1.389(15) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O10 177.1(2) . . ? O3 Co1 N2 89.3(2) . . ? O10 Co1 N2 90.4(3) . . ? O3 Co1 N1 88.7(3) . . ? O10 Co1 N1 88.4(3) . . ? N2 Co1 N1 91.1(3) . . ? O3 Co1 O1 93.4(2) . . ? O10 Co1 O1 89.5(2) . . ? N2 Co1 O1 92.2(3) . . ? N1 Co1 O1 176.2(3) . . ? O3 Co1 O8 92.8(2) . . ? O10 Co1 O8 87.9(2) . . ? N2 Co1 O8 171.6(2) . . ? N1 Co1 O8 97.1(3) . . ? O1 Co1 O8 79.6(2) . . ? O4 Co2 O4 180.000(1) 3_656 . ? O4 Co2 O1 95.4(2) 3_656 3_656 ? O4 Co2 O1 84.6(2) . 3_656 ? O4 Co2 O1 84.6(2) 3_656 . ? O4 Co2 O1 95.4(2) . . ? O1 Co2 O1 180.000(1) 3_656 . ? O4 Co2 O8 88.1(2) 3_656 . ? O4 Co2 O8 91.9(2) . . ? O1 Co2 O8 99.8(2) 3_656 . ? O1 Co2 O8 80.2(2) . . ? O4 Co2 O8 91.9(2) 3_656 3_656 ? O4 Co2 O8 88.1(2) . 3_656 ? O1 Co2 O8 80.2(2) 3_656 3_656 ? O1 Co2 O8 99.8(2) . 3_656 ? O8 Co2 O8 180.00(19) . 3_656 ? C5 N1 C1 115.5(8) . . ? C5 N1 Co1 121.8(6) . . ? C1 N1 Co1 121.6(6) . . ? C6 N2 C10 116.1(8) . . ? C6 N2 Co1 122.9(6) . . ? C10 N2 Co1 121.0(6) . . ? C23 O1 Co2 120.1(5) . . ? C23 O1 Co1 127.7(5) . . ? Co2 O1 Co1 94.0(2) . . ? C25 O3 Co1 130.0(5) . . ? C25 O4 Co2 132.4(5) . . ? C29 O5 C32 120.3(8) . . ? C38 O6 H6A 109.5 . . ? C24 O8 Co2 126.3(6) . . ? C24 O8 Co1 127.5(6) . . ? Co2 O8 Co1 93.4(2) . . ? Co1 O10 H10B 106.6 . . ? Co1 O10 H10A 109.8 . . ? H10B O10 H10A 107.3 . . ? N1 C1 C2 123.3(9) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 121.4(9) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 115.2(9) . . ? C2 C3 C8 122.0(8) . 2_545 ? C4 C3 C8 122.8(8) . 2_545 ? C5 C4 C3 121.5(9) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? N1 C5 C4 123.1(9) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N2 C6 C7 123.3(8) . . ? N2 C6 H6 118.4 . . ? C7 C6 H6 118.4 . . ? C8 C7 C6 119.5(9) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 C7 117.9(9) . . ? C9 C8 C3 120.9(8) . 2 ? C7 C8 C3 121.2(8) . 2 ? C8 C9 C10 118.7(9) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 124.5(9) . . ? N2 C10 H10 117.7 . . ? C9 C10 H10 117.7 . . ? C16 C11 C12 119.1(9) . . ? C16 C11 C24 122.5(8) . 3_656 ? C12 C11 C24 118.4(8) . 3_656 ? C13 C12 C11 121.3(9) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 118.5(10) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 120.8(10) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 120.3(9) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 120.0(8) . . ? C11 C16 C17 119.7(9) . . ? C15 C16 C17 120.1(9) . . ? C22 C17 C18 118.4(9) . . ? C22 C17 C16 122.6(9) . . ? C18 C17 C16 119.0(8) . . ? C19 C18 C17 123.0(10) . . ? C19 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C18 C19 C20 119.3(11) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 C19 119.3(10) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 121.8(10) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C17 C22 C21 118.3(9) . . ? C17 C22 C23 123.3(8) . . ? C21 C22 C23 118.5(9) . . ? O2 C23 O1 124.3(8) . . ? O2 C23 C22 116.8(8) . . ? O1 C23 C22 118.9(8) . . ? O9 C24 O8 122.5(9) . . ? O9 C24 C11 118.8(8) . 3_656 ? O8 C24 C11 118.7(8) . 3_656 ? O4 C25 O3 124.4(7) . . ? O4 C25 C26 116.5(7) . . ? O3 C25 C26 119.1(7) . . ? C27 C26 C31 119.3(8) . . ? C27 C26 C25 119.5(8) . . ? C31 C26 C25 121.2(8) . . ? C28 C27 C26 120.0(9) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 121.1(9) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 119.4(9) . . ? C30 C29 O5 122.5(10) . . ? C28 C29 O5 117.4(10) . . ? C29 C30 C31 121.3(9) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C30 C31 C26 118.8(9) . . ? C30 C31 H31 120.6 . . ? C26 C31 H31 120.6 . . ? C37 C32 C33 121.9(11) . . ? C37 C32 O5 116.1(11) . . ? C33 C32 O5 121.6(10) . . ? C32 C33 C34 121.6(10) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C33 C34 C35 118.4(11) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C34 C35 C36 118.9(10) . . ? C34 C35 C38 123.6(11) . . ? C36 C35 C38 117.5(10) . . ? C37 C36 C35 119.7(10) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C32 C37 C36 119.2(12) . . ? C32 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? O7 C38 O6 117.7(11) . . ? O7 C38 C35 121.1(12) . . ? O6 C38 C35 121.2(10) . . ? 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 O3 Co1 N1 C5 2.1(8) . . . . ? O10 Co1 N1 C5 -178.2(8) . . . . ? N2 Co1 N1 C5 91.4(8) . . . . ? O1 Co1 N1 C5 -121(4) . . . . ? O8 Co1 N1 C5 -90.5(8) . . . . ? O3 Co1 N1 C1 -165.7(8) . . . . ? O10 Co1 N1 C1 13.9(8) . . . . ? N2 Co1 N1 C1 -76.4(8) . . . . ? O1 Co1 N1 C1 71(4) . . . . ? O8 Co1 N1 C1 101.7(8) . . . . ? O3 Co1 N2 C6 -147.7(8) . . . . ? O10 Co1 N2 C6 35.2(8) . . . . ? N1 Co1 N2 C6 123.6(8) . . . . ? O1 Co1 N2 C6 -54.4(8) . . . . ? O8 Co1 N2 C6 -43(2) . . . . ? O3 Co1 N2 C10 30.5(7) . . . . ? O10 Co1 N2 C10 -146.6(7) . . . . ? N1 Co1 N2 C10 -58.2(7) . . . . ? O1 Co1 N2 C10 123.8(7) . . . . ? O8 Co1 N2 C10 134.8(15) . . . . ? O4 Co2 O1 C23 22.7(6) 3_656 . . . ? O4 Co2 O1 C23 -157.3(6) . . . . ? O1 Co2 O1 C23 -146(100) 3_656 . . . ? O8 Co2 O1 C23 111.7(6) . . . . ? O8 Co2 O1 C23 -68.3(6) 3_656 . . . ? O4 Co2 O1 Co1 -115.9(2) 3_656 . . . ? O4 Co2 O1 Co1 64.1(2) . . . . ? O1 Co2 O1 Co1 75(100) 3_656 . . . ? O8 Co2 O1 Co1 -26.8(2) . . . . ? O8 Co2 O1 Co1 153.2(2) 3_656 . . . ? O3 Co1 O1 C23 160.9(7) . . . . ? O10 Co1 O1 C23 -18.9(7) . . . . ? N2 Co1 O1 C23 71.5(7) . . . . ? N1 Co1 O1 C23 -76(4) . . . . ? O8 Co1 O1 C23 -106.9(7) . . . . ? O3 Co1 O1 Co2 -65.6(2) . . . . ? O10 Co1 O1 Co2 114.7(2) . . . . ? N2 Co1 O1 Co2 -155.0(2) . . . . ? N1 Co1 O1 Co2 57(4) . . . . ? O8 Co1 O1 Co2 26.66(19) . . . . ? O10 Co1 O3 C25 -140(5) . . . . ? N2 Co1 O3 C25 135.8(7) . . . . ? N1 Co1 O3 C25 -133.1(7) . . . . ? O1 Co1 O3 C25 43.7(7) . . . . ? O8 Co1 O3 C25 -36.1(7) . . . . ? O4 Co2 O4 C25 -54(100) 3_656 . . . ? O1 Co2 O4 C25 143.0(8) 3_656 . . . ? O1 Co2 O4 C25 -37.0(8) . . . . ? O8 Co2 O4 C25 43.4(8) . . . . ? O8 Co2 O4 C25 -136.6(8) 3_656 . . . ? O4 Co2 O8 C24 -31.7(7) 3_656 . . . ? O4 Co2 O8 C24 148.3(7) . . . . ? O1 Co2 O8 C24 63.5(7) 3_656 . . . ? O1 Co2 O8 C24 -116.5(7) . . . . ? O8 Co2 O8 C24 167(100) 3_656 . . . ? O4 Co2 O8 Co1 111.5(2) 3_656 . . . ? O4 Co2 O8 Co1 -68.5(2) . . . . ? O1 Co2 O8 Co1 -153.37(19) 3_656 . . . ? O1 Co2 O8 Co1 26.63(19) . . . . ? O8 Co2 O8 Co1 -50(100) 3_656 . . . ? O3 Co1 O8 C24 -151.1(7) . . . . ? O10 Co1 O8 C24 26.1(7) . . . . ? N2 Co1 O8 C24 104.8(17) . . . . ? N1 Co1 O8 C24 -62.1(7) . . . . ? O1 Co1 O8 C24 116.0(7) . . . . ? O3 Co1 O8 Co2 66.4(2) . . . . ? O10 Co1 O8 Co2 -116.4(2) . . . . ? N2 Co1 O8 Co2 -37.7(17) . . . . ? N1 Co1 O8 Co2 155.5(2) . . . . ? O1 Co1 O8 Co2 -26.51(19) . . . . ? C5 N1 C1 C2 0.8(16) . . . . ? Co1 N1 C1 C2 169.4(9) . . . . ? N1 C1 C2 C3 -3.5(18) . . . . ? C1 C2 C3 C4 3.8(17) . . . . ? C1 C2 C3 C8 -175.3(10) . . . 