# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_1188 _database_code_depnum_ccdc_archive 'CCDC 898018' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 N8 Ni4 O24 Pr2, 8(H2 O)' _chemical_formula_sum 'C60 H74 N8 Ni4 O32 Pr2' _chemical_formula_weight 1935.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.770(4) _cell_length_b 18.183(6) _cell_length_c 15.616(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.262(5) _cell_angle_gamma 90.00 _cell_volume 3568(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2200 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.96 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6514 _exptl_absorpt_correction_T_max 0.7730 _exptl_absorpt_process_details 'SADABS (Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14792 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6260 _reflns_number_gt 4236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^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 6260 _refine_ls_number_parameters 488 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.987 _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 Pr1 Pr 0.08488(3) -0.06212(2) 0.59547(3) 0.02416(13) Uani 1 1 d . . . Ni2 Ni 0.31692(7) -0.05487(5) 0.71169(6) 0.0278(2) Uani 1 1 d . . . Ni1 Ni 0.16464(7) 0.10151(5) 0.71143(6) 0.0287(2) Uani 1 1 d . . . N1 N 0.3088(5) 0.1597(3) 0.7698(4) 0.0317(15) Uani 1 1 d . . . N2 N 0.1506(5) 0.1802(4) 0.6185(5) 0.0491(19) Uani 1 1 d . . . H2A H 0.1260 0.1605 0.5659 0.059 Uiso 1 1 calc R . . H2B H 0.1050 0.2153 0.6292 0.059 Uiso 1 1 calc R . . N3 N 0.1073(5) 0.1497(3) 0.8052(4) 0.0385(17) Uani 1 1 d . . . N4 N 0.3430(5) 0.0046(3) 0.8223(4) 0.0347(16) Uani 1 1 d . . . O1 O 0.0278(4) 0.0427(3) 0.6777(3) 0.0298(12) Uani 1 1 d . . . O2 O -0.0921(3) -0.0188(3) 0.5319(3) 0.0278(12) Uani 1 1 d . . . O3 O -0.2552(4) -0.0535(3) 0.5426(3) 0.0425(14) Uani 1 1 d . . . O4 O 0.1753(4) -0.0860(3) 0.7408(3) 0.0298(12) Uani 1 1 d . . . O5 O -0.0209(4) -0.1375(3) 0.6685(3) 0.0413(14) Uani 1 1 d . . . O6 O -0.1102(6) -0.1840(5) 0.7629(5) 0.097(3) Uani 1 1 d U . . O7 O 0.4525(4) -0.0314(3) 0.6632(4) 0.0394(13) Uani 1 1 d . . . O8 O 0.2633(4) -0.1135(3) 0.6012(3) 0.0290(12) Uani 1 1 d . . . O9 O 0.0831(4) -0.1599(3) 0.4950(3) 0.0377(13) Uani 1 1 d . . . O10 O 0.1158(5) -0.2539(3) 0.4131(4) 0.0606(19) Uani 1 1 d . . . O11 O 0.2298(3) 0.0272(3) 0.6439(3) 0.0275(11) Uani 1 1 d . . . H11 H 0.2364 0.0556 0.6043 0.06(3) Uiso 1 1 d R . . C1 C 0.2568(7) 0.2115(5) 0.6207(6) 0.049(2) Uani 1 1 d . . . H1A H 0.2512 0.2573 0.5883 0.059 Uiso 1 1 calc R . . H1B H 0.3002 0.1777 0.5941 0.059 Uiso 1 1 calc R . . C2 C 0.3066(7) 0.2251(5) 0.7120(6) 0.049(2) Uani 1 1 d . . . H2C H 0.2682 0.2644 0.7349 0.059 Uiso 1 1 calc R . . H2D H 0.3790 0.2419 0.7134 0.059 Uiso 1 1 calc R . . C3 C 0.2938(6) 0.1834(5) 0.8582(5) 0.044(2) Uani 1 1 d . . . H3A H 0.3383 0.2258 0.8764 0.053 Uiso 1 1 calc R . . H3B H 0.3152 0.1439 0.8995 0.053 Uiso 1 1 calc R . . C4 C 0.1797(6) 0.2026(4) 0.8574(5) 0.044(2) Uani 1 1 d . . . H4A H 0.1663 0.2029 0.9167 0.053 Uiso 1 1 calc R . . H4B H 0.1656 0.2516 0.8336 0.053 Uiso 1 1 calc R . . C5 C 0.0138(7) 0.1437(4) 0.8201(5) 0.040(2) Uani 1 1 d . . . H5 H -0.0012 0.1709 0.8669 0.048 Uiso 1 1 calc R . . C6 C -0.0729(6) 0.1003(5) 0.7741(5) 0.042(2) Uani 1 1 d . . . C7 C -0.1716(7) 0.1077(6) 0.8026(6) 0.061(3) Uani 1 1 d . . . H7 H -0.1764 0.1385 0.8493 0.074 Uiso 1 1 calc R . . C8 C -0.2604(7) 0.0702(6) 0.7626(6) 0.061(3) Uani 1 1 d . . . H8 H -0.3240 0.0737 0.7834 0.073 Uiso 1 1 calc R . . C9 C -0.2538(6) 0.0275(5) 0.6916(6) 0.051(2) Uani 1 1 d . . . H9 H -0.3146 0.0030 0.6642 0.061 Uiso 1 1 calc R . . C10 C -0.1593(6) 0.0192(4) 0.6583(5) 0.0356(19) Uani 1 1 d . . . C11 C -0.1713(6) -0.0205(4) 0.5744(5) 0.0307(18) Uani 1 1 d . . . C12 C -0.0642(6) 0.0530(4) 0.7017(5) 0.0286(17) Uani 1 1 d . . . C13 C 0.4111(6) 0.1207(4) 0.7732(5) 0.036(2) Uani 1 1 d . . . H13A H 0.4683 0.1560 0.7883 0.044 Uiso 1 1 calc R . . H13B H 0.4142 0.1026 0.7152 0.044 Uiso 1 1 calc R . . C14 C 0.4321(6) 0.0567(5) 0.8360(5) 0.043(2) Uani 1 1 d . . . H14A H 0.4967 0.0316 0.8279 0.052 Uiso 1 1 calc R . . H14B H 0.4427 0.0750 0.8953 0.052 Uiso 1 1 calc R . . C15 C 0.2941(7) -0.0070(5) 0.8865(5) 0.043(2) Uani 1 1 d . . . H15 H 0.3242 0.0148 0.9390 0.052 Uiso 1 1 calc R . . C16 C 0.1990(7) -0.0495(5) 0.8874(5) 0.047(2) Uani 1 1 d . . . C17 C 0.1602(9) -0.0476(6) 0.9647(6) 0.070(3) Uani 1 1 d . . . H17 H 0.2003 -0.0247 1.0129 0.084 Uiso 1 1 calc R . . C18 C 0.0646(11) -0.0783(7) 0.9721(8) 0.092(4) Uani 1 1 d . . . H18 H 0.0404 -0.0772 1.0248 0.110 Uiso 1 1 calc R . . C19 C 0.0052(8) -0.1108(6) 0.9009(7) 0.067(3) Uani 1 1 d . . . H19 H -0.0596 -0.1321 0.9058 0.080 Uiso 1 1 calc R . . C20 C 0.0393(7) -0.1128(4) 0.8209(5) 0.039(2) Uani 1 1 d . . . C21 C -0.0345(6) -0.1472(5) 0.7452(6) 0.044(2) Uani 1 1 d . . . C22 C 0.1386(6) -0.0833(4) 0.8134(5) 0.0347(19) Uani 1 1 d . . . C23 C 0.4781(6) -0.0612(5) 0.5995(6) 0.043(2) Uani 1 1 d . . . H23 H 0.5463 -0.0501 0.5902 0.051 Uiso 1 1 calc R . . C24 C 0.4194(6) -0.1102(4) 0.5376(5) 0.0317(18) Uani 1 1 d . . . C25 C 0.4730(7) -0.1361(5) 0.4723(6) 0.051(2) Uani 1 1 d . . . H25 H 0.5431 -0.1220 0.4727 0.061 Uiso 1 1 calc R . . C26 C 0.4231(7) -0.1817(5) 0.4083(6) 0.057(3) Uani 1 1 d . . . H26 H 0.4598 -0.1993 0.3661 0.068 Uiso 1 1 calc R . . C27 C 0.3165(7) -0.2021(5) 0.4058(5) 0.041(2) Uani 1 1 d . . . H27 H 0.2838 -0.2335 0.3622 0.050 Uiso 1 1 calc R . . C28 C 0.2584(6) -0.1762(4) 0.4674(5) 0.0316(18) Uani 1 1 d . . . C29 C 0.1451(6) -0.1985(4) 0.4581(5) 0.0343(19) Uani 1 1 d . . . C30 C 0.3126(6) -0.1321(4) 0.5379(5) 0.0288(17) Uani 1 1 d . . . O1W O 0.3955(4) -0.1424(3) 0.7778(3) 0.0408(14) Uani 1 1 d . . . H1WA H 0.3805 -0.1705 0.8175 0.049 Uiso 1 1 d R . . H1WB H 0.4599 -0.1525 0.7752 0.049 Uiso 1 1 d R . . O2W O 0.7167(5) 0.8107(4) 0.6360(4) 0.078(2) Uani 1 1 d . . . H2WA H 0.7215 0.8461 0.6013 0.093 Uiso 1 1 d R . . H2WB H 0.7634 0.8201 0.6806 0.093 Uiso 1 1 d R . . O3W O 0.4641(5) 0.8513(4) 0.9546(4) 0.078(2) Uani 1 1 d . . . H3WA H 0.5230 0.8742 0.9600 0.094 Uiso 1 1 d R . . H3WB H 0.4791 0.8075 0.9421 0.094 Uiso 1 1 d R . . O4W O 0.8828(6) 0.7258(4) 0.5795(5) 0.104(3) Uani 1 1 d . . . H4WA H 0.9180 0.6932 0.5578 0.125 Uiso 1 1 d R . . H4WB H 0.9289 0.7578 0.6004 0.125 Uiso 1 1 d R . . O5W O 0.5716(6) 0.8021(5) 0.7412(5) 0.068(3) Uani 0.75 1 d P . . H5WA H 0.5784 0.7559 0.7354 0.082 Uiso 0.75 1 d PR . . H5WB H 0.6050 0.8113 0.7922 0.082 Uiso 0.75 1 d PR . . O6W O 0.2758(17) 0.1011(11) 0.0866(13) 0.047(6) Uani 0.25 1 d PU . . H6WA H 0.2863 0.1428 0.0650 0.056 Uiso 0.25 1 d PR . . H6WB H 0.3376 0.0823 0.0997 0.056 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0273(2) 0.0203(2) 0.0240(2) 0.00122(19) 0.00202(15) -0.00153(19) Ni2 0.0305(5) 0.0242(6) 0.0269(5) -0.0022(4) -0.0002(4) 0.0002(4) Ni1 0.0341(6) 0.0217(5) 0.0295(6) -0.0045(4) 0.0035(4) -0.0033(4) N1 0.035(4) 0.021(4) 0.037(4) -0.001(3) 0.002(3) -0.007(3) N2 0.043(4) 0.044(5) 0.054(5) 0.010(4) -0.008(3) 0.002(4) N3 0.049(4) 0.030(4) 0.036(4) -0.017(3) 0.008(3) -0.007(3) N4 0.036(4) 0.027(4) 0.038(4) -0.002(3) -0.001(3) 0.004(3) O1 0.030(3) 0.022(3) 0.038(3) -0.009(2) 0.007(2) -0.004(2) O2 0.023(3) 0.036(3) 0.024(3) 0.004(2) 0.004(2) 0.000(2) O3 0.033(3) 0.057(4) 0.035(3) -0.005(3) 0.003(2) -0.015(3) O4 0.031(3) 0.034(3) 0.024(3) 0.002(2) 0.006(2) -0.002(2) O5 0.048(3) 0.042(4) 0.036(3) 0.013(3) 0.013(3) -0.013(3) O6 0.074(5) 0.140(7) 0.072(5) 0.054(5) 0.003(4) -0.046(5) O7 0.038(3) 0.037(3) 0.043(4) -0.010(3) 0.008(3) -0.005(3) O8 0.030(3) 0.027(3) 0.031(3) -0.005(2) 0.005(2) 0.002(2) O9 0.037(3) 0.032(3) 0.042(3) -0.018(3) 0.003(3) -0.005(3) O10 0.064(4) 0.058(4) 0.064(5) -0.040(4) 0.023(3) -0.025(3) O11 0.035(3) 0.020(3) 0.026(3) 0.004(2) 0.001(2) -0.003(2) C1 0.057(6) 0.034(5) 0.055(6) 0.012(4) 0.003(5) -0.020(4) C2 0.051(6) 0.034(5) 0.062(6) 0.009(5) 0.010(5) -0.009(4) C3 0.045(5) 0.036(5) 0.048(6) -0.016(4) 0.002(4) -0.004(4) C4 0.059(6) 0.034(5) 0.040(5) -0.018(4) 0.009(4) -0.004(4) C5 0.056(6) 0.035(5) 0.030(5) -0.011(4) 0.010(4) 0.001(4) C6 0.042(5) 0.050(6) 0.034(5) -0.011(4) 0.006(4) -0.002(4) C7 0.047(6) 0.097(8) 0.047(6) -0.023(6) 0.026(5) 0.007(6) C8 0.032(5) 0.111(9) 0.043(6) -0.022(6) 0.017(4) -0.017(5) C9 0.031(5) 0.077(7) 0.045(6) -0.012(5) 0.005(4) -0.007(5) C10 0.040(5) 0.040(5) 0.029(5) -0.003(4) 0.012(4) -0.002(4) C11 0.025(4) 0.034(5) 0.032(4) 0.004(4) 0.003(3) 0.004(4) C12 0.031(4) 0.027(4) 0.026(4) 0.006(3) 0.002(3) 0.002(4) C13 0.038(5) 0.034(5) 0.036(5) -0.012(4) 0.004(4) -0.007(4) C14 0.040(5) 0.044(6) 0.041(5) -0.009(4) -0.008(4) -0.006(4) C15 0.057(6) 0.038(5) 0.031(5) -0.001(4) -0.001(4) -0.001(4) C16 0.069(6) 0.047(6) 0.026(5) 0.002(4) 0.016(4) -0.002(5) C17 0.108(9) 0.071(8) 0.034(6) -0.005(5) 0.021(6) -0.023(7) C18 0.140(12) 0.092(10) 0.058(8) -0.015(7) 0.058(8) -0.032(8) C19 0.077(7) 0.064(7) 0.068(8) 0.006(6) 0.037(6) -0.010(6) C20 0.055(6) 0.026(5) 0.040(5) 0.010(4) 0.019(4) 0.006(4) C21 0.037(5) 0.034(5) 0.062(6) 0.025(5) 0.012(4) -0.002(4) C22 0.047(5) 0.035(5) 0.024(4) 0.015(4) 0.010(4) 0.009(4) C23 0.029(4) 0.048(6) 0.052(6) 0.004(5) 0.010(4) 0.004(4) C24 0.028(4) 0.034(5) 0.033(5) -0.001(4) 0.005(3) -0.007(4) C25 0.044(5) 0.060(6) 0.054(6) -0.017(5) 0.024(5) -0.004(5) C26 0.060(6) 0.059(6) 0.063(6) -0.020(5) 0.042(5) -0.003(5) C27 0.052(6) 0.041(5) 0.034(5) -0.006(4) 0.015(4) 0.001(4) C28 0.040(5) 0.026(4) 0.029(4) -0.001(4) 0.005(3) -0.005(4) C29 0.042(5) 0.033(5) 0.028(4) -0.008(4) 0.006(4) -0.012(4) C30 0.036(4) 0.025(4) 0.023(4) 0.004(3) 0.001(3) 0.008(3) O1W 0.040(3) 0.037(3) 0.043(3) 0.007(3) 0.001(3) 0.007(3) O2W 0.062(4) 0.096(6) 0.073(5) 0.025(4) 0.007(4) -0.018(4) O3W 0.104(6) 0.081(5) 0.047(4) -0.003(4) 0.004(4) 0.016(4) O4W 0.121(7) 0.090(6) 0.096(7) -0.028(5) 0.004(5) 0.010(5) O5W 0.054(5) 0.098(7) 0.055(6) 0.031(5) 0.017(4) 0.053(5) O6W 0.076(13) 0.026(11) 0.041(12) -0.021(9) 0.019(10) -0.052(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 Pr1 O5 2.356(5) . y Pr1 O9 2.369(5) . y Pr1 O4 2.395(5) . y Pr1 O2 2.432(4) . y Pr1 O8 2.449(4) . y Pr1 O11 2.477(5) . y Pr1 O1 2.479(5) . y Pr1 O2 2.489(5) 3_556 y Ni2 N4 2.015(6) . y Ni2 O4 2.022(5) . y Ni2 O8 2.040(5) . y Ni2 O11 2.042(5) . y Ni2 O7 2.055(5) . y Ni2 O1W 2.059(5) . y Ni1 N3 1.956(6) . y Ni1 O11 1.986(5) . y Ni1 N2 2.022(7) . y Ni1 O1 2.036(5) . y Ni1 N1 2.178(6) . y N1 C13 1.480(9) . ? N1 C2 1.490(10) . ? N1 C3 1.491(9) . ? N2 C1 1.466(9) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C5 1.261(9) . ? N3 C4 1.475(9) . ? N4 C15 1.288(10) . ? N4 C14 1.467(9) . ? O1 C12 1.309(8) . ? O2 C11 1.304(8) . ? O2 Pr1 2.489(5) 3_556 y O3 C11 1.251(8) . ? O4 C22 1.304(8) . ? O5 C21 1.254(9) . ? O6 C21 1.246(9) . ? O7 C23 1.227(9) . ? O8 C30 1.307(8) . ? O9 C29 1.270(9) . ? O10 C29 1.247(9) . ? O11 H11 0.8200 . ? C1 C2 1.474(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.496(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.444(11) . ? C5 H5 0.9300 . ? C6 C7 1.416(11) . ? C6 C12 1.440(10) . ? C7 C8 1.374(12) . ? C7 H7 0.9300 . ? C8 C9 1.366(12) . ? C8 H8 0.9300 . ? C9 C10 1.405(10) . ? C9 H9 0.9300 . ? C10 C12 1.421(10) . ? C10 C11 1.480(10) . ? C13 C14 1.515(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.443(11) . ? C15 H15 0.9300 . ? C16 C17 1.383(11) . ? C16 C22 1.411(11) . ? C17 C18 1.367(14) . ? C17 H17 0.9300 . ? C18 C19 1.362(14) . ? C18 H18 0.9300 . ? C19 C20 1.395(12) . ? C19 H19 0.9300 . ? C20 C22 1.400(11) . ? C20 C21 1.510(12) . ? C23 C24 1.427(11) . ? C23 H23 0.9300 . ? C24 C25 1.407(10) . ? C24 C30 1.422(9) . ? C25 C26 1.367(12) . ? C25 H25 0.9300 . ? C26 C27 1.404(11) . ? C26 H26 0.9300 . ? C27 C28 1.396(10) . ? C27 H27 0.9300 . ? C28 C30 1.436(10) . ? C28 C29 1.484(10) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8500 . ? 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 O5 Pr1 O9 86.84(19) . . y O5 Pr1 O4 69.96(17) . . y O9 Pr1 O4 115.93(18) . . y O5 Pr1 O2 79.32(17) . . y O9 Pr1 O2 94.27(17) . . y O4 Pr1 O2 134.54(15) . . y O5 Pr1 O8 111.73(18) . . y O9 Pr1 O8 68.72(16) . . y O4 Pr1 O8 66.92(16) . . y O2 Pr1 O8 158.33(16) . . y O5 Pr1 O11 134.07(18) . . y O9 Pr1 O11 127.79(16) . . y O4 Pr1 O11 67.80(16) . . y O2 Pr1 O11 120.10(16) . . y O8 Pr1 O11 66.38(15) . . y O5 Pr1 O1 87.13(18) . . y O9 Pr1 O1 162.03(16) . . y O4 Pr1 O1 77.59(16) . . y O2 Pr1 O1 67.96(16) . . y O8 Pr1 O1 129.16(15) . . y O11 Pr1 O1 67.07(15) . . y O5 Pr1 O2 146.79(17) . 3_556 y O9 Pr1 O2 84.95(18) . 3_556 y O4 Pr1 O2 141.62(15) . 3_556 y O2 Pr1 O2 69.31(17) . 3_556 y O8 Pr1 O2 95.02(15) . 3_556 y O11 Pr1 O2 73.98(15) . 3_556 y O1 Pr1 O2 90.91(16) . 3_556 y O5 Pr1 Pr1 113.77(14) . 3_556 y O9 Pr1 Pr1 89.46(13) . 3_556 y O4 Pr1 Pr1 154.60(12) . 3_556 y O2 Pr1 Pr1 35.12(11) . 3_556 y O8 Pr1 Pr1 127.75(11) . 3_556 y O11 Pr1 Pr1 97.56(11) . 3_556 y O1 Pr1 Pr1 77.55(12) . 3_556 y O2 Pr1 Pr1 34.20(10) 3_556 3_556 y N4 Ni2 O4 88.6(2) . . y N4 Ni2 O8 170.1(2) . . y O4 Ni2 O8 82.25(19) . . y N4 Ni2 O11 92.5(2) . . y O4 Ni2 O11 83.96(19) . . y O8 Ni2 O11 82.71(19) . . y N4 Ni2 O7 100.6(2) . . y O4 Ni2 O7 170.8(2) . . y O8 Ni2 O7 88.54(19) . . y O11 Ni2 O7 94.2(2) . . y N4 Ni2 O1W 89.7(2) . . y O4 Ni2 O1W 92.7(2) . . y O8 Ni2 O1W 94.6(2) . . y O11 Ni2 O1W 175.9(2) . . y O7 Ni2 O1W 88.8(2) . . y N3 Ni1 O11 161.8(2) . . y N3 Ni1 N2 102.9(3) . . y O11 Ni1 N2 95.3(3) . . y N3 Ni1 O1 90.6(2) . . y O11 Ni1 O1 85.79(19) . . y N2 Ni1 O1 102.9(2) . . y N3 Ni1 N1 82.6(3) . . y O11 Ni1 N1 98.6(2) . . y N2 Ni1 N1 85.2(2) . . y O1 Ni1 N1 170.4(2) . . y C13 N1 C2 109.1(6) . . ? C13 N1 C3 111.3(6) . . ? C2 N1 C3 109.8(6) . . ? C13 N1 Ni1 117.2(4) . . ? C2 N1 Ni1 102.2(5) . . ? C3 N1 Ni1 106.8(4) . . ? C1 N2 Ni1 107.2(5) . . ? C1 N2 H2A 110.3 . . ? Ni1 N2 H2A 110.3 . . ? C1 N2 H2B 110.3 . . ? Ni1 N2 H2B 110.3 . . ? H2A N2 H2B 108.5 . . ? C5 N3 C4 118.3(6) . . ? C5 N3 Ni1 126.4(5) . . ? C4 N3 Ni1 115.1(5) . . ? C15 N4 C14 117.6(7) . . ? C15 N4 Ni2 123.3(6) . . ? C14 N4 Ni2 118.5(5) . . ? C12 O1 Ni1 128.5(4) . . ? C12 O1 Pr1 128.4(4) . . ? Ni1 O1 Pr1 102.71(18) . . ? C11 O2 Pr1 122.2(4) . . ? C11 O2 Pr1 124.3(4) . 3_556 ? Pr1 O2 Pr1 110.69(17) . 3_556 ? C22 O4 Ni2 131.3(5) . . ? C22 O4 Pr1 129.1(4) . . ? Ni2 O4 Pr1 92.06(17) . . ? C21 O5 Pr1 137.2(5) . . ? C23 O7 Ni2 124.8(5) . . ? C30 O8 Ni2 129.9(4) . . ? C30 O8 Pr1 129.9(4) . . ? Ni2 O8 Pr1 90.09(17) . . ? C29 O9 Pr1 141.4(5) . . ? Ni1 O11 Ni2 117.6(2) . . ? Ni1 O11 Pr1 104.32(19) . . ? Ni2 O11 Pr1 89.27(18) . . ? Ni1 O11 H11 94.6 . . ? Ni2 O11 H11 136.9 . . ? Pr1 O11 H11 110.8 . . ? N2 C1 C2 109.0(7) . . ? N2 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N2 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C1 C2 N1 114.2(7) . . ? C1 C2 H2C 108.7 . . ? N1 C2 H2C 108.7 . . ? C1 C2 H2D 108.7 . . ? N1 C2 H2D 108.7 . . ? H2C C2 H2D 107.6 . . ? N1 C3 C4 110.2(6) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N3 C4 C3 111.4(6) . . ? N3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N3 C5 C6 128.5(7) . . ? N3 C5 H5 115.8 . . ? C6 C5 H5 115.8 . . ? C7 C6 C12 120.1(7) . . ? C7 C6 C5 116.0(8) . . ? C12 C6 C5 123.9(7) . . ? C8 C7 C6 121.2(8) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C9 C8 C7 119.1(8) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 122.8(8) . . ? C8 C9 H9 118.6 . . ? C10 C9 H9 118.6 . . ? C9 C10 C12 119.6(7) . . ? C9 C10 C11 114.9(7) . . ? C12 C10 C11 125.3(7) . . ? O3 C11 O2 119.8(7) . . ? O3 C11 C10 122.1(7) . . ? O2 C11 C10 118.1(7) . . ? O1 C12 C10 122.4(7) . . ? O1 C12 C6 120.6(6) . . ? C10 C12 C6 117.0(7) . . ? N1 C13 C14 116.5(6) . . ? N1 C13 H13A 108.2 . . ? C14 C13 H13A 108.2 . . ? N1 C13 H13B 108.2 . . ? C14 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? N4 C14 C13 111.0(6) . . ? N4 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? N4 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N4 C15 C16 128.5(8) . . ? N4 C15 H15 115.8 . . ? C16 C15 H15 115.8 . . ? C17 C16 C22 119.8(8) . . ? C17 C16 C15 115.4(8) . . ? C22 C16 C15 124.3(7) . . ? C18 C17 C16 121.8(10) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 118.9(9) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 121.7(10) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C22 119.7(8) . . ? C19 C20 C21 117.5(8) . . ? C22 C20 C21 122.8(7) . . ? O6 C21 O5 122.1(9) . . ? O6 C21 C20 116.7(8) . . ? O5 C21 C20 121.1(7) . . ? O4 C22 C20 122.0(7) . . ? O4 C22 C16 120.0(7) . . ? C20 C22 C16 118.0(7) . . ? O7 C23 C24 129.9(7) . . ? O7 C23 H23 115.0 . . ? C24 C23 H23 115.0 . . ? C25 C24 C30 120.0(7) . . ? C25 C24 C23 115.8(7) . . ? C30 C24 C23 124.2(7) . . ? C26 C25 C24 120.6(8) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 120.2(7) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 121.6(8) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C30 118.3(7) . . ? C27 C28 C29 117.9(7) . . ? C30 C28 C29 123.7(6) . . ? O10 C29 O9 123.5(7) . . ? O10 C29 C28 117.7(7) . . ? O9 C29 C28 118.7(7) . . ? O8 C30 C24 121.4(7) . . ? O8 C30 C28 119.6(6) . . ? C24 C30 C28 119.0(6) . . ? Ni2 O1W H1WA 132.6 . . ? Ni2 O1W H1WB 122.1 . . ? H1WA O1W H1WB 104.5 . . ? H2WA O2W H2WB 104.5 . . ? H3WA O3W H3WB 104.5 . . ? H4WA O4W H4WB 104.5 . . ? H5WA O5W H5WB 104.5 . . ? H6WA O6W H6WB 104.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ni1 N1 C13 141.8(5) . . . . ? O11 Ni1 N1 C13 -19.9(5) . . . . ? N2 Ni1 N1 C13 -114.6(5) . . . . ? N3 Ni1 N1 C2 -99.1(5) . . . . ? O11 Ni1 N1 C2 99.2(5) . . . . ? N2 Ni1 N1 C2 4.5(5) . . . . ? N3 Ni1 N1 C3 16.2(5) . . . . ? O11 Ni1 N1 C3 -145.5(5) . . . . ? N2 Ni1 N1 C3 119.9(5) . . . . ? N3 Ni1 N2 C1 103.1(6) . . . . ? O11 Ni1 N2 C1 -76.4(6) . . . . ? O1 Ni1 N2 C1 -163.3(5) . . . . ? N1 Ni1 N2 C1 21.8(5) . . . . ? O11 Ni1 N3 C5 -84.7(11) . . . . ? N2 Ni1 N3 C5 97.0(7) . . . . ? O1 Ni1 N3 C5 -6.5(7) . . . . ? N1 Ni1 N3 C5 -179.7(7) . . . . ? O11 Ni1 N3 C4 100.9(9) . . . . ? N2 Ni1 N3 C4 -77.4(6) . . . . ? O1 Ni1 N3 C4 179.2(6) . . . . ? N1 Ni1 N3 C4 5.9(6) . . . . ? O4 Ni2 N4 C15 20.3(6) . . . . ? O11 Ni2 N4 C15 104.2(6) . . . . ? O7 Ni2 N4 C15 -161.0(6) . . . . ? O1W Ni2 N4 C15 -72.3(6) . . . . ? O4 Ni2 N4 C14 -168.7(5) . . . . ? O11 Ni2 N4 C14 -84.8(5) . . . . ? O7 Ni2 N4 C14 10.0(6) . . . . ? O1W Ni2 N4 C14 98.7(5) . . . . ? N3 Ni1 O1 C12 13.8(6) . . . . ? O11 Ni1 O1 C12 176.0(6) . . . . ? N2 Ni1 O1 C12 -89.6(6) . . . . ? N3 Ni1 O1 Pr1 -159.4(2) . . . . ? O11 Ni1 O1 Pr1 2.8(2) . . . . ? N2 Ni1 O1 Pr1 97.2(3) . . . . ? O5 Pr1 O1 C12 -34.6(5) . . . . ? O9 Pr1 O1 C12 35.9(9) . . . . ? O4 Pr1 O1 C12 -104.7(5) . . . . ? O2 Pr1 O1 C12 45.0(5) . . . . ? O8 Pr1 O1 C12 -150.6(5) . . . . ? O11 Pr1 O1 C12 -175.6(6) . . . . ? O2 Pr1 O1 C12 112.2(5) 3_556 . . . ? Pr1 Pr1 O1 C12 80.5(5) 3_556 . . . ? O5 Pr1 O1 Ni1 138.6(2) . . . . ? O9 Pr1 O1 Ni1 -150.9(5) . . . . ? O4 Pr1 O1 Ni1 68.5(2) . . . . ? O2 Pr1 O1 Ni1 -141.7(2) . . . . ? O8 Pr1 O1 Ni1 22.7(3) . . . . ? O11 Pr1 O1 Ni1 -2.40(17) . . . . ? O2 Pr1 O1 Ni1 -74.5(2) 3_556 . . . ? Pr1 Pr1 O1 Ni1 -106.27(18) 3_556 . . . ? O5 Pr1 O2 C11 29.4(5) . . . . ? O9 Pr1 O2 C11 115.4(5) . . . . ? O4 Pr1 O2 C11 -18.1(6) . . . . ? O8 Pr1 O2 C11 152.5(5) . . . . ? O11 Pr1 O2 C11 -105.7(5) . . . . ? O1 Pr1 O2 C11 -61.8(5) . . . . ? O2 Pr1 O2 C11 -161.6(6) 3_556 . . . ? Pr1 Pr1 O2 C11 -161.6(6) 3_556 . . . ? O5 Pr1 O2 Pr1 -168.9(2) . . . 