# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_Dy _database_code_depnum_ccdc_archive 'CCDC 872217' #TrackingRef '15314_web_deposit_cif_file_0_KlausHarms_1352392481.Ni2_Ln_oct.cif' _audit_update_record ; 2012-08-23 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H84 Dy N16 Ni2 O21, 3(N O3), 15(H2 O)' _chemical_formula_sum 'C56 H114 Dy N19 Ni2 O36' _chemical_formula_weight 1909.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 14.8795(9) _cell_length_b 16.0919(8) _cell_length_c 18.6121(10) _cell_angle_alpha 102.704(4) _cell_angle_beta 106.785(5) _cell_angle_gamma 103.584(4) _cell_volume 3944.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16527 _cell_measurement_theta_min 4.58 _cell_measurement_theta_max 26.82 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1986 _exptl_absorpt_coefficient_mu 1.511 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7325 _exptl_absorpt_correction_T_max 0.9320 _exptl_absorpt_process_details 'STOE X-SHAPE / X-RED' _exptl_special_details ? _diffrn_ambient_temperature 100(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 25555 _diffrn_reflns_av_R_equivalents 0.0858 _diffrn_reflns_av_sigmaI/netI 0.1831 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13546 _reflns_number_gt 7334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA (STOE & Cie, 2006)' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material 'ENCIFER, PUBLCIF' _refine_special_details ; The solvent water oxygen atoms have been refined as a mixture of fully and partly occupied positions. Hydrogen atoms have not been included into the refinement. Restraints have been included for the geometry of disordered parts of the cation and for the geometry of the NO3-ions ("SADI") and for the shape of the thermal ellipsoids of the water oxygen atoms and the nitrate anions ("SIMU, "ISOR"). The remaining non ideal geometries of the NO3 ions and high anisotropic temperature factors of oxygen atoms (O102 O103 O202 O203 O201 O902 O904 O905 O906 O911 O912 O913 O914) indicate disorder that has not been resolved. 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^)+(0.0415P)^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 13546 _refine_ls_number_parameters 1093 _refine_ls_number_restraints 264 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.882 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3003(6) 1.0402(6) 0.1253(5) 0.037(2) Uani 1 1 d . . . C2 C 0.3054(6) 1.1356(6) 0.1551(5) 0.034(2) Uani 1 1 d . . . C3 C 0.2540(6) 1.1613(6) 0.2055(4) 0.033(2) Uani 1 1 d . . . C4 C 0.2643(6) 1.2533(6) 0.2339(4) 0.032(2) Uani 1 1 d . . . C5 C 0.3276(6) 1.3169(6) 0.2129(5) 0.039(2) Uani 1 1 d . . . H5 H 0.3359 1.3788 0.2333 0.047 Uiso 1 1 calc R . . C6 C 0.3764(6) 1.2925(6) 0.1652(5) 0.040(2) Uani 1 1 d . . . H6 H 0.4192 1.3364 0.1529 0.048 Uiso 1 1 calc R . . C7 C 0.3624(6) 1.2011(6) 0.1345(5) 0.037(2) Uani 1 1 d . . . H7 H 0.3931 1.1832 0.0983 0.045 Uiso 1 1 calc R . . C8 C 0.2158(6) 1.2852(6) 0.2837(4) 0.031(2) Uani 1 1 d . . . H8 H 0.2270 1.3479 0.3027 0.038 Uiso 1 1 calc R . . C10 C 0.1010(6) 1.2567(6) 0.3532(5) 0.039(2) Uani 1 1 d . . . H10A H 0.1195 1.3230 0.3719 0.047 Uiso 1 1 calc R . . H10B H 0.1172 1.2353 0.3998 0.047 Uiso 1 1 calc R . . C11 C -0.0100(6) 1.2156(6) 0.3046(5) 0.041(2) Uani 1 1 d . . . H11A H -0.0477 1.2283 0.3393 0.049 Uiso 1 1 calc R . . H11B H -0.0270 1.2444 0.2630 0.049 Uiso 1 1 calc R . . C13 C -0.1269(6) 1.0876(6) 0.1958(5) 0.040(2) Uani 1 1 d . . . H13A H -0.1671 1.1284 0.1991 0.048 Uiso 1 1 calc R . . H13B H -0.1681 1.0267 0.1900 0.048 Uiso 1 1 calc R . . C14 C -0.0967(7) 1.0850(6) 0.1254(5) 0.041(2) Uani 1 1 d . . . H14A H -0.1554 1.0734 0.0781 0.049 Uiso 1 1 calc R . . H14B H -0.0485 1.1437 0.1341 0.049 Uiso 1 1 calc R . . C16 C -0.0880(6) 0.9433(6) 0.0510(5) 0.035(2) Uani 1 1 d . . . H16 H -0.1479 0.9392 0.0120 0.042 Uiso 1 1 calc R . . C17 C -0.0482(6) 0.8718(6) 0.0355(5) 0.034(2) Uani 1 1 d . . . C18 C 0.0377(6) 0.8674(5) 0.0924(5) 0.0317(19) Uani 1 1 d . . . C19 C 0.0756(6) 0.7984(6) 0.0678(4) 0.034(2) Uani 1 1 d . . . C20 C 0.0295(6) 0.7372(6) -0.0077(5) 0.036(2) Uani 1 1 d . . . H20 H 0.0574 0.6921 -0.0230 0.043 Uiso 1 1 calc R . . C21 C -0.0572(6) 0.7397(6) -0.0622(5) 0.042(2) Uani 1 1 d . . . H21 H -0.0884 0.6965 -0.1132 0.050 Uiso 1 1 calc R . . C22 C -0.0951(6) 0.8068(6) -0.0391(5) 0.035(2) Uani 1 1 d . . . H22 H -0.1544 0.8091 -0.0744 0.043 Uiso 1 1 calc R . . C23 C 0.1662(6) 0.7837(6) 0.1193(5) 0.036(2) Uani 1 1 d . . . C24 C -0.0502(6) 1.0693(6) 0.3258(5) 0.037(2) Uani 1 1 d . . . H24A H -0.1095 1.0735 0.3384 0.044 Uiso 1 1 calc R . . H24B H 0.0083 1.0978 0.3753 0.044 Uiso 1 1 calc R . . C25 C -0.0601(6) 0.9708(6) 0.2939(5) 0.037(2) Uani 1 1 d . . . H25A H -0.1256 0.9392 0.2514 0.044 Uiso 1 1 calc R . . H25B H -0.0085 0.9661 0.2709 0.044 Uiso 1 1 calc R . . C27 C 0.1366(6) 0.8335(6) 0.3545(5) 0.035(2) Uani 1 1 d . B . C28 C 0.2324(6) 0.8141(5) 0.3852(4) 0.0310(19) Uani 1 1 d . . . C29 C 0.3235(6) 0.8672(5) 0.3855(4) 0.0273(18) Uani 1 1 d . . . C30 C 0.4103(6) 0.8464(6) 0.4224(4) 0.0291(19) Uani 1 1 d . . . C31 C 0.4045(6) 0.7731(6) 0.4527(4) 0.037(2) Uani 1 1 d . . . H31 H 0.4630 0.7598 0.4760 0.044 Uiso 1 1 calc R . . C32 C 0.3168(6) 0.7221(6) 0.4488(5) 0.037(2) Uani 1 1 d . . . H32 H 0.3130 0.6716 0.4678 0.044 Uiso 1 1 calc R . . C33 C 0.2308(6) 0.7431(5) 0.4168(4) 0.034(2) Uani 1 1 d . . . H33 H 0.1697 0.7080 0.4165 0.040 Uiso 1 1 calc R . . C34 C 0.5063(6) 0.8996(6) 0.4309(4) 0.037(2) Uani 1 1 d . . . H34 H 0.5610 0.8823 0.4560 0.045 Uiso 1 1 calc R . . C36 C 0.6270(6) 1.0182(6) 0.4143(5) 0.039(2) Uani 1 1 d . . . H36A H 0.6752 1.0119 0.4606 0.047 Uiso 1 1 calc R . . H36B H 0.6359 1.0830 0.4229 0.047 Uiso 1 1 calc R . . C37 C 0.6468(6) 0.9801(7) 0.3409(5) 0.046(3) Uani 1 1 d . . . H37A H 0.7178 1.0069 0.3499 0.055 Uiso 1 1 calc R . . H37B H 0.6322 0.9143 0.3297 0.055 Uiso 1 1 calc R . . C39 C 0.6376(6) 1.0861(7) 0.2666(5) 0.050(3) Uani 1 1 d . . . H39A H 0.6785 1.0760 0.2340 0.060 Uiso 1 1 calc R . . H39B H 0.6827 1.1257 0.3200 0.060 Uiso 1 1 calc R . . C40 C 0.5683(8) 1.1326(8) 0.2311(6) 0.063(3) Uani 1 1 d . . . H40A H 0.6067 1.1887 0.2258 0.075 Uiso 1 1 calc R . . H40B H 0.5227 1.0933 0.1777 0.075 Uiso 1 1 calc R . . C42 C 0.5227(7) 1.2328(7) 0.3241(5) 0.044(2) Uani 1 1 d . . . H42 H 0.5719 1.2821 0.3234 0.053 Uiso 1 1 calc R . . C43 C 0.4680(6) 1.2518(6) 0.3727(5) 0.036(2) Uani 1 1 d . . . C44 C 0.3929(6) 1.1805(6) 0.3760(4) 0.0300(19) Uani 1 1 d . . . C45 C 0.3407(6) 1.2032(5) 0.4261(4) 0.0309(19) Uani 1 1 d . . . C46 C 0.3629(7) 1.2928(6) 0.4682(5) 0.042(2) Uani 1 1 d . . . H46 H 0.3279 1.3080 0.5018 0.051 Uiso 1 1 calc R . . C47 C 0.4358(7) 1.3612(6) 0.4623(5) 0.048(2) Uani 1 1 d . . . H47 H 0.4493 1.4220 0.4914 0.057 Uiso 1 1 calc R . . C48 C 0.4866(6) 1.3412(6) 0.4155(5) 0.044(2) Uani 1 1 d . . . H48 H 0.5356 1.3880 0.4115 0.053 Uiso 1 1 calc R . . C49 C 0.2585(6) 1.1349(6) 0.4324(5) 0.032(2) Uani 1 1 d . . . C50 C 0.5602(9) 0.9301(9) 0.1987(6) 0.086(4) Uani 1 1 d D . . H50A H 0.6226 0.9357 0.1882 0.103 Uiso 0.51(2) 1 calc PR A 1 H50B H 0.5169 0.9476 0.1575 0.103 Uiso 0.51(2) 1 calc PR A 1 H50C H 0.6142 0.9040 0.1982 0.103 Uiso 0.49(2) 1 calc PR A 2 H50D H 0.5422 0.9522 0.1527 0.103 Uiso 0.49(2) 1 calc PR A 2 C51 C 0.5088(12) 0.8250(12) 0.1814(10) 0.045(6) Uani 0.51(2) 1 d PD A 1 H51A H 0.5149 0.7899 0.1331 0.055 Uiso 0.51(2) 1 calc PR A 1 H51B H 0.5413 0.8054 0.2261 0.055 Uiso 0.51(2) 1 calc PR A 1 C51A C 0.4668(15) 0.8609(13) 0.2027(12) 0.043(6) Uani 0.49(2) 1 d PD A 2 H51C H 0.4883 0.8356 0.2462 0.052 Uiso 0.49(2) 1 calc PR A 2 H51D H 0.4194 0.8919 0.2125 0.052 Uiso 0.49(2) 1 calc PR A 2 C54 C -0.0667(6) 0.6259(6) 0.2420(5) 0.041(2) Uani 1 1 d . . . H54A H -0.0899 0.5601 0.2162 0.049 Uiso 1 1 calc R . . H54B H 0.0041 0.6442 0.2754 0.049 Uiso 1 1 calc R . . C55 C -0.0783(7) 0.6736(7) 0.1791(5) 0.050(3) Uani 1 1 d . . . H55A H -0.0259 0.6719 0.1565 0.061 Uiso 1 1 calc R . . H55B H -0.1433 0.6415 0.1360 0.061 Uiso 1 1 calc R . . C57 C -0.0910(7) 0.6265(6) 0.3671(5) 0.047(2) Uani 1 1 d . . . H57A H -0.0180 0.6415 0.3871 0.057 Uiso 1 1 calc R . . H57B H -0.1207 0.5614 0.3575 0.057 Uiso 1 1 calc R . . C58 C -0.1224(8) 0.6798(7) 0.4274(6) 0.060(3) Uani 1 1 d . . . H58A H -0.1952 0.6560 0.4122 0.072 Uiso 1 1 calc R . . H58B H -0.0913 0.6729 0.4795 0.072 Uiso 1 1 calc R . . C60 C -0.2327(6) 0.6058(7) 0.2496(6) 0.054(3) Uani 1 1 d D . . H60A H -0.2545 0.5494 0.2621 0.065 Uiso 0.38(3) 1 calc PR B 1 H60B H -0.2473 0.5901 0.1921 0.065 Uiso 0.38(3) 1 calc PR B 1 H60C H -0.2633 0.5889 0.2872 0.065 Uiso 0.62(3) 1 calc PR B 2 H60D H -0.2450 0.5499 0.2078 0.065 Uiso 0.62(3) 1 calc PR B 2 C61 C -0.290(2) 0.6663(15) 0.272(2) 0.077(13) Uani 0.38(3) 1 d PD B 1 H61A H -0.2922 0.6681 0.3248 0.092 Uiso 0.38(3) 1 calc PR B 1 H61B H -0.3594 0.6424 0.2336 0.092 Uiso 0.38(3) 1 calc PR B 1 C61A C -0.2823(12) 0.6662(10) 0.2126(12) 0.060(7) Uani 0.62(3) 1 d PD B 2 H61C H -0.3549 0.6425 0.1988 0.071 Uiso 0.62(3) 1 calc PR B 2 H61D H -0.2692 0.6676 0.1636 0.071 Uiso 0.62(3) 1 calc PR B 2 C64 C 0.1524(8) 0.5259(7) 0.0069(6) 0.058(3) Uani 1 1 d . . . H64A H 0.1126 0.4614 -0.0153 0.070 Uiso 1 1 calc R . . H64B H 0.1060 0.5613 0.0012 0.070 Uiso 1 1 calc R . . C65 C 0.2167(10) 0.5468(8) -0.0385(7) 0.072(3) Uani 1 1 d . . . H65A H 0.1762 0.5455 -0.0916 0.086 Uiso 1 1 calc R . . H65B H 0.2509 0.5014 -0.0450 0.086 Uiso 1 1 calc R . . C67 C 0.2631(8) 0.4796(7) 0.1059(6) 0.064(3) Uani 1 1 d . . . H67A H 0.2615 0.4672 0.1554 0.076 Uiso 1 1 calc R . . H67B H 0.2279 0.4225 0.0622 0.076 Uiso 1 1 calc R . . C68 C 0.3677(10) 0.5116(9) 0.1116(9) 0.101(5) Uani 1 1 d . . . H68A H 0.4048 0.4768 0.1387 0.121 Uiso 1 1 calc R . . H68B H 0.3697 0.4996 0.0577 0.121 Uiso 1 1 calc R . . C70 C 0.1482(8) 0.5544(8) 0.1413(6) 0.061(3) Uani 1 1 d . . . H70A H 0.1101 0.4940 0.1392 0.073 Uiso 1 1 calc R . . H70B H 0.1008 0.5854 0.1214 0.073 Uiso 1 1 calc R . . C71 C 0.2162(10) 0.6080(10) 0.2258(6) 0.082(4) Uani 1 1 d . . . H71A H 0.1754 0.6244 0.2568 0.099 Uiso 1 1 calc R . . H71B H 0.2507 0.5695 0.2494 0.099 Uiso 1 1 calc R . . Dy1 Dy 0.22719(3) 0.97812(3) 0.26488(2) 0.02687(12) Uani 1 1 d . . . N9 N 0.1560(5) 1.2301(5) 0.3041(4) 0.0335(17) Uani 1 1 d . . . N12 N -0.0392(5) 1.1191(5) 0.2682(4) 0.0339(17) Uani 1 1 d . . . N15 N -0.0508(5) 1.0124(5) 0.1124(4) 0.0340(17) Uani 1 1 d . . . N26 N -0.0499(5) 0.9265(5) 0.3564(4) 0.0398(18) Uani 1 1 d . . . H26A H -0.0882 0.9426 0.3844 0.048 Uiso 1 1 calc R . . H26B H 0.0150 0.9500 0.3906 0.048 Uiso 1 1 calc R . . N35 N 0.5256(5) 0.9710(5) 0.4068(4) 0.0329(16) Uani 1 1 d . . . N38 N 0.5854(5) 0.9991(6) 0.2723(4) 0.048(2) Uani 1 1 d . A . N41 N 0.5113(5) 1.1536(6) 0.2804(4) 0.045(2) Uani 1 1 d . . . N52 N 0.4036(11) 0.8103(11) 0.1707(14) 0.045(5) Uani 0.49(2) 1 d PD A 1 H52A H 0.3790 0.8407 0.1373 0.054 Uiso 0.49(2) 1 calc PR A 1 H52B H 0.3996 0.8351 0.2187 0.054 Uiso 0.49(2) 1 calc PR A 1 N52A N 0.4202(14) 0.7895(13) 0.1274(12) 0.061(6) Uani 0.51(2) 1 d PD A 2 H52C H 0.4689 0.7714 0.1138 0.073 Uiso 0.51(2) 1 calc PR A 2 H52D H 0.3904 0.8127 0.0895 0.073 Uiso 0.51(2) 1 calc PR A 2 N53 N -0.1243(5) 0.6484(5) 0.2918(4) 0.0419(18) Uani 1 1 d . B . N56 N -0.0718(5) 0.7678(5) 0.2121(4) 0.0382(18) Uani 1 1 d . . . H56A H -0.1209 0.7812 0.1783 0.046 Uiso 1 1 calc R . . H56B H -0.0116 0.8053 0.2172 0.046 Uiso 1 1 calc R . . N59 N -0.0928(5) 0.7780(5) 0.4334(4) 0.0452(19) Uani 1 1 d . . . H59A H -0.0318 0.8081 0.4726 0.054 Uiso 1 1 calc R . . H59B H -0.1382 0.8029 0.4456 0.054 Uiso 1 1 calc R . . N62 N -0.2411(5) 0.7617(6) 0.2716(5) 0.053(2) Uani 1 1 d D . . H62A H -0.2614 0.8028 0.3004 0.064 Uiso 0.38(3) 1 calc PR B 1 H62B H -0.2577 0.7647 0.2209 0.064 Uiso 0.38(3) 1 calc PR B 1 H62C H -0.2693 0.7647 0.3097 0.064 Uiso 0.62(3) 1 calc PR B 2 H62D H -0.2544 0.8028 0.2461 0.064 Uiso 0.62(3) 1 calc PR B 2 N63 N 0.2097(5) 0.5462(5) 0.0920(4) 0.046(2) Uani 1 1 d . A . N66 N 0.2917(7) 0.6388(6) 0.0051(5) 0.072(3) Uani 1 1 d . A . H66A H 0.2704 0.6803 -0.0160 0.087 Uiso 1 1 calc R . . H66B H 0.3510 0.6392 -0.0009 0.087 Uiso 1 1 calc R . . N69 N 0.4167(6) 0.6071(6) 0.1541(6) 0.074(3) Uani 1 1 d . A . H69A H 0.4698 0.6287 0.1399 0.089 Uiso 1 1 calc R . . H69B H 0.4396 0.6162 0.2076 0.089 Uiso 1 1 calc R . . N72 N 0.2894(7) 0.6891(6) 0.2320(5) 0.071(3) Uani 1 1 d . A . H72A H 0.3478 0.6991 0.2721 0.085 Uiso 1 1 calc R . . H72B H 0.2675 0.7376 0.2433 0.085 Uiso 1 1 calc R . . Ni1 Ni -0.08679(8) 0.78899(8) 0.32317(6) 0.0372(3) Uani 1 1 d . B . Ni2 Ni 0.31271(9) 0.67445(8) 0.12484(8) 0.0560(4) Uani 1 1 d D . . O1 O 0.2994(4) 0.9912(4) 0.1711(3) 0.0359(14) Uani 1 1 d . . . O2 O 0.2951(5) 1.0102(4) 0.0549(3) 0.0548(18) Uani 1 1 d . . . O3 O 0.1970(4) 1.1015(4) 0.2245(3) 0.0306(13) Uani 1 1 d . . . H3 H 0.1665 1.1273 0.2497 0.046 Uiso 1 1 d R . . O4 O 0.0763(4) 0.9261(4) 0.1619(3) 0.0332(13) Uani 1 1 d . . . H4 H 0.0430 0.9622 0.1645 0.050 Uiso 1 1 d R . . O5 O 0.2079(4) 0.8309(4) 0.1919(3) 0.0361(14) Uani 1 1 d . . . O6 O 0.1945(5) 0.7234(4) 0.0870(3) 0.0581(19) Uani 1 1 d . A . O7 O 0.1297(4) 0.8834(4) 0.3101(3) 0.0317(13) Uani 1 1 d . . . O8 O 0.0665(4) 0.7974(4) 0.3737(3) 0.0348(13) Uani 1 1 d . . . O9 O 0.3321(4) 0.9327(3) 0.3568(3) 0.0301(13) Uani 1 1 d . . . H9 H 0.3919 0.9671 0.3773 0.045 Uiso 1 1 d R . . O10 O 0.3765(4) 1.0968(4) 0.3384(3) 0.0322(13) Uani 1 1 d . . . H10 H 0.4158 1.0938 0.3133 0.048 Uiso 1 1 d R . . O11 O 0.2040(4) 1.0670(4) 0.3734(3) 0.0328(13) Uani 1 1 d . . . O12 O 0.2448(4) 1.1485(4) 0.4976(3) 0.0440(15) Uani 1 1 d . . . N100 N -0.3086(10) 0.7545(10) 0.0674(10) 0.139(5) Uani 1 1 d DU C 2 O101 O -0.2497(7) 0.8213(7) 0.1153(5) 0.104(3) Uani 1 1 d DU . . O102 O -0.2881(12) 0.6875(11) 0.0355(10) 0.216(7) Uani 1 1 d DU . . O103 O -0.3990(12) 0.7519(12) 0.0412(10) 0.232(8) Uani 1 1 d DU C 2 N200 N 0.6000(11) 1.4814(11) 0.3074(9) 0.146(6) Uani 1 1 d DU D 2 O202 O 0.6516(9) 1.4292(10) 0.3119(9) 0.176(6) Uani 1 1 d DU D 2 O203 O 0.5962(12) 1.5371(11) 0.3626(9) 0.222(8) Uani 1 1 d DU D 2 O201 O 0.5558(14) 1.4850(12) 0.2350(10) 0.251(9) Uani 1 1 d DU . . N300 N 0.0483(11) 0.4556(11) 0.2877(10) 0.078(6) Uani 0.533(15) 1 d PDU E 1 N30A N -0.0026(13) 0.4134(19) 0.2398(9) 0.100(8) Uani 0.467(15) 1 d PDU E 2 O300 O 0.1100(10) 0.5189(9) 0.3368(8) 0.084(6) Uani 0.533(15) 1 d PDU E 1 O30A O -0.0612(15) 0.3916(17) 0.1760(9) 0.132(9) Uani 0.467(15) 1 d PDU E 2 O301 O 0.0728(10) 0.4118(8) 0.2408(6) 0.133(4) Uani 1 1 d DU . . O302 O -0.0261(8) 0.4335(7) 0.2972(6) 0.111(3) Uani 1 1 d DU . . O900 O 0.7967(8) 1.2898(8) 0.3969(6) 0.126(4) Uani 1 1 d U . . O901 O 0.2971(8) 1.5011(6) 0.3800(6) 0.131(4) Uani 1 1 d U . . O902 O 0.2643(10) 1.4785(10) 0.5084(9) 0.178(5) Uani 1 1 d U F 1 O903 O -0.1360(5) 1.1661(5) 0.4632(4) 0.0637(19) Uani 1 1 d U . . O904 O -0.3404(14) 0.9334(12) 0.0580(9) 0.196(6) Uani 1 1 d U G 1 O905 O 0.533(2) 0.602(2) 0.0273(17) 0.178(11) Uani 0.50 1 d PU H 2 O906 O 0.0857(12) 0.5258(13) 0.4806(10) 0.213(7) Uani 1 1 d U I 1 O907 O 0.4530(8) 0.5963(8) 0.3253(5) 0.131(4) Uani 1 1 d U J 2 O908 O 0.6095(7) 0.7659(6) 0.3576(4) 0.089(3) Uani 1 1 d U . . O909 O 0.1274(5) 1.0054(4) 0.5202(3) 0.0472(16) Uani 1 1 d . . . O910 O 0.3137(7) 0.8481(6) 0.0011(5) 0.100(3) Uani 1 1 d U . . O911 O 0.4539(18) 0.823(2) -0.0502(15) 0.158(9) Uani 0.50 1 d PU K 1 O912 O 0.1755(13) 0.7173(11) -0.1335(8) 0.199(6) Uani 1 1 d U L 1 O913 O 0.3668(14) 0.6444(14) -0.1763(13) 0.253(8) Uani 1 1 d U M 1 O914 O 0.2179(14) 0.6755(14) -0.2528(11) 0.236(8) Uani 1 1 d U N 1 O921 O 0.566(2) 0.9122(18) 0.0162(15) 0.133(8) Uani 0.50 1 d PU O 2 O925 O 0.4485(12) 0.5898(16) -0.0654(13) 0.139(8) Uani 0.50 1 d PU P 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(5) 0.046(6) 0.034(5) 0.020(4) 0.013(4) 0.023(4) C2 0.038(5) 0.037(5) 0.030(4) 0.018(4) 0.003(4) 0.020(4) C3 0.028(4) 0.038(5) 0.026(4) 0.014(4) -0.001(4) 0.009(4) C4 0.028(4) 0.038(5) 0.025(4) 0.012(4) -0.001(4) 0.014(4) C5 0.037(5) 0.038(5) 0.035(5) 0.014(4) -0.001(4) 0.014(4) C6 0.033(5) 0.046(6) 0.040(5) 0.021(4) 0.008(4) 0.012(4) C7 0.030(5) 0.047(6) 0.038(5) 0.021(4) 0.008(4) 0.014(4) C8 0.033(5) 0.026(5) 0.033(5) 0.013(4) 0.002(4) 0.014(4) C10 0.043(5) 0.036(5) 0.051(5) 0.025(4) 0.015(4) 0.026(4) C11 0.045(5) 0.037(6) 0.052(6) 0.018(4) 0.021(5) 0.025(5) C13 0.034(5) 0.042(6) 0.060(6) 0.019(5) 0.025(4) 0.024(4) C14 0.038(5) 0.045(6) 0.050(6) 0.025(5) 0.015(4) 0.026(5) C16 0.031(5) 0.047(6) 0.032(5) 0.021(4) 0.005(4) 0.019(4) C17 0.033(4) 0.045(5) 0.035(5) 0.024(4) 0.013(4) 0.023(4) C18 0.036(5) 0.027(5) 0.030(4) 0.012(4) 0.005(4) 0.011(4) C19 0.039(5) 0.042(5) 0.028(4) 0.018(4) 0.008(4) 0.024(4) C20 0.035(5) 0.033(5) 0.035(5) 0.009(4) 0.004(4) 0.014(4) C21 0.047(5) 0.050(6) 0.027(4) 0.008(4) 0.007(4) 0.024(5) C22 0.028(5) 0.051(6) 0.028(5) 0.017(4) 0.004(4) 0.018(4) C23 0.034(5) 0.035(5) 0.033(5) 0.007(4) -0.001(4) 0.017(4) C24 0.044(5) 0.039(5) 0.045(5) 0.026(4) 0.023(4) 0.023(4) C25 0.042(5) 0.036(5) 0.047(5) 0.026(4) 0.021(4) 0.020(4) C27 0.032(5) 0.032(5) 0.041(5) 0.010(4) 0.011(4) 0.013(4) C28 0.034(5) 0.027(5) 0.032(4) 0.010(4) 0.011(4) 0.010(4) C29 0.036(5) 0.028(5) 0.021(4) 0.008(4) 0.010(3) 0.016(4) C30 0.027(4) 0.040(5) 0.024(4) 0.011(4) 0.008(3) 0.016(4) C31 0.037(5) 0.044(6) 0.024(4) 0.013(4) -0.001(4) 0.016(4) C32 0.041(5) 0.031(5) 0.040(5) 0.017(4) 0.009(4) 0.016(4) C33 0.039(5) 0.028(5) 0.034(5) 0.013(4) 0.011(4) 0.011(4) C34 0.040(5) 0.051(6) 0.027(4) 0.017(4) 0.009(4) 0.023(5) C36 0.030(5) 0.056(6) 0.039(5) 0.022(4) 0.014(4) 0.018(4) C37 0.034(5) 0.076(7) 0.033(5) 0.021(5) 0.010(4) 0.024(5) C39 0.033(5) 0.081(8) 0.046(6) 0.024(5) 0.020(4) 0.022(5) C40 0.055(6) 0.100(9) 0.069(7) 0.056(7) 0.034(6) 0.046(6) C42 0.040(5) 0.053(7) 0.035(5) 0.023(5) -0.002(4) 0.013(5) C43 0.037(5) 0.040(6) 0.033(5) 0.028(4) 0.006(4) 0.009(4) C44 0.030(4) 0.037(5) 0.021(4) 0.014(4) 0.000(3) 0.014(4) C45 0.030(4) 0.032(5) 0.029(4) 0.018(4) 0.002(4) 0.009(4) C46 0.047(5) 0.039(6) 0.035(5) 0.017(4) 0.000(4) 0.017(5) C47 0.053(6) 0.032(6) 0.046(6) 0.018(4) -0.001(5) 0.011(5) C48 0.035(5) 0.041(6) 0.050(6) 0.031(5) 0.002(4) 0.003(4) C49 0.033(5) 0.040(6) 0.035(5) 0.017(4) 0.015(4) 0.023(4) C50 0.084(9) 0.092(10) 0.051(7) 0.045(7) 0.001(6) -0.018(8) C51 0.036(11) 0.086(17) 0.026(10) 0.015(10) 0.008(8) 0.045(11) C51A 0.056(15) 0.043(15) 0.054(14) 0.029(11) 0.031(12) 0.029(12) C54 0.038(5) 0.034(5) 0.044(5) 0.012(4) 0.013(4) 0.003(4) C55 0.050(6) 0.051(7) 0.044(6) 0.015(5) 0.012(5) 0.010(5) C57 0.064(6) 0.044(6) 0.053(6) 0.028(5) 0.027(5) 0.031(5) C58 0.071(7) 0.062(7) 0.077(7) 0.040(6) 0.046(6) 0.036(6) C60 0.038(5) 0.055(7) 0.070(7) 0.029(5) 0.017(5) 0.009(5) C61 0.07(2) 0.09(3) 0.08(3) 0.04(2) 0.030(19) 0.03(2) C61A 0.041(10) 0.049(12) 0.071(14) 0.022(10) -0.005(9) 0.010(8) C64 0.064(7) 0.040(6) 0.057(6) 0.000(5) 0.010(6) 0.022(5) C65 0.105(10) 0.062(8) 0.059(7) 0.014(6) 0.032(7) 0.044(7) C67 0.083(8) 0.046(7) 0.063(7) 0.019(5) 0.017(6) 0.033(6) C68 0.092(10) 0.063(9) 0.157(13) 0.034(9) 0.032(9) 0.060(8) C70 0.075(7) 0.070(8) 0.051(6) 0.020(5) 0.025(6) 0.041(6) C71 0.111(11) 0.105(11) 0.047(7) 0.020(7) 0.023(7) 0.074(10) Dy1 0.0278(2) 0.0286(2) 0.0269(2) 0.01176(17) 0.00640(16) 0.01511(17) N9 0.033(4) 0.035(4) 0.036(4) 0.015(3) 0.011(3) 0.015(3) N12 0.037(4) 0.033(4) 0.043(4) 0.021(3) 0.018(3) 0.021(3) N15 0.041(4) 0.038(4) 0.036(4) 0.020(4) 0.019(3) 0.023(4) N26 0.046(4) 0.043(5) 0.048(4) 0.029(4) 0.023(4) 0.025(4) N35 0.033(4) 0.039(4) 0.030(4) 0.013(3) 0.014(3) 0.013(3) N38 0.033(4) 0.086(7) 0.035(4) 0.033(4) 0.012(3) 0.023(4) N41 0.028(4) 0.076(6) 0.035(4) 0.030(4) 0.007(3) 0.017(4) N52 0.058(13) 0.056(14) 0.029(12) 0.019(10) 0.012(10) 0.033(11) N52A 0.076(14) 0.066(14) 0.032(12) 0.020(10) 0.005(10) 0.018(11) N53 0.036(4) 0.047(5) 0.053(5) 0.024(4) 0.023(4) 0.016(4) N56 0.029(4) 0.034(4) 0.058(5) 0.023(4) 0.016(3) 0.012(3) N59 0.045(4) 0.044(5) 0.066(5) 0.032(4) 0.031(4) 0.023(4) N62 0.054(5) 0.059(6) 0.064(5) 0.036(5) 0.029(4) 0.024(4) N63 0.047(5) 0.048(5) 0.042(4) 0.009(4) 0.007(4) 0.028(4) N66 0.088(7) 0.069(7) 0.097(7) 0.045(6) 0.045(6) 0.057(6) N69 0.049(5) 0.073(7) 0.110(7) 0.045(6) 0.012(5) 0.038(5) N72 0.088(7) 0.055(6) 0.049(5) 0.005(5) -0.014(5) 0.043(6) Ni1 0.0361(6) 0.0402(7) 0.0477(7) 0.0239(6) 0.0197(5) 0.0189(6) Ni2 0.0452(7) 0.0437(8) 0.0640(8) 0.0142(7) -0.0085(6) 0.0247(6) O1 0.038(3) 0.045(4) 0.034(3) 0.020(3) 0.010(3) 0.025(3) O2 0.084(5) 0.061(5) 0.034(4) 0.024(3) 0.022(3) 0.039(4) O3 0.031(3) 0.036(3) 0.036(3) 0.017(3) 0.016(3) 0.021(3) O4 0.029(3) 0.032(3) 0.042(3) 0.017(3) 0.008(3) 0.017(3) O5 0.041(3) 0.031(3) 0.029(3) 0.003(3) -0.001(3) 0.020(3) O6 0.057(4) 0.055(4) 0.047(4) 0.000(3) -0.010(3) 0.041(4) O7 0.036(3) 0.033(3) 0.031(3) 0.016(3) 0.006(2) 0.020(3) O8 0.030(3) 0.038(4) 0.040(3) 0.016(3) 0.014(3) 0.011(3) O9 0.022(3) 0.034(3) 0.033(3) 0.016(3) 0.004(2) 0.009(2) O10 0.033(3) 0.039(4) 0.032(3) 0.013(3) 0.014(2) 0.020(3) O11 0.031(3) 0.036(4) 0.040(3) 0.018(3) 0.017(3) 0.013(3) O12 0.061(4) 0.045(4) 0.033(3) 0.016(3) 0.022(3) 0.020(3) N100 0.140(9) 0.129(9) 0.159(10) 0.044(7) 0.057(8) 0.059(8) O101 0.114(7) 0.123(8) 0.065(5) 0.024(5) 0.016(5) 0.047(6) O102 0.245(14) 0.198(13) 0.234(14) 0.058(11) 0.087(11) 0.128(12) O103 0.195(12) 0.276(16) 0.229(14) 0.054(11) 0.024(10) 0.168(12) N200 0.126(9) 0.142(9) 0.174(10) 0.080(8) 0.034(7) 0.044(7) O202 0.133(9) 0.181(11) 0.280(14) 0.153(11) 0.079(9) 0.086(9) O203 0.222(14) 0.198(13) 0.194(12) -0.020(10) 0.123(11) -0.012(10) O201 0.229(15) 0.276(16) 0.223(14) 0.150(13) 0.016(11) 0.050(12) N300 0.070(9) 0.080(9) 0.106(10) 0.044(7) 0.036(7) 0.043(7) N30A 0.095(11) 0.095(11) 0.115(11) 0.042(9) 0.029(8) 0.041(8) O300 0.074(10) 0.053(9) 0.094(10) 0.010(7) -0.003(8) 0.019(7) O30A 0.157(16) 0.149(17) 0.083(12) 0.019(11) 0.014(11) 0.091(14) O301 0.180(8) 0.109(7) 0.135(7) 0.051(5) 0.078(6) 0.051(6) O302 0.131(7) 0.107(6) 0.099(6) 0.022(5) 0.036(5) 0.065(6) O900 0.148(8) 0.144(9) 0.142(8) 0.073(7) 0.072(7) 0.092(7) O901 0.148(8) 0.057(6) 0.130(8) 0.000(5) -0.021(6) 0.047(6) O902 0.145(10) 0.157(11) 0.195(11) 0.056(9) 0.047(9) -0.005(8) O903 0.087(5) 0.057(5) 0.065(4) 0.028(4) 0.043(4) 0.028(4) O904 0.201(13) 0.217(13) 0.142(10) 0.040(9) 0.081(10) 0.006(11) O905 0.157(16) 0.201(19) 0.182(17) 0.027(13) 0.134(15) 0.010(13) O906 0.210(12) 0.299(15) 0.217(13) 0.138(11) 0.092(10) 0.162(12) O907 0.140(8) 0.164(9) 0.045(5) 0.008(5) -0.001(5) 0.032(7) O908 0.121(7) 0.108(7) 0.037(4) 0.024(4) 0.019(4) 0.044(5) O909 0.060(4) 0.048(4) 0.035(3) 0.013(3) 0.018(3) 0.020(3) O910 0.155(8) 0.088(6) 0.077(5) 0.034(5) 0.031(5) 0.077(6) O911 0.136(15) 0.212(19) 0.163(16) 0.078(14) 0.099(13) 0.047(13) O912 0.246(14) 0.198(12) 0.128(9) 0.043(8) 0.004(9) 0.113(11) O913 0.195(13) 0.232(15) 0.318(17) 0.131(13) 0.075(12) 0.025(11) O914 0.241(15) 0.270(16) 0.234(14) 0.120(12) 0.086(12) 0.109(12) O921 0.137(15) 0.148(16) 0.142(15) 0.047(12) 0.079(13) 0.060(13) O925 0.052(9) 0.185(16) 0.134(14) -0.028(11) 0.071(10) -0.017(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.265(10) . ? C1 O1 1.281(9) . ? C1 C2 1.489(12) . ? C2 C7 1.387(12) . ? C2 C3 1.425(12) . ? C3 O3 1.308(9) . ? C3 C4 1.413(11) . ? C4 C8 1.412(11) . ? C4 C5 1.421(12) . ? C5 C6 1.351(12) . ? C5 H5 0.9500 . ? C6 C7 1.396(12) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N9 1.301(10) . ? C8 H8 0.9500 . ? C10 N9 1.452(11) . ? C10 C11 1.531(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N12 1.453(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 N12 1.467(10) . ? C13 C14 1.498(12) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N15 1.494(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C16 N15 1.279(10) . ? C16 C17 1.425(11) . ? C16 H16 0.9500 . ? C17 C22 1.403(11) . ? C17 C18 1.433(10) . ? C18 O4 1.294(9) . ? C18 C19 1.407(11) . ? C19 C20 1.390(11) . ? C19 C23 1.515(10) . ? C20 C21 1.407(10) . ? C20 H20 0.9500 . ? C21 C22 1.375(11) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 O6 1.249(9) . ? C23 O5 1.277(9) . ? C24 N12 1.495(10) . ? C24 C25 1.521(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N26 1.482(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 O8 1.255(10) . ? C27 O7 1.273(10) . ? C27 C28 1.508(11) . ? C28 