2_545 ? C2 C3 C4 C5 -1.9(16) . . . . ? C8 C3 C4 C5 177.2(11) 2_545 . . . ? C1 N1 C5 C4 1.2(16) . . . . ? Co1 N1 C5 C4 -167.4(9) . . . . ? C3 C4 C5 N1 -0.6(18) . . . . ? C10 N2 C6 C7 -1.7(15) . . . . ? Co1 N2 C6 C7 176.6(8) . . . . ? N2 C6 C7 C8 -0.6(16) . . . . ? C6 C7 C8 C9 1.8(15) . . . . ? C6 C7 C8 C3 -177.7(9) . . . 2 ? C7 C8 C9 C10 -0.6(15) . . . . ? C3 C8 C9 C10 178.8(9) 2 . . . ? C6 N2 C10 C9 2.9(15) . . . . ? Co1 N2 C10 C9 -175.4(8) . . . . ? C8 C9 C10 N2 -1.8(16) . . . . ? C16 C11 C12 C13 -1.0(14) . . . . ? C24 C11 C12 C13 176.6(9) 3_656 . . . ? C11 C12 C13 C14 0.0(15) . . . . ? C12 C13 C14 C15 1.3(16) . . . . ? C13 C14 C15 C16 -1.6(16) . . . . ? C12 C11 C16 C15 0.7(13) . . . . ? C24 C11 C16 C15 -176.8(9) 3_656 . . . ? C12 C11 C16 C17 -173.3(8) . . . . ? C24 C11 C16 C17 9.1(13) 3_656 . . . ? C14 C15 C16 C11 0.6(15) . . . . ? C14 C15 C16 C17 174.6(9) . . . . ? C11 C16 C17 C22 -109.4(11) . . . . ? C15 C16 C17 C22 76.6(12) . . . . ? C11 C16 C17 C18 73.3(12) . . . . ? C15 C16 C17 C18 -100.7(11) . . . . ? C22 C17 C18 C19 -1.3(16) . . . . ? C16 C17 C18 C19 176.2(10) . . . . ? C17 C18 C19 C20 1.9(18) . . . . ? C18 C19 C20 C21 -0.9(18) . . . . ? C19 C20 C21 C22 -0.7(17) . . . . ? C18 C17 C22 C21 -0.3(14) . . . . ? C16 C17 C22 C21 -177.7(9) . . . . ? C18 C17 C22 C23 -179.9(9) . . . . ? C16 C17 C22 C23 2.7(14) . . . . ? C20 C21 C22 C17 1.3(15) . . . . ? C20 C21 C22 C23 -179.1(9) . . . . ? Co2 O1 C23 O2 -113.5(8) . . . . ? Co1 O1 C23 O2 9.8(12) . . . . ? Co2 O1 C23 C22 66.9(9) . . . . ? Co1 O1 C23 C22 -169.8(6) . . . . ? C17 C22 C23 O2 -149.6(9) . . . . ? C21 C22 C23 O2 30.8(13) . . . . ? C17 C22 C23 O1 30.1(13) . . . . ? C21 C22 C23 O1 -149.5(8) . . . . ? Co2 O8 C24 O9 143.0(7) . . . . ? Co1 O8 C24 O9 12.0(13) . . . . ? Co2 O8 C24 C11 -36.7(11) . . . 3_656 ? Co1 O8 C24 C11 -167.8(5) . . . 3_656 ? Co2 O4 C25 O3 -0.1(13) . . . . ? Co2 O4 C25 C26 -179.4(5) . . . . ? Co1 O3 C25 O4 -4.2(13) . . . . ? Co1 O3 C25 C26 175.1(5) . . . . ? O4 C25 C26 C27 7.1(12) . . . . ? O3 C25 C26 C27 -172.2(8) . . . . ? O4 C25 C26 C31 -172.6(8) . . . . ? O3 C25 C26 C31 8.1(12) . . . . ? C31 C26 C27 C28 -3.3(14) . . . . ? C25 C26 C27 C28 177.0(8) . . . . ? C26 C27 C28 C29 3.8(16) . . . . ? C27 C28 C29 C30 -1.8(16) . . . . ? C27 C28 C29 O5 -172.6(9) . . . . ? C32 O5 C29 C30 49.6(15) . . . . ? C32 O5 C29 C28 -139.9(11) . . . . ? C28 C29 C30 C31 -0.6(16) . . . . ? O5 C29 C30 C31 169.7(9) . . . . ? C29 C30 C31 C26 1.0(15) . . . . ? C27 C26 C31 C30 0.9(14) . . . . ? C25 C26 C31 C30 -179.3(8) . . . . ? C29 O5 C32 C37 -143.5(11) . . . . ? C29 O5 C32 C33 44.1(15) . . . . ? C37 C32 C33 C34 3.0(19) . . . . ? O5 C32 C33 C34 175.0(11) . . . . ? C32 C33 C34 C35 2.2(18) . . . . ? C33 C34 C35 C36 -3.5(17) . . . . ? C33 C34 C35 C38 178.2(11) . . . . ? C34 C35 C36 C37 0.0(17) . . . . ? C38 C35 C36 C37 178.4(12) . . . . ? C33 C32 C37 C36 -6.6(19) . . . . ? O5 C32 C37 C36 -179.0(10) . . . . ? C35 C36 C37 C32 5.1(19) . . . . ? C34 C35 C38 O7 -172.2(13) . . . . ? C36 C35 C38 O7 9.5(19) . . . . ? C34 C35 C38 O6 7.6(19) . . . . ? C36 C35 C38 O6 -170.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.757 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.146 data_5 _database_code_depnum_ccdc_archive 'CCDC 884075' #TrackingRef 'web_deposit_cif_file_0_feilonghu_1350638779.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H33 Co3 N0 O19' _chemical_formula_weight 1186.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.001(10) _cell_length_b 10.758(8) _cell_length_c 16.911(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.111(8) _cell_angle_gamma 90.00 _cell_volume 2459(3) _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 clavate _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7966 _exptl_absorpt_correction_T_max 0.8126 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13463 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4329 _reflns_number_gt 3236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0394P)^2^+1.1194P] 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 4329 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Co1 Co 0.09027(3) 0.55767(4) 0.69550(2) 0.02144(13) Uani 1 1 d . . . Co2 Co 0.0000 0.5000 0.5000 0.02021(16) Uani 1 2 d S . . O1 O 0.13597(15) 0.4249(2) 0.53011(13) 0.0252(5) Uani 1 1 d . C . O2 O 0.20753(15) 0.4788(2) 0.65943(13) 0.0320(6) Uani 1 1 d . C . O3 O 0.5505(2) 0.1591(3) 0.57636(18) 0.0638(9) Uani 1 1 d . . . O4 O 0.33916(18) 0.6351(3) 0.75101(17) 0.0583(8) Uani 1 1 d . . . O5 O 0.19037(17) 0.7072(2) 0.75014(15) 0.0420(7) Uani 1 1 d . . . O6 O 0.0000 0.6644(3) 0.7500 0.0241(7) Uani 1 2 d S . . H6A H -0.0364 0.7110 0.7138 0.029 Uiso 0.50 1 d PR . . O7 O 0.04979(18) 0.2025(2) 0.38004(14) 0.0393(6) Uani 1 1 d . . . O8 O -0.02045(14) 0.4429(2) 0.62455(12) 0.0233(5) Uani 1 1 d . . . O9 O 0.12930(16) 0.4506(2) 0.79877(13) 0.0345(6) Uani 1 1 d . . . O10 O 0.04524(15) 0.6538(2) 0.58254(12) 0.0238(5) Uani 1 1 d . . . C1 C 0.2068(2) 0.4235(3) 0.5930(2) 0.0254(8) Uani 