3_556 ? O9 Pr1 O2 Pr1 -83.0(2) . . . 3_556 ? O4 Pr1 O2 Pr1 143.52(19) . . . 3_556 ? O8 Pr1 O2 Pr1 -45.8(5) . . . 3_556 ? O11 Pr1 O2 Pr1 56.0(2) . . . 3_556 ? O1 Pr1 O2 Pr1 99.9(2) . . . 3_556 ? O2 Pr1 O2 Pr1 0.0 3_556 . . 3_556 ? N4 Ni2 O4 C22 -16.6(6) . . . . ? O8 Ni2 O4 C22 167.3(6) . . . . ? O11 Ni2 O4 C22 -109.3(6) . . . . ? O1W Ni2 O4 C22 73.0(6) . . . . ? N4 Ni2 O4 Pr1 134.0(2) . . . . ? O8 Ni2 O4 Pr1 -42.13(17) . . . . ? O11 Ni2 O4 Pr1 41.31(17) . . . . ? O1W Ni2 O4 Pr1 -136.43(19) . . . . ? O5 Pr1 O4 C22 -45.7(6) . . . . ? O9 Pr1 O4 C22 -121.6(6) . . . . ? O2 Pr1 O4 C22 4.9(7) . . . . ? O8 Pr1 O4 C22 -171.4(6) . . . . ? O11 Pr1 O4 C22 115.8(6) . . . . ? O1 Pr1 O4 C22 45.8(6) . . . . ? O2 Pr1 O4 C22 121.2(6) 3_556 . . . ? Pr1 Pr1 O4 C22 57.8(7) 3_556 . . . ? O5 Pr1 O4 Ni2 162.7(2) . . . . ? O9 Pr1 O4 Ni2 86.8(2) . . . . ? O2 Pr1 O4 Ni2 -146.76(18) . . . . ? O8 Pr1 O4 Ni2 36.99(16) . . . . ? O11 Pr1 O4 Ni2 -35.76(16) . . . . ? O1 Pr1 O4 Ni2 -105.82(19) . . . . ? O2 Pr1 O4 Ni2 -30.4(3) 3_556 . . . ? Pr1 Pr1 O4 Ni2 -93.9(3) 3_556 . . . ? O9 Pr1 O5 C21 148.9(8) . . . . ? O4 Pr1 O5 C21 29.8(7) . . . . ? O2 Pr1 O5 C21 -116.1(8) . . . . ? O8 Pr1 O5 C21 83.4(8) . . . . ? O11 Pr1 O5 C21 5.7(9) . . . . ? O1 Pr1 O5 C21 -48.0(8) . . . . ? O2 Pr1 O5 C21 -135.3(7) 3_556 . . . ? Pr1 Pr1 O5 C21 -123.0(7) 3_556 . . . ? N4 Ni2 O7 C23 172.4(6) . . . . ? O8 Ni2 O7 C23 -11.6(7) . . . . ? O11 Ni2 O7 C23 -94.2(7) . . . . ? O1W Ni2 O7 C23 83.0(7) . . . . ? O4 Ni2 O8 C30 -172.3(6) . . . . ? O11 Ni2 O8 C30 102.9(6) . . . . ? O7 Ni2 O8 C30 8.4(6) . . . . ? O1W Ni2 O8 C30 -80.2(6) . . . . ? O4 Ni2 O8 Pr1 40.96(17) . . . . ? O11 Ni2 O8 Pr1 -43.89(17) . . . . ? O7 Ni2 O8 Pr1 -138.35(19) . . . . ? O1W Ni2 O8 Pr1 133.02(18) . . . . ? O5 Pr1 O8 C30 121.4(6) . . . . ? O9 Pr1 O8 C30 44.1(6) . . . . ? O4 Pr1 O8 C30 176.6(6) . . . . ? O2 Pr1 O8 C30 3.9(8) . . . . ? O11 Pr1 O8 C30 -108.6(6) . . . . ? O1 Pr1 O8 C30 -133.8(5) . . . . ? O2 Pr1 O8 C30 -38.5(6) 3_556 . . . ? Pr1 Pr1 O8 C30 -27.6(6) 3_556 . . . ? O5 Pr1 O8 Ni2 -91.8(2) . . . . ? O9 Pr1 O8 Ni2 -169.1(2) . . . . ? O4 Pr1 O8 Ni2 -36.59(16) . . . . ? O2 Pr1 O8 Ni2 150.6(4) . . . . ? O11 Pr1 O8 Ni2 38.22(16) . . . . ? O1 Pr1 O8 Ni2 13.0(3) . . . . ? O2 Pr1 O8 Ni2 108.29(17) 3_556 . . . ? Pr1 Pr1 O8 Ni2 119.19(13) 3_556 . . . ? O5 Pr1 O9 C29 -129.9(8) . . . . ? O4 Pr1 O9 C29 -64.0(8) . . . . ? O2 Pr1 O9 C29 151.1(8) . . . . ? O8 Pr1 O9 C29 -15.1(8) . . . . ? O11 Pr1 O9 C29 17.1(9) . . . . ? O1 Pr1 O9 C29 159.6(7) . . . . ? O2 Pr1 O9 C29 82.3(8) 3_556 . . . ? Pr1 Pr1 O9 C29 116.3(8) 3_556 . . . ? N3 Ni1 O11 Ni2 -20.6(9) . . . . ? N2 Ni1 O11 Ni2 157.8(3) . . . . ? O1 Ni1 O11 Ni2 -99.6(3) . . . . ? N1 Ni1 O11 Ni2 71.8(3) . . . . ? N3 Ni1 O11 Pr1 76.2(8) . . . . ? N2 Ni1 O11 Pr1 -105.4(2) . . . . ? O1 Ni1 O11 Pr1 -2.8(2) . . . . ? N1 Ni1 O11 Pr1 168.7(2) . . . . ? N4 Ni2 O11 Ni1 -22.1(3) . . . . ? O4 Ni2 O11 Ni1 66.2(3) . . . . ? O8 Ni2 O11 Ni1 149.1(3) . . . . ? O7 Ni2 O11 Ni1 -122.9(3) . . . . ? N4 Ni2 O11 Pr1 -128.0(2) . . . . ? O4 Ni2 O11 Pr1 -39.64(17) . . . . ? O8 Ni2 O11 Pr1 43.28(16) . . . . ? O7 Ni2 O11 Pr1 131.26(18) . . . . ? O5 Pr1 O11 Ni1 -58.5(3) . . . . ? O9 Pr1 O11 Ni1 170.70(19) . . . . ? O4 Pr1 O11 Ni1 -83.0(2) . . . . ? O2 Pr1 O11 Ni1 46.7(3) . . . . ? O8 Pr1 O11 Ni1 -156.5(3) . . . . ? O1 Pr1 O11 Ni1 2.48(18) . . . . ? O2 Pr1 O11 Ni1 100.5(2) 3_556 . . . ? Pr1 Pr1 O11 Ni1 75.48(18) 3_556 . . . ? O5 Pr1 O11 Ni2 59.8(3) . . . . ? O9 Pr1 O11 Ni2 -71.0(2) . . . . ? O4 Pr1 O11 Ni2 35.35(16) . . . . ? O2 Pr1 O11 Ni2 165.06(15) . . . . ? O8 Pr1 O11 Ni2 -38.18(16) . . . . ? O1 Pr1 O11 Ni2 120.8(2) . . . . ? O2 Pr1 O11 Ni2 -141.18(19) 3_556 . . . ? Pr1 Pr1 O11 Ni2 -166.20(12) 3_556 . . . ? Ni1 N2 C1 C2 -45.0(8) . . . . ? N2 C1 C2 N1 53.6(10) . . . . ? C13 N1 C2 C1 93.1(8) . . . . ? C3 N1 C2 C1 -144.7(7) . . . . ? Ni1 N1 C2 C1 -31.6(8) . . . . ? C13 N1 C3 C4 -163.7(6) . . . . ? C2 N1 C3 C4 75.4(8) . . . . ? Ni1 N1 C3 C4 -34.6(7) . . . . ? C5 N3 C4 C3 157.6(8) . . . . ? Ni1 N3 C4 C3 -27.5(9) . . . . ? N1 C3 C4 N3 41.4(9) . . . . ? C4 N3 C5 C6 175.1(8) . . . . ? Ni1 N3 C5 C6 0.9(13) . . . . ? N3 C5 C6 C7 -176.5(9) . . . . ? N3 C5 C6 C12 2.0(14) . . . . ? C12 C6 C7 C8 0.2(14) . . . . ? C5 C6 C7 C8 178.7(9) . . . . ? C6 C7 C8 C9 -2.8(16) . . . . ? C7 C8 C9 C10 1.2(16) . . . . ? C8 C9 C10 C12 3.2(14) . . . . ? C8 C9 C10 C11 -171.9(9) . . . . ? Pr1 O2 C11 O3 -123.9(6) . . . . ? Pr1 O2 C11 O3 76.9(8) 3_556 . . . ? Pr1 O2 C11 C10 57.9(8) . . . . ? Pr1 O2 C11 C10 -101.2(7) 3_556 . . . ? C9 C10 C11 O3 -10.3(11) . . . . ? C12 C10 C11 O3 175.0(7) . . . . ? C9 C10 C11 O2 167.7(7) . . . . ? C12 C10 C11 O2 -7.0(12) . . . . ? Ni1 O1 C12 C10 165.1(5) . . . . ? Pr1 O1 C12 C10 -23.4(9) . . . . ? Ni1 O1 C12 C6 -14.7(10) . . . . ? Pr1 O1 C12 C6 156.8(6) . . . . ? C9 C10 C12 O1 174.7(7) . . . . ? C11 C10 C12 O1 -10.9(12) . . . . ? C9 C10 C12 C6 -5.6(11) . . . . ? C11 C10 C12 C6 168.9(7) . . . . ? C7 C6 C12 O1 -176.2(8) . . . . ? C5 C6 C12 O1 5.4(12) . . . . ? C7 C6 C12 C10 4.0(12) . . . . ? C5 C6 C12 C10 -174.4(8) . . . . ? C2 N1 C13 C14 174.2(7) . . . . ? C3 N1 C13 C14 52.8(8) . . . . ? Ni1 N1 C13 C14 -70.4(7) . . . . ? C15 N4 C14 C13 -119.7(8) . . . . ? Ni2 N4 C14 C13 68.8(8) . . . . ? N1 C13 C14 N4 52.2(9) . . . . ? C14 N4 C15 C16 173.5(8) . . . . ? Ni2 N4 C15 C16 -15.4(12) . . . . ? N4 C15 C16 C17 -175.2(9) . . . . ? N4 C15 C16 C22 -3.7(15) . . . . ? C22 C16 C17 C18 0.6(16) . . . . ? C15 C16 C17 C18 172.6(10) . . . . ? C16 C17 C18 C19 -1.0(19) . . . . ? C17 C18 C19 C20 -0.5(18) . . . . ? C18 C19 C20 C22 2.3(15) . . . . ? C18 C19 C20 C21 -177.4(10) . . . . ? Pr1 O5 C21 O6 168.1(7) . . . . ? Pr1 O5 C21 C20 -10.3(12) . . . . ? C19 C20 C21 O6 -13.8(12) . . . . ? C22 C20 C21 O6 166.4(8) . . . . ? C19 C20 C21 O5 164.7(8) . . . . ? C22 C20 C21 O5 -15.1(12) . . . . ? Ni2 O4 C22 C20 -175.6(5) . . . . ? Pr1 O4 C22 C20 43.6(10) . . . . ? Ni2 O4 C22 C16 4.9(11) . . . . ? Pr1 O4 C22 C16 -135.9(6) . . . . ? C19 C20 C22 O4 177.8(8) . . . . ? C21 C20 C22 O4 -2.4(12) . . . . ? C19 C20 C22 C16 -2.6(12) . . . . ? C21 C20 C22 C16 177.1(7) . . . . ? C17 C16 C22 O4 -179.3(8) . . . . ? C15 C16 C22 O4 9.5(13) . . . . ? C17 C16 C22 C20 1.2(13) . . . . ? C15 C16 C22 C20 -170.0(8) . . . . ? Ni2 O7 C23 C24 8.9(13) . . . . ? O7 C23 C24 C25 -178.9(9) . . . . ? O7 C23 C24 C30 2.4(14) . . . . ? C30 C24 C25 C26 0.6(13) . . . . ? C23 C24 C25 C26 -178.1(9) . . . . ? C24 C25 C26 C27 1.4(15) . . . . ? C25 C26 C27 C28 0.6(14) . . . . ? C26 C27 C28 C30 -4.5(12) . . . . ? C26 C27 C28 C29 177.9(8) . . . . ? Pr1 O9 C29 O10 171.5(6) . . . . ? Pr1 O9 C29 C28 -9.4(12) . . . . ? C27 C28 C29 O10 20.0(11) . . . . ? C30 C28 C29 O10 -157.4(8) . . . . ? C27 C28 C29 O9 -159.1(7) . . . . ? C30 C28 C29 O9 23.5(11) . . . . ? Ni2 O8 C30 C24 -1.5(10) . . . . ? Pr1 O8 C30 C24 132.9(6) . . . . ? Ni2 O8 C30 C28 177.9(5) . . . . ? Pr1 O8 C30 C28 -47.6(9) . . . . ? C25 C24 C30 O8 174.9(7) . . . . ? C23 C24 C30 O8 -6.5(12) . . . . ? C25 C24 C30 C28 -4.5(11) . . . . ? C23 C24 C30 C28 174.1(7) . . . . ? C27 C28 C30 O8 -173.0(7) . . . . ? C29 C28 C30 O8 4.4(11) . . . . ? C27 C28 C30 C24 6.4(11) . . . . ? C29 C28 C30 C24 -176.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.785 _refine_diff_density_min -1.499 _refine_diff_density_rms 0.139 data_1314 _database_code_depnum_ccdc_archive 'CCDC 898019' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C60 H58 N8 Ni4 O24 Sm2), 17(H2 O)' _chemical_formula_sum 'C120 H150 N16 Ni8 O65 Sm4' _chemical_formula_weight 3927.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7048(6) _cell_length_b 18.1777(9) _cell_length_c 15.5866(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.9870(10) _cell_angle_gamma 90.00 _cell_volume 3545.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3962 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.91 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1974 _exptl_absorpt_coefficient_mu 2.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5813 _exptl_absorpt_correction_T_max 0.7507 _exptl_absorpt_process_details 'SADABS(Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18163 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6250 _reflns_number_gt 4817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2005)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2005)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^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 6250 _refine_ls_number_parameters 487 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.915669(15) 1.058414(10) 0.403651(12) 0.02470(5) Uani 1 1 d . . . Ni1 Ni 0.83695(4) 0.89620(3) 0.28935(3) 0.02941(13) Uani 1 1 d . . . Ni2 Ni 0.68422(4) 1.05203(3) 0.28988(3) 0.02781(12) Uani 1 1 d . . . N1 N 0.6931(3) 0.83768(17) 0.2327(2) 0.0372(9) Uani 1 1 d . . . N2 N 0.8946(3) 0.84923(18) 0.1947(2) 0.0395(9) Uani 1 1 d . . . N3 N 0.6583(3) 0.99284(17) 0.1784(2) 0.0345(9) Uani 1 1 d . . . N4 N 0.8517(3) 0.81738(18) 0.3820(2) 0.0460(10) Uani 1 1 d . . . H4A H 0.8964 0.7818 0.3702 0.055 Uiso 1 1 calc R . . H4B H 0.8779 0.8367 0.4345 0.055 Uiso 1 1 calc R . . O1 O 0.97338(19) 0.95644(13) 0.32197(16) 0.0303(7) Uani 1 1 d . . . O2 O 1.09040(18) 1.01739(14) 0.46812(16) 0.0283(6) Uani 1 1 d . . . O3 O 1.2543(2) 1.05348(15) 0.45751(18) 0.0411(8) Uani 1 1 d . . . O4 O 0.8260(2) 1.08272(14) 0.26103(16) 0.0317(7) Uani 1 1 d . . . O5 O 1.0224(2) 1.13354(15) 0.33318(18) 0.0421(8) Uani 1 1 d . . . O6 O 1.1107(3) 1.1846(2) 0.2405(2) 0.1008(14) Uani 1 1 d . . . O7 O 0.5488(2) 1.02990(15) 0.34049(18) 0.0393(7) Uani 1 1 d . . . O8 O 0.73965(19) 1.10978(13) 0.40004(16) 0.0293(6) Uani 1 1 d . . . O9 O 0.9224(2) 1.15658(14) 0.50219(18) 0.0383(7) Uani 1 1 d . . . O10 O 0.8951(2) 1.24859(17) 0.5882(2) 0.0584(9) Uani 1 1 d . . . O11 O 0.77225(19) 0.97009(13) 0.35797(15) 0.0270(6) Uani 1 1 d . . . H11 H 0.7406 0.9495 0.4058 0.032 Uiso 1 1 calc R . . C1 C 0.7097(3) 0.8150(2) 0.1432(3) 0.0470(13) Uani 1 1 d . . . H1A H 0.6639 0.7735 0.1234 0.056 Uiso 1 1 calc R . . H1B H 0.6903 0.8553 0.1028 0.056 Uiso 1 1 calc R . . C2 C 0.8231(3) 0.7944(2) 0.1442(3) 0.0481(13) Uani 1 1 d . . . H2A H 0.8369 0.7461 0.1703 0.058 Uiso 1 1 calc R . . H2B H 0.8370 0.7922 0.0850 0.058 Uiso 1 1 calc R . . C3 C 0.9904(4) 0.8550(2) 0.1796(3) 0.0435(12) Uani 1 1 d . . . H3 H 1.0066 0.8276 0.1332 0.052 Uiso 1 1 calc R . . C4 C 1.0761(3) 0.8993(2) 0.2268(3) 0.0399(11) Uani 1 1 d . . . C5 C 1.1744(4) 0.8932(3) 0.1983(3) 0.0598(15) Uani 1 1 d . . . H5 H 1.1792 0.8624 0.1515 0.072 Uiso 1 1 calc R . . C6 C 1.2632(4) 0.9307(3) 0.2363(3) 0.0693(17) Uani 1 1 d . . . H6 H 1.3269 0.9273 0.2147 0.083 Uiso 1 1 calc R . . C7 C 1.2558(3) 0.9738(3) 0.3078(3) 0.0502(13) Uani 1 1 d . . . H7 H 1.3161 0.9993 0.3346 0.060 Uiso 1 1 calc R . . C8 C 1.1619(3) 0.9808(2) 0.3414(2) 0.0315(10) Uani 1 1 d . . . C9 C 1.1704(3) 1.0213(2) 0.4265(2) 0.0298(10) Uani 1 1 d . . . C10 C 1.0670(3) 0.9454(2) 0.2981(2) 0.0316(10) Uani 1 1 d . . . C11 C 0.5898(3) 0.8765(2) 0.2284(3) 0.0405(11) Uani 1 1 d . . . H11A H 0.5853 0.8945 0.2863 0.049 Uiso 1 1 calc R . . H11B H 0.5327 0.8410 0.2126 0.049 Uiso 1 1 calc R . . C12 C 0.5697(3) 0.9406(2) 0.1655(3) 0.0428(12) Uani 1 1 d . . . H12A H 0.5594 0.9221 0.1062 0.051 Uiso 1 1 calc R . . H12B H 0.5047 0.9657 0.1735 0.051 Uiso 1 1 calc R . . C13 C 0.7059(4) 1.0043(2) 0.1147(3) 0.0463(13) Uani 1 1 d . . . H13 H 0.6751 0.9827 0.0623 0.056 Uiso 1 1 calc R . . C14 C 0.8022(4) 1.0466(2) 0.1129(3) 0.0467(13) Uani 1 1 d . . . C15 C 0.8412(5) 1.0468(3) 0.0351(3) 0.0758(18) Uani 1 1 d . . . H15 H 0.8010 1.0251 -0.0139 0.091 Uiso 1 1 calc R . . C16 C 0.9382(5) 1.0784(3) 0.0288(4) 0.0830(19) Uani 1 1 d . . . H16 H 0.9629 1.0786 -0.0240 0.100 Uiso 1 1 calc R . . C17 C 0.9981(4) 1.1099(3) 0.1018(3) 0.0657(16) Uani 1 1 d . . . H17 H 1.0639 1.1307 0.0975 0.079 Uiso 1 1 calc R . . C18 C 0.9637(3) 1.1116(2) 0.1809(3) 0.0415(11) Uani 1 1 d . . . C19 C 1.0369(3) 1.1462(2) 0.2563(3) 0.0470(13) Uani 1 1 d . . . C20 C 0.8627(3) 1.0807(2) 0.1884(3) 0.0358(11) Uani 1 1 d . . . C21 C 0.8624(3) 1.1947(2) 0.5416(3) 0.0356(11) Uani 1 1 d . . . C22 C 0.7458(3) 1.1746(2) 0.5336(2) 0.0310(10) Uani 1 1 d . . . C23 C 0.6887(4) 1.2010(2) 0.5941(3) 0.0466(12) Uani 1 1 d . . . H23 H 0.7237 1.2311 0.6382 0.056 Uiso 1 1 calc R . . C24 C 0.5806(4) 1.1852(3) 0.5931(3) 0.0584(14) Uani 1 1 d . . . H24 H 0.5438 1.2054 0.6341 0.070 Uiso 1 1 calc R . . C25 C 0.5313(3) 1.1387(3) 0.5292(3) 0.0487(13) Uani 1 1 d . . . H25 H 0.4608 1.1251 0.5291 0.058 Uiso 1 1 calc R . . C26 C 0.5834(3) 1.1112(2) 0.4644(3) 0.0337(10) Uani 1 1 d . . . C27 C 0.5235(3) 1.0604(2) 0.4042(3) 0.0414(11) Uani 1 1 d . . . H27 H 0.4557 1.0489 0.4151 0.050 Uiso 1 1 calc R . . C28 C 0.6920(3) 1.13024(19) 0.4636(2) 0.0276(9) Uani 1 1 d . . . C29 C 0.6941(3) 0.7716(2) 0.2890(3) 0.0458(13) Uani 1 1 d . . . H29A H 0.7333 0.7325 0.2663 0.055 Uiso 1 1 calc R . . H29B H 0.6214 0.7548 0.2875 0.055 Uiso 1 1 calc R . . C30 C 0.7444(3) 0.7871(3) 0.3813(3) 0.0499(13) Uani 1 1 d . . . H30A H 0.7013 0.8221 0.4069 0.060 Uiso 1 1 calc R . . H30B H 0.7492 0.7422 0.4153 0.060 Uiso 1 1 calc R . . O1W O 0.6048(2) 1.13918(14) 0.22258(18) 0.0406(8) Uani 1 1 d . . . H1WA H 0.5663 1.1717 0.2413 0.049 Uiso 1 1 d R . . H1WB H 0.6200 1.1546 0.1747 0.049 Uiso 1 1 d R . . O2W O 0.2827(3) 0.1905(2) 0.3667(2) 0.0790(12) Uani 1 1 d . . . H2WA H 0.2396 0.1566 0.3460 0.095 Uiso 1 1 d R . . H2WB H 0.3025 0.2125 0.3241 0.095 Uiso 1 1 d R . . O3W O 0.5353(3) 0.1446(2) 0.0458(2) 0.0857(13) Uani 1 1 d . . . H3WA H 0.4744 0.1259 0.0510 0.103 Uiso 1 1 d R . . H3WB H 0.5264 0.1905 0.0369 0.103 Uiso 1 1 d R . . O4W O 0.0763(3) 0.6943(2) 0.2433(3) 0.1170(16) Uani 1 1 d U . . H4WA H 0.0210 0.6679 0.2280 0.140 Uiso 1 1 d R . . H4WB H 0.0599 0.7288 0.2753 0.140 Uiso 1 1 d R . . O5W O 0.1107(4) 0.2729(2) 0.4213(3) 0.1081(17) Uani 1 1 d . . . H5WA H 0.0754 0.3050 0.4440 0.130 Uiso 1 1 d R . . H5WB H 0.0676 0.2392 0.4003 0.130 Uiso 1 1 d R . . O6W O 0.7867(12) 0.3976(8) 0.5882(9) 0.079(5) Uani 0.25 1 d P . . H6WA H 0.7998 0.4413 0.5738 0.095 Uiso 0.25 1 d PR . . H6WB H 0.7807 0.3710 0.5427 0.095 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02191(10) 0.02524(10) 0.02521(10) 0.00093(8) -0.00079(8) -0.00141(8) Ni1 0.0287(3) 0.0259(3) 0.0324(3) -0.0043(2) 0.0017(2) -0.0035(2) Ni2 0.0247(2) 0.0288(3) 0.0272(3) -0.0025(2) -0.0033(2) 0.0007(2) N1 0.0335(18) 0.0288(18) 0.046(2) -0.0055(16) -0.0014(17) -0.0061(15) N2 0.038(2) 0.0363(19) 0.043(2) -0.0167(16) 0.0057(17) -0.0076(16) N3 0.0367(19) 0.0337(18) 0.0297(18) 0.0007(15) -0.0032(16) 0.0023(15) N4 0.043(2) 0.035(2) 0.056(2) 0.0047(18) -0.0049(19) -0.0016(17) O1 0.0227(13) 0.0330(15) 0.0339(15) -0.0054(12) 0.0013(12) -0.0005(11) O2 0.0176(12) 0.0372(15) 0.0285(14) 0.0030(12) -0.0006(11) -0.0005(11) O3 0.0258(14) 0.0554(18) 0.0406(16) -0.0042(14) 0.0021(13) -0.0119(13) O4 0.0275(14) 0.0395(15) 0.0276(14) 0.0044(12) 0.0027(12) 0.0025(12) O5 0.0365(16) 0.0448(17) 0.0451(17) 0.0116(14) 0.0075(14) -0.0106(13) O6 0.070(2) 0.149(3) 0.077(3) 0.061(2) -0.003(2) -0.058(2) O7 0.0284(15) 0.0443(16) 0.0434(17) -0.0099(14) 0.0014(14) -0.0074(13) O8 0.0234(13) 0.0353(15) 0.0289(14) -0.0068(12) 0.0031(12) 0.0009(11) O9 0.0260(14) 0.0371(15) 0.0482(17) -0.0127(14) -0.0032(13) 0.0001(12) O10 0.0494(19) 0.060(2) 0.066(2) -0.0357(17) 0.0113(17) -0.0219(16) O11 0.0254(13) 0.0271(13) 0.0265(13) 0.0007(11) -0.0006(12) -0.0025(11) C1 0.041(3) 0.044(3) 0.051(3) -0.019(2) -0.004(2) -0.009(2) C2 0.049(3) 0.041(3) 0.052(3) -0.020(2) 0.002(2) -0.010(2) C3 0.056(3) 0.039(2) 0.036(2) -0.014(2) 0.011(2) -0.003(2) C4 0.039(2) 0.045(3) 0.036(2) -0.008(2) 0.008(2) -0.002(2) C5 0.052(3) 0.085(4) 0.045(3) -0.024(3) 0.018(2) -0.008(3) C6 0.035(3) 0.116(4) 0.062(3) -0.034(3) 0.023(2) -0.012(3) C7 0.026(2) 0.076(3) 0.050(3) -0.015(2) 0.012(2) -0.010(2) C8 0.026(2) 0.039(2) 0.029(2) -0.0005(18) 0.0027(18) -0.0024(17) C9 0.026(2) 0.034(2) 0.028(2) 0.0030(17) 0.0014(18) 0.0020(17) C10 0.027(2) 0.039(2) 0.029(2) 0.0068(18) 0.0062(17) -0.0003(18) C11 0.033(2) 0.039(2) 0.048(3) -0.010(2) 0.000(2) -0.0073(19) C12 0.038(2) 0.044(3) 0.040(2) -0.008(2) -0.011(2) -0.005(2) C13 0.065(3) 0.039(3) 0.031(2) -0.005(2) -0.002(2) 0.000(2) C14 0.070(3) 0.039(3) 0.032(2) 0.002(2) 0.012(2) -0.005(2) C15 0.112(5) 0.079(4) 0.041(3) -0.011(3) 0.027(3) -0.022(3) C16 0.114(5) 0.093(4) 0.056(3) -0.009(3) 0.054(3) -0.023(4) C17 0.072(3) 0.067(3) 0.065(3) 0.010(3) 0.030(3) -0.010(3) C18 0.048(3) 0.037(2) 0.042(2) 0.017(2) 0.014(2) 0.008(2) C19 0.034(2) 0.050(3) 0.057(3) 0.027(2) 0.006(2) 0.004(2) C20 0.044(2) 0.030(2) 0.034(2) 0.0073(18) 0.008(2) 0.0098(18) C21 0.042(2) 0.031(2) 0.030(2) -0.0010(18) -0.003(2) -0.0074(19) C22 0.033(2) 0.026(2) 0.033(2) 0.0005(17) 0.0023(18) -0.0002(17) C23 0.055(3) 0.047(3) 0.039(2) -0.013(2) 0.011(2) -0.005(2) C24 0.049(3) 0.071(3) 0.061(3) -0.031(3) 0.025(2) -0.007(2) C25 0.033(2) 0.063(3) 0.053(3) -0.016(2) 0.013(2) -0.002(2) C26 0.026(2) 0.039(2) 0.035(2) -0.0029(19) 0.0004(18) -0.0003(17) C27 0.025(2) 0.051(3) 0.047(3) -0.008(2) 0.003(2) -0.004(2) C28 0.025(2) 0.0239(19) 0.032(2) 0.0011(17) 0.0010(18) 0.0049(16) C29 0.038(2) 0.029(2) 0.064(3) 0.002(2) -0.009(2) -0.0059(19) C30 0.044(3) 0.047(3) 0.056(3) 0.012(2) 0.002(2) -0.010(2) O1W 0.0401(16) 0.0393(16) 0.0408(16) 0.0029(13) 0.0031(14) 0.0104(13) O2W 0.062(2) 0.092(3) 0.082(3) 0.023(2) 0.009(2) -0.022(2) O3W 0.095(3) 0.087(3) 0.067(2) -0.003(2) -0.008(2) 0.024(2) O4W 0.095(3) 0.151(4) 0.116(3) -0.082(3) 0.050(3) -0.075(3) O5W 0.128(4) 0.092(3) 0.096(3) -0.021(3) -0.005(3) 0.008(3) O6W 0.110(11) 0.071(9) 0.063(8) 0.044(7) 0.030(8) 0.054(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 Sm1 O5 2.329(3) . ? Sm1 O9 2.346(3) . ? Sm1 O4 2.357(2) . ? Sm1 O2 2.392(2) . ? Sm1 O8 2.415(2) . ? Sm1 O1 2.433(2) . ? Sm1 O2 2.440(2) 3_776 ? Sm1 O11 2.440(2) . ? Sm1 Sm1 3.9862(4) 3_776 ? Ni1 N2 1.954(3) . ? Ni1 O11 1.982(3) . ? Ni1 N4 2.019(3) . ? Ni1 O1 2.039(2) . ? Ni1 N1 2.166(3) . ? Ni2 O4 2.010(3) . ? Ni2 N3 2.021(3) . ? Ni2 O8 2.031(2) . ? Ni2 O11 2.046(2) . ? Ni2 O7 2.053(3) . ? Ni2 O1W 2.064(3) . ? N1 C11 1.482(5) . ? N1 C29 1.487(5) . ? N1 C1 1.504(5) . ? N2 C3 1.283(6) . ? N2 C2 1.480(5) . ? N3 C13 1.266(6) . ? N3 C12 1.460(5) . ? N4 C30 1.469(5) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? O1 C10 1.322(5) . ? O2 C9 1.299(4) . ? O2 Sm1 2.440(2) 3_776 ? O3 C9 1.238(4) . ? O4 C20 1.298(5) . ? O5 C19 1.264(5) . ? O6 C19 1.227(5) . ? O7 C27 1.228(5) . ? O8 C28 1.301(4) . ? O9 C21 1.266(5) . ? O10 C21 1.248(5) . ? O11 H11 0.9800 . ? C1 C2 1.486(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.449(6) . ? C3 H3 0.9300 . ? C4 C5 1.401(6) . ? C4 C10 1.412(6) . ? C5 C6 1.362(7) . ? C5 H5 0.9300 . ? C6 C7 1.379(7) . ? C6 H6 0.9300 . ? C7 C8 1.390(6) . ? C7 H7 0.9300 . ? C8 C10 1.429(5) . ? C8 C9 1.504(5) . ? C11 C12 1.515(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.450(7) . ? C13 H13 0.9300 . ? C14 C15 1.388(7) . ? C14 C20 1.430(6) . ? C15 C16 1.379(8) . ? C15 H15 0.9300 . ? C16 C17 1.380(7) . ? C16 H16 0.9300 . ? C17 C18 1.378(7) . ? C17 H17 0.9300 . ? C18 C20 1.424(6) . ? C18 C19 1.504(6) . ? C21 C22 1.509(6) . ? C22 C23 1.372(6) . ? C22 C28 1.432(5) . ? C23 C24 1.400(6) . ? C23 H23 0.9300 . ? C24 C25 1.373(6) . ? C24 H24 0.9300 . ? C25 C26 1.393(6) . ? C25 H25 0.9300 . ? C26 C28 1.425(5) . ? C26 C27 1.436(5) . ? C27 H27 0.9300 . ? C29 C30 1.497(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? O1W H1WA 0.8502 . ? O1W H1WB 0.8501 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8614 . ? O3W H3WB 0.8506 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8499 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8502 . ? 