C33 1.393(11) . ? C28 C29 1.420(11) . ? C29 O9 1.279(9) . ? C29 C30 1.430(10) . ? C30 C31 1.412(11) . ? C30 C34 1.425(12) . ? C31 C32 1.341(12) . ? C31 H31 0.9500 . ? C32 C33 1.399(11) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N35 1.321(10) . ? C34 H34 0.9500 . ? C36 N35 1.473(10) . ? C36 C37 1.508(12) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 N38 1.480(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C39 N38 1.476(12) . ? C39 C40 1.498(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N41 1.457(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C42 N41 1.295(11) . ? C42 C43 1.413(13) . ? C42 H42 0.9500 . ? C43 C48 1.401(12) . ? C43 C44 1.427(12) . ? C44 O10 1.303(9) . ? C44 C45 1.417(11) . ? C45 C46 1.391(11) . ? C45 C49 1.492(12) . ? C46 C47 1.400(13) . ? C46 H46 0.9500 . ? C47 C48 1.343(13) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O11 1.265(9) . ? C49 O12 1.268(9) . ? C50 N38 1.445(14) . ? C50 C51A 1.60(2) . ? C50 C51 1.600(19) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C50 H50C 0.9900 . ? C50 H50D 0.9900 . ? C51 N52 1.474(17) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C51A N52A 1.457(18) . ? C51A H51C 0.9900 . ? C51A H51D 0.9900 . ? C54 N53 1.477(11) . ? C54 C55 1.525(12) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 N56 1.473(11) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C57 N53 1.493(11) . ? C57 C58 1.511(13) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 N59 1.505(12) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C60 N53 1.484(11) . ? C60 C61 1.51(2) . ? C60 C61A 1.518(16) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C60 H60C 0.9900 . ? C60 H60D 0.9900 . ? C61 N62 1.54(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C61A N62 1.541(16) . ? C61A H61C 0.9900 . ? C61A H61D 0.9900 . ? C64 C65 1.478(15) . ? C64 N63 1.485(11) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N66 1.506(14) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C67 C68 1.484(17) . ? C67 N63 1.501(11) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 N69 1.458(14) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C70 N63 1.477(12) . ? C70 C71 1.522(14) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 N72 1.448(16) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? Dy1 O4 2.311(5) . ? Dy1 O7 2.316(6) . ? Dy1 O1 2.321(5) . ? Dy1 O9 2.332(5) . ? Dy1 O10 2.357(5) . ? Dy1 O5 2.362(5) . ? Dy1 O3 2.365(5) . ? Dy1 O11 2.368(5) . ? N26 Ni1 2.052(7) . ? N26 H26A 0.9200 . ? N26 H26B 0.9200 . ? N52 Ni2 2.112(16) . ? N52 H52A 0.9200 . ? N52 H52B 0.9200 . ? N52A Ni2 2.124(15) . ? N52A H52C 0.9200 . ? N52A H52D 0.9200 . ? N53 Ni1 2.100(7) . ? N56 Ni1 2.105(7) . ? N56 H56A 0.9200 . ? N56 H56B 0.9200 . ? N59 Ni1 2.123(7) . ? N59 H59A 0.9200 . ? N59 H59B 0.9200 . ? N62 Ni1 2.111(7) . ? N62 H62A 0.9200 . ? N62 H62B 0.9200 . ? N62 H62C 0.9200 . ? N62 H62D 0.9200 . ? N63 Ni2 2.098(8) . ? N66 Ni2 2.084(9) . ? N66 H66A 0.9200 . ? N66 H66B 0.9200 . ? N69 Ni2 2.104(7) . ? N69 H69A 0.9200 . ? N69 H69B 0.9200 . ? N72 Ni2 2.093(10) . ? N72 H72A 0.9200 . ? N72 H72B 0.9200 . ? Ni1 O8 2.160(5) . ? Ni2 O6 2.095(5) . ? O3 H3 0.8507 . ? O4 H4 0.8501 . ? O9 H9 0.8504 . ? O10 H10 0.8501 . ? N100 O101 1.184(12) . ? N100 O102 1.260(13) . ? N100 O103 1.278(13) . ? N200 O203 1.231(13) . ? N200 O202 1.264(12) . ? N200 O201 1.339(13) . ? N300 O302 1.158(12) . ? N300 O300 1.175(13) . ? N300 O301 1.194(12) . ? N30A O301 1.123(13) . ? N30A O30A 1.170(14) . ? N30A O302 1.219(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 122.6(8) . . ? O2 C1 C2 118.3(7) . . ? O1 C1 C2 119.1(7) . . ? C7 C2 C3 119.1(8) . . ? C7 C2 C1 119.6(8) . . ? C3 C2 C1 121.2(8) . . ? O3 C3 C4 120.1(8) . . ? O3 C3 C2 121.2(8) . . ? C4 C3 C2 118.6(8) . . ? C8 C4 C3 122.7(8) . . ? C8 C4 C5 118.4(8) . . ? C3 C4 C5 118.8(8) . . ? C6 C5 C4 122.5(8) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C7 118.3(9) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C2 C7 C6 122.4(9) . . ? C2 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? N9 C8 C4 121.2(8) . . ? N9 C8 H8 119.4 . . ? C4 C8 H8 119.4 . . ? N9 C10 C11 108.9(7) . . ? N9 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N9 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N12 C11 C10 112.2(6) . . ? N12 C11 H11A 109.2 . . ? C10 C11 H11A 109.2 . . ? N12 C11 H11B 109.2 . . ? C10 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N12 C13 C14 110.3(7) . . ? N12 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N12 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N15 C14 C13 109.7(7) . . ? N15 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? N15 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? N15 C16 C17 126.2(7) . . ? N15 C16 H16 116.9 . . ? C17 C16 H16 116.9 . . ? C22 C17 C16 117.0(7) . . ? C22 C17 C18 121.1(7) . . ? C16 C17 C18 121.9(7) . . ? O4 C18 C19 123.9(7) . . ? O4 C18 C17 119.4(7) . . ? C19 C18 C17 116.7(7) . . ? C20 C19 C18 120.6(7) . . ? C20 C19 C23 115.1(7) . . ? C18 C19 C23 124.3(7) . . ? C19 C20 C21 122.4(7) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C22 C21 C20 117.7(7) . . ? C22 C21 H21 121.2 . . ? C20 C21 H21 121.2 . . ? C21 C22 C17 121.4(7) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? O6 C23 O5 123.9(7) . . ? O6 C23 C19 116.5(7) . . ? O5 C23 C19 119.6(7) . . ? N12 C24 C25 112.1(7) . . ? N12 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N12 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N26 C25 C24 111.8(7) . . ? N26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? N26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? O8 C27 O7 123.4(7) . . ? O8 C27 C28 117.1(7) . . ? O7 C27 C28 119.5(8) . . ? C33 C28 C29 119.6(7) . . ? C33 C28 C27 118.0(7) . . ? C29 C28 C27 122.4(7) . . ? O9 C29 C28 124.1(7) . . ? O9 C29 C30 119.1(7) . . ? C28 C29 C30 116.8(7) . . ? C31 C30 C34 117.4(7) . . ? C31 C30 C29 121.3(7) . . ? C34 C30 C29 121.3(7) . . ? C32 C31 C30 120.4(7) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 120.0(8) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C28 C33 C32 121.9(8) . . ? C28 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? N35 C34 C30 125.5(7) . . ? N35 C34 H34 117.2 . . ? C30 C34 H34 117.2 . . ? N35 C36 C37 110.7(7) . . ? N35 C36 H36A 109.5 . . ? C37 C36 H36A 109.5 . . ? N35 C36 H36B 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? N38 C37 C36 111.1(7) . . ? N38 C37 H37A 109.4 . . ? C36 C37 H37A 109.4 . . ? N38 C37 H37B 109.4 . . ? C36 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? N38 C39 C40 112.8(8) . . ? N38 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? N38 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? N41 C40 C39 110.4(8) . . ? N41 C40 H40A 109.6 . . ? C39 C40 H40A 109.6 . . ? N41 C40 H40B 109.6 . . ? C39 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? N41 C42 C43 125.3(10) . . ? N41 C42 H42 117.3 . . ? C43 C42 H42 117.3 . . ? C48 C43 C42 119.2(9) . . ? C48 C43 C44 120.9(9) . . ? C42 C43 C44 119.9(9) . . ? O10 C44 C45 120.6(8) . . ? O10 C44 C43 121.7(8) . . ? C45 C44 C43 117.6(8) . . ? C46 C45 C44 119.3(8) . . ? C46 C45 C49 118.2(8) . . ? C44 C45 C49 122.5(7) . . ? C45 C46 C47 121.5(9) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C48 C47 C46 120.3(9) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C43 120.5(9) . . ? C47 C48 H48 119.8 . . ? C43 C48 H48 119.8 . . ? O11 C49 O12 122.1(8) . . ? O11 C49 C45 120.0(7) . . ? O12 C49 C45 117.9(8) . . ? N38 C50 C51A 98.3(11) . . ? N38 C50 C51 125.2(10) . . ? C51A C50 C51 38.3(9) . . ? N38 C50 H50A 106.0 . . ? C51A C50 H50A 144.2 . . ? C51 C50 H50A 106.0 . . ? N38 C50 H50B 106.0 . . ? C51A C50 H50B 91.4 . . ? C51 C50 H50B 106.0 . . ? H50A C50 H50B 106.3 . . ? N38 C50 H50C 112.1 . . ? C51A C50 H50C 112.1 . . ? C51 C50 H50C 76.1 . . ? H50A C50 H50C 33.9 . . ? H50B C50 H50C 130.7 . . ? N38 C50 H50D 112.1 . . ? C51A C50 H50D 112.1 . . ? C51 C50 H50D 115.1 . . ? H50A C50 H50D 82.7 . . ? H50B C50 H50D 23.6 . . ? H50C C50 H50D 109.7 . . ? N52 C51 C50 107.6(12) . . ? N52 C51 H51A 110.2 . . ? C50 C51 H51A 110.2 . . ? N52 C51 H51B 110.2 . . ? C50 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? N52A C51A C50 107.8(12) . . ? N52A C51A H51C 110.1 . . ? C50 C51A H51C 110.1 . . ? N52A C51A H51D 110.1 . . ? C50 C51A H51D 110.1 . . ? H51C C51A H51D 108.5 . . ? N53 C54 C55 110.7(7) . . ? N53 C54 H54A 109.5 . . ? C55 C54 H54A 109.5 . . ? N53 C54 H54B 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? N56 C55 C54 111.4(7) . . ? N56 C55 H55A 109.3 . . ? C54 C55 H55A 109.3 . . ? N56 C55 H55B 109.3 . . ? C54 C55 H55B 109.3 . . ? H55A C55 H55B 108.0 . . ? N53 C57 C58 109.5(7) . . ? N53 C57 H57A 109.8 . . ? C58 C57 H57A 109.8 . . ? N53 C57 H57B 109.8 . . ? C58 C57 H57B 109.8 . . ? H57A C57 H57B 108.2 . . ? N59 C58 C57 111.1(8) . . ? N59 C58 H58A 109.4 . . ? C57 C58 H58A 109.4 . . ? N59 C58 H58B 109.4 . . ? C57 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? N53 C60 C61 112.4(15) . . ? N53 C60 C61A 113.3(9) . . ? C61 C60 C61A 44.3(13) . . ? N53 C60 H60A 109.1 . . ? C61 C60 H60A 109.1 . . ? C61A C60 H60A 136.4 . . ? N53 C60 H60B 109.1 . . ? C61 C60 H60B 109.1 . . ? C61A C60 H60B 67.3 . . ? H60A C60 H60B 107.9 . . ? N53 C60 H60C 108.9 . . ? C61 C60 H60C 67.7 . . ? C61A C60 H60C 108.9 . . ? H60A C60 H60C 45.4 . . ? H60B C60 H60C 139.5 . . ? N53 C60 H60D 108.9 . . ? C61 C60 H60D 137.5 . . ? C61A C60 H60D 108.9 . . ? H60A C60 H60D 64.8 . . ? H60B C60 H60D 45.7 . . ? H60C C60 H60D 107.7 . . ? C60 C61 N62 109.6(14) . . ? C60 C61 H61A 109.7 . . ? N62 C61 H61A 109.7 . . ? C60 C61 H61B 109.7 . . ? N62 C61 H61B 109.7 . . ? H61A C61 H61B 108.2 . . ? C60 C61A N62 109.1(10) . . ? C60 C61A H61C 109.9 . . ? N62 C61A H61C 109.9 . . ? C60 C61A H61D 109.9 . . ? N62 C61A H61D 109.9 . . ? H61C C61A H61D 108.3 . . ? C65 C64 N63 112.5(9) . . ? C65 C64 H64A 109.1 . . ? N63 C64 H64A 109.1 . . ? C65 C64 H64B 109.1 . . ? N63 C64 H64B 109.1 . . ? H64A C64 H64B 107.8 . . ? C64 C65 N66 108.9(9) . . ? C64 C65 H65A 109.9 . . ? N66 C65 H65A 109.9 . . ? C64 C65 H65B 109.9 . . ? N66 C65 H65B 109.9 . . ? H65A C65 H65B 108.3 . . ? C68 C67 N63 112.8(9) . . ? C68 C67 H67A 109.0 . . ? N63 C67 H67A 109.0 . . ? C68 C67 H67B 109.0 . . ? N63 C67 H67B 109.0 . . ? H67A C67 H67B 107.8 . . ? N69 C68 C67 113.4(10) . . ? N69 C68 H68A 108.9 . . ? C67 C68 H68A 108.9 . . ? N69 C68 H68B 108.9 . . ? C67 C68 H68B 108.9 . . ? H68A C68 H68B 107.7 . . ? N63 C70 C71 108.5(9) . . ? N63 C70 H70A 110.0 . . ? C71 C70 H70A 110.0 . . ? N63 C70 H70B 110.0 . . ? C71 C70 H70B 110.0 . . ? H70A C70 H70B 108.4 . . ? N72 C71 C70 113.4(10) . . ? N72 C71 H71A 108.9 . . ? C70 C71 H71A 108.9 . . ? N72 C71 H71B 108.9 . . ? C70 C71 H71B 108.9 . . ? H71A C71 H71B 107.7 . . ? O4 Dy1 O7 78.31(18) . . ? O4 Dy1 O1 86.67(18) . . ? O7 Dy1 O1 147.00(19) . . ? O4 Dy1 O9 142.40(18) . . ? O7 Dy1 O9 72.28(17) . . ? O1 Dy1 O9 105.63(17) . . ? O4 Dy1 O10 147.43(18) . . ? O7 Dy1 O10 128.49(17) . . ? O1 Dy1 O10 77.59(19) . . ? O9 Dy1 O10 69.98(17) . . ? O4 Dy1 O5 72.51(17) . . ? O7 Dy1 O5 74.55(19) . . ? O1 Dy1 O5 72.9(2) . . ? O9 Dy1 O5 77.39(17) . . ? O10 Dy1 O5 127.47(18) . . ? O4 Dy1 O3 71.77(18) . . ? O7 Dy1 O3 127.28(17) . . ? O1 Dy1 O3 73.35(18) . . ? O9 Dy1 O3 145.61(18) . . ? O10 Dy1 O3 76.43(17) . . ? O5 Dy1 O3 131.55(17) . . ? O4 Dy1 O11 106.08(18) . . ? O7 Dy1 O11 71.65(18) . . ? O1 Dy1 O11 141.25(19) . . ? O9 Dy1 O11 86.52(17) . . ? O10 Dy1 O11 72.31(18) . . ? O5 Dy1 O11 145.62(19) . . ? O3 Dy1 O11 76.28(17) . . ? C8 N9 C10 124.9(7) . . ? C11 N12 C13 111.5(6) . . ? C11 N12 C24 111.5(7) . . ? C13 N12 C24 113.3(7) . . ? C16 N15 C14 123.6(7) . . ? C25 N26 Ni1 118.3(5) . . ? C25 N26 H26A 107.7 . . ? Ni1 N26 H26A 107.7 . . ? C25 N26 H26B 107.7 . . ? Ni1 N26 H26B 107.7 . . ? H26A N26 H26B 107.1 . . ? C34 N35 C36 121.2(7) . . ? C50 N38 C39 108.7(7) . . ? C50 N38 C37 112.6(8) . . ? C39 N38 C37 110.3(7) . . ? C42 N41 C40 126.1(9) . . ? C51 N52 Ni2 115.1(11) . . ? C51 N52 H52A 108.5 . . ? Ni2 N52 H52A 108.5 . . ? C51 N52 H52B 108.5 . . ? Ni2 N52 H52B 108.5 . . ? H52A N52 H52B 107.5 . . ? C51A N52A Ni2 115.5(14) . . ? C51A N52A H52C 108.4 . . ? Ni2 N52A H52C 108.4 . . ? C51A N52A H52D 108.4 . . ? Ni2 N52A H52D 108.4 . . ? H52C N52A H52D 107.5 . . ? C54 N53 C60 112.7(7) . . ? C54 N53 C57 111.5(6) . . ? C60 N53 C57 111.0(7) . . ? C54 N53 Ni1 104.5(5) . . ? C60 N53 Ni1 110.4(5) . . ? C57 N53 Ni1 106.3(5) . . ? C55 N56 Ni1 110.4(5) . . ? C55 N56 H56A 109.6 . . ? Ni1 N56 H56A 109.6 . . ? C55 N56 H56B 109.6 . . ? Ni1 N56 H56B 109.6 . . ? H56A N56 H56B 108.1 . . ? C58 N59 Ni1 108.3(5) . . ? C58 N59 H59A 110.0 . . ? Ni1 N59 H59A 110.0 . . ? C58 N59 H59B 110.0 . . ? Ni1 N59 H59B 110.0 . . ? H59A N59 H59B 108.4 . . ? C61 N62 C61A 43.5(12) . . ? C61 N62 Ni1 106.6(12) . . ? C61A N62 Ni1 106.4(7) . . ? C61 N62 H62A 110.4 . . ? C61A N62 H62A 140.5 . . ? Ni1 N62 H62A 110.4 . . ? C61 N62 H62B 110.4 . . ? C61A N62 H62B 70.2 . . ? Ni1 N62 H62B 110.4 . . ? H62A N62 H62B 108.6 . . ? C61 N62 H62C 70.1 . . ? C61A N62 H62C 110.5 . . ? Ni1 N62 H62C 110.5 . . ? H62A N62 H62C 42.5 . . ? H62B N62 H62C 136.8 . . ? C61 N62 H62D 140.3 . . ? C61A N62 H62D 110.5 . . ? Ni1 N62 H62D 110.5 . . ? H62A N62 H62D 69.3 . . ? H62B N62 H62D 42.4 . . ? H62C N62 H62D 108.6 . . ? C70 N63 C64 112.5(7) . . ? C70 N63 C67 111.7(8) . . ? C64 N63 C67 111.6(7) . . ? C70 N63 Ni2 105.9(6) . . ? C64 N63 Ni2 104.9(6) . . ? C67 N63 Ni2 109.7(6) . . ? C65 N66 Ni2 111.1(7) . . ? C65 N66 H66A 109.4 . . ? Ni2 N66 H66A 109.4 . . ? C65 N66 H66B 109.4 . . ? Ni2 N66 H66B 109.4 . . ? H66A N66 H66B 108.0 . . ? C68 N69 Ni2 107.9(6) . . ? C68 N69 H69A 110.1 . . ? Ni2 N69 H69A 110.1 . . ? C68 N69 H69B 110.1 . . ? Ni2 N69 H69B 110.1 . . ? H69A N69 H69B 108.4 . . ? C71 N72 Ni2 109.0(6) . . ? C71 N72 H72A 109.9 . . ? Ni2 N72 H72A 109.9 . . ? C71 N72 H72B 109.9 . . ? Ni2 N72 H72B 109.9 . . ? H72A N72 H72B 108.3 . . ? N26 Ni1 N53 178.7(3) . . ? N26 Ni1 N56 98.6(3) . . ? N53 Ni1 N56 82.7(3) . . ? N26 Ni1 N62 96.4(3) . . ? N53 Ni1 N62 83.8(3) . . ? N56 Ni1 N62 91.6(3) . . ? N26 Ni1 N59 95.1(3) . . ? N53 Ni1 N59 83.6(3) . . ? N56 Ni1 N59 164.7(3) . . ? N62 Ni1 N59 93.8(3) . . ? N26 Ni1 O8 91.3(2) . . ? N53 Ni1 O8 88.4(2) . . ? N56 Ni1 O8 88.4(2) . . ? N62 Ni1 O8 172.2(3) . . ? N59 Ni1 O8 84.4(2) . . ? N66 Ni2 N72 163.1(4) . . ? N66 Ni2 O6 82.3(3) . . ? N72 Ni2 O6 87.5(3) . . ? N66 Ni2 N63 82.9(3) . . ? N72 Ni2 N63 83.4(4) . . ? O6 Ni2 N63 88.7(3) . . ? N66 Ni2 N69 94.7(4) . . ? N72 Ni2 N69 93.5(4) . . ? O6 Ni2 N69 171.9(3) . . ? N63 Ni2 N69 83.4(3) . . ? N66 Ni2 N52 104.6(7) . . ? N72 Ni2 N52 88.0(7) . . ? O6 Ni2 N52 86.2(4) . . ? N63 Ni2 N52 170.2(6) . . ? N69 Ni2 N52 101.9(5) . . ? N66 Ni2 N52A 81.8(7) . . ? N72 Ni2 N52A 112.3(7) . . ? O6 Ni2 N52A 93.8(6) . . ? N63 Ni2 N52A 164.1(7) . . ? N69 Ni2 N52A 93.3(7) . . ? N52 Ni2 N52A 25.2(6) . . ? C1 O1 Dy1 134.3(5) . . ? C3 O3 Dy1 129.2(4) . . ? C3 O3 H3 108.8 . . ? Dy1 O3 H3 112.1 . . ? C18 O4 Dy1 136.2(5) . . ? C18 O4 H4 109.1 . . ? Dy1 O4 H4 112.6 . . ? C23 O5 Dy1 135.0(5) . . ? C23 O6 Ni2 134.3(5) . . ? C27 O7 Dy1 140.7(5) . . ? C27 O8 Ni1 126.7(5) . . ? C29 O9 Dy1 136.2(5) . . ? C29 O9 H9 109.1 . . ? Dy1 O9 H9 114.7 . . ? C44 O10 Dy1 131.0(5) . . ? C44 O10 H10 109.5 . . ? Dy1 O10 H10 107.8 . . ? C49 O11 Dy1 135.1(5) . . ? O101 N100 O102 124.8(13) . . ? O101 N100 O103 118.3(12) . . ? O102 N100 O103 116.7(12) . . ? O203 N200 O202 126.9(13) . . ? O203 N200 O201 116.3(12) . . ? O202 N200 O201 116.1(12) . . ? O302 N300 O300 116.0(13) . . ? O302 N300 O301 125.3(14) . . ? O300 N300 O301 117.4(13) . . ? O301 N30A O30A 113.3(14) . . ? O301 N30A O302 126.2(14) . . ? O30A N30A O302 120.5(14) . . ? N30A O301 N300 49.1(13) . . ? N300 O302 N30A 47.8(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -40.0(11) . . . . ? O1 C1 C2 C7 141.3(8) . . . . ? O2 C1 C2 C3 141.1(8) . . . . ? O1 C1 C2 C3 -37.7(11) . . . . ? C7 C2 C3 O3 177.9(6) . . . . ? C1 C2 C3 O3 -3.1(10) . . . . ? C7 C2 C3 C4 -1.0(10) . . . . ? C1 C2 C3 C4 177.9(6) . . . . ? O3 C3 C4 C8 0.7(10) . . . . ? C2 C3 C4 C8 179.6(6) . . . . ? O3 C3 C4 C5 179.3(6) . . . . ? C2 C3 C4 C5 -1.7(10) . . . . ? C8 C4 C5 C6 -179.6(7) . . . . ? C3 C4 C5 C6 1.7(10) . . . . ? C4 C5 C6 C7 1.1(11) . . . . ? C3 C2 C7 C6 4.0(11) . . . . ? C1 C2 C7 C6 -175.0(7) . . . . ? C5 C6 C7 C2 -4.0(11) . . . . ? C3 C4 C8 N9 -2.2(11) . . . . ? C5 C4 C8 N9 179.1(6) . . . . ? N9 C10 C11 N12 53.0(9) . . . . ? N12 C13 C14 N15 68.7(9) . . . . ? N15 C16 C17 C22 -173.6(8) . . . . ? N15 C16 C17 C18 4.5(14) . . . . ? C22 C17 C18 O4 -176.8(8) . . . . ? C16 C17 C18 O4 5.2(12) . . . . ? C22 C17 C18 C19 3.8(12) . . . . ? C16 C17 C18 C19 -174.2(8) . . . . ? O4 C18 C19 C20 179.4(8) . . . . ? C17 C18 C19 C20 -1.3(12) . . . . ? O4 C18 C19 C23 0.1(14) . . . . ? C17 C18 C19 C23 179.5(8) . . . . ? C18 C19 C20 C21 -1.2(13) . . . . ? C23 C19 C20 C21 178.1(8) . . . . ? C19 C20 C21 C22 1.3(13) . . . . ? C20 C21 C22 C17 1.3(13) . . . . ? C16 C17 C22 C21 174.2(8) . . . . ? C18 C17 C22 C21 -4.0(13) . . . . ? C20 C19 C23 O6 5.5(12) . . . . ? C18 C19 C23 O6 -175.2(9) . . . . ? C20 C19 C23 O5 -173.2(8) . . . . ? C18 C19 C23 O5 6.1(13) . . . . ? N12 C24 C25 N26 168.1(7) . . . . ? O8 C27 C28 C33 14.4(11) . . . . ? O7 C27 C28 C33 -164.5(7) . . . . ? O8 C27 C28 C29 -163.3(7) . . . . ? O7 C27 C28 C29 17.8(12) . . . . ? C33 C28 C29 O9 178.8(7) . . . . ? C27 C28 C29 O9 -3.5(12) . . . . ? C33 C28 C29 C30 -2.9(11) . . . . ? C27 C28 C29 C30 174.8(7) . . . . ? O9 C29 C30 C31 -177.9(7) . . . . ? C28 C29 C30 C31 3.7(11) . . . . ? O9 C29 C30 C34 2.9(11) . . . . ? C28 C29 C30 C34 -175.5(7) . . . . ? C34 C30 C31 C32 177.9(8) . . . . ? C29 C30 C31 C32 -1.3(12) . . . . ? C30 C31 C32 C33 -2.0(12) . . . . ? C29 C28 C33 C32 -0.3(12) . . . . ? C27 C28 C33 C32 -178.0(7) . . . . ? C31 C32 C33 C28 2.8(13) . . . . ? C31 C30 C34 N35 -179.3(8) . . . . ? C29 C30 C34 N35 -0.1(13) . . . . ? N35 C36 C37 N38 66.7(10) . . . . ? N38 C39 C40 N41 62.4(12) . . . . ? N41 C42 C43 C48 -178.5(7) . . . . ? N41 C42 C43 C44 -0.2(12) . . . . ? C48 C43 C44 O10 -178.0(6) . . . . ? C42 C43 C44 O10 3.7(10) . . . . ? C48 C43 C44 C45 -2.2(10) . . . . ? C42 C43 C44 C45 179.6(6) . . . . ? O10 C44 C45 C46 177.1(6) . . . . ? C43 C44 C45 C46 1.2(10) . . . . ? O10 C44 C45 C49 -6.1(10) . . . . ? C43 C44 C45 C49 178.0(6) . . . . ? C44 C45 C46 C47 0.0(10) . . . . ? C49 C45 C46 C47 -176.9(7) . . . . ? C45 C46 C47 C48 -0.4(11) . . . . ? C46 C47 C48 C43 -0.5(12) . . . . ? C42 C43 C48 C47 -179.9(7) . . . . ? C44 C43 C48 C47 1.8(11) . . . . ? C46 C45 C49 O11 145.4(7) . . . . ? C44 C45 C49 O11 -31.4(10) . . . . ? C46 C45 C49 O12 -33.2(10) . . . . ? C44 C45 C49 O12 150.0(7) . . . . ? N38 C50 C51 N52 74.5(18) . . . . ? C51A C50 C51 N52 22.0(13) . . . . ? N38 C50 C51A N52A 172.4(15) . . . . ? C51 C50 C51A N52A -48.6(14) . . . . ? N53 C54 C55 N56 43.3(10) . . . . ? N53 C57 C58 N59 -50.1(11) . . . . ? N53 C60 C61 N62 45(3) . . . . ? C61A C60 C61 N62 -55.6(15) . . . . ? N53 C60 C61A N62 -43.5(19) . . . . ? C61 C60 C61A N62 55.3(14) . . . . ? N63 C64 C65 N66 -47.0(11) . . . . ? N63 C67 C68 N69 39.0(15) . . . . ? N63 C70 C71 N72 47.2(11) . . . . ? C4 C8 N9 C10 -178.2(7) . . . . ? C11 C10 N9 C8 116.5(8) . . . . ? C10 C11 N12 C13 -152.7(7) . . . . ? C10 C11 N12 C24 79.5(9) . . . . ? C14 C13 N12 C11 93.3(8) . . . . ? C14 C13 N12 C24 -139.8(7) . . . . ? C25 C24 N12 C11 -168.5(7) . . . . ? C25 C24 N12 C13 64.8(9) . . . . ? C17 C16 N15 C14 -179.5(8) . . . . ? C13 C14 N15 C16 115.9(9) . . . . ? C24 C25 N26 Ni1 168.5(5) . . . . ? C30 C34 N35 C36 -176.3(8) . . . . ? C37 C36 N35 C34 91.0(9) . . . . ? C51A C50 N38 C39 -154.1(10) . . . . ? C51 C50 N38 C39 176.1(11) . . . . ? C51A C50 N38 C37 83.5(12) . . . . ? C51 C50 N38 C37 53.7(15) . . . . ? C40 C39 N38 C50 86.7(10) . . . . ? C40 C39 N38 C37 -149.5(8) . . . . ? C36 C37 N38 C50 -149.2(9) . . . . ? C36 C37 N38 C39 89.3(9) . . . . ? C43 C42 N41 C40 -178.7(7) . . . . ? C39 C40 N41 C42 107.7(10) . . . . ? C50 C51 N52 Ni2 168.4(11) . . . . ? C50 C51A N52A Ni2 167.6(12) . . . . ? C55 C54 N53 C60 71.7(9) . . . . ? C55 C54 N53 C57 -162.7(7) . . . . ? C55 C54 N53 Ni1 -48.2(7) . . . . ? C61 C60 N53 C54 -142.7(15) . . . . ? C61A C60 N53 C54 -94.3(13) . . . . ? C61 C60 N53 C57 91.4(16) . . . . ? C61A C60 N53 C57 139.7(12) . . . . ? C61 C60 N53 Ni1 -26.3(16) . . . . ? C61A C60 N53 Ni1 22.1(13) . . . . ? C58 C57 N53 C54 159.2(8) . . . . ? C58 C57 N53 C60 -74.2(10) . . . . ? C58 C57 N53 Ni1 45.9(9) . . . . ? C54 C55 N56 Ni1 -14.9(9) . . . . ? C57 C58 N59 Ni1 27.6(9) . . . . ? C60 C61 N62 C61A 55.6(15) . . . . ? C60 C61 N62 Ni1 -41(3) . . . . ? C60 C61A N62 C61 -54.8(14) . . . . ? C60 C61A N62 Ni1 42.2(17) . . . . ? C71 C70 N63 C64 -158.9(8) . . . . ? C71 C70 N63 C67 74.6(10) . . . . ? C71 C70 N63 Ni2 -44.8(9) . . . . ? C65 C64 N63 C70 161.1(9) . . . . ? C65 C64 N63 C67 -72.4(11) . . . . ? C65 C64 N63 Ni2 46.4(9) . . . . ? C68 C67 N63 C70 -137.0(10) . . . . ? C68 C67 N63 C64 96.1(11) . . . . ? C68 C67 N63 Ni2 -19.8(11) . . . . ? C64 C65 N66 Ni2 23.0(10) . . . . ? C67 C68 N69 Ni2 -37.3(13) . . . . ? C70 C71 N72 Ni2 -23.6(10) . . . . ? C25 N26 Ni1 N53 -171(12) . . . . ? C25 N26 Ni1 N56 22.0(6) . . . . ? C25 N26 Ni1 N62 -70.5(6) . . . . ? C25 N26 Ni1 N59 -164.9(6) . . . . ? C25 N26 Ni1 O8 110.6(6) . . . . ? C54 N53 Ni1 N26 -136(12) . . . . ? C60 N53 Ni1 N26 102(12) . . . . ? C57 N53 Ni1 N26 -18(12) . . . . ? C54 N53 Ni1 N56 31.0(5) . . . . ? C60 N53 Ni1 N56 -90.4(6) . . . . ? C57 N53 Ni1 N56 149.1(6) . . . . ? C54 N53 Ni1 N62 123.4(5) . . . . ? C60 N53 Ni1 N62 2.0(6) . . . . ? C57 N53 Ni1 N62 -118.5(6) . . . . ? C54 N53 Ni1 N59 -142.1(5) . . . . ? C60 N53 Ni1 N59 96.5(6) . . . . ? C57 N53 Ni1 N59 -24.0(5) . . . . ? C54 N53 Ni1 O8 -57.6(5) . . . . ? C60 N53 Ni1 O8 -179.0(6) . . . . ? C57 N53 Ni1 O8 60.5(5) . . . . ? C55 N56 Ni1 N26 170.6(5) . . . . ? C55 N56 Ni1 N53 -9.1(5) . . . . ? C55 N56 Ni1 N62 -92.6(6) . . . . ? C55 N56 Ni1 N59 17.9(13) . . . . ? C55 N56 Ni1 O8 79.6(5) . . . . ? C61 N62 Ni1 N26 -157.5(14) . . . . ? C61A N62 Ni1 N26 157.0(10) . . . . ? C61 N62 Ni1 N53 21.2(14) . . . . ? C61A N62 Ni1 N53 -24.3(10) . . . . ? C61 N62 Ni1 N56 103.7(14) . . . . ? C61A N62 Ni1 N56 58.2(10) . . . . ? C61 N62 Ni1 N59 -62.0(14) . . . . ? C61A N62 Ni1 N59 -107.5(10) . . . . ? C61 N62 Ni1 O8 14(3) . . . . ? C61A N62 Ni1 O8 -32(2) . . . . ? C58 N59 Ni1 N26 178.4(6) . . . . ? C58 N59 Ni1 N53 -1.7(6) . . . . ? C58 N59 Ni1 N56 -28.6(13) . . . . ? C58 N59 Ni1 N62 81.6(6) . . . . ? C58 N59 Ni1 O8 -90.8(6) . . . . ? C65 N66 Ni2 N72 -35.0(14) . . . . ? C65 N66 Ni2 O6 -88.3(7) . . . . ? C65 N66 Ni2 N63 1.4(6) . . . . ? C65 N66 Ni2 N69 84.1(7) . . . . ? C65 N66 Ni2 N52 -172.3(7) . . . . ? C65 N66 Ni2 N52A 176.7(9) . . . . ? C71 N72 Ni2 N66 34.8(15) . . . . ? C71 N72 Ni2 O6 87.5(7) . . . . ? C71 N72 Ni2 N63 -1.5(6) . . . . ? C71 N72 Ni2 N69 -84.5(7) . . . . ? C71 N72 Ni2 N52 173.7(8) . . . . ? C71 N72 Ni2 N52A -179.5(9) . . . . ? C70 N63 Ni2 N66 -144.0(6) . . . . ? C64 N63 Ni2 N66 -24.7(6) . . . . ? C67 N63 Ni2 N66 95.3(6) . . . . ? C70 N63 Ni2 N72 26.0(5) . . . . ? C64 N63 Ni2 N72 145.3(6) . . . . ? C67 N63 Ni2 N72 -94.7(6) . . . . ? C70 N63 Ni2 O6 -61.6(5) . . . . ? C64 N63 Ni2 O6 57.6(6) . . . . ? C67 N63 Ni2 O6 177.7(6) . . . . ? C70 N63 Ni2 N69 120.4(6) . . . . ? C64 N63 Ni2 N69 -120.4(6) . . . . ? C67 N63 Ni2 N69 -0.3(6) . . . . ? C70 N63 Ni2 N52 -3(3) . . . . ? C64 N63 Ni2 N52 116(3) . . . . ? C67 N63 Ni2 N52 -124(3) . . . . ? C70 N63 Ni2 N52A -161(2) . . . . ? C64 N63 Ni2 N52A -42(2) . . . . ? C67 N63 Ni2 N52A 78(2) . . . . ? C68 N69 Ni2 N66 -62.2(9) . . . . ? C68 N69 Ni2 N72 103.1(9) . . . . ? C68 N69 Ni2 O6 6(3) . . . . ? C68 N69 Ni2 N63 20.1(9) . . . . ? C68 N69 Ni2 N52 -168.2(11) . . . . ? C68 N69 Ni2 N52A -144.3(11) . . . . ? C51 N52 Ni2 N66 -75.9(15) . . . . ? C51 N52 Ni2 N72 115.4(15) . . . . ? C51 N52 Ni2 O6 -156.9(15) . . . . ? C51 N52 Ni2 N63 144(2) . . . . ? C51 N52 Ni2 N69 22.2(16) . . . . ? C51 N52 Ni2 N52A -49.7(15) . . . . ? C51A N52A Ni2 N66 173.3(17) . . . . ? C51A N52A Ni2 N72 2.8(18) . . . . ? C51A N52A Ni2 O6 91.7(16) . . . . ? C51A N52A Ni2 N63 -169.7(13) . . . . ? C51A N52A Ni2 N69 -92.4(16) . . . . ? C51A N52A Ni2 N52 