1 1 d . . . C3 C 0.3897(3) 0.2300(4) 0.5171(3) 0.0548(13) Uani 1 1 d . . . H3 H 0.3945 0.1919 0.4689 0.066 Uiso 1 1 calc R A 1 C7 C 0.5867(3) 0.0536(4) 0.6189(2) 0.0459(11) Uani 1 1 d . C . C8 C 0.5299(3) -0.0323(4) 0.6442(3) 0.0567(13) Uani 1 1 d . . . H8 H 0.4626 -0.0182 0.6365 0.068 Uiso 1 1 calc R C . C9 C 0.5725(3) -0.1406(5) 0.6813(2) 0.0545(12) Uani 1 1 d . . . H9 H 0.5331 -0.1992 0.6982 0.065 Uiso 1 1 calc R . . C10 C 0.3267(2) 0.8365(4) 0.8060(2) 0.0359(9) Uani 1 1 d . . . C11 C 0.2795(3) 0.7215(4) 0.7670(2) 0.0352(9) Uani 1 1 d . . . C12 C 0.7302(3) -0.0745(4) 0.6680(2) 0.0463(11) Uani 1 1 d . . . H12 H 0.7977 -0.0877 0.6760 0.056 Uiso 1 1 calc R . . C13 C 0.6875(3) 0.0337(4) 0.6302(3) 0.0497(11) Uani 1 1 d . . . H13 H 0.7260 0.0926 0.6126 0.060 Uiso 1 1 calc R C . C14 C -0.1040(2) 0.4191(3) 0.63886(19) 0.0238(7) Uani 1 1 d . . . C15 C -0.1780(2) 0.3504(3) 0.57343(18) 0.0254(8) Uani 1 1 d . . . C16 C -0.2752(2) 0.3920(3) 0.5536(2) 0.0344(9) Uani 1 1 d . . . H16 H -0.2943 0.4521 0.5860 0.041 Uiso 1 1 calc R . . C17 C -0.3437(3) 0.3448(4) 0.4860(2) 0.0451(10) Uani 1 1 d . . . H17 H -0.4086 0.3735 0.4723 0.054 Uiso 1 1 calc R . . C18 C -0.3145(3) 0.2549(4) 0.4393(2) 0.0477(11) Uani 1 1 d . . . H18 H -0.3596 0.2253 0.3926 0.057 Uiso 1 1 calc R . . C19 C -0.2194(3) 0.2081(4) 0.4609(2) 0.0375(9) Uani 1 1 d . . . H19 H -0.2022 0.1446 0.4300 0.045 Uiso 1 1 calc R . . C20 C -0.1490(2) 0.2551(3) 0.52837(19) 0.0258(8) Uani 1 1 d . . . C21 C -0.0503(2) 0.1938(3) 0.55710(19) 0.0266(8) Uani 1 1 d . . . C22 C -0.0286(3) 0.1393(3) 0.6338(2) 0.0404(9) Uani 1 1 d . . . H22 H -0.0741 0.1454 0.6650 0.049 Uiso 1 1 calc R . . C23 C 0.0586(3) 0.0763(4) 0.6649(2) 0.0509(12) Uani 1 1 d . . . H23 H 0.0712 0.0402 0.7166 0.061 Uiso 1 1 calc R . . C24 C 0.1270(3) 0.0666(4) 0.6198(2) 0.0454(10) Uani 1 1 d . . . H24 H 0.1871 0.0268 0.6418 0.054 Uiso 1 1 calc R . . C25 C 0.3064(3) 0.2971(4) 0.5203(2) 0.0500(11) Uani 1 1 d . C . H25 H 0.2541 0.2958 0.4733 0.060 Uiso 1 1 calc R B 1 C26 C 0.1063(3) 0.1162(3) 0.5418(2) 0.0344(8) Uani 1 1 d . . . H26 H 0.1510 0.1059 0.5102 0.041 Uiso 1 1 calc R . . C27 C 0.0186(2) 0.1817(3) 0.51038(19) 0.0247(7) Uani 1 1 d . . . C28 C 0.0071(2) 0.2452(3) 0.42971(19) 0.0255(8) Uani 1 1 d . . . C2 C 0.293(8) 0.361(9) 0.581(5) 0.038(7) Uani 0.469(15) 1 d P C 1 C5 C 0.4712(7) 0.3058(14) 0.6455(6) 0.056(4) Uani 0.531(15) 1 d P C 1 H5 H 0.5317 0.3219 0.6827 0.067 Uiso 0.531(15) 1 calc PR C 1 C6 C 0.3880(7) 0.3708(14) 0.6511(5) 0.050(3) Uani 0.531(15) 1 d P C 1 H6 H 0.3893 0.4196 0.6968 0.060 Uiso 0.531(15) 1 calc PR C 1 C4 C 0.466(6) 0.222(10) 0.588(7) 0.048(15) Uani 0.531(15) 1 d P C 1 C2' C 0.300(7) 0.341(8) 0.597(4) 0.038(7) Uani 0.531(15) 1 d P C 2 C6' C 0.3522(9) 0.2888(14) 0.6599(6) 0.048(4) Uani 0.469(15) 1 d P C 2 H6' H 0.3355 0.2975 0.7093 0.058 Uiso 0.469(15) 1 calc PR C 2 C5' C 0.4345(8) 0.2189(15) 0.6573(6) 0.054(4) Uani 0.469(15) 1 d P C 2 H5' H 0.4733 0.1810 0.7042 0.065 Uiso 0.469(15) 1 calc PR C 2 C4' C 0.459(7) 0.207(11) 0.576(8) 0.047(14) Uani 0.469(15) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0192(2) 0.0267(3) 0.0186(2) -0.0015(2) 0.00537(17) 0.00030(19) Co2 0.0173(3) 0.0221(4) 0.0199(3) -0.0020(3) 0.0026(2) 0.0029(3) O1 0.0199(11) 0.0290(14) 0.0250(12) -0.0013(10) 0.0026(10) 0.0039(10) O2 0.0235(12) 0.0484(17) 0.0237(12) -0.0073(11) 0.0052(10) 0.0093(11) O3 0.0443(17) 0.079(2) 0.076(2) 0.0251(19) 0.0288(15) 0.0429(16) O4 0.0297(15) 0.073(2) 0.069(2) -0.0261(17) 0.0089(14) 0.0029(15) O5 0.0265(14) 0.0483(17) 0.0520(16) -0.0128(14) 0.0114(12) -0.0093(12) O6 0.0211(16) 0.0255(18) 0.0260(16) 0.000 0.0069(13) 0.000 O7 0.0557(16) 0.0332(15) 0.0367(14) 0.0078(12) 0.0259(13) 0.0164(13) O8 0.0212(11) 0.0247(12) 0.0235(11) -0.0009(10) 0.0052(9) -0.0041(10) O9 0.0352(14) 0.0441(16) 0.0273(13) 0.0104(12) 0.0134(11) 0.0106(12) O10 0.0253(12) 0.0232(13) 0.0224(11) 0.0006(10) 0.0053(9) 0.0022(10) C1 0.0225(17) 0.028(2) 0.0272(18) 0.0026(16) 0.0090(15) 0.0055(15) C3 0.041(2) 0.071(3) 0.051(3) -0.020(2) 0.009(2) 0.027(2) C7 0.034(2) 0.063(3) 0.042(2) 0.004(2) 0.0120(18) 0.025(2) C8 0.028(2) 0.088(4) 0.058(3) 0.025(3) 0.018(2) 0.032(2) C9 0.032(2) 0.086(4) 0.052(3) 0.020(3) 0.0212(19) 0.014(2) C10 0.0243(19) 0.055(3) 0.0291(19) -0.0011(18) 0.0073(15) -0.0112(17) C11 0.029(2) 0.048(3) 0.0272(19) -0.0002(18) 0.0063(16) -0.0064(18) C12 0.0204(19) 0.050(3) 0.063(3) -0.001(2) 0.0010(18) 0.0093(18) C13 0.029(2) 0.046(3) 0.072(3) 0.002(2) 0.009(2) 0.0068(19) C14 0.0258(18) 0.0222(19) 0.0234(17) 0.0018(15) 0.0067(14) 0.0000(14) C15 0.0268(18) 0.030(2) 0.0201(16) 0.0024(15) 0.0075(14) -0.0069(15) C16 0.0291(19) 0.035(2) 0.041(2) -0.0039(18) 0.0126(17) -0.0058(17) C17 0.027(2) 0.057(3) 0.047(2) 0.002(2) 0.0024(18) -0.0110(19) C18 0.042(2) 0.055(3) 0.038(2) -0.005(2) -0.0042(19) -0.017(2) C19 0.046(2) 0.034(2) 0.031(2) -0.0100(17) 0.0078(17) -0.0114(18) C20 0.0319(19) 0.024(2) 0.0234(17) 0.0019(15) 0.0105(15) -0.0079(15) C21 0.037(2) 0.0174(18) 0.0241(17) -0.0017(15) 0.0057(15) -0.0040(15) C22 0.062(3) 0.034(2) 0.0287(19) 0.0057(18) 0.0168(18) 0.011(2) C23 0.085(3) 0.041(3) 0.0237(19) 0.0004(18) 0.008(2) 0.025(2) C24 0.062(3) 0.034(2) 0.033(2) -0.0006(19) -0.0005(19) 0.023(2) C25 0.034(2) 0.068(3) 0.042(2) -0.016(2) -0.0024(18) 0.023(2) C26 0.040(2) 0.027(2) 0.034(2) -0.0037(17) 0.0064(17) 0.0063(17) C27 0.0328(19) 0.0148(18) 0.0241(17) -0.0024(14) 0.0031(15) 0.0004(14) C28 0.0282(18) 0.0203(19) 0.0273(18) -0.0007(15) 0.0060(15) -0.0038(15) C2 0.030(10) 0.05(2) 0.03(2) 0.001(12) 0.006(17) 0.015(13) C5 0.028(5) 0.082(10) 0.049(5) -0.001(6) -0.006(4) 0.022(6) C6 0.036(5) 0.068(9) 0.040(5) -0.013(5) 0.001(4) 0.021(5) C4 0.030(12) 0.07(2) 0.05(3) 0.00(2) 0.011(16) 0.034(17) C2' 0.030(10) 0.05(2) 0.03(2) 0.001(12) 0.006(17) 0.015(13) C6' 0.042(6) 0.066(10) 0.037(5) -0.002(6) 0.009(5) 0.026(6) C5' 0.041(6) 0.074(10) 