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 O5 Sm1 O9 84.53(10) . . ? O5 Sm1 O4 70.78(9) . . ? O9 Sm1 O4 115.57(9) . . ? O5 Sm1 O2 78.89(9) . . ? O9 Sm1 O2 92.08(8) . . ? O4 Sm1 O2 135.73(9) . . ? O5 Sm1 O8 112.00(9) . . ? O9 Sm1 O8 69.49(8) . . ? O4 Sm1 O8 67.15(9) . . ? O2 Sm1 O8 156.72(8) . . ? O5 Sm1 O1 86.97(9) . . ? O9 Sm1 O1 160.39(8) . . ? O4 Sm1 O1 77.84(8) . . ? O2 Sm1 O1 68.92(8) . . ? O8 Sm1 O1 130.11(8) . . ? O5 Sm1 O2 145.19(8) . 3_776 ? O9 Sm1 O2 84.03(9) . 3_776 ? O4 Sm1 O2 143.10(8) . 3_776 ? O2 Sm1 O2 68.82(10) . 3_776 ? O8 Sm1 O2 94.40(8) . 3_776 ? O1 Sm1 O2 93.08(8) . 3_776 ? O5 Sm1 O11 135.59(9) . . ? O9 Sm1 O11 129.20(9) . . ? O4 Sm1 O11 68.53(8) . . ? O2 Sm1 O11 120.60(8) . . ? O8 Sm1 O11 66.80(8) . . ? O1 Sm1 O11 67.88(8) . . ? O2 Sm1 O11 74.89(8) 3_776 . ? O5 Sm1 Sm1 112.76(7) . 3_776 ? O9 Sm1 Sm1 87.60(6) . 3_776 ? O4 Sm1 Sm1 156.80(6) . 3_776 ? O2 Sm1 Sm1 34.80(6) . 3_776 ? O8 Sm1 Sm1 126.73(6) . 3_776 ? O1 Sm1 Sm1 79.46(6) . 3_776 ? O2 Sm1 Sm1 34.02(5) 3_776 3_776 ? O11 Sm1 Sm1 98.39(5) . 3_776 ? N2 Ni1 O11 161.53(12) . . ? N2 Ni1 N4 103.26(15) . . ? O11 Ni1 N4 95.21(13) . . ? N2 Ni1 O1 90.52(12) . . ? O11 Ni1 O1 85.16(10) . . ? N4 Ni1 O1 103.48(12) . . ? N2 Ni1 N1 82.98(14) . . ? O11 Ni1 N1 98.82(12) . . ? N4 Ni1 N1 84.86(13) . . ? O1 Ni1 N1 170.47(12) . . ? O4 Ni2 N3 88.53(12) . . ? O4 Ni2 O8 81.54(10) . . ? N3 Ni2 O8 169.25(12) . . ? O4 Ni2 O11 83.54(10) . . ? N3 Ni2 O11 92.93(11) . . ? O8 Ni2 O11 81.92(10) . . ? O4 Ni2 O7 169.64(11) . . ? N3 Ni2 O7 101.74(13) . . ? O8 Ni2 O7 88.12(10) . . ? O11 Ni2 O7 94.42(11) . . ? O4 Ni2 O1W 92.95(11) . . ? N3 Ni2 O1W 88.82(12) . . ? O8 Ni2 O1W 95.75(10) . . ? O11 Ni2 O1W 176.03(10) . . ? O7 Ni2 O1W 88.71(11) . . ? C11 N1 C29 109.2(3) . . ? C11 N1 C1 110.8(3) . . ? C29 N1 C1 109.8(3) . . ? C11 N1 Ni1 117.6(2) . . ? C29 N1 Ni1 103.6(2) . . ? C1 N1 Ni1 105.6(2) . . ? C3 N2 C2 118.1(4) . . ? C3 N2 Ni1 126.5(3) . . ? C2 N2 Ni1 114.8(3) . . ? C13 N3 C12 117.4(4) . . ? C13 N3 Ni2 123.9(3) . . ? C12 N3 Ni2 118.1(3) . . ? C30 N4 Ni1 106.9(3) . . ? C30 N4 H4A 110.4 . . ? Ni1 N4 H4A 110.4 . . ? C30 N4 H4B 110.4 . . ? Ni1 N4 H4B 110.4 . . ? H4A N4 H4B 108.6 . . ? C10 O1 Ni1 128.0(2) . . ? C10 O1 Sm1 129.1(2) . . ? Ni1 O1 Sm1 102.67(10) . . ? C9 O2 Sm1 121.5(2) . . ? C9 O2 Sm1 125.4(2) . 3_776 ? Sm1 O2 Sm1 111.18(10) . 3_776 ? C20 O4 Ni2 131.2(2) . . ? C20 O4 Sm1 129.0(2) . . ? Ni2 O4 Sm1 92.42(10) . . ? C19 O5 Sm1 138.2(3) . . ? C27 O7 Ni2 125.2(3) . . ? C28 O8 Ni2 130.7(2) . . ? C28 O8 Sm1 130.1(2) . . ? Ni2 O8 Sm1 90.22(9) . . ? C21 O9 Sm1 141.0(2) . . ? Ni1 O11 Ni2 117.00(12) . . ? Ni1 O11 Sm1 104.17(10) . . ? Ni2 O11 Sm1 89.18(9) . . ? Ni1 O11 H11 114.4 . . ? Ni2 O11 H11 114.4 . . ? Sm1 O11 H11 114.4 . . ? C2 C1 N1 110.5(3) . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 109.9(3) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 127.2(4) . . ? N2 C3 H3 116.4 . . ? C4 C3 H3 116.4 . . ? C5 C4 C10 119.7(4) . . ? C5 C4 C3 115.3(4) . . ? C10 C4 C3 125.0(4) . . ? C6 C5 C4 122.6(4) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C7 117.9(4) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C6 C7 C8 122.7(4) . . ? C6 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C7 C8 C10 119.3(4) . . ? C7 C8 C9 116.3(3) . . ? C10 C8 C9 124.3(3) . . ? O3 C9 O2 121.7(3) . . ? O3 C9 C8 120.0(4) . . ? O2 C9 C8 118.1(3) . . ? O1 C10 C4 120.8(3) . . ? O1 C10 C8 121.6(3) . . ? C4 C10 C8 117.5(4) . . ? N1 C11 C12 116.3(4) . . ? N1 C11 H11A 108.2 . . ? C12 C11 H11A 108.2 . . ? N1 C11 H11B 108.2 . . ? C12 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? N3 C12 C11 111.8(3) . . ? N3 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N3 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? N3 C13 C14 128.4(4) . . ? N3 C13 H13 115.8 . . ? C14 C13 H13 115.8 . . ? C15 C14 C20 119.7(5) . . ? C15 C14 C13 116.6(4) . . ? C20 C14 C13 123.4(4) . . ? C16 C15 C14 121.5(5) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 119.1(5) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 122.2(5) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C20 119.6(4) . . ? C17 C18 C19 117.4(4) . . ? C20 C18 C19 123.0(4) . . ? O6 C19 O5 122.4(4) . . ? O6 C19 C18 118.1(4) . . ? O5 C19 C18 119.5(4) . . ? O4 C20 C18 121.7(4) . . ? O4 C20 C14 120.4(4) . . ? C18 C20 C14 117.9(4) . . ? O10 C21 O9 123.0(4) . . ? O10 C21 C22 117.5(4) . . ? O9 C21 C22 119.5(3) . . ? C23 C22 C28 118.7(4) . . ? C23 C22 C21 119.2(4) . . ? C28 C22 C21 122.1(4) . . ? C22 C23 C24 123.8(4) . . ? C22 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C25 C24 C23 117.2(4) . . ? C25 C24 H24 121.4 . . ? C23 C24 H24 121.4 . . ? C24 C25 C26 122.2(4) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C28 120.1(4) . . ? C25 C26 C27 116.1(4) . . ? C28 C26 C27 123.7(4) . . ? O7 C27 C26 129.4(4) . . ? O7 C27 H27 115.3 . . ? C26 C27 H27 115.3 . . ? O8 C28 C26 121.0(3) . . ? O8 C28 C22 121.2(3) . . ? C26 C28 C22 117.7(4) . . ? N1 C29 C30 112.0(3) . . ? N1 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? N1 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? N4 C30 C29 108.5(4) . . ? N4 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? N4 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? Ni2 O1W H1WA 128.2 . . ? Ni2 O1W H1WB 122.2 . . ? H1WA O1W H1WB 107.7 . . ? H2WA O2W H2WB 107.7 . . ? H3WA O3W H3WB 107.8 . . ? H4WA O4W H4WB 107.7 . . ? H5WA O5W H5WB 107.7 . . ? H6WA O6W H6WB 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C11 -140.2(3) . . . . ? O11 Ni1 N1 C11 21.2(3) . . . . ? N4 Ni1 N1 C11 115.7(3) . . . . ? N2 Ni1 N1 C29 99.3(3) . . . . ? O11 Ni1 N1 C29 -99.3(3) . . . . ? N4 Ni1 N1 C29 -4.8(3) . . . . ? N2 Ni1 N1 C1 -16.1(3) . . . . ? O11 Ni1 N1 C1 145.3(2) . . . . ? N4 Ni1 N1 C1 -120.2(3) . . . . ? O11 Ni1 N2 C3 84.4(5) . . . . ? N4 Ni1 N2 C3 -95.8(4) . . . . ? O1 Ni1 N2 C3 8.2(4) . . . . ? N1 Ni1 N2 C3 -178.8(4) . . . . ? O11 Ni1 N2 C2 -104.4(4) . . . . ? N4 Ni1 N2 C2 75.5(3) . . . . ? O1 Ni1 N2 C2 179.4(3) . . . . ? N1 Ni1 N2 C2 -7.5(3) . . . . ? O4 Ni2 N3 C13 -20.9(3) . . . . ? O8 Ni2 N3 C13 -43.3(8) . . . . ? O11 Ni2 N3 C13 -104.3(3) . . . . ? O7 Ni2 N3 C13 160.5(3) . . . . ? O1W Ni2 N3 C13 72.1(3) . . . . ? O4 Ni2 N3 C12 167.8(3) . . . . ? O8 Ni2 N3 C12 145.4(6) . . . . ? O11 Ni2 N3 C12 84.3(3) . . . . ? O7 Ni2 N3 C12 -10.8(3) . . . . ? O1W Ni2 N3 C12 -99.2(3) . . . . ? N2 Ni1 N4 C30 -104.6(3) . . . . ? O11 Ni1 N4 C30 75.4(3) . . . . ? O1 Ni1 N4 C30 161.7(3) . . . . ? N1 Ni1 N4 C30 -23.0(3) . . . . ? N2 Ni1 O1 C10 -15.8(3) . . . . ? O11 Ni1 O1 C10 -177.8(3) . . . . ? N4 Ni1 O1 C10 88.0(3) . . . . ? N2 Ni1 O1 Sm1 159.30(13) . . . . ? O11 Ni1 O1 Sm1 -2.71(10) . . . . ? N4 Ni1 O1 Sm1 -96.92(13) . . . . ? O5 Sm1 O1 C10 34.9(3) . . . . ? O9 Sm1 O1 C10 -29.5(5) . . . . ? O4 Sm1 O1 C10 105.8(3) . . . . ? O2 Sm1 O1 C10 -44.4(3) . . . . ? O8 Sm1 O1 C10 151.3(3) . . . . ? O2 Sm1 O1 C10 -110.3(3) 3_776 . . . ? O11 Sm1 O1 C10 177.4(3) . . . . ? Sm1 Sm1 O1 C10 -79.0(3) 3_776 . . . ? O5 Sm1 O1 Ni1 -140.16(11) . . . . ? O9 Sm1 O1 Ni1 155.5(2) . . . . ? O4 Sm1 O1 Ni1 -69.17(10) . . . . ? O2 Sm1 O1 Ni1 140.58(12) . . . . ? O8 Sm1 O1 Ni1 -23.68(16) . . . . ? O2 Sm1 O1 Ni1 74.70(10) 3_776 . . . ? O11 Sm1 O1 Ni1 2.37(9) . . . . ? Sm1 Sm1 O1 Ni1 106.01(9) 3_776 . . . ? O5 Sm1 O2 C9 -28.3(3) . . . . ? O9 Sm1 O2 C9 -112.3(3) . . . . ? O4 Sm1 O2 C9 18.7(3) . . . . ? O8 Sm1 O2 C9 -148.9(3) . . . . ? O1 Sm1 O2 C9 62.7(3) . . . . ? O2 Sm1 O2 C9 164.9(3) 3_776 . . . ? O11 Sm1 O2 C9 108.6(3) . . . . ? Sm1 Sm1 O2 C9 164.9(3) 3_776 . . . ? O5 Sm1 O2 Sm1 166.79(12) . . . 3_776 ? O9 Sm1 O2 Sm1 82.78(11) . . . 3_776 ? O4 Sm1 O2 Sm1 -146.22(10) . . . 3_776 ? O8 Sm1 O2 Sm1 46.2(3) . . . 3_776 ? O1 Sm1 O2 Sm1 -102.19(11) . . . 3_776 ? O2 Sm1 O2 Sm1 -0.001(1) 3_776 . . 3_776 ? O11 Sm1 O2 Sm1 -56.36(13) . . . 3_776 ? N3 Ni2 O4 C20 17.2(3) . . . . ? O8 Ni2 O4 C20 -166.9(3) . . . . ? O11 Ni2 O4 C20 110.3(3) . . . . ? O7 Ni2 O4 C20 -170.5(5) . . . . ? O1W Ni2 O4 C20 -71.5(3) . . . . ? N3 Ni2 O4 Sm1 -133.85(11) . . . . ? O8 Ni2 O4 Sm1 42.03(9) . . . . ? O11 Ni2 O4 Sm1 -40.73(9) . . . . ? O7 Ni2 O4 Sm1 38.4(6) . . . . ? O1W Ni2 O4 Sm1 137.41(10) . . . . ? O5 Sm1 O4 C20 45.5(3) . . . . ? O9 Sm1 O4 C20 119.3(3) . . . . ? O2 Sm1 O4 C20 -4.0(4) . . . . ? O8 Sm1 O4 C20 170.8(3) . . . . ? O1 Sm1 O4 C20 -45.5(3) . . . . ? O2 Sm1 O4 C20 -124.3(3) 3_776 . . . ? O11 Sm1 O4 C20 -116.3(3) . . . . ? Sm1 Sm1 O4 C20 -57.6(4) 3_776 . . . ? O5 Sm1 O4 Ni2 -162.46(12) . . . . ? O9 Sm1 O4 Ni2 -88.64(11) . . . . ? O2 Sm1 O4 Ni2 148.08(10) . . . . ? O8 Sm1 O4 Ni2 -37.19(9) . . . . ? O1 Sm1 O4 Ni2 106.52(10) . . . . ? O2 Sm1 O4 Ni2 27.80(18) 3_776 . . . ? O11 Sm1 O4 Ni2 35.73(9) . . . . ? Sm1 Sm1 O4 Ni2 94.43(16) 3_776 . . . ? O9 Sm1 O5 C19 -147.3(4) . . . . ? O4 Sm1 O5 C19 -27.8(4) . . . . ? O2 Sm1 O5 C19 119.4(4) . . . . ? O8 Sm1 O5 C19 -82.1(4) . . . . ? O1 Sm1 O5 C19 50.3(4) . . . . ? O2 Sm1 O5 C19 141.4(4) 3_776 . . . ? O11 Sm1 O5 C19 -3.3(5) . . . . ? Sm1 Sm1 O5 C19 127.6(4) 3_776 . . . ? O4 Ni2 O7 C27 16.1(8) . . . . ? N3 Ni2 O7 C27 -171.8(3) . . . . ? O8 Ni2 O7 C27 12.5(3) . . . . ? O11 Ni2 O7 C27 94.3(3) . . . . ? O1W Ni2 O7 C27 -83.3(3) . . . . ? O4 Ni2 O8 C28 170.8(3) . . . . ? N3 Ni2 O8 C28 -166.6(6) . . . . ? O11 Ni2 O8 C28 -104.6(3) . . . . ? O7 Ni2 O8 C28 -9.9(3) . . . . ? O1W Ni2 O8 C28 78.6(3) . . . . ? O4 Ni2 O8 Sm1 -40.75(9) . . . . ? N3 Ni2 O8 Sm1 -18.1(7) . . . . ? O11 Ni2 O8 Sm1 43.86(9) . . . . ? O7 Ni2 O8 Sm1 138.60(10) . . . . ? O1W Ni2 O8 Sm1 -132.89(10) . . . . ? O5 Sm1 O8 C28 -118.2(3) . . . . ? O9 Sm1 O8 C28 -43.4(3) . . . . ? O4 Sm1 O8 C28 -174.5(3) . . . . ? O2 Sm1 O8 C28 -3.8(4) . . . . ? O1 Sm1 O8 C28 136.4(3) . . . . ? O2 Sm1 O8 C28 38.6(3) 3_776 . . . ? O11 Sm1 O8 C28 110.1(3) . . . . ? Sm1 Sm1 O8 C28 27.1(3) 3_776 . . . ? O5 Sm1 O8 Ni2 92.95(11) . . . . ? O9 Sm1 O8 Ni2 167.83(12) . . . . ? O4 Sm1 O8 Ni2 36.70(9) . . . . ? O2 Sm1 O8 Ni2 -152.65(17) . . . . ? O1 Sm1 O8 Ni2 -12.46(15) . . . . ? O2 Sm1 O8 Ni2 -110.23(9) 3_776 . . . ? O11 Sm1 O8 Ni2 -38.73(8) . . . . ? Sm1 Sm1 O8 Ni2 -121.74(6) 3_776 . . . ? O5 Sm1 O9 C21 133.6(4) . . . . ? O4 Sm1 O9 C21 67.9(4) . . . . ? O2 Sm1 O9 C21 -147.8(4) . . . . ? O8 Sm1 O9 C21 17.6(4) . . . . ? O1 Sm1 O9 C21 -161.7(4) . . . . ? O2 Sm1 O9 C21 -79.3(4) 3_776 . . . ? O11 Sm1 O9 C21 -14.4(4) . . . . ? Sm1 Sm1 O9 C21 -113.3(4) 3_776 . . . ? N2 Ni1 O11 Ni2 22.1(4) . . . . ? N4 Ni1 O11 Ni2 -157.71(14) . . . . ? O1 Ni1 O11 Ni2 99.16(13) . . . . ? N1 Ni1 O11 Ni2 -72.12(15) . . . . ? N2 Ni1 O11 Sm1 -74.3(4) . . . . ? N4 Ni1 O11 Sm1 105.86(12) . . . . ? O1 Ni1 O11 Sm1 2.72(10) . . . . ? N1 Ni1 O11 Sm1 -168.56(11) . . . . ? O4 Ni2 O11 Ni1 -66.48(13) . . . . ? N3 Ni2 O11 Ni1 21.70(15) . . . . ? O8 Ni2 O11 Ni1 -148.81(14) . . . . ? O7 Ni2 O11 Ni1 123.72(13) . . . . ? O4 Ni2 O11 Sm1 39.03(9) . . . . ? N3 Ni2 O11 Sm1 127.21(11) . . . . ? O8 Ni2 O11 Sm1 -43.30(9) . . . . ? O7 Ni2 O11 Sm1 -130.76(9) . . . . ? O5 Sm1 O11 Ni1 57.78(16) . . . . ? O9 Sm1 O11 Ni1 -171.17(9) . . . . ? O4 Sm1 O11 Ni1 82.70(11) . . . . ? O2 Sm1 O11 Ni1 -48.70(13) . . . . ? O8 Sm1 O11 Ni1 156.11(12) . . . . ? O1 Sm1 O11 Ni1 -2.45(9) . . . . ? O2 Sm1 O11 Ni1 -102.22(11) 3_776 . . . ? Sm1 Sm1 O11 Ni1 -77.41(9) 3_776 . . . ? O5 Sm1 O11 Ni2 -59.91(15) . . . . ? O9 Sm1 O11 Ni2 71.13(13) . . . . ? O4 Sm1 O11 Ni2 -34.99(9) . . . . ? O2 Sm1 O11 Ni2 -166.40(8) . . . . ? O8 Sm1 O11 Ni2 38.42(8) . . . . ? O1 Sm1 O11 Ni2 -120.15(11) . . . . ? O2 Sm1 O11 Ni2 140.08(10) 3_776 . . . ? Sm1 Sm1 O11 Ni2 164.90(6) 3_776 . . . ? C11 N1 C1 C2 165.0(3) . . . . ? C29 N1 C1 C2 -74.3(4) . . . . ? Ni1 N1 C1 C2 36.8(4) . . . . ? C3 N2 C2 C1 -157.4(4) . . . . ? Ni1 N2 C2 C1 30.6(5) . . . . ? N1 C1 C2 N2 -44.8(5) . . . . ? C2 N2 C3 C4 -173.5(4) . . . . ? Ni1 N2 C3 C4 -2.5(7) . . . . ? N2 C3 C4 C5 177.8(4) . . . . ? N2 C3 C4 C10 -1.0(7) . . . . ? C10 C4 C5 C6 -0.5(8) . . . . ? C3 C4 C5 C6 -179.3(5) . . . . ? C4 C5 C6 C7 2.6(8) . . . . ? C5 C6 C7 C8 -0.6(8) . . . . ? C6 C7 C8 C10 -3.4(7) . . . . ? C6 C7 C8 C9 171.9(5) . . . . ? Sm1 O2 C9 O3 124.9(3) . . . . ? Sm1 O2 C9 O3 -72.4(4) 3_776 . . . ? Sm1 O2 C9 C8 -59.4(4) . . . . ? Sm1 O2 C9 C8 103.3(3) 3_776 . . . ? C7 C8 C9 O3 8.4(6) . . . . ? C10 C8 C9 O3 -176.6(4) . . . . ? C7 C8 C9 O2 -167.4(4) . . . . ? C10 C8 C9 O2 7.7(6) . . . . ? Ni1 O1 C10 C4 16.7(5) . . . . ? Sm1 O1 C10 C4 -157.1(3) . . . . ? Ni1 O1 C10 C8 -165.0(3) . . . . ? Sm1 O1 C10 C8 21.1(5) . . . . ? C5 C4 C10 O1 174.8(4) . . . . ? C3 C4 C10 O1 -6.5(6) . . . . ? C5 C4 C10 C8 -3.5(6) . . . . ? C3 C4 C10 C8 175.2(4) . . . . ? C7 C8 C10 O1 -172.9(4) . . . . ? C9 C8 C10 O1 12.2(6) . . . . ? C7 C8 C10 C4 5.4(6) . . . . ? C9 C8 C10 C4 -169.5(4) . . . . ? C29 N1 C11 C12 -173.3(3) . . . . ? C1 N1 C11 C12 -52.3(4) . . . . ? Ni1 N1 C11 C12 69.1(4) . . . . ? C13 N3 C12 C11 120.0(4) . . . . ? Ni2 N3 C12 C11 -68.0(4) . . . . ? N1 C11 C12 N3 -51.6(5) . . . . ? C12 N3 C13 C14 -172.7(4) . . . . ? Ni2 N3 C13 C14 15.9(6) . . . . ? N3 C13 C14 C15 176.4(5) . . . . ? N3 C13 C14 C20 2.9(7) . . . . ? C20 C14 C15 C16 0.8(8) . . . . ? C13 C14 C15 C16 -172.9(5) . . . . ? C14 C15 C16 C17 0.7(9) . . . . ? C15 C16 C17 C18 -0.8(9) . . . . ? C16 C17 C18 C20 -0.6(7) . . . . ? C16 C17 C18 C19 178.9(5) . . . . ? Sm1 O5 C19 O6 -171.1(3) . . . . ? Sm1 O5 C19 C18 7.1(7) . . . . ? C17 C18 C19 O6 15.5(6) . . . . ? C20 C18 C19 O6 -165.1(4) . . . . ? C17 C18 C19 O5 -162.8(4) . . . . ? C20 C18 C19 O5 16.7(6) . . . . ? Ni2 O4 C20 C18 174.4(3) . . . . ? Sm1 O4 C20 C18 -44.1(5) . . . . ? Ni2 O4 C20 C14 -6.0(5) . . . . ? Sm1 O4 C20 C14 135.6(3) . . . . ? C17 C18 C20 O4 -178.3(4) . . . . ? C19 C18 C20 O4 2.3(6) . . . . ? C17 C18 C20 C14 2.1(6) . . . . ? C19 C18 C20 C14 -177.4(4) . . . . ? C15 C14 C20 O4 178.2(4) . . . . ? C13 C14 C20 O4 -8.6(6) . . . . ? C15 C14 C20 C18 -2.2(6) . . . . ? C13 C14 C20 C18 171.1(4) . . . . ? Sm1 O9 C21 O10 -175.5(3) . . . . ? Sm1 O9 C21 C22 5.0(6) . . . . ? O10 C21 C22 C23 -18.1(6) . . . . ? O9 C21 C22 C23 161.4(4) . . . . ? O10 C21 C22 C28 160.4(4) . . . . ? O9 C21 C22 C28 -20.1(6) . . . . ? C28 C22 C23 C24 2.1(7) . . . . ? C21 C22 C23 C24 -179.4(4) . . . . ? C22 C23 C24 C25 2.1(7) . . . . ? C23 C24 C25 C26 -3.7(7) . . . . ? C24 C25 C26 C28 0.9(7) . . . . ? C24 C25 C26 C27 177.2(4) . . . . ? Ni2 O7 C27 C26 -7.6(6) . . . . ? C25 C26 C27 O7 177.8(4) . . . . ? C28 C26 C27 O7 -6.1(7) . . . . ? Ni2 O8 C28 C26 1.4(5) . . . . ? Sm1 O8 C28 C26 -135.5(3) . . . . ? Ni2 O8 C28 C22 -176.6(2) . . . . ? Sm1 O8 C28 C22 46.5(5) . . . . ? C25 C26 C28 O8 -174.7(4) . . . . ? C27 C26 C28 O8 9.3(6) . . . . ? C25 C26 C28 C22 3.3(6) . . . . ? C27 C26 C28 C22 -172.6(4) . . . . ? C23 C22 C28 O8 173.3(4) . . . . ? C21 C22 C28 O8 -5.2(5) . . . . ? C23 C22 C28 C26 -4.7(5) . . . . ? C21 C22 C28 C26 176.7(3) . . . . ? C11 N1 C29 C30 -93.8(4) . . . . ? C1 N1 C29 C30 144.6(4) . . . . ? Ni1 N1 C29 C30 32.3(4) . . . . ? Ni1 N4 C30 C29 47.2(4) . . . . ? N1 C29 C30 N4 -55.0(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.598 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.103 data_1 _database_code_depnum_ccdc_archive 'CCDC 898020' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 Eu2 N8 Ni4 O24, 9(H2 O)' _chemical_formula_sum 'C60 H76 Eu2 N8 Ni4 O33' _chemical_formula_weight 1976.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.703(3) _cell_length_b 18.339(5) _cell_length_c 15.578(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.101(4) _cell_angle_gamma 90.00 _cell_volume 3592.9(16) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2215 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.25 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 2.