18.9(14) . . . . ? O2 C1 O1 Dy1 -140.6(7) . . . . ? C2 C1 O1 Dy1 38.1(11) . . . . ? O4 Dy1 O1 C1 65.6(7) . . . . ? O7 Dy1 O1 C1 128.1(7) . . . . ? O9 Dy1 O1 C1 -150.5(7) . . . . ? O10 Dy1 O1 C1 -85.7(7) . . . . ? O5 Dy1 O1 C1 138.3(8) . . . . ? O3 Dy1 O1 C1 -6.3(7) . . . . ? O11 Dy1 O1 C1 -46.1(8) . . . . ? C4 C3 O3 Dy1 -136.1(6) . . . . ? C2 C3 O3 Dy1 45.0(9) . . . . ? O4 Dy1 O3 C3 -128.2(6) . . . . ? O7 Dy1 O3 C3 173.1(6) . . . . ? O1 Dy1 O3 C3 -36.2(6) . . . . ? O9 Dy1 O3 C3 57.3(7) . . . . ? O10 Dy1 O3 C3 44.7(6) . . . . ? O5 Dy1 O3 C3 -83.8(6) . . . . ? O11 Dy1 O3 C3 119.5(6) . . . . ? C19 C18 O4 Dy1 17.9(13) . . . . ? C17 C18 O4 Dy1 -161.4(5) . . . . ? O7 Dy1 O4 C18 -102.6(7) . . . . ? O1 Dy1 O4 C18 47.9(7) . . . . ? O9 Dy1 O4 C18 -63.6(8) . . . . ? O10 Dy1 O4 C18 108.5(7) . . . . ? O5 Dy1 O4 C18 -25.3(7) . . . . ? O3 Dy1 O4 C18 121.4(7) . . . . ? O11 Dy1 O4 C18 -169.3(7) . . . . ? O6 C23 O5 Dy1 150.8(7) . . . . ? C19 C23 O5 Dy1 -30.6(12) . . . . ? O4 Dy1 O5 C23 32.4(8) . . . . ? O7 Dy1 O5 C23 114.8(8) . . . . ? O1 Dy1 O5 C23 -59.5(8) . . . . ? O9 Dy1 O5 C23 -170.4(8) . . . . ? O10 Dy1 O5 C23 -118.2(7) . . . . ? O3 Dy1 O5 C23 -11.7(9) . . . . ? O11 Dy1 O5 C23 125.5(7) . . . . ? O5 C23 O6 Ni2 -3.0(15) . . . . ? C19 C23 O6 Ni2 178.4(6) . . . . ? N66 Ni2 O6 C23 -153.8(10) . . . . ? N72 Ni2 O6 C23 39.7(10) . . . . ? N63 Ni2 O6 C23 123.2(9) . . . . ? N69 Ni2 O6 C23 137(2) . . . . ? N52 Ni2 O6 C23 -48.5(11) . . . . ? N52A Ni2 O6 C23 -72.6(11) . . . . ? O8 C27 O7 Dy1 171.2(5) . . . . ? C28 C27 O7 Dy1 -9.9(13) . . . . ? O4 Dy1 O7 C27 151.2(8) . . . . ? O1 Dy1 O7 C27 86.5(8) . . . . ? O9 Dy1 O7 C27 -5.0(8) . . . . ? O10 Dy1 O7 C27 -49.5(9) . . . . ? O5 Dy1 O7 C27 76.4(8) . . . . ? O3 Dy1 O7 C27 -152.7(8) . . . . ? O11 Dy1 O7 C27 -97.2(8) . . . . ? O7 C27 O8 Ni1 11.7(12) . . . . ? C28 C27 O8 Ni1 -167.1(5) . . . . ? N26 Ni1 O8 C27 -60.5(7) . . . . ? N53 Ni1 O8 C27 120.8(7) . . . . ? N56 Ni1 O8 C27 38.1(7) . . . . ? N62 Ni1 O8 C27 128.0(19) . . . . ? N59 Ni1 O8 C27 -155.4(7) . . . . ? C28 C29 O9 Dy1 -21.5(11) . . . . ? C30 C29 O9 Dy1 160.3(5) . . . . ? O4 Dy1 O9 C29 -18.5(8) . . . . ? O7 Dy1 O9 C29 21.7(7) . . . . ? O1 Dy1 O9 C29 -123.8(7) . . . . ? O10 Dy1 O9 C29 166.0(7) . . . . ? O5 Dy1 O9 C29 -55.8(7) . . . . ? O3 Dy1 O9 C29 152.9(6) . . . . ? O11 Dy1 O9 C29 93.6(7) . . . . ? C45 C44 O10 Dy1 46.1(9) . . . . ? C43 C44 O10 Dy1 -138.1(6) . . . . ? O4 Dy1 O10 C44 55.6(8) . . . . ? O7 Dy1 O10 C44 -84.2(6) . . . . ? O1 Dy1 O10 C44 118.6(6) . . . . ? O9 Dy1 O10 C44 -129.5(6) . . . . ? O5 Dy1 O10 C44 175.4(6) . . . . ? O3 Dy1 O10 C44 43.0(6) . . . . ? O11 Dy1 O10 C44 -36.7(6) . . . . ? O12 C49 O11 Dy1 -149.8(5) . . . . ? C45 C49 O11 Dy1 31.7(10) . . . . ? O4 Dy1 O11 C49 -149.6(7) . . . . ? O7 Dy1 O11 C49 139.0(7) . . . . ? O1 Dy1 O11 C49 -44.3(8) . . . . ? O9 Dy1 O11 C49 66.5(7) . . . . ? O10 Dy1 O11 C49 -3.6(7) . . . . ? O5 Dy1 O11 C49 128.1(7) . . . . ? O3 Dy1 O11 C49 -83.5(7) . . . . ? O30A N30A O301 N300 153(4) . . . . ? O302 N30A O301 N300 -28(2) . . . . ? O302 N300 O301 N30A 29(2) . . . . ? O300 N300 O301 N30A -164(3) . . . . ? O300 N300 O302 N30A 166(3) . . . . ? O301 N300 O302 N30A -27(2) . . . . ? O301 N30A O302 N300 30(2) . . . . ? O30A N30A O302 N300 -152(4) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.947 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.110 data_Er _database_code_depnum_ccdc_archive 'CCDC 872218' #TrackingRef '15314_web_deposit_cif_file_0_KlausHarms_1352392481.Ni2_Ln_oct.cif' # start Validation Reply Form _vrf_PLAT241_Er ; PROBLEM: Check High Ueq as Compared to Neighbors for C65 RESPONSE: Unresolved disorder of CH2-group ; _vrf_PLAT780_Er ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: This is due to the refinement of solvent water as oxygen atoms at split positions. ; # end Validation Reply Form #Added by publCIF (Fr 24. Aug 12:12:06 2012) _audit_update_record ; 2012-08-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H84 Er N16 Ni2 O12, 3(N O3), 20(H2 O)' _chemical_formula_sum 'C56 H124 Er N19 Ni2 O41' _chemical_formula_weight 2004.42 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' Er Er -0.2586 4.9576 '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 16.2644(15) _cell_length_b 16.3118(12) _cell_length_c 19.4070(14) _cell_angle_alpha 110.568(5) _cell_angle_beta 111.377(6) _cell_angle_gamma 88.898(7) _cell_volume 4453.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11535 _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 23.83 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2090 _exptl_absorpt_coefficient_mu 1.449 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7459 _exptl_absorpt_correction_T_max 0.9397 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ? _diffrn_ambient_temperature 100(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30546 _diffrn_reflns_av_R_equivalents 0.1237 _diffrn_reflns_av_sigmaI/netI 0.2450 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.12 _reflns_number_total 15737 _reflns_number_gt 5500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA (Steo & Cie., 2006)' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SIR2008 (Burla et al., 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material 'ENCIFER, PUBLCIF' _refine_special_details ; Disordered solvent water has been refined as a mixture of fully and partly occupied positions of oxygen atoms. These atoms were allowed to refine isotropically. Hydrogen atoms for the water molecules were not included into the model but used for the calculation of moleculae weight etc. Restraints were included for the geometry of the NO3-ions and the shape of their thermal ellipsoids. Some remaining unusual anisotropic temperature factors and distorted geometries of the anions indicate disorder that has not been resolved (regarding atoms C65 O301 O302 O303 N200 O200 O202 N100 O100 O102 O400 O405 O406 O408 O409 O410 O412 O413 O411 O415 O421 O422 O423 O424 O425 O426 O427 O429 O433 O435). 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^)+(0.0822P)^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 15737 _refine_ls_number_parameters 1062 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.1709 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1908 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 0.747 _refine_ls_restrained_S_all 0.754 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9992(9) 0.7835(6) 0.6009(9) 0.067(4) Uani 1 1 d . . . C2 C 1.0981(8) 0.7892(6) 0.6330(7) 0.056(3) Uani 1 1 d . . . C3 C 1.1436(8) 0.7509(7) 0.6898(7) 0.061(3) Uani 1 1 d . . . C4 C 1.2398(9) 0.7636(7) 0.7200(6) 0.060(3) Uani 1 1 d . . . C5 C 1.2844(8) 0.8126(8) 0.6957(7) 0.069(3) Uani 1 1 d . . . H5 H 1.3476 0.8202 0.7170 0.083 Uiso 1 1 calc R . . C6 C 1.2405(11) 0.8498(7) 0.6427(8) 0.082(4) Uani 1 1 d . . . H6 H 1.2719 0.8852 0.6283 0.098 Uiso 1 1 calc R . . C7 C 1.1456(9) 0.8343(7) 0.6091(7) 0.067(3) Uani 1 1 d . . . H7 H 1.1142 0.8561 0.5685 0.081 Uiso 1 1 calc R . . C8 C 1.2875(10) 0.7213(8) 0.7750(7) 0.075(4) Uani 1 1 d . . . H8 H 1.3506 0.7276 0.7931 0.090 Uiso 1 1 calc R . . C10 C 1.2983(9) 0.6309(8) 0.8547(8) 0.085(4) Uani 1 1 d . . . H10A H 1.2787 0.6470 0.9000 0.102 Uiso 1 1 calc R . . H10B H 1.3633 0.6485 0.8760 0.102 Uiso 1 1 calc R . . C11 C 1.2761(9) 0.5301(7) 0.8065(8) 0.079(4) Uani 1 1 d . . . H11A H 1.2996 0.5145 0.7637 0.095 Uiso 1 1 calc R . . H11B H 1.3060 0.4983 0.8422 0.095 Uiso 1 1 calc R . . C13 C 1.1594(8) 0.4205(7) 0.7009(7) 0.081(4) Uani 1 1 d . . . H13A H 1.1101 0.3830 0.6979 0.097 Uiso 1 1 calc R . . H13B H 1.2116 0.3875 0.7059 0.097 Uiso 1 1 calc R . . C14 C 1.1326(8) 0.4382(7) 0.6267(7) 0.077(4) Uani 1 1 d . . . H14A H 1.1793 0.4799 0.6310 0.092 Uiso 1 1 calc R . . H14B H 1.1260 0.3826 0.5815 0.092 Uiso 1 1 calc R . . C16 C 0.9739(10) 0.4331(8) 0.5572(8) 0.074(4) Uani 1 1 d . . . H16 H 0.9754 0.3737 0.5263 0.089 Uiso 1 1 calc R . . C17 C 0.8893(9) 0.4647(7) 0.5378(8) 0.073(4) Uani 1 1 d . . . C18 C 0.8801(8) 0.5530(6) 0.5864(7) 0.061(3) Uani 1 1 d . . . C19 C 0.7940(8) 0.5819(7) 0.5570(6) 0.060(3) Uani 1 1 d . . . C20 C 0.7275(9) 0.5264(8) 0.4922(8) 0.075(4) Uani 1 1 d . . . H20 H 0.6716 0.5473 0.4749 0.091 Uiso 1 1 calc R . . C21 C 0.7359(9) 0.4387(7) 0.4479(7) 0.081(4) Uani 1 1 d . . . H21 H 0.6869 0.4018 0.4028 0.097 Uiso 1 1 calc R . . C22 C 0.8159(9) 0.4094(8) 0.4721(7) 0.070(4) Uani 1 1 d . . . H22 H 0.8227 0.3504 0.4443 0.084 Uiso 1 1 calc R . . C23 C 0.7728(10) 0.6722(7) 0.6035(8) 0.068(4) Uani 1 1 d . . . C24 C 1.1462(8) 0.4967(7) 0.8310(7) 0.071(4) Uani 1 1 d . . . H24A H 1.1706 0.5502 0.8800 0.085 Uiso 1 1 calc R . . H24B H 1.1657 0.4449 0.8452 0.085 Uiso 1 1 calc R . . C25 C 1.0453(8) 0.4887(7) 0.7983(7) 0.068(3) Uani 1 1 d . . . H25A H 1.0257 0.5384 0.7809 0.082 Uiso 1 1 calc R . . H25B H 1.0209 0.4332 0.7513 0.082 Uiso 1 1 calc R . . C27 C 0.8804(7) 0.6676(7) 0.8488(7) 0.059(3) Uani 1 1 d . . . C28 C 0.8605(8) 0.7584(7) 0.8900(6) 0.060(3) Uani 1 1 d . . . C29 C 0.8836(8) 0.8355(6) 0.8795(6) 0.058(3) Uani 1 1 d . . . C30 C 0.8597(9) 0.9189(6) 0.9230(6) 0.069(3) Uani 1 1 d . . . C31 C 0.8117(10) 0.9182(8) 0.9703(8) 0.089(4) Uani 1 1 d . . . H31 H 0.7923 0.9718 0.9953 0.107 Uiso 1 1 calc R . . C32 C 0.7913(11) 0.8439(7) 0.9823(7) 0.097(5) Uani 1 1 d . . . H32 H 0.7625 0.8463 1.0175 0.117 Uiso 1 1 calc R . . C33 C 0.8155(9) 0.7639(7) 0.9398(7) 0.080(4) Uani 1 1 d . . . H33 H 0.8002 0.7114 0.9455 0.096 Uiso 1 1 calc R . . C34 C 0.8867(9) 0.9995(7) 0.9225(7) 0.075(4) Uani 1 1 d . . . H34 H 0.8693 1.0508 0.9533 0.090 Uiso 1 1 calc R . . C36 C 0.9584(10) 1.0973(7) 0.8853(8) 0.088(4) Uani 1 1 d . . . H36A H 1.0221 1.1039 0.8936 0.105 Uiso 1 1 calc R . . H36B H 0.9495 1.1444 0.9299 0.105 Uiso 1 1 calc R . . C37 C 0.9016(9) 1.1057(6) 0.8070(8) 0.086(4) Uani 1 1 d . . . H37A H 0.8379 1.0907 0.7949 0.103 Uiso 1 1 calc R . . H37B H 0.9108 1.1672 0.8108 0.103 Uiso 1 1 calc R . . C39 C 0.9965(10) 1.0915(8) 0.7332(9) 0.096(5) Uani 1 1 d . . . H39A H 1.0349 1.1360 0.7852 0.115 Uiso 1 1 calc R . . H39B H 0.9681 1.1227 0.6967 0.115 Uiso 1 1 calc R . . C40 C 1.0540(9) 1.0259(7) 0.6990(8) 0.082(4) Uani 1 1 d . . . H40A H 1.0169 0.9833 0.6454 0.099 Uiso 1 1 calc R . . H40B H 1.1017 1.0578 0.6944 0.099 Uiso 1 1 calc R . . C42 C 1.1775(11) 0.9919(7) 0.7994(8) 0.074(4) Uani 1 1 d . . . H42 H 1.2168 1.0313 0.7959 0.089 Uiso 1 1 calc R . . C43 C 1.2133(10) 0.9481(8) 0.8555(8) 0.070(4) Uani 1 1 d . . . C44 C 1.1581(10) 0.8857(8) 0.8589(7) 0.067(3) Uani 1 1 d . . . C45 C 1.1974(9) 0.8431(7) 0.9162(6) 0.059(3) Uani 1 1 d . . . C46 C 1.2847(11) 0.8666(9) 0.9607(9) 0.089(4) Uani 1 1 d . . . H46 H 1.3097 0.8406 0.9993 0.106 Uiso 1 1 calc R . . C47 C 1.3431(10) 0.9249(9) 0.9568(8) 0.081(4) Uani 1 1 d . . . H47 H 1.4049 0.9361 0.9890 0.098 Uiso 1 1 calc R . . C48 C 1.3033(10) 0.9667(8) 0.9007(8) 0.081(4) Uani 1 1 d . . . H48 H 1.3390 1.0071 0.8948 0.097 Uiso 1 1 calc R . . C49 C 1.1409(10) 0.7761(8) 0.9189(9) 0.069(4) Uani 1 1 d . . . C50 C 0.8512(11) 1.0025(8) 0.6675(9) 0.087(4) Uani 1 1 d . . . H50A H 0.8738 0.9741 0.6249 0.105 Uiso 1 1 calc R . . H50B H 0.8146 1.0479 0.6538 0.105 Uiso 1 1 calc R . . C51 C 0.7928(9) 0.9327(8) 0.6713(8) 0.078(4) Uani 1 1 d . . . H51A H 0.8303 0.8886 0.6867 0.094 Uiso 1 1 calc R . . H51B H 0.7700 0.9618 0.7137 0.094 Uiso 1 1 calc R . . C54 C 0.6908(8) 0.4899(7) 0.7339(6) 0.061(3) Uani 1 1 d . . . H54A H 0.6992 0.5550 0.7602 0.073 Uiso 1 1 calc R . . H54B H 0.6261 0.4696 0.7078 0.073 Uiso 1 1 calc R . . C55 C 0.7328(9) 0.4632(7) 0.6711(7) 0.079(4) Uani 1 1 d . . . H55A H 0.7106 0.4010 0.6351 0.094 Uiso 1 1 calc R . . H55B H 0.7152 0.5006 0.6387 0.094 Uiso 1 1 calc R . . C57 C 0.7040(8) 0.3533(7) 0.7588(7) 0.078(4) Uani 1 1 d . . . H57A H 0.6780 0.3342 0.7001 0.094 Uiso 1 1 calc R . . H57B H 0.6573 0.3405 0.7763 0.094 Uiso 1 1 calc R . . C58 C 0.7833(10) 0.3004(8) 0.7839(9) 0.098(5) Uani 1 1 d . . . H58A H 0.7937 0.3013 0.8377 0.118 Uiso 1 1 calc R . . H58B H 0.7672 0.2382 0.7464 0.118 Uiso 1 1 calc R . . C60 C 0.7150(8) 0.4917(9) 0.8671(7) 0.078(4) Uani 1 1 d . . . H60A H 0.6543 0.4692 0.8579 0.093 Uiso 1 1 calc R . . H60B H 0.7182 0.5563 0.8807 0.093 Uiso 1 1 calc R . . C61 C 0.7841(10) 0.4710(9) 0.9361(7) 0.085(4) Uani 1 1 d . . . H61A H 0.7819 0.5110 0.9872 0.102 Uiso 1 1 calc R . . H61B H 0.7689 0.4096 0.9299 0.102 Uiso 1 1 calc R . . C64 C 0.4585(10) 0.7618(10) 0.6127(9) 0.110(5) Uani 1 1 d . . . H64A H 0.4024 0.7381 0.5653 0.132 Uiso 1 1 calc R . . H64B H 0.4506 0.7505 0.6569 0.132 Uiso 1 1 calc R . . C65 C 0.4728(13) 0.8517(12) 0.6331(17) 0.185(11) Uani 1 1 d . . . H65A H 0.4830 0.8792 0.6903 0.221 Uiso 1 1 calc R . . H65B H 0.4162 0.8693 0.6036 0.221 Uiso 1 1 calc R . . C67 C 0.4994(9) 0.6454(8) 0.5132(9) 0.097(5) Uani 1 1 d . . . H67A H 0.4447 0.6102 0.5037 0.117 Uiso 1 1 calc R . . H67B H 0.5447 0.6048 0.5083 0.117 Uiso 1 1 calc R . . C68 C 0.4792(11) 0.6851(12) 0.4502(10) 0.115(6) Uani 1 1 d . . . H68A H 0.4686 0.6384 0.3977 0.138 Uiso 1 1 calc R . . H68B H 0.4253 0.7154 0.4463 0.138 Uiso 1 1 calc R . . C70 C 0.5789(10) 0.6750(8) 0.6574(9) 0.097(5) Uani 1 1 d . . . H70A H 0.5348 0.6449 0.6676 0.117 Uiso 1 1 calc R . . H70B H 0.6168 0.6313 0.6391 0.117 Uiso 1 1 calc R . . C71 C 0.6347(10) 0.7484(9) 0.7318(8) 0.088(4) Uani 1 1 d . . . H71A H 0.5958 0.7822 0.7576 0.106 Uiso 1 1 calc R . . H71B H 0.6759 0.7233 0.7689 0.106 Uiso 1 1 calc R . . N9 N 1.2513(7) 0.6766(6) 0.8007(6) 0.069(3) Uani 1 1 d . . . N12 N 1.1819(8) 0.5020(5) 0.7718(6) 0.072(3) Uani 1 1 d . . . N15 N 1.0481(8) 0.4758(6) 0.6118(7) 0.071(3) Uani 1 1 d . . . N26 N 1.0095(6) 0.4891(5) 0.8585(5) 0.064(3) Uani 1 1 d . . . H26A H 1.0315 0.5419 0.9009 0.077 Uiso 1 1 calc R . . H26B H 1.0323 0.4453 0.8769 0.077 Uiso 1 1 calc R . . N35 N 0.9335(7) 1.0110(5) 0.8837(6) 0.068(3) Uani 1 1 d . . . N38 N 0.9270(8) 1.0453(6) 0.7434(7) 0.083(3) Uani 1 1 d . . . N41 N 1.0930(8) 0.9791(6) 0.7535(7) 0.083(3) Uani 1 1 d . . . N52 N 0.7196(7) 0.8881(6) 0.5994(6) 0.081(3) Uani 1 1 d . . . H52A H 0.7420 0.8580 0.5616 0.097 Uiso 1 1 calc R . . H52B H 0.6888 0.9301 0.5831 0.097 Uiso 1 1 calc R . . N53 N 0.7336(6) 0.4494(6) 0.7945(6) 0.070(3) Uani 1 1 d . . . N56 N 0.8306(7) 0.4734(5) 0.7097(5) 0.065(3) Uani 1 1 d . . . H56A H 0.8540 0.5259 0.7123 0.078 Uiso 1 1 calc R . . H56B H 0.8524 0.4283 0.6795 0.078 Uiso 1 1 calc R . . N59 N 0.8635(8) 0.3355(6) 0.7845(6) 0.084(3) Uani 1 1 d . . . H59A H 0.8638 0.3138 0.7340 0.100 Uiso 1 1 calc R . . H59B H 0.9119 0.3190 0.8174 0.100 Uiso 1 1 calc R . . N62 N 0.8730(7) 0.4814(6) 0.9380(6) 0.075(3) Uani 1 1 d . . . H62A H 0.9041 0.4386 0.9527 0.090 Uiso 1 1 calc R . . H62B H 0.9020 0.5355 0.9756 0.090 Uiso 1 1 calc R . . N63 N 0.5319(7) 0.7118(6) 0.5945(7) 0.085(3) Uani 1 1 d . . . N66 N 0.5396(8) 0.8909(7) 0.6225(8) 0.114(5) Uani 1 1 d . . . H66A H 0.5701 0.9390 0.6677 0.137 Uiso 1 1 calc R . . H66B H 0.5152 0.9101 0.5809 0.137 Uiso 1 1 calc R . . N69 N 0.5580(9) 0.7496(7) 0.4741(7) 0.104(4) Uani 1 1 d . . . H69A H 0.5392 0.7956 0.4577 0.125 Uiso 1 1 calc R . . H69B H 0.5952 0.7223 0.4494 0.125 Uiso 1 1 calc R . . N72 N 0.6867(7) 0.8087(7) 0.7175(6) 0.089(3) Uani 1 1 d . . . H72A H 0.7439 0.7948 0.7283 0.107 Uiso 1 1 calc R . . H72B H 0.6890 0.8658 0.7508 0.107 Uiso 1 1 calc R . . O1 O 0.9585(5) 0.7905(5) 0.6474(5) 0.068(2) Uani 1 1 d . . . O2 O 0.9612(6) 0.7761(5) 0.5311(6) 0.076(2) Uani 1 1 d . . . O3 O 1.1022(5) 0.7068(4) 0.7141(5) 0.065(2) Uani 1 1 d . . . H3 H 1.1259 0.6545 0.7190 0.079 Uiso 1 1 calc R . . O4 O 0.9472(5) 0.5996(4) 0.6498(5) 0.065(2) Uani 1 1 d . . . H4 H 0.9976 0.5683 0.6579 0.078 Uiso 1 1 calc R . . O5 O 0.8258(5) 0.7177(4) 0.6701(5) 0.067(2) Uani 1 1 d . . . O6 O 0.7010(6) 0.6931(5) 0.5645(5) 0.082(3) Uani 1 1 d . . . O7 O 0.9070(6) 0.6578(4) 0.7921(5) 0.079(2) Uani 1 1 d . . . O8 O 0.8684(5) 0.6097(5) 0.8724(4) 0.073(2) Uani 1 1 d . . . O9 O 0.9223(5) 0.8367(4) 0.8330(5) 0.070(2) Uani 1 1 d . . . H9 H 0.9309 0.8947 0.8341 0.084 Uiso 1 1 calc R . . O10 O 1.0734(6) 0.8705(4) 0.8147(5) 0.070(2) Uani 1 1 d . . . H10 H 1.0465 0.9211 0.8086 0.084 Uiso 1 1 calc R . . O11 O 1.0827(6) 0.7244(5) 0.8599(5) 0.071(2) Uani 1 1 d . . . O12 O 1.1636(7) 0.7723(5) 0.9886(6) 0.098(3) Uani 1 1 d . . . Ni1 Ni 0.87068(10) 0.47175(8) 0.82480(9) 0.0647(5) Uani 1 1 d . . . Ni2 Ni 0.62780(11) 0.79877(10) 0.59793(10) 0.0797(5) Uani 1 1 d . . . Er1 Er 0.97675(4) 0.73769(3) 0.74779(3) 0.0629(2) Uani 1 1 d . . . N300 N 0.5666(19) 0.5385(17) 0.2968(12) 0.141(9) Uani 0.50 1 d PDU A 1 N301 N 0.545(2) 0.4410(14) 0.2639(11) 0.128(8) Uani 0.50 1 d PDU A 2 O300 O 0.6251(15) 0.6073(17) 0.3491(12) 0.105(7) Uani 0.50 1 d PDU A 1 O301 O 0.5235(10) 0.4920(10) 0.2192(10) 0.177(5) Uani 1 1 d DU . . O302 O 0.5447(9) 0.4952(9) 0.3335(8) 0.155(5) Uani 1 1 d DU . . O303 O 0.529(2) 0.3553(14) 0.2384(14) 0.201(12) Uani 0.50 1 d PDU A 2 N200 N 0.1068(13) 0.2989(19) 0.8644(11) 0.265(12) Uani 1 1 d DU . . O200 O 0.0570(17) 0.287(2) 0.7855(12) 0.420(18) Uani 1 1 d DU . . O201 O 0.1821(8) 0.2546(8) 0.8778(7) 0.148(5) Uani 1 1 d DU . . O202 O 0.0661(11) 0.3312(8) 0.9160(8) 0.180(6) Uani 1 1 d DU . . N100 N 0.2025(11) 0.7652(11) 0.4289(11) 0.169(7) Uani 1 1 d DU . . O100 O 0.1933(13) 0.8512(12) 0.4553(12) 0.279(10) Uani 1 1 d DU . . O101 O 0.1297(7) 0.7109(6) 0.3822(6) 0.108(3) Uani 1 1 d DU . . O102 O 0.2745(15) 0.7530(17) 0.412(2) 0.436(19) Uani 1 1 d DU . . O400 O 0.6536(14) 0.6608(14) 0.0087(13) 0.193(8) Uiso 0.75 1 d P B 2 O401 O 0.642(3) 0.640(3) 0.078(3) 0.121(14) Uiso 0.25 1 d P C 1 O402 O 0.8292(7) 0.7901(8) 0.2795(7) 0.133(4) Uiso 1 1 d . . . O403 O 0.5165(12) 0.7726(12) 0.0295(11) 0.100(6) Uiso 0.50 1 d P D 1 O404 O 0.5707(14) 0.9253(14) 0.1568(14) 0.115(7) Uiso 0.50 1 d P E 1 O405 O 0.604(3) 0.930(3) 0.220(3) 0.237(16) Uiso 0.50 1 d P F 2 O406 O 0.711(3) 0.911(4) 0.280(3) 0.157(18) Uiso 0.25 1 d P G 1 O407 O 0.6890(12) 0.7835(12) 0.3310(11) 0.099(6) Uiso 0.50 1 d P . . O408 O 0.764(3) 0.942(3) 0.431(2) 0.219(14) Uiso 0.50 1 d P H 1 O409 O 0.849(2) 0.983(2) 0.4706(18) 0.168(10) Uiso 0.50 1 d P I 2 O410 O 0.408(4) 0.857(5) 0.236(4) 0.20(3) Uiso 0.25 1 d P J 2 O412 O 0.643(4) -0.013(4) 0.461(4) 0.166(19) Uiso 0.25 1 d P K 1 O413 O 0.428(3) 0.095(3) 0.596(2) 0.248(16) Uiso 0.50 1 d P L 2 O416 O 0.6321(16) 0.0583(19) 0.5212(16) 0.147(9) Uiso 0.50 1 d P M 2 O411 O 0.382(2) 0.902(2) 0.317(2) 0.216(14) Uiso 0.50 1 d P N 2 O414 O 0.458(3) 0.863(3) 0.365(3) 0.119(13) Uiso 0.25 1 d P O 1 O415 O 0.390(2) 0.868(3) 0.425(2) 0.224(14) Uiso 0.50 1 d P P 2 O417 O 0.9324(9) 0.0273(8) 0.5175(7) 0.140(4) Uiso 1 1 d . Q 1 O418 O -0.0120(7) 0.7915(7) 0.4043(6) 0.111(3) Uiso 1 1 d . . . O419 O 0.5211(12) 0.9318(12) 0.8411(11) 0.098(5) Uiso 0.50 1 d P R 1 O420 O 0.5032(14) 0.7861(16) 0.8880(13) 0.116(7) Uiso 0.50 1 d P S 1 O421 O 0.5749(13) 0.6470(13) 0.8440(12) 0.180(7) Uiso 0.75 1 d P T 2 O422 O 0.654(2) 0.658(2) 0.362(2) 0.176(15) Uiso 0.50 1 d P U 2 O423 O 0.451(3) 0.300(3) 0.746(3) 0.30(2) Uiso 0.50 1 d P V 1 O424 O 0.4216(19) 0.3487(19) 0.8037(18) 0.169(10) Uiso 0.50 1 d P W 2 O425 O 0.530(3) 0.523(3) 0.943(2) 0.263(18) Uiso 0.50 1 d P X 1 O426 O 0.6127(18) 0.4801(18) 1.0077(16) 0.160(9) Uiso 0.50 1 d P Y 2 O427 O 0.587(2) 0.368(3) 0.961(2) 0.208(13) Uiso 0.50 1 d P Z 1 O428 O 0.5852(16) 0.3036(18) 0.9013(16) 0.145(8) Uiso 0.50 1 d P A 2 O429 O 0.6902(19) 0.265(2) 0.9096(17) 0.172(10) Uiso 0.50 1 d P B 1 O430 O 0.6994(16) 0.1807(17) 0.8615(15) 0.141(8) Uiso 0.50 1 d P C 2 O431 O 0.9305(13) 0.3279(12) 0.9942(11) 0.068(6) Uiso 0.50 1 d P D 2 O432 O 0.9616(12) 0.3369(11) 0.9903(10) 0.059(5) Uiso 0.50 1 d P E 1 O433 O 0.3240(19) -0.020(2) 0.1883(18) 0.158(11) Uiso 0.50 1 d P F 1 O434 O 0.3409(14) 0.0138(14) 0.1741(12) 0.099(7) Uiso 0.50 1 d P G 2 O435 O 0.520(3) 0.841(3) 0.878(2) 0.232(16) Uiso 0.50 1 d P H 2 O436 O 0.802(3) 0.807(4) 0.477(3) 0.121(17) Uiso 0.25 1 d P I 2 O437 O 0.7766(8) 0.7641(9) 0.4666(7) 0.122(4) Uiso 1 1 d . J 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.090(11) 0.034(6) 0.071(10) 0.022(6) 0.023(9) 0.023(6) C2 0.074(9) 0.032(6) 0.061(8) 0.013(5) 0.029(7) 0.017(6) C3 0.074(9) 0.037(6) 0.053(8) -0.007(5) 0.027(7) 0.011(6) C4 0.080(10) 0.043(6) 0.047(7) 0.006(5) 0.023(7) 0.015(6) C5 0.075(9) 0.060(7) 0.070(9) 0.008(7) 0.041(7) 0.016(7) C6 0.119(13) 0.053(7) 0.075(9) 0.021(7) 0.041(9) 0.016(8) C7 0.079(10) 0.038(6) 0.081(9) 0.010(6) 0.038(8) 0.018(6) C8 0.109(11) 0.049(7) 0.063(9) 0.000(6) 0.048(8) 0.025(7) C10 0.101(11) 0.073(9) 0.085(10) 0.025(7) 0.046(8) 0.021(8) C11 0.088(11) 0.056(7) 0.084(9) 0.024(7) 0.025(8) 0.032(7) C13 0.090(10) 0.054(7) 0.082(10) 0.008(7) 0.031(8) 0.030(7) C14 0.106(10) 0.052(7) 0.062(8) 0.017(6) 0.027(7) 0.043(7) C16 0.097(11) 0.058(7) 0.074(9) 0.028(7) 0.039(8) 0.042(8) C17 0.113(11) 0.034(6) 0.076(9) 0.018(6) 0.045(8) 0.030(7) C18 0.083(9) 0.033(5) 0.057(8) 0.014(5) 0.020(7) 0.015(6) C19 0.082(9) 0.051(6) 0.035(7) 0.014(5) 0.011(6) 0.021(6) C20 0.088(10) 0.065(8) 0.075(9) 0.025(7) 0.035(8) 0.029(7) C21 0.112(11) 0.056(7) 0.047(7) 0.004(6) 0.016(7) 0.025(7) C22 0.102(10) 0.059(7) 0.057(8) 0.022(7) 0.039(8) 0.028(8) C23 0.097(11) 0.035(6) 0.079(10) 0.020(7) 0.042(8) 0.025(7) C24 0.083(10) 0.053(7) 0.070(9) 0.028(6) 0.018(7) 0.027(6) C25 0.088(10) 0.063(7) 0.066(8) 0.036(6) 0.032(7) 0.033(7) C27 0.070(8) 0.051(7) 0.045(7) 0.012(6) 0.017(6) 0.029(6) C28 0.081(8) 0.051(6) 0.056(7) 0.024(5) 0.032(6) 0.030(6) C29 0.081(8) 0.040(6) 0.053(7) 0.018(5) 0.027(7) 0.022(6) C30 0.125(11) 0.038(6) 0.050(7) 0.011(5) 0.047(7) 0.033(6) C31 0.137(13) 0.057(8) 0.084(10) 0.019(7) 0.062(9) 0.045(8) C32 0.206(16) 0.048(7) 0.083(9) 0.034(7) 0.096(10) 0.061(9) C33 0.132(11) 0.047(6) 0.086(9) 0.035(6) 0.061(9) 0.042(7) C34 0.100(10) 0.039(6) 0.071(9) 0.002(6) 0.033(8) 0.026(6) C36 0.124(12) 0.041(7) 0.101(11) 0.011(7) 0.062(9) 0.023(7) C37 0.125(12) 0.024(5) 0.129(12) 0.027(7) 0.071(10) 0.035(6) C39 0.125(12) 0.054(8) 0.145(13) 0.047(8) 0.083(11) 0.036(8) C40 0.109(11) 0.055(7) 0.089(10) 0.023(7) 0.048(8) 0.029(7) C42 0.124(13) 0.046(7) 0.063(9) 0.004(6) 0.063(9) 0.020(8) C43 0.081(10) 0.055(7) 0.066(9) -0.002(7) 0.043(8) 0.019(7) C44 0.086(10) 0.049(7) 0.061(9) 0.000(6) 0.045(8) 0.020(7) C45 0.071(9) 0.048(7) 0.042(7) 0.000(5) 0.019(6) 0.023(6) C46 0.097(12) 0.061(8) 0.097(11) 0.004(8) 0.050(10) 0.023(8) C47 0.074(10) 0.073(9) 0.078(10) 0.009(8) 0.026(8) 0.018(8) C48 0.100(12) 0.052(7) 0.080(10) -0.007(7) 0.054(9) 0.009(7) C49 0.117(12) 0.040(7) 0.075(10) 0.026(7) 0.060(10) 0.033(8) C50 0.134(13) 0.056(8) 0.096(12) 0.037(8) 0.063(11) 0.035(9) C51 0.091(10) 0.065(8) 0.071(9) 0.034(7) 0.016(8) 0.032(7) C54 0.077(8) 0.053(6) 0.050(7) 0.029(5) 0.012(6) 0.020(6) C55 0.119(12) 0.049(7) 0.073(9) 0.022(6) 0.044(9) 0.026(7) C57 0.085(9) 0.058(7) 0.087(9) 0.051(7) 0.003(7) 0.005(6) C58 0.107(12) 0.045(7) 0.125(13) 0.024(8) 0.033(10) 0.020(8) C60 0.075(9) 0.088(9) 0.074(9) 0.043(8) 0.018(7) 0.015(7) C61 0.108(12) 0.094(10) 0.061(9) 0.035(7) 0.035(8) 0.012(8) C64 0.110(12) 0.111(12) 0.117(12) 0.046(10) 0.050(10) 0.058(10) C65 0.140(17) 0.107(14) 0.40(4) 0.113(19) 0.18(2) 0.080(13) C67 0.072(10) 0.066(8) 0.123(13) -0.001(9) 0.038(9) 0.008(7) C68 0.107(14) 0.123(14) 0.092(12) 0.025(11) 0.028(10) 0.046(12) C70 0.104(11) 0.058(8) 0.124(13) 0.028(9) 0.044(10) 0.015(8) C71 0.097(11) 0.079(9) 0.099(11) 0.046(9) 0.038(9) 0.028(8) N9 0.097(8) 0.052(6) 0.069(7) 0.025(5) 0.045(6) 0.038(5) N12 0.099(9) 0.042(5) 0.074(7) 0.018(5) 0.038(7) 0.024(5) N15 0.095(8) 0.054(6) 0.086(8) 0.035(6) 0.050(7) 0.035(6) N26 0.085(7) 0.037(5) 0.064(6) 0.023(4) 0.017(5) 0.018(4) N35 0.081(7) 0.037(5) 0.078(7) 0.008(5) 0.035(6) 0.017(5) N38 0.114(9) 0.048(6) 0.104(9) 0.035(6) 0.055(8) 0.027(6) N41 0.098(9) 0.056(6) 0.093(9) 0.019(6) 0.044(7) 0.034(6) N52 0.098(8) 0.067(6) 0.074(8) 0.030(6) 0.025(7) 0.036(6) N53 0.091(8) 0.057(6) 0.069(7) 0.033(5) 0.030(6) 0.019(5) N56 0.093(8) 0.032(4) 0.067(6) 0.011(4) 0.034(6) 0.025(5) N59 0.097(9) 0.044(5) 0.098(8) 0.027(5) 0.025(7) 0.022(6) N62 0.107(9) 0.053(5) 0.072(7) 0.030(5) 0.036(6) 0.025(5) N63 0.090(8) 0.059(6) 0.091(8) 0.013(6) 0.033(6) 0.029(6) N66 0.099(10) 0.064(7) 0.149(11) 0.025(7) 0.027(8) 0.045(7) N69 0.117(11) 0.077(8) 0.100(9) 0.032(7) 0.024(8) 