0.043(6) 0.010(6) 0.004(5) 0.032(7) C4' 0.040(17) 0.06(2) 0.036(19) 0.00(2) 0.011(14) 0.023(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 Co1 O9 2.044(2) . ? Co1 O2 2.076(2) . ? Co1 O6 2.0913(19) . ? Co1 O8 2.097(2) . ? Co1 O10 2.118(2) . ? Co1 O5 2.175(3) . ? Co2 O1 2.008(2) . ? Co2 O1 2.008(2) 3_566 ? Co2 O10 2.151(2) . ? Co2 O10 2.151(2) 3_566 ? Co2 O8 2.283(2) 3_566 ? Co2 O8 2.283(2) . ? O1 C1 1.251(4) . ? O2 C1 1.269(4) . ? O3 C7 1.368(5) . ? O3 C4' 1.38(8) . ? O3 C4 1.42(6) . ? O4 C11 1.324(4) . ? O5 C11 1.215(4) . ? O6 Co1 2.0913(19) 2_556 ? O6 H6A 0.8500 . ? O7 C28 1.239(4) . ? O8 C14 1.280(4) . ? O9 C14 1.244(4) 2_556 ? O10 C28 1.296(4) 3_566 ? C1 C2 1.44(11) . ? C1 C2' 1.56(9) . ? C3 C4' 1.22(11) . ? C3 C25 1.384(5) . ? C3 C4 1.39(10) . ? C3 H3 0.9300 . ? C7 C8 1.359(6) . ? C7 C13 1.390(5) . ? C8 C9 1.383(6) . ? C8 H8 0.9300 . ? C9 C10 1.393(5) 2_646 ? C9 H9 0.9300 . ? C10 C12 1.389(5) 2_666 ? C10 C9 1.393(5) 2_666 ? C10 C11 1.475(5) . ? C12 C13 1.386(5) . ? C12 C10 1.389(5) 2_646 ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O9 1.244(4) 2_556 ? C14 C15 1.500(4) . ? C15 C16 1.388(4) . ? C15 C20 1.399(5) . ? C16 C17 1.383(5) . ? C16 H16 0.9300 . ? C17 C18 1.376(5) . ? C17 H17 0.9300 . ? C18 C19 1.380(5) . ? C18 H18 0.9300 . ? C19 C20 1.394(4) . ? C19 H19 0.9300 . ? C20 C21 1.493(5) . ? C21 C22 1.383(4) . ? C21 C27 1.403(4) . ? C22 C23 1.375(5) . ? C22 H22 0.9300 . ? C23 C24 1.376(6) . ? C23 H23 0.9300 . ? C24 C26 1.382(5) . ? C24 H24 0.9300 . ? C25 C2 1.29(10) . ? C25 C2' 1.40(8) . ? C25 H25 0.9300 . ? C26 C27 1.395(4) . ? C26 H26 0.9300 . ? C27 C28 1.496(4) . ? C28 O10 1.296(4) 3_566 ? C2 C6 1.54(10) . ? C5 C4 1.31(12) . ? C5 C6 1.383(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C2' C6' 1.26(6) . ? C6' C5' 1.386(12) . ? C6' H6' 0.9300 . ? C5' C4' 1.50(11) . ? C5' H5' 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Co1 O2 88.00(9) . . ? O9 Co1 O6 89.46(9) . . ? O2 Co1 O6 165.71(8) . . ? O9 Co1 O8 98.63(10) . . ? O2 Co1 O8 96.58(10) . . ? O6 Co1 O8 97.70(9) . . ? O9 Co1 O10 174.85(9) . . ? O2 Co1 O10 90.39(9) . . ? O6 Co1 O10 93.28(8) . . ? O8 Co1 O10 76.69(9) . . ? O9 Co1 O5 93.13(11) . . ? O2 Co1 O5 87.46(10) . . ? O6 Co1 O5 78.64(10) . . ? O8 Co1 O5 167.67(9) . . ? O10 Co1 O5 91.68(10) . . ? O1 Co2 O1 180.0 . 3_566 ? O1 Co2 O10 92.61(9) . . ? O1 Co2 O10 87.39(9) 3_566 . ? O1 Co2 O10 87.39(9) . 3_566 ? O1 Co2 O10 92.61(9) 3_566 3_566 ? O10 Co2 O10 180.0 . 3_566 ? O1 Co2 O8 90.21(8) . 3_566 ? O1 Co2 O8 89.79(8) 3_566 3_566 ? O10 Co2 O8 107.77(9) . 3_566 ? O10 Co2 O8 72.23(9) 3_566 3_566 ? O1 Co2 O8 89.79(8) . . ? O1 Co2 O8 90.21(8) 3_566 . ? O10 Co2 O8 72.23(9) . . ? O10 Co2 O8 107.77(9) 3_566 . ? O8 Co2 O8 180.0 3_566 . ? C1 O1 Co2 135.2(2) . . ? C1 O2 Co1 128.9(2) . . ? C7 O3 C4' 122(4) . . ? C7 O3 C4 122(4) . . ? C4' O3 C4 10(10) . . ? C11 O5 Co1 134.6(3) . . ? Co1 O6 Co1 113.37(15) . 2_556 ? Co1 O6 H6A 108.9 . . ? Co1 O6 H6A 108.9 2_556 . ? C14 O8 Co1 125.8(2) . . ? C14 O8 Co2 124.66(19) . . ? Co1 O8 Co2 96.75(9) . . ? C14 O9 Co1 143.7(2) 2_556 . ? C28 O10 Co1 125.18(19) 3_566 . ? C28 O10 Co2 118.84(19) 3_566 . ? Co1 O10 Co2 100.24(10) . . ? O1 C1 O2 124.6(3) . . ? O1 C1 C2 113(4) . . ? O2 C1 C2 122(4) . . ? O1 C1 C2' 120(3) . . ? O2 C1 C2' 115(3) . . ? C2 C1 C2' 12(4) . . ? C4' C3 C25 125(5) . . ? C4' C3 C4 9(10) . . ? C25 C3 C4 118(3) . . ? C4' C3 H3 113.8 . . ? C25 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? C8 C7 O3 124.2(3) . . ? C8 C7 C13 120.5(4) . . ? O3 C7 C13 115.1(4) . . ? C7 C8 C9 119.8(4) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 121.2(4) . 2_646 ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 2_646 . ? C12 C10 C9 118.1(4) 2_666 2_666 ? C12 C10 C11 119.5(3) 2_666 . ? C9 C10 C11 122.4(4) 2_666 . ? O5 C11 O4 121.8(3) . . ? O5 C11 C10 121.6(3) . . ? O4 C11 C10 116.6(3) . . ? C13 C12 C10 120.7(3) . 2_646 ? C13 C12 H12 119.6 . . ? C10 C12 H12 119.6 2_646 . ? C12 C13 C7 119.6(4) . . ? C12 C13 H13 120.2 . . ? C7 C13 H13 120.2 . . ? O9 C14 O8 125.6(3) 2_556 . ? O9 C14 C15 117.7(3) 2_556 . ? O8 C14 C15 116.7(3) . . ? C16 C15 C20 120.7(3) . . ? C16 C15 C14 117.7(3) . . ? C20 C15 C14 121.3(3) . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 119.1(4) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C20 120.8(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C15 117.8(3) . . ? C19 C20 C21 120.2(3) . . ? C15 C20 C21 121.5(3) . . ? C22 C21 C27 118.3(3) . . ? C22 C21 C20 116.8(3) . . ? C27 C21 C20 124.8(3) . . ? C23 C22 C21 121.6(3) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 120.1(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C26 119.8(4) . . ? C23 C24 H24 120.1 . . ? C26 C24 H24 120.1 . . ? C2 C25 C3 127(4) . . ? C2 C25 C2' 14(5) . . ? C3 C25 C2' 118(3) . . ? C2 C25 H25 116.3 . . ? C3 C25 H25 116.3 . . ? C2' C25 H25 124.3 . . ? C24 C26 C27 120.2(3) . . ? C24 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C21 119.9(3) . . ? C26 C27 C28 117.0(3) . . ? C21 C27 C28 123.0(3) . . ? O7 C28 O10 123.7(3) . 3_566 ? O7 C28 C27 119.5(3) . . ? O10 C28 C27 116.8(3) 3_566 . ? C25 C2 C1 131(8) . . ? C25 C2 C6 112(7) . . ? C1 C2 C6 116(7) . . ? C4 C5 C6 121(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C2 119(4) . . ? C5 C6 H6 120.5 . . ? C2 C6 H6 120.5 . . ? C5 C4 C3 119(5) . . ? C5 C4 O3 123(8) . . ? C3 C4 O3 113(7) . . ? C6' C2' C25 118(6) . . ? C6' C2' C1 126(6) . . ? C25 C2' C1 114(4) . . ? C2' C6' C5' 121(4) . . ? C2' C6' H6' 119.3 . . ? C5' C6' H6' 119.3 . . ? C6' C5' C4' 118(3) . . ? C6' C5' H5' 121.2 . . ? C4' C5' H5' 121.2 . . ? C3 C4' O3 128(9) . . ? C3 C4' C5' 114(6) . . ? O3 C4' C5' 117(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co2 O1 C1 -100(6) 3_566 . . . ? O10 Co2 O1 C1 30.1(3) . . . . ? O10 Co2 O1 C1 -149.9(3) 3_566 . . . ? O8 Co2 O1 C1 137.9(3) 3_566 . . . ? O8 Co2 O1 C1 -42.1(3) . . . . ? O9 Co1 O2 C1 125.5(3) . . . . ? O6 Co1 O2 C1 -154.6(3) . . . . ? O8 Co1 O2 C1 27.1(3) . . . . ? O10 Co1 O2 C1 -49.6(3) . . . . ? O5 Co1 O2 C1 -141.2(3) . . . . ? O9 Co1 O5 C11 73.9(3) . . . . ? O2 Co1 O5 C11 -14.0(3) . . . . ? O6 Co1 O5 C11 162.7(3) . . . . ? O8 Co1 O5 C11 -123.5(4) . . . . ? O10 Co1 O5 C11 -104.3(3) . . . . ? O9 Co1 O6 Co1 -47.12(7) . . . 