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6437 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_process_details 'SADABS (Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17947 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6331 _reflns_number_gt 5156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^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 6331 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Ni1 Ni 0.15540(6) 0.89262(4) 0.70755(5) 0.0353(2) Uani 1 1 d . . . Ni2 Ni 0.30926(6) 1.04742(4) 0.70947(5) 0.03202(19) Uani 1 1 d . . . Eu1 Eu 0.08134(2) 1.055429(13) 0.597304(17) 0.02785(12) Uani 1 1 d . . . C1 C -0.1671(4) 0.9789(3) 0.6583(4) 0.0359(13) Uani 1 1 d . . . C2 C -0.2628(5) 0.9723(4) 0.6930(5) 0.0585(19) Uani 1 1 d . . . H2 H -0.3222 0.9977 0.6668 0.070 Uiso 1 1 calc R . . C3 C -0.2722(6) 0.9299(5) 0.7640(6) 0.073(3) Uani 1 1 d . . . H3 H -0.3362 0.9279 0.7864 0.088 Uiso 1 1 calc R . . C4 C -0.1866(6) 0.8906(5) 0.8016(5) 0.071(2) Uani 1 1 d . . . H4 H -0.1942 0.8596 0.8476 0.085 Uiso 1 1 calc R . . C5 C -0.0871(5) 0.8960(3) 0.7718(4) 0.0483(16) Uani 1 1 d . . . C6 C -0.0745(5) 0.9434(3) 0.7004(4) 0.0357(14) Uani 1 1 d . . . C7 C -0.1727(4) 1.0204(3) 0.5750(4) 0.0323(12) Uani 1 1 d . . . C8 C -0.0032(6) 0.8503(4) 0.8164(5) 0.0579(19) Uani 1 1 d . . . H8 H -0.0217 0.8217 0.8613 0.070 Uiso 1 1 calc R . . C9 C 0.1619(6) 0.7886(4) 0.8513(5) 0.064(2) Uani 1 1 d . . . H9A H 0.1476 0.7410 0.8252 0.076 Uiso 1 1 calc R . . H9B H 0.1465 0.7866 0.9105 0.076 Uiso 1 1 calc R . . C10 C 0.2763(6) 0.8083(4) 0.8509(5) 0.062(2) Uani 1 1 d . . . H10A H 0.3207 0.7665 0.8688 0.075 Uiso 1 1 calc R . . H10B H 0.2958 0.8474 0.8921 0.075 Uiso 1 1 calc R . . C11 C 0.3982(5) 0.8708(3) 0.7655(4) 0.0480(16) Uani 1 1 d . . . H11A H 0.4030 0.8901 0.7082 0.058 Uiso 1 1 calc R . . H11B H 0.4548 0.8353 0.7786 0.058 Uiso 1 1 calc R . . C12 C 0.4183(6) 0.9336(4) 0.8314(5) 0.061(2) Uani 1 1 d . . . H12A H 0.4257 0.9142 0.8899 0.073 Uiso 1 1 calc R . . H12B H 0.4840 0.9583 0.8241 0.073 Uiso 1 1 calc R . . C13 C 0.2787(7) 0.9979(4) 0.8832(5) 0.075(3) Uani 1 1 d . . . H13 H 0.3061 0.9756 0.9352 0.090 Uiso 1 1 calc R . . C14 C 0.1824(8) 1.0427(5) 0.8845(5) 0.074(3) Uani 1 1 d . . . C15 C 0.1364(12) 1.0453(6) 0.9627(7) 0.137(6) Uani 1 1 d . . . H15 H 0.1701 1.0204 1.0109 0.165 Uiso 1 1 calc R . . C16 C 0.0478(12) 1.0815(7) 0.9702(8) 0.130(5) Uani 1 1 d . . . H16 H 0.0233 1.0846 1.0235 0.156 Uiso 1 1 calc R . . C17 C -0.0069(8) 1.1142(5) 0.8992(6) 0.091(3) Uani 1 1 d . . . H17 H -0.0702 1.1384 0.9042 0.109 Uiso 1 1 calc R . . C18 C 0.0299(6) 1.1122(3) 0.8197(5) 0.0524(18) Uani 1 1 d . . . C19 C 0.1283(5) 1.0776(3) 0.8115(4) 0.0453(15) Uani 1 1 d . . . C20 C -0.0405(5) 1.1451(4) 0.7448(5) 0.0570(19) Uani 1 1 d . . . C21 C 0.2955(6) 0.7677(3) 0.7054(5) 0.0592(19) Uani 1 1 d . . . H21A H 0.2534 0.7294 0.7269 0.071 Uiso 1 1 calc R . . H21B H 0.3677 0.7498 0.7075 0.071 Uiso 1 1 calc R . . C22 C 0.2512(6) 0.7848(4) 0.6141(5) 0.0569(18) Uani 1 1 d . . . H22A H 0.2479 0.7407 0.5794 0.068 Uiso 1 1 calc R . . H22B H 0.2970 0.8194 0.5902 0.068 Uiso 1 1 calc R . . C24 C 0.4151(4) 1.1099(3) 0.5357(4) 0.0381(13) Uani 1 1 d . . . C25 C 0.4679(5) 1.1392(4) 0.4699(5) 0.0546(17) Uani 1 1 d . . . H25 H 0.5387 1.1268 0.4692 0.066 Uiso 1 1 calc R . . C26 C 0.4202(5) 1.1844(4) 0.4078(5) 0.060(2) Uani 1 1 d . . . H26 H 0.4581 1.2043 0.3666 0.073 Uiso 1 1 calc R . . C27 C 0.3123(5) 1.2007(3) 0.4071(4) 0.0474(16) Uani 1 1 d . . . H27 H 0.2788 1.2312 0.3640 0.057 Uiso 1 1 calc R . . C28 C 0.2532(5) 1.1728(3) 0.4687(4) 0.0341(12) Uani 1 1 d . . . C29 C 0.3057(4) 1.1289(3) 0.5370(4) 0.0305(12) Uani 1 1 d . . . C30 C 0.1383(5) 1.1929(3) 0.4618(4) 0.0370(13) Uani 1 1 d . . . N1 N 0.0931(4) 0.8444(3) 0.8015(4) 0.0513(15) Uani 1 1 d . . . N2 N 0.2956(4) 0.8324(3) 0.7622(4) 0.0466(13) Uani 1 1 d . . . N3 N 0.3292(4) 0.9860(3) 0.8187(3) 0.0460(13) Uani 1 1 d . . . N4 N 0.1422(4) 0.8163(3) 0.6115(4) 0.0557(15) Uani 1 1 d . . . H4A H 0.0953 0.7815 0.6211 0.067 Uiso 1 1 calc R . . H4B H 0.1205 0.8370 0.5596 0.067 Uiso 1 1 calc R . . C31 C 0.4729(5) 1.0594(3) 0.5940(4) 0.0419(15) Uani 1 1 d . . . H31 H 0.5413 1.0493 0.5826 0.050 Uiso 1 1 calc R . . O1 O 0.0197(3) 0.95372(19) 0.6760(3) 0.0346(9) Uani 1 1 d . . . O2 O -0.0914(3) 1.0169(2) 0.5326(2) 0.0320(8) Uani 1 1 d . . . O3 O -0.2552(3) 1.0538(2) 0.5447(3) 0.0448(11) Uani 1 1 d . . . O4 O 0.1657(3) 1.0787(2) 0.7385(2) 0.0379(9) Uani 1 1 d . . . O5 O -0.1131(5) 1.1865(5) 0.7604(5) 0.131(3) Uani 1 1 d . . . O6 O -0.0277(3) 1.1297(2) 0.6678(3) 0.0514(11) Uani 1 1 d . . . O7 O 0.4462(3) 1.0268(2) 0.6576(3) 0.0420(10) Uani 1 1 d . . . O8 O 0.2574(3) 1.1070(2) 0.6019(2) 0.0338(9) Uani 1 1 d . . . O9 O 0.0753(3) 1.1553(2) 0.5009(3) 0.0442(10) Uani 1 1 d . . . O10 O 0.1053(4) 1.2465(3) 0.4164(3) 0.0615(14) Uani 1 1 d . . . O1W O 0.3891(3) 1.1331(2) 0.7791(3) 0.0537(11) Uani 1 1 d . . . H1WA H 0.3877 1.1230 0.8322 0.064 Uiso 1 1 d R . . H1WB H 0.4543 1.1297 0.7728 0.064 Uiso 1 1 d R . . O12 O 0.2228(3) 0.96722(19) 0.6397(2) 0.0302(8) Uani 1 1 d . . . H12 H 0.2558 0.9475 0.5914 0.036 Uiso 1 1 calc R . . O2W O 0.7178(5) 0.1897(3) 0.6368(4) 0.0913(19) Uani 1 1 d . . . H2WA H 0.6677 0.1752 0.6634 0.110 Uiso 1 1 d R . . H2WB H 0.7710 0.1939 0.6761 0.110 Uiso 1 1 d R . . O3W O 0.5770(6) 0.1855(5) 0.7533(6) 0.162(5) Uani 1 1 d . . . H3WA H 0.6037 0.1985 0.7086 0.194 Uiso 1 1 d R . . H3WB H 0.5218 0.2118 0.7523 0.194 Uiso 1 1 d R . . O4W O 0.5840(8) 0.7738(4) 0.9226(5) 0.149(4) Uani 1 1 d . . . H4WA H 0.6358 0.7467 0.9430 0.179 Uiso 1 1 d R . . H4WB H 0.5846 0.7734 0.8682 0.179 Uiso 1 1 d R . . O5W O 0.4565(8) 0.1332(6) 0.9589(5) 0.182(5) Uani 1 1 d . . . H5WA H 0.4374 0.1654 0.9206 0.218 Uiso 1 1 d R . . H5WB H 0.4015 0.1070 0.9598 0.218 Uiso 1 1 d R . . O6W O 0.7106(15) 0.1135(8) 0.9155(11) 0.144(7) Uani 0.50 1 d P . . H6WA H 0.7702 0.1205 0.9467 0.173 Uiso 0.50 1 d PR . . H6WB H 0.6648 0.1224 0.9490 0.173 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0337(4) 0.0299(4) 0.0427(4) 0.0097(3) 0.0067(3) 0.0071(3) Ni2 0.0305(4) 0.0333(4) 0.0305(4) 0.0001(3) -0.0019(3) 0.0027(3) Eu1 0.02472(18) 0.02512(18) 0.03318(19) 0.00045(10) 0.00228(12) 0.00197(10) C1 0.033(3) 0.035(3) 0.041(3) 0.000(3) 0.009(3) 0.004(2) C2 0.035(4) 0.088(5) 0.056(5) 0.010(4) 0.016(3) 0.010(4) C3 0.040(4) 0.116(7) 0.068(5) 0.040(5) 0.028(4) 0.017(4) C4 0.050(4) 0.095(6) 0.072(5) 0.037(5) 0.023(4) 0.012(4) C5 0.045(4) 0.050(4) 0.052(4) 0.013(3) 0.014(3) 0.002(3) C6 0.037(3) 0.030(3) 0.042(3) 0.000(2) 0.011(3) -0.002(2) C7 0.026(3) 0.037(3) 0.034(3) -0.009(2) 0.004(2) 0.001(2) C8 0.054(4) 0.067(5) 0.057(4) 0.030(4) 0.023(4) 0.012(3) C9 0.063(5) 0.055(4) 0.075(5) 0.031(4) 0.018(4) 0.026(4) C10 0.059(5) 0.063(5) 0.066(5) 0.037(4) 0.010(4) 0.018(4) C11 0.046(4) 0.046(4) 0.052(4) 0.012(3) 0.007(3) 0.015(3) C12 0.067(5) 0.068(5) 0.044(4) 0.006(3) -0.003(4) 0.018(4) C13 0.113(7) 0.075(5) 0.036(4) 0.023(4) 0.008(4) 0.046(5) C14 0.096(7) 0.086(6) 0.044(5) 0.008(4) 0.024(4) 0.036(5) C15 0.219(15) 0.150(10) 0.060(7) 0.049(6) 0.076(9) 0.093(10) C16 0.183(13) 0.146(10) 0.079(8) 0.012(7) 0.079(9) 0.073(10) C17 0.106(8) 0.100(7) 0.078(7) 0.007(5) 0.047(6) 0.033(6) C18 0.057(4) 0.048(4) 0.058(4) -0.009(3) 0.028(4) 0.002(3) C19 0.053(4) 0.044(3) 0.038(4) -0.002(3) 0.005(3) 0.007(3) C20 0.040(4) 0.053(4) 0.080(6) -0.032(4) 0.013(4) 0.002(3) C21 0.047(4) 0.039(4) 0.091(6) 0.009(4) 0.009(4) 0.014(3) C22 0.052(4) 0.050(4) 0.069(5) -0.008(3) 0.011(4) 0.015(3) C24 0.033(3) 0.040(3) 0.041(3) 0.001(3) 0.005(3) 0.000(2) C25 0.038(4) 0.066(4) 0.062(5) 0.013(4) 0.014(3) 0.003(3) C26 0.049(4) 0.077(5) 0.061(5) 0.024(4) 0.025(4) 0.003(4) C27 0.052(4) 0.044(3) 0.045(4) 0.018(3) 0.006(3) 0.006(3) C28 0.040(3) 0.027(3) 0.034(3) 0.001(2) 0.001(2) 0.001(2) C29 0.028(3) 0.025(3) 0.038(3) -0.005(2) 0.003(2) -0.002(2) C30 0.042(3) 0.027(3) 0.042(3) 0.008(2) 0.002(3) 0.000(2) N1 0.049(3) 0.050(3) 0.056(4) 0.031(3) 0.012(3) 0.017(3) N2 0.040(3) 0.041(3) 0.058(3) 0.019(2) 0.005(3) 0.016(2) N3 0.055(3) 0.047(3) 0.034(3) 0.006(2) 0.000(2) 0.014(3) N4 0.044(3) 0.042(3) 0.080(4) -0.008(3) 0.005(3) 0.004(2) C31 0.032(3) 0.048(4) 0.045(4) 0.002(3) 0.003(3) 0.007(3) O1 0.030(2) 0.034(2) 0.041(2) 0.0090(16) 0.0076(18) 0.0038(16) O2 0.0241(19) 0.036(2) 0.035(2) -0.0033(16) 0.0027(16) 0.0025(15) O3 0.030(2) 0.058(3) 0.047(3) 0.004(2) 0.006(2) 0.0140(19) O4 0.037(2) 0.047(2) 0.030(2) -0.0033(18) 0.0099(18) 0.0008(18) O5 0.075(4) 0.202(8) 0.106(5) -0.095(5) -0.026(4) 0.080(5) O6 0.041(3) 0.050(3) 0.064(3) -0.013(2) 0.009(2) 0.011(2) O7 0.031(2) 0.046(2) 0.048(3) 0.008(2) 0.0021(19) 0.0088(18) O8 0.0243(19) 0.039(2) 0.038(2) 0.0096(17) 0.0031(16) 0.0009(16) O9 0.037(2) 0.039(2) 0.054(3) 0.016(2) -0.002(2) 0.0018(18) O10 0.055(3) 0.055(3) 0.076(3) 0.037(3) 0.014(3) 0.020(2) O1W 0.042(3) 0.058(3) 0.057(3) -0.015(2) -0.006(2) 0.000(2) O12 0.030(2) 0.0294(18) 0.030(2) -0.0021(15) -0.0006(16) 0.0000(16) O2W 0.078(4) 0.095(4) 0.100(5) -0.026(4) 0.011(4) 0.015(3) O3W 0.104(6) 0.222(9) 0.175(8) -0.132(8) 0.075(6) -0.097(6) O4W 0.257(11) 0.072(5) 0.097(6) -0.001(4) -0.050(6) -0.005(6) O5W 0.190(10) 0.252(12) 0.085(6) -0.034(7) -0.041(6) 0.076(9) O6W 0.185(18) 0.105(12) 0.134(14) 0.018(10) -0.009(13) 0.059(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.970(5) . y Ni1 O12 1.994(4) . y Ni1 N4 2.039(6) . y Ni1 O1 2.057(4) . y Ni1 N2 2.165(5) . y Ni2 O4 2.022(4) . y Ni2 N3 2.026(5) . y Ni2 O8 2.030(4) . y Ni2 O12 2.053(4) . y Ni2 O7 2.054(4) . y Ni2 O1W 2.090(4) . y Ni2 Eu1 3.1672(10) . y Eu1 O6 2.325(4) . y Eu1 O9 2.363(4) . y Eu1 O2 2.389(4) . y Eu1 O8 2.420(4) . y Eu1 O1 2.422(4) . y Eu1 O2 2.437(4) 3_576 y Eu1 O12 2.438(4) . y C1 C2 1.405(8) . ? C1 C6 1.422(8) . ? C1 C7 1.497(8) . ? C2 C3 1.371(10) . ? C2 H2 0.9300 . ? C3 C4 1.365(11) . ? C3 H3 0.9300 . ? C4 C5 1.410(9) . ? C4 H4 0.9300 . ? C5 C6 1.438(8) . ? C5 C8 1.454(9) . ? C6 O1 1.319(7) . ? C7 O3 1.248(7) . ? C7 O2 1.303(6) . ? C8 N1 1.281(8) . ? C8 H8 0.9300 . ? C9 N1 1.490(8) . ? C9 C10 1.499(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.504(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.475(8) . ? C11 C12 1.542(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.477(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.284(9) . ? C13 C14 1.477(11) . ? C13 H13 0.9300 . ? C14 C19 1.398(11) . ? C14 C15 1.425(11) . ? C15 C16 1.325(16) . ? C15 H15 0.9300 . ? C16 C17 1.359(16) . ? C16 H16 0.9300 . ? C17 C18 1.385(10) . ? C17 H17 0.9300 . ? C18 C19 1.423(9) . ? C18 C20 1.494(11) . ? C19 O4 1.294(7) . ? C20 O5 1.244(8) . ? C20 O6 1.266(8) . ? C21 N2 1.480(9) . ? C21 C22 1.488(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N4 1.496(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C25 1.407(8) . ? C24 C31 1.425(9) . ? C24 C29 1.436(7) . ? C25 C26 1.352(10) . ? C25 H25 0.9300 . ? C26 C27 1.401(9) . ? C26 H26 0.9300 . ? C27 C28 1.396(8) . ? C27 H27 0.9300 . ? C28 C29 1.424(8) . ? C28 C30 1.494(8) . ? C29 O8 1.318(6) . ? C30 O10 1.248(7) . ? C30 O9 1.275(6) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C31 O7 1.246(7) . ? C31 H31 0.9300 . ? O2 Eu1 2.438(4) 3_576 y O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O12 H12 0.9800 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 O12 161.8(2) . . y N1 Ni1 N4 103.7(2) . . y O12 Ni1 N4 94.5(2) . . y N1 Ni1 O1 90.64(18) . . y O12 Ni1 O1 84.68(15) . . y N4 Ni1 O1 102.7(2) . . y N1 Ni1 N2 82.7(2) . . y O12 Ni1 N2 99.65(17) . . y N4 Ni1 N2 85.2(2) . . y O1 Ni1 N2 170.78(19) . . y O4 Ni2 N3 88.84(19) . . y O4 Ni2 O8 80.44(15) . . y N3 Ni2 O8 168.35(19) . . y O4 Ni2 O12 83.64(15) . . y N3 Ni2 O12 92.33(19) . . y O8 Ni2 O12 82.03(15) . . y O4 Ni2 O7 168.66(16) . . y N3 Ni2 O7 102.43(19) . . y O8 Ni2 O7 88.23(15) . . y O12 Ni2 O7 94.57(16) . . y O4 Ni2 O1W 93.31(17) . . y N3 Ni2 O1W 89.3(2) . . y O8 Ni2 O1W 95.80(17) . . y O12 Ni2 O1W 176.50(16) . . y O7 Ni2 O1W 88.09(18) . . y O4 Ni2 Eu1 47.71(11) . . y N3 Ni2 Eu1 119.03(16) . . y O8 Ni2 Eu1 49.82(10) . . y O12 Ni2 Eu1 50.34(10) . . y O7 Ni2 Eu1 123.42(12) . . y O1W Ni2 Eu1 126.20(13) . . y O6 Eu1 O9 82.99(15) . . y O6 Eu1 O2 78.45(14) . . y O9 Eu1 O2 90.89(14) . . y O6 Eu1 O8 111.50(14) . . y O9 Eu1 O8 70.32(13) . . y O2 Eu1 O8 156.67(13) . . y O6 Eu1 O1 87.45(14) . . y O9 Eu1 O1 159.20(14) . . y O2 Eu1 O1 69.05(14) . . y O8 Eu1 O1 130.49(13) . . y O6 Eu1 O2 144.59(14) . 3_576 y O9 Eu1 O2 83.97(13) . 3_576 y O2 Eu1 O2 68.98(13) . 3_576 y O8 Eu1 O2 94.63(12) . 3_576 y O1 Eu1 O2 93.43(13) . 3_576 y O6 Eu1 O12 136.54(15) . . y O9 Eu1 O12 130.02(13) . . y O2 Eu1 O12 121.04(12) . . y O8 Eu1 O12 66.96(12) . . y O1 Eu1 O12 68.31(12) . . y O2 Eu1 O12 74.98(12) 3_576 . y O6 Eu1 Ni2 109.00(12) . . y O9 Eu1 Ni2 109.38(10) . . y O2 Eu1 Ni2 158.89(9) . . y O8 Eu1 Ni2 39.87(9) . . y O1 Eu1 Ni2 91.18(10) . . y O2 Eu1 Ni2 106.37(9) 3_576 . y O12 Eu1 Ni2 40.41(8) . . y O6 Eu1 Eu1 112.28(12) . 3_576 y O9 Eu1 Eu1 86.85(11) . 3_576 y O2 Eu1 Eu1 34.88(8) . 3_576 y O8 Eu1 Eu1 126.94(9) . 3_576 y O1 Eu1 Eu1 79.74(10) . 3_576 y O2 Eu1 Eu1 34.10(8) 3_576 3_576 y O12 Eu1 Eu1 98.68(8) . 3_576 y Ni2 Eu1 Eu1 137.133(17) . 3_576 y C2 C1 C6 119.2(6) . . ? C2 C1 C7 116.1(5) . . ? C6 C1 C7 124.6(5) . . ? C3 C2 C1 122.5(7) . . ? C3 C2 H2 118.7 . . ? C1 C2 H2 118.7 . . ? C4 C3 C2 119.5(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.2(7) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 120.0(6) . . ? C4 C5 C8 115.7(6) . . ? C6 C5 C8 124.3(5) . . ? O1 C6 C1 121.7(5) . . ? O1 C6 C5 121.0(5) . . ? C1 C6 C5 117.3(5) . . ? O3 C7 O2 121.0(5) . . ? O3 C7 C1 120.8(5) . . ? O2 C7 C1 118.0(5) . . ? N1 C8 C5 128.1(6) . . ? N1 C8 H8 116.0 . . ? C5 C8 H8 116.0 . . ? N1 C9 C10 109.3(5) . . ? N1 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? N1 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? C9 C10 N2 111.0(6) . . ? C9 C10 H10A 109.4 . . ? N2 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? N2 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C12 116.3(5) . . ? N2 C11 H11A 108.2 . . ? C12 C11 H11A 108.2 . . ? N2 C11 H11B 108.2 . . ? C12 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? N3 C12 C11 110.2(6) . . ? N3 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N3 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N3 C13 C14 127.7(7) . . ? N3 C13 H13 116.2 . . ? C14 C13 H13 116.2 . . ? C19 C14 C15 117.8(8) . . ? C19 C14 C13 123.8(6) . . ? C15 C14 C13 118.1(8) . . ? C16 C15 C14 123.1(10) . . ? C16 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C15 C16 C17 119.6(9) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 121.1(9) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C19 120.3(8) . . ? C17 C18 C20 116.6(7) . . ? C19 C18 C20 123.1(6) . . ? O4 C19 C14 121.5(6) . . ? O4 C19 C18 120.6(6) . . ? C14 C19 C18 117.9(6) . . ? O5 C20 O6 121.3(8) . . ? O5 C20 C18 118.2(7) . . ? O6 C20 C18 120.5(6) . . ? N2 C21 C22 111.8(5) . . ? N2 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? N2 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? C21 C22 N4 109.3(6) . . ? C21 C22 H22A 109.8 . . ? N4 C22 H22A 109.8 . . ? C21 C22 H22B 109.8 . . ? N4 C22 H22B 109.8 . . ? H22A C22 H22B 108.3 . . ? C25 C24 C31 117.1(6) . . ? C25 C24 C29 118.6(6) . . ? C31 C24 C29 124.1(5) . . ? C26 C25 C24 123.0(6) . . ? C26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C25 C26 C27 118.4(6) . . ? C25 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C28 C27 C26 122.5(6) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 118.7(5) . . ? C27 C28 C30 118.3(5) . . ? C29 C28 C30 122.9(5) . . ? O8 C29 C28 121.8(5) . . ? O8 C29 C24 119.6(5) . . ? C28 C29 C24 118.7(5) . . ? O10 C30 O9 120.9(5) . . ? O10 C30 C28 118.8(5) . . ? O9 C30 C28 120.3(5) . . ? C8 N1 C9 118.0(5) . . ? C8 N1 Ni1 126.2(4) . . ? C9 N1 Ni1 115.3(4) . . ? C11 N2 C21 109.3(5) . . ? C11 N2 C10 111.5(5) . . ? C21 N2 C10 109.1(5) . . ? C11 N2 Ni1 116.4(4) . . ? C21 N2 Ni1 104.0(4) . . ? C10 N2 Ni1 106.2(4) . . ? C13 N3 C12 117.5(6) . . ? C13 N3 Ni2 123.1(4) . . ? C12 N3 Ni2 118.5(4) . . ? C22 N4 Ni1 105.4(4) . . ? C22 N4 H4A 110.7 . . ? Ni1 N4 H4A 110.7 . . ? C22 N4 H4B 110.7 . . ? Ni1 N4 H4B 110.7 . . ? H4A N4 H4B 108.8 . . ? O7 C31 C24 130.3(6) . . ? O7 C31 H31 114.9 . . ? C24 C31 H31 114.9 . . ? C6 O1 Ni1 128.1(3) . . ? C6 O1 Eu1 128.9(3) . . ? Ni1 O1 Eu1 102.75(15) . . ? C7 O2 Eu1 121.1(3) . . ? C7 O2 Eu1 125.9(3) . 3_576 ? Eu1 O2 Eu1 111.02(13) . 3_576 ? C19 O4 Ni2 130.3(4) . . ? C20 O6 Eu1 138.1(5) . . ? C31 O7 Ni2 124.4(4) . . ? C29 O8 Ni2 131.7(3) . . ? C29 O8 Eu1 128.6(3) . . ? Ni2 O8 Eu1 90.31(13) . . ? C30 O9 Eu1 139.2(4) . . ? Ni2 O1W H1WA 105.4 . . ? Ni2 O1W H1WB 107.1 . . ? H1WA O1W H1WB 104.5 . . ? Ni1 O12 Ni2 116.62(18) . . ? Ni1 O12 Eu1 104.12(15) . . ? Ni2 O12 Eu1 89.25(13) . . ? Ni1 O12 H12 114.6 . . ? Ni2 O12 H12 114.6 . . ? Eu1 O12 H12 114.6 . . ? H2WA O2W H2WB 104.5 . . ? H3WA O3W H3WB 104.5 . . ? H4WA O4W H4WB 104.5 . . ? H5WA O5W H5WB 104.5 . . ? H6WA O6W H6WB 104.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ni2 Eu1 O6 17.21(19) . . . . ? N3 Ni2 Eu1 O6 74.8(2) . . . . ? O8 Ni2 Eu1 O6 -101.09(19) . . . . ? O12 Ni2 Eu1 O6 141.23(18) . . . . ? O7 Ni2 Eu1 O6 -153.81(19) . . . . ? O1W Ni2 Eu1 O6 -38.1(2) . . . . ? O4 Ni2 Eu1 O9 106.31(19) . . . . ? N3 Ni2 Eu1 O9 163.9(2) . . . . ? O8 Ni2 Eu1 O9 -11.99(18) . . . . ? O12 Ni2 Eu1 O9 -129.67(17) . . . . ? O7 Ni2 Eu1 O9 -64.71(18) . . . . ? O1W Ni2 Eu1 O9 51.0(2) . . . . ? O4 Ni2 Eu1 O2 -90.5(3) . . . . ? N3 Ni2 Eu1 O2 -32.9(3) . . . . ? O8 Ni2 Eu1 O2 151.2(3) . . . . ? O12 Ni2 Eu1 O2 33.5(3) . . . . ? O7 Ni2 Eu1 O2 98.5(3) . . . . ? O1W Ni2 Eu1 O2 -145.8(3) . . . . ? O4 Ni2 Eu1 O8 118.3(2) . . . . ? N3 Ni2 Eu1 O8 175.9(2) . . . . ? O12 Ni2 Eu1 O8 -117.67(19) . . . . ? O7 Ni2 Eu1 O8 -52.7(2) . . . . ? O1W Ni2 Eu1 O8 63.0(2) . . . . ? O4 Ni2 Eu1 O1 -70.50(18) . . . . ? N3 Ni2 Eu1 O1 -12.91(19) . . . . ? O8 Ni2 Eu1 O1 171.20(17) . . . . ? O12 Ni2 Eu1 O1 53.53(16) . . . . ? O7 Ni2 Eu1 O1 118.48(17) . . . . ? O1W Ni2 Eu1 O1 -125.82(19) . . . . ? O4 Ni2 Eu1 O2 -164.42(18) . . . 3_576 ? N3 Ni2 Eu1 O2 -106.8(2) . . . 3_576 ? O8 Ni2 Eu1 O2 77.27(17) . . . 3_576 ? O12 Ni2 Eu1 O2 -40.40(16) . . . 3_576 ? O7 Ni2 Eu1 O2 24.56(17) . . . 3_576 ? O1W Ni2 Eu1 O2 140.26(19) . . . 3_576 ? O4 Ni2 Eu1 O12 -124.0(2) . . . . ? N3 Ni2 Eu1 O12 -66.4(2) . . . . ? O8 Ni2 Eu1 O12 117.67(19) . . . . ? O7 Ni2 Eu1 O12 64.95(19) . . . . ? O1W Ni2 Eu1 O12 -179.3(2) . . . . ? O4 Ni2 Eu1 Eu1 -146.64(16) . . . 3_576 ? N3 Ni2 Eu1 Eu1 -89.05(17) . . . 3_576 ? O8 Ni2 Eu1 Eu1 95.06(14) . . . 