0.047(8) N72 0.093(8) 0.072(7) 0.097(8) 0.019(6) 0.043(7) 0.041(6) O1 0.083(6) 0.052(4) 0.077(6) 0.027(4) 0.039(5) 0.033(4) O2 0.087(6) 0.068(5) 0.082(6) 0.031(5) 0.040(5) 0.027(4) O3 0.088(6) 0.042(4) 0.088(6) 0.033(4) 0.049(5) 0.032(4) O4 0.088(6) 0.046(4) 0.069(5) 0.024(4) 0.037(5) 0.036(4) O5 0.084(6) 0.032(4) 0.072(6) 0.005(4) 0.029(5) 0.010(4) O6 0.098(7) 0.060(5) 0.069(5) 0.017(4) 0.019(5) 0.034(5) O7 0.113(7) 0.045(4) 0.094(6) 0.017(4) 0.066(6) 0.031(4) O8 0.114(7) 0.043(4) 0.076(6) 0.030(4) 0.044(5) 0.036(4) O9 0.104(6) 0.047(4) 0.072(5) 0.021(4) 0.048(5) 0.027(4) O10 0.095(7) 0.039(4) 0.086(6) 0.025(4) 0.046(5) 0.034(4) O11 0.092(7) 0.039(4) 0.080(6) 0.014(4) 0.038(5) 0.019(4) O12 0.132(8) 0.073(6) 0.091(7) 0.030(5) 0.044(6) 0.038(5) Ni1 0.0942(12) 0.0397(7) 0.0649(10) 0.0250(7) 0.0310(9) 0.0293(8) Ni2 0.0857(12) 0.0555(9) 0.0928(13) 0.0239(9) 0.0329(10) 0.0321(8) Er1 0.0892(4) 0.0356(3) 0.0701(4) 0.0172(2) 0.0405(3) 0.0297(2) N300 0.141(11) 0.146(12) 0.142(12) 0.049(8) 0.064(9) 0.019(9) N301 0.142(11) 0.129(11) 0.130(11) 0.055(8) 0.063(8) 0.017(9) O300 0.110(14) 0.121(15) 0.079(12) 0.032(11) 0.038(10) 0.038(12) O301 0.161(8) 0.204(9) 0.164(8) 0.076(7) 0.052(7) 0.014(7) O302 0.153(8) 0.158(8) 0.143(8) 0.068(6) 0.032(6) 0.023(7) O303 0.195(19) 0.21(2) 0.199(19) 0.066(15) 0.089(15) 0.035(16) N200 0.278(15) 0.255(15) 0.273(15) 0.086(10) 0.127(10) 0.048(10) O200 0.43(2) 0.37(2) 0.41(2) 0.175(18) 0.070(16) 0.099(18) O201 0.156(10) 0.148(9) 0.156(10) 0.081(8) 0.057(7) 0.070(8) O202 0.338(15) 0.122(9) 0.158(10) 0.092(8) 0.145(10) 0.101(9) N100 0.184(11) 0.162(10) 0.158(10) 0.050(8) 0.074(8) 0.041(9) O100 0.355(18) 0.228(15) 0.259(16) 0.101(13) 0.117(13) 0.110(14) O101 0.135(8) 0.078(6) 0.108(7) 0.025(5) 0.054(6) 0.039(6) O102 0.37(2) 0.45(3) 0.45(2) 0.111(17) 0.170(18) 0.150(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.228(13) . ? C1 O1 1.275(15) . ? C1 C2 1.490(17) . ? C2 C7 1.370(15) . ? C2 C3 1.422(15) . ? C3 O3 1.298(13) . ? C3 C4 1.447(16) . ? C4 C5 1.387(16) . ? C4 C8 1.452(16) . ? C5 C6 1.349(16) . ? C5 H5 0.9500 . ? C6 C7 1.427(17) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N9 1.271(15) . ? C8 H8 0.9500 . ? C10 N9 1.476(15) . ? C10 C11 1.551(15) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N12 1.438(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 N12 1.470(13) . ? C13 C14 1.475(16) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N15 1.467(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C16 N15 1.284(15) . ? C16 C17 1.425(16) . ? C16 H16 0.9500 . ? C17 C22 1.410(16) . ? C17 C18 1.459(13) . ? C18 O4 1.295(12) . ? C18 C19 1.445(14) . ? C19 C20 1.348(15) . ? C19 C23 1.541(13) . ? C20 C21 1.420(14) . ? C20 H20 0.9500 . ? C21 C22 1.353(15) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 O5 1.226(13) . ? C23 O6 1.255(13) . ? C24 N12 1.491(15) . ? C24 C25 1.518(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N26 1.481(13) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 O8 1.232(13) . ? C27 O7 1.281(13) . ? C27 C28 1.508(13) . ? C28 C33 1.390(15) . ? C28 C29 1.420(15) . ? C29 O9 1.280(12) . ? C29 C30 1.459(12) . ? C30 C34 1.399(16) . ? C30 C31 1.407(17) . ? C31 C32 1.379(17) . ? C31 H31 0.9500 . ? C32 C33 1.412(14) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N35 1.304(15) . ? C34 H34 0.9500 . ? C36 N35 1.459(15) . ? C36 C37 1.516(17) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 N38 1.472(14) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C39 N38 1.480(16) . ? C39 C40 1.540(15) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N41 1.470(15) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C42 N41 1.310(15) . ? C42 C43 1.451(17) . ? C42 H42 0.9500 . ? C43 C48 1.378(17) . ? C43 C44 1.404(17) . ? C44 O10 1.303(14) . ? C44 C45 1.461(16) . ? C45 C46 1.343(17) . ? C45 C49 1.468(17) . ? C46 C47 1.397(18) . ? C46 H46 0.9500 . ? C47 C48 1.434(17) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O11 1.216(15) . ? C49 O12 1.289(14) . ? C50 N38 1.470(16) . ? C50 C51 1.535(18) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 N52 1.415(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C54 N53 1.495(12) . ? C54 C55 1.537(15) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 N56 1.474(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C57 N53 1.481(13) . ? C57 C58 1.561(15) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 N59 1.429(16) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C60 N53 1.474(14) . ? C60 C61 1.542(16) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 N62 1.445(15) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C64 C65 1.38(2) . ? C64 N63 1.510(15) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N66 1.384(19) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C67 N63 1.468(15) . ? C67 C68 1.51(2) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 N69 1.496(19) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C70 C71 1.488(17) . ? C70 N63 1.499(16) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 N72 1.468(16) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? N26 Ni1 2.103(9) . ? N26 H26A 0.9200 . ? N26 H26B 0.9200 . ? N52 Ni2 2.091(11) . ? N52 H52A 0.9200 . ? N52 H52B 0.9200 . ? N53 Ni1 2.091(10) . ? N56 Ni1 2.098(9) . ? N56 H56A 0.9200 . ? N56 H56B 0.9200 . ? N59 Ni1 2.070(8) . ? N59 H59A 0.9200 . ? N59 H59B 0.9200 . ? N62 Ni1 2.134(10) . ? N62 H62A 0.9200 . ? N62 H62B 0.9200 . ? N63 Ni2 2.097(12) . ? N66 Ni2 2.110(10) . ? N66 H66A 0.9200 . ? N66 H66B 0.9200 . ? N69 Ni2 2.097(11) . ? N69 H69A 0.9200 . ? N69 H69B 0.9200 . ? N72 Ni2 2.109(11) . ? N72 H72A 0.9200 . ? N72 H72B 0.9200 . ? O1 Er1 2.318(8) . ? O3 Er1 2.355(7) . ? O3 H3 0.9500 . ? O4 Er1 2.300(7) . ? O4 H4 0.9500 . ? O5 Er1 2.323(8) . ? O6 Ni2 2.124(7) . ? O7 Er1 2.299(9) . ? O8 Ni1 2.116(7) . ? O9 Er1 2.294(7) . ? O9 H9 0.9500 . ? O10 Er1 2.349(8) . ? O10 H10 0.9500 . ? O11 Er1 2.310(9) . ? N300 O302 1.297(15) . ? N300 O300 1.316(15) . ? N300 O301 1.335(15) . ? N301 O303 1.304(14) . ? N301 O302 1.329(14) . ? N301 O301 1.356(14) . ? N200 O202 1.348(14) . ? N200 O200 1.389(15) . ? N200 O201 1.399(14) . ? N100 O101 1.304(14) . ? N100 O102 1.319(17) . ? N100 O100 1.340(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.2(13) . . ? O2 C1 C2 117.6(13) . . ? O1 C1 C2 119.1(12) . . ? C7 C2 C3 119.9(12) . . ? C7 C2 C1 119.2(11) . . ? C3 C2 C1 120.9(12) . . ? O3 C3 C2 122.6(11) . . ? O3 C3 C4 120.8(11) . . ? C2 C3 C4 116.6(12) . . ? C5 C4 C3 120.9(11) . . ? C5 C4 C8 121.5(13) . . ? C3 C4 C8 117.5(12) . . ? C6 C5 C4 121.9(13) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 118.0(13) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C2 C7 C6 122.5(12) . . ? C2 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? N9 C8 C4 125.0(13) . . ? N9 C8 H8 117.5 . . ? C4 C8 H8 117.5 . . ? N9 C10 C11 108.1(10) . . ? N9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? N9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N12 C11 C10 112.1(9) . . ? N12 C11 H11A 109.2 . . ? C10 C11 H11A 109.2 . . ? N12 C11 H11B 109.2 . . ? C10 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N12 C13 C14 112.3(10) . . ? N12 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N12 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? N15 C14 C13 110.3(10) . . ? N15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? N15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? N15 C16 C17 127.4(11) . . ? N15 C16 H16 116.3 . . ? C17 C16 H16 116.3 . . ? C22 C17 C16 119.1(10) . . ? C22 C17 C18 121.3(11) . . ? C16 C17 C18 119.6(12) . . ? O4 C18 C19 125.2(9) . . ? O4 C18 C17 119.7(10) . . ? C19 C18 C17 115.1(11) . . ? C20 C19 C18 120.2(10) . . ? C20 C19 C23 118.3(10) . . ? C18 C19 C23 121.2(10) . . ? C19 C20 C21 124.2(11) . . ? C19 C20 H20 117.9 . . ? C21 C20 H20 117.9 . . ? C22 C21 C20 117.8(12) . . ? C22 C21 H21 121.1 . . ? C20 C21 H21 121.1 . . ? C21 C22 C17 121.2(10) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? O5 C23 O6 126.3(9) . . ? O5 C23 C19 120.5(11) . . ? O6 C23 C19 113.1(11) . . ? N12 C24 C25 111.5(10) . . ? N12 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? N12 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N26 C25 C24 111.8(9) . . ? N26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? N26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? O8 C27 O7 126.2(9) . . ? O8 C27 C28 116.6(11) . . ? O7 C27 C28 117.2(11) . . ? C33 C28 C29 119.9(9) . . ? C33 C28 C27 116.0(10) . . ? C29 C28 C27 124.1(11) . . ? O9 C29 C28 124.6(9) . . ? O9 C29 C30 117.4(10) . . ? C28 C29 C30 118.0(11) . . ? C34 C30 C31 119.2(10) . . ? C34 C30 C29 122.2(11) . . ? C31 C30 C29 118.5(11) . . ? C32 C31 C30 123.5(10) . . ? C32 C31 H31 118.2 . . ? C30 C31 H31 118.2 . . ? C31 C32 C33 116.9(12) . . ? C31 C32 H32 121.6 . . ? C33 C32 H32 121.6 . . ? C28 C33 C32 123.1(11) . . ? C28 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? N35 C34 C30 126.3(10) . . ? N35 C34 H34 116.8 . . ? C30 C34 H34 116.8 . . ? N35 C36 C37 109.3(10) . . ? N35 C36 H36A 109.8 . . ? C37 C36 H36A 109.8 . . ? N35 C36 H36B 109.8 . . ? C37 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? N38 C37 C36 109.0(9) . . ? N38 C37 H37A 109.9 . . ? C36 C37 H37A 109.9 . . ? N38 C37 H37B 109.9 . . ? C36 C37 H37B 109.9 . . ? H37A C37 H37B 108.3 . . ? N38 C39 C40 110.9(10) . . ? N38 C39 H39A 109.5 . . ? C40 C39 H39A 109.5 . . ? N38 C39 H39B 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 108.0 . . ? N41 C40 C39 107.9(10) . . ? N41 C40 H40A 110.1 . . ? C39 C40 H40A 110.1 . . ? N41 C40 H40B 110.1 . . ? C39 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? N41 C42 C43 122.2(13) . . ? N41 C42 H42 118.9 . . ? C43 C42 H42 118.9 . . ? C48 C43 C44 122.5(14) . . ? C48 C43 C42 117.1(14) . . ? C44 C43 C42 120.2(13) . . ? O10 C44 C43 120.0(12) . . ? O10 C44 C45 121.7(13) . . ? C43 C44 C45 118.2(13) . . ? C46 C45 C44 116.3(14) . . ? C46 C45 C49 125.0(13) . . ? C44 C45 C49 118.6(12) . . ? C45 C46 C47 127.6(15) . . ? C45 C46 H46 116.2 . . ? C47 C46 H46 116.2 . . ? C46 C47 C48 115.3(13) . . ? C46 C47 H47 122.4 . . ? C48 C47 H47 122.4 . . ? C43 C48 C47 120.0(14) . . ? C43 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? O11 C49 O12 123.0(13) . . ? O11 C49 C45 123.1(13) . . ? O12 C49 C45 113.6(14) . . ? N38 C50 C51 112.1(11) . . ? N38 C50 H50A 109.2 . . ? C51 C50 H50A 109.2 . . ? N38 C50 H50B 109.2 . . ? C51 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? N52 C51 C50 114.7(11) . . ? N52 C51 H51A 108.6 . . ? C50 C51 H51A 108.6 . . ? N52 C51 H51B 108.6 . . ? C50 C51 H51B 108.6 . . ? H51A C51 H51B 107.6 . . ? N53 C54 C55 109.6(8) . . ? N53 C54 H54A 109.8 . . ? C55 C54 H54A 109.8 . . ? N53 C54 H54B 109.8 . . ? C55 C54 H54B 109.8 . . ? H54A C54 H54B 108.2 . . ? N56 C55 C54 110.6(10) . . ? N56 C55 H55A 109.5 . . ? C54 C55 H55A 109.5 . . ? N56 C55 H55B 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? N53 C57 C58 111.1(10) . . ? N53 C57 H57A 109.4 . . ? C58 C57 H57A 109.4 . . ? N53 C57 H57B 109.4 . . ? C58 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? N59 C58 C57 112.6(11) . . ? N59 C58 H58A 109.1 . . ? C57 C58 H58A 109.1 . . ? N59 C58 H58B 109.1 . . ? C57 C58 H58B 109.1 . . ? H58A C58 H58B 107.8 . . ? N53 C60 C61 109.2(10) . . ? N53 C60 H60A 109.8 . . ? C61 C60 H60A 109.8 . . ? N53 C60 H60B 109.8 . . ? C61 C60 H60B 109.8 . . ? H60A C60 H60B 108.3 . . ? N62 C61 C60 111.4(11) . . ? N62 C61 H61A 109.4 . . ? C60 C61 H61A 109.4 . . ? N62 C61 H61B 109.4 . . ? C60 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? C65 C64 N63 114.9(14) . . ? C65 C64 H64A 108.5 . . ? N63 C64 H64A 108.5 . . ? C65 C64 H64B 108.5 . . ? N63 C64 H64B 108.5 . . ? H64A C64 H64B 107.5 . . ? C64 C65 N66 122.3(13) . . ? C64 C65 H65A 106.8 . . ? N66 C65 H65A 106.8 . . ? C64 C65 H65B 106.8 . . ? N66 C65 H65B 106.8 . . ? H65A C65 H65B 106.6 . . ? N63 C67 C68 113.1(12) . . ? N63 C67 H67A 109.0 . . ? C68 C67 H67A 109.0 . . ? N63 C67 H67B 109.0 . . ? C68 C67 H67B 109.0 . . ? H67A C67 H67B 107.8 . . ? N69 C68 C67 107.5(12) . . ? N69 C68 H68A 110.2 . . ? C67 C68 H68A 110.2 . . ? N69 C68 H68B 110.2 . . ? C67 C68 H68B 110.2 . . ? H68A C68 H68B 108.5 . . ? C71 C70 N63 109.1(10) . . ? C71 C70 H70A 109.9 . . ? N63 C70 H70A 109.9 . . ? C71 C70 H70B 109.9 . . ? N63 C70 H70B 109.9 . . ? H70A C70 H70B 108.3 . . ? N72 C71 C70 112.7(12) . . ? N72 C71 H71A 109.0 . . ? C70 C71 H71A 109.0 . . ? N72 C71 H71B 109.0 . . ? C70 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? C8 N9 C10 125.8(12) . . ? C11 N12 C13 110.7(9) . . ? C11 N12 C24 112.7(10) . . ? C13 N12 C24 113.7(10) . . ? C16 N15 C14 123.6(10) . . ? C25 N26 Ni1 118.6(7) . . ? C25 N26 H26A 107.7 . . ? Ni1 N26 H26A 107.7 . . ? C25 N26 H26B 107.7 . . ? Ni1 N26 H26B 107.7 . . ? H26A N26 H26B 107.1 . . ? C34 N35 C36 123.3(9) . . ? C50 N38 C37 113.7(11) . . ? C50 N38 C39 111.6(11) . . ? C37 N38 C39 110.2(10) . . ? C42 N41 C40 123.5(12) . . ? C51 N52 Ni2 119.1(8) . . ? C51 N52 H52A 107.5 . . ? Ni2 N52 H52A 107.5 . . ? C51 N52 H52B 107.5 . . ? Ni2 N52 H52B 107.5 . . ? H52A N52 H52B 107.0 . . ? C60 N53 C57 111.3(10) . . ? C60 N53 C54 111.8(8) . . ? C57 N53 C54 109.5(8) . . ? C60 N53 Ni1 108.4(7) . . ? C57 N53 Ni1 109.7(7) . . ? C54 N53 Ni1 106.0(7) . . ? C55 N56 Ni1 111.0(7) . . ? C55 N56 H56A 109.4 . . ? Ni1 N56 H56A 109.4 . . ? C55 N56 H56B 109.4 . . ? Ni1 N56 H56B 109.4 . . ? H56A N56 H56B 108.0 . . ? C58 N59 Ni1 108.8(7) . . ? C58 N59 H59A 109.9 . . ? Ni1 N59 H59A 109.9 . . ? C58 N59 H59B 109.9 . . ? Ni1 N59 H59B 109.9 . . ? H59A N59 H59B 108.3 . . ? C61 N62 Ni1 111.4(7) . . ? C61 N62 H62A 109.3 . . ? Ni1 N62 H62A 109.3 . . ? C61 N62 H62B 109.3 . . ? Ni1 N62 H62B 109.3 . . ? H62A N62 H62B 108.0 . . ? C67 N63 C70 113.6(10) . . ? C67 N63 C64 111.8(10) . . ? C70 N63 C64 110.4(11) . . ? C67 N63 Ni2 104.9(9) . . ? C70 N63 Ni2 106.3(8) . . ? C64 N63 Ni2 109.4(8) . . ? C65 N66 Ni2 109.5(9) . . ? C65 N66 H66A 109.8 . . ? Ni2 N66 H66A 109.8 . . ? C65 N66 H66B 109.8 . . ? Ni2 N66 H66B 109.8 . . ? H66A N66 H66B 108.2 . . ? C68 N69 Ni2 111.0(10) . . ? C68 N69 H69A 109.4 . . ? Ni2 N69 H69A 109.4 . . ? C68 N69 H69B 109.4 . . ? Ni2 N69 H69B 109.4 . . ? H69A N69 H69B 108.0 . . ? C71 N72 Ni2 110.0(8) . . ? C71 N72 H72A 109.7 . . ? Ni2 N72 H72A 109.7 . . ? C71 N72 H72B 109.7 . . ? Ni2 N72 H72B 109.7 . . ? H72A N72 H72B 108.2 . . ? C1 O1 Er1 133.7(7) . . ? C3 O3 Er1 129.3(6) . . ? C3 O3 H3 115.4 . . ? Er1 O3 H3 115.4 . . ? C18 O4 Er1 137.0(6) . . ? C18 O4 H4 111.5 . . ? Er1 O4 H4 111.5 . . ? C23 O5 Er1 139.8(7) . . ? C23 O6 Ni2 131.6(7) . . ? C27 O7 Er1 140.7(7) . . ? C27 O8 Ni1 130.3(7) . . ? C29 O9 Er1 137.6(6) . . ? C29 O9 H9 111.2 . . ? Er1 O9 H9 111.2 . . ? C44 O10 Er1 130.1(7) . . ? C44 O10 H10 115.0 . . ? Er1 O10 H10 115.0 . . ? C49 O11 Er1 133.5(8) . . ? N59 Ni1 N53 84.6(4) . . ? N59 Ni1 N56 93.0(4) . . ? N53 Ni1 N56 83.1(4) . . ? N59 Ni1 N26 93.2(4) . . ? N53 Ni1 N26 176.8(3) . . ? N56 Ni1 N26 99.4(4) . . ? N59 Ni1 O8 173.5(4) . . ? N53 Ni1 O8 90.7(3) . . ? N56 Ni1 O8 90.8(3) . . ? N26 Ni1 O8 91.4(3) . . ? N59 Ni1 N62 92.7(4) . . ? N53 Ni1 N62 81.4(4) . . ? N56 Ni1 N62 162.9(4) . . ? N26 Ni1 N62 96.4(4) . . ? O8 Ni1 N62 82.2(3) . . ? N52 Ni2 N63 177.8(4) . . ? N52 Ni2 N69 95.7(5) . . ? N63 Ni2 N69 83.3(5) . . ? N52 Ni2 N72 99.1(4) . . ? N63 Ni2 N72 82.3(5) . . ? N69 Ni2 N72 162.6(5) . . ? N52 Ni2 N66 95.7(5) . . ? N63 Ni2 N66 82.5(5) . . ? N69 Ni2 N66 95.0(5) . . ? N72 Ni2 N66 92.7(4) . . ? N52 Ni2 O6 91.0(4) . . ? N63 Ni2 O6 90.7(3) . . ? N69 Ni2 O6 80.4(3) . . ? N72 Ni2 O6 90.2(3) . . ? N66 Ni2 O6 172.2(4) . . ? O9 Er1 O7 73.0(3) . . ? O9 Er1 O4 144.1(3) . . ? O7 Er1 O4 78.2(3) . . ? O9 Er1 O11 86.4(3) . . ? O7 Er1 O11 72.7(3) . . ? O4 Er1 O11 105.3(3) . . ? O9 Er1 O1 105.7(3) . . ? O7 Er1 O1 144.5(3) . . ? O4 Er1 O1 85.7(2) . . ? O11 Er1 O1 142.6(3) . . ? O9 Er1 O5 77.8(3) . . ? O7 Er1 O5 73.2(3) . . ? O4 Er1 O5 73.5(2) . . ? O11 Er1 O5 145.3(3) . . ? O1 Er1 O5 71.9(3) . . ? O9 Er1 O10 71.1(3) . . ? O7 Er1 O10 131.7(3) . . ? O4 Er1 O10 144.6(3) . . ? O11 Er1 O10 73.8(3) . . ? O1 Er1 O10 76.9(3) . . ? O5 Er1 O10 127.4(2) . . ? O9 Er1 O3 144.7(3) . . ? O7 Er1 O3 127.8(2) . . ? O4 Er1 O3 71.0(3) . . ? O11 Er1 O3 76.1(3) . . ? O1 Er1 O3 74.0(3) . . ? O5 Er1 O3 131.9(3) . . ? O10 Er1 O3 74.6(3) . . ? O302 N300 O300 110(2) . . ? O302 N300 O301 105.7(18) . . ? O300 N300 O301 145(2) . . ? O303 N301 O302 123.7(16) . . ? O303 N301 O301 127.0(17) . . ? O302 N301 O301 102.8(16) . . ? N300 O301 N301 67.0(17) . . ? N300 O302 N301 68.9(17) . . ? O202 N200 O200 116.3(13) . . ? O202 N200 O201 125.2(14) . . ? O200 N200 O201 115.9(12) . . ? O101 N100 O102 119.6(15) . . ? O101 N100 O100 116.5(13) . . ? O102 N100 O100 110.9(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 36.9(14) . . . . ? O1 C1 C2 C7 -140.0(10) . . . . ? O2 C1 C2 C3 -145.1(10) . . . . ? O1 C1 C2 C3 38.0(13) . . . . ? C7 C2 C3 O3 -179.3(9) . . . . ? C1 C2 C3 O3 2.7(14) . . . . ? C7 C2 C3 C4 0.8(13) . . . . ? C1 C2 C3 C4 -177.2(9) . . . . ? O3 C3 C4 C5 -178.4(9) . . . . ? C2 C3 C4 C5 1.5(13) . . . . ? O3 C3 C4 C8 3.2(13) . . . . ? C2 C3 C4 C8 -176.9(8) . . . . ? C3 C4 C5 C6 -0.5(15) . . . . ? C8 C4 C5 C6 177.8(10) . . . . ? C4 C5 C6 C7 -2.6(16) . . . . ? C3 C2 C7 C6 -4.1(15) . . . . ? C1 C2 C7 C6 173.9(9) . . . . ? C5 C6 C7 C2 5.0(15) . . . . ? C5 C4 C8 N9 179.0(10) . . . . ? C3 C4 C8 N9 -2.6(15) . . . . ? N9 C10 C11 N12 -57.6(14) . . . . ? N12 C13 C14 N15 -66.9(14) . . . . ? N15 C16 C17 C22 176.0(13) . . . . ? N15 C16 C17 C18 -5(2) . . . . ? C22 C17 C18 O4 174.8(11) . . . . ? C16 C17 C18 O4 -4.7(17) . . . . ? C22 C17 C18 C19 -6.3(17) . . . . ? C16 C17 C18 C19 174.2(11) . . . . ? O4 C18 C19 C20 -177.0(12) . . . . ? C17 C18 C19 C20 4.1(17) . . . . ? O4 C18 C19 C23 -3.6(18) . . . . ? C17 C18 C19 C23 177.6(10) . . . . ? C18 C19 C20 C21 -1(2) . . . . ? C23 C19 C20 C21 -174.4(11) . . . . ? C19 C20 C21 C22 -1(2) . . . . ? C20 C21 C22 C17 -1.6(19) . . . . ? C16 C17 C22 C21 -175.2(12) . . . . ? C18 C17 C22 C21 5.3(19) . . . . ? C20 C19 C23 O5 166.5(12) . . . . ? C18 C19 C23 O5 -7.1(18) . . . . ? C20 C19 C23 O6 -16.9(16) . . . . ? C18 C19 C23 O6 169.5(11) . . . . ? N12 C24 C25 N26 -176.4(8) . . . . ? O8 C27 C28 C33 -11.5(15) . . . . ? O7 C27 C28 C33 167.7(11) . . . . ? O8 C27 C28 C29 169.5(11) . . . . ? O7 C27 C28 C29 -11.3(16) . . . . ? C33 C28 C29 O9 -177.6(11) . . . . ? C27 C28 C29 O9 1.4(18) . . . . ? C33 C28 C29 C30 0.7(16) . . . . ? C27 C28 C29 C30 179.7(10) . . . . ? O9 C29 C30 C34 -7.6(17) . . . . ? C28 C29 C30 C34 173.9(11) . . . . ? O9 C29 C30 C31 175.7(11) . . . . ? C28 C29 C30 C31 -2.7(17) . . . . ? C34 C30 C31 C32 -172.0(13) . . . . ? C29 C30 C31 C32 5(2) . . . . ? C30 C31 C32 C33 -4(2) . . . . ? C29 C28 C33 C32 -0.6(19) . . . . ? C27 C28 C33 C32 -179.6(12) . . . . ? C31 C32 C33 C28 2(2) . . . . ? C31 C30 C34 N35 177.9(13) . . . . ? C29 C30 C34 N35 1(2) . . . . ? N35 C36 C37 N38 -69.0(14) . . . . ? N38 C39 C40 N41 -57.6(16) . . . . ? N41 C42 C43 C48 180.0(9) . . . . ? N41 C42 C43 C44 3.8(15) . . . . ? C48 C43 C44 O10 -179.8(9) . . . . ? C42 C43 C44 O10 -3.8(14) . . . . ? C48 C43 C44 C45 3.7(14) . . . . ? C42 C43 C44 C45 179.7(8) . . . . ? O10 C44 C45 C46 -177.4(9) . . . . ? C43 C44 C45 C46 -1.0(13) . . . . ? O10 C44 C45 C49 5.1(13) . . . . ? C43 C44 C45 C49 -178.5(9) . . . . ? C44 C45 C46 C47 -2.4(16) . . . . ? C49 C45 C46 C47 175.0(11) . . . . ? C45 C46 C47 C48 2.9(17) . . . . ? C44 C43 C48 C47 -3.2(15) . . . . ? C42 C43 C48 C47 -179.4(9) . . . . ? C46 C47 C48 C43 0.1(15) . . . . ? C46 C45 C49 O11 -141.1(12) . . . . ? C44 C45 C49 O11 36.2(14) . . . . ? C46 C45 C49 O12 33.2(14) . . . . ? C44 C45 C49 O12 -149.5(9) . . . . ? N38 C50 C51 N52 -178.9(9) . . . . ? N53 C54 C55 N56 -45.9(12) . . . . ? N53 C57 C58 N59 -40.1(16) . . . . ? N53 C60 C61 N62 44.5(14) . . . . ? N63 C64 C65 N66 12(3) . . . . ? N63 C67 C68 N69 49.2(15) . . . . ? N63 C70 C71 N72 -45.9(15) . . . . ? C4 C8 N9 C10 178.1(9) . . . . ? C11 C10 N9 C8 -110.3(13) . . . . ? C10 C11 N12 C13 154.6(11) . . . . ? C10 C11 N12 C24 -76.9(12) . . . . ? C14 C13 N12 C11 -94.4(12) . . . . ? C14 C13 N12 C24 137.6(11) . . . . ? C25 C24 N12 C11 166.3(8) . . . . ? C25 C24 N12 C13 -66.7(11) . . . . ? C17 C16 N15 C14 -178.8(11) . . . . ? C13 C14 N15 C16 -107.3(14) . . . . ? C24 C25 N26 Ni1 -176.7(6) . . . . ? C30 C34 N35 C36 179.3(12) . . . . ? C37 C36 N35 C34 -105.2(13) . . . . ? C51 C50 N38 C37 -71.7(12) . . . . ? C51 C50 N38 C39 162.9(9) . . . . ? C36 C37 N38 C50 141.8(11) . . . . ? C36 C37 N38 C39 -92.0(12) . . . . ? C40 C39 N38 C50 -79.2(13) . . . . ? C40 C39 N38 C37 153.5(11) . . . . ? C43 C42 N41 C40 176.8(9) . . . . ? C39 C40 N41 C42 -108.8(13) . . . . ? C50 C51 N52 Ni2 -174.9(7) . . . . ? C61 C60 N53 C57 76.3(12) . . . . ? C61 C60 N53 C54 -160.9(10) . . . . ? C61 C60 N53 Ni1 -44.5(11) . . . . ? C58 C57 N53 C60 -97.9(12) . . . . ? C58 C57 N53 C54 137.9(11) . . . . ? C58 C57 N53 Ni1 22.0(13) . . . . ? C55 C54 N53 C60 163.9(10) . . . . ? C55 C54 N53 C57 -72.2(12) . . . . ? C55 C54 N53 Ni1 46.1(10) . . . . ? C54 C55 N56 Ni1 21.9(10) . . . . ? C57 C58 N59 Ni1 36.8(13) . . . . ? C60 C61 N62 Ni1 -22.0(12) . . . . ? C68 C67 N63 C70 -161.6(12) . . . . ? C68 C67 N63 C64 72.6(16) . . . . ? C68 C67 N63 Ni2 -46.0(12) . . . . ? C71 C70 N63 C67 160.8(12) . . . . ? C71 C70 N63 C64 -72.6(15) . . . . ? C71 C70 N63 Ni2 46.0(12) . . . . ? C65 C64 N63 C67 -120.6(19) . . . . ? C65 C64 N63 C70 111.8(18) . . . . ? C65 C64 N63 Ni2 -5(2) . . . . ? C64 C65 N66 Ni2 -13(3) . . . . ? C67 C68 N69 Ni2 -26.2(13) . . . . ? C70 C71 N72 Ni2 21.8(12) . . . . ? O2 C1 O1 Er1 142.9(8) . . . . ? C2 C1 O1 Er1 -40.4(15) . . . . ? C2 C3 O3 Er1 -42.0(13) . . . . ? C4 C3 O3 Er1 137.9(7) . . . . ? C19 C18 O4 Er1 0.6(18) . . . . ? C17 C18 O4 Er1 179.4(8) . . . . ? O6 C23 O5 Er1 -152.5(9) . . . . ? C19 C23 O5 Er1 23.6(19) . . . . ? O5 C23 O6 Ni2 -12(2) . . . . ? C19 C23 O6 Ni2 171.8(8) . . . . ? O8 C27 O7 Er1 -156.2(9) . . . . ? C28 C27 O7 Er1 24.7(17) . . . . ? O7 C27 O8 Ni1 -8.0(18) . . . . ? C28 C27 O8 Ni1 171.1(7) . . . . ? C28 C29 O9 Er1 -1.0(18) . . . . ? C30 C29 O9 Er1 -179.3(7) . . . . ? C43 C44 O10 Er1 142.6(8) . . . . ? C45 C44 O10 Er1 -41.1(13) . . . . ? O12 C49 O11 Er1 144.8(9) . . . . ? C45 C49 O11 Er1 -41.4(16) . . . . ? C58 N59 Ni1 N53 -19.3(9) . . . . ? C58 N59 Ni1 N56 -102.1(9) . . . . ? C58 N59 Ni1 N26 158.3(9) . . . . ? C58 N59 Ni1 O8 24(4) . . . . ? C58 N59 Ni1 N62 61.8(9) . . . . ? C60 N53 Ni1 N59 119.4(7) . . . . ? C57 N53 Ni1 N59 -2.3(8) . . . . ? C54 N53 Ni1 N59 -120.5(7) . . . . ? C60 N53 Ni1 N56 -146.9(7) . . . . ? C57 N53 Ni1 N56 91.4(7) . . . . ? C54 N53 Ni1 N56 -26.8(6) . . . . ? C60 N53 Ni1 N26 72(7) . . . . ? C57 N53 Ni1 N26 -49(7) . . . . ? C54 N53 Ni1 N26 -167(6) . . . . ? C60 N53 Ni1 O8 -56.2(7) . . . . ? C57 N53 Ni1 O8 -177.9(7) . . . . ? C54 N53 Ni1 O8 63.9(6) . . . . ? C60 N53 Ni1 N62 25.8(7) . . . . ? C57 N53 Ni1 N62 -95.9(7) . . . . ? C54 N53 Ni1 N62 145.9(7) . . . . ? C55 N56 Ni1 N59 86.9(7) . . . . ? C55 N56 Ni1 N53 2.7(6) . . . . ? C55 N56 Ni1 N26 -179.3(6) . . . . ? C55 N56 Ni1 O8 -87.8(6) . . . . ? C55 N56 Ni1 N62 -22.6(15) . . . . ? C25 N26 Ni1 N59 87.5(7) . . . . ? C25 N26 Ni1 N53 134(6) . . . . ? C25 N26 Ni1 N56 -6.1(7) . . . . ? C25 N26 Ni1 O8 -97.1(7) . . . . ? C25 N26 Ni1 N62 -179.4(7) . . . . ? C27 O8 Ni1 N59 -154(3) . . . . ? C27 O8 Ni1 N53 -111.6(10) . . . . ? C27 O8 Ni1 N56 -28.5(10) . . . . ? C27 O8 Ni1 N26 70.9(10) . . . . ? C27 O8 Ni1 N62 167.1(10) . . . . ? C61 N62 Ni1 N59 -85.8(8) . . . . ? C61 N62 Ni1 N53 -1.7(8) . . . . ? C61 N62 Ni1 N56 23.7(16) . . . . ? C61 N62 Ni1 N26 -179.3(8) . . . . ? C61 N62 Ni1 O8 90.2(8) . . . . ? C51 N52 Ni2 N63 128(11) . . . . ? C51 N52 Ni2 N69 -171.6(8) . . . . ? C51 N52 Ni2 N72 -0.9(8) . . . . ? C51 N52 Ni2 N66 92.7(9) . . . . ? C51 N52 Ni2 O6 -91.2(8) . . . . ? C67 N63 Ni2 N52 84(11) . . . . ? C70 N63 Ni2 N52 -156(11) . . . . ? C64 N63 Ni2 N52 -37(11) . . . . ? C67 N63 Ni2 N69 22.8(8) . . . . ? C70 N63 Ni2 N69 143.4(8) . . . . ? C64 N63 Ni2 N69 -97.3(9) . . . . ? C67 N63 Ni2 N72 -147.5(8) . . . . ? C70 N63 Ni2 N72 -26.8(7) . . . . ? C64 N63 Ni2 N72 92.4(9) . . . . ? C67 N63 Ni2 N66 118.8(8) . . . . ? C70 N63 Ni2 N66 -120.6(8) . . . . ? C64 