2_556 ? O2 Co1 O6 Co1 -126.8(4) . . . 2_556 ? O8 Co1 O6 Co1 51.52(6) . . . 2_556 ? O10 Co1 O6 Co1 128.52(6) . . . 2_556 ? O5 Co1 O6 Co1 -140.42(8) . . . 2_556 ? O9 Co1 O8 C14 67.4(3) . . . . ? O2 Co1 O8 C14 156.4(2) . . . . ? O6 Co1 O8 C14 -23.2(2) . . . . ? O10 Co1 O8 C14 -114.8(3) . . . . ? O5 Co1 O8 C14 -95.0(5) . . . . ? O9 Co1 O8 Co2 -150.27(8) . . . . ? O2 Co1 O8 Co2 -61.31(10) . . . . ? O6 Co1 O8 Co2 119.10(8) . . . . ? O10 Co1 O8 Co2 27.53(8) . . . . ? O5 Co1 O8 Co2 47.3(4) . . . . ? O1 Co2 O8 C14 -152.0(2) . . . . ? O1 Co2 O8 C14 28.0(2) 3_566 . . . ? O10 Co2 O8 C14 115.2(2) . . . . ? O10 Co2 O8 C14 -64.8(2) 3_566 . . . ? O8 Co2 O8 C14 -123(100) 3_566 . . . ? O1 Co2 O8 Co1 65.08(10) . . . . ? O1 Co2 O8 Co1 -114.92(10) 3_566 . . . ? O10 Co2 O8 Co1 -27.73(8) . . . . ? O10 Co2 O8 Co1 152.27(8) 3_566 . . . ? O8 Co2 O8 Co1 94(100) 3_566 . . . ? O2 Co1 O9 C14 -173.7(4) . . . 2_556 ? O6 Co1 O9 C14 20.3(4) . . . 2_556 ? O8 Co1 O9 C14 -77.4(4) . . . 2_556 ? O10 Co1 O9 C14 -101.9(10) . . . 2_556 ? O5 Co1 O9 C14 98.9(4) . . . 2_556 ? O9 Co1 O10 C28 131.9(9) . . . 3_566 ? O2 Co1 O10 C28 -156.4(2) . . . 3_566 ? O6 Co1 O10 C28 9.8(2) . . . 3_566 ? O8 Co1 O10 C28 107.0(2) . . . 3_566 ? O5 Co1 O10 C28 -68.9(2) . . . 3_566 ? O9 Co1 O10 Co2 -4.7(10) . . . . ? O2 Co1 O10 Co2 67.00(10) . . . . ? O6 Co1 O10 Co2 -126.82(9) . . . . ? O8 Co1 O10 Co2 -29.67(8) . . . . ? O5 Co1 O10 Co2 154.47(9) . . . . ? O1 Co2 O10 C28 158.6(2) . . . 3_566 ? O1 Co2 O10 C28 -21.4(2) 3_566 . . 3_566 ? O10 Co2 O10 C28 142(100) 3_566 . . 3_566 ? O8 Co2 O10 C28 67.5(2) 3_566 . . 3_566 ? O8 Co2 O10 C28 -112.5(2) . . . 3_566 ? O1 Co2 O10 Co1 -61.25(9) . . . . ? O1 Co2 O10 Co1 118.75(9) 3_566 . . . ? O10 Co2 O10 Co1 -78(100) 3_566 . . . ? O8 Co2 O10 Co1 -152.30(8) 3_566 . . . ? O8 Co2 O10 Co1 27.70(8) . . . . ? Co2 O1 C1 O2 -1.4(5) . . . . ? Co2 O1 C1 C2 -176(4) . . . . ? Co2 O1 C1 C2' 173(4) . . . . ? Co1 O2 C1 O1 13.0(5) . . . . ? Co1 O2 C1 C2 -173(4) . . . . ? Co1 O2 C1 C2' -162(4) . . . . ? C4' O3 C7 C8 20(7) . . . . ? C4 O3 C7 C8 32(6) . . . . ? C4' O3 C7 C13 -165(7) . . . . ? C4 O3 C7 C13 -153(6) . . . . ? O3 C7 C8 C9 175.1(4) . . . . ? C13 C7 C8 C9 -0.2(7) . . . . ? C7 C8 C9 C10 0.4(7) . . . 2_646 ? Co1 O5 C11 O4 1.3(6) . . . . ? Co1 O5 C11 C10 -179.1(2) . . . . ? C12 C10 C11 O5 6.9(5) 2_666 . . . ? C9 C10 C11 O5 -173.7(4) 2_666 . . . ? C12 C10 C11 O4 -173.5(3) 2_666 . . . ? C9 C10 C11 O4 5.9(5) 2_666 . . . ? C10 C12 C13 C7 0.5(6) 2_646 . . . ? C8 C7 C13 C12 -0.3(6) . . . . ? O3 C7 C13 C12 -175.9(4) . . . . ? Co1 O8 C14 O9 -7.3(5) . . . 2_556 ? Co2 O8 C14 O9 -139.7(3) . . . 2_556 ? Co1 O8 C14 C15 171.02(19) . . . . ? Co2 O8 C14 C15 38.6(4) . . . . ? O9 C14 C15 C16 42.6(4) 2_556 . . . ? O8 C14 C15 C16 -135.8(3) . . . . ? O9 C14 C15 C20 -143.4(3) 2_556 . . . ? O8 C14 C15 C20 38.2(4) . . . . ? C20 C15 C16 C17 -3.7(5) . . . . ? C14 C15 C16 C17 170.4(3) . . . . ? C15 C16 C17 C18 0.8(5) . . . . ? C16 C17 C18 C19 2.6(6) . . . . ? C17 C18 C19 C20 -3.1(6) . . . . ? C18 C19 C20 C15 0.3(5) . . . . ? C18 C19 C20 C21 172.6(3) . . . . ? C16 C15 C20 C19 3.1(5) . . . . ? C14 C15 C20 C19 -170.8(3) . . . . ? C16 C15 C20 C21 -169.1(3) . . . . ? C14 C15 C20 C21 17.0(5) . . . . ? C19 C20 C21 C22 -114.7(4) . . . . ? C15 C20 C21 C22 57.3(4) . . . . ? C19 C20 C21 C27 61.5(5) . . . . ? C15 C20 C21 C27 -126.5(4) . . . . ? C27 C21 C22 C23 1.0(5) . . . . ? C20 C21 C22 C23 177.5(3) . . . . ? C21 C22 C23 C24 0.3(6) . . . . ? C22 C23 C24 C26 -2.5(6) . . . . ? C4' C3 C25 C2 11(9) . . . . ? C4 C3 C25 C2 5(7) . . . . ? C4' C3 C25 C2' -1(8) . . . . ? C4 C3 C25 C2' -7(6) . . . . ? C23 C24 C26 C27 3.4(6) . . . . ? C24 C26 C27 C21 -2.1(5) . . . . ? C24 C26 C27 C28 173.0(3) . . . . ? C22 C21 C27 C26 -0.1(5) . . . . ? C20 C21 C27 C26 -176.3(3) . . . . ? C22 C21 C27 C28 -174.9(3) . . . . ? C20 C21 C27 C28 9.0(5) . . . . ? C26 C27 C28 O7 28.2(4) . . . . ? C21 C27 C28 O7 -157.0(3) . . . . ? C26 C27 C28 O10 -149.3(3) . . . 3_566 ? C21 C27 C28 O10 25.6(5) . . . 3_566 ? C3 C25 C2 C1 -173(5) . . . . ? C2' C25 C2 C1 -122(46) . . . . ? C3 C25 C2 C6 7(8) . . . . ? C2' C25 C2 C6 58(36) . . . . ? O1 C1 C2 C25 -8(10) . . . . ? O2 C1 C2 C25 177(6) . . . . ? C2' C1 C2 C25 122(46) . . . . ? O1 C1 C2 C6 172(4) . . . . ? O2 C1 C2 C6 -3(8) . . . . ? C2' C1 C2 C6 -59(35) . . . . ? C4 C5 C6 C2 -11(6) . . . . ? C25 C2 C6 C5 -5(7) . . . . ? C1 C2 C6 C5 176(4) . . . . ? C6 C5 C4 C3 24(9) . . . . ? C6 C5 C4 O3 175(5) . . . . ? C4' C3 C4 C5 -168(61) . . . . ? C25 C3 C4 C5 -22(9) . . . . ? C4' C3 C4 O3 39(49) . . . . ? C25 C3 C4 O3 -175(4) . . . . ? C7 O3 C4 C5 87(8) . . . . ? C4' O3 C4 C5 180(52) . . . . ? C7 O3 C4 C3 -121(5) . . . . ? C4' O3 C4 C3 -28(39) . . . . ? C2 C25 C2' C6' -156(47) . . . . ? C3 C25 C2' C6' -20(9) . . . . ? C2 C25 C2' C1 40(35) . . . . ? C3 C25 C2' C1 176(4) . . . . ? O1 C1 C2' C6' -147(7) . . . . ? O2 C1 C2' C6' 28(10) . . . . ? C2 C1 C2' C6' 157(48) . . . . ? O1 C1 C2' C25 15(8) . . . . ? O2 C1 C2' C25 -170(4) . . . . ? C2 C1 C2' C25 -40(34) . . . . ? C25 C2' C6' C5' 19(10) . . . . ? C1 C2' C6' C5' -179(5) . . . . ? C2' C6' C5' C4' 0(8) . . . . ? C25 C3 C4' O3 -168(8) . . . . ? C4 C3 C4' O3 -131(63) . . . . ? C25 C3 C4' C5' 19(12) . . . . ? C4 C3 C4' C5' 56(50) . . . . ? C7 O3 C4' C3 -125(9) . . . . ? C4 O3 C4' C3 142(54) . . . . ? C7 O3 C4' C5' 48(12) . . . . ? C4 O3 C4' C5' -46(40) . . . . ? C6' C5' C4' C3 -19(12) . . . . ? C6' C5' C4' O3 167(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.998 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.069 data_6 _database_code_depnum_ccdc_archive 'CCDC 884076' #TrackingRef 'web_deposit_cif_file_0_feilonghu_1350638779.