3_576 ? O12 Ni2 Eu1 Eu1 -22.61(13) . . . 3_576 ? O7 Ni2 Eu1 Eu1 42.34(15) . . . 3_576 ? O1W Ni2 Eu1 Eu1 158.05(16) . . . 3_576 ? C6 C1 C2 C3 -3.2(11) . . . . ? C7 C1 C2 C3 173.4(7) . . . . ? C1 C2 C3 C4 -2.0(14) . . . . ? C2 C3 C4 C5 3.7(15) . . . . ? C3 C4 C5 C6 -0.3(13) . . . . ? C3 C4 C5 C8 -178.9(9) . . . . ? C2 C1 C6 O1 -172.9(6) . . . . ? C7 C1 C6 O1 10.7(9) . . . . ? C2 C1 C6 C5 6.4(9) . . . . ? C7 C1 C6 C5 -170.0(6) . . . . ? C4 C5 C6 O1 174.6(7) . . . . ? C8 C5 C6 O1 -7.0(10) . . . . ? C4 C5 C6 C1 -4.7(10) . . . . ? C8 C5 C6 C1 173.7(7) . . . . ? C2 C1 C7 O3 7.8(8) . . . . ? C6 C1 C7 O3 -175.7(5) . . . . ? C2 C1 C7 O2 -167.9(6) . . . . ? C6 C1 C7 O2 8.5(8) . . . . ? C4 C5 C8 N1 179.1(8) . . . . ? C6 C5 C8 N1 0.7(13) . . . . ? N1 C9 C10 N2 -43.5(9) . . . . ? N2 C11 C12 N3 -53.2(8) . . . . ? N3 C13 C14 C19 2.6(16) . . . . ? N3 C13 C14 C15 176.8(10) . . . . ? C19 C14 C15 C16 -3(2) . . . . ? C13 C14 C15 C16 -177.4(13) . . . . ? C14 C15 C16 C17 4(2) . . . . ? C15 C16 C17 C18 -2(2) . . . . ? C16 C17 C18 C19 -2.1(15) . . . . ? C16 C17 C18 C20 175.6(11) . . . . ? C15 C14 C19 O4 178.9(9) . . . . ? C13 C14 C19 O4 -6.9(14) . . . . ? C15 C14 C19 C18 -1.2(13) . . . . ? C13 C14 C19 C18 173.0(8) . . . . ? C17 C18 C19 O4 -176.6(7) . . . . ? C20 C18 C19 O4 5.9(10) . . . . ? C17 C18 C19 C14 3.6(11) . . . . ? C20 C18 C19 C14 -174.0(7) . . . . ? C17 C18 C20 O5 16.6(11) . . . . ? C19 C18 C20 O5 -165.8(8) . . . . ? C17 C18 C20 O6 -161.7(7) . . . . ? C19 C18 C20 O6 15.9(10) . . . . ? N2 C21 C22 N4 -55.7(8) . . . . ? C31 C24 C25 C26 176.3(7) . . . . ? C29 C24 C25 C26 0.0(11) . . . . ? C24 C25 C26 C27 -2.5(12) . . . . ? C25 C26 C27 C28 1.0(11) . . . . ? C26 C27 C28 C29 2.8(10) . . . . ? C26 C27 C28 C30 -179.5(6) . . . . ? C27 C28 C29 O8 173.0(5) . . . . ? C30 C28 C29 O8 -4.6(8) . . . . ? C27 C28 C29 C24 -5.2(8) . . . . ? C30 C28 C29 C24 177.2(5) . . . . ? C25 C24 C29 O8 -174.4(5) . . . . ? C31 C24 C29 O8 9.6(9) . . . . ? C25 C24 C29 C28 3.8(8) . . . . ? C31 C24 C29 C28 -172.2(6) . . . . ? C27 C28 C30 O10 -17.4(9) . . . . ? C29 C28 C30 O10 160.2(6) . . . . ? C27 C28 C30 O9 161.8(6) . . . . ? C29 C28 C30 O9 -20.6(9) . . . . ? C5 C8 N1 C9 -174.8(8) . . . . ? C5 C8 N1 Ni1 -3.7(12) . . . . ? C10 C9 N1 C8 -158.7(7) . . . . ? C10 C9 N1 Ni1 29.2(8) . . . . ? O12 Ni1 N1 C8 83.0(9) . . . . ? N4 Ni1 N1 C8 -95.0(7) . . . . ? O1 Ni1 N1 C8 8.2(7) . . . . ? N2 Ni1 N1 C8 -178.3(7) . . . . ? O12 Ni1 N1 C9 -105.8(7) . . . . ? N4 Ni1 N1 C9 76.2(6) . . . . ? O1 Ni1 N1 C9 179.5(5) . . . . ? N2 Ni1 N1 C9 -7.0(5) . . . . ? C12 C11 N2 C21 -171.9(5) . . . . ? C12 C11 N2 C10 -51.3(7) . . . . ? C12 C11 N2 Ni1 70.7(6) . . . . ? C22 C21 N2 C11 -91.5(6) . . . . ? C22 C21 N2 C10 146.4(6) . . . . ? C22 C21 N2 Ni1 33.4(6) . . . . ? C9 C10 N2 C11 164.2(6) . . . . ? C9 C10 N2 C21 -75.0(7) . . . . ? C9 C10 N2 Ni1 36.6(7) . . . . ? N1 Ni1 N2 C11 -140.9(5) . . . . ? O12 Ni1 N2 C11 20.8(5) . . . . ? N4 Ni1 N2 C11 114.5(5) . . . . ? N1 Ni1 N2 C21 98.8(4) . . . . ? O12 Ni1 N2 C21 -99.5(4) . . . . ? N4 Ni1 N2 C21 -5.7(4) . . . . ? N1 Ni1 N2 C10 -16.3(5) . . . . ? O12 Ni1 N2 C10 145.5(4) . . . . ? N4 Ni1 N2 C10 -120.8(5) . . . . ? C14 C13 N3 C12 -174.6(9) . . . . ? C14 C13 N3 Ni2 16.2(13) . . . . ? C11 C12 N3 C13 121.5(8) . . . . ? C11 C12 N3 Ni2 -68.8(7) . . . . ? O4 Ni2 N3 C13 -22.0(7) . . . . ? O8 Ni2 N3 C13 -44.9(13) . . . . ? O12 Ni2 N3 C13 -105.6(7) . . . . ? O7 Ni2 N3 C13 159.2(7) . . . . ? O1W Ni2 N3 C13 71.3(7) . . . . ? Eu1 Ni2 N3 C13 -60.6(7) . . . . ? O4 Ni2 N3 C12 168.9(5) . . . . ? O8 Ni2 N3 C12 146.0(8) . . . . ? O12 Ni2 N3 C12 85.4(5) . . . . ? O7 Ni2 N3 C12 -9.8(5) . . . . ? O1W Ni2 N3 C12 -97.7(5) . . . . ? Eu1 Ni2 N3 C12 130.3(5) . . . . ? C21 C22 N4 Ni1 46.5(6) . . . . ? N1 Ni1 N4 C22 -103.0(4) . . . . ? O12 Ni1 N4 C22 77.6(4) . . . . ? O1 Ni1 N4 C22 163.2(4) . . . . ? N2 Ni1 N4 C22 -21.7(4) . . . . ? C25 C24 C31 O7 178.8(7) . . . . ? C29 C24 C31 O7 -5.1(11) . . . . ? C1 C6 O1 Ni1 -165.0(4) . . . . ? C5 C6 O1 Ni1 15.8(8) . . . . ? C1 C6 O1 Eu1 22.6(8) . . . . ? C5 C6 O1 Eu1 -156.7(4) . . . . ? N1 Ni1 O1 C6 -14.7(5) . . . . ? O12 Ni1 O1 C6 -177.0(5) . . . . ? N4 Ni1 O1 C6 89.5(5) . . . . ? N1 Ni1 O1 Eu1 159.3(2) . . . . ? O12 Ni1 O1 Eu1 -3.06(15) . . . . ? N4 Ni1 O1 Eu1 -96.5(2) . . . . ? O6 Eu1 O1 C6 33.5(5) . . . . ? O9 Eu1 O1 C6 -29.1(7) . . . . ? O2 Eu1 O1 C6 -45.1(5) . . . . ? O8 Eu1 O1 C6 149.8(4) . . . . ? O2 Eu1 O1 C6 -111.1(5) 3_576 . . . ? O12 Eu1 O1 C6 176.6(5) . . . . ? Ni2 Eu1 O1 C6 142.4(5) . . . . ? Eu1 Eu1 O1 C6 -79.7(5) 3_576 . . . ? O6 Eu1 O1 Ni1 -140.42(18) . . . . ? O9 Eu1 O1 Ni1 157.1(3) . . . . ? O2 Eu1 O1 Ni1 140.97(19) . . . . ? O8 Eu1 O1 Ni1 -24.0(2) . . . . ? O2 Eu1 O1 Ni1 75.03(17) 3_576 . . . ? O12 Eu1 O1 Ni1 2.68(14) . . . . ? Ni2 Eu1 O1 Ni1 -31.45(14) . . . . ? Eu1 Eu1 O1 Ni1 106.39(14) 3_576 . . . ? O3 C7 O2 Eu1 125.1(5) . . . . ? C1 C7 O2 Eu1 -59.2(6) . . . . ? O3 C7 O2 Eu1 -72.3(6) . . . 3_576 ? C1 C7 O2 Eu1 103.4(5) . . . 3_576 ? O6 Eu1 O2 C7 -29.2(4) . . . . ? O9 Eu1 O2 C7 -111.8(4) . . . . ? O8 Eu1 O2 C7 -147.3(4) . . . . ? O1 Eu1 O2 C7 62.5(4) . . . . ? O2 Eu1 O2 C7 165.0(5) 3_576 . . . ? O12 Eu1 O2 C7 108.7(4) . . . . ? Ni2 Eu1 O2 C7 84.0(4) . . . . ? Eu1 Eu1 O2 C7 165.0(5) 3_576 . . . ? O6 Eu1 O2 Eu1 165.85(19) . . . 3_576 ? O9 Eu1 O2 Eu1 83.19(16) . . . 3_576 ? O8 Eu1 O2 Eu1 47.7(4) . . . 3_576 ? O1 Eu1 O2 Eu1 -102.46(17) . . . 3_576 ? O2 Eu1 O2 Eu1 0.0 3_576 . . 3_576 ? O12 Eu1 O2 Eu1 -56.27(19) . . . 3_576 ? Ni2 Eu1 O2 Eu1 -81.0(3) . . . 3_576 ? C14 C19 O4 Ni2 -9.3(10) . . . . ? C18 C19 O4 Ni2 170.8(4) . . . . ? N3 Ni2 O4 C19 20.1(5) . . . . ? O8 Ni2 O4 C19 -164.4(5) . . . . ? O12 Ni2 O4 C19 112.6(5) . . . . ? O7 Ni2 O4 C19 -165.9(8) . . . . ? O1W Ni2 O4 C19 -69.1(5) . . . . ? Eu1 Ni2 O4 C19 152.5(6) . . . . ? O5 C20 O6 Eu1 -176.3(6) . . . . ? C18 C20 O6 Eu1 2.0(10) . . . . ? O9 Eu1 O6 C20 -142.0(7) . . . . ? O2 Eu1 O6 C20 125.7(7) . . . . ? O8 Eu1 O6 C20 -76.4(7) . . . . ? O1 Eu1 O6 C20 56.5(6) . . . . ? O2 Eu1 O6 C20 148.9(6) 3_576 . . . ? O12 Eu1 O6 C20 2.3(7) . . . . ? Ni2 Eu1 O6 C20 -33.8(7) . . . . ? Eu1 Eu1 O6 C20 134.4(6) 3_576 . . . ? C24 C31 O7 Ni2 -8.6(10) . . . . ? O4 Ni2 O7 C31 14.0(12) . . . . ? N3 Ni2 O7 C31 -172.2(5) . . . . ? O8 Ni2 O7 C31 12.5(5) . . . . ? O12 Ni2 O7 C31 94.4(5) . . . . ? O1W Ni2 O7 C31 -83.4(5) . . . . ? Eu1 Ni2 O7 C31 50.0(5) . . . . ? C28 C29 O8 Ni2 -178.0(4) . . . . ? C24 C29 O8 Ni2 0.1(7) . . . . ? C28 C29 O8 Eu1 45.8(7) . . . . ? C24 C29 O8 Eu1 -136.1(4) . . . . ? O4 Ni2 O8 C29 171.4(5) . . . . ? N3 Ni2 O8 C29 -165.3(9) . . . . ? O12 Ni2 O8 C29 -103.8(5) . . . . ? O7 Ni2 O8 C29 -8.9(5) . . . . ? O1W Ni2 O8 C29 79.0(5) . . . . ? Eu1 Ni2 O8 C29 -147.3(5) . . . . ? O4 Ni2 O8 Eu1 -41.34(14) . . . . ? N3 Ni2 O8 Eu1 -18.1(10) . . . . ? O12 Ni2 O8 Eu1 43.50(13) . . . . ? O7 Ni2 O8 Eu1 138.36(15) . . . . ? O1W Ni2 O8 Eu1 -133.73(15) . . . . ? O6 Eu1 O8 C29 -116.9(4) . . . . ? O9 Eu1 O8 C29 -43.1(4) . . . . ? O2 Eu1 O8 C29 -5.1(6) . . . . ? O1 Eu1 O8 C29 137.3(4) . . . . ? O2 Eu1 O8 C29 38.8(4) 3_576 . . . ? O12 Eu1 O8 C29 110.3(4) . . . . ? Ni2 Eu1 O8 C29 148.9(5) . . . . ? Eu1 Eu1 O8 C29 26.9(4) 3_576 . . . ? O6 Eu1 O8 Ni2 94.26(17) . . . . ? O9 Eu1 O8 Ni2 167.98(18) . . . . ? O2 Eu1 O8 Ni2 -154.0(2) . . . . ? O1 Eu1 O8 Ni2 -11.6(2) . . . . ? O2 Eu1 O8 Ni2 -110.12(14) 3_576 . . . ? O12 Eu1 O8 Ni2 -38.60(12) . . . . ? Eu1 Eu1 O8 Ni2 -122.02(10) 3_576 . . . ? O10 C30 O9 Eu1 -176.8(5) . . . . ? C28 C30 O9 Eu1 4.0(9) . . . . ? O6 Eu1 O9 C30 134.8(6) . . . . ? O2 Eu1 O9 C30 -146.9(6) . . . . ? O8 Eu1 O9 C30 19.0(6) . . . . ? O1 Eu1 O9 C30 -161.9(5) . . . . ? O2 Eu1 O9 C30 -78.2(6) 3_576 . . . ? O12 Eu1 O9 C30 -13.6(7) . . . . ? Ni2 Eu1 O9 C30 27.1(6) . . . . ? Eu1 Eu1 O9 C30 -112.3(6) 3_576 . . . ? N1 Ni1 O12 Ni2 23.7(7) . . . . ? N4 Ni1 O12 Ni2 -158.2(2) . . . . ? O1 Ni1 O12 Ni2 99.4(2) . . . . ? N2 Ni1 O12 Ni2 -72.4(2) . . . . ? N1 Ni1 O12 Eu1 -72.7(6) . . . . ? N4 Ni1 O12 Eu1 105.39(19) . . . . ? O1 Ni1 O12 Eu1 3.06(15) . . . . ? N2 Ni1 O12 Eu1 -168.73(18) . . . . ? O4 Ni2 O12 Ni1 -67.4(2) . . . . ? N3 Ni2 O12 Ni1 21.2(2) . . . . ? O8 Ni2 O12 Ni1 -148.5(2) . . . . ? O7 Ni2 O12 Ni1 123.9(2) . . . . ? Eu1 Ni2 O12 Ni1 -105.4(2) . . . . ? O4 Ni2 O12 Eu1 38.09(14) . . . . ? N3 Ni2 O12 Eu1 126.66(17) . . . . ? O8 Ni2 O12 Eu1 -43.10(12) . . . . ? O7 Ni2 O12 Eu1 -130.66(14) . . . . ? O6 Eu1 O12 Ni1 57.9(2) . . . . ? O9 Eu1 O12 Ni1 -171.21(15) . . . . ? O2 Eu1 O12 Ni1 -49.27(19) . . . . ? O8 Eu1 O12 Ni1 155.41(19) . . . . ? O1 Eu1 O12 Ni1 -2.78(14) . . . . ? O2 Eu1 O12 Ni1 -102.77(16) 3_576 . . . ? Ni2 Eu1 O12 Ni1 117.3(2) . . . . ? Eu1 Eu1 O12 Ni1 -78.03(13) 3_576 . . . ? O6 Eu1 O12 Ni2 -59.4(2) . . . . ? O9 Eu1 O12 Ni2 71.5(2) . . . . ? O2 Eu1 O12 Ni2 -166.58(11) . . . . ? O8 Eu1 O12 Ni2 38.09(12) . . . . ? O1 Eu1 O12 Ni2 -120.09(16) . . . . ? O2 Eu1 O12 Ni2 139.92(15) 3_576 . . . ? Eu1 Eu1 O12 Ni2 164.66(9) 3_576 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O10 0.90 2.58 3.319(7) 139.3 3_576 N4 H4B O9 0.90 2.54 3.099(7) 121.2 3_576 O1W H1WA O5W 0.85 2.05 2.811(9) 148.4 1_565 O1W H1WB O3W 0.85 1.92 2.656(7) 143.4 1_565 O12 H12 O3 0.98 2.12 2.983(6) 146.1 3_576 O2W H2WA O3W 0.85 1.94 2.723(9) 151.8 . O2W H2WB O5 0.85 1.83 2.676(8) 170.6 1_645 O3W H3WA O2W 0.85 1.96 2.723(9) 149.1 . O4W H4WA O2W 0.85 2.60 3.199(11) 128.8 2_656 O4W H4WB O5 0.85 2.62 3.337(12) 142.2 2_546 O5W H5WA O1W 0.85 2.28 2.811(9) 120.7 1_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.935 _refine_diff_density_min -1.419 _refine_diff_density_rms 0.234 data_1813 _database_code_depnum_ccdc_archive 'CCDC 898021' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 N8 Ni4 O24 Tb2, 8(H2 O)' _chemical_formula_sum 'C60 H74 N8 Ni4 O32 Tb2' _chemical_formula_weight 1971.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6435(13) _cell_length_b 18.3018(19) _cell_length_c 15.4157(16) _cell_angle_alpha 90.00 _cell_angle_beta 96.424(2) _cell_angle_gamma 90.00 _cell_volume 3544.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5068 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 25.70 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 3.104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4561 _exptl_absorpt_correction_T_max 0.7071 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18031 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6232 _reflns_number_gt 4985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+2.3046P] 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 6232 _refine_ls_number_parameters 496 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.085 _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 Tb1 Tb 0.57899(2) 1.051608(15) 0.099155(18) 0.02477(11) Uani 1 1 d . . . N1 N 0.7851(4) 0.8264(3) 0.2562(4) 0.0407(13) Uani 1 1 d . . . N2 N 0.6370(4) 0.8147(3) 0.1028(4) 0.0443(14) Uani 1 1 d . . . H2A H 0.5895 0.7794 0.1109 0.053 Uiso 1 1 calc R . . H2B H 0.6168 0.8372 0.0517 0.053 Uiso 1 1 calc R . . N3 N 0.5797(4) 0.8368(3) 0.2949(4) 0.0440(14) Uani 1 1 d . . . N4 N 0.8175(5) 0.9782(3) 0.3182(4) 0.0438(14) Uani 1 1 d . . . Ni2 Ni 0.80369(6) 1.04185(4) 0.20976(5) 0.02955(19) Uani 1 1 d . . . Ni3 Ni 0.64703(6) 0.88780(4) 0.20319(5) 0.0307(2) Uani 1 1 d . . . O1 O 0.5142(3) 0.9499(2) 0.1749(3) 0.0305(9) Uani 1 1 d . . . O2 O 0.4088(3) 1.0166(2) 0.0325(2) 0.0283(9) Uani 1 1 d . . . O3 O 0.2449(3) 1.0542(2) 0.0462(3) 0.0386(11) Uani 1 1 d . . . O4 O 0.6594(3) 1.0721(2) 0.2391(3) 0.0353(10) Uani 1 1 d . . . O5 O 0.4691(3) 1.1240(3) 0.1708(3) 0.0458(12) Uani 1 1 d . . . O6 O 0.3884(5) 1.1883(5) 0.2613(5) 0.108(2) Uani 1 1 d U . . O7 O 0.9425(3) 1.0231(2) 0.1569(3) 0.0394(11) Uani 1 1 d . . . O8 O 0.7530(3) 1.1029(2) 0.1027(3) 0.0298(9) Uani 1 1 d . . . O9 O 0.5739(3) 1.1528(2) 0.0082(3) 0.0410(11) Uani 1 1 d . . . O10 O 0.6024(4) 1.2447(3) -0.0783(3) 0.0554(14) Uani 1 1 d . . . O11 O 0.7174(3) 0.9635(2) 0.1379(2) 0.0277(9) Uani 1 1 d . . . H11 H 0.7515 0.9447 0.0884 0.033 Uiso 1 1 calc R . . O1W O 0.8856(4) 1.1234(3) 0.2848(3) 0.0509(12) Uani 1 1 d . . . H1WA H 0.9419 1.1421 0.2689 0.061 Uiso 1 1 d R . . H1WB H 0.8947 1.1252 0.3402 0.061 Uiso 1 1 d R . . C1 C 0.7876(6) 0.7635(4) 0.1962(5) 0.0500(18) Uani 1 1 d . . . H1A H 0.7453 0.7240 0.2162 0.060 Uiso 1 1 calc R . . H1B H 0.8603 0.7463 0.1972 0.060 Uiso 1 1 calc R . . C2 C 0.7449(5) 0.7834(4) 0.1033(5) 0.0498(18) Uani 1 1 d . . . H2C H 0.7916 0.8188 0.0802 0.060 Uiso 1 1 calc R . . H2D H 0.7422 0.7402 0.0666 0.060 Uiso 1 1 calc R . . C3 C 0.7617(6) 0.7994(4) 0.3436(5) 0.056(2) Uani 1 1 d . . . H3A H 0.7798 0.8370 0.3871 0.067 Uiso 1 1 calc R . . H3B H 0.8049 0.7567 0.3597 0.067 Uiso 1 1 calc R . . C4 C 0.6455(6) 0.7800(5) 0.3419(5) 0.059(2) Uani 1 1 d . . . H4A H 0.6320 0.7332 0.3131 0.071 Uiso 1 1 calc R . . H4B H 0.6271 0.7758 0.4011 0.071 Uiso 1 1 calc R . . C5 C 0.4823(6) 0.8433(4) 0.3103(5) 0.0521(19) Uani 1 1 d . . . H5 H 0.4611 0.8135 0.3541 0.062 Uiso 1 1 calc R . . C6 C 0.4030(5) 0.8906(4) 0.2687(4) 0.0422(16) Uani 1 1 d . . . C7 C 0.3036(6) 0.8862(5) 0.2993(5) 0.061(2) Uani 1 1 d . . . H7 H 0.2944 0.8540 0.3445 0.073 Uiso 1 1 calc R . . C8 C 0.2183(6) 0.9283(5) 0.2647(5) 0.062(2) Uani 1 1 d . . . H8 H 0.1538 0.9268 0.2884 0.074 Uiso 1 1 calc R . . C9 C 0.2312(5) 0.9726(4) 0.1940(5) 0.0465(18) Uani 1 1 d . . . H9 H 0.1735 0.9997 0.1688 0.056 Uiso 1 1 calc R . . C10 C 0.3281(4) 0.9780(3) 0.1595(4) 0.0291(13) Uani 1 1 d . . . C11 C 0.3250(4) 1.0201(3) 0.0751(4) 0.0296(13) Uani 1 1 d . . . C12 C 0.4177(5) 0.9396(3) 0.1997(4) 0.0288(13) Uani 1 1 d . . . C13 C 0.8903(5) 0.8654(4) 0.2624(5) 0.0433(16) Uani 1 1 d . . . H13A H 0.9465 0.8296 0.2753 0.052 Uiso 1 1 calc R . . H13B H 0.8987 0.8863 0.2058 0.052 Uiso 1 1 calc R . . C14 C 0.9052(6) 0.9248(4) 0.3295(5) 0.0528(19) Uani 1 1 d . . . H14A H 0.9087 0.9035 0.3874 0.063 Uiso 1 1 calc R . . H14B H 0.9721 0.9497 0.3248 0.063 Uiso 1 1 calc R . . C15 C 0.7647(7) 0.9911(5) 0.3839(5) 0.062(2) Uani 1 1 d . . . H15 H 0.7878 0.9665 0.4354 0.074 Uiso 1 1 calc R . . C16 C 0.6742(9) 1.0391(5) 0.3871(5) 0.072(3) Uani 1 1 d U . . C17 C 0.6300(10) 1.0452(6) 0.4676(7) 0.101(3) Uani 1 1 d U . . H17 H 0.6642 1.0218 0.5165 0.121 Uiso 1 1 calc R . . C18 C 0.5403(10) 1.0836(6) 0.4763(7) 0.104(3) Uani 1 1 d U . . H18 H 0.5155 1.0878 0.5306 0.125 Uiso 1 1 calc R . . C19 C 0.4866(9) 1.1160(6) 0.4051(6) 0.092(3) Uani 1 1 d U . . H19 H 0.4248 1.1422 0.4109 0.110 Uiso 1 1 calc R . . C20 C 0.5242(6) 1.1101(4) 0.3222(5) 0.0498(19) Uani 1 1 d . . . C21 C 0.4577(5) 1.1431(4) 0.2466(5) 0.053(2) Uani 1 1 d . . . C22 C 0.6189(6) 1.0738(4) 0.3138(4) 0.0400(16) Uani 1 1 d . . . C23 C 0.9707(5) 1.0571(4) 0.0934(5) 0.0394(16) Uani 1 1 d . . . H23 H 1.0402 1.0480 0.0819 0.047 Uiso 1 1 calc R . . C24 C 0.9135(5) 1.1079(3) 0.0351(4) 0.0359(15) Uani 1 1 d . . . C25 C 0.9680(5) 1.1374(4) -0.0309(5) 0.0518(19) Uani 1 1 d . . . H25 H 1.0391 1.1254 -0.0331 0.062 Uiso 1 1 calc R . . C26 C 0.9179(6) 1.1838(5) -0.0922(5) 0.059(2) Uani 1 1 d . . . H26 H 0.9554 1.2045 -0.1346 0.071 Uiso 1 1 calc R . . C27 C 0.8115(5) 1.1994(4) -0.0906(4) 0.0448(17) Uani 1 1 d . . . H27 H 0.7784 1.2301 -0.1334 0.054 Uiso 1 1 calc R . . C28 C 0.7510(5) 1.1716(3) -0.0281(4) 0.0307(13) Uani 1 1 d . . . C29 C 0.6364(5) 1.1913(3) -0.0333(4) 0.0341(14) Uani 1 1 d . . . C30 C 0.8035(5) 1.1258(3) 0.0390(4) 0.0283(13) Uani 1 1 d . . . O2W O 0.4362(6) 0.2745(3) 0.0811(4) 0.101(2) Uani 1 1 d . . . H2WA H 0.3728 0.2591 0.0699 0.121 Uiso 1 1 d R . . H2WB H 0.4574 0.2568 0.1310 0.121 Uiso 1 1 d R . . O3W O 0.2140(5) 0.1877(4) 0.1436(4) 0.093(2) Uani 1 1 d . . . H3WA H 0.2710 0.1858 0.1785 0.111 Uiso 1 1 d R . . H3WB H 0.2095 0.1459 0.1195 0.111 Uiso 1 1 d R . . O4W O 0.0775(7) 0.1759(6) 0.2649(6) 0.060(3) Uani 0.50 1 d PU . . H4WA H 0.1065 0.2023 0.3063 0.073 Uiso 0.50 1 d PR . . H4WB H 0.1291 0.1536 0.2457 0.073 Uiso 0.50 1 d PR . . O5W O 0.9240(9) 0.1121(6) 0.4679(6) 0.078(4) Uani 0.50 1 d P . . H5WA H 0.8971 0.1226 0.5145 0.093 Uiso 0.50 1 d PR . . H5WB H 0.9823 0.0909 0.4854 0.093 Uiso 0.50 1 d PR . . O6W O 0.9031(10) 0.9706(7) 0.5731(8) 0.101(4) Uani 0.60 1 d P A 1 H6WA H 0.9573 0.9477 0.5594 0.122 Uiso 0.60 1 d PR A 1 H6WB H 0.8606 0.9372 0.5857 0.122 Uiso 0.60 1 d PR A 1 O7W O 0.7783(17) 0.8768(10) 0.5820(12) 0.115(7) Uani 0.40 1 d P B 2 H7WA H 0.8355 0.8834 0.5588 0.138 Uiso 0.40 1 d PR B 2 H7WB H 0.7290 0.8845 0.5409 0.138 Uiso 0.40 1 d PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02231(16) 0.02303(17) 0.02863(17) 0.00144(12) 0.00132(11) 0.00199(12) N1 0.040(3) 0.034(3) 0.049(3) 0.013(3) 0.007(2) 0.009(3) N2 0.035(3) 0.039(3) 0.059(4) -0.004(3) 0.002(3) 0.006(3) N3 0.048(3) 0.040(3) 0.045(3) 0.021(3) 0.011(3) 0.014(3) N4 0.052(4) 0.042(3) 0.035(3) -0.001(3) -0.006(3) 0.007(3) Ni2 0.0277(4) 0.0306(4) 0.0290(4) 0.0000(3) -0.0028(3) 0.0015(3) Ni3 0.0307(4) 0.0268(4) 0.0349(4) 0.0065(3) 0.0044(3) 0.0063(3) O1 0.025(2) 0.030(2) 0.036(2) 0.0097(18) 0.0031(17) 0.0029(18) O2 0.022(2) 0.031(2) 0.032(2) 0.0031(18) 0.0028(17) 0.0029(17) O3 0.029(2) 0.051(3) 0.036(2) 0.003(2) 0.0020(19) 0.009(2) O4 0.031(2) 0.045(3) 0.030(2) -0.009(2) 0.0055(18) 0.002(2) O5 0.038(3) 0.041(3) 0.060(3) -0.008(2) 0.013(2) 0.007(2) O6 0.089(4) 0.127(4) 0.102(4) -0.050(4) -0.007(3) 0.045(3) O7 0.030(2) 0.043(3) 0.044(3) 0.005(2) 0.002(2) 0.010(2) O8 0.022(2) 0.033(2) 0.034(2) 0.0089(19) 0.0018(17) 0.0011(18) O9 0.029(2) 0.040(3) 0.053(3) 0.017(2) 0.000(2) -0.001(2) O10 0.047(3) 0.048(3) 0.073(4) 0.035(3) 0.012(2) 0.014(2) O11 0.028(2) 0.028(2) 0.027(2) 0.0013(17) 0.0034(17) 0.0051(17) O1W 0.045(3) 0.047(3) 0.058(3) -0.012(2) -0.008(2) -0.004(2) C1 0.048(4) 0.034(4) 0.068(5) 0.001(4) 0.011(4) 0.006(3) C2 0.049(4) 0.050(4) 0.053(4) -0.008(4) 0.013(3) 0.010(4) C3 0.049(4) 0.057(5) 0.060(5) 0.028(4) -0.002(4) 0.013(4) C4 0.057(5) 0.067(5) 0.057(5) 0.031(4) 0.022(4) 0.029(4) C5 0.057(5) 0.047(4) 0.055(5) 0.022(4) 0.019(4) 0.011(4) C6 0.037(4) 0.049(4) 0.043(4) 0.012(3) 0.015(3) 0.008(3) C7 0.055(5) 0.075(6) 0.058(5) 0.033(4) 0.023(4) 0.007(4) C8 0.035(4) 0.089(6) 0.064(5) 0.031(5) 0.021(4) 0.010(4) C9 0.030(3) 0.068(5) 0.043(4) 0.010(4) 0.012(3) 0.007(3) C10 0.027(3) 0.030(3) 0.031(3) 0.002(3) 0.007(2) 0.004(3) C11 0.024(3) 0.029(3) 0.035(3) -0.008(3) 0.003(3) -0.005(3) C12 0.025(3) 0.031(3) 0.031(3) 0.000(3) 0.007(2) 0.000(3) C13 0.034(4) 0.042(4) 0.053(4) 0.008(3) 0.000(3) 