N63 Ni2 N66 -1.3(9) . . . . ? C67 N63 Ni2 O6 -57.4(7) . . . . ? C70 N63 Ni2 O6 63.2(7) . . . . ? C64 N63 Ni2 O6 -177.5(9) . . . . ? C68 N69 Ni2 N52 -175.9(9) . . . . ? C68 N69 Ni2 N63 2.2(9) . . . . ? C68 N69 Ni2 N72 36.2(19) . . . . ? C68 N69 Ni2 N66 -79.6(9) . . . . ? C68 N69 Ni2 O6 94.0(9) . . . . ? C71 N72 Ni2 N52 -178.3(7) . . . . ? C71 N72 Ni2 N63 3.4(7) . . . . ? C71 N72 Ni2 N69 -30.7(18) . . . . ? C71 N72 Ni2 N66 85.5(8) . . . . ? C71 N72 Ni2 O6 -87.2(8) . . . . ? C65 N66 Ni2 N52 -174.2(15) . . . . ? C65 N66 Ni2 N63 7.1(15) . . . . ? C65 N66 Ni2 N69 89.6(15) . . . . ? C65 N66 Ni2 N72 -74.8(15) . . . . ? C65 N66 Ni2 O6 36(4) . . . . ? C23 O6 Ni2 N52 74.8(11) . . . . ? C23 O6 Ni2 N63 -106.5(11) . . . . ? C23 O6 Ni2 N69 170.4(12) . . . . ? C23 O6 Ni2 N72 -24.3(12) . . . . ? C23 O6 Ni2 N66 -135(3) . . . . ? C29 O9 Er1 O7 5.5(11) . . . . ? C29 O9 Er1 O4 43.8(13) . . . . ? C29 O9 Er1 O11 -67.5(11) . . . . ? C29 O9 Er1 O1 148.5(11) . . . . ? C29 O9 Er1 O5 81.5(11) . . . . ? C29 O9 Er1 O10 -141.6(11) . . . . ? C29 O9 Er1 O3 -127.1(11) . . . . ? C27 O7 Er1 O9 -19.4(11) . . . . ? C27 O7 Er1 O4 -177.6(12) . . . . ? C27 O7 Er1 O11 72.1(11) . . . . ? C27 O7 Er1 O1 -112.7(11) . . . . ? C27 O7 Er1 O5 -101.5(11) . . . . ? C27 O7 Er1 O10 24.1(13) . . . . ? C27 O7 Er1 O3 128.0(10) . . . . ? C18 O4 Er1 O9 45.0(12) . . . . ? C18 O4 Er1 O7 82.3(11) . . . . ? C18 O4 Er1 O11 150.4(11) . . . . ? C18 O4 Er1 O1 -65.9(11) . . . . ? C18 O4 Er1 O5 6.5(10) . . . . ? C18 O4 Er1 O10 -126.1(11) . . . . ? C18 O4 Er1 O3 -140.5(11) . . . . ? C49 O11 Er1 O9 -61.2(12) . . . . ? C49 O11 Er1 O7 -134.5(12) . . . . ? C49 O11 Er1 O4 153.4(11) . . . . ? C49 O11 Er1 O1 50.1(13) . . . . ? C49 O11 Er1 O5 -123.6(11) . . . . ? C49 O11 Er1 O10 10.2(11) . . . . ? C49 O11 Er1 O3 87.9(12) . . . . ? C1 O1 Er1 O9 152.5(11) . . . . ? C1 O1 Er1 O7 -124.9(11) . . . . ? C1 O1 Er1 O4 -62.2(11) . . . . ? C1 O1 Er1 O11 47.4(12) . . . . ? C1 O1 Er1 O5 -136.3(11) . . . . ? C1 O1 Er1 O10 86.7(11) . . . . ? C1 O1 Er1 O3 9.3(10) . . . . ? C23 O5 Er1 O9 -178.3(12) . . . . ? C23 O5 Er1 O7 -102.6(12) . . . . ? C23 O5 Er1 O4 -20.3(12) . . . . ? C23 O5 Er1 O11 -113.5(12) . . . . ? C23 O5 Er1 O1 70.5(12) . . . . ? C23 O5 Er1 O10 127.2(11) . . . . ? C23 O5 Er1 O3 23.5(13) . . . . ? C44 O10 Er1 O9 122.7(10) . . . . ? C44 O10 Er1 O7 78.6(10) . . . . ? C44 O10 Er1 O4 -62.7(11) . . . . ? C44 O10 Er1 O11 31.0(9) . . . . ? C44 O10 Er1 O1 -125.4(9) . . . . ? C44 O10 Er1 O5 179.9(9) . . . . ? C44 O10 Er1 O3 -48.7(9) . . . . ? C3 O3 Er1 O9 -62.1(11) . . . . ? C3 O3 Er1 O7 -179.2(8) . . . . ? C3 O3 Er1 O4 123.5(9) . . . . ? C3 O3 Er1 O11 -124.6(9) . . . . ? C3 O3 Er1 O1 32.6(9) . . . . ? C3 O3 Er1 O5 78.9(10) . . . . ? C3 O3 Er1 O10 -47.9(9) . . . . ? O302 N300 O301 N301 -30(2) . . . . ? O300 N300 O301 N301 144(6) . . . . ? O303 N301 O301 N300 -179(4) . . . . ? O302 N301 O301 N300 29(2) . . . . ? O300 N300 O302 N301 -146(3) . . . . ? O301 N300 O302 N301 31(2) . . . . ? O303 N301 O302 N300 177(4) . . . . ? O301 N301 O302 N300 -30(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.882 _refine_diff_density_min -1.919 _refine_diff_density_rms 0.116 data_Lu _database_code_depnum_ccdc_archive 'CCDC 872219' #TrackingRef '15314_web_deposit_cif_file_0_KlausHarms_1352392481.Ni2_Ln_oct.cif' # start Validation Reply Form _vrf_PLAT316_Lu ; PROBLEM: Too many H on C in C=N Moiety in Main Residue .. C51 RESPONSE: The disorder of this CH2 group has not been resolved. ; # end Validation Reply Form #Added by publCIF (Do 23. Aug 10:04:25 2012) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H122 Lu N19 Ni2 O40' _chemical_formula_weight 1994.12 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' Lu Lu -0.4720 5.8584 '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 16.3087(6) _cell_length_b 16.3388(5) _cell_length_c 19.2433(7) _cell_angle_alpha 110.903(3) _cell_angle_beta 110.911(3) _cell_angle_gamma 90.224(3) _cell_volume 4423.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36150 _cell_measurement_theta_min 1.23 _cell_measurement_theta_max 27.07 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 1.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5340 _exptl_absorpt_correction_T_max 0.7758 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; PLATON/MULTISCAN ; _diffrn_ambient_temperature 100(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42995 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 25.12 _reflns_number_total 15710 _reflns_number_gt 10841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material 'ENCIFER, PUBLCIF' _refine_special_details ; Disordered water has been refined using split atom positons. Hydrogen atoms were not included. Restraints have been included for the geometry of the NO3-ions and the shape of the thermal ellipsoids of the anions and of the oxygen atoms of disordered water. Some unusual anisotropic displacement parameters and the remaining distorted geometries of the anions indicate disorder that has not been resolved (regarding atoms O100 O102 N200 O200 O301 O302 O413 O414 O415 O416 O417 O418 O419 O422 O423 O425 O426 O427 O428 O431 O436 O439 O440) 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^)+(0.0827P)^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 15710 _refine_ls_number_parameters 1225 _refine_ls_number_restraints 321 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0006(4) 0.2171(4) 0.3991(5) 0.0460(16) Uani 1 1 d . . . C3 C -0.1446(4) 0.2483(4) 0.3092(4) 0.0394(15) Uani 1 1 d . . . C4 C -0.2395(4) 0.2359(4) 0.2793(4) 0.0401(15) Uani 1 1 d . . . C5 C -0.2857(5) 0.1859(5) 0.3044(4) 0.0491(18) Uani 1 1 d . . . H5 H -0.3487 0.1763 0.2823 0.059 Uiso 1 1 calc R . . C6 C -0.2412(4) 0.1513(5) 0.3598(4) 0.0498(17) Uani 1 1 d . . . H6 H -0.2731 0.1182 0.3763 0.060 Uiso 1 1 calc R . . C7 C -0.1478(5) 0.1651(4) 0.3922(4) 0.0467(16) Uani 1 1 d . . . H7 H -0.1169 0.1428 0.4322 0.056 Uiso 1 1 calc R . . C8 C -0.2890(4) 0.2739(4) 0.2244(4) 0.0466(17) Uani 1 1 d . . . H8 H -0.3519 0.2641 0.2055 0.056 Uiso 1 1 calc R . . C10 C -0.2982(5) 0.3659(5) 0.1470(4) 0.0518(18) Uani 1 1 d . . . H10A H -0.3629 0.3470 0.1270 0.062 Uiso 1 1 calc R . . H10B H -0.2809 0.3488 0.0999 0.062 Uiso 1 1 calc R . . C11 C -0.2774(4) 0.4648(5) 0.1911(5) 0.0523(17) Uani 1 1 d . . . H11A H -0.3056 0.4936 0.1529 0.063 Uiso 1 1 calc R . . H11B H -0.3027 0.4826 0.2331 0.063 Uiso 1 1 calc R . . C13 C -0.1587(5) 0.5784(4) 0.3023(4) 0.0486(16) Uani 1 1 d . . . H13A H -0.2112 0.6095 0.2979 0.058 Uiso 1 1 calc R . . H13B H -0.1098 0.6183 0.3065 0.058 Uiso 1 1 calc R . . C14 C -0.1311(5) 0.5571(5) 0.3775(4) 0.0511(17) Uani 1 1 d . . . H14A H -0.1234 0.6117 0.4249 0.061 Uiso 1 1 calc R . . H14B H -0.1781 0.5138 0.3717 0.061 Uiso 1 1 calc R . . C16 C 0.0280(5) 0.5658(4) 0.4451(4) 0.0436(15) Uani 1 1 d . . . H16 H 0.0277 0.6252 0.4777 0.052 Uiso 1 1 calc R . . C17 C 0.1108(4) 0.5342(4) 0.4603(4) 0.0395(14) Uani 1 1 d . . . C18 C 0.1201(4) 0.4468(4) 0.4127(4) 0.0357(14) Uani 1 1 d . . . C19 C 0.2045(4) 0.4189(4) 0.4393(4) 0.0404(15) Uani 1 1 d . . . C20 C 0.2728(5) 0.4761(5) 0.5066(4) 0.0469(16) Uani 1 1 d . . . H20 H 0.3280 0.4558 0.5244 0.056 Uiso 1 1 calc R . . C21 C 0.2648(5) 0.5628(5) 0.5500(4) 0.0516(17) Uani 1 1 d . . . H21 H 0.3145 0.6015 0.5944 0.062 Uiso 1 1 calc R . . C22 C 0.1833(5) 0.5912(5) 0.5270(4) 0.0478(17) Uani 1 1 d . . . H22 H 0.1763 0.6494 0.5565 0.057 Uiso 1 1 calc R . . C23 C 0.2239(4) 0.3296(4) 0.3948(5) 0.0442(16) Uani 1 1 d . . . C24 C -0.1456(4) 0.5049(5) 0.1722(4) 0.0459(16) Uani 1 1 d . . . H24A H -0.1628 0.5588 0.1618 0.055 Uiso 1 1 calc R . . H24B H -0.1723 0.4532 0.1205 0.055 Uiso 1 1 calc R . . C25 C -0.0458(4) 0.5112(4) 0.2027(4) 0.0428(15) Uani 1 1 d . . . H25A H -0.0192 0.5659 0.2518 0.051 Uiso 1 1 calc R . . H25B H -0.0286 0.4601 0.2180 0.051 Uiso 1 1 calc R . . C27 C 0.1150(4) 0.3305(4) 0.1502(4) 0.0376(14) Uani 1 1 d . . . C28 C 0.1372(4) 0.2423(4) 0.1099(4) 0.0361(13) Uani 1 1 d . . . C29 C 0.1134(4) 0.1642(4) 0.1205(4) 0.0374(14) Uani 1 1 d . . . C30 C 0.1389(5) 0.0834(4) 0.0775(4) 0.0443(15) Uani 1 1 d . . . C31 C 0.1914(6) 0.0838(5) 0.0325(5) 0.062(2) Uani 1 1 d . . . H31 H 0.2102 0.0305 0.0067 0.075 Uiso 1 1 calc R . . C32 C 0.2153(6) 0.1602(5) 0.0259(5) 0.069(2) Uani 1 1 d . . . H32 H 0.2518 0.1606 -0.0029 0.083 Uiso 1 1 calc R . . C33 C 0.1849(5) 0.2377(5) 0.0624(4) 0.0502(17) Uani 1 1 d . . . H33 H 0.1978 0.2894 0.0541 0.060 Uiso 1 1 calc R . . C34 C 0.1125(5) 0.0019(4) 0.0779(4) 0.0546(19) Uani 1 1 d . . . H34 H 0.1330 -0.0487 0.0495 0.066 Uiso 1 1 calc R . . C36 C 0.0389(6) -0.0978(4) 0.1139(6) 0.065(2) Uani 1 1 d . . . H36A H 0.0464 -0.1449 0.0681 0.078 Uiso 1 1 calc R . . H36B H -0.0242 -0.1059 0.1069 0.078 Uiso 1 1 calc R . . C37 C 0.0956(6) -0.1057(5) 0.1901(6) 0.075(3) Uani 1 1 d . . . H37A H 0.1588 -0.0897 0.2010 0.090 Uiso 1 1 calc R . . H37B H 0.0863 -0.1678 0.1852 0.090 Uiso 1 1 calc R . . C39 C 0.0045(6) -0.0917(5) 0.2697(7) 0.079(3) Uani 1 1 d . . . H39A H 0.0331 -0.1215 0.3069 0.094 Uiso 1 1 calc R . . H39B H -0.0347 -0.1377 0.2176 0.094 Uiso 1 1 calc R . . C40 C -0.0513(7) -0.0264(6) 0.3044(6) 0.080(3) Uani 1 1 d . . . H40A H -0.0972 -0.0584 0.3118 0.095 Uiso 1 1 calc R . . H40B H -0.0129 0.0184 0.3576 0.095 Uiso 1 1 calc R . . C42 C -0.1768(5) 0.0028(5) 0.2014(5) 0.060(2) Uani 1 1 d . . . H42 H -0.2160 -0.0396 0.2025 0.071 Uiso 1 1 calc R . . C43 C -0.2130(5) 0.0458(5) 0.1486(5) 0.056(2) Uani 1 1 d . . . C44 C -0.1578(5) 0.1089(4) 0.1432(4) 0.0494(18) Uani 1 1 d . . . C45 C -0.1993(5) 0.1490(5) 0.0870(4) 0.056(2) Uani 1 1 d . . . C46 C -0.2886(6) 0.1262(6) 0.0399(5) 0.069(2) Uani 1 1 d . . . H46 H -0.3146 0.1527 0.0021 0.083 Uiso 1 1 calc R . . C47 C -0.3403(6) 0.0658(7) 0.0469(6) 0.085(3) Uani 1 1 d . . . H47 H -0.4020 0.0521 0.0142 0.102 Uiso 1 1 calc R . . C48 C -0.3059(6) 0.0234(6) 0.1003(5) 0.070(2) Uani 1 1 d . . . H48 H -0.3427 -0.0185 0.1044 0.084 Uiso 1 1 calc R . . C49 C -0.1454(6) 0.2182(5) 0.0799(5) 0.061(2) Uani 1 1 d . . . C50 C 0.1496(7) -0.0060(7) 0.3331(7) 0.095(3) Uani 1 1 d . . . H50A H 0.1868 -0.0516 0.3427 0.114 Uiso 1 1 calc R . . H50B H 0.1289 0.0183 0.3779 0.114 Uiso 1 1 calc R . . C51 C 0.2069(6) 0.0708(7) 0.3312(6) 0.080(3) Uani 1 1 d . . . H51A H 0.2296 0.0451 0.2879 0.095 Uiso 1 1 calc R . . H51B H 0.1678 0.1135 0.3173 0.095 Uiso 1 1 calc R . . C54 C 0.3048(5) 0.5097(5) 0.2637(4) 0.0512(17) Uani 1 1 d . . . H54A H 0.3700 0.5273 0.2888 0.061 Uiso 1 1 calc R . . H54B H 0.2921 0.4445 0.2344 0.061 Uiso 1 1 calc R . . C55 C 0.2674(4) 0.5353(5) 0.3285(4) 0.0492(17) Uani 1 1 d . . . H55A H 0.2844 0.4966 0.3593 0.059 Uiso 1 1 calc R . . H55B H 0.2923 0.5973 0.3662 0.059 Uiso 1 1 calc R . . C57 C 0.2958(5) 0.6496(5) 0.2429(5) 0.064(2) Uani 1 1 d . . . H57A H 0.3443 0.6629 0.2273 0.077 Uiso 1 1 calc R . . H57B H 0.3199 0.6689 0.3023 0.077 Uiso 1 1 calc R . . C58 C 0.2217(5) 0.7022(5) 0.2179(6) 0.076(3) Uani 1 1 d . . . H58A H 0.2404 0.7654 0.2544 0.091 Uiso 1 1 calc R . . H58B H 0.2102 0.6979 0.1625 0.091 Uiso 1 1 calc R . . C60 C 0.2804(5) 0.5082(6) 0.1298(5) 0.061(2) Uani 1 1 d . . . H60A H 0.2734 0.4433 0.1152 0.073 Uiso 1 1 calc R . . H60B H 0.3416 0.5283 0.1378 0.073 Uiso 1 1 calc R . . C61 C 0.2143(5) 0.5296(6) 0.0621(5) 0.065(2) Uani 1 1 d . . . H61A H 0.2315 0.5913 0.0696 0.078 Uiso 1 1 calc R . . H61B H 0.2151 0.4895 0.0099 0.078 Uiso 1 1 calc R . . C64 C 0.5382(5) 0.2397(6) 0.3873(6) 0.066(2) Uani 1 1 d . . . H64A H 0.5499 0.2526 0.3449 0.079 Uiso 1 1 calc R . . H64B H 0.5934 0.2611 0.4364 0.079 Uiso 1 1 calc R . . C65 C 0.5164(7) 0.1445(7) 0.3610(9) 0.112(4) Uani 1 1 d . . . H65A H 0.4987 0.1186 0.3018 0.134 Uiso 1 1 calc R . . H65B H 0.5717 0.1222 0.3844 0.134 Uiso 1 1 calc R . . C67 C 0.4990(6) 0.3565(6) 0.4876(6) 0.077(3) Uani 1 1 d . . . H67A H 0.4542 0.3963 0.4934 0.092 Uiso 1 1 calc R . . H67B H 0.5543 0.3928 0.4986 0.092 Uiso 1 1 calc R . . C68 C 0.5163(6) 0.3140(8) 0.5461(6) 0.094(3) Uani 1 1 d . . . H68A H 0.5676 0.2816 0.5463 0.113 Uiso 1 1 calc R . . H68B H 0.5314 0.3598 0.6008 0.113 Uiso 1 1 calc R . . C70 C 0.4215(6) 0.3271(6) 0.3444(6) 0.077(3) Uani 1 1 d . . . H70A H 0.4662 0.3594 0.3358 0.093 Uiso 1 1 calc R . . H70B H 0.3838 0.3696 0.3638 0.093 Uiso 1 1 calc R . . C71 C 0.3641(6) 0.2522(7) 0.2650(6) 0.080(3) Uani 1 1 d . . . H71A H 0.3247 0.2776 0.2279 0.096 Uiso 1 1 calc R . . H71B H 0.4026 0.2181 0.2393 0.096 Uiso 1 1 calc R . . C222 C -0.0993(4) 0.2109(4) 0.3666(4) 0.0421(15) Uani 1 1 d . . . N9 N -0.2516(4) 0.3219(4) 0.1989(3) 0.0450(13) Uani 1 1 d . . . N12 N -0.1804(3) 0.4959(4) 0.2292(3) 0.0436(13) Uani 1 1 d . . . N15 N -0.0479(4) 0.5203(4) 0.3899(3) 0.0444(13) Uani 1 1 d . . . N26 N -0.0087(3) 0.5122(3) 0.1426(3) 0.0407(12) Uani 1 1 d . . . H26A H -0.0299 0.5567 0.1255 0.049 Uiso 1 1 calc R . . H26B H -0.0318 0.4596 0.0987 0.049 Uiso 1 1 calc R . . N35 N 0.0622(4) -0.0103(3) 0.1141(4) 0.0540(16) Uani 1 1 d . . . N38 N 0.0735(5) -0.0463(4) 0.2574(5) 0.0692(19) Uani 1 1 d . . . N41 N -0.0929(5) 0.0165(4) 0.2497(4) 0.0609(17) Uani 1 1 d . . . N52 N 0.2763(5) 0.1152(6) 0.4009(6) 0.098(3) Uani 1 1 d . . . H52A H 0.3065 0.0743 0.4182 0.117 Uiso 1 1 calc R . . H52B H 0.2541 0.1465 0.4388 0.117 Uiso 1 1 calc R . . N53 N 0.2661(4) 0.5527(4) 0.2061(3) 0.0482(14) Uani 1 1 d . . . N56 N 0.1699(4) 0.5264(3) 0.2921(3) 0.0432(13) Uani 1 1 d . . . H56A H 0.1506 0.5719 0.3242 0.052 Uiso 1 1 calc R . . H56B H 0.1450 0.4738 0.2887 0.052 Uiso 1 1 calc R . . N59 N 0.1400(4) 0.6680(3) 0.2210(4) 0.0521(15) Uani 1 1 d . . . H59A H 0.0914 0.6853 0.1900 0.063 Uiso 1 1 calc R . . H59B H 0.1429 0.6896 0.2731 0.063 Uiso 1 1 calc R . . N62 N 0.1240(4) 0.5192(4) 0.0613(3) 0.0486(14) Uani 1 1 d . . . H62A H 0.0934 0.4648 0.0232 0.058 Uiso 1 1 calc R . . H62B H 0.0940 0.5623 0.0476 0.058 Uiso 1 1 calc R . . N63 N 0.4665(4) 0.2896(4) 0.4049(4) 0.0567(16) Uani 1 1 d . . . N66 N 0.4535(5) 0.1117(5) 0.3775(7) 0.098(3) Uani 1 1 d . . . H66A H 0.4796 0.0981 0.4222 0.118 Uiso 1 1 calc R . . H66B H 0.4219 0.0603 0.3349 0.118 Uiso 1 1 calc R . . N69 N 0.4386(5) 0.2526(6) 0.5253(5) 0.092(3) Uani 1 1 d . . . H69A H 0.4030 0.2813 0.5512 0.111 Uiso 1 1 calc R . . H69B H 0.4558 0.2066 0.5414 0.111 Uiso 1 1 calc R . . N72 N 0.3103(4) 0.1932(5) 0.2797(4) 0.0693(19) Uani 1 1 d . . . H72A H 0.3058 0.1357 0.2454 0.083 Uiso 1 1 calc R . . H72B H 0.2540 0.2081 0.2693 0.083 Uiso 1 1 calc R . . O1 O 0.0395(3) 0.2129(3) 0.3529(3) 0.0442(11) Uani 1 1 d . . . O2 O 0.0381(3) 0.2244(3) 0.4703(3) 0.0559(12) Uani 1 1 d . . . O3 O -0.1023(3) 0.2926(3) 0.2845(3) 0.0401(10) Uani 1 1 d . . . H3 H -0.1248 0.3447 0.2796 0.048 Uiso 1 1 calc R . . O4 O 0.0518(3) 0.3994(3) 0.3493(3) 0.0433(11) Uani 1 1 d . . . H4 H 0.0021 0.4302 0.3418 0.052 Uiso 1 1 calc R . . O5 O 0.1709(3) 0.2812(3) 0.3256(3) 0.0517(12) Uani 1 1 d . . . O6 O 0.2962(3) 0.3086(3) 0.4309(3) 0.0599(13) Uani 1 1 d . . . O7 O 0.0873(4) 0.3434(3) 0.2060(4) 0.0647(15) Uani 1 1 d . . . O8 O 0.1286(3) 0.3908(3) 0.1277(3) 0.0479(11) Uani 1 1 d . . . O9 O 0.0723(3) 0.1627(3) 0.1655(3) 0.0468(11) Uani 1 1 d . . . H9 H 0.0600 0.1043 0.1621 0.056 Uiso 1 1 calc R . . O10 O -0.0729(3) 0.1271(3) 0.1880(3) 0.0436(11) Uani 1 1 d . . . H10 H -0.0456 0.0781 0.1958 0.052 Uiso 1 1 calc R . . O11 O -0.0843(4) 0.2687(4) 0.1375(3) 0.0588(13) Uani 1 1 d . . . O12 O -0.1703(6) 0.2215(4) 0.0095(4) 0.100(2) Uani 1 1 d . . . N100 N 0.2024(8) 0.7697(7) 0.4250(6) 0.124(4) Uani 1 1 d D . . O100 O 0.1916(8) 0.8520(6) 0.4560(6) 0.155(4) Uani 1 1 d D . . O101 O 0.1324(6) 0.7106(5) 0.3881(5) 0.108(3) Uani 1 1 d D . . O102 O 0.2797(8) 0.7573(11) 0.4281(11) 0.283(11) Uani 1 1 d D . . N200 N 0.1040(13) 0.3051(17) 0.8787(13) 0.297(13) Uani 1 1 d DU . . O200 O 0.0605(13) 0.3021(16) 0.7957(10) 0.321(9) Uani 1 1 d DU . . O201 O 0.1701(5) 0.2574(6) 0.8818(4) 0.105(2) Uani 1 1 d DU . . O202 O 0.0382(6) 0.3274(5) 0.9087(6) 0.137(3) Uani 1 1 d DU . . N300 N 0.4306(9) 0.4749(9) 0.6973(7) 0.067(4) Uani 0.50 1 d PDU A 1 O300 O 0.3753(7) 0.4044(8) 0.6564(6) 0.069(3) Uani 0.50 1 d PDU A 1 O301 O 0.4798(7) 0.5026(7) 0.7737(6) 0.154(4) Uani 1 1 d DU . . O302 O 0.4579(8) 0.5060(7) 0.6622(7) 0.176(4) Uani 1 1 d DU . . N301 N 0.4609(12) 0.5498(10) 0.7326(9) 0.097(6) Uani 0.50 1 d PDU A 2 O303 O 0.4481(14) 0.6234(12) 0.7478(10) 0.141(7) Uani 0.50 1 d PDU A 2 Ni1 Ni 0.12904(5) 0.52955(5) 0.17635(5) 0.03851(19) Uani 1 1 d . . . Ni2 Ni 0.36721(6) 0.20301(6) 0.39869(7) 0.0604(3) Uani 1 1 d . . . Lu1 Lu 0.020357(18) 0.260986(17) 0.250972(19) 0.03799(10) Uani 1 1 d . . . O401 O 0.0593(4) 0.6712(4) 0.0027(4) 0.089(2) Uani 1 1 d U . . O402 O -0.0123(5) 0.7899(5) 0.4025(4) 0.101(2) Uani 1 1 d U . . O403 O 0.7797(6) 0.7609(7) 0.4639(6) 0.080(2) Uani 0.75 1 d PU B 1 O404 O 0.8370(6) 0.7783(6) 0.2731(5) 0.126(3) Uani 1 1 d U . . O405 O 0.5853(7) 0.6553(7) 0.8479(6) 0.064(3) Uani 0.50 1 d PU . . O406 O 0.6542(6) 0.6665(7) 0.0051(6) 0.148(4) Uani 1 1 d U . . O407 O 0.3290(8) -0.0039(10) 0.1686(7) 0.141(5) Uani 0.75 1 d PU C 4 O408 O 0.4959(6) 0.1972(8) 0.1118(7) 0.133(4) Uani 0.75 1 d PU D 1 O409 O 0.0746(9) 0.9797(7) 0.4929(8) 0.134(4) Uani 0.75 1 d PU . . O410 O 0.5308(8) 0.7791(10) 0.0415(9) 0.142(5) Uani 0.75 1 d PU E 1 O411 O 0.6968(9) 0.2604(11) 0.9094(9) 0.099(5) Uani 0.50 1 d PU F 1 O412 O 0.7008(10) 0.7614(9) 0.3134(9) 0.101(5) Uani 0.50 1 d PU . . O413 O 0.526(3) 0.964(2) 0.8435(19) 0.189(14) Uani 0.50 1 d PU . . O414 O 0.5745(13) 0.9313(9) 0.1802(10) 0.182(6) Uani 0.75 1 d PU . . O415 O 0.5898(15) 0.415(2) 0.9828(16) 0.164(8) Uani 0.50 1 d PU G 2 O416 O 0.6102(15) 0.1255(14) 0.5533(14) 0.174(9) Uani 0.50 1 d PU H 1 O417 O 0.638(4) 0.267(3) 0.925(3) 0.151(15) Uani 0.25 1 d PU I 2 O418 O 0.3680(18) 0.017(2) 0.5311(18) 0.231(12) Uani 0.50 1 d PU J 2 O419 O 0.4679(17) 0.8444(15) 0.3383(16) 0.186(9) Uani 0.50 1 d PU . . O420 O 0.6992(18) 0.9029(19) 0.265(2) 0.099(8) Uani 0.25 1 d PU . . O422 O 0.3973(17) -0.0974(19) 0.1972(17) 0.214(11) Uani 0.50 1 d PU K 3 O423 O 0.3577(15) -0.0773(15) 0.2805(16) 0.196(10) Uani 0.50 1 d PU L 1 O424 O 0.5727(12) 0.3317(15) 0.9194(14) 0.133(6) Uani 0.50 1 d PU M 1 O425 O 0.5622(18) 0.6359(18) 0.1856(14) 0.182(9) Uani 0.50 1 d PU N 1 O426 O 0.3297(16) 0.3066(18) 0.8022(15) 0.187(9) Uani 0.50 1 d PU O 1 O427 O 0.222(2) 0.0608(19) 0.5710(16) 0.210(11) Uani 0.50 1 d PU P 1 O428 O 0.4619(16) 0.3123(19) 0.7479(16) 0.186(10) Uani 0.50 1 d PU Q 2 O429 O 0.278(2) -0.068(2) 0.1420(17) 0.096(9) Uani 0.25 1 d PU R 1 O431 O 0.6014(13) 0.5180(17) 1.0225(11) 0.153(8) Uani 0.50 1 d PU S 1 O433 O 0.4893(18) 0.0806(17) 0.1488(14) 0.140(9) Uani 0.50 1 d PU T 2 O435 O 0.3385(17) 0.3475(16) 0.6367(16) 0.074(7) Uani 0.25 1 d PU U 2 O436 O 0.608(3) 0.929(3) 0.327(3) 0.165(16) Uani 0.25 1 d PU . . O437 O 0.799(2) 0.823(2) 0.494(2) 0.096(10) Uani 0.25 1 d PU V 2 O439 O 0.508(3) 0.843(3) 0.019(3) 0.152(14) Uani 0.25 1 d PU W 2 O440 O 0.472(3) 0.370(3) 0.055(3) 0.157(15) Uani 0.25 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(4) 0.033(3) 0.062(5) 0.019(3) 0.029(4) 0.010(3) C3 0.041(3) 0.025(3) 0.047(4) -0.003(3) 0.029(3) 0.002(3) C4 0.042(3) 0.032(3) 0.044(4) 0.003(3) 0.025(3) 0.005(3) C5 0.045(4) 0.045(4) 0.053(4) 0.004(3) 0.029(3) -0.003(3) C6 0.048(4) 0.047(4) 0.061(4) 0.016(4) 0.035(4) 0.001(3) C7 0.055(4) 0.037(4) 0.054(4) 0.014(3) 0.030(3) 0.005(3) C8 0.043(4) 0.039(4) 0.050(4) 0.000(3) 0.027(3) 0.002(3) C10 0.044(4) 0.059(4) 0.046(4) 0.009(4) 0.021(3) 0.006(3) C11 0.046(4) 0.055(4) 0.063(5) 0.023(4) 0.029(3) 0.019(3) C13 0.056(4) 0.040(4) 0.055(4) 0.016(3) 0.030(3) 0.020(3) C14 0.054(4) 0.046(4) 0.059(4) 0.015(3) 0.032(4) 0.018(3) C16 0.060(4) 0.040(4) 0.038(4) 0.014(3) 0.027(3) 0.011(3) C17 0.050(4) 0.035(3) 0.040(3) 0.014(3) 0.025(3) 0.009(3) C18 0.042(3) 0.033(3) 0.040(3) 0.016(3) 0.023(3) 0.003(3) C19 0.048(4) 0.038(3) 0.047(4) 0.020(3) 0.028(3) 0.009(3) C20 0.050(4) 0.055(4) 0.048(4) 0.028(4) 0.023(3) 0.014(3) C21 0.062(4) 0.047(4) 0.042(4) 0.011(3) 0.023(3) 0.009(3) C22 0.064(4) 0.044(4) 0.036(4) 0.011(3) 0.024(3) 0.010(3) C23 0.044(4) 0.034(3) 0.065(5) 0.020(4) 0.031(4) 0.005(3) C24 0.048(4) 0.043(4) 0.053(4) 0.024(3) 0.021(3) 0.015(3) C25 0.050(4) 0.040(4) 0.048(4) 0.020(3) 0.026(3) 0.016(3) C27 0.037(3) 0.030(3) 0.046(4) 0.013(3) 0.018(3) 0.007(2) C28 0.041(3) 0.031(3) 0.033(3) 0.009(3) 0.015(3) 0.011(3) C29 0.040(3) 0.028(3) 0.039(3) 0.004(3) 0.017(3) 0.002(2) C30 0.060(4) 0.031(3) 0.042(4) 0.007(3) 0.026(3) 0.008(3) C31 0.099(6) 0.035(4) 0.065(5) 0.006(4) 0.059(5) 0.014(4) C32 0.118(7) 0.049(4) 0.074(5) 0.023(4) 0.073(5) 0.023(4) C33 0.077(5) 0.039(4) 0.048(4) 0.018(3) 0.036(4) 0.017(3) C34 0.072(5) 0.030(3) 0.054(4) -0.001(3) 0.032(4) 0.003(3) C36 0.079(5) 0.021(3) 0.100(7) 0.012(4) 0.053(5) 0.002(3) C37 0.079(6) 0.027(4) 0.130(8) 0.031(5) 0.053(6) 0.009(4) C39 0.087(6) 0.045(5) 0.125(8) 0.041(5) 0.056(6) 0.005(4) C40 0.103(7) 0.052(5) 0.112(7) 0.039(5) 0.066(6) 0.010(5) C42 0.066(5) 0.037(4) 0.073(5) -0.005(4) 0.050(5) -0.009(3) C43 0.067(5) 0.043(4) 0.058(5) 0.000(4) 0.042(4) 0.002(3) C44 0.058(4) 0.030(3) 0.052(4) -0.009(3) 0.038(4) -0.001(3) C45 0.055(4) 0.048(4) 0.038(4) -0.010(3) 0.013(3) 0.019(3) C46 0.072(5) 0.060(5) 0.050(5) -0.005(4) 0.022(4) 0.012(4) C47 0.070(6) 0.084(7) 0.063(6) -0.017(5) 0.028(5) 0.009(5) C48 0.068(5) 0.055(5) 0.064(5) -0.014(4) 0.038(5) -0.007(4) C49 0.097(6) 0.051(5) 0.056(5) 0.022(4) 0.050(5) 0.036(5) C50 0.090(7) 0.087(7) 0.138(10) 0.065(7) 0.055(7) -0.002(6) C51 0.070(6) 0.086(7) 0.091(7) 0.044(6) 0.030(5) 0.013(5) C54 0.051(4) 0.063(5) 0.056(4) 0.039(4) 0.024(3) 0.017(3) C55 0.046(4) 0.057(4) 0.052(4) 0.032(4) 0.017(3) 0.008(3) C57 0.050(4) 0.069(5) 0.077(5) 0.047(5) 0.010(4) -0.005(4) C58 0.066(5) 0.046(4) 0.107(7) 0.037(5) 0.017(5) -0.010(4) C60 0.057(4) 0.090(6) 0.063(5) 0.047(5) 0.035(4) 0.020(4) C61 0.058(5) 0.091(6) 0.067(5) 0.049(5) 0.028(4) 0.009(4) C64 0.046(4) 0.072(6) 0.081(6) 0.024(5) 0.030(4) 0.011(4) C65 0.082(7) 0.072(7) 0.183(12) 0.012(7) 0.090(8) 0.022(5) C67 0.051(5) 0.072(6) 0.089(7) 0.013(5) 0.022(5) 0.006(4) C68 0.068(6) 0.123(9) 0.073(6) 0.022(6) 0.021(5) 0.028(6) C70 0.074(6) 0.067(6) 0.116(8) 0.052(6) 0.048(6) 0.015(4) C71 0.078(6) 0.100(7) 0.080(6) 0.050(6) 0.035(5) 0.036(5) C222 0.045(4) 0.033(3) 0.050(4) 0.008(3) 0.028(3) 0.003(3) N9 0.048(3) 0.042(3) 0.045(3) 0.012(3) 0.023(3) 0.011(2) N12 0.045(3) 0.043(3) 0.048(3) 0.016(3) 0.025(3) 0.013(2) N15 0.051(3) 0.045(3) 0.053(3) 0.024(3) 0.034(3) 0.020(3) N26 0.051(3) 0.031(3) 0.042(3) 0.014(2) 0.020(2) 0.007(2) N35 0.063(4) 0.026(3) 0.076(4) 0.008(3) 0.041(3) 0.001(2) N38 0.084(5) 0.041(4) 0.094(5) 0.031(4) 0.042(4) -0.002(3) N41 0.089(5) 0.033(3) 0.074(4) 0.015(3) 0.052(4) 0.012(3) N52 0.079(5) 0.083(6) 0.146(8) 0.047(6) 0.056(6) 0.008(4) N53 0.045(3) 0.057(4) 0.053(3) 0.035(3) 0.017(3) 0.010(3) N56 0.058(3) 0.029(3) 0.052(3) 0.017(3) 0.031(3) 0.011(2) N59 0.057(3) 0.032(3) 0.060(4) 0.022(3) 0.009(3) 0.002(2) N62 0.051(3) 0.049(3) 0.057(4) 0.032(3) 0.022(3) 0.010(3) N63 0.042(3) 0.052(4) 0.070(4) 0.019(3) 0.020(3) 0.006(3) N66 0.066(5) 0.067(5) 0.189(9) 0.060(6) 0.069(5) 0.031(4) N69 0.086(6) 0.123(7) 0.106(6) 0.077(6) 0.046(5) 0.045(5) N72 0.046(4) 0.069(4) 0.074(5) 0.006(4) 0.023(3) 0.007(3) O1 0.044(2) 0.041(2) 0.055(3) 0.018(2) 0.028(2) 0.0087(19) O2 0.054(3) 0.066(3) 0.057(3) 0.028(3) 0.028(3) 0.011(2) O3 0.044(2) 0.026(2) 0.058(3) 0.014(2) 0.031(2) 0.0087(17) O4 0.043(2) 0.031(2) 0.061(3) 0.013(2) 0.029(2) 0.0106(19) O5 0.041(2) 0.031(2) 0.080(4) 0.012(2) 0.028(3) 0.006(2) O6 0.052(3) 0.052(3) 0.073(3) 0.021(3) 0.023(3) 0.018(2) O7 0.098(4) 0.027(2) 0.102(4) 0.018(3) 0.082(4) 0.013(2) O8 0.073(3) 0.038(2) 0.052(3) 0.026(2) 0.035(2) 0.022(2) O9 0.060(3) 0.024(2) 0.073(3) 0.012(2) 0.049(3) 0.0089(19) O10 0.049(3) 0.027(2) 0.059(3) 0.011(2) 0.030(2) 0.0050(19) O11 0.070(3) 0.059(3) 0.065(3) 0.029(3) 0.039(3) 0.024(3) O12 0.164(7) 0.075(4) 0.062(4) 0.026(3) 0.045(4) 0.033(4) N100 0.210(14) 0.104(9) 0.072(6) 0.033(6) 0.072(8) 0.054(9) O100 0.253(13) 0.104(7) 0.161(9) 0.058(7) 0.129(9) 0.049(8) O101 0.174(8) 0.066(5) 0.101(6) 0.019(4) 0.082(6) 0.027(5) O102 0.174(12) 0.37(2) 0.32(2) 0.107(18) 0.132(13) 0.184(15) N200 0.30(3) 0.41(4) 0.41(2) 0.33(3) 0.22(2) 0.24(2) O200 0.382(18) 