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H50 Co3 N8 O22 S' _chemical_formula_weight 1347.85 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.685(8) _cell_length_b 18.809(5) _cell_length_c 10.441(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.500(3) _cell_angle_gamma 90.00 _cell_volume 5780(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Pink _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2764 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8144 _exptl_absorpt_correction_T_max 0.8292 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16114 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5083 _reflns_number_gt 4049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0651P)^2^+10.5797P] 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 5083 _refine_ls_number_parameters 390 _refine_ls_number_restraints 882 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.147 _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 Co1 Co 0.083767(15) 0.12842(2) 0.48867(4) 0.02674(16) Uani 1 1 d . . . Co2 Co 0.0000 0.23479(3) 0.2500 0.02598(18) Uani 1 2 d S . . N1 N 0.13391(10) 0.14663(17) 0.3609(3) 0.0343(7) Uani 1 1 d U . . N2 N 0.27872(11) 0.2100(2) 0.1817(3) 0.0477(9) Uani 1 1 d U . . N3 N 0.31012(11) 0.2109(2) 0.0914(3) 0.0499(9) Uani 1 1 d U . . N4 N 0.05143(10) 0.24099(17) 0.1195(3) 0.0346(7) Uani 1 1 d U . . O1 O 0.13856(9) 0.12152(15) 0.6319(3) 0.0441(7) Uani 1 1 d U . . O2 O 0.11399(11) 0.05915(19) 0.7874(3) 0.0615(9) Uani 1 1 d U . . O3 O 0.32925(13) 0.04572(19) 0.9328(6) 0.1216(19) Uani 1 1 d U . . O4 O 0.03920(9) 0.10675(15) 0.6300(3) 0.0432(7) Uani 1 1 d U . . H4C H 0.0619 0.0899 0.7072 0.052 Uiso 1 1 d R . . H4 H 0.0280 0.0671 0.6173 0.052 Uiso 1 1 d R . . O5 O 0.08467(10) 0.01594(14) 0.4738(3) 0.0444(7) Uani 1 1 d U . . H5C H 0.0621 -0.0084 0.5067 0.053 Uiso 1 1 d R . . H5 H 0.0919 0.0044 0.4035 0.053 Uiso 1 1 d R . . O6 O 0.03158(7) 0.13534(12) 0.3286(2) 0.0302(5) Uani 1 1 d U . . O7 O 0.02434(10) 0.04199(16) 0.1661(3) 0.0553(8) Uani 1 1 d U . . O8 O 0.03789(8) 0.29823(14) 0.3743(3) 0.0414(6) Uani 1 1 d U . . O9 O 0.08293(10) 0.23647(14) 0.5234(3) 0.0456(7) Uani 1 1 d U . . O10 O 0.9824(6) 0.4571(17) 0.468(4) 0.70(3) Uani 1 1 d . . . H10A H 0.9957 0.4278 0.4233 0.836 Uiso 1 1 d R . . H10B H 0.9547 0.4629 0.4379 0.836 Uiso 1 1 d R . . O11 O 0.5000 0.077(2) 0.2500 0.604(14) Uani 1 2 d SU . . H11C H 0.4953 0.0505 0.3128 0.725 Uiso 0.50 1 d PR . . S1 S 0.0000 0.08429(6) 0.2500 0.0307(3) Uani 1 2 d S . . C1 C 0.07078(13) 0.2925(2) 0.4630(4) 0.0368(9) Uani 1 1 d U . . C2 C 0.09820(14) 0.3583(2) 0.4929(4) 0.0478(11) Uani 1 1 d U . . C3 C 0.08954(19) 0.4190(3) 0.4186(6) 0.0803(17) Uani 1 1 d U . . H3 H 0.0659 0.4188 0.3507 0.096 Uiso 1 1 calc R . . C4 C 0.1152(2) 0.4796(3) 0.4432(7) 0.093(2) Uani 1 1 d U . . H4A H 0.1091 0.5197 0.3919 0.112 Uiso 1 1 calc R . . C5 C 0.1619(2) 0.4209(3) 0.6077(6) 0.092(2) Uani 1 1 d U . . H5A H 0.1876 0.4202 0.6688 0.111 Uiso 1 1 calc R . . C6 C 0.13574(19) 0.3598(3) 0.5830(5) 0.0721(16) Uani 1 1 d U . . H6 H 0.1442 0.3187 0.6295 0.087 Uiso 1 1 calc R . . C7 C 0.35039(18) -0.0197(2) 0.9570(7) 0.087(2) Uani 1 1 d U . . C8 C 0.28357(18) 0.0484(3) 0.8806(7) 0.0829(18) Uani 1 1 d U . . C9 C 0.2507(2) 0.0131(3) 0.9331(7) 0.0851(18) Uani 1 1 d U . . H9 H 0.2586 -0.0184 1.0009 0.102 Uiso 1 1 calc R . . C10 C 0.20572(18) 0.0236(2) 0.8865(5) 0.0634(13) Uani 1 1 d U . . H10 H 0.1832 0.0001 0.9239 0.076 Uiso 1 1 calc R . . C11 C 0.19408(14) 0.0697(2) 0.7833(4) 0.0426(10) Uani 1 1 d U . . C12 C 0.22812(15) 0.1047(3) 0.7305(5) 0.0572(12) Uani 1 1 d U . . H12 H 0.2206 0.1359 0.6620 0.069 Uiso 1 1 calc R . . C13 C 0.27314(17) 0.0939(3) 0.7783(6) 0.0730(15) Uani 1 1 d U . . H13 H 0.2960 0.1171 0.7417 0.088 Uiso 1 1 calc R . . C14 C 0.14532(13) 0.0839(2) 0.7308(4) 0.0369(9) Uani 1 1 d U . . C15 C 0.16980(13) 0.1882(2) 0.4035(4) 0.0420(9) Uani 1 1 d U . . H15 H 0.1705 0.2102 0.4836 0.050 Uiso 1 1 calc R . . C16 C 0.20545(13) 0.1996(2) 0.3342(4) 0.0445(10) Uani 1 1 d U . . H16 H 0.2295 0.2287 0.3673 0.053 Uiso 1 1 calc R . . C17 C 0.20532(13) 0.1675(2) 0.2145(4) 0.0411(9) Uani 1 1 d U . . C18 C 0.16806(13) 0.1252(2) 0.1700(4) 0.0441(10) Uani 1 1 d U . . H18 H 0.1664 0.1031 0.0899 0.053 Uiso 1 1 calc R . . C19 C 0.13362(13) 0.1163(2) 0.2452(4) 0.0393(9) Uani 1 1 d U . . H19 H 0.1090 0.0879 0.2138 0.047 Uiso 1 1 calc R . . C20 C 0.24274(13) 0.1770(2) 0.1375(4) 0.0458(10) Uani 1 1 d U . . H20 H 0.2401 0.1583 0.0543 0.055 Uiso 1 1 calc R . . C21 C 0.34633(14) 0.2438(2) 0.1315(4) 0.0455(10) Uani 1 1 d U . . H21 H 0.3501 0.2653 0.2124 0.055 Uiso 1 1 calc R . . C22 C 0.38266(13) 0.2474(2) 0.0475(4) 0.0389(9) Uani 1 1 d U . . C23 C 0.42146(17) 0.2868(3) 0.0800(5) 0.0682(15) Uani 1 1 d U . . H23 H 0.4264 0.3104 0.1588 0.082 Uiso 1 1 calc R . . C24 C 0.37883(14) 0.2112(3) -0.0667(4) 0.0491(11) Uani 1 1 d U . . H24 H 0.3540 0.1817 -0.0904 0.059 Uiso 1 1 calc R . . C25 C 0.08827(13) 0.2814(2) 0.1464(4) 0.0470(10) Uani 1 1 d U . . H25 H 0.0919 0.3062 0.2241 0.056 Uiso 1 1 calc R . . C26 C 0.04685(15) 0.2091(3) 0.0060(5) 0.0620(14) Uani 1 1 d U . . H26 H 0.0208 0.1823 -0.0177 0.074 Uiso 1 1 calc R . . O12 O 0.5000 0.2657(14) 0.2500 0.405(9) Uani 1 2 d SU . . H12C H 0.4851 0.2924 0.2951 0.486 Uiso 0.50 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 Co1 0.0205(3) 0.0305(3) 0.0293(3) 0.00431(19) 0.00380(18) -0.00106(18) Co2 0.0161(3) 0.0244(4) 0.0371(4) 0.000 0.0025(3) 0.000 N1 0.0240(15) 0.0446(18) 0.0349(17) 0.0080(14) 0.0060(12) -0.0042(13) N2 0.0309(17) 0.064(2) 0.051(2) 0.0089(17) 0.0176(15) -0.0051(16) N3 0.0323(18) 0.070(2) 0.051(2) 0.0086(18) 0.0197(16) -0.0095(17) N4 0.0233(15) 0.0385(17) 0.0421(18) 0.0029(14) 