0.010(3) C14 0.051(4) 0.055(5) 0.048(4) 0.007(4) -0.012(3) 0.012(4) C15 0.095(6) 0.058(5) 0.032(4) 0.008(4) 0.002(4) 0.018(5) C16 0.120(7) 0.060(5) 0.040(4) 0.002(4) 0.030(4) 0.032(5) C17 0.155(7) 0.100(6) 0.055(5) 0.018(4) 0.041(5) 0.044(6) C18 0.157(7) 0.102(6) 0.065(5) 0.011(5) 0.066(5) 0.047(6) C19 0.132(8) 0.083(6) 0.071(6) -0.001(5) 0.061(6) 0.030(6) C20 0.053(4) 0.043(4) 0.058(5) -0.011(4) 0.023(4) -0.004(4) C21 0.034(4) 0.048(4) 0.078(6) -0.036(4) 0.009(4) 0.010(3) C22 0.057(4) 0.031(3) 0.034(4) -0.005(3) 0.014(3) 0.002(3) C23 0.024(3) 0.047(4) 0.047(4) 0.002(3) 0.005(3) 0.008(3) C24 0.030(3) 0.034(3) 0.044(4) -0.001(3) 0.007(3) 0.000(3) C25 0.032(4) 0.063(5) 0.063(5) 0.013(4) 0.017(3) 0.002(4) C26 0.051(5) 0.068(5) 0.064(5) 0.025(4) 0.032(4) 0.011(4) C27 0.052(4) 0.044(4) 0.037(4) 0.009(3) 0.003(3) 0.002(3) C28 0.033(3) 0.026(3) 0.033(3) 0.004(3) 0.004(3) -0.003(3) C29 0.037(3) 0.027(3) 0.039(4) 0.005(3) 0.004(3) 0.001(3) C30 0.031(3) 0.022(3) 0.032(3) -0.005(3) 0.004(3) -0.004(3) O2W 0.143(6) 0.062(4) 0.088(5) -0.002(4) -0.027(4) 0.009(4) O3W 0.090(5) 0.089(5) 0.096(5) -0.034(4) -0.006(4) 0.031(4) O4W 0.031(4) 0.078(6) 0.078(6) -0.065(5) 0.031(4) -0.038(4) O5W 0.096(8) 0.091(9) 0.033(6) -0.038(6) -0.044(5) 0.054(7) O6W 0.111(10) 0.098(9) 0.091(9) -0.009(7) -0.009(7) 0.040(8) O7W 0.154(19) 0.086(13) 0.101(14) 0.002(11) -0.004(12) 0.049(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O5 2.292(4) . ? Tb1 O4 2.310(4) . ? Tb1 O9 2.320(4) . ? Tb1 O2 2.367(4) . ? Tb1 O8 2.387(4) . ? Tb1 O1 2.390(4) . ? Tb1 O2 2.403(4) 3_675 ? Tb1 O11 2.406(4) . ? N1 C1 1.480(9) . ? N1 C3 1.495(8) . ? N1 C13 1.502(8) . ? N1 Ni3 2.158(5) . ? N2 C2 1.479(8) . ? N2 Ni3 2.038(6) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C5 1.287(8) . ? N3 C4 1.470(8) . ? N3 Ni3 1.966(5) . ? N4 C15 1.295(9) . ? N4 C14 1.474(9) . ? N4 Ni2 2.029(6) . ? Ni2 O4 2.006(4) . ? Ni2 O8 2.036(4) . ? Ni2 O7 2.045(4) . ? Ni2 O11 2.050(4) . ? Ni2 O1W 2.091(5) . ? Ni3 O11 1.981(4) . ? Ni3 O1 2.035(4) . ? O1 C12 1.332(7) . ? O2 C11 1.309(7) . ? O2 Tb1 2.403(4) 3_675 ? O3 C11 1.230(7) . ? O4 C22 1.312(7) . ? O5 C21 1.242(8) . ? O6 C21 1.245(8) . ? O7 C23 1.245(8) . ? O8 C30 1.300(7) . ? O9 C29 1.282(7) . ? O10 C29 1.247(7) . ? O11 H11 0.9800 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? C1 C2 1.517(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.509(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.422(9) . ? C5 H5 0.9300 . ? C6 C7 1.393(9) . ? C6 C12 1.419(8) . ? C7 C8 1.383(11) . ? C7 H7 0.9300 . ? C8 C9 1.384(10) . ? C8 H8 0.9300 . ? C9 C10 1.392(8) . ? C9 H9 0.9300 . ? C10 C12 1.415(8) . ? C10 C11 1.510(8) . ? C13 C14 1.499(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.448(12) . ? C15 H15 0.9300 . ? C16 C22 1.412(11) . ? C16 C17 1.421(12) . ? C17 C18 1.354(14) . ? C17 H17 0.9300 . ? C18 C19 1.359(15) . ? C18 H18 0.9300 . ? C19 C20 1.416(10) . ? C19 H19 0.9300 . ? C20 C22 1.387(9) . ? C20 C21 1.487(11) . ? C23 C24 1.432(9) . ? C23 H23 0.9300 . ? C24 C25 1.398(9) . ? C24 C30 1.438(8) . ? C25 C26 1.372(10) . ? C25 H25 0.9300 . ? C26 C27 1.378(9) . ? C26 H26 0.9300 . ? C27 C28 1.391(8) . ? C27 H27 0.9300 . ? C28 C30 1.435(8) . ? C28 C29 1.487(8) . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8500 . ? O7W H7WA 0.8500 . ? O7W H7WB 0.8500 . ? 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 O5 Tb1 O4 71.53(16) . . ? O5 Tb1 O9 81.50(16) . . ? O4 Tb1 O9 114.50(16) . . ? O5 Tb1 O2 78.16(15) . . ? O4 Tb1 O2 137.11(13) . . ? O9 Tb1 O2 89.50(14) . . ? O5 Tb1 O8 111.61(15) . . ? O4 Tb1 O8 66.84(14) . . ? O9 Tb1 O8 70.31(13) . . ? O2 Tb1 O8 155.15(13) . . ? O5 Tb1 O1 87.43(15) . . ? O4 Tb1 O1 78.98(15) . . ? O9 Tb1 O1 158.31(14) . . ? O2 Tb1 O1 69.91(14) . . ? O8 Tb1 O1 131.34(13) . . ? O5 Tb1 O2 143.87(15) . 3_675 ? O4 Tb1 O2 144.09(13) . 3_675 ? O9 Tb1 O2 84.52(14) . 3_675 ? O2 Tb1 O2 68.54(14) . 3_675 ? O8 Tb1 O2 94.46(13) . 3_675 ? O1 Tb1 O2 93.80(13) . 3_675 ? O5 Tb1 O11 137.02(15) . . ? O4 Tb1 O11 69.20(14) . . ? O9 Tb1 O11 130.98(14) . . ? O2 Tb1 O11 121.82(13) . . ? O8 Tb1 O11 67.36(13) . . ? O1 Tb1 O11 68.67(13) . . ? O2 Tb1 O11 75.37(13) 3_675 . ? O5 Tb1 Tb1 111.66(12) . 3_675 ? O4 Tb1 Tb1 159.02(11) . 3_675 ? O9 Tb1 Tb1 86.36(11) . 3_675 ? O2 Tb1 Tb1 34.56(9) . 3_675 ? O8 Tb1 Tb1 126.32(10) . 3_675 ? O1 Tb1 Tb1 80.45(10) . 3_675 ? O2 Tb1 Tb1 33.98(9) 3_675 3_675 ? O11 Tb1 Tb1 99.36(9) . 3_675 ? C1 N1 C3 109.1(6) . . ? C1 N1 C13 109.1(5) . . ? C3 N1 C13 111.3(5) . . ? C1 N1 Ni3 103.9(4) . . ? C3 N1 Ni3 106.3(4) . . ? C13 N1 Ni3 116.7(4) . . ? C2 N2 Ni3 105.8(4) . . ? C2 N2 H2A 110.6 . . ? Ni3 N2 H2A 110.6 . . ? C2 N2 H2B 110.6 . . ? Ni3 N2 H2B 110.6 . . ? H2A N2 H2B 108.7 . . ? C5 N3 C4 118.4(6) . . ? C5 N3 Ni3 126.1(5) . . ? C4 N3 Ni3 115.1(4) . . ? C15 N4 C14 118.3(6) . . ? C15 N4 Ni2 122.4(5) . . ? C14 N4 Ni2 118.2(5) . . ? O4 Ni2 N4 88.2(2) . . ? O4 Ni2 O8 79.60(16) . . ? N4 Ni2 O8 166.7(2) . . ? O4 Ni2 O7 168.21(18) . . ? N4 Ni2 O7 103.5(2) . . ? O8 Ni2 O7 88.61(16) . . ? O4 Ni2 O11 82.67(16) . . ? N4 Ni2 O11 92.0(2) . . ? O8 Ni2 O11 81.15(16) . . ? O7 Ni2 O11 95.48(17) . . ? O4 Ni2 O1W 94.87(18) . . ? N4 Ni2 O1W 87.8(2) . . ? O8 Ni2 O1W 98.49(18) . . ? O7 Ni2 O1W 86.94(19) . . ? O11 Ni2 O1W 177.54(17) . . ? N3 Ni3 O11 162.3(2) . . ? N3 Ni3 O1 90.36(19) . . ? O11 Ni3 O1 84.70(16) . . ? N3 Ni3 N2 103.8(2) . . ? O11 Ni3 N2 93.8(2) . . ? O1 Ni3 N2 102.97(19) . . ? N3 Ni3 N1 82.9(2) . . ? O11 Ni3 N1 99.55(18) . . ? O1 Ni3 N1 170.15(19) . . ? N2 Ni3 N1 85.7(2) . . ? C12 O1 Ni3 128.3(4) . . ? C12 O1 Tb1 128.7(3) . . ? Ni3 O1 Tb1 102.71(16) . . ? C11 O2 Tb1 121.1(4) . . ? C11 O2 Tb1 125.6(4) . 3_675 ? Tb1 O2 Tb1 111.46(14) . 3_675 ? C22 O4 Ni2 131.2(4) . . ? C22 O4 Tb1 130.5(4) . . ? Ni2 O4 Tb1 93.49(15) . . ? C21 O5 Tb1 139.1(5) . . ? C23 O7 Ni2 124.3(4) . . ? C30 O8 Ni2 130.8(4) . . ? C30 O8 Tb1 129.7(4) . . ? Ni2 O8 Tb1 90.49(14) . . ? C29 O9 Tb1 139.8(4) . . ? Ni3 O11 Ni2 117.18(19) . . ? Ni3 O11 Tb1 103.83(16) . . ? Ni2 O11 Tb1 89.61(14) . . ? Ni3 O11 H11 114.4 . . ? Ni2 O11 H11 114.4 . . ? Tb1 O11 H11 114.4 . . ? Ni2 O1W H1WA 120.4 . . ? Ni2 O1W H1WB 125.9 . . ? H1WA O1W H1WB 104.5 . . ? N1 C1 C2 111.9(6) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 109.1(5) . . ? N2 C2 H2C 109.9 . . ? C1 C2 H2C 109.9 . . ? N2 C2 H2D 109.9 . . ? C1 C2 H2D 109.9 . . ? H2C C2 H2D 108.3 . . ? N1 C3 C4 110.7(6) . . ? N1 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? N3 C4 C3 109.7(6) . . ? N3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 127.9(6) . . ? N3 C5 H5 116.0 . . ? C6 C5 H5 116.0 . . ? C7 C6 C12 119.3(6) . . ? C7 C6 C5 115.4(6) . . ? C12 C6 C5 125.3(6) . . ? C8 C7 C6 122.2(7) . . ? C8 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C7 C8 C9 118.3(7) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C8 C9 C10 121.9(7) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C9 C10 C12 119.6(6) . . ? C9 C10 C11 115.2(5) . . ? C12 C10 C11 125.0(5) . . ? O3 C11 O2 121.5(6) . . ? O3 C11 C10 120.9(5) . . ? O2 C11 C10 117.5(5) . . ? O1 C12 C10 121.2(5) . . ? O1 C12 C6 120.4(5) . . ? C10 C12 C6 118.4(5) . . ? C14 C13 N1 115.5(6) . . ? C14 C13 H13A 108.4 . . ? N1 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? N1 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? N4 C14 C13 111.4(6) . . ? N4 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? N4 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N4 C15 C16 128.0(7) . . ? N4 C15 H15 116.0 . . ? C16 C15 H15 116.0 . . ? C22 C16 C17 117.1(8) . . ? C22 C16 C15 124.6(7) . . ? C17 C16 C15 117.9(8) . . ? C18 C17 C16 122.9(10) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C17 C18 C19 119.7(9) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C19 C20 120.5(9) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C22 C20 C19 120.1(8) . . ? C22 C20 C21 122.6(6) . . ? C19 C20 C21 117.3(7) . . ? O5 C21 O6 121.1(8) . . ? O5 C21 C20 120.6(6) . . ? O6 C21 C20 118.3(7) . . ? O4 C22 C20 121.3(6) . . ? O4 C22 C16 119.0(6) . . ? C20 C22 C16 119.7(6) . . ? O7 C23 C24 130.5(6) . . ? O7 C23 H23 114.8 . . ? C24 C23 H23 114.8 . . ? C25 C24 C23 116.9(6) . . ? C25 C24 C30 120.0(6) . . ? C23 C24 C30 123.0(6) . . ? C26 C25 C24 120.9(6) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 119.5(6) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 123.4(6) . . ? C26 C27 H27 118.3 . . ? C28 C27 H27 118.3 . . ? C27 C28 C30 117.8(5) . . ? C27 C28 C29 118.8(5) . . ? C30 C28 C29 123.3(5) . . ? O10 C29 O9 121.0(6) . . ? O10 C29 C28 119.5(5) . . ? O9 C29 C28 119.5(5) . . ? O8 C30 C28 120.5(5) . . ? O8 C30 C24 121.2(5) . . ? C28 C30 C24 118.3(5) . . ? H2WA O2W H2WB 104.5 . . ? H3WA O3W H3WB 104.5 . . ? H4WA O4W H4WB 104.5 . . ? H5WA O5W H5WB 104.5 . . ? H6WA O6W H6WB 104.5 . . ? H7WA O7W H7WB 104.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 N4 Ni2 O4 -24.0(6) . . . . ? C14 N4 Ni2 O4 168.1(5) . . . . ? C15 N4 Ni2 O8 -47.8(12) . . . . ? C14 N4 Ni2 O8 144.3(8) . . . . ? C15 N4 Ni2 O7 157.3(6) . . . . ? C14 N4 Ni2 O7 -10.6(5) . . . . ? C15 N4 Ni2 O11 -106.6(6) . . . . ? C14 N4 Ni2 O11 85.5(5) . . . . ? C15 N4 Ni2 O1W 70.9(6) . . . . ? C14 N4 Ni2 O1W -96.9(5) . . . . ? C5 N3 Ni3 O11 81.0(10) . . . . ? C4 N3 Ni3 O11 -106.8(7) . . . . ? C5 N3 Ni3 O1 7.5(7) . . . . ? C4 N3 Ni3 O1 179.8(5) . . . . ? C5 N3 Ni3 N2 -95.9(7) . . . . ? C4 N3 Ni3 N2 76.3(6) . . . . ? C5 N3 Ni3 N1 -179.7(7) . . . . ? C4 N3 Ni3 N1 -7.5(5) . . . . ? C2 N2 Ni3 N3 -103.7(4) . . . . ? C2 N2 Ni3 O11 77.2(4) . . . . ? C2 N2 Ni3 O1 162.7(4) . . . . ? C2 N2 Ni3 N1 -22.1(4) . . . . ? C1 N1 Ni3 N3 99.0(4) . . . . ? C3 N1 Ni3 N3 -16.0(5) . . . . ? C13 N1 Ni3 N3 -140.7(5) . . . . ? C1 N1 Ni3 O11 -98.6(4) . . . . ? C3 N1 Ni3 O11 146.3(4) . . . . ? C13 N1 Ni3 O11 21.6(5) . . . . ? C1 N1 Ni3 N2 -5.5(4) . . . . ? C3 N1 Ni3 N2 -120.5(5) . . . . ? C13 N1 Ni3 N2 114.7(5) . . . . ? N3 Ni3 O1 C12 -14.0(5) . . . . ? O11 Ni3 O1 C12 -177.0(5) . . . . ? N2 Ni3 O1 C12 90.3(5) . . . . ? N3 Ni3 O1 Tb1 160.5(2) . . . . ? O11 Ni3 O1 Tb1 -2.51(16) . . . . ? N2 Ni3 O1 Tb1 -95.2(2) . . . . ? O5 Tb1 O1 C12 33.2(5) . . . . ? O4 Tb1 O1 C12 104.9(5) . . . . ? O9 Tb1 O1 C12 -25.9(7) . . . . ? O2 Tb1 O1 C12 -45.2(4) . . . . ? O8 Tb1 O1 C12 150.0(4) . . . . ? O2 Tb1 O1 C12 -110.7(5) 3_675 . . . ? O11 Tb1 O1 C12 176.7(5) . . . . ? Tb1 Tb1 O1 C12 -79.3(5) 3_675 . . . ? O5 Tb1 O1 Ni3 -141.27(19) . . . . ? O4 Tb1 O1 Ni3 -69.59(17) . . . . ? O9 Tb1 O1 Ni3 159.6(3) . . . . ? O2 Tb1 O1 Ni3 140.4(2) . . . . ? O8 Tb1 O1 Ni3 -24.4(3) . . . . ? O2 Tb1 O1 Ni3 74.90(17) 3_675 . . . ? O11 Tb1 O1 Ni3 2.21(14) . . . . ? Tb1 Tb1 O1 Ni3 106.26(15) 3_675 . . . ? O5 Tb1 O2 C11 -29.0(4) . . . . ? O4 Tb1 O2 C11 16.4(5) . . . . ? O9 Tb1 O2 C11 -110.4(4) . . . . ? O8 Tb1 O2 C11 -145.3(4) . . . . ? O1 Tb1 O2 C11 62.6(4) . . . . ? O2 Tb1 O2 C11 165.3(5) 3_675 . . . ? O11 Tb1 O2 C11 109.5(4) . . . . ? Tb1 Tb1 O2 C11 165.3(5) 3_675 . . . ? O5 Tb1 O2 Tb1 165.7(2) . . . 3_675 ? O4 Tb1 O2 Tb1 -148.82(18) . . . 3_675 ? O9 Tb1 O2 Tb1 84.31(17) . . . 3_675 ? O8 Tb1 O2 Tb1 49.5(4) . . . 3_675 ? O1 Tb1 O2 Tb1 -102.68(18) . . . 3_675 ? O2 Tb1 O2 Tb1 0.0 3_675 . . 3_675 ? O11 Tb1 O2 Tb1 -55.7(2) . . . 3_675 ? N4 Ni2 O4 C22 24.8(6) . . . . ? O8 Ni2 O4 C22 -160.7(6) . . . . ? O7 Ni2 O4 C22 -161.3(8) . . . . ? O11 Ni2 O4 C22 117.0(6) . . . . ? O1W Ni2 O4 C22 -62.9(6) . . . . ? N4 Ni2 O4 Tb1 -132.0(2) . . . . ? O8 Ni2 O4 Tb1 42.62(15) . . . . ? O7 Ni2 O4 Tb1 42.0(10) . . . . ? O11 Ni2 O4 Tb1 -39.68(15) . . . . ? O1W Ni2 O4 Tb1 140.38(18) . . . . ? O5 Tb1 O4 C22 40.4(5) . . . . ? O9 Tb1 O4 C22 111.6(5) . . . . ? O2 Tb1 O4 C22 -6.9(6) . . . . ? O8 Tb1 O4 C22 164.9(6) . . . . ? O1 Tb1 O4 C22 -50.5(5) . . . . ? O2 Tb1 O4 C22 -131.7(5) 3_675 . . . ? O11 Tb1 O4 C22 -121.7(5) . . . . ? Tb1 Tb1 O4 C22 -62.0(6) 3_675 . . . ? O5 Tb1 O4 Ni2 -162.6(2) . . . . ? O9 Tb1 O4 Ni2 -91.46(18) . . . . ? O2 Tb1 O4 Ni2 150.08(15) . . . . ? O8 Tb1 O4 Ni2 -38.16(14) . . . . ? O1 Tb1 O4 Ni2 106.45(17) . . . . ? O2 Tb1 O4 Ni2 25.3(3) 3_675 . . . ? O11 Tb1 O4 Ni2 35.26(14) . . . . ? Tb1 Tb1 O4 Ni2 95.0(3) 3_675 . . . ? O4 Tb1 O5 C21 -15.4(7) . . . . ? O9 Tb1 O5 C21 -134.9(7) . . . . ? O2 Tb1 O5 C21 133.8(7) . . . . ? O8 Tb1 O5 C21 -70.1(7) . . . . ? O1 Tb1 O5 C21 63.8(7) . . . . ? O2 Tb1 O5 C21 156.7(6) 3_675 . . . ? O11 Tb1 O5 C21 9.4(8) . . . . ? Tb1 Tb1 O5 C21 142.5(7) 3_675 . . . ? O4 Ni2 O7 C23 13.3(12) . . . . ? N4 Ni2 O7 C23 -172.9(5) . . . . ? O8 Ni2 O7 C23 12.7(5) . . . . ? O11 Ni2 O7 C23 93.7(5) . . . . ? O1W Ni2 O7 C23 -85.9(5) . . . . ? O4 Ni2 O8 C30 170.9(5) . . . . ? N4 Ni2 O8 C30 -164.9(8) . . . . ? O7 Ni2 O8 C30 -9.3(5) . . . . ? O11 Ni2 O8 C30 -105.0(5) . . . . ? O1W Ni2 O8 C30 77.4(5) . . . . ? O4 Ni2 O8 Tb1 -40.85(15) . . . . ? N4 Ni2 O8 Tb1 -16.6(9) . . . . ? O7 Ni2 O8 Tb1 139.02(17) . . . . ? O11 Ni2 O8 Tb1 43.25(14) . . . . ? O1W Ni2 O8 Tb1 -134.29(16) . . . . ? O5 Tb1 O8 C30 -116.4(5) . . . . ? O4 Tb1 O8 C30 -173.7(5) . . . . ? O9 Tb1 O8 C30 -44.5(4) . . . . ? O2 Tb1 O8 C30 -7.2(6) . . . . ? O1 Tb1 O8 C30 137.1(4) . . . . ? O2 Tb1 O8 C30 38.0(5) 3_675 . . . ? O11 Tb1 O8 C30 110.1(5) . . . . ? Tb1 Tb1 O8 C30 25.2(5) 3_675 . . . ? O5 Tb1 O8 Ni2 94.73(18) . . . . ? O4 Tb1 O8 Ni2 37.42(14) . . . . ? O9 Tb1 O8 Ni2 166.63(19) . . . . ? O2 Tb1 O8 Ni2 -156.0(3) . . . . ? O1 Tb1 O8 Ni2 -11.8(2) . . . . ? O2 Tb1 O8 Ni2 -110.82(15) 3_675 . . . ? O11 Tb1 O8 Ni2 -38.69(13) . . . . ? Tb1 Tb1 O8 Ni2 -123.65(10) 3_675 . . . ? O5 Tb1 O9 C29 138.3(7) . . . . ? O4 Tb1 O9 C29 73.2(7) . . . . ? O2 Tb1 O9 C29 -143.6(6) . . . . ? O8 Tb1 O9 C29 21.7(6) . . . . ? O1 Tb1 O9 C29 -161.6(5) . . . . ? O2 Tb1 O9 C29 -75.1(6) 3_675 . . . ? O11 Tb1 O9 C29 -9.9(7) . . . . ? Tb1 Tb1 O9 C29 -109.1(6) 3_675 . . . ? N3 Ni3 O11 Ni2 25.0(7) . . . . ? O1 Ni3 O11 Ni2 99.3(2) . . . . ? N2 Ni3 O11 Ni2 -158.0(2) . . . . ? N1 Ni3 O11 Ni2 -71.7(2) . . . . ? N3 Ni3 O11 Tb1 -71.8(7) . . . . ? O1 Ni3 O11 Tb1 2.51(16) . . . . ? N2 Ni3 O11 Tb1 105.19(19) . . . . ? N1 Ni3 O11 Tb1 -168.53(19) . . . . ? O4 Ni2 O11 Ni3 -67.6(2) . . . . ? N4 Ni2 O11 Ni3 20.3(2) . . . . ? O8 Ni2 O11 Ni3 -148.2(2) . . . . ? O7 Ni2 O11 Ni3 124.1(2) . . . . ? O4 Ni2 O11 Tb1 37.73(15) . . . . ? N4 Ni2 O11 Tb1 125.67(19) . . . . ? O8 Ni2 O11 Tb1 -42.82(13) . . . . ? O7 Ni2 O11 Tb1 -130.55(15) . . . . ? O5 Tb1 O11 Ni3 58.4(3) . . . . ? O4 Tb1 O11 Ni3 83.63(18) . . . . ? O9 Tb1 O11 Ni3 -171.44(16) . . . . ? O2 Tb1 O11 Ni3 -49.7(2) . . . . ? O8 Tb1 O11 Ni3 156.3(2) . . . . ? O1 Tb1 O11 Ni3 -2.28(15) . . . . ? O2 Tb1 O11 Ni3 -102.38(17) 3_675 . . . ? Tb1 Tb1 O11 Ni3 -78.11(14) 3_675 . . . ? O5 Tb1 O11 Ni2 -59.5(2) . . . . ? O4 Tb1 O11 Ni2 -34.32(14) . . . . ? O9 Tb1 O11 Ni2 70.6(2) . . . . ? O2 Tb1 O11 Ni2 -167.69(12) . . . . ? O8 Tb1 O11 Ni2 38.37(13) . . . . ? O1 Tb1 O11 Ni2 -120.23(17) . . . . ? O2 Tb1 O11 Ni2 139.67(16) 3_675 . . . ? Tb1 Tb1 O11 Ni2 163.94(10) 3_675 . . . ? C3 N1 C1 C2 145.5(6) . . . . ? C13 N1 C1 C2 -92.8(6) . . . . ? Ni3 N1 C1 C2 32.5(6) . . . . ? Ni3 N2 C2 C1 45.9(6) . . . . ? N1 C1 C2 N2 -54.8(8) . . . . ? C1 N1 C3 C4 -75.5(7) . . . . ? C13 N1 C3 C4 164.0(6) . . . . ? Ni3 N1 C3 C4 36.0(7) . . . . ? C5 N3 C4 C3 -157.5(7) . . . . ? Ni3 N3 C4 C3 29.6(8) . . . . ? N1 C3 C4 N3 -43.6(9) . . . . ? C4 N3 C5 C6 -175.4(8) . . . . ? Ni3 N3 C5 C6 -3.3(12) . . . . ? N3 C5 C6 C7 -179.7(8) . . . . ? N3 C5 C6 C12 1.0(13) . . . . ? C12 C6 C7 C8 -0.1(13) . . . . ? C5 C6 C7 C8 -179.4(8) . . . . ? C6 C7 C8 C9 3.9(14) . . . . ? C7 C8 C9 C10 -2.5(13) . . . . ? C8 C9 C10 C12 -2.8(11) . . . . ? C8 C9 C10 C11 171.7(7) . . . . ? Tb1 O2 C11 O3 125.4(5) . . . . ? Tb1 O2 C11 O3 -71.6(7) 3_675 . . . ? Tb1 O2 C11 C10 -57.4(6) . . . . ? Tb1 O2 C11 C10 105.7(5) 3_675 . . . ? C9 C10 C11 O3 8.4(9) . . . . ? C12 C10 C11 O3 -177.4(6) . . . . ? C9 C10 C11 O2 -168.9(6) . . . . ? C12 C10 C11 O2 5.3(9) . . . . ? Ni3 O1 C12 C10 -165.9(4) . . . . ? Tb1 O1 C12 C10 21.0(8) . . . . ? Ni3 O1 C12 C6 15.4(8) . . . . ? Tb1 O1 C12 C6 -157.7(5) . . . . ? C9 C10 C12 O1 -172.1(6) . . . . ? C11 C10 C12 O1 13.9(9) . . . . ? C9 C10 C12 C6 6.6(9) . . . . ? C11 C10 C12 C6 -167.4(6) . . . . ? C7 C6 C12 O1 173.5(7) . . . . ? C5 C6 C12 O1 -7.2(11) . . . . ? C7 C6 C12 C10 -5.2(10) . . . . ? C5 C6 C12 C10 174.1(7) . . . . ? C1 N1 C13 C14 -172.6(6) . . . . ? C3 N1 C13 C14 -52.2(7) . . . . ? Ni3 N1 C13 C14 70.0(7) . . . . ? C15 N4 C14 C13 124.3(8) . . . . ? Ni2 N4 C14 C13 -67.3(7) . . . . ? N1 C13 C14 N4 -53.6(8) . . . . ? C14 N4 C15 C16 -177.8(9) . . . . ? Ni2 N4 C15 C16 14.3(13) . . . . ? N4 C15 C16 C22 8.5(16) . . . . ? N4 C15 C16 C17 -179.1(10) . . . . ? C22 C16 C17 C18 -1.5(18) . . . . ? C15 C16 C17 C18 -174.5(11) . . . . ? C16 C17 C18 C19 2(2) . . . . ? C17 C18 C19 C20 -0.3(19) . . . . ? C18 C19 C20 C22 -2.9(15) . . . . ? C18 C19 C20 C21 176.3(10) . . . . ? Tb1 O5 C21 O6 176.3(6) . . . . ? Tb1 O5 C21 C20 -5.9(12) . . . . ? C22 C20 C21 O5 18.5(11) . . . . ? C19 C20 C21 O5 -160.7(8) . . . . ? C22 C20 C21 O6 -163.7(8) . . . . ? C19 C20 C21 O6 17.1(11) . . . . ? Ni2 O4 C22 C20 167.1(5) . . . . ? Tb1 O4 C22 C20 -44.1(9) . . . . ? Ni2 O4 C22 C16 -11.7(10) . . . . ? Tb1 O4 C22 C16 137.0(6) . . . . ? C19 C20 C22 O4 -175.0(8) . . . . ? C21 C20 C22 O4 5.9(11) . . . . ? C19 C20 C22 C16 3.8(12) . . . . ? C21 C20 C22 C16 -175.3(7) . . . . ? C17 C16 C22 O4 177.2(8) . . . . ? C15 C16 C22 O4 -10.4(13) . . . . ? C17 C16 C22 C20 -1.7(13) . . . . ? C15 C16 C22 C20 170.8(8) . . . . ? Ni2 O7 C23 C24 -9.3(10) . . . . ? O7 C23 C24 C25 179.9(7) . . . . ? O7 C23 C24 C30 -3.7(11) . . . . ? C23 C24 C25 C26 176.8(7) . . . . ? C30 C24 C25 C26 0.3(11) . . . . ? C24 C25 C26 C27 -2.3(13) . . . . ? C25 C26 C27 C28 1.4(12) . . . . ? C26 C27 C28 C30 1.5(10) . . . . ? C26 C27 C28 C29 -179.1(7) . . . . ? Tb1 O9 C29 O10 179.7(5) . . . . ? Tb1 O9 C29 C28 0.0(10) . . . . ? C27 C28 C29 O10 -17.4(9) . . . . ? C30 C28 C29 O10 161.9(6) . . . . ? C27 C28 C29 O9 162.3(6) . . . . ? C30 C28 C29 O9 -18.4(9) . . . . ? Ni2 O8 C30 C28 -177.1(4) . . . . ? Tb1 O8 C30 C28 46.0(7) . . . . ? Ni2 O8 C30 C24 1.0(8) . . . . ? Tb1 O8 C30 C24 -135.9(5) . . . . ? C27 C28 C30 O8 174.8(6) . . . . ? C29 C28 C30 O8 -4.6(9) . . . . ? C27 C28 C30 C24 -3.4(8) . . . . ? C29 C28 C30 C24 177.2(6) . . . . ? C25 C24 C30 O8 -175.6(6) . . . . ? C23 C24 C30 O8 8.2(9) . . . . ? C25 C24 C30 C28 2.6(9) . . . . ? C23 C24 C30 C28 -173.6(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O10 0.90 2.46 3.198(7) 139.3 3_675 N2 H2B O9 0.90 2.49 3.061(7) 121.7 3_675 O11 H11 O3 0.98 2.08 2.947(6) 146.5 3_675 O1W H1WA O4W 0.85 1.83 2.659(9) 164.5 1_665 O1W H1WB O5W 0.85 1.98 2.818(10) 170.5 1_565 O2W H2WB O5 0.85 2.51 3.090(8) 126.6 1_545 O2W H2WB O6 0.85 2.60 3.309(11) 141.7 1_545 O3W H3WA O6 0.85 1.85 2.695(9) 174.2 1_545 O3W H3WB O3 0.85 2.10 2.917(8) 161.2 1_545 O4W H4WA O10 0.85 2.03 2.808(9) 151.3 4_576 O4W H4WA O7W 0.85 2.57 2.98(2) 110.3 3_666 O4W H4WB O3W 0.85 2.10 2.692(10) 126.5 . O5W H5WA O2W 0.85 2.17 2.703(11) 120.2 4_666 O5W H5WB O6W 0.85 2.11 2.790(15) 136.0 3_766 O6W H6WA O5W 0.85 1.94 2.790(15) 175.1 3_766 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.642 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.121 data_1296 _database_code_depnum_ccdc_archive 'CCDC 898022' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 Gd2 N8 Ni4 O24, 8(H2 O)' _chemical_formula_sum 'C60 H74 Gd2 N8 Ni4 O32' _chemical_formula_weight 1968.