0.344(18) 0.269(13) 0.174(14) 0.101(11) 0.169(15) O201 0.099(5) 0.122(6) 0.101(5) 0.056(5) 0.034(4) 0.004(4) O202 0.129(6) 0.077(5) 0.191(8) 0.066(6) 0.029(6) 0.019(4) N300 0.066(7) 0.074(8) 0.051(7) 0.030(6) 0.006(6) -0.005(6) O300 0.069(7) 0.082(8) 0.040(6) 0.007(6) 0.019(5) -0.012(6) O301 0.138(7) 0.186(8) 0.163(7) 0.109(7) 0.045(5) 0.011(6) O302 0.174(8) 0.173(8) 0.171(8) 0.084(7) 0.039(6) 0.006(6) N301 0.125(10) 0.100(10) 0.116(9) 0.056(8) 0.087(8) 0.004(7) O303 0.169(14) 0.187(16) 0.134(12) 0.083(12) 0.110(11) 0.087(12) Ni1 0.0469(5) 0.0293(4) 0.0473(5) 0.0202(4) 0.0215(4) 0.0085(3) Ni2 0.0475(5) 0.0442(5) 0.1021(8) 0.0320(5) 0.0388(5) 0.0140(4) Lu1 0.04390(16) 0.02362(13) 0.05499(18) 0.01172(11) 0.03183(13) 0.00735(10) O401 0.095(4) 0.055(3) 0.061(4) -0.009(3) -0.002(3) 0.031(3) O402 0.099(5) 0.133(6) 0.068(4) 0.044(4) 0.024(3) -0.017(4) O403 0.060(5) 0.104(7) 0.084(6) 0.037(6) 0.035(4) 0.020(5) O404 0.147(7) 0.113(6) 0.119(6) 0.075(5) 0.024(5) -0.018(5) O405 0.080(7) 0.064(6) 0.067(6) 0.032(5) 0.044(6) 0.022(5) O406 0.115(6) 0.173(9) 0.135(7) 0.042(7) 0.043(5) 0.015(6) O407 0.104(8) 0.149(10) 0.111(8) -0.003(7) 0.029(6) 0.040(8) O408 0.058(5) 0.128(8) 0.136(8) -0.010(7) 0.014(5) 0.011(5) O409 0.211(12) 0.094(7) 0.146(9) 0.073(7) 0.094(8) 0.044(7) O410 0.125(9) 0.131(10) 0.175(11) 0.047(9) 0.074(8) -0.006(7) O411 0.077(8) 0.128(11) 0.113(10) 0.091(9) 0.017(7) -0.014(7) O412 0.104(9) 0.088(9) 0.117(10) 0.063(8) 0.026(8) 0.003(7) O413 0.20(2) 0.19(2) 0.133(16) 0.070(16) 0.001(13) -0.010(16) O414 0.274(15) 0.113(9) 0.213(13) 0.074(9) 0.141(12) 0.033(9) O415 0.139(14) 0.245(19) 0.158(15) 0.106(14) 0.084(12) 0.076(14) O416 0.175(15) 0.132(13) 0.170(15) 0.077(12) -0.005(12) 0.010(12) O417 0.18(2) 0.13(2) 0.14(2) 0.047(17) 0.057(18) 0.029(19) O418 0.191(17) 0.29(2) 0.223(19) 0.140(16) 0.045(13) 0.128(16) O419 0.190(16) 0.137(14) 0.210(17) 0.080(13) 0.039(13) -0.025(12) O420 0.093(14) 0.093(15) 0.162(19) 0.063(14) 0.091(14) 0.020(11) O422 0.155(15) 0.195(18) 0.205(18) 0.015(14) 0.036(14) -0.063(14) O423 0.157(14) 0.141(14) 0.244(18) -0.001(13) 0.102(13) -0.080(11) O424 0.100(10) 0.142(13) 0.168(14) 0.091(12) 0.032(10) -0.016(10) O425 0.228(18) 0.198(17) 0.153(14) 0.121(14) 0.054(13) 0.021(14) O426 0.165(16) 0.193(17) 0.181(16) 0.077(14) 0.038(12) 0.040(14) O427 0.24(2) 0.213(18) 0.194(17) 0.127(15) 0.057(14) 0.018(15) O428 0.162(15) 0.208(18) 0.191(16) 0.030(13) 0.117(13) 0.036(13) O429 0.101(16) 0.099(16) 0.082(15) 0.017(13) 0.046(13) -0.002(13) O431 0.150(13) 0.212(17) 0.110(11) 0.112(12) 0.017(9) -0.029(12) O433 0.131(14) 0.131(15) 0.093(12) 0.011(11) 0.002(10) 0.027(13) O435 0.089(14) 0.054(12) 0.107(15) 0.030(11) 0.071(12) 0.016(10) O436 0.14(2) 0.17(2) 0.18(2) 0.031(17) 0.089(18) 0.035(17) O437 0.082(15) 0.107(17) 0.094(17) 0.026(14) 0.038(12) 0.037(14) O439 0.13(2) 0.12(2) 0.18(2) 0.068(18) 0.021(16) -0.012(16) O440 0.13(2) 0.17(2) 0.15(2) 0.041(17) 0.054(16) 0.022(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.246(8) . ? C1 O1 1.264(8) . ? C1 C222 1.493(9) . ? C3 O3 1.306(7) . ? C3 C222 1.429(10) . ? C3 C4 1.430(9) . ? C4 C5 1.415(9) . ? C4 C8 1.420(10) . ? C5 C6 1.365(10) . ? C5 H5 0.9500 . ? C6 C7 1.408(9) . ? C6 H6 0.9500 . ? C7 C222 1.401(9) . ? C7 H7 0.9500 . ? C8 N9 1.309(8) . ? C8 H8 0.9500 . ? C10 N9 1.438(9) . ? C10 C11 1.502(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N12 1.482(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 N12 1.487(8) . ? C13 C14 1.520(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N15 1.462(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C16 N15 1.305(8) . ? C16 C17 1.417(9) . ? C16 H16 0.9500 . ? C17 C22 1.402(9) . ? C17 C18 1.438(9) . ? C18 O4 1.295(7) . ? C18 C19 1.425(9) . ? C19 C20 1.374(9) . ? C19 C23 1.507(9) . ? C20 C21 1.399(10) . ? C20 H20 0.9500 . ? C21 C22 1.382(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 O5 1.252(8) . ? C23 O6 1.256(8) . ? C24 N12 1.453(9) . ? C24 C25 1.509(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N26 1.490(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 O8 1.257(7) . ? C27 O7 1.259(8) . ? C27 C28 1.489(8) . ? C28 C33 1.381(9) . ? C28 C29 1.435(8) . ? C29 O9 1.277(7) . ? C29 C30 1.439(9) . ? C30 C34 1.400(9) . ? C30 C31 1.421(10) . ? C31 C32 1.366(10) . ? C31 H31 0.9500 . ? C32 C33 1.399(10) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N35 1.306(9) . ? C34 H34 0.9500 . ? C36 N35 1.476(8) . ? C36 C37 1.479(13) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 N38 1.480(11) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C39 N38 1.475(9) . ? C39 C40 1.532(13) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N41 1.443(11) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C42 N41 1.315(10) . ? C42 C43 1.400(12) . ? C42 H42 0.9500 . ? C43 C44 1.421(10) . ? C43 C48 1.429(11) . ? C44 O10 1.308(8) . ? C44 C45 1.430(11) . ? C45 C46 1.376(11) . ? C45 C49 1.503(12) . ? C46 C47 1.369(14) . ? C46 H46 0.9500 . ? C47 C48 1.397(14) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O11 1.206(10) . ? C49 O12 1.290(10) . ? C50 N38 1.454(12) . ? C50 C51 1.580(12) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 N52 1.350(12) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C54 N53 1.477(8) . ? C54 C55 1.509(10) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 N56 1.473(8) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C57 N53 1.479(10) . ? C57 C58 1.523(12) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 N59 1.473(10) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C60 N53 1.490(10) . ? C60 C61 1.519(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 N62 1.476(9) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C64 C65 1.451(13) . ? C64 N63 1.497(10) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N66 1.338(12) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C67 N63 1.469(11) . ? C67 C68 1.470(14) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 N69 1.454(13) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C70 N63 1.474(11) . ? C70 C71 1.531(13) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 N72 1.463(11) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? N26 Ni1 2.091(5) . ? N26 H26A 0.9200 . ? N26 H26B 0.9200 . ? N52 Ni2 2.081(7) . ? N52 H52A 0.9200 . ? N52 H52B 0.9200 . ? N53 Ni1 2.096(5) . ? N56 Ni1 2.106(5) . ? N56 H56A 0.9200 . ? N56 H56B 0.9200 . ? N59 Ni1 2.095(5) . ? N59 H59A 0.9200 . ? N59 H59B 0.9200 . ? N62 Ni1 2.130(6) . ? N62 H62A 0.9200 . ? N62 H62B 0.9200 . ? N63 Ni2 2.089(6) . ? N66 Ni2 2.089(7) . ? N66 H66A 0.9200 . ? N66 H66B 0.9200 . ? N69 Ni2 2.122(9) . ? N69 H69A 0.9200 . ? N69 H69B 0.9200 . ? N72 Ni2 2.086(7) . ? N72 H72A 0.9200 . ? N72 H72B 0.9200 . ? O1 Lu1 2.286(4) . ? O3 Lu1 2.319(4) . ? O3 H3 0.9500 . ? O4 Lu1 2.280(4) . ? O4 H4 0.9500 . ? O5 Lu1 2.311(5) . ? O6 Ni2 2.113(5) . ? O7 Lu1 2.291(4) . ? O8 Ni1 2.121(4) . ? O9 Lu1 2.262(4) . ? O9 H9 0.9500 . ? O10 Lu1 2.309(4) . ? O10 H10 0.9500 . ? O11 Lu1 2.288(6) . ? N100 O102 1.262(11) . ? N100 O101 1.290(10) . ? N100 O100 1.303(10) . ? N200 O201 1.330(12) . ? N200 O202 1.383(12) . ? N200 O200 1.482(14) . ? N300 O302 1.170(12) . ? N300 O300 1.264(12) . ? N300 O301 1.300(11) . ? O301 N301 1.256(13) . ? O302 N301 1.269(13) . ? N301 O303 1.171(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.1(6) . . ? O2 C1 C222 118.2(6) . . ? O1 C1 C222 118.6(7) . . ? O3 C3 C222 122.3(5) . . ? O3 C3 C4 120.3(6) . . ? C222 C3 C4 117.5(5) . . ? C5 C4 C8 118.9(6) . . ? C5 C4 C3 120.4(6) . . ? C8 C4 C3 120.7(6) . . ? C6 C5 C4 121.2(6) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 119.4(6) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C222 C7 C6 121.3(7) . . ? C222 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? N9 C8 C4 122.9(6) . . ? N9 C8 H8 118.6 . . ? C4 C8 H8 118.6 . . ? N9 C10 C11 110.8(6) . . ? N9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N9 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N12 C11 C10 111.7(6) . . ? N12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? N12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? N12 C13 C14 110.5(5) . . ? N12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N15 C14 C13 110.3(6) . . ? N15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? N15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? N15 C16 C17 125.5(6) . . ? N15 C16 H16 117.3 . . ? C17 C16 H16 117.3 . . ? C22 C17 C16 116.4(6) . . ? C22 C17 C18 121.2(6) . . ? C16 C17 C18 122.3(6) . . ? O4 C18 C19 124.9(6) . . ? O4 C18 C17 118.1(6) . . ? C19 C18 C17 117.0(5) . . ? C20 C19 C18 119.6(6) . . ? C20 C19 C23 117.6(6) . . ? C18 C19 C23 122.8(6) . . ? C19 C20 C21 123.1(7) . . ? C19 C20 H20 118.4 . . ? C21 C20 H20 118.4 . . ? C22 C21 C20 118.7(7) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C21 C22 C17 120.2(7) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? O5 C23 O6 123.3(6) . . ? O5 C23 C19 120.9(6) . . ? O6 C23 C19 115.8(6) . . ? N12 C24 C25 112.0(5) . . ? N12 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N12 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N26 C25 C24 113.3(5) . . ? N26 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? N26 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? O8 C27 O7 122.8(6) . . ? O8 C27 C28 116.5(6) . . ? O7 C27 C28 120.6(5) . . ? C33 C28 C29 119.7(6) . . ? C33 C28 C27 117.4(6) . . ? C29 C28 C27 122.8(5) . . ? O9 C29 C28 124.2(6) . . ? O9 C29 C30 119.0(5) . . ? C28 C29 C30 116.8(5) . . ? C34 C30 C31 117.7(6) . . ? C34 C30 C29 121.7(6) . . ? C31 C30 C29 120.6(6) . . ? C32 C31 C30 120.7(7) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 118.9(7) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C28 C33 C32 122.9(6) . . ? C28 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? N35 C34 C30 125.3(7) . . ? N35 C34 H34 117.3 . . ? C30 C34 H34 117.3 . . ? N35 C36 C37 110.9(6) . . ? N35 C36 H36A 109.4 . . ? C37 C36 H36A 109.4 . . ? N35 C36 H36B 109.4 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C36 C37 N38 110.1(7) . . ? C36 C37 H37A 109.6 . . ? N38 C37 H37A 109.6 . . ? C36 C37 H37B 109.6 . . ? N38 C37 H37B 109.6 . . ? H37A C37 H37B 108.2 . . ? N38 C39 C40 111.4(6) . . ? N38 C39 H39A 109.3 . . ? C40 C39 H39A 109.3 . . ? N38 C39 H39B 109.3 . . ? C40 C39 H39B 109.3 . . ? H39A C39 H39B 108.0 . . ? N41 C40 C39 109.0(8) . . ? N41 C40 H40A 109.9 . . ? C39 C40 H40A 109.9 . . ? N41 C40 H40B 109.9 . . ? C39 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? N41 C42 C43 125.0(7) . . ? N41 C42 H42 117.5 . . ? C43 C42 H42 117.5 . . ? C42 C43 C44 120.3(7) . . ? C42 C43 C48 118.0(7) . . ? C44 C43 C48 121.7(8) . . ? O10 C44 C43 119.8(7) . . ? O10 C44 C45 123.1(6) . . ? C43 C44 C45 117.0(7) . . ? C46 C45 C44 121.0(8) . . ? C46 C45 C49 119.2(8) . . ? C44 C45 C49 119.8(6) . . ? C47 C46 C45 120.7(10) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C46 C47 C48 122.5(9) . . ? C46 C47 H47 118.8 . . ? C48 C47 H47 118.8 . . ? C47 C48 C43 117.1(8) . . ? C47 C48 H48 121.5 . . ? C43 C48 H48 121.5 . . ? O11 C49 O12 122.6(8) . . ? O11 C49 C45 121.4(7) . . ? O12 C49 C45 115.9(8) . . ? N38 C50 C51 110.7(8) . . ? N38 C50 H50A 109.5 . . ? C51 C50 H50A 109.5 . . ? N38 C50 H50B 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? N52 C51 C50 114.6(9) . . ? N52 C51 H51A 108.6 . . ? C50 C51 H51A 108.6 . . ? N52 C51 H51B 108.6 . . ? C50 C51 H51B 108.6 . . ? H51A C51 H51B 107.6 . . ? N53 C54 C55 111.3(6) . . ? N53 C54 H54A 109.4 . . ? C55 C54 H54A 109.4 . . ? N53 C54 H54B 109.4 . . ? C55 C54 H54B 109.4 . . ? H54A C54 H54B 108.0 . . ? N56 C55 C54 110.1(6) . . ? N56 C55 H55A 109.6 . . ? C54 C55 H55A 109.6 . . ? N56 C55 H55B 109.6 . . ? C54 C55 H55B 109.6 . . ? H55A C55 H55B 108.2 . . ? N53 C57 C58 113.1(6) . . ? N53 C57 H57A 109.0 . . ? C58 C57 H57A 109.0 . . ? N53 C57 H57B 109.0 . . ? C58 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? N59 C58 C57 110.5(6) . . ? N59 C58 H58A 109.6 . . ? C57 C58 H58A 109.6 . . ? N59 C58 H58B 109.6 . . ? C57 C58 H58B 109.6 . . ? H58A C58 H58B 108.1 . . ? N53 C60 C61 110.4(7) . . ? N53 C60 H60A 109.6 . . ? C61 C60 H60A 109.6 . . ? N53 C60 H60B 109.6 . . ? C61 C60 H60B 109.6 . . ? H60A C60 H60B 108.1 . . ? N62 C61 C60 110.4(6) . . ? N62 C61 H61A 109.6 . . ? C60 C61 H61A 109.6 . . ? N62 C61 H61B 109.6 . . ? C60 C61 H61B 109.6 . . ? H61A C61 H61B 108.1 . . ? C65 C64 N63 113.4(7) . . ? C65 C64 H64A 108.9 . . ? N63 C64 H64A 108.9 . . ? C65 C64 H64B 108.9 . . ? N63 C64 H64B 108.9 . . ? H64A C64 H64B 107.7 . . ? N66 C65 C64 119.8(8) . . ? N66 C65 H65A 107.4 . . ? C64 C65 H65A 107.4 . . ? N66 C65 H65B 107.4 . . ? C64 C65 H65B 107.4 . . ? H65A C65 H65B 106.9 . . ? N63 C67 C68 110.7(8) . . ? N63 C67 H67A 109.5 . . ? C68 C67 H67A 109.5 . . ? N63 C67 H67B 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 108.1 . . ? N69 C68 C67 110.2(8) . . ? N69 C68 H68A 109.6 . . ? C67 C68 H68A 109.6 . . ? N69 C68 H68B 109.6 . . ? C67 C68 H68B 109.6 . . ? H68A C68 H68B 108.1 . . ? N63 C70 C71 109.4(7) . . ? N63 C70 H70A 109.8 . . ? C71 C70 H70A 109.8 . . ? N63 C70 H70B 109.8 . . ? C71 C70 H70B 109.8 . . ? H70A C70 H70B 108.2 . . ? N72 C71 C70 110.3(7) . . ? N72 C71 H71A 109.6 . . ? C70 C71 H71A 109.6 . . ? N72 C71 H71B 109.6 . . ? C70 C71 H71B 109.6 . . ? H71A C71 H71B 108.1 . . ? C7 C222 C3 120.0(6) . . ? C7 C222 C1 118.3(6) . . ? C3 C222 C1 121.6(5) . . ? C8 N9 C10 125.1(6) . . ? C24 N12 C11 111.7(5) . . ? C24 N12 C13 112.9(5) . . ? C11 N12 C13 110.5(5) . . ? C16 N15 C14 122.6(6) . . ? C25 N26 Ni1 119.0(4) . . ? C25 N26 H26A 107.6 . . ? Ni1 N26 H26A 107.6 . . ? C25 N26 H26B 107.6 . . ? Ni1 N26 H26B 107.6 . . ? H26A N26 H26B 107.0 . . ? C34 N35 C36 122.6(6) . . ? C50 N38 C39 109.8(7) . . ? C50 N38 C37 114.1(8) . . ? C39 N38 C37 111.7(6) . . ? C42 N41 C40 127.7(7) . . ? C51 N52 Ni2 117.2(7) . . ? C51 N52 H52A 108.0 . . ? Ni2 N52 H52A 108.0 . . ? C51 N52 H52B 108.0 . . ? Ni2 N52 H52B 108.0 . . ? H52A N52 H52B 107.2 . . ? C54 N53 C57 112.1(6) . . ? C54 N53 C60 111.5(6) . . ? C57 N53 C60 113.3(6) . . ? C54 N53 Ni1 104.3(4) . . ? C57 N53 Ni1 108.6(5) . . ? C60 N53 Ni1 106.4(4) . . ? C55 N56 Ni1 110.3(4) . . ? C55 N56 H56A 109.6 . . ? Ni1 N56 H56A 109.6 . . ? C55 N56 H56B 109.6 . . ? Ni1 N56 H56B 109.6 . . ? H56A N56 H56B 108.1 . . ? C58 N59 Ni1 107.1(5) . . ? C58 N59 H59A 110.3 . . ? Ni1 N59 H59A 110.3 . . ? C58 N59 H59B 110.3 . . ? Ni1 N59 H59B 110.3 . . ? H59A N59 H59B 108.5 . . ? C61 N62 Ni1 110.8(4) . . ? C61 N62 H62A 109.5 . . ? Ni1 N62 H62A 109.5 . . ? C61 N62 H62B 109.5 . . ? Ni1 N62 H62B 109.5 . . ? H62A N62 H62B 108.1 . . ? C67 N63 C70 112.5(7) . . ? C67 N63 C64 111.9(6) . . ? C70 N63 C64 112.3(7) . . ? C67 N63 Ni2 105.0(5) . . ? C70 N63 Ni2 105.2(4) . . ? C64 N63 Ni2 109.6(5) . . ? C65 N66 Ni2 110.8(6) . . ? C65 N66 H66A 109.5 . . ? Ni2 N66 H66A 109.5 . . ? C65 N66 H66B 109.5 . . ? Ni2 N66 H66B 109.5 . . ? H66A N66 H66B 108.1 . . ? C68 N69 Ni2 108.9(6) . . ? C68 N69 H69A 109.9 . . ? Ni2 N69 H69A 109.9 . . ? C68 N69 H69B 109.9 . . ? Ni2 N69 H69B 109.9 . . ? H69A N69 H69B 108.3 . . ? C71 N72 Ni2 110.7(5) . . ? C71 N72 H72A 109.5 . . ? Ni2 N72 H72A 109.5 . . ? C71 N72 H72B 109.5 . . ? Ni2 N72 H72B 109.5 . . ? H72A N72 H72B 108.1 . . ? C1 O1 Lu1 135.1(4) . . ? C3 O3 Lu1 128.5(4) . . ? C3 O3 H3 115.7 . . ? Lu1 O3 H3 115.7 . . ? C18 O4 Lu1 136.3(4) . . ? C18 O4 H4 111.8 . . ? Lu1 O4 H4 111.8 . . ? C23 O5 Lu1 137.0(4) . . ? C23 O6 Ni2 134.5(5) . . ? C27 O7 Lu1 138.1(4) . . ? C27 O8 Ni1 131.7(4) . . ? C29 O9 Lu1 137.5(4) . . ? C29 O9 H9 111.2 . . ? Lu1 O9 H9 111.2 . . ? C44 O10 Lu1 129.5(4) . . ? C44 O10 H10 115.3 . . ? Lu1 O10 H10 115.3 . . ? C49 O11 Lu1 135.4(5) . . ? O102 N100 O101 126.5(11) . . ? O102 N100 O100 115.9(11) . . ? O101 N100 O100 117.3(10) . . ? O201 N200 O202 142.5(14) . . ? O201 N200 O200 108.9(12) . . ? O202 N200 O200 102.0(11) . . ? O302 N300 O300 117.3(11) . . ? O302 N300 O301 113.4(10) . . ? O300 N300 O301 126.0(11) . . ? N301 O301 N300 54.4(10) . . ? N300 O302 N301 57.0(10) . . ? O303 N301 O301 132.6(14) . . ? O303 N301 O302 117.5(12) . . ? O301 N301 O302 109.9(11) . . ? N26 Ni1 N59 93.1(2) . . ? N26 Ni1 N53 176.1(2) . . ? N59 Ni1 N53 84.4(2) . . ? N26 Ni1 N56 100.1(2) . . ? N59 Ni1 N56 92.8(2) . . ? N53 Ni1 N56 83.0(2) . . ? N26 Ni1 O8 91.65(19) . . ? N59 Ni1 O8 174.3(2) . . ? N53 Ni1 O8 90.7(2) . . ? N56 Ni1 O8 89.44(19) . . ? N26 Ni1 N62 95.0(2) . . ? N59 Ni1 N62 93.8(2) . . ? N53 Ni1 N62 82.2(2) . . ? N56 Ni1 N62 163.1(2) . . ? O8 Ni1 N62 82.7(2) . . ? N52 Ni2 N72 101.5(3) . . ? N52 Ni2 N63 175.1(3) . . ? N72 Ni2 N63 83.0(3) . . ? N52 Ni2 N66 95.1(3) . . ? N72 Ni2 N66 94.8(4) . . ? N63 Ni2 N66 82.6(3) . . ? N52 Ni2 O6 91.2(3) . . ? N72 Ni2 O6 88.8(3) . . ? N63 Ni2 O6 90.8(2) . . ? N66 Ni2 O6 171.9(3) . . ? N52 Ni2 N69 93.5(4) . . ? N72 Ni2 N69 162.6(3) . . ? N63 Ni2 N69 82.3(3) . . ? N66 Ni2 N69 92.6(4) . . ? O6 Ni2 N69 82.0(3) . . ? O9 Lu1 O4 143.94(15) . . ? O9 Lu1 O1 106.20(16) . . ? O4 Lu1 O1 84.83(16) . . ? O9 Lu1 O11 85.39(18) . . ? O4 Lu1 O11 106.44(18) . . ? O1 Lu1 O11 143.14(17) . . ? O9 Lu1 O7 74.48(15) . . ? O4 Lu1 O7 77.11(16) . . ? O1 Lu1 O7 144.52(19) . . ? O11 Lu1 O7 72.0(2) . . ? O9 Lu1 O10 70.90(14) . . ? O4 Lu1 O10 144.70(15) . . ? O1 Lu1 O10 76.24(15) . . ? O11 Lu1 O10 74.90(18) . . ? O7 Lu1 O10 133.33(18) . . ? O9 Lu1 O5 76.44(17) . . ? O4 Lu1 O5 74.62(16) . . ? O1 Lu1 O5 72.09(16) . . ? O11 Lu1 O5 144.44(18) . . ? O7 Lu1 O5 73.8(2) . . ? O10 Lu1 O5 125.11(16) . . ? O9 Lu1 O3 144.95(14) . . ? O4 Lu1 O3 70.76(14) . . ? O1 Lu1 O3 74.98(15) . . ? O11 Lu1 O3 76.03(17) . . ? O7 Lu1 O3 125.15(16) . . ? O10 Lu1 O3 75.63(14) . . ? O5 Lu1 O3 133.67(17) . . ? 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 C3 C4 C5 178.4(5) . . . . ? C222 C3 C4 C5 -1.9(9) . . . . ? O3 C3 C4 C8 -2.0(9) . . . . ? C222 C3 C4 C8 177.7(6) . . . . ? C8 C4 C5 C6 -177.1(6) . . . . ? C3 C4 C5 C6 2.5(10) . . . . ? C4 C5 C6 C7 -0.4(10) . . . . ? C5 C6 C7 C222 -2.4(10) . . . . ? C5 C4 C8 N9 179.2(6) . . . . ? C3 C4 C8 N9 -0.4(9) . . . . ? N9 C10 C11 N12 53.6(8) . . . . ? N12 C13 C14 N15 65.6(7) . . . . ? N15 C16 C17 C22 -174.6(6) . . . . ? N15 C16 C17 C18 2.6(10) . . . . ? C22 C17 C18 O4 -176.2(5) . . . . ? C16 C17 C18 O4 6.8(9) . . . . ? C22 C17 C18 C19 3.9(8) . . . . ? C16 C17 C18 C19 -173.2(6) . . . . ? O4 C18 C19 C20 178.3(5) . . . . ? C17 C18 C19 C20 -1.7(8) . . . . ? O4 C18 C19 C23 0.8(9) . . . . ? C17 C18 C19 C23 -179.3(5) . . . . ? C18 C19 C20 C21 -1.9(10) . . . . ? C23 C19 C20 C21 175.7(6) . . . . ? C19 C20 C21 C22 3.5(10) . . . . ? C20 C21 C22 C17 -1.3(10) . . . . ? C16 C17 C22 C21 174.8(6) . . . . ? C18 C17 C22 C21 -2.4(10) . . . . ? C20 C19 C23 O5 -166.3(6) . . . . ? C18 C19 C23 O5 11.2(9) . . . . ? C20 C19 C23 O6 12.5(8) . . . . ? C18 C19 C23 O6 -170.0(6) . . . . ? N12 C24 C25 N26 174.8(5) . . . . ? O8 C27 C28 C33 11.3(9) . . . . ? O7 C27 C28 C33 -166.2(6) . . . . ? O8 C27 C28 C29 -170.6(6) . . . . ? O7 C27 C28 C29 12.0(9) . . . . ? C33 C28 C29 O9 177.4(6) . . . . ? C27 C28 C29 O9 -0.7(10) . . . . ? C33 C28 C29 C30 -2.2(9) . . . . ? C27 C28 C29 C30 179.7(6) . . . . ? O9 C29 C30 C34 6.0(10) . . . . ? C28 C29 C30 C34 -174.4(6) . . . . ? O9 C29 C30 C31 -174.5(7) . . . . ? C28 C29 C30 C31 5.1(10) . . . . ? C34 C30 C31 C32 176.4(8) . . . . ? C29 C30 C31 C32 -3.2(12) . . . . ? C30 C31 C32 C33 -1.8(13) . . . . ? C29 C28 C33 C32 -2.8(11) . . . . ? C27 C28 C33 C32 175.4(7) . . . . ? C31 C32 C33 C28 4.9(13) . . . . ? C31 C30 C34 N35 -177.9(8) . . . . ? C29 C30 C34 N35 1.7(12) . . . . ? N35 C36 C37 N38 69.1(8) . . . . ? N38 C39 C40 N41 59.2(10) . . . . ? N41 C42 C43 C44 1.0(11) . . . . ? N41 C42 C43 C48 -179.8(7) . . . . ? C42 C43 C44 O10 -0.3(10) . . . . ? C48 C43 C44 O10 -179.5(6) . . . . ? C42 C43 C44 C45 179.1(6) . . . . ? C48 C43 C44 C45 -0.1(10) . . . . ? O10 C44 C45 C46 178.6(6) . . . . ? C43 C44 C45 C46 -0.8(9) . . . . ? O10 C44 C45 C49 -2.3(10) . . . . ? C43 C44 C45 C49 178.3(6) . . . . ? C44 C45 C46 C47 1.4(11) . . . . ? C49 C45 C46 C47 -177.7(7) . . . . ? C45 C46 C47 C48 -1.1(13) . . . . ? C46 C47 C48 C43 0.1(12) . . . . ? C42 C43 C48 C47 -178.8(7) . . . . ? C44 C43 C48 C47 0.5(11) . . . . ? C46 C45 C49 O11 145.8(8) . . . . ? C44 C45 C49 O11 -33.3(10) . . . . ? C46 C45 C49 O12 -32.2(10) . . . . ? C44 C45 C49 O12 148.7(7) . . . . ? N38 C50 C51 N52 176.4(9) . . . . ? N53 C54 C55 N56 47.6(8) . . . . ? N53 C57 C58 N59 44.4(10) . . . . ? N53 C60 C61 N62 -46.4(9) . . . . ? N63 C64 C65 N66 -20.3(17) . . . . ? N63 C67 C68 N69 -52.7(11) . . . . ? N63 C70 C71 N72 48.0(10) . . . . ? C6 C7 C222 C3 2.9(10) . . . . ? C6 C7 C222 C1 -175.5(6) . . . . ? O3 C3 C222 C7 179.0(6) . . . . ? C4 C3 C222 C7 -0.7(9) . . . . ? O3 C3 C222 C1 -2.7(9) . . . . ? C4 C3 C222 C1 177.6(6) . . . . ? O2 C1 C222 C7 -35.7(9) . . . . ? O1 C1 C222 C7 142.9(6) . . . . ? O2 C1 C222 C3 145.9(6) . . . . ? O1 C1 C222 C3 -35.4(9) . . . . ? C4 C8 N9 C10 -176.3(6) . . . . ? C11 C10 N9 C8 112.2(7) . . . . ? C25 C24 N12 C11 -164.0(5) . . . . ? C25 C24 N12 C13 70.7(7) . . . . ? C10 C11 N12 C24 82.2(7) . . . . ? C10 C11 N12 C13 -151.2(6) . . . . ? C14 C13 N12 C24 -137.8(6) . . . . ? C14 C13 N12 C11 96.3(7) . . . . ? C17 C16 N15 C14 179.8(6) . . . . ? C13 C14 N15 C16 104.9(7) . . . . ? C24 C25 N26 Ni1 175.8(4) . . . . ? C30 C34 N35 C36 -178.3(7) . . . . ? C37 C36 N35 C34 99.5(9) . . . . ? C51 C50 N38 C39 -158.6(8) . . . . ? C51 C50 N38 C37 75.1(10) . . . . ? C40 C39 N38 C50 81.6(10) . . . . ? C40 C39 N38 C37 -150.7(8) . . . . ? C36 C37 N38 C50 -143.7(7) . . . . ? C36 C37 N38 C39 91.1(8) . . . . ? C43 C42 N41 C40 -178.9(8) . . . . ? C39 C40 N41 C42 106.2(9) . . . . ? C50 C51 N52 Ni2 170.2(7) . . . . ? C55 C54 N53 C57 69.1(8) . . . . ? C55 C54 N53 C60 -162.7(6) . . . . ? C55 C54 N53 Ni1 -48.2(6) . . . . ? C58 C57 N53 C54 -139.1(7) . . . . ? C58 C57 N53 C60 93.6(8) . . . . ? C58 C57 N53 Ni1 -24.4(8) . . . . ? C61 C60 N53 C54 159.5(6) . . . . ? C61 C60 N53 C57 -72.9(8) . . . . ? C61 C60 N53 Ni1 46.4(7) . . . . ? C54 C55 N56 Ni1 -21.2(7) . . . . ? C57 C58 N59 Ni1 -40.1(8) . . . . ? C60 C61 N62 Ni1 22.4(8) . . . . ? C68 C67 N63 C70 161.5(7) . . . . ? C68 C67 N63 C64 -71.1(9) . . . . ? C68 C67 N63 Ni2 47.7(8) . . . . ? C71 C70 N63 C67 -161.6(7) . . . . ? C71 C70 N63 C64 71.2(8) . . . . ? C71 C70 N63 Ni2 -47.9(8) . . . . ? C65 C64 N63 C67 123.2(10) . . . . ? C65 C64 N63 C70 -109.3(10) . . . . ? C65 C64 N63 Ni2 7.2(11) . . . . ? C64 C65 N66 Ni2 22.3(16) . . . . ? C67 C68 N69 Ni2 29.0(10) . . . . ? C70 C71 N72 Ni2 -22.5(9) . . . . ? O2 C1 O1 Lu1 -145.8(5) . . . . ? C222 C1 O1 Lu1 35.6(9) . . . . ? C222 C3 O3 Lu1 41.8(8) . . . . ? C4 C3 O3 Lu1 -138.5(5) . . . . ? C19 C18 O4 Lu1 0.5(9) . . . . ? C17 C18 O4 Lu1 -179.5(4) . . . . ? O6 C23 O5 Lu1 154.7(5) . . . . ? C19 C23 O5 Lu1 -26.6(9) . . . . ? O5 C23 O6 Ni2 6.3(10) . . . . ? C19 C23 O6 Ni2 -172.5(4) . . . . ? O8 C27 O7 Lu1 160.9(5) . . . . ? C28 C27 O7 Lu1 -21.8(11) . . . . ? O7 C27 O8 Ni1 8.9(10) . . . . ? C28 C27 O8 Ni1 -168.6(4) . . . . ? C28 C29 O9 Lu1 -3.1(10) . . . . ? C30 C29 O9 Lu1 176.5(4) . . . . ? C43 C44 O10 Lu1 -142.7(5) . . . . ? C45 C44 O10 Lu1 37.9(8) . . . . ? O12 C49 O11 Lu1 -148.5(6) . . . . ? C45 C49 O11 Lu1 33.6(11) . . . . ? O302 N300 O301 N301 41.1(14) . . . . ? O300 N300 O301 N301 -160(2) . . . . ? O300 N300 O302 N301 160(2) . . . . ? O301 N300 O302 N301 -39.0(14) . . . . ? N300 O301 N301 O303 146(3) . . . . ? N300 O301 N301 O302 -36.2(13) . . . . ? N300 O302 N301 O303 -142(3) . . . . ? N300 O302 N301 O301 39.5(14) . . . . ? C25 N26 Ni1 N59 -87.6(5) . . . . ? C25 N26 Ni1 N53 -138(3) . . . . ? C25 N26 Ni1 N56 5.9(5) . . . . ? C25 N26 Ni1 O8 95.6(4) . . . . ? C25 N26 Ni1 N62 178.4(4) . . . . ? C58 N59 Ni1 N26 -155.6(5) . . . . ? C58 N59 Ni1 N53 21.4(5) . . . . ? C58 N59 Ni1 N56 104.1(5) . . . . ? C58 N59 Ni1 O8 -9(2) . . . . ? C58 N59 Ni1 N62 -60.4(5) . . . . ? C54 N53 Ni1 N26 172(3) . . . . ? C57 N53 Ni1 N26 52(4) . . . . ? C60 N53 Ni1 N26 -70(4) . . . . ? C54 N53 Ni1 N59 121.3(5) . . . . ? C57 N53 Ni1 N59 1.6(5) . . . . ? C60 N53 Ni1 N59 -120.7(5) . . . . ? C54 N53 Ni1 N56 27.7(4) . . . . ? C57 N53 Ni1 N56 -92.0(5) . . . . ? C60 N53 Ni1 N56 145.7(5) . . . . ? C54 N53 Ni1 O8 -61.6(4) . . . . ? C57 N53 Ni1 O8 178.6(5) . . . . ? C60 