0.0050(13) -0.0026(13) O1 0.0317(14) 0.0550(18) 0.0435(16) 0.0191(13) -0.0037(12) -0.0070(12) O2 0.0516(19) 0.077(2) 0.058(2) 0.0332(17) 0.0149(15) 0.0096(17) O3 0.067(2) 0.040(2) 0.232(5) 0.002(3) -0.078(3) 0.0081(18) O4 0.0448(16) 0.0373(15) 0.0511(16) 0.0003(13) 0.0200(13) -0.0025(13) O5 0.0565(18) 0.0375(16) 0.0428(16) 0.0007(12) 0.0198(13) 0.0021(13) O6 0.0219(12) 0.0272(13) 0.0399(14) 0.0025(10) -0.0019(10) -0.0031(10) O7 0.0444(17) 0.0429(17) 0.078(2) -0.0221(15) 0.0063(15) 0.0144(13) O8 0.0309(14) 0.0379(15) 0.0530(17) -0.0077(12) -0.0044(12) -0.0051(11) O9 0.0533(17) 0.0310(15) 0.0503(16) 0.0012(12) -0.0016(13) -0.0058(12) O10 0.24(2) 0.78(7) 1.10(7) -0.44(5) 0.24(4) 0.16(3) O11 0.53(3) 0.49(3) 0.79(3) 0.000 0.06(3) 0.000 S1 0.0216(6) 0.0223(6) 0.0473(8) 0.000 0.0012(5) 0.000 C1 0.0327(19) 0.034(2) 0.043(2) -0.0055(16) 0.0016(17) -0.0054(16) C2 0.042(2) 0.031(2) 0.065(3) 0.0008(19) -0.015(2) -0.0054(17) C3 0.065(3) 0.046(3) 0.114(4) 0.012(3) -0.047(3) -0.011(2) C4 0.078(4) 0.041(3) 0.145(5) 0.016(3) -0.045(4) -0.016(3) C5 0.085(4) 0.050(3) 0.121(4) 0.006(3) -0.067(4) -0.015(3) C6 0.081(3) 0.041(3) 0.081(3) 0.010(2) -0.040(3) -0.011(2) C7 0.054(3) 0.031(2) 0.160(5) 0.005(3) -0.051(3) 0.002(2) C8 0.057(3) 0.034(2) 0.141(5) -0.006(3) -0.053(3) 0.009(2) C9 0.080(4) 0.043(3) 0.116(4) 0.017(3) -0.047(3) 0.005(3) C10 0.064(3) 0.044(2) 0.073(3) 0.012(2) -0.023(2) 0.004(2) C11 0.041(2) 0.033(2) 0.050(2) -0.0008(17) -0.0091(18) 0.0057(17) C12 0.042(2) 0.052(3) 0.072(3) 0.002(2) -0.013(2) 0.004(2) C13 0.043(3) 0.052(3) 0.115(4) -0.001(3) -0.020(3) 0.000(2) C14 0.040(2) 0.034(2) 0.036(2) 0.0027(16) 0.0009(17) 0.0038(16) C15 0.035(2) 0.056(2) 0.036(2) 0.0022(18) 0.0063(16) -0.0111(18) C16 0.030(2) 0.057(3) 0.047(2) 0.0057(19) 0.0061(17) -0.0117(18) C17 0.0288(19) 0.050(2) 0.046(2) 0.0083(18) 0.0107(17) -0.0013(17) C18 0.035(2) 0.056(3) 0.043(2) -0.0030(19) 0.0119(17) -0.0058(18) C19 0.0284(19) 0.046(2) 0.045(2) 0.0027(18) 0.0083(16) -0.0073(16) C20 0.034(2) 0.059(3) 0.047(2) 0.0096(19) 0.0146(18) -0.0022(19) C21 0.038(2) 0.052(2) 0.050(2) 0.0028(19) 0.0174(18) -0.0069(19) C22 0.0296(19) 0.043(2) 0.046(2) 0.0038(18) 0.0125(17) -0.0059(16) C23 0.057(3) 0.086(4) 0.068(3) -0.032(3) 0.032(2) -0.032(3) C24 0.036(2) 0.061(3) 0.053(3) -0.005(2) 0.0144(19) -0.022(2) C25 0.037(2) 0.056(3) 0.050(2) -0.009(2) 0.0135(18) -0.0176(19) C26 0.042(2) 0.079(3) 0.070(3) -0.025(3) 0.023(2) -0.034(2) O12 0.474(18) 0.405(18) 0.333(17) 0.000 0.040(17) 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 Co1 O9 2.065(3) . ? Co1 O1 2.065(3) . ? Co1 O5 2.122(3) . ? Co1 O6 2.129(2) . ? Co1 O4 2.146(3) . ? Co1 N1 2.152(3) . ? Co2 O8 1.998(3) . ? Co2 O8 1.998(3) 2 ? Co2 N4 2.178(3) . ? Co2 N4 2.178(3) 2 ? Co2 O6 2.202(2) . ? Co2 O6 2.202(2) 2 ? N1 C19 1.335(5) . ? N1 C15 1.349(5) . ? N2 C20 1.270(5) . ? N2 N3 1.410(5) . ? N3 C21 1.264(5) . ? N4 C26 1.319(6) . ? N4 C25 1.331(5) . ? O1 C14 1.245(4) . ? O2 C14 1.255(5) . ? O3 C7 1.390(6) . ? O3 C8 1.395(6) . ? O4 H4C 1.0302 . ? O4 H4 0.8200 . ? O5 H5C 0.9152 . ? O5 H5 0.8200 . ? O6 S1 1.508(2) . ? O7 S1 1.445(3) . ? O8 C1 1.260(5) . ? O9 C1 1.256(5) . ? O10 H10A 0.8500 . ? O10 H10B 0.8499 . ? O11 H11C 0.8501 . ? S1 O7 1.445(3) 2 ? S1 O6 1.508(2) 2 ? C1 C2 1.492(5) . ? C2 C6 1.361(6) . ? C2 C3 1.386(7) . ? C3 C4 1.376(7) . ? C3 H3 0.9300 . ? C4 C7 1.361(7) 4_556 ? C4 H4A 0.9300 . ? C5 C7 1.331(7) 4_556 ? C5 C6 1.391(7) . ? C5 H5A 0.9300 . ? C6 H6 0.9300 . ? C7 C5 1.331(7) 4_546 ? C7 C4 1.361(7) 4_546 ? C8 C9 1.354(9) . ? C8 C13 1.373(8) . ? C9 C10 1.374(7) . ? C9 H9 0.9300 . ? C10 C11 1.390(6) . ? C10 H10 0.9300 . ? C11 C12 1.380(6) . ? C11 C14 1.504(5) . ? C12 C13 1.379(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.375(5) . ? C15 H15 0.9300 . ? C16 C17 1.388(6) . ? C16 H16 0.9300 . ? C17 C18 1.392(6) . ? C17 C20 1.465(5) . ? C18 C19 1.378(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.477(5) . ? C21 H21 0.9300 . ? C22 C24 1.365(6) . ? C22 C23 1.374(6) . ? C23 C26 1.385(6) 7 ? C23 H23 0.9300 . ? C24 C25 1.370(6) 7 ? C24 H24 0.9300 . ? C25 C24 1.370(6) 7 ? C25 H25 0.9300 . ? C26 C23 1.385(6) 7 ? C26 H26 0.9300 . ? O12 H12C 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 O9 Co1 O1 87.76(11) . . ? O9 Co1 O5 174.09(11) . . ? O1 Co1 O5 88.52(11) . . ? O9 Co1 O6 93.07(10) . . ? O1 Co1 O6 174.81(10) . . ? O5 Co1 O6 91.05(10) . . ? O9 Co1 O4 92.49(11) . . ? O1 Co1 O4 89.30(11) . . ? O5 Co1 O4 82.87(10) . . ? O6 Co1 O4 95.78(10) . . ? O9 Co1 N1 88.71(12) . . ? O1 Co1 N1 85.18(11) . . ? O5 Co1 N1 95.56(11) . . ? O6 Co1 N1 89.71(10) . . ? O4 Co1 N1 174.31(11) . . ? O8 Co2 O8 106.65(16) . 2 ? O8 Co2 N4 89.61(12) . . ? O8 Co2 N4 86.73(11) 2 . ? O8 Co2 N4 86.73(11) . 2 ? O8 Co2 N4 89.61(12) 2 2 ? N4 Co2 N4 173.86(17) . 2 ? O8 Co2 O6 95.10(10) . . ? O8 Co2 O6 157.74(10) 2 . ? N4 Co2 O6 88.83(10) . . ? N4 Co2 O6 96.39(10) 2 . ? O8 Co2 O6 157.74(10) . 2 ? O8 Co2 O6 95.10(10) 2 2 ? N4 Co2 O6 96.39(10) . 2 ? N4 Co2 O6 88.83(10) 2 2 ? O6 Co2 O6 63.73(12) . 2 ? C19 N1 C15 117.3(3) . . ? C19 N1 Co1 124.7(2) . . ? C15 N1 Co1 117.9(3) . . ? C20 N2 N3 111.1(4) . . ? C21 N3 N2 113.1(4) . . ? C26 N4 C25 115.7(3) . . ? C26 N4 Co2 122.6(3) . . ? C25 N4 Co2 121.5(3) . . ? C14 O1 Co1 131.5(3) . . ? C7 O3 C8 119.7(4) . . ? Co1 O4 H4C 101.4 . . ? Co1 O4 H4 109.5 . . ? H4C O4 H4 93.2 . . ? Co1 O5 H5C 117.0 . . ? Co1 O5 H5 109.7 . . ? H5C O5 H5 119.7 . . ? S1 O6 Co1 136.49(14) . . ? S1 O6 Co2 97.69(12) . . ? Co1 O6 Co2 125.12(11) . . ? C1 O8 Co2 138.0(3) . . ? C1 O9 Co1 138.3(3) . . ? H10A O10 H10B 112.1 . . ? O7 S1 O7 113.2(3) . 2 ? O7 S1 O6 110.86(15) . . ? O7 S1 O6 110.19(16) 2 . ? O7 S1 O6 110.19(16) . 2 ? O7 S1 O6 110.86(15) 2 2 ? O6 S1 O6 100.90(19) . 