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6620(10) _cell_length_b 18.1513(14) _cell_length_c 15.5428(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.7790(10) _cell_angle_gamma 90.00 _cell_volume 3520.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4906 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.39 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 3.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5092 _exptl_absorpt_correction_T_max 0.6964 _exptl_absorpt_process_details 'SADABS(Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17591 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6191 _reflns_number_gt 4815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2005)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2005)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+2.2778P] 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 6191 _refine_ls_number_parameters 487 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.015 _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 Gd1 Gd 0.084030(13) 1.056658(9) 0.596635(11) 0.02290(5) Uani 1 1 d . . . Ni1 Ni 0.16239(4) 0.89530(2) 0.71051(3) 0.02777(12) Uani 1 1 d . . . Ni2 Ni 0.31503(4) 1.05075(2) 0.70923(3) 0.02627(11) Uani 1 1 d . . . N1 N 0.3061(2) 0.83655(16) 0.7678(2) 0.0341(8) Uani 1 1 d . . . N2 N 0.1030(3) 0.84825(16) 0.8053(2) 0.0361(8) Uani 1 1 d . . . N3 N 0.3403(2) 0.99142(16) 0.82118(19) 0.0330(8) Uani 1 1 d . . . N4 N 0.1473(3) 0.81625(17) 0.6172(2) 0.0446(10) Uani 1 1 d . . . H4A H 0.1022 0.7807 0.6288 0.054 Uiso 1 1 calc R . . H4B H 0.1215 0.8357 0.5645 0.054 Uiso 1 1 calc R . . O1 O -0.2537(2) 1.05375(14) 0.54187(17) 0.0400(7) Uani 1 1 d . . . O2 O -0.09007(18) 1.01693(12) 0.53170(15) 0.0272(6) Uani 1 1 d . . . O3 O 0.02613(18) 0.95593(12) 0.67797(15) 0.0274(6) Uani 1 1 d . . . O4 O -0.1105(3) 1.1843(2) 0.7581(2) 0.0895(12) Uani 1 1 d U . . O5 O -0.0233(2) 1.13171(14) 0.66512(17) 0.0389(7) Uani 1 1 d . . . O6 O 0.17261(19) 1.08119(13) 0.73789(15) 0.0300(6) Uani 1 1 d . . . O7 O 0.0998(2) 1.24544(16) 0.41080(19) 0.0546(8) Uani 1 1 d . . . O8 O 0.07514(19) 1.15476(13) 0.49851(16) 0.0356(7) Uani 1 1 d . . . O9 O 0.25805(18) 1.10830(13) 0.59925(15) 0.0287(6) Uani 1 1 d . . . O10 O 0.4508(2) 1.02890(14) 0.65800(16) 0.0362(7) Uani 1 1 d . . . O11 O 0.22602(18) 0.96910(12) 0.64079(14) 0.0257(6) Uani 1 1 d D . . H11 H 0.2574 0.9484 0.5926 0.031 Uiso 1 1 calc RD . . C1 C 0.2899(3) 0.8137(2) 0.8563(3) 0.0418(11) Uani 1 1 d . . . H1A H 0.3098 0.8537 0.8971 0.050 Uiso 1 1 calc R . . H1B H 0.3355 0.7718 0.8754 0.050 Uiso 1 1 calc R . . C2 C 0.1746(3) 0.7931(2) 0.8557(3) 0.0460(12) Uani 1 1 d . . . H2A H 0.1604 0.7448 0.8296 0.055 Uiso 1 1 calc R . . H2B H 0.1607 0.7910 0.9152 0.055 Uiso 1 1 calc R . . C3 C 0.0069(3) 0.8544(2) 0.8199(3) 0.0412(11) Uani 1 1 d . . . H3 H -0.0099 0.8269 0.8662 0.049 Uiso 1 1 calc R . . C4 C -0.0782(3) 0.8986(2) 0.7735(2) 0.0349(10) Uani 1 1 d . . . C5 C -0.1752(4) 0.8925(3) 0.8019(3) 0.0573(13) Uani 1 1 d . . . H5 H -0.1802 0.8618 0.8490 0.069 Uiso 1 1 calc R . . C6 C -0.2639(4) 0.9299(3) 0.7635(3) 0.0634(15) Uani 1 1 d . . . H6 H -0.3281 0.9259 0.7847 0.076 Uiso 1 1 calc R . . C7 C -0.2563(3) 0.9737(3) 0.6924(3) 0.0478(12) Uani 1 1 d . . . H7 H -0.3168 0.9994 0.6662 0.057 Uiso 1 1 calc R . . C8 C -0.1630(3) 0.9812(2) 0.6583(2) 0.0285(9) Uani 1 1 d . . . C9 C -0.1706(3) 1.0212(2) 0.5735(2) 0.0287(9) Uani 1 1 d . . . C10 C -0.0677(3) 0.94574(19) 0.7020(2) 0.0275(8) Uani 1 1 d . . . C11 C 0.4098(3) 0.8754(2) 0.7708(3) 0.0357(10) Uani 1 1 d . . . H11A H 0.4135 0.8936 0.7127 0.043 Uiso 1 1 calc R . . H11B H 0.4672 0.8400 0.7860 0.043 Uiso 1 1 calc R . . C12 C 0.4297(3) 0.9390(2) 0.8337(3) 0.0409(11) Uani 1 1 d . . . H12A H 0.4402 0.9204 0.8930 0.049 Uiso 1 1 calc R . . H12B H 0.4948 0.9643 0.8255 0.049 Uiso 1 1 calc R . . C13 C 0.2918(3) 1.0036(2) 0.8856(3) 0.0410(11) Uani 1 1 d . . . H13 H 0.3224 0.9824 0.9384 0.049 Uiso 1 1 calc R . . C14 C 0.1967(4) 1.0457(2) 0.8866(3) 0.0440(11) Uani 1 1 d . . . C15 C 0.1558(5) 1.0466(3) 0.9646(3) 0.0701(16) Uani 1 1 d . . . H15 H 0.1952 1.0245 1.0138 0.084 Uiso 1 1 calc R . . C16 C 0.0604(5) 1.0789(3) 0.9713(3) 0.0836(18) Uani 1 1 d . . . H16 H 0.0363 1.0798 1.0246 0.100 Uiso 1 1 calc R . . C17 C -0.0001(4) 1.1099(3) 0.8983(3) 0.0620(14) Uani 1 1 d . . . H17 H -0.0661 1.1307 0.9027 0.074 Uiso 1 1 calc R . . C18 C 0.0350(3) 1.1111(2) 0.8184(3) 0.0393(10) Uani 1 1 d . . . C19 C -0.0374(3) 1.1443(2) 0.7426(3) 0.0453(12) Uani 1 1 d . . . C20 C 0.1355(3) 1.07952(19) 0.8122(2) 0.0323(10) Uani 1 1 d . . . C21 C 0.3053(3) 0.7703(2) 0.7112(3) 0.0420(11) Uani 1 1 d . . . H21A H 0.2658 0.7311 0.7340 0.050 Uiso 1 1 calc R . . H21B H 0.3783 0.7535 0.7127 0.050 Uiso 1 1 calc R . . C22 C 0.2550(3) 0.7860(2) 0.6182(3) 0.0472(12) Uani 1 1 d . . . H22A H 0.2985 0.8211 0.5927 0.057 Uiso 1 1 calc R . . H22B H 0.2505 0.7410 0.5842 0.057 Uiso 1 1 calc R . . C23 C 0.4754(3) 1.0608(2) 0.5939(3) 0.0404(10) Uani 1 1 d . . . H23 H 0.5438 1.0505 0.5829 0.048 Uiso 1 1 calc R . . C24 C 0.4151(3) 1.1112(2) 0.5343(2) 0.0319(9) Uani 1 1 d . . . C25 C 0.4668(3) 1.1396(2) 0.4696(3) 0.0454(11) Uani 1 1 d . . . H25 H 0.5377 1.1268 0.4690 0.055 Uiso 1 1 calc R . . C26 C 0.4157(4) 1.1859(3) 0.4070(3) 0.0548(13) Uani 1 1 d . . . H26 H 0.4524 1.2066 0.3660 0.066 Uiso 1 1 calc R . . C27 C 0.3088(3) 1.2016(2) 0.4052(3) 0.0418(11) Uani 1 1 d . . . H27 H 0.2740 1.2322 0.3614 0.050 Uiso 1 1 calc R . . C28 C 0.2511(3) 1.17355(19) 0.4663(2) 0.0296(9) Uani 1 1 d . . . C29 C 0.1350(3) 1.19239(19) 0.4581(2) 0.0309(9) Uani 1 1 d . . . C30 C 0.3059(3) 1.12961(18) 0.5353(2) 0.0250(8) Uani 1 1 d . . . O1W O 0.3960(2) 1.13764(13) 0.77683(17) 0.0403(7) Uani 1 1 d . . . H1WA H 0.3824 1.1640 0.8188 0.048 Uiso 1 1 d R . . H1WB H 0.3852 1.1639 0.7309 0.048 Uiso 1 1 d R . . O2W O 0.7173(3) 0.19172(19) 0.6333(2) 0.0759(11) Uani 1 1 d . . . H2WA H 0.7142 0.1559 0.5977 0.091 Uiso 1 1 d R . . H2WB H 0.7631 0.1808 0.6780 0.091 Uiso 1 1 d R . . O3W O 0.9672(3) 0.3555(2) 0.4544(2) 0.0908(13) Uani 1 1 d . . . H3WA H 0.9276 0.3819 0.4169 0.109 Uiso 1 1 d R . . H3WB H 1.0130 0.3837 0.4843 0.109 Uiso 1 1 d R . . O4W O 0.8949(4) 0.2733(2) 0.5763(3) 0.1091(16) Uani 1 1 d . . . H4WA H 0.9057 0.3043 0.6178 0.131 Uiso 1 1 d R . . H4WB H 0.9301 0.2345 0.5933 0.131 Uiso 1 1 d R . . O5W O 0.5744(3) 0.1933(2) 0.7441(3) 0.0751(13) Uani 0.75 1 d P . . H5WA H 0.6073 0.1986 0.7962 0.090 Uiso 0.75 1 d PR . . H5WB H 0.5707 0.2354 0.7198 0.090 Uiso 0.75 1 d PR . . O6W O 0.2096(12) 0.3955(8) 0.4159(8) 0.083(5) Uani 0.25 1 d P . . H6WA H 0.2280 0.4376 0.3997 0.099 Uiso 0.25 1 d PR . . H6WB H 0.1910 0.3695 0.3703 0.099 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02202(8) 0.02164(8) 0.02458(9) -0.00062(8) 0.00261(7) 0.00150(8) Ni1 0.0287(2) 0.0232(2) 0.0313(3) 0.00394(19) 0.0049(2) 0.0032(2) Ni2 0.0249(2) 0.0262(2) 0.0263(2) 0.0019(2) 0.00057(19) -0.0002(2) N1 0.0337(17) 0.0281(16) 0.0401(18) 0.0050(14) 0.0049(15) 0.0035(15) N2 0.0406(19) 0.0331(17) 0.0352(18) 0.0128(14) 0.0081(15) 0.0063(15) N3 0.0363(17) 0.0305(17) 0.0292(17) 0.0014(14) -0.0027(14) -0.0021(15) N4 0.042(2) 0.0339(18) 0.054(2) -0.0058(16) -0.0018(18) 0.0034(16) O1 0.0279(13) 0.0521(16) 0.0394(15) 0.0037(13) 0.0039(12) 0.0124(13) O2 0.0219(12) 0.0333(13) 0.0265(13) -0.0044(11) 0.0045(10) 0.0014(11) O3 0.0244(12) 0.0272(13) 0.0311(13) 0.0039(10) 0.0065(11) 0.0024(11) O4 0.064(2) 0.135(3) 0.064(2) -0.054(2) -0.0046(18) 0.046(2) O5 0.0358(15) 0.0404(15) 0.0414(15) -0.0073(12) 0.0092(13) 0.0108(13) O6 0.0280(13) 0.0367(14) 0.0256(13) -0.0031(11) 0.0051(11) 0.0020(11) O7 0.0487(17) 0.0543(17) 0.0635(19) 0.0327(15) 0.0170(15) 0.0174(15) O8 0.0261(13) 0.0349(14) 0.0440(16) 0.0094(12) 0.0010(12) -0.0004(12) O9 0.0242(12) 0.0336(13) 0.0288(13) 0.0069(11) 0.0060(11) 0.0003(11) O10 0.0306(14) 0.0389(14) 0.0397(15) 0.0092(12) 0.0071(12) 0.0043(12) O11 0.0264(12) 0.0235(12) 0.0263(13) -0.0009(10) 0.0024(10) 0.0027(10) C1 0.044(2) 0.033(2) 0.047(2) 0.0142(19) 0.003(2) 0.0044(19) C2 0.051(3) 0.038(2) 0.048(2) 0.0234(19) 0.007(2) 0.010(2) C3 0.045(2) 0.042(2) 0.039(2) 0.0161(18) 0.015(2) 0.000(2) C4 0.036(2) 0.035(2) 0.034(2) 0.0076(17) 0.0081(18) 0.0028(18) C5 0.047(3) 0.084(3) 0.045(3) 0.027(2) 0.019(2) 0.008(3) C6 0.035(2) 0.101(4) 0.060(3) 0.025(3) 0.025(2) 0.009(3) C7 0.029(2) 0.074(3) 0.042(2) 0.009(2) 0.0110(19) 0.012(2) C8 0.0248(18) 0.039(2) 0.0226(18) 0.0005(16) 0.0065(15) 0.0020(17) C9 0.0234(18) 0.0325(19) 0.030(2) -0.0080(16) 0.0022(16) 0.0013(17) C10 0.0300(19) 0.0271(18) 0.0267(18) -0.0043(16) 0.0087(15) -0.0011(17) C11 0.028(2) 0.036(2) 0.041(2) 0.0072(18) 0.0000(18) 0.0058(18) C12 0.040(2) 0.040(2) 0.037(2) 0.0118(19) -0.0091(19) 0.000(2) C13 0.058(3) 0.038(2) 0.027(2) 0.0027(18) 0.007(2) 0.002(2) C14 0.067(3) 0.035(2) 0.031(2) 0.0001(18) 0.014(2) 0.004(2) C15 0.105(4) 0.070(3) 0.041(3) 0.006(2) 0.028(3) 0.023(3) C16 0.121(5) 0.095(4) 0.048(3) 0.011(3) 0.050(3) 0.026(4) C17 0.065(3) 0.067(3) 0.062(3) -0.011(3) 0.036(3) 0.002(3) C18 0.043(2) 0.038(2) 0.039(2) -0.0142(18) 0.0148(19) -0.0076(19) C19 0.033(2) 0.050(3) 0.053(3) -0.025(2) 0.009(2) 0.001(2) C20 0.043(2) 0.0252(19) 0.030(2) -0.0071(16) 0.0099(18) -0.0083(17) C21 0.037(2) 0.030(2) 0.058(3) -0.003(2) 0.003(2) 0.0067(18) C22 0.043(2) 0.042(2) 0.056(3) -0.011(2) 0.007(2) 0.011(2) C23 0.027(2) 0.048(2) 0.046(2) 0.004(2) 0.0066(18) 0.004(2) C24 0.0274(19) 0.037(2) 0.032(2) 0.0040(17) 0.0078(17) 0.0023(17) C25 0.032(2) 0.055(3) 0.053(3) 0.013(2) 0.015(2) 0.009(2) C26 0.046(2) 0.068(3) 0.056(3) 0.029(2) 0.024(2) 0.004(2) C27 0.050(3) 0.039(2) 0.037(2) 0.0131(18) 0.009(2) 0.004(2) C28 0.036(2) 0.0218(18) 0.030(2) -0.0001(16) 0.0019(17) 0.0023(17) C29 0.036(2) 0.0283(19) 0.029(2) 0.0032(16) 0.0060(17) 0.0056(17) C30 0.0288(19) 0.0207(17) 0.0257(18) -0.0021(15) 0.0059(16) -0.0037(15) O1W 0.0462(16) 0.0292(14) 0.0430(16) -0.0003(12) 0.0004(13) -0.0038(13) O2W 0.064(2) 0.088(2) 0.073(2) -0.0241(19) 0.0032(19) 0.015(2) O3W 0.105(3) 0.097(3) 0.060(2) -0.008(2) -0.016(2) 0.020(2) O4W 0.149(4) 0.081(3) 0.085(3) 0.000(2) -0.014(3) 0.001(3) O5W 0.065(3) 0.104(3) 0.065(3) -0.055(2) 0.036(2) -0.063(2) O6W 0.114(11) 0.083(9) 0.049(8) -0.033(7) 0.010(8) -0.059(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O5 2.308(3) . ? Gd1 O6 2.332(2) . ? Gd1 O8 2.335(2) . ? Gd1 O2 2.375(2) . ? Gd1 O9 2.389(2) . ? Gd1 O3 2.407(2) . ? Gd1 O11 2.410(2) . ? Gd1 O2 2.413(2) 3_576 ? Gd1 Gd1 3.9511(4) 3_576 ? Ni1 N2 1.960(3) . ? Ni1 O11 1.979(2) . ? Ni1 N4 2.026(3) . ? Ni1 O3 2.036(2) . ? Ni1 N1 2.166(3) . ? Ni2 O6 2.007(2) . ? Ni2 N3 2.025(3) . ? Ni2 O9 2.028(2) . ? Ni2 O11 2.047(2) . ? Ni2 O10 2.052(3) . ? Ni2 O1W 2.068(2) . ? N1 C1 1.484(5) . ? N1 C11 1.485(5) . ? N1 C21 1.489(5) . ? N2 C3 1.280(5) . ? N2 C2 1.481(5) . ? N3 C13 1.279(5) . ? N3 C12 1.466(5) . ? N4 C22 1.468(5) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? O1 C9 1.234(4) . ? O2 C9 1.301(4) . ? O2 Gd1 2.413(2) 3_576 ? O3 C10 1.318(4) . ? O4 C19 1.232(5) . ? O5 C19 1.268(5) . ? O6 C20 1.319(4) . ? O7 C29 1.247(4) . ? O8 C29 1.264(4) . ? O9 C30 1.307(4) . ? O10 C23 1.237(5) . ? O11 H11 0.9800 . ? C1 C2 1.505(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.435(5) . ? C3 H3 0.9300 . ? C4 C5 1.378(6) . ? C4 C10 1.428(5) . ? C5 C6 1.360(6) . ? C5 H5 0.9300 . ? C6 C7 1.378(6) . ? C6 H6 0.9300 . ? C7 C8 1.382(5) . ? C7 H7 0.9300 . ? C8 C10 1.432(5) . ? C8 C9 1.494(5) . ? C11 C12 1.506(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.428(6) . ? C13 H13 0.9300 . ? C14 C15 1.397(6) . ? C14 C20 1.418(5) . ? C15 C16 1.362(8) . ? C15 H15 0.9300 . ? C16 C17 1.377(7) . ? C16 H16 0.9300 . ? C17 C18 1.389(6) . ? C17 H17 0.9300 . ? C18 C20 1.414(6) . ? C18 C19 1.492(6) . ? C21 C22 1.504(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.427(5) . ? C23 H23 0.9300 . ? C24 C25 1.388(5) . ? C24 C30 1.426(5) . ? C25 C26 1.362(6) . ? C25 H25 0.9300 . ? C26 C27 1.378(6) . ? C26 H26 0.9300 . ? C27 C28 1.390(5) . ? C27 H27 0.9300 . ? C28 C30 1.419(5) . ? C28 C29 1.494(5) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8501 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8499 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8500 . ? 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 O5 Gd1 O6 71.33(9) . . ? O5 Gd1 O8 83.36(9) . . ? O6 Gd1 O8 115.56(8) . . ? O5 Gd1 O2 78.37(8) . . ? O6 Gd1 O2 136.15(8) . . ? O8 Gd1 O2 90.90(8) . . ? O5 Gd1 O9 111.98(9) . . ? O6 Gd1 O9 67.31(8) . . ? O8 Gd1 O9 69.75(8) . . ? O2 Gd1 O9 155.96(8) . . ? O5 Gd1 O3 87.15(9) . . ? O6 Gd1 O3 77.95(8) . . ? O8 Gd1 O3 159.59(8) . . ? O2 Gd1 O3 69.45(8) . . ? O9 Gd1 O3 130.66(7) . . ? O5 Gd1 O11 136.64(8) . . ? O6 Gd1 O11 69.00(8) . . ? O8 Gd1 O11 129.77(8) . . ? O2 Gd1 O11 120.95(8) . . ? O9 Gd1 O11 67.20(8) . . ? O3 Gd1 O11 68.20(8) . . ? O5 Gd1 O2 144.28(8) . 3_576 ? O6 Gd1 O2 143.73(8) . 3_576 ? O8 Gd1 O2 83.51(8) . 3_576 ? O2 Gd1 O2 68.78(9) . 3_576 ? O9 Gd1 O2 94.16(8) . 3_576 ? O3 Gd1 O2 93.96(8) . 3_576 ? O11 Gd1 O2 75.14(7) . 3_576 ? O5 Gd1 Gd1 112.00(6) . 3_576 ? O6 Gd1 Gd1 157.80(6) . 3_576 ? O8 Gd1 Gd1 86.58(6) . 3_576 ? O2 Gd1 Gd1 34.70(5) . 3_576 ? O9 Gd1 Gd1 126.40(6) . 3_576 ? O3 Gd1 Gd1 80.28(5) . 3_576 ? O11 Gd1 Gd1 98.78(5) . 3_576 ? O2 Gd1 Gd1 34.09(5) 3_576 3_576 ? N2 Ni1 O11 161.91(11) . . ? N2 Ni1 N4 103.18(14) . . ? O11 Ni1 N4 94.88(12) . . ? N2 Ni1 O3 90.30(11) . . ? O11 Ni1 O3 84.53(9) . . ? N4 Ni1 O3 103.40(11) . . ? N2 Ni1 N1 83.06(12) . . ? O11 Ni1 N1 99.60(11) . . ? N4 Ni1 N1 85.20(12) . . ? O3 Ni1 N1 170.19(11) . . ? O6 Ni2 N3 88.42(11) . . ? O6 Ni2 O9 80.85(9) . . ? N3 Ni2 O9 168.42(11) . . ? O6 Ni2 O11 83.03(9) . . ? N3 Ni2 O11 93.10(10) . . ? O9 Ni2 O11 81.33(9) . . ? O6 Ni2 O10 169.34(10) . . ? N3 Ni2 O10 102.13(12) . . ? O9 Ni2 O10 88.51(10) . . ? O11 Ni2 O10 94.71(10) . . ? O6 Ni2 O1W 93.66(10) . . ? N3 Ni2 O1W 88.66(11) . . ? O9 Ni2 O1W 96.32(10) . . ? O11 Ni2 O1W 176.20(10) . . ? O10 Ni2 O1W 88.20(11) . . ? C1 N1 C11 111.4(3) . . ? C1 N1 C21 109.5(3) . . ? C11 N1 C21 108.7(3) . . ? C1 N1 Ni1 106.3(2) . . ? C11 N1 Ni1 117.1(2) . . ? C21 N1 Ni1 103.5(2) . . ? C3 N2 C2 118.7(3) . . ? C3 N2 Ni1 126.3(3) . . ? C2 N2 Ni1 114.4(3) . . ? C13 N3 C12 118.1(3) . . ? C13 N3 Ni2 123.6(3) . . ? C12 N3 Ni2 117.7(2) . . ? C22 N4 Ni1 106.4(2) . . ? C22 N4 H4A 110.4 . . ? Ni1 N4 H4A 110.4 . . ? C22 N4 H4B 110.4 . . ? Ni1 N4 H4B 110.4 . . ? H4A N4 H4B 108.6 . . ? C9 O2 Gd1 121.3(2) . . ? C9 O2 Gd1 125.7(2) . 3_576 ? Gd1 O2 Gd1 111.22(9) . 3_576 ? C10 O3 Ni1 128.4(2) . . ? C10 O3 Gd1 128.7(2) . . ? Ni1 O3 Gd1 102.72(10) . . ? C19 O5 Gd1 137.2(3) . . ? C20 O6 Ni2 130.9(2) . . ? C20 O6 Gd1 129.3(2) . . ? Ni2 O6 Gd1 92.58(9) . . ? C29 O8 Gd1 140.4(2) . . ? C30 O9 Ni2 130.4(2) . . ? C30 O9 Gd1 130.4(2) . . ? Ni2 O9 Gd1 90.42(9) . . ? C23 O10 Ni2 124.3(2) . . ? Ni1 O11 Ni2 116.43(11) . . ? Ni1 O11 Gd1 104.41(10) . . ? Ni2 O11 Gd1 89.36(8) . . ? Ni1 O11 H11 114.5 . . ? Ni2 O11 H11 114.5 . . ? Gd1 O11 H11 114.5 . . ? N1 C1 C2 110.5(3) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 110.0(3) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 128.0(4) . . ? N2 C3 H3 116.0 . . ? C4 C3 H3 116.0 . . ? C5 C4 C10 120.2(4) . . ? C5 C4 C3 115.4(4) . . ? C10 C4 C3 124.4(4) . . ? C6 C5 C4 122.3(4) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 118.4(4) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C6 C7 C8 123.1(4) . . ? C6 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? C7 C8 C10 118.7(3) . . ? C7 C8 C9 117.1(3) . . ? C10 C8 C9 124.0(3) . . ? O1 C9 O2 121.1(3) . . ? O1 C9 C8 120.5(3) . . ? O2 C9 C8 118.2(3) . . ? O3 C10 C4 120.8(3) . . ? O3 C10 C8 122.0(3) . . ? C4 C10 C8 117.2(3) . . ? N1 C11 C12 115.8(3) . . ? N1 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? N1 C11 H11B 108.3 . . ? C12 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? N3 C12 C11 111.8(3) . . ? N3 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N3 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? N3 C13 C14 128.2(4) . . ? N3 C13 H13 115.9 . . ? C14 C13 H13 115.9 . . ? C15 C14 C20 118.1(4) . . ? C15 C14 C13 117.0(4) . . ? C20 C14 C13 124.6(4) . . ? C16 C15 C14 122.4(5) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C15 C16 C17 119.3(5) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 121.7(5) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C20 118.9(4) . . ? C17 C18 C19 117.8(4) . . ? C20 C18 C19 123.3(4) . . ? O4 C19 O5 121.6(4) . . ? O4 C19 C18 117.7(4) . . ? O5 C19 C18 120.7(4) . . ? O6 C20 C18 120.6(3) . . ? O6 C20 C14 119.8(4) . . ? C18 C20 C14 119.6(4) . . ? N1 C21 C22 112.0(3) . . ? N1 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N1 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N4 C22 C21 108.8(3) . . ? N4 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? N4 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? O10 C23 C24 130.0(4) . . ? O10 C23 H23 115.0 . . ? C24 C23 H23 115.0 . . ? C25 C24 C30 119.9(3) . . ? C25 C24 C23 116.3(3) . . ? C30 C24 C23 123.8(3) . . ? C26 C25 C24 121.4(4) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 119.1(4) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C26 C27 C28 122.6(4) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C30 118.4(3) . . ? C27 C28 C29 118.8(3) . . ? C30 C28 C29 122.8(3) . . ? O7 C29 O8 121.7(3) . . ? O7 C29 C28 118.4(3) . . ? O8 C29 C28 119.9(3) . . ? O9 C30 C28 120.7(3) . . ? O9 C30 C24 121.0(3) . . ? C28 C30 C24 118.3(3) . . ? Ni2 O1W H1WA 132.2 . . ? Ni2 O1W H1WB 90.3 . . ? H1WA O1W H1WB 107.7 . . ? H2WA O2W H2WB 107.7 . . ? H3WA O3W H3WB 107.7 . . ? H4WA O4W H4WB 107.7 . . ? H5WA O5W H5WB 107.7 . . ? H6WA O6W H6WB 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C1 -16.0(2) . . . . ? O11 Ni1 N1 C1 145.9(2) . . . . ? N4 Ni1 N1 C1 -120.0(2) . . . . ? N2 Ni1 N1 C11 -141.2(3) . . . . ? O11 Ni1 N1 C11 20.7(3) . . . . ? N4 Ni1 N1 C11 114.9(3) . . . . ? N2 Ni1 N1 C21 99.3(2) . . . . ? O11 Ni1 N1 C21 -98.8(2) . . . . ? N4 Ni1 N1 C21 -4.7(2) . . . . ? O11 Ni1 N2 C3 81.4(5) . . . . ? N4 Ni1 N2 C3 -95.6(3) . . . . ? O3 Ni1 N2 C3 8.3(3) . . . . ? N1 Ni1 N2 C3 -179.0(3) . . . . ? O11 Ni1 N2 C2 -107.4(4) . . . . ? N4 Ni1 N2 C2 75.7(3) . . . . ? O3 Ni1 N2 C2 179.5(3) . . . . ? N1 Ni1 N2 C2 -7.7(3) . . . . ? O6 Ni2 N3 C13 -21.5(3) . . . . ? O9 Ni2 N3 C13 -43.6(7) . . . . ? O11 Ni2 N3 C13 -104.4(3) . . . . ? O10 Ni2 N3 C13 160.1(3) . . . . ? O1W Ni2 N3 C13 72.2(3) . . . . ? O6 Ni2 N3 C12 167.7(3) . . . . ? O9 Ni2 N3 C12 145.6(5) . . . . ? O11 Ni2 N3 C12 84.7(2) . . . . ? O10 Ni2 N3 C12 -10.8(3) . . . . ? O1W Ni2 N3 C12 -98.6(3) . . . . ? N2 Ni1 N4 C22 -104.8(3) . . . . ? O11 Ni1 N4 C22 76.2(3) . . . . ? O3 Ni1 N4 C22 161.7(2) . . . . ? N1 Ni1 N4 C22 -23.1(3) . . . . ? O5 Gd1 O2 C9 -28.8(2) . . . . ? O6 Gd1 O2 C9 17.9(3) . . . . ? O8 Gd1 O2 C9 -111.8(3) . . . . ? O9 Gd1 O2 C9 -147.3(2) . . . . ? O3 Gd1 O2 C9 62.5(2) . . . . ? O11 Gd1 O2 C9 109.1(2) . . . . ? O2 Gd1 O2 C9 165.5(3) 3_576 . . . ? Gd1 Gd1 O2 C9 165.5(3) 3_576 . . . ? O5 Gd1 O2 Gd1 165.71(11) . . . 