N53 Ni1 O8 56.4(5) . . . . ? C54 N53 Ni1 N62 -144.2(5) . . . . ? C57 N53 Ni1 N62 96.1(5) . . . . ? C60 N53 Ni1 N62 -26.2(5) . . . . ? C55 N56 Ni1 N26 178.5(4) . . . . ? C55 N56 Ni1 N59 -87.8(4) . . . . ? C55 N56 Ni1 N53 -3.8(4) . . . . ? C55 N56 Ni1 O8 87.0(4) . . . . ? C55 N56 Ni1 N62 25.1(9) . . . . ? C27 O8 Ni1 N26 -70.7(6) . . . . ? C27 O8 Ni1 N59 143.1(19) . . . . ? C27 O8 Ni1 N53 112.4(6) . . . . ? C27 O8 Ni1 N56 29.4(6) . . . . ? C27 O8 Ni1 N62 -165.5(6) . . . . ? C61 N62 Ni1 N26 179.4(5) . . . . ? C61 N62 Ni1 N59 86.0(5) . . . . ? C61 N62 Ni1 N53 2.1(5) . . . . ? C61 N62 Ni1 N56 -26.8(10) . . . . ? C61 N62 Ni1 O8 -89.5(5) . . . . ? C51 N52 Ni2 N72 2.3(8) . . . . ? C51 N52 Ni2 N63 -155(3) . . . . ? C51 N52 Ni2 N66 -93.7(8) . . . . ? C51 N52 Ni2 O6 91.4(8) . . . . ? C51 N52 Ni2 N69 173.4(8) . . . . ? C71 N72 Ni2 N52 179.0(6) . . . . ? C71 N72 Ni2 N63 -2.8(6) . . . . ? C71 N72 Ni2 N66 -84.7(6) . . . . ? C71 N72 Ni2 O6 88.1(6) . . . . ? C71 N72 Ni2 N69 30.2(13) . . . . ? C67 N63 Ni2 N52 -55(4) . . . . ? C70 N63 Ni2 N52 -174(4) . . . . ? C64 N63 Ni2 N52 65(4) . . . . ? C67 N63 Ni2 N72 146.8(6) . . . . ? C70 N63 Ni2 N72 27.9(5) . . . . ? C64 N63 Ni2 N72 -92.9(5) . . . . ? C67 N63 Ni2 N66 -117.4(6) . . . . ? C70 N63 Ni2 N66 123.7(6) . . . . ? C64 N63 Ni2 N66 2.9(6) . . . . ? C67 N63 Ni2 O6 58.0(5) . . . . ? C70 N63 Ni2 O6 -60.8(5) . . . . ? C64 N63 Ni2 O6 178.3(5) . . . . ? C67 N63 Ni2 N69 -23.8(5) . . . . ? C70 N63 Ni2 N69 -142.6(6) . . . . ? C64 N63 Ni2 N69 96.5(6) . . . . ? C65 N66 Ni2 N52 171.1(9) . . . . ? C65 N66 Ni2 N72 69.1(9) . . . . ? C65 N66 Ni2 N63 -13.2(9) . . . . ? C65 N66 Ni2 O6 -48(3) . . . . ? C65 N66 Ni2 N69 -95.1(9) . . . . ? C23 O6 Ni2 N52 -72.8(7) . . . . ? C23 O6 Ni2 N72 28.7(6) . . . . ? C23 O6 Ni2 N63 111.7(7) . . . . ? C23 O6 Ni2 N66 146(2) . . . . ? C23 O6 Ni2 N69 -166.2(7) . . . . ? C68 N69 Ni2 N52 175.0(7) . . . . ? C68 N69 Ni2 N72 -35.5(14) . . . . ? C68 N69 Ni2 N63 -2.5(7) . . . . ? C68 N69 Ni2 N66 79.7(7) . . . . ? C68 N69 Ni2 O6 -94.3(7) . . . . ? C29 O9 Lu1 O4 -40.5(8) . . . . ? C29 O9 Lu1 O1 -144.3(6) . . . . ? C29 O9 Lu1 O11 71.3(6) . . . . ? C29 O9 Lu1 O7 -1.2(6) . . . . ? C29 O9 Lu1 O10 146.9(7) . . . . ? C29 O9 Lu1 O5 -77.9(6) . . . . ? C29 O9 Lu1 O3 128.9(6) . . . . ? C18 O4 Lu1 O9 -44.6(7) . . . . ? C18 O4 Lu1 O1 66.0(5) . . . . ? C18 O4 Lu1 O11 -149.8(5) . . . . ? C18 O4 Lu1 O7 -83.3(5) . . . . ? C18 O4 Lu1 O10 123.2(5) . . . . ? C18 O4 Lu1 O5 -6.8(5) . . . . ? C18 O4 Lu1 O3 141.9(6) . . . . ? C1 O1 Lu1 O9 -149.4(6) . . . . ? C1 O1 Lu1 O4 65.6(6) . . . . ? C1 O1 Lu1 O11 -45.0(7) . . . . ? C1 O1 Lu1 O7 124.8(6) . . . . ? C1 O1 Lu1 O10 -84.4(6) . . . . ? C1 O1 Lu1 O5 141.1(6) . . . . ? C1 O1 Lu1 O3 -5.8(6) . . . . ? C49 O11 Lu1 O9 66.1(7) . . . . ? C49 O11 Lu1 O4 -148.6(7) . . . . ? C49 O11 Lu1 O1 -44.9(9) . . . . ? C49 O11 Lu1 O7 141.3(8) . . . . ? C49 O11 Lu1 O10 -5.3(7) . . . . ? C49 O11 Lu1 O5 125.0(7) . . . . ? C49 O11 Lu1 O3 -83.9(7) . . . . ? C27 O7 Lu1 O9 14.9(7) . . . . ? C27 O7 Lu1 O4 172.4(8) . . . . ? C27 O7 Lu1 O1 111.1(7) . . . . ? C27 O7 Lu1 O11 -75.3(7) . . . . ? C27 O7 Lu1 O10 -28.4(9) . . . . ? C27 O7 Lu1 O5 94.9(7) . . . . ? C27 O7 Lu1 O3 -132.7(7) . . . . ? C44 O10 Lu1 O9 -121.2(5) . . . . ? C44 O10 Lu1 O4 66.3(6) . . . . ? C44 O10 Lu1 O1 125.9(5) . . . . ? C44 O10 Lu1 O11 -30.9(5) . . . . ? C44 O10 Lu1 O7 -76.9(6) . . . . ? C44 O10 Lu1 O5 -178.1(5) . . . . ? C44 O10 Lu1 O3 48.2(5) . . . . ? C23 O5 Lu1 O9 179.4(6) . . . . ? C23 O5 Lu1 O4 21.1(6) . . . . ? C23 O5 Lu1 O1 -68.3(6) . . . . ? C23 O5 Lu1 O11 118.0(6) . . . . ? C23 O5 Lu1 O7 101.9(6) . . . . ? C23 O5 Lu1 O10 -126.1(6) . . . . ? C23 O5 Lu1 O3 -21.6(7) . . . . ? C3 O3 Lu1 O9 63.1(6) . . . . ? C3 O3 Lu1 O4 -123.5(5) . . . . ? C3 O3 Lu1 O1 -33.8(5) . . . . ? C3 O3 Lu1 O11 123.2(5) . . . . ? C3 O3 Lu1 O7 178.9(5) . . . . ? C3 O3 Lu1 O10 45.6(5) . . . . ? C3 O3 Lu1 O5 -79.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.446 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.121 #==END data_Gd _database_code_depnum_ccdc_archive 'CCDC 898064' #TrackingRef '15314_web_deposit_cif_file_0_KlausHarms_1352392481.Ni2_Ln_oct.cif' # start Validation Reply Form _vrf_CHEMW03_Gd ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: 20 "squeezed" water molecules have been included ; #data_484 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H84 Gd N16 Ni2 O12, 3 (N O3), 20 (H2 O)' _chemical_formula_sum 'C56 H124 Gd N19 Ni2 O41' _chemical_formula_weight 1994.41 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' Gd Gd -0.1653 3.9035 '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 15.9709(9) _cell_length_b 16.0363(7) _cell_length_c 20.1336(11) _cell_angle_alpha 109.136(4) _cell_angle_beta 112.815(4) _cell_angle_gamma 88.400(4) _cell_volume 4461.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24560 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 24.16 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2082 _exptl_absorpt_coefficient_mu 1.249 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5314 _exptl_absorpt_correction_T_max 0.8773 _exptl_absorpt_process_details PLATON _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38926 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_av_sigmaI/netI 0.1692 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15625 _reflns_number_gt 8108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA (STOE & Cie, 2006)' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'Lu compound as start model' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material 'ENCIFER, PUBLCIF' _refine_special_details ; >From the refinement of the analogue Er and Lu compounds we know that there is disordered water present, approximately 20 molecules per asymmetric unit. The contribution of this disordered water has been subtracted from the current data set (PLATON "SQUEEZE" procedure). For the refinement of the nitrate ions contraints have been included for the geometry of the ions and the shape of the anisotropic temperature factors. The geometries of the anions are still not perfect. This and the shape of some temperature factors (e. g. of O100) indicate disorder that has not been resolved. 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^)+(0.0800P)^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 15625 _refine_ls_number_parameters 892 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.1929 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0322(8) 0.2117(6) 0.3879(6) 0.050(3) Uani 1 1 d . . . C3 C -0.1736(8) 0.2431(6) 0.2952(6) 0.045(3) Uani 1 1 d . . . C4 C -0.2737(8) 0.2332(6) 0.2610(7) 0.055(3) Uani 1 1 d . . . C5 C -0.3258(9) 0.1822(7) 0.2811(7) 0.058(3) Uani 1 1 d . . . H5 H -0.3906 0.1733 0.2565 0.070 Uiso 1 1 calc R . . C6 C -0.2793(9) 0.1456(8) 0.3379(8) 0.073(4) Uani 1 1 d . . . H6 H -0.3126 0.1116 0.3522 0.087 Uiso 1 1 calc R . . C7 C -0.1847(9) 0.1591(7) 0.3731(7) 0.063(3) Uani 1 1 d . . . H7 H -0.1554 0.1349 0.4125 0.076 Uiso 1 1 calc R . . C8 C -0.3220(9) 0.2682(7) 0.2050(8) 0.061(3) Uani 1 1 d . . . H8 H -0.3869 0.2611 0.1849 0.074 Uiso 1 1 calc R . . C10 C -0.3247(8) 0.3523(7) 0.1190(7) 0.054(3) Uani 1 1 d . . . H10A H -0.3913 0.3337 0.0946 0.065 Uiso 1 1 calc R . . H10B H -0.3001 0.3324 0.0789 0.065 Uiso 1 1 calc R . . C11 C -0.3070(8) 0.4506(7) 0.1554(8) 0.063(3) Uani 1 1 d . . . H11A H -0.3360 0.4777 0.1155 0.076 Uiso 1 1 calc R . . H11B H -0.3357 0.4701 0.1928 0.076 Uiso 1 1 calc R . . C13 C -0.1924(8) 0.5677(7) 0.2607(6) 0.052(3) Uani 1 1 d . . . H13A H -0.1390 0.6049 0.2679 0.063 Uiso 1 1 calc R . . H13B H -0.2463 0.6006 0.2477 0.063 Uiso 1 1 calc R . . C14 C -0.1763(8) 0.5539(7) 0.3328(7) 0.061(3) Uani 1 1 d . . . H14A H -0.2270 0.5129 0.3252 0.073 Uiso 1 1 calc R . . H14B H -0.1743 0.6113 0.3722 0.073 Uiso 1 1 calc R . . C16 C -0.0220(9) 0.5588(7) 0.4190(7) 0.060(3) Uani 1 1 d . . . H16 H -0.0318 0.6154 0.4479 0.071 Uiso 1 1 calc R . . C17 C 0.0688(8) 0.5320(7) 0.4492(6) 0.050(3) Uani 1 1 d . . . C18 C 0.0888(7) 0.4467(6) 0.4058(6) 0.045(2) Uani 1 1 d . . . C19 C 0.1765(7) 0.4204(7) 0.4411(6) 0.050(3) Uani 1 1 d . . . C20 C 0.2417(8) 0.4795(7) 0.5144(6) 0.054(3) Uani 1 1 d . . . H20 H 0.2998 0.4614 0.5378 0.065 Uiso 1 1 calc R . . C21 C 0.2204(9) 0.5632(7) 0.5516(7) 0.062(3) Uani 1 1 d . . . H21 H 0.2642 0.6021 0.5989 0.074 Uiso 1 1 calc R . . C22 C 0.1371(8) 0.5869(7) 0.5190(7) 0.060(3) Uani 1 1 d . . . H22 H 0.1234 0.6436 0.5442 0.073 Uiso 1 1 calc R . . C23 C 0.2084(8) 0.3356(7) 0.4089(6) 0.047(3) Uani 1 1 d . . . C24 C -0.1665(7) 0.4872(7) 0.1439(6) 0.047(3) Uani 1 1 d . . . H24A H -0.1853 0.5391 0.1275 0.057 Uiso 1 1 calc R . . H24B H -0.1898 0.4332 0.0974 0.057 Uiso 1 1 calc R . . C25 C -0.0626(7) 0.4945(6) 0.1797(5) 0.043(2) Uani 1 1 d . . . H25A H -0.0403 0.5477 0.2269 0.052 Uiso 1 1 calc R . . H25B H -0.0448 0.4420 0.1954 0.052 Uiso 1 1 calc R . . C27 C 0.1071(6) 0.3162(6) 0.1498(6) 0.039(2) Uani 1 1 d . . . C28 C 0.1150(6) 0.2217(6) 0.1054(5) 0.036(2) Uani 1 1 d . . . C29 C 0.1011(6) 0.1441(6) 0.1254(5) 0.039(2) Uani 1 1 d . . . C30 C 0.1142(7) 0.0632(6) 0.0818(6) 0.047(2) Uani 1 1 d . . . C31 C 0.1411(9) 0.0521(7) 0.0204(6) 0.060(3) Uani 1 1 d . . . H31 H 0.1530 -0.0045 -0.0066 0.072 Uiso 1 1 calc R . . C32 C 0.1498(8) 0.1252(7) 0.0001(6) 0.057(3) Uani 1 1 d . . . H32 H 0.1618 0.1184 -0.0440 0.069 Uiso 1 1 calc R . . C33 C 0.1409(6) 0.2075(6) 0.0448(6) 0.041(2) Uani 1 1 d . . . H33 H 0.1531 0.2577 0.0335 0.049 Uiso 1 1 calc R . . C34 C 0.0989(8) -0.0191(6) 0.0946(6) 0.056(3) Uani 1 1 d . . . H34 H 0.1119 -0.0722 0.0635 0.067 Uiso 1 1 calc R . . C36 C 0.0564(8) -0.1101(6) 0.1517(6) 0.053(3) Uani 1 1 d . . . H36A H 0.0775 -0.1577 0.1179 0.064 Uiso 1 1 calc R . . H36B H -0.0096 -0.1256 0.1361 0.064 Uiso 1 1 calc R . . C37 C 0.1092(8) -0.1045(6) 0.2358(6) 0.050(3) Uani 1 1 d . . . H37A H 0.1052 -0.1640 0.2399 0.060 Uiso 1 1 calc R . . H37B H 0.1745 -0.0838 0.2532 0.060 Uiso 1 1 calc R . . C39 C -0.0024(7) -0.0878(6) 0.2893(6) 0.047(3) Uani 1 1 d . . . H39A H 0.0249 -0.1138 0.3303 0.056 Uiso 1 1 calc R . . H39B H -0.0323 -0.1374 0.2402 0.056 Uiso 1 1 calc R . . C40 C -0.0755(8) -0.0311(6) 0.3053(6) 0.056(3) Uani 1 1 d . . . H40A H -0.1248 -0.0688 0.3037 0.067 Uiso 1 1 calc R . . H40B H -0.0484 0.0150 0.3569 0.067 Uiso 1 1 calc R . . C42 C -0.2009(9) -0.0015(7) 0.1966(7) 0.056(3) Uani 1 1 d . . . H42 H -0.2418 -0.0410 0.1993 0.067 Uiso 1 1 calc R . . C43 C -0.2363(7) 0.0384(6) 0.1418(6) 0.040(2) Uani 1 1 d . . . C44 C -0.1759(7) 0.1019(6) 0.1379(6) 0.043(2) Uani 1 1 d . . . C45 C -0.2186(7) 0.1422(6) 0.0787(6) 0.041(2) Uani 1 1 d . . . C46 C -0.3085(7) 0.1195(7) 0.0322(7) 0.054(3) Uani 1 1 d . . . H46 H -0.3337 0.1450 -0.0068 0.064 Uiso 1 1 calc R . . C47 C -0.3668(8) 0.0605(8) 0.0379(7) 0.059(3) Uani 1 1 d . . . H47 H -0.4300 0.0480 0.0050 0.071 Uiso 1 1 calc R . . C48 C -0.3293(7) 0.0218(7) 0.0925(6) 0.051(3) Uani 1 1 d . . . H48 H -0.3679 -0.0179 0.0973 0.061 Uiso 1 1 calc R . . C49 C -0.1637(7) 0.2116(6) 0.0710(7) 0.046(3) Uani 1 1 d . . . C50 C 0.1394(7) 0.0065(7) 0.3588(6) 0.051(3) Uani 1 1 d . . . H50A H 0.1787 -0.0359 0.3790 0.061 Uiso 1 1 calc R . . H50B H 0.1109 0.0361 0.3950 0.061 Uiso 1 1 calc R . . C51 C 0.1980(7) 0.0759(6) 0.3545(6) 0.047(3) Uani 1 1 d . . . H51A H 0.2210 0.0470 0.3143 0.056 Uiso 1 1 calc R . . H51B H 0.1595 0.1212 0.3390 0.056 Uiso 1 1 calc R . . C54 C 0.3010(7) 0.4927(7) 0.2643(6) 0.049(3) Uani 1 1 d . . . H54A H 0.3682 0.5073 0.2912 0.058 Uiso 1 1 calc R . . H54B H 0.2872 0.4272 0.2415 0.058 Uiso 1 1 calc R . . C55 C 0.2559(7) 0.5293(7) 0.3227(6) 0.049(3) Uani 1 1 d . . . H55A H 0.2750 0.4984 0.3606 0.059 Uiso 1 1 calc R . . H55B H 0.2763 0.5935 0.3506 0.059 Uiso 1 1 calc R . . C57 C 0.2977(7) 0.6288(6) 0.2309(6) 0.045(2) Uani 1 1 d . . . H57A H 0.3462 0.6370 0.2138 0.054 Uiso 1 1 calc R . . H57B H 0.3247 0.6508 0.2877 0.054 Uiso 1 1 calc R . . C58 C 0.2206(7) 0.6843(6) 0.2028(6) 0.044(2) Uani 1 1 d . . . H58A H 0.2398 0.7475 0.2357 0.053 Uiso 1 1 calc R . . H58B H 0.2098 0.6796 0.1497 0.053 Uiso 1 1 calc R . . C60 C 0.2846(7) 0.4865(7) 0.1382(7) 0.055(3) Uani 1 1 d . . . H60A H 0.2761 0.4218 0.1274 0.065 Uiso 1 1 calc R . . H60B H 0.3492 0.5032 0.1494 0.065 Uiso 1 1 calc R . . C61 C 0.2225(7) 0.5078(7) 0.0683(5) 0.046(2) Uani 1 1 d . . . H61A H 0.2415 0.5685 0.0731 0.055 Uiso 1 1 calc R . . H61B H 0.2265 0.4653 0.0215 0.055 Uiso 1 1 calc R . . C64 C 0.5355(9) 0.2587(9) 0.4164(10) 0.091(5) Uani 1 1 d . . . H64A H 0.5883 0.2727 0.4664 0.110 Uiso 1 1 calc R . . H64B H 0.5527 0.2828 0.3834 0.110 Uiso 1 1 calc R . . C65 C 0.5101(10) 0.1564(9) 0.3777(10) 0.089(5) Uani 1 1 d . . . H65A H 0.4747 0.1416 0.3219 0.107 Uiso 1 1 calc R . . H65B H 0.5668 0.1271 0.3852 0.107 Uiso 1 1 calc R . . C67 C 0.4877(10) 0.3698(10) 0.5086(10) 0.106(6) Uani 1 1 d . . . H67A H 0.5430 0.4072 0.5195 0.127 Uiso 1 1 calc R . . H67B H 0.4388 0.4086 0.5103 0.127 Uiso 1 1 calc R . . C68 C 0.5074(9) 0.3289(9) 0.5665(8) 0.080(4) Uani 1 1 d . . . H68A H 0.5626 0.2976 0.5704 0.096 Uiso 1 1 calc R . . H68B H 0.5200 0.3753 0.6169 0.096 Uiso 1 1 calc R . . C70 C 0.4017(9) 0.3388(9) 0.3673(9) 0.081(4) Uani 1 1 d . . . H70A H 0.4428 0.3773 0.3605 0.097 Uiso 1 1 calc R . . H70B H 0.3575 0.3753 0.3837 0.097 Uiso 1 1 calc R . . C71 C 0.3509(9) 0.2628(9) 0.2920(8) 0.076(4) Uani 1 1 d . . . H71A H 0.3060 0.2864 0.2545 0.091 Uiso 1 1 calc R . . H71B H 0.3949 0.2342 0.2704 0.091 Uiso 1 1 calc R . . C2 C -0.1299(8) 0.2052(7) 0.3549(7) 0.055(3) Uani 1 1 d . . . N9 N -0.2803(6) 0.3118(5) 0.1781(6) 0.059(3) Uani 1 1 d . . . N12 N -0.2081(6) 0.4831(5) 0.1953(5) 0.046(2) Uani 1 1 d . . . N15 N -0.0884(7) 0.5161(6) 0.3596(6) 0.053(2) Uani 1 1 d . . . N26 N -0.0161(6) 0.5004(5) 0.1332(5) 0.051(2) Uani 1 1 d . . . H26A H -0.0363 0.5476 0.1172 0.062 Uiso 1 1 calc R . . H26B H -0.0379 0.4502 0.0900 0.062 Uiso 1 1 calc R . . N35 N 0.0705(7) -0.0259(6) 0.1424(5) 0.058(3) Uani 1 1 d . . . N38 N 0.0691(6) -0.0413(5) 0.2853(4) 0.043(2) Uani 1 1 d . . . N41 N -0.1129(7) 0.0109(5) 0.2466(5) 0.048(2) Uani 1 1 d . . . N52 N 0.2780(6) 0.1214(6) 0.4288(5) 0.059(2) Uani 1 1 d . . . H52A H 0.3120 0.0787 0.4441 0.071 Uiso 1 1 calc R . . H52B H 0.2561 0.1498 0.4655 0.071 Uiso 1 1 calc R . . N53 N 0.2656(6) 0.5323(5) 0.2022(5) 0.047(2) Uani 1 1 d . . . N56 N 0.1574(6) 0.5155(5) 0.2824(5) 0.044(2) Uani 1 1 d . . . H56A H 0.1317 0.5604 0.3074 0.052 Uiso 1 1 calc R . . H56B H 0.1350 0.4624 0.2810 0.052 Uiso 1 1 calc R . . N59 N 0.1343(5) 0.6551(5) 0.2039(5) 0.0422(19) Uani 1 1 d . . . H59A H 0.0853 0.6732 0.1709 0.051 Uiso 1 1 calc R . . H59B H 0.1354 0.6789 0.2525 0.051 Uiso 1 1 calc R . . N62 N 0.1282(5) 0.5016(5) 0.0625(4) 0.0406(19) Uani 1 1 d . . . H62A H 0.0975 0.4478 0.0267 0.049 Uiso 1 1 calc R . . H62B H 0.0989 0.5457 0.0459 0.049 Uiso 1 1 calc R . . N63 N 0.4569(7) 0.2986(8) 0.4276(7) 0.082(3) Uani 1 1 d . . . N66 N 0.4575(6) 0.1235(6) 0.4090(6) 0.067(3) Uani 1 1 d . . . H66A H 0.4953 0.1179 0.4549 0.080 Uiso 1 1 calc R . . H66B H 0.4272 0.0684 0.3758 0.080 Uiso 1 1 calc R . . N69 N 0.4325(7) 0.2677(6) 0.5474(6) 0.068(3) Uani 1 1 d . . . H69A H 0.3930 0.2962 0.5683 0.081 Uiso 1 1 calc R . . H69B H 0.4530 0.2232 0.5672 0.081 Uiso 1 1 calc R . . N72 N 0.3035(6) 0.1970(6) 0.3059(5) 0.060(3) Uani 1 1 d . . . H72A H 0.3082 0.1406 0.2771 0.072 Uiso 1 1 calc R . . H72B H 0.2425 0.2048 0.2913 0.072 Uiso 1 1 calc R . . O1 O 0.0153(5) 0.2027(4) 0.3488(4) 0.0472(17) Uani 1 1 d . . . O2 O 0.0077(6) 0.2218(6) 0.4604(5) 0.074(2) Uani 1 1 d . . . O3 O -0.1277(5) 0.2863(4) 0.2753(4) 0.0510(18) Uani 1 1 d . . . H3 H -0.1509 0.3396 0.2688 0.061 Uiso 1 1 calc R . . O4 O 0.0294(5) 0.4017(4) 0.3401(4) 0.0446(16) Uani 1 1 d . . . H4 H -0.0187 0.4352 0.3217 0.054 Uiso 1 1 calc R . . O5 O 0.1631(5) 0.2876(4) 0.3423(4) 0.0512(18) Uani 1 1 d . . . O6 O 0.2793(6) 0.3142(5) 0.4514(4) 0.068(2) Uani 1 1 d . . . O7 O 0.0863(4) 0.3315(4) 0.2074(4) 0.0409(15) Uani 1 1 d . . . O8 O 0.1235(5) 0.3731(4) 0.1267(4) 0.0467(17) Uani 1 1 d . . . O9 O 0.0803(4) 0.1514(4) 0.1840(4) 0.0416(16) Uani 1 1 d . . . H9 H 0.0986 0.1045 0.2037 0.050 Uiso 1 1 calc R . . O10 O -0.0900(4) 0.1185(4) 0.1823(4) 0.0389(15) Uani 1 1 d . . . H10 H -0.0605 0.0677 0.1887 0.047 Uiso 1 1 calc R . . O11 O -0.0984(5) 0.2635(4) 0.1323(4) 0.0444(16) Uani 1 1 d . . . O12 O -0.1852(5) 0.2144(5) 0.0061(4) 0.0513(18) Uani 1 1 d . . . N200 N 0.1000(5) 0.2960(5) 0.8805(4) 0.0435(19) Uani 1 1 d DU . . O202 O 0.0796(6) 0.3027(5) 0.8160(4) 0.060(2) Uani 1 1 d DU . . O201 O 0.1642(6) 0.2528(6) 0.9010(6) 0.085(3) Uani 1 1 d DU . . O200 O 0.0526(5) 0.3262(4) 0.9186(4) 0.0514(18) Uani 1 1 d DU . . Ni1 Ni 0.12323(9) 0.51397(7) 0.16845(7) 0.0382(3) Uani 1 1 d . . . Ni2 Ni 0.36340(10) 0.21253(9) 0.42587(9) 0.0601(4) Uani 1 1 d . . . Gd1 Gd 0.00749(4) 0.25581(3) 0.25121(3) 0.03668(16) Uani 1 1 d . . . O102 O 0.3453(7) 0.9403(7) 0.3580(8) 0.116(4) Uani 1 1 d DU . . O101 O 0.4144(8) 0.8284(7) 0.3680(7) 0.118(4) Uani 1 1 d DU . . N100 N 0.3842(8) 0.8954(9) 0.3990(7) 0.088(3) Uani 1 1 d DU . . O100 O 0.3889(10) 0.9152(18) 0.4633(9) 0.230(10) Uani 1 1 d DU . . O300 O 0.4795(8) 0.5593(8) 0.7862(7) 0.109(3) Uani 1 1 d DU . . N300 N 0.4621(9) 0.5861(8) 0.7303(7) 0.091(3) Uani 1 1 d DU . . O301 O 0.4879(8) 0.6660(8) 0.7462(7) 0.117(4) Uani 1 1 d DU . . O302 O 0.4441(8) 0.5301(10) 0.6687(7) 0.138(5) Uani 1 1 d DU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.084(9) 0.030(5) 0.046(7) 0.013(5) 0.037(6) 0.016(5) C3 0.072(8) 0.024(5) 0.050(6) 0.003(4) 0.045(6) 0.004(5) C4 0.080(9) 0.029(5) 0.068(7) -0.003(5) 0.059(7) 0.010(5) C5 0.075(8) 0.053(7) 0.065(7) 0.021(6) 0.045(7) 0.010(6) C6 0.071(9) 0.063(8) 0.101(11) 0.027(8) 0.052(8) 0.012(7) C7 0.097(10) 0.045(7) 0.069(8) 0.019(6) 0.057(8) 0.024(7) C8 0.069(8) 0.034(6) 0.100(10) 0.016(6) 0.059(8) 0.016(6) C10 0.062(7) 0.039(6) 0.069(8) 0.015(6) 0.038(6) 0.000(5) C11 0.051(7) 0.047(7) 0.110(10) 0.030(7) 0.048(7) 0.015(5) C13 0.060(7) 0.042(6) 0.071(8) 0.025(6) 0.040(6) 0.020(5) C14 0.075(8) 0.035(6) 0.074(8) -0.003(5) 0.050(7) 0.021(5) C16 0.072(8) 0.039(6) 0.070(8) 0.009(6) 0.040(7) 0.025(6) C17 0.077(8) 0.039(6) 0.040(6) 0.010(5) 0.034(6) 0.014(6) C18 0.064(7) 0.032(5) 0.035(6) 0.000(4) 0.026(5) 0.011(5) C19 0.059(7) 0.042(6) 0.041(6) 0.006(5) 0.020(5) 0.013(5) C20 0.073(8) 0.044(6) 0.035(6) 0.006(5) 0.019(6) 0.000(6) C21 0.074(8) 0.039(6) 0.055(7) -0.005(5) 0.025(6) 0.002(6) C22 0.075(8) 0.035(6) 0.059(8) 0.011(6) 0.020(6) 0.023(6) C23 0.057(7) 0.036(6) 0.029(6) 0.005(5) 0.004(5) 0.008(5) C24 0.047(6) 0.042(6) 0.063(7) 0.030(5) 0.025(6) 0.014(5) C25 0.056(7) 0.033(5) 0.038(6) -0.002(4) 0.027(5) 0.001(5) C27 0.041(6) 0.033(5) 0.055(7) 0.023(5) 0.024(5) 0.014(4) C28 0.044(6) 0.031(5) 0.034(5) 0.005(4) 0.022(5) 0.007(4) C29 0.045(6) 0.039(5) 0.039(6) 0.021(4) 0.018(5) 0.014(4) C30 0.065(7) 0.032(5) 0.049(6) 0.008(5) 0.033(5) 0.011(5) C31 0.112(10) 0.034(6) 0.058(7) 0.024(5) 0.054(7) 0.038(6) C32 0.096(9) 0.046(6) 0.052(7) 0.025(5) 0.048(7) 0.032(6) C33 0.044(6) 0.030(5) 0.050(6) 0.016(4) 0.018(5) 0.013(4) C34 0.093(9) 0.027(5) 0.053(7) 0.007(5) 0.042(7) 0.013(5) C36 0.086(8) 0.020(5) 0.061(7) 0.007(5) 0.043(6) 0.013(5) C37 0.078(8) 0.025(5) 0.050(6) 0.016(5) 0.029(6) 0.023(5) C39 0.072(7) 0.027(5) 0.041(6) 0.006(4) 0.026(5) 0.006(5) C40 0.089(9) 0.025(5) 0.042(6) -0.001(4) 0.025(6) 0.002(5) C42 0.069(8) 0.032(6) 0.071(8) 0.010(6) 0.038(7) 0.007(6) C43 0.052(7) 0.027(5) 0.045(6) 0.010(4) 0.026(5) 0.010(5) C44 0.048(7) 0.032(5) 0.048(6) 0.003(5) 0.026(5) 0.006(5) C45 0.051(7) 0.028(5) 0.047(6) 0.003(4) 0.031(5) 0.002(5) C46 0.045(7) 0.033(6) 0.075(8) 0.005(5) 0.027(6) 0.004(5) C47 0.054(7) 0.065(8) 0.060(7) 0.018(6) 0.026(6) -0.008(6) C48 0.050(7) 0.040(6) 0.062(7) 0.014(5) 0.025(6) -0.005(5) C49 0.042(6) 0.028(5) 0.074(8) 0.025(5) 0.024(6) 0.013(5) C50 0.060(7) 0.037(6) 0.052(7) 0.013(5) 0.023(6) 0.016(5) C51 0.052(6) 0.030(5) 0.060(7) 0.017(5) 0.024(6) 0.017(5) C54 0.057(7) 0.052(6) 0.042(6) 0.018(5) 0.024(5) 0.010(5) C55 0.066(8) 0.031(5) 0.052(7) 0.005(5) 0.032(6) -0.007(5) C57 0.054(6) 0.031(5) 0.043(6) 0.010(4) 0.015(5) 0.014(5) C58 0.057(7) 0.022(5) 0.066(7) 0.028(5) 0.028(5) 0.022(4) C60 0.052(7) 0.048(6) 0.076(8) 0.025(6) 0.038(6) 0.022(5) C61 0.064(7) 0.040(6) 0.033(5) 0.004(4) 0.027(5) 0.009(5) C64 0.067(9) 0.083(10) 0.132(14) 0.065(10) 0.025(9) 0.010(8) C65 0.079(9) 0.077(10) 0.156(15) 0.072(10) 0.070(10) 0.055(8) C67 0.057(9) 0.080(10) 0.125(14) 0.024(10) -0.013(9) -0.024(8) C68 0.062(9) 0.072(9) 0.076(9) 0.036(8) -0.012(7) 0.010(7) C70 0.064(8) 0.084(10) 0.106(12) 0.061(9) 0.022(8) 0.016(7) C71 0.061(8) 0.067(8) 0.090(10) 0.050(8) 0.002(7) 0.014(7) C2 0.078(9) 0.034(6) 0.068(8) 0.001(5) 0.059(7) 0.007(6) N9 0.071(6) 0.028(5) 0.091(7) 0.010(5) 0.054(6) 0.007(4) N12 0.055(5) 0.025(4) 0.066(6) 0.011(4) 0.040(5) 0.018(4) N15 0.058(6) 0.046(5) 0.054(6) 0.014(5) 0.024(5) 0.022(5) N26 0.081(6) 0.039(5) 0.047(5) 0.002(4) 0.047(5) -0.007(4) N35 0.090(7) 0.037(5) 0.049(6) 0.001(4) 0.042(6) -0.005(5) N38 0.056(5) 0.040(5) 0.033(5) 0.009(4) 0.021(4) 0.005(4) N41 0.074(7) 0.027(4) 0.060(6) 0.013(4) 0.045(5) 0.008(4) N52 0.064(6) 0.049(5) 0.058(6) 0.014(5) 0.024(5) 0.018(5) N53 0.063(6) 0.028(4) 0.061(6) 0.010(4) 0.042(5) 0.006(4) N56 0.056(6) 0.023(4) 0.055(5) 0.015(4) 0.025(5) 0.010(4) N59 0.048(5) 0.028(4) 0.057(5) 0.013(4) 0.030(4) 0.010(4) N62 0.059(5) 0.034(4) 0.035(4) 0.014(4) 0.023(4) 0.009(4) N63 0.048(6) 0.098(9) 0.082(8) 0.036(7) 0.005(6) 0.004(6) N66 0.059(6) 0.054(6) 0.098(8) 0.034(6) 0.035(6) 0.012(5) N69 0.060(6) 0.046(6) 0.071(7) 0.017(5) 0.003(5) 0.010(5) N72 0.055(6) 0.057(6) 0.067(6) 0.025(5) 0.021(5) 0.020(5) O1 0.067(5) 0.041(4) 0.048(4) 0.018(3) 0.036(4) 0.014(3) O2 0.086(6) 0.087(6) 0.081(6) 0.052(5) 0.048(5) 0.047(5) O3 0.062(5) 0.024(3) 0.077(5) 0.007(3) 0.046(4) 0.013(3) O4 0.063(5) 0.028(3) 0.039(4) 0.008(3) 0.021(4) 0.015(3) O5 0.049(4) 0.043(4) 0.055(5) 0.018(4) 0.014(4) 0.009(3) O6 0.087(6) 0.041(4) 0.050(5) 0.007(4) 0.008(4) 0.026(4) O7 0.057(4) 0.023(3) 0.050(4) 0.006(3) 0.035(4) 0.004(3) O8 0.070(5) 0.034(4) 0.050(4) 0.020(3) 0.036(4) 0.016(3) O9 0.049(4) 0.035(4) 0.051(4) 0.020(3) 0.027(3) 0.014(3) O10 0.049(4) 0.022(3) 0.055(4) 0.012(3) 0.032(4) 0.014(3) O11 0.059(5) 0.027(3) 0.047(4) 0.008(3) 0.025(4) 0.003(3) O12 0.071(5) 0.052(4) 0.035(4) 0.017(3) 0.022(4) 0.003(4) N200 0.055(5) 0.035(4) 0.049(5) 0.025(4) 0.022(4) 0.012(4) O202 0.096(6) 0.043(4) 0.047(4) 0.018(3) 0.032(4) 0.012(4) O201 0.090(6) 0.090(7) 0.113(7) 0.068(6) 0.055(6) 0.045(5) O200 0.078(5) 0.035(4) 0.053(4) 0.023(3) 0.031(4) 0.015(3) Ni1 0.0517(8) 0.0269(6) 0.0430(7) 0.0129(5) 0.0258(6) 0.0094(6) Ni2 0.0561(9) 0.0349(8) 0.0788(11) 0.0183(7) 0.0179(8) 0.0134(7) Gd1 0.0507(3) 0.0231(2) 0.0413(3) 0.00892(19) 0.0256(2) 0.0082(2) O102 0.092(7) 0.069(6) 0.183(10) 0.061(7) 0.035(7) 0.027(5) O101 0.109(8) 0.070(7) 0.143(9) 0.056(6) 0.004(7) 0.033(6) N100 0.059(7) 0.119(10) 0.079(8) 0.040(7) 0.015(6) 0.020(7) O100 0.117(11) 0.46(3) 0.127(10) 0.105(14) 0.057(10) 0.084(15) O300 0.124(9) 0.125(9) 0.119(8) 0.074(7) 0.064(7) 0.036(7) N300 0.111(10) 0.085(7) 0.088(8) 0.036(6) 0.047(8) 0.019(8) O301 0.139(10) 0.096(6) 0.149(10) 0.063(7) 0.077(8) 0.044(7) O302 0.092(8) 0.179(11) 0.086(7) -0.001(7) 0.014(7) -0.028(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.265(12) . ? C1 O2 1.300(13) . ? C1 C2 1.430(16) . ? C3 O3 1.272(11) . ? C3 C2 1.451(15) . ? C3 C4 1.465(16) . ? C4 C8 1.378(16) . ? C4 C5 1.428(15) . ? C5 C6 1.399(17) . ? C5 H5 0.9500 . ? C6 C7 1.386(17) . ? C6 H6 0.9500 . ? C7 C2 1.383(15) . ? C7 H7 0.9500 . ? C8 N9 1.335(14) . ? C8 H8 0.9500 . ? C10 N9 1.471(14) . ? C10 C11 1.486(15) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N12 1.483(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C14 1.463(15) . ? C13 N12 1.492(13) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N15 1.487(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C16 N15 1.243(14) . ? C16 C17 1.453(15) . ? C16 H16 0.9500 . ? C17 C22 1.413(15) . ? C17 C18 1.465(13) . ? C18 O4 1.269(11) . ? C18 C19 1.427(14) . ? C19 C20 1.451(14) . ? C19 C23 1.472(13) . ? C20 C21 1.412(14) . ? C20 H20 0.9500 . ? C21 C22 1.342(15) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 O5 1.232(12) . ? C23 O6 1.246(12) . ? C24 N12 1.449(12) . ? C24 C25 1.522(14) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N26 1.428(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 O8 1.225(11) . ? C27 O7 1.273(11) . ? C27 C28 1.517(12) . ? C28 C33 1.384(13) . ? C28 C29 1.472(12) . ? C29 O9 1.314(11) . ? C29 C30 1.372(13) . ? C30 C31 1.417(14) . ? C30 C34 1.469(14) . ? C31 C32 1.388(14) . ? C31 H31 0.9500 . ? C32 C33 1.371(13) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N35 1.246(13) . ? C34 H34 0.9500 . ? C36 N35 1.458(13) . ? C36 C37 1.544(14) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 N38 1.492(12) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C39 N38 1.424(12) . ? C39 C40 1.527(14) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N41 1.468(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C42 N41 1.347(14) . ? C42 C43 1.380(15) . ? C42 H42 0.9500 . ? C43 C48 1.403(14) . ? C43 C44 1.462(13) . ? C44 O10 1.291(11) . ? C44 C45 1.468(14) . ? C45 C46 1.354(14) . ? C45 C49 1.518(13) . ? C46 C47 1.408(15) . ? C46 H46 0.9500 . ? C47 C48 1.367(15) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O12 1.232(12) . ? C49 O11 1.296(12) . ? C50 N38 1.433(13) . ? C50 C51 1.519(14) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 N52 1.502(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C54 N53 1.496(12) . ? C54 C55 1.557(13) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 N56 1.447(13) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C57 N53 1.489(12) . ? C57 C58 1.535(12) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 N59 1.479(12) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C60 N53 1.402(13) . ? C60 C61 1.516(14) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 N62 1.469(12) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C64 N63 1.454(17) . ? C64 C65 1.55(2) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N66 1.427(15) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C67 C68 1.45(2) . ? C67 N63 1.55(2) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 N69 1.416(15) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C70 N63 1.522(15) . ? C70 C71 1.526(19) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 N72 1.472(15) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? N26 Ni1 2.050(9) . ? N26 H26A 0.9200 . ? N26 H26B 0.9200 . ? N52 Ni2 2.056(10) . ? N52 H52A 0.9200 . ? N52 H52B 0.9200 . ? N53 Ni1 2.104(8) . ? N56 Ni1 2.134(8) . ? N56 H56A 0.9200 . ? N56 H56B 0.9200 . ? N59 Ni1 2.128(7) . ? N59 H59A 0.9200 . ? N59 H59B 0.9200 . ? N62 Ni1 2.109(7) . ? N62 H62A 0.9200 . ? N62 H62B 0.9200 . ? N63 Ni2 2.046(11) . ? N66 Ni2 2.091(9) . ? N66 H66A 0.9200 . ? N66 H66B 0.9200 . ? N69 Ni2 2.129(10) . ? N69 H69A 0.9200 . ? N69 H69B 0.9200 . ? N72 Ni2 2.154(9) . ? N72 H72A 0.9200 . ? N72 H72B 0.9200 . ? O1 Gd1 2.345(6) . ? O3 Gd1 2.393(6) . ? O3 H3 0.9500 . ? O4 Gd1 2.369(6) . ? O4 H4 0.9500 . ? O5 Gd1 2.392(7) . ? O6 Ni2 2.143(7) . ? O7 Gd1 2.342(6) . ? O8 Ni1 2.138(6) . ? O9 Gd1 2.370(6) . ? O9 H9 0.9500 . ? O10 Gd1 2.389(6) . ? O10 H10 0.9500 . ? O11 Gd1 2.376(7) . ? N200 O201 1.234(8) . ? N200 O202 1.251(8) . ? N200 O200 1.257(8) . ? O102 N100 1.245(11) . ? O101 N100 1.241(11) . ? N100 O100 1.199(11) . ? O300 N300 1.262(11) . ? N300 O302 1.199(11) . ? N300 O301 1.254(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 119.6(11) . . ? O1 C1 C2 122.8(10) . . ? O2 C1 C2 117.5(10) . . ? O3 C3 C2 121.9(10) . . ? O3 C3 C4 121.0(10) . . ? C2 C3 C4 117.0(9) . . ? C8 C4 C5 116.9(11) . . ? C8 C4 C3 121.7(10) . . ? C5 C4 C3 121.3(11) . . ? C6 C5 C4 118.7(12) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C7 C6 C5 119.9(12) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C2 C7 C6 124.6(12) . . ? C2 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? N9 C8 C4 121.9(11) . . ? N9 C8 H8 119.0 . . ? C4 C8 H8 119.0 . . ? N9 C10 C11 109.2(10) . . ? N9 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N9 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N12 C11 C10 112.8(8) . . ? N12 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? N12 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C14 C13 N12 113.3(8) . . ? C14 C13 H13A 108.9 . . ? N12 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? N12 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 N15 110.1(8) . . ? C13 C14 H14A 109.6 . . ? N15 C14 H14A 109.6 . . ? C13 C14 H14B 109.6 . . ? N15 C14 H14B 109.6 . . ? H14A C14 H14B 108.2 . . ? N15 C16 C17 127.3(10) . . ? N15 C16 H16 116.4 . . ? C17 C16 H16 116.4 . . ? C22 C17 C16 120.9(9) . . ? C22 C17 C18 120.2(10) . . ? C16 C17 C18 118.9(10) . . ? O4 C18 C19 124.2(8) . . ? O4 C18 C17 119.3(9) . . ? C19 C18 C17 116.5(9) . . ? C18 C19 C20 119.7(9) . . ? C18 C19 C23 125.0(9) . . ? C20 C19 C23 115.3(9) . . ? C21 C20 C19 121.3(10) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 118.8(11) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C17 123.4(10) . . ? C21 C22 H22 118.3 . . ? C17 C22 H22 118.3 . . ? O5 C23 O6 122.6(9) . . ? O5 C23 C19 119.3(9) . . ? O6 C23 C19 118.1(9) . . ? N12 C24 C25 113.3(9) . . ? N12 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N12 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? N26 C25 C24 116.9(9) . . ? N26 C25 H25A 108.1 . . ? C24 C25 H25A 108.1 . . ? N26 C25 H25B 108.1 . . ? C24 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? O8 C27 O7 125.1(8) . . ? O8 C27 C28 115.2(8) . . ? O7 C27 C28 119.7(8) . . ? C33 C28 C29 117.7(8) . . ? C33 C28 C27 118.4(8) . . ? C29 C28 C27 123.8(8) . . ? O9 C29 C30 120.6(8) . . ? O9 C29 C28 122.2(8) . . ? C30 C29 C28 117.1(8) . . ? C29 C30 C31 123.0(9) . . ? C29 C30 C34 121.8(9) . . ? C31 C30 C34 115.2(8) . . ? C32 C31 C30 119.1(9) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C33 C32 C31 118.8(9) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C28 123.9(9) . . ? C32 C33 H33 118.0 . . ? C28 C33 H33 118.0 . . ? N35 C34 C30 126.3(9) . . ? N35 C34 H34 116.8 . . ? C30 C34 H34 116.8 . . ? N35 C36 C37 110.9(8) . . ? N35 C36 H36A 109.5 . . ? C37 C36 H36A 109.5 . . ? N35 C36 H36B 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 108.0 . . ? N38 C37 C36 109.4(7) . . ? N38 C37 H37A 109.8 . . ? C36 C37 H37A 109.8 . . ? N38 C37 H37B 109.8 . . ? C36 C37 H37B 109.8 . . ? H37A C37 H37B 108.2 . . ? N38 C39 C40 114.8(8) . . ? N38 C39 H39A 108.6 . . ? C40 C39 H39A 108.6 . . ? N38 C39 H39B 108.6 . . ? C40 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? N41 C40 C39 108.6(8) . . ? N41 C40 H40A 110.0 . . ? C39 C40 H40A 110.0 . . ? N41 C40 H40B 110.0 . . ? C39 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? N41 C42 C43 125.3(10) . . ? N41 C42 H42 117.4 . . ? C43 C42 H42 117.4 . . ? C42 C43 C48 121.2(10) . . ? C42 C43 C44 118.9(10) . . ? C48 C43 C44 119.9(9) . . ? O10 C44 C43 121.6(9) . . ? O10 C44 C45 122.7(9) . . ? C43 C44 C45 115.8(9) . . ? C46 C45 C44 119.8(9) . . ? C46 C45 C49 119.6(10) . . ? C44 C45 C49 120.6(9) . . ? C45 C46 C47 124.1(11) . . ? C45 C46 H46 117.9 . . ? C47 C46 H46 117.9 . . ? C48 C47 C46 117.6(11) . . ? C48 C47 H47 121.2 . . ? C46 C47 H47 121.2 . . ? C47 C48 C43 122.8(10) . . ? C47 C48 H48 118.6 . . ? C43 C48 H48 118.6 . . ? O12 C49 O11 124.7(9) . . ? O12 C49 C45 116.9(10) . . ? O11 C49 C45 118.4(9) . . ? N38 C50 C51 111.9(9) . . ? N38 C50 H50A 109.2 . . ? C51 C50 H50A 109.2 . . ? N38 C50 H50B 109.2 . . ? C51 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? N52 C51 C50 113.6(9) . . ? N52 C51 H51A 108.8 . . ? C50 C51 H51A 108.8 . . ? N52 C51 H51B 108.8 . . ? C50 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? N53 C54 C55 110.3(8) . . ? N53 C54 H54A 109.6 . . ? C55 C54 H54A 109.6 . . ? N53 C54 H54B 109.6 . . ? C55 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? N56 C55 C54 109.7(9) . . ? N56 C55 H55A 109.7 . . ? C54 C55 H55A 109.7 . . ? N56 C55 H55B 109.7 . . ? C54 C55 H55B 109.7 . . ? H55A C55 H55B 108.2 . . ? N53 C57 C58 112.8(8) . . ? N53 C57 H57A 109.0 . . ? C58 C57 H57A 109.0 . . ? N53 C57 H57B 109.0 . . ? C58 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? N59 C58 C57 112.4(7) . . ? N59 C58 H58A 109.1 . . ? C57 C58 H58A 109.1 . . ? N59 C58 H58B 109.1 . . ? C57 C58 H58B 109.1 . . ? H58A C58 H58B 107.9 . . ? N53 C60 C61 110.9(8) . . ? N53 C60 H60A 109.5 . . ? C61 C60 H60A 109.5 . . ? N53 C60 H60B 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 108.0 . . ? N62 C61 C60 108.7(8) . . ? N62 C61 H61A 109.9 . . ? C60 C61 H61A 109.9 . . ? N62 C61 H61B 109.9 . . ? C60 C61 H61B 109.9 . . ? H61A C61 H61B 108.3 . . ? N63 C64 C65 108.8(11) . . ? N63 C64 H64A 109.9 . . ? C65 C64 H64A 109.9 . . ? N63 C64 H64B 109.9 . . ? C65 C64 H64B 109.9 . . ? H64A C64 H64B 108.3 . . ? N66 C65 C64 111.4(12) . . ? N66 C65 H65A 109.3 . . ? C64 C65 H65A 109.3 . . ? N66 C65 H65B 109.3 . . ? C64 C65 H65B 109.3 . . ? H65A C65 H65B 108.0 . . ? C68 C67 N63 111.0(12) . . ? C68 C67 H67A 109.4 . . ? N63 C67 H67A 109.4 . . ? C68 C67 H67B 109.4 . . ? N63 C67 H67B 109.4 . . ? H67A C67 H67B 108.0 . . ? N69 C68 C67 110.4(10) . . ? N69 C68 H68A 109.6 . . ? C67 C68 H68A 109.6 . . ? N69 C68 H68B 109.6 . . ? C67 C68 H68B 109.6 . . ? H68A C68 H68B 108.1 . . ? N63 C70 C71 108.1(10) . . ? N63 C70 H70A 110.1 . . ? C71 C70 H70A 110.1 . . ? N63 C70 H70B 110.1 . . ? C71 C70 H70B 110.1 . . ? H70A C70 H70B 108.4 . . ? N72 C71 C70 109.7(11) . . ? N72 C71 H71A 109.7 . . ? C70 C71 H71A 109.7 . . ? N72 C71 H71B 109.7 . . ? C70 C71 H71B 109.7 . . ? H71A C71 H71B 108.2 . . ? C7 C2 C1 123.1(11) . . ? C7 C2 C3 118.4(11) . . ? C1 C2 C3 118.3(9) . . ? C8 N9 C10 126.6(10) . . ? C24 N12 C11 113.3(9) . . ? C24 N12 C13 114.3(8) . . ? C11 N12 C13 110.0(7) . . ? C16 N15 C14 121.6(9) . . ? C25 N26 Ni1 124.8(7) . . ? C25 N26 H26A 106.1 . . ? Ni1 N26 H26A 106.1 . . ? C25 N26 H26B 106.1 . . ? Ni1 N26 H26B 106.1 . . ? H26A N26 H26B 106.3 . . ? C34 N35 C36 123.3(9) . . ? C39 N38 C50 113.6(8) . . ? C39 N38 C37 109.7(8) . . ? C50 N38 C37 110.3(8) . . ? C42 N41 C40 125.2(9) . . ? C51 N52 Ni2 115.6(7) . . ? C51 N52 H52A 108.4 . . ? Ni2 N52 H52A 108.4 . . ? C51 N52 H52B 108.4 . . ? Ni2 N52 H52B 108.4 . . ? H52A N52 H52B 107.4 . . ? C60 N53 C57 110.9(8) . . ? C60 N53 C54 113.1(7) . . ? C57 N53 C54 112.3(8) . . ? C60 N53 Ni1 107.7(7) . . ? C57 N53 Ni1 110.0(6) . . ? C54 N53 Ni1 102.5(6) . . ? C55 N56 Ni1 108.6(6) . . ? C55 N56 H56A 110.0 . . ? Ni1 N56 H56A 110.0 . . ? C55 N56 H56B 110.0 . . ? Ni1 N56 H56B 110.0 . . ? H56A N56 H56B 108.4 . . ? C58 N59 Ni1 106.7(5) . . ? C58 N59 H59A 110.4 . . ? Ni1 N59 H59A 110.4 . . ? C58 N59 H59B 110.4 . . ? Ni1 N59 H59B 110.4 . . ? H59A N59 H59B 108.6 . . ? C61 N62 Ni1 112.0(5) . . ? C61 N62 H62A 109.2 . . ? Ni1 N62 H62A 109.2 . . ? C61 N62 H62B 109.2 . . ? Ni1 N62 H62B 109.2 . . ? H62A N62 H62B 107.9 . . ? C64 N63 C70 114.1(11) . . ? C64 N63 C67 110.2(11) . . ? C70 N63 C67 109.8(11) . . ? C64 N63 Ni2 114.3(9) . . ? C70 N63 Ni2 104.5(7) . . ? C67 N63 Ni2 103.3(9) . . ? C65 N66 Ni2 108.6(7) . . ? C65 N66 H66A 110.0 . . ? Ni2 N66 H66A 110.0 . . ? C65 N66 H66B 110.0 . . ? Ni2 N66 H66B 110.0 . . ? H66A N66 H66B 108.3 . . ? C68 N69 Ni2 109.1(8) . . ? C68 N69 H69A 109.9 . . ? Ni2 N69 H69A 109.9 . . ? C68 N69 H69B 109.9 . . ? Ni2 N69 H69B 109.9 . . ? H69A N69 H69B 108.3 . . ? C71 N72 Ni2 109.8(8) . . ? C71 N72 H72A 109.7 . . ? Ni2 N72 H72A 109.7 . . ? C71 N72 H72B 109.7 . . ? Ni2 N72 H72B 109.7 . . ? H72A N72 H72B 108.2 . . ? C1 O1 Gd1 132.8(6) . . ? C3 O3 Gd1 130.8(6) . . ? C3 O3 H3 114.6 . . ? Gd1 O3 H3 114.6 . . ? C18 O4 Gd1 136.5(6) . . ? C18 O4 H4 111.8 . . ? Gd1 O4 H4 111.8 . . ? C23 O5 Gd1 138.9(7) . . ? C23 O6 Ni2 131.1(7) . . ? C27 O7 Gd1 138.0(6) . . ? C27 O8 Ni1 130.2(6) . . ? C29 O9 Gd1 134.0(5) . . ? C29 O9 H9 113.0 . . ? Gd1 O9 H9 113.0 . . ? C44 O10 Gd1 130.8(5) . . ? C44 O10 H10 114.6 . . ? Gd1 O10 H10 114.6 . . ? C49 O11 Gd1 137.5(6) . . ? O201 N200 O202 116.0(8) . . ? O201 N200 O200 122.8(8) . . ? O202 N200 O200 121.0(7) . . ? N26 Ni1 N53 177.4(3) . . ? N26 Ni1 N62 98.3(3) . . ? N53 Ni1 N62 80.0(3) . . ? N26 Ni1 N59 93.8(3) . . ? N53 Ni1 N59 84.2(3) . . ? N62 Ni1 N59 92.5(3) . . ? N26 Ni1 N56 97.3(3) . . ? N53 Ni1 N56 84.6(3) . . ? N62 Ni1 N56 163.3(3) . . ? N59 Ni1 N56 92.4(3) . . ? N26 Ni1 O8 91.2(3) . . ? N53 Ni1 O8 90.6(3) . . ? N62 Ni1 O8 82.0(3) . . ? N59 Ni1 O8 173.1(3) . . ? N56 Ni1 O8 91.7(3) . . ? N63 Ni2 N52 175.4(4) . . ? N63 Ni2 N66 81.9(4) . . ? N52 Ni2 N66 94.5(4) . . ? N63 Ni2 N69 83.6(4) . . ? N52 Ni2 N69 94.0(4) . . ? N66 Ni2 N69 96.2(4) . . ? N63 Ni2 O6 93.3(4) . . ? N52 Ni2 O6 90.1(3) . . ? N66 Ni2 O6 173.9(4) . . ? N69 Ni2 O6 79.5(3) . . ? N63 Ni2 N72 82.1(4) . . ? N52 Ni2 N72 100.8(4) . . ? N66 Ni2 N72 91.4(4) . . ? N69 Ni2 N72 162.7(4) . . ? O6 Ni2 N72 91.6(3) . . ? O7 Gd1 O1 146.5(2) . . ? O7 Gd1 O4 79.6(2) . . ? O1 Gd1 O4 87.9(2) . . ? O7 Gd1 O9 71.9(2) . . ? O1 Gd1 O9 102.9(2) . . ? O4 Gd1 O9 142.8(2) . . ? O7 Gd1 O11 72.7(2) . . ? O1 Gd1 O11 140.8(2) . . ? O4 Gd1 O11 104.8(2) . . ? O9 Gd1 O11 89.2(2) . . ? O7 Gd1 O10 128.4(2) . . ? O1 Gd1 O10 76.9(2) . . ? O4 Gd1 O10 145.7(2) . . ? O9 Gd1 O10 71.2(2) . . ? O11 Gd1 O10 72.0(2) . . ? O7 Gd1 O5 73.4(2) . . ? O1 Gd1 O5 73.2(2) . . ? O4 Gd1 O5 71.1(2) . . ? O9 Gd1 O5 78.1(2) . . ? O11 Gd1 O5 146.0(2) . . ? O10 Gd1 O5 130.5(2) . . ? O7 Gd1 O3 130.4(2) . . ? O1 Gd1 O3 71.7(2) . . ? O4 Gd1 O3 70.5(2) . . ? O9 Gd1 O3 146.6(2) . . ? O11 Gd1 O3 77.8(2) . . ? O10 Gd1 O3 75.6(2) . . ? O5 Gd1 O3 128.1(3) . . ? O100 N100 O101 123.2(16) . . ? O100 N100 O102 121.2(16) . . ? O101 N100 O102 115.6(12) . . ? O302 N300 O301 123.8(14) . . ? O302 N300 O300 116.7(14) . . ? O301 N300 O300 116.7(13) . . ? 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 C3 C4 C8 1.4(14) . . . . ? C2 C3 C4 C8 178.7(9) . . . . ? O3 C3 C4 C5 177.8(9) . . . . ? C2 C3 C4 C5 -4.9(13) . . . . ? C8 C4 C5 C6 -179.9(10) . . . . ? C3 C4 C5 C6 3.6(15) . . . . ? C4 C5 C6 C7 -0.2(17) . . . . ? C5 C6 C7 C2 -2.0(18) . . . . ? C5 C4 C8 N9 -175.4(9) . . . . ? C3 C4 C8 N9 1.1(15) . . . . ? N9 C10 C11 N12 57.8(12) . . . . ? N12 C13 C14 N15 66.6(12) . . . . ? N15 C16 C17 C22 -178.3(12) . . . . ? N15 C16 C17 C18 1.9(18) . . . . ? C22 C17 C18 O4 -173.9(10) . . . . ? C16 C17 C18 O4 5.9(15) . . . . ? C22 C17 C18 C19 5.2(15) . . . . ? C16 C17 C18 C19 -175.1(10) . . . . ? O4 C18 C19 C20 176.0(10) . . . . ? C17 C18 C19 C20 -3.0(15) . . . . ? O4 C18 C19 C23 -4.0(17) . . . . ? C17 C18 C19 C23 177.0(10) . . . . ? C18 C19 C20 C21 -0.4(16) . . . . ? C23 C19 C20 C21 179.5(10) . . . . ? C19 C20 C21 C22 1.8(17) . . . . ? C20 C21 C22 C17 0.4(19) . . . . ? C16 C17 C22 C21 176.2(11) . . . . ? C18 C17 C22 C21 -4.1(18) . . . . ? C18 C19 C23 O5 10.5(17) . . . . ? C20 C19 C23 O5 -169.4(10) . . . . ? C18 C19 C23 O6 -167.3(10) . . . . ? C20 C19 C23 O6 12.7(15) . . . . ? N12 C24 C25 N26 -178.9(8) . . . . ? O8 C27 C28 C33 1.1(13) . . . . ? O7 C27 C28 C33 -177.8(9) . . . . ? O8 C27 C28 C29 178.0(9) . . . . ? O7 C27 C28 C29 -0.9(14) . . . . ? C33 C28 C29 O9 177.0(9) . . . . ? C27 C28 C29 O9 0.1(14) . . . . ? C33 C28 C29 C30 -0.4(14) . . . . ? C27 C28 C29 C30 -177.4(9) . . . . ? O9 C29 C30 C31 -176.8(10) . . . . ? C28 C29 C30 C31 0.7(16) . . . . ? O9 C29 C30 C34 4.9(16) . . . . ? C28 C29 C30 C34 -177.7(9) . . . . ? C29 C30 C31 C32 -3.7(18) . . . . ? C34 C30 C31 C32 174.8(11) . . . . ? C30 C31 C32 C33 6.3(18) . . . . ? C31 C32 C33 C28 -6.3(17) . . . . ? C29 C28 C33 C32 3.3(15) . . . . ? C27 C28 C33 C32 -179.6(10) . . . . ? C29 C30 C34 N35 2.5(19) . . . . ? C31 C30 C34 N35 -176.0(12) . . . . ? N35 C36 C37 N38 66.5(11) . . . . ? N38 C39 C40 N41 55.7(11) . . . . ? N41 C42 C43 C48 -179.4(9) . . . . ? N41 C42 C43 C44 -2.2(15) . . . . ? C42 C43 C44 O10 2.8(13) . . . . ? C48 C43 C44 O10 -179.9(8) . . . . ? C42 C43 C44 C45 -179.4(8) . . . . ? C48 C43 C44 C45 -2.1(12) . . . . ? O10 C44 C45 C46 177.6(8) . . . . ? C43 C44 C45 C46 -0.1(12) . . . . ? O10 C44 C45 C49 -4.5(13) . . . . ? C43 C44 C45 C49 177.8(8) . . . . ? C44 C45 C46 C47 2.3(15) . . . . ? C49 C45 C46 C47 -175.7(10) . . . . ? C45 C46 C47 C48 -2.1(16) . . . . ? C46 C47 C48 C43 -0.4(16) . . . . ? C42 C43 C48 C47 179.7(10) . . . . ? C44 C43 C48 C47 2.4(15) . . . . ? C46 C45 C49 O12 -33.2(12) . . . . ? C44 C45 C49 O12 148.8(9) . . . . ? C46 C45 C49 O11 146.5(9) . . . . ? C44 C45 C49 O11 -31.4(12) . . . . ? N38 C50 C51 N52 -174.4(8) . . . . ? N53 C54 C55 N56 53.9(11) . . . . ? N53 C57 C58 N59 40.6(11) . . . . ? N53 C60 C61 N62 -46.7(11) . . . . ? N63 C64 C65 N66 -40.5(16) . . . . ? N63 C67 C68 N69 -52.8(16) . . . . ? N63 C70 C71 N72 49.2(13) . . . . ? C6 C7 C2 C1 -174.8(10) . . . . ? C6 C7 C2 C3 0.5(16) . . . . ? O1 C1 C2 C7 136.3(10) . . . . ? O2 C1 C2 C7 -39.2(14) . . . . ? O1 C1 C2 C3 -39.0(13) . . . . ? O2 C1 C2 C3 145.5(9) . . . . ? O3 C3 C2 C7 -179.9(9) . . . . ? C4 C3 C2 C7 2.8(13) . . . . ? O3 C3 C2 C1 -4.4(13) . . . . ? C4 C3 C2 C1 178.3(8) . . . . ? C4 C8 N9 C10 -179.5(9) . . . . ? C11 C10 N9 C8 110.3(11) . . . . ? C25 C24 N12 C11 -163.5(8) . . . . ? C25 C24 N12 C13 69.4(10) . . . . ? C10 C11 N12 C24 79.8(11) . . . . ? C10 C11 N12 C13 -150.9(9) . . . . ? C14 C13 N12 C24 -141.2(9) . . . . ? C14 C13 N12 C11 90.0(11) . . . . ? C17 C16 N15 C14 -176.3(10) . . . . ? C13 C14 N15 C16 113.3(12) . . . . ? C24 C25 N26 Ni1 178.3(6) . . . . ? C30 C34 N35 C36 179.7(11) . . . . ? C37 C36 N35 C34 125.5(12) . . . . ? C40 C39 N38 C50 82.4(10) . . . . ? C40 C39 N38 C37 -153.6(8) . . . . ? C51 C50 N38 C39 -162.9(8) . . . . ? C51 C50 N38 C37 73.4(10) . . . . ? C36 C37 N38 C39 89.3(9) . . . . ? C36 C37 N38 C50 -144.8(9) . . . . ? C43 C42 N41 C40 179.5(9) . . . . ? C39 C40 N41 C42 118.8(10) . . . . ? C50 C51 N52 Ni2 177.6(6) . . . . ? C61 C60 N53 C57 -72.0(11) . . . . ? C61 C60 N53 C54 160.9(9) . . . . ? C61 C60 N53 Ni1 48.4(10) . . . . ? C58 C57 N53 C60 98.6(10) . . . . ? C58 C57 N53 C54 -133.9(8) . . . . ? C58 C57 N53 Ni1 -20.5(10) . . . . ? C55 C54 N53 C60 -164.6(9) . . . . ? C55 C54 N53 C57 69.0(10) . . . . ? C55 C54 N53 Ni1 -49.0(9) . . . . ? C54 C55 N56 Ni1 -27.7(9) . . . . ? C57 C58 N59 Ni1 -38.5(9) . . . . ? C60 C61 N62 Ni1 21.2(9) . . . . ? C65 C64 N63 C70 -100.0(13) . . . . ? C65 C64 N63 C67 135.9(13) . . . . ? C65 C64 N63 Ni2 20.2(14) . . . . ? C71 C70 N63 C64 71.3(14) . . . . ? C71 C70 N63 C67 -164.4(11) . . . . ? C71 C70 N63 Ni2 -54.2(12) . . . . ? C68 C67 N63 C64 -76.1(15) . . . . ? C68 C67 N63 C70 157.4(12) . . . . ? C68 C67 N63 Ni2 46.4(13) . . . . ? C64 C65 N66 Ni2 40.5(13) . . . . ? C67 C68 N69 Ni2 30.5(14) . . . . ? C70 C71 N72 Ni2 -19.8(11) . . . . ? O2 C1 O1 Gd1 -141.3(8) . . . . ? C2 C1 O1 Gd1 43.2(14) . . . . ? C2 C3 O3 Gd1 44.2(13) . . . . ? C4 C3 O3 Gd1 -138.7(7) . . . . ? C19 C18 O4 Gd1 12.6(16) . . . . ? C17 C18 O4 Gd1 -168.5(7) . . . . ? O6 C23 O5 Gd1 149.7(8) . . . . ? C19 C23 O5 Gd1 -28.1(16) . . . . ? O5 C23 O6 Ni2 14.8(17) . . . . ? C19 C23 O6 Ni2 -167.4(8) . . . . ? O8 C27 O7 Gd1 155.2(7) . . . . ? C28 C27 O7 Gd1 -26.1(14) . . . . ? O7 C27 O8 Ni1 -0.8(15) . . . . ? C28 C27 O8 Ni1 -179.5(6) . . . . ? C30 C29 O9 Gd1 -157.1(7) . . . . ? C28 C29 O9 Gd1 25.5(13) . . . . ? C43 C44 O10 Gd1 -137.6(7) . . . . ? C45 C44 O10 Gd1 44.8(12) . . . . ? O12 C49 O11 Gd1 -149.1(7) . . . . ? C45 C49 O11 Gd1 31.3(13) . . . . ? C25 N26 Ni1 N53 -136(7) . . . . ? C25 N26 Ni1 N62 173.6(7) . . . . ? C25 N26 Ni1 N59 -93.2(8) . . . . ? C25 N26 Ni1 N56 -0.3(8) . . . . ? C25 N26 Ni1 O8 91.6(7) . . . . ? C60 N53 Ni1 N26 -78(7) . . . . ? C57 N53 Ni1 N26 43(7) . . . . ? C54 N53 Ni1 N26 162(7) . . . . ? C60 N53 Ni1 N62 -27.8(6) . . . . ? C57 N53 Ni1 N62 93.1(6) . . . . ? C54 N53 Ni1 N62 -147.3(6) . . . . ? C60 N53 Ni1 N59 -121.4(6) . . . . ? C57 N53 Ni1 N59 -0.5(6) . . . . ? C54 N53 Ni1 N59 119.1(6) . . . . ? C60 N53 Ni1 N56 145.6(6) . . . . ? C57 N53 Ni1 N56 -93.5(6) . . . . ? C54 N53 Ni1 N56 26.1(6) . . . . ? C60 N53 Ni1 O8 53.9(6) . . . . ? C57 N53 Ni1 O8 174.9(6) . . . . ? C54 N53 Ni1 O8 -65.6(6) . . . . ? C61 N62 Ni1 N26 -179.4(6) . . . . ? C61 N62 Ni1 N53 2.6(6) . . . . ? C61 N62 Ni1 N59 86.3(6) . . . . ? C61 N62 Ni1 N56 -20.9(14) . . . . ? C61 N62 Ni1 O8 -89.4(6) . . . . ? C58 N59 Ni1 N26 -156.9(6) . . . . ? C58 N59 Ni1 N53 21.3(6) . . . . ? C58 N59 Ni1 N62 -58.4(6) . . . . ? C58 N59 Ni1 N56 105.7(6) . . . . ? C58 N59 Ni1 O8 -21(3) . . . . ? C55 N56 Ni1 N26 -177.2(6) . . . . ? C55 N56 Ni1 N53 1.0(6) . . . . ? C55 N56 Ni1 N62 24.2(13) . . . . ? C55 N56 Ni1 N59 -83.0(6) . . . . ? C55 N56 Ni1 O8 91.4(6) . . . . ? C27 O8 Ni1 N26 -68.9(9) . . . . ? C27 O8 Ni1 N53 113.1(9) . . . . ? C27 O8 Ni1 N62 -167.1(9) . . . . ? C27 O8 Ni1 N59 155(2) . . . . ? C27 O8 Ni1 N56 28.5(9) . . . . ? C64 N63 Ni2 N52 38(6) . . . . ? C70 N63 Ni2 N52 164(5) . . . . ? C67 N63 Ni2 N52 -81(6) . . . . ? C64 N63 Ni2 N66 0.5(10) . . . . ? C70 N63 Ni2 N66 125.9(9) . . . . ? C67 N63 Ni2 N66 -119.1(8) . . . . ? C64 N63 Ni2 N69 97.8(10) . . . . ? C70 N63 Ni2 N69 -136.8(9) . . . . ? C67 N63 Ni2 N69 -21.9(8) . . . . ? C64 N63 Ni2 O6 176.8(9) . . . . ? C70 N63 Ni2 O6 -57.8(9) . . . . ? C67 N63 Ni2 O6 57.1(8) . . . . ? C64 N63 Ni2 N72 -92.0(10) . . . . ? C70 N63 Ni2 N72 33.4(9) . . . . ? C67 N63 Ni2 N72 148.3(8) . . . . ? C51 N52 Ni2 N63 -134(5) . . . . ? C51 N52 Ni2 N66 -96.5(7) . . . . ? C51 N52 Ni2 N69 166.9(7) . . . . ? C51 N52 Ni2 O6 87.5(7) . . . . ? C51 N52 Ni2 N72 -4.2(7) . . . . ? C65 N66 Ni2 N63 -23.1(10) . . . . ? C65 N66 Ni2 N52 159.7(10) . . . . ? C65 N66 Ni2 N69 -105.7(10) . . . . ? C65 N66 Ni2 O6 -61(4) . . . . ? C65 N66 Ni2 N72 58.7(10) . . . . ? C68 N69 Ni2 N63 -3.3(8) . . . . ? C68 N69 Ni2 N52 172.8(8) . . . . ? C68 N69 Ni2 N66 77.8(8) . . . . ? C68 N69 Ni2 O6 -97.9(8) . . . . ? C68 N69 Ni2 N72 -37.8(16) . . . . ? C23 O6 Ni2 N63 98.5(11) . . . . ? C23 O6 Ni2 N52 -84.5(10) . . . . ? C23 O6 Ni2 N66 136(3) . . . . ? C23 O6 Ni2 N69 -178.6(11) . . . . ? C23 O6 Ni2 N72 16.3(11) . . . . ? C71 N72 Ni2 N63 -8.1(8) . . . . ? C71 N72 Ni2 N52 175.4(7) . . . . ? C71 N72 Ni2 N66 -89.7(8) . . . . ? C71 N72 Ni2 N69 26.6(16) . . . . ? C71 N72 Ni2 O6 85.0(8) . . . . ? C27 O7 Gd1 O1 119.8(9) . . . . ? C27 O7 Gd1 O4 -170.5(9) . . . . ? C27 O7 Gd1 O9 33.6(8) . . . . ? C27 O7 Gd1 O11 -61.3(9) . . . . ? C27 O7 Gd1 O10 -12.6(10) . . . . ? C27 O7 Gd1 O5 116.3(9) . . . . ? C27 O7 Gd1 O3 -117.5(8) . . . . ? C1 O1 Gd1 O7 127.7(9) . . . . ? C1 O1 Gd1 O4 60.3(9) . . . . ? C1 O1 Gd1 O9 -155.6(9) . . . . ? C1 O1 Gd1 O11 -50.7(10) . . . . ? C1 O1 Gd1 O10 -88.7(9) . . . . ? C1 O1 Gd1 O5 131.3(10) . . . . ? C1 O1 Gd1 O3 -9.8(9) . . . . ? C18 O4 Gd1 O7 -92.1(9) . . . . ? C18 O4 Gd1 O1 56.7(9) . . . . ? C18 O4 Gd1 O9 -52.1(11) . . . . ? C18 O4 Gd1 O11 -160.9(9) . . . . ? C18 O4 Gd1 O10 119.6(9) . . . . ? C18 O4 Gd1 O5 -16.2(9) . . . . ? C18 O4 Gd1 O3 128.1(10) . . . . ? C29 O9 Gd1 O7 -31.9(8) . . . . ? C29 O9 Gd1 O1 -177.4(8) . . . . ? C29 O9 Gd1 O4 -73.6(9) . . . . ? C29 O9 Gd1 O11 40.2(8) . . . . ? C29 O9 Gd1 O10 111.4(8) . . . . ? C29 O9 Gd1 O5 -108.0(8) . . . . ? C29 O9 Gd1 O3 106.2(9) . . . . ? C49 O11 Gd1 O7 138.5(9) . . . . ? C49 O11 Gd1 O1 -42.4(10) . . . . ? C49 O11 Gd1 O4 -147.6(9) . . . . ? C49 O11 Gd1 O9 67.2(9) . . . . ? C49 O11 Gd1 O10 -3.2(9) . . . . ? C49 O11 Gd1 O5 134.3(9) . . . . ? C49 O11 Gd1 O3 -81.8(9) . . . . ? C44 O10 Gd1 O7 -85.1(8) . . . . ? C44 O10 Gd1 O1 119.7(8) . . . . ? C44 O10 Gd1 O4 53.7(9) . . . . ? C44 O10 Gd1 O9 -131.6(8) . . . . ? C44 O10 Gd1 O11 -36.2(7) . . . . ? C44 O10 Gd1 O5 173.6(7) . . . . ? C44 O10 Gd1 O3 45.5(7) . . . . ? C23 O5 Gd1 O7 110.2(10) . . . . ? C23 O5 Gd1 O1 -67.8(10) . . . . ? C23 O5 Gd1 O4 25.8(10) . . . . ? C23 O5 Gd1 O9 -175.4(11) . . . . ? C23 O5 Gd1 O11 114.4(10) . . . . ? C23 O5 Gd1 O10 -123.1(10) . . . . ? C23 O5 Gd1 O3 -18.5(11) . . . . ? C3 O3 Gd1 O7 175.8(8) . . . . ? C3 O3 Gd1 O1 -33.5(9) . . . . ? C3 O3 Gd1 O4 -127.8(9) . . . . ? C3 O3 Gd1 O9 52.3(11) . . . . ? C3 O3 Gd1 O11 121.5(9) . . . . ? C3 O3 Gd1 O10 47.2(9) . . . . ? C3 O3 Gd1 O5 -83.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.354 _refine_diff_density_min -1.510 _refine_diff_density_rms 0.164 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 -0.007 0.486 1307 9 ' ' 2 0.059 0.690 0.010 7 0 ' ' 3 0.940 0.309 0.990 7 0 ' ' _platon_squeeze_details ; disordered solvent water ;