2 ? O9 C1 O8 125.8(4) . . ? O9 C1 C2 118.5(3) . . ? O8 C1 C2 115.6(4) . . ? C6 C2 C3 116.4(4) . . ? C6 C2 C1 122.5(4) . . ? C3 C2 C1 120.7(4) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C7 C4 C3 119.6(5) 4_556 . ? C7 C4 H4A 120.2 4_556 . ? C3 C4 H4A 120.2 . . ? C7 C5 C6 119.3(5) 4_556 . ? C7 C5 H5A 120.3 4_556 . ? C6 C5 H5A 120.3 . . ? C2 C6 C5 122.1(5) . . ? C2 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C5 C7 C4 120.6(5) 4_546 4_546 ? C5 C7 O3 124.3(5) 4_546 . ? C4 C7 O3 115.1(5) 4_546 . ? C9 C8 C13 121.3(5) . . ? C9 C8 O3 122.7(6) . . ? C13 C8 O3 115.8(6) . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 119.7(5) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.1(4) . . ? C12 C11 C14 119.3(4) . . ? C10 C11 C14 121.6(4) . . ? C13 C12 C11 120.7(5) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C8 C13 C12 118.9(6) . . ? C8 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? O1 C14 O2 123.5(4) . . ? O1 C14 C11 116.5(4) . . ? O2 C14 C11 119.9(4) . . ? N1 C15 C16 123.0(4) . . ? N1 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C17 119.7(4) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 117.2(4) . . ? C16 C17 C20 121.9(4) . . ? C18 C17 C20 120.9(4) . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? N1 C19 C18 123.1(4) . . ? N1 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? N2 C20 C17 121.5(4) . . ? N2 C20 H20 119.3 . . ? C17 C20 H20 119.3 . . ? N3 C21 C22 118.7(4) . . ? N3 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C24 C22 C23 117.1(4) . . ? C24 C22 C21 120.8(4) . . ? C23 C22 C21 122.1(4) . . ? C22 C23 C26 119.3(4) . 7 ? C22 C23 H23 120.4 . . ? C26 C23 H23 120.4 7 . ? C22 C24 C25 119.7(4) . 7 ? C22 C24 H24 120.1 . . ? C25 C24 H24 120.1 7 . ? N4 C25 C24 124.1(4) . 7 ? N4 C25 H25 117.9 . . ? C24 C25 H25 117.9 7 . ? N4 C26 C23 123.9(4) . 7 ? N4 C26 H26 118.0 . . ? C23 C26 H26 118.0 7 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Co1 N1 C19 -136.2(3) . . . . ? O1 Co1 N1 C19 135.9(3) . . . . ? O5 Co1 N1 C19 47.9(3) . . . . ? O6 Co1 N1 C19 -43.2(3) . . . . ? O4 Co1 N1 C19 121.6(11) . . . . ? O9 Co1 N1 C15 48.1(3) . . . . ? O1 Co1 N1 C15 -39.8(3) . . . . ? O5 Co1 N1 C15 -127.8(3) . . . . ? O6 Co1 N1 C15 141.1(3) . . . . ? O4 Co1 N1 C15 -54.1(13) . . . . ? C20 N2 N3 C21 179.5(4) . . . . ? O8 Co2 N4 C26 -178.3(4) . . . . ? O8 Co2 N4 C26 -71.6(4) 2 . . . ? N4 Co2 N4 C26 -125.1(4) 2 . . . ? O6 Co2 N4 C26 86.5(4) . . . . ? O6 Co2 N4 C26 23.1(4) 2 . . . ? O8 Co2 N4 C25 -2.9(3) . . . . ? O8 Co2 N4 C25 103.8(3) 2 . . . ? N4 Co2 N4 C25 50.4(3) 2 . . . ? O6 Co2 N4 C25 -98.0(3) . . . . ? O6 Co2 N4 C25 -161.4(3) 2 . . . ? O9 Co1 O1 C14 126.3(4) . . . . ? O5 Co1 O1 C14 -49.1(4) . . . . ? O6 Co1 O1 C14 -134.4(10) . . . . ? O4 Co1 O1 C14 33.8(4) . . . . ? N1 Co1 O1 C14 -144.8(4) . . . . ? O9 Co1 O6 S1 -164.5(2) . . . . ? O1 Co1 O6 S1 96.4(11) . . . . ? O5 Co1 O6 S1 11.2(2) . . . . ? O4 Co1 O6 S1 -71.7(2) . . . . ? N1 Co1 O6 S1 106.8(2) . . . . ? O9 Co1 O6 Co2 3.47(15) . . . . ? O1 Co1 O6 Co2 -95.6(11) . . . . ? O5 Co1 O6 Co2 179.22(14) . . . . ? O4 Co1 O6 Co2 96.28(14) . . . . ? N1 Co1 O6 Co2 -85.22(15) . . . . ? O8 Co2 O6 S1 172.79(12) . . . . ? O8 Co2 O6 S1 -19.3(3) 2 . . . ? N4 Co2 O6 S1 -97.71(13) . . . . ? N4 Co2 O6 S1 85.52(13) 2 . . . ? O6 Co2 O6 S1 0.0 2 . . . ? O8 Co2 O6 Co1 1.08(15) . . . . ? O8 Co2 O6 Co1 169.0(2) 2 . . . ? N4 Co2 O6 Co1 90.58(15) . . . . ? N4 Co2 O6 Co1 -86.19(15) 2 . . . ? O6 Co2 O6 Co1 -171.7(2) 2 . . . ? O8 Co2 O8 C1 -170.5(4) 2 . . . ? N4 Co2 O8 C1 -84.1(4) . . . . ? N4 Co2 O8 C1 100.9(4) 2 . . . ? O6 Co2 O8 C1 4.7(4) . . . . ? O6 Co2 O8 C1 22.0(6) 2 . . . ? O1 Co1 O9 C1 153.0(4) . . . . ? O5 Co1 O9 C1 -155.9(9) . . . . ? O6 Co1 O9 C1 -21.8(4) . . . . ? O4 Co1 O9 C1 -117.8(4) . . . . ? N1 Co1 O9 C1 67.8(4) . . . . ? Co1 O6 S1 O7 -73.2(3) . . . . ? Co2 O6 S1 O7 116.72(17) . . . . ? Co1 O6 S1 O7 52.9(3) . . . 2 ? Co2 O6 S1 O7 -117.21(16) . . . 2 ? Co1 O6 S1 O6 170.1(3) . . . 2 ? Co2 O6 S1 O6 0.0 . . . 2 ? Co1 O9 C1 O8 32.4(7) . . . . ? Co1 O9 C1 C2 -144.8(3) . . . . ? Co2 O8 C1 O9 -20.2(7) . . . . ? Co2 O8 C1 C2 157.1(3) . . . . ? O9 C1 C2 C6 -0.1(7) . . . . ? O8 C1 C2 C6 -177.6(5) . . . . ? O9 C1 C2 C3 172.2(5) . . . . ? O8 C1 C2 C3 -5.3(7) . . . . ? C6 C2 C3 C4 -5.8(10) . . . . ? C1 C2 C3 C4 -178.5(6) . . . . ? C2 C3 C4 C7 -0.5(12) . . . 4_556 ? C3 C2 C6 C5 5.5(10) . . . . ? C1 C2 C6 C5 178.2(6) . . . . ? C7 C5 C6 C2 1.1(11) 4_556 . . . ? C8 O3 C7 C5 27.7(12) . . . 4_546 ? C8 O3 C7 C4 -150.4(7) . . . 4_546 ? C7 O3 C8 C9 52.7(10) . . . . ? C7 O3 C8 C13 -132.5(7) . . . . ? C13 C8 C9 C10 -1.6(10) . . . . ? O3 C8 C9 C10 172.8(5) . . . . ? C8 C9 C10 C11 1.3(9) . . . . ? C9 C10 C11 C12 -0.8(7) . . . . ? C9 C10 C11 C14 -178.8(5) . . . . ? C10 C11 C12 C13 0.6(7) . . . . ? C14 C11 C12 C13 178.7(4) . . . . ? C9 C8 C13 C12 1.4(9) . . . . ? O3 C8 C13 C12 -173.4(5) . . . . ? C11 C12 C13 C8 -0.9(8) . . . . ? Co1 O1 C14 O2 -25.7(6) . . . . ? Co1 O1 C14 C11 155.4(3) . . . . ? C12 C11 C14 O1 7.5(6) . . . . ? C10 C11 C14 O1 -174.5(4) . . . . ? C12 C11 C14 O2 -171.5(4) . . . . ? C10 C11 C14 O2 6.5(6) . . . . ? C19 N1 C15 C16 -0.6(6) . . . . ? Co1 N1 C15 C16 175.4(3) . . . . ? N1 C15 C16 C17 0.0(7) . . . . ? C15 C16 C17 C18 0.6(6) . . . . ? C15 C16 C17 C20 -179.1(4) . . . . ? C16 C17 C18 C19 -0.6(6) . . . . ? C20 C17 C18 C19 179.0(4) . . . . ? C15 N1 C19 C18 0.6(6) . . . . ? Co1 N1 C19 C18 -175.1(3) . . . . ? C17 C18 C19 N1 0.0(6) . . . . ? N3 N2 C20 C17 178.7(4) . . . . ? C16 C17 C20 N2 6.1(7) . . . . ? C18 C17 C20 N2 -173.6(4) . . . . ? N2 N3 C21 C22 178.7(4) . . . . ? N3 C21 C22 C24 -5.1(7) . . . . ? N3 C21 C22 C23 174.8(5) . . . . ? C24 C22 C23 C26 3.2(8) . . . 7 ? C21 C22 C23 C26 -176.7(5) . . . 7 ? C23 C22 C24 C25 -3.7(7) . . . 7 ? C21 C22 C24 C25 176.3(4) . . . 7 ? C26 N4 C25 C24 -2.6(7) . . . 7 ? Co2 N4 C25 C24 -178.3(4) . . . 7 ? C25 N4 C26 C23 3.0(8) . . . 7 ? Co2 N4 C26 C23 178.7(4) . . . 7 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.620 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.073