3_576 ? O6 Gd1 O2 Gd1 -147.60(9) . . . 3_576 ? O8 Gd1 O2 Gd1 82.68(10) . . . 3_576 ? O9 Gd1 O2 Gd1 47.2(2) . . . 3_576 ? O3 Gd1 O2 Gd1 -102.98(10) . . . 3_576 ? O11 Gd1 O2 Gd1 -56.38(12) . . . 3_576 ? O2 Gd1 O2 Gd1 0.001(1) 3_576 . . 3_576 ? N2 Ni1 O3 C10 -15.2(3) . . . . ? O11 Ni1 O3 C10 -177.8(3) . . . . ? N4 Ni1 O3 C10 88.4(3) . . . . ? N2 Ni1 O3 Gd1 159.65(11) . . . . ? O11 Ni1 O3 Gd1 -2.99(9) . . . . ? N4 Ni1 O3 Gd1 -96.72(12) . . . . ? O5 Gd1 O3 C10 34.0(3) . . . . ? O6 Gd1 O3 C10 105.5(3) . . . . ? O8 Gd1 O3 C10 -28.3(4) . . . . ? O2 Gd1 O3 C10 -44.7(2) . . . . ? O9 Gd1 O3 C10 150.8(2) . . . . ? O11 Gd1 O3 C10 177.5(3) . . . . ? O2 Gd1 O3 C10 -110.3(3) 3_576 . . . ? Gd1 Gd1 O3 C10 -78.9(3) 3_576 . . . ? O5 Gd1 O3 Ni1 -140.87(10) . . . . ? O6 Gd1 O3 Ni1 -69.36(10) . . . . ? O8 Gd1 O3 Ni1 156.9(2) . . . . ? O2 Gd1 O3 Ni1 140.48(11) . . . . ? O9 Gd1 O3 Ni1 -24.04(14) . . . . ? O11 Gd1 O3 Ni1 2.63(8) . . . . ? O2 Gd1 O3 Ni1 74.90(9) 3_576 . . . ? Gd1 Gd1 O3 Ni1 106.23(8) 3_576 . . . ? O6 Gd1 O5 C19 -27.5(4) . . . . ? O8 Gd1 O5 C19 -147.4(4) . . . . ? O2 Gd1 O5 C19 120.3(4) . . . . ? O9 Gd1 O5 C19 -82.4(4) . . . . ? O3 Gd1 O5 C19 50.7(4) . . . . ? O11 Gd1 O5 C19 -2.9(4) . . . . ? O2 Gd1 O5 C19 143.5(3) 3_576 . . . ? Gd1 Gd1 O5 C19 129.0(4) 3_576 . . . ? N3 Ni2 O6 C20 17.9(3) . . . . ? O9 Ni2 O6 C20 -166.5(3) . . . . ? O11 Ni2 O6 C20 111.2(3) . . . . ? O10 Ni2 O6 C20 -170.5(5) . . . . ? O1W Ni2 O6 C20 -70.7(3) . . . . ? N3 Ni2 O6 Gd1 -133.63(10) . . . . ? O9 Ni2 O6 Gd1 41.99(9) . . . . ? O11 Ni2 O6 Gd1 -40.31(8) . . . . ? O10 Ni2 O6 Gd1 38.0(6) . . . . ? O1W Ni2 O6 Gd1 137.81(9) . . . . ? O5 Gd1 O6 C20 45.6(3) . . . . ? O8 Gd1 O6 C20 118.3(3) . . . . ? O2 Gd1 O6 C20 -3.2(3) . . . . ? O9 Gd1 O6 C20 170.3(3) . . . . ? O3 Gd1 O6 C20 -45.4(3) . . . . ? O11 Gd1 O6 C20 -116.5(3) . . . . ? O2 Gd1 O6 C20 -125.6(3) 3_576 . . . ? Gd1 Gd1 O6 C20 -57.0(4) 3_576 . . . ? O5 Gd1 O6 Ni2 -162.15(11) . . . . ? O8 Gd1 O6 Ni2 -89.43(10) . . . . ? O2 Gd1 O6 Ni2 149.05(9) . . . . ? O9 Gd1 O6 Ni2 -37.44(8) . . . . ? O3 Gd1 O6 Ni2 106.79(9) . . . . ? O11 Gd1 O6 Ni2 35.74(8) . . . . ? O2 Gd1 O6 Ni2 26.67(18) 3_576 . . . ? Gd1 Gd1 O6 Ni2 95.23(16) 3_576 . . . ? O5 Gd1 O8 C29 135.2(4) . . . . ? O6 Gd1 O8 C29 69.6(4) . . . . ? O2 Gd1 O8 C29 -146.6(4) . . . . ? O9 Gd1 O8 C29 18.8(3) . . . . ? O3 Gd1 O8 C29 -162.0(3) . . . . ? O11 Gd1 O8 C29 -13.6(4) . . . . ? O2 Gd1 O8 C29 -78.1(4) 3_576 . . . ? Gd1 Gd1 O8 C29 -112.2(4) 3_576 . . . ? O6 Ni2 O9 C30 170.1(3) . . . . ? N3 Ni2 O9 C30 -167.5(5) . . . . ? O11 Ni2 O9 C30 -105.6(3) . . . . ? O10 Ni2 O9 C30 -10.6(3) . . . . ? O1W Ni2 O9 C30 77.4(3) . . . . ? O6 Ni2 O9 Gd1 -40.74(8) . . . . ? N3 Ni2 O9 Gd1 -18.4(6) . . . . ? O11 Ni2 O9 Gd1 43.53(8) . . . . ? O10 Ni2 O9 Gd1 138.52(9) . . . . ? O1W Ni2 O9 Gd1 -133.45(9) . . . . ? O5 Gd1 O9 C30 -116.8(3) . . . . ? O6 Gd1 O9 C30 -173.9(3) . . . . ? O8 Gd1 O9 C30 -43.2(3) . . . . ? O2 Gd1 O9 C30 -5.0(4) . . . . ? O3 Gd1 O9 C30 137.2(3) . . . . ? O11 Gd1 O9 C30 110.3(3) . . . . ? O2 Gd1 O9 C30 38.3(3) 3_576 . . . ? Gd1 Gd1 O9 C30 26.3(3) 3_576 . . . ? O5 Gd1 O9 Ni2 94.05(10) . . . . ? O6 Gd1 O9 Ni2 36.94(8) . . . . ? O8 Gd1 O9 Ni2 167.68(11) . . . . ? O2 Gd1 O9 Ni2 -154.14(15) . . . . ? O3 Gd1 O9 Ni2 -11.97(13) . . . . ? O11 Gd1 O9 Ni2 -38.85(8) . . . . ? O2 Gd1 O9 Ni2 -110.82(9) 3_576 . . . ? Gd1 Gd1 O9 Ni2 -122.87(6) 3_576 . . . ? O6 Ni2 O10 C23 17.4(7) . . . . ? N3 Ni2 O10 C23 -171.2(3) . . . . ? O9 Ni2 O10 C23 13.5(3) . . . . ? O11 Ni2 O10 C23 94.6(3) . . . . ? O1W Ni2 O10 C23 -82.9(3) . . . . ? N2 Ni1 O11 Ni2 25.6(4) . . . . ? N4 Ni1 O11 Ni2 -157.37(13) . . . . ? O3 Ni1 O11 Ni2 99.60(12) . . . . ? N1 Ni1 O11 Ni2 -71.42(14) . . . . ? N2 Ni1 O11 Gd1 -71.0(4) . . . . ? N4 Ni1 O11 Gd1 106.04(11) . . . . ? O3 Ni1 O11 Gd1 3.00(9) . . . . ? N1 Ni1 O11 Gd1 -168.02(10) . . . . ? O6 Ni2 O11 Ni1 -67.09(12) . . . . ? N3 Ni2 O11 Ni1 20.93(14) . . . . ? O9 Ni2 O11 Ni1 -148.85(13) . . . . ? O10 Ni2 O11 Ni1 123.38(12) . . . . ? O6 Ni2 O11 Gd1 38.71(8) . . . . ? N3 Ni2 O11 Gd1 126.74(11) . . . . ? O9 Ni2 O11 Gd1 -43.04(8) . . . . ? O10 Ni2 O11 Gd1 -130.81(9) . . . . ? O5 Gd1 O11 Ni1 57.18(15) . . . . ? O6 Gd1 O11 Ni1 82.27(10) . . . . ? O8 Gd1 O11 Ni1 -171.37(9) . . . . ? O2 Gd1 O11 Ni1 -49.83(12) . . . . ? O9 Gd1 O11 Ni1 155.60(12) . . . . ? O3 Gd1 O11 Ni1 -2.72(8) . . . . ? O2 Gd1 O11 Ni1 -103.27(10) 3_576 . . . ? Gd1 Gd1 O11 Ni1 -78.50(8) 3_576 . . . ? O5 Gd1 O11 Ni2 -59.99(14) . . . . ? O6 Gd1 O11 Ni2 -34.90(8) . . . . ? O8 Gd1 O11 Ni2 71.46(12) . . . . ? O2 Gd1 O11 Ni2 -167.01(7) . . . . ? O9 Gd1 O11 Ni2 38.43(8) . . . . ? O3 Gd1 O11 Ni2 -119.90(10) . . . . ? O2 Gd1 O11 Ni2 139.56(10) 3_576 . . . ? Gd1 Gd1 O11 Ni2 164.33(6) 3_576 . . . ? C11 N1 C1 C2 164.9(3) . . . . ? C21 N1 C1 C2 -74.9(4) . . . . ? Ni1 N1 C1 C2 36.3(3) . . . . ? C3 N2 C2 C1 -157.9(4) . . . . ? Ni1 N2 C2 C1 30.1(4) . . . . ? N1 C1 C2 N2 -44.3(4) . . . . ? C2 N2 C3 C4 -173.6(4) . . . . ? Ni1 N2 C3 C4 -2.7(6) . . . . ? N2 C3 C4 C5 177.9(4) . . . . ? N2 C3 C4 C10 -1.4(7) . . . . ? C10 C4 C5 C6 0.6(7) . . . . ? C3 C4 C5 C6 -178.7(4) . . . . ? C4 C5 C6 C7 1.6(8) . . . . ? C5 C6 C7 C8 0.2(7) . . . . ? C6 C7 C8 C10 -4.2(6) . . . . ? C6 C7 C8 C9 171.0(4) . . . . ? Gd1 O2 C9 O1 125.2(3) . . . . ? Gd1 O2 C9 O1 -71.5(4) 3_576 . . . ? Gd1 O2 C9 C8 -58.8(4) . . . . ? Gd1 O2 C9 C8 104.5(3) 3_576 . . . ? C7 C8 C9 O1 9.0(5) . . . . ? C10 C8 C9 O1 -176.2(3) . . . . ? C7 C8 C9 O2 -167.0(3) . . . . ? C10 C8 C9 O2 7.8(5) . . . . ? Ni1 O3 C10 C4 15.6(5) . . . . ? Gd1 O3 C10 C4 -158.0(2) . . . . ? Ni1 O3 C10 C8 -164.7(2) . . . . ? Gd1 O3 C10 C8 21.8(4) . . . . ? C5 C4 C10 O3 175.3(4) . . . . ? C3 C4 C10 O3 -5.4(6) . . . . ? C5 C4 C10 C8 -4.4(5) . . . . ? C3 C4 C10 C8 174.8(3) . . . . ? C7 C8 C10 O3 -173.7(3) . . . . ? C9 C8 C10 O3 11.6(5) . . . . ? C7 C8 C10 C4 6.1(5) . . . . ? C9 C8 C10 C4 -168.7(3) . . . . ? C1 N1 C11 C12 -52.4(4) . . . . ? C21 N1 C11 C12 -173.1(3) . . . . ? Ni1 N1 C11 C12 70.1(4) . . . . ? C13 N3 C12 C11 120.5(4) . . . . ? Ni2 N3 C12 C11 -68.1(4) . . . . ? N1 C11 C12 N3 -51.9(4) . . . . ? C12 N3 C13 C14 -172.8(4) . . . . ? Ni2 N3 C13 C14 16.4(6) . . . . ? N3 C13 C14 C15 175.9(4) . . . . ? N3 C13 C14 C20 3.0(7) . . . . ? C20 C14 C15 C16 -0.2(7) . . . . ? C13 C14 C15 C16 -173.6(5) . . . . ? C14 C15 C16 C17 1.9(9) . . . . ? C15 C16 C17 C18 -1.8(8) . . . . ? C16 C17 C18 C20 0.0(7) . . . . ? C16 C17 C18 C19 178.5(5) . . . . ? Gd1 O5 C19 O4 -172.9(3) . . . . ? Gd1 O5 C19 C18 7.3(6) . . . . ? C17 C18 C19 O4 17.4(6) . . . . ? C20 C18 C19 O4 -164.2(4) . . . . ? C17 C18 C19 O5 -162.9(4) . . . . ? C20 C18 C19 O5 15.5(6) . . . . ? Ni2 O6 C20 C18 173.6(2) . . . . ? Gd1 O6 C20 C18 -44.4(4) . . . . ? Ni2 O6 C20 C14 -6.5(5) . . . . ? Gd1 O6 C20 C14 135.5(3) . . . . ? C17 C18 C20 O6 -178.4(4) . . . . ? C19 C18 C20 O6 3.2(6) . . . . ? C17 C18 C20 C14 1.7(6) . . . . ? C19 C18 C20 C14 -176.7(4) . . . . ? C15 C14 C20 O6 178.5(4) . . . . ? C13 C14 C20 O6 -8.7(6) . . . . ? C15 C14 C20 C18 -1.6(6) . . . . ? C13 C14 C20 C18 171.3(4) . . . . ? C1 N1 C21 C22 145.0(3) . . . . ? C11 N1 C21 C22 -93.1(4) . . . . ? Ni1 N1 C21 C22 32.0(4) . . . . ? Ni1 N4 C22 C21 47.1(4) . . . . ? N1 C21 C22 N4 -55.0(4) . . . . ? Ni2 O10 C23 C24 -8.8(6) . . . . ? O10 C23 C24 C25 178.2(4) . . . . ? O10 C23 C24 C30 -5.3(7) . . . . ? C30 C24 C25 C26 0.8(6) . . . . ? C23 C24 C25 C26 177.4(4) . . . . ? C24 C25 C26 C27 -3.5(7) . . . . ? C25 C26 C27 C28 1.7(7) . . . . ? C26 C27 C28 C30 2.8(6) . . . . ? C26 C27 C28 C29 -178.7(4) . . . . ? Gd1 O8 C29 O7 -177.2(2) . . . . ? Gd1 O8 C29 C28 2.8(6) . . . . ? C27 C28 C29 O7 -16.8(5) . . . . ? C30 C28 C29 O7 161.6(3) . . . . ? C27 C28 C29 O8 163.1(3) . . . . ? C30 C28 C29 O8 -18.5(5) . . . . ? Ni2 O9 C30 C28 -176.4(2) . . . . ? Gd1 O9 C30 C28 46.0(4) . . . . ? Ni2 O9 C30 C24 1.9(5) . . . . ? Gd1 O9 C30 C24 -135.8(3) . . . . ? C27 C28 C30 O9 172.9(3) . . . . ? C29 C28 C30 O9 -5.5(5) . . . . ? C27 C28 C30 C24 -5.3(5) . . . . ? C29 C28 C30 C24 176.3(3) . . . . ? C25 C24 C30 O9 -174.6(3) . . . . ? C23 C24 C30 O9 9.0(5) . . . . ? C25 C24 C30 C28 3.7(5) . . . . ? C23 C24 C30 C28 -172.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6W H6WB O5W 0.85 2.52 3.332(13) 160.5 4_565 O5W H5WA O7 0.85 2.07 2.787(5) 142.0 4_676 O4W H4WB O5 0.85 2.20 3.015(5) 159.9 1_645 O3W H3WA O1W 0.85 2.17 2.757(4) 125.6 4_675 O2W H2WB O4 0.85 1.85 2.664(5) 158.9 1_645 O2W H2WA O1 0.85 2.12 2.933(4) 161.1 1_645 O1W H1WB O9 0.85 2.58 3.052(3) 115.9 . O1W H1WA O3W 0.85 2.23 2.757(4) 120.6 4_576 O11 H11 O1 0.98 2.08 2.948(3) 146.2 3_576 N4 H4B O8 0.90 2.52 3.118(4) 124.2 3_576 N4 H4A O7 0.90 2.57 3.281(4) 136.3 3_576 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.669 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.096 data_1248 _database_code_depnum_ccdc_archive 'CCDC 898023' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 Ho2 N8 Ni4 O24, C H4 O, 7(H2 O)' _chemical_formula_sum 'C61 H76 Ho2 N8 Ni4 O32' _chemical_formula_weight 1998.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.636(4) _cell_length_b 18.317(5) _cell_length_c 15.566(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.222(5) _cell_angle_gamma 90.00 _cell_volume 3565.8(18) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5023 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.67 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 3.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5422 _exptl_absorpt_correction_T_max 0.6356 _exptl_absorpt_process_details 'SADABS(Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18183 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6267 _reflns_number_gt 4917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2005)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2005)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^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 6267 _refine_ls_number_parameters 498 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.014 _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 Ho1 Ho 0.919384(13) 1.053968(9) 0.903764(10) 0.02296(5) Uani 1 1 d . . . Ni1 Ni 0.84316(4) 0.89431(2) 0.79190(3) 0.02800(12) Uani 1 1 d . . . Ni2 Ni 0.69199(4) 1.04909(2) 0.79276(3) 0.02652(12) Uani 1 1 d . . . C1 C 0.7469(4) 0.7862(2) 0.8858(3) 0.0479(13) Uani 1 1 d . . . H1A H 0.7018 0.8205 0.9111 0.057 Uiso 1 1 calc R . . H1B H 0.7511 0.7416 0.9197 0.057 Uiso 1 1 calc R . . C2 C 0.7003(3) 0.7703(2) 0.7938(3) 0.0438(12) Uani 1 1 d . . . H2A H 0.7409 0.7314 0.7717 0.053 Uiso 1 1 calc R . . H2B H 0.6273 0.7534 0.7924 0.053 Uiso 1 1 calc R . . C3 C 0.5979(3) 0.8749(2) 0.7325(3) 0.0362(11) Uani 1 1 d . . . H3A H 0.5922 0.8935 0.7900 0.043 Uiso 1 1 calc R . . H3B H 0.5400 0.8404 0.7174 0.043 Uiso 1 1 calc R . . C4 C 0.5822(3) 0.9382(2) 0.6686(3) 0.0405(11) Uani 1 1 d . . . H4A H 0.5749 0.9193 0.6099 0.049 Uiso 1 1 calc R . . H4B H 0.5168 0.9639 0.6755 0.049 Uiso 1 1 calc R . . C5 C 0.7246(4) 1.0015(2) 0.6186(3) 0.0467(13) Uani 1 1 d . . . H5 H 0.6979 0.9790 0.5664 0.056 Uiso 1 1 calc R . . C6 C 0.8195(4) 1.0456(2) 0.6176(3) 0.0411(12) Uani 1 1 d . . . C7 C 0.8755(3) 1.0789(2) 0.6916(2) 0.0301(10) Uani 1 1 d . . . C8 C 0.9742(3) 1.1133(2) 0.6856(3) 0.0388(11) Uani 1 1 d . . . C9 C 1.0418(3) 1.1474(2) 0.7635(3) 0.0409(11) Uani 1 1 d . . . C10 C 1.0124(4) 1.1151(3) 0.6061(3) 0.0573(14) Uani 1 1 d . . . H10 H 1.0768 1.1386 0.6022 0.069 Uiso 1 1 calc R . . C11 C 0.9578(5) 1.0834(3) 0.5340(3) 0.0748(17) Uani 1 1 d . . . H11A H 0.9844 1.0854 0.4813 0.090 Uiso 1 1 calc R . . C12 C 0.8636(5) 1.0487(3) 0.5400(3) 0.0672(16) Uani 1 1 d . . . H12 H 0.8272 1.0264 0.4908 0.081 Uiso 1 1 calc R . . C13 C 0.7211(3) 0.8116(2) 0.6482(3) 0.0435(12) Uani 1 1 d . . . H13A H 0.7013 0.8507 0.6070 0.052 Uiso 1 1 calc R . . H13B H 0.6765 0.7697 0.6300 0.052 Uiso 1 1 calc R . . C14 C 0.8376(3) 0.7916(2) 0.6471(3) 0.0469(12) Uani 1 1 d . . . H14A H 0.8523 0.7438 0.6728 0.056 Uiso 1 1 calc R . . H14B H 0.8529 0.7901 0.5878 0.056 Uiso 1 1 calc R . . C15 C 1.0016(3) 0.8535(2) 0.6819(3) 0.0406(11) Uani 1 1 d . . . H15 H 1.0196 0.8264 0.6355 0.049 Uiso 1 1 calc R . . C16 C 1.0859(3) 0.8975(2) 0.7276(3) 0.0360(11) Uani 1 1 d . . . C17 C 1.0739(3) 0.94430(19) 0.7998(2) 0.0281(9) Uani 1 1 d . . . C18 C 1.1671(3) 0.9792(2) 0.8426(2) 0.0292(10) Uani 1 1 d . . . C19 C 1.1728(3) 1.0202(2) 0.9268(2) 0.0287(9) Uani 1 1 d . . . C20 C 1.2640(3) 0.9707(3) 0.8101(3) 0.0473(12) Uani 1 1 d . . . H20 H 1.3239 0.9955 0.8370 0.057 Uiso 1 1 calc R . . C21 C 1.2742(4) 0.9265(3) 0.7394(3) 0.0605(15) Uani 1 1 d . . . H21 H 1.3398 0.9219 0.7193 0.073 Uiso 1 1 calc R . . C22 C 1.1870(4) 0.8903(3) 0.6999(3) 0.0521(13) Uani 1 1 d . . . H22 H 1.1939 0.8598 0.6532 0.063 Uiso 1 1 calc R . . C23 C 0.8689(3) 1.1901(2) 1.0401(2) 0.0326(10) Uani 1 1 d . . . C24 C 0.7513(3) 1.17348(19) 1.0329(2) 0.0293(10) Uani 1 1 d . . . C25 C 0.6974(3) 1.12923(18) 0.9644(2) 0.0240(9) Uani 1 1 d . . . C26 C 0.5878(3) 1.1125(2) 0.9657(3) 0.0328(10) Uani 1 1 d . . . C27 C 0.5274(3) 1.0624(2) 0.9075(3) 0.0394(11) Uani 1 1 d . . . H27 H 0.4584 1.0531 0.9189 0.047 Uiso 1 1 calc R . . C28 C 0.5343(3) 1.1423(2) 1.0307(3) 0.0444(12) Uani 1 1 d . . . H28 H 0.4628 1.1308 1.0314 0.053 Uiso 1 1 calc R . . C29 C 0.5850(4) 1.1877(3) 1.0927(3) 0.0536(13) Uani 1 1 d . . . H29 H 0.5478 1.2085 1.1339 0.064 Uiso 1 1 calc R . . C30 C 0.6921(3) 1.2024(2) 1.0934(3) 0.0409(11) Uani 1 1 d . . . H30 H 0.7263 1.2331 1.1363 0.049 Uiso 1 1 calc R . . N1 N 0.8551(3) 0.81739(17) 0.8869(2) 0.0411(10) Uani 1 1 d . . . H1C H 0.9016 0.7823 0.8766 0.049 Uiso 1 1 calc R . . H1D H 0.8781 0.8377 0.9388 0.049 Uiso 1 1 calc R . . N2 N 0.7006(3) 0.83536(16) 0.7362(2) 0.0345(9) Uani 1 1 d . . . N3 N 0.6727(3) 0.98947(16) 0.6822(2) 0.0312(8) Uani 1 1 d . . . N4 N 0.9051(3) 0.84681(17) 0.6969(2) 0.0366(9) Uani 1 1 d . . . O1 O 0.8361(2) 1.07926(13) 0.76547(16) 0.0309(7) Uani 1 1 d . . . O2 O 1.0299(2) 1.12709(14) 0.83922(17) 0.0382(7) Uani 1 1 d . . . O3 O 1.1082(3) 1.1944(2) 0.7502(2) 0.0901(13) Uani 1 1 d U . . O4 O 0.9784(2) 0.95569(12) 0.82316(16) 0.0289(6) Uani 1 1 d . . . O5 O 1.08931(19) 1.01595(13) 0.96840(15) 0.0261(6) Uani 1 1 d . . . O6 O 1.2546(2) 1.05273(14) 0.95768(17) 0.0384(7) Uani 1 1 d . . . O7 O 0.5536(2) 1.02937(14) 0.84383(18) 0.0381(7) Uani 1 1 d . . . O8 O 0.74718(19) 1.10643(13) 0.90141(16) 0.0294(7) Uani 1 1 d . . . O9 O 0.9289(2) 1.15104(13) 0.99897(17) 0.0346(7) Uani 1 1 d . . . O10 O 0.9046(2) 1.24238(15) 1.08771(19) 0.0476(8) Uani 1 1 d . . . O11 O 0.77876(19) 0.96848(12) 0.86124(15) 0.0258(6) Uani 1 1 d . . . H11 H 0.7586 0.9518 0.9050 0.031 Uiso 1 1 d R . . O1W O 0.6133(2) 1.13500(14) 0.72312(18) 0.0417(8) Uani 1 1 d . . . H1WA H 0.5501 1.1512 0.7225 0.050 Uiso 1 1 d R . . H1WB H 0.6175 1.1252 0.6703 0.050 Uiso 1 1 d R . . O2W O 0.2871(3) 0.1912(2) 0.8666(2) 0.0785(12) Uani 1 1 d . . . H2WA H 0.2849 0.1568 0.9029 0.094 Uiso 1 1 d R . . H2WB H 0.2410 0.1794 0.8236 0.094 Uiso 1 1 d R . . O3W O 0.4315(3) 0.1947(2) 0.7534(3) 0.1010(14) Uani 1 1 d U . . H3WA H 0.4189 0.2351 0.7271 0.121 Uiso 1 1 d R . . H3WB H 0.4625 0.2066 0.8036 0.121 Uiso 1 1 d R . . O4W O 0.0813(4) 0.2737(2) 0.9266(3) 0.0757(17) Uani 0.75 1 d P . . H4WA H 0.0751 0.2611 0.8736 0.091 Uiso 0.75 1 d PR . . H4WB H 0.0341 0.2487 0.9473 0.091 Uiso 0.75 1 d PR . . O5W O 0.5520(4) 0.1269(3) 0.5455(3) 0.0891(18) Uani 0.75 1 d P . . H5WA H 0.5938 0.0934 0.5329 0.107 Uiso 0.75 1 d PR . . H5WB H 0.5647 0.1628 0.5140 0.107 Uiso 0.75 1 d PR . . O12 O 0.8277(7) 0.3826(3) 0.0585(4) 0.077(3) Uani 0.50 1 d PD . . H12A H 0.8499 0.3421 0.0749 0.116 Uiso 0.50 1 calc PR . . C31 C 0.8180(9) 0.4222(6) 0.1240(7) 0.076(4) Uani 0.50 1 d PD . . H31A H 0.8613 0.4026 0.1744 0.115 Uiso 0.50 1 calc PR . . H31B H 0.7445 0.4229 0.1332 0.115 Uiso 0.50 1 calc PR . . H31C H 0.8409 0.4710 0.1138 0.115 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.02245(9) 0.02324(9) 0.02282(9) -0.00029(7) 0.00200(7) -0.00145(8) Ni1 0.0289(3) 0.0251(2) 0.0298(3) -0.0043(2) 0.0037(2) -0.0041(2) Ni2 0.0256(3) 0.0279(2) 0.0248(2) -0.0031(2) -0.0008(2) 0.0001(2) C1 0.049(3) 0.048(3) 0.047(3) 0.011(2) 0.008(2) -0.012(2) C2 0.034(2) 0.033(2) 0.065(3) 0.003(2) 0.008(2) -0.0069(19) C3 0.023(2) 0.038(2) 0.046(3) -0.010(2) -0.0001(19) -0.0062(18) C4 0.036(2) 0.046(2) 0.037(2) -0.007(2) -0.0044(19) -0.001(2) C5 0.070(3) 0.041(2) 0.026(2) -0.004(2) -0.002(2) 0.000(2) C6 0.059(3) 0.036(2) 0.031(2) 0.0007(19) 0.015(2) -0.001(2) C7 0.039(2) 0.0276(19) 0.025(2) 0.0052(16) 0.0083(18) 0.0068(18) C8 0.047(3) 0.036(2) 0.036(2) 0.0146(19) 0.012(2) 0.006(2) C9 0.031(2) 0.040(2) 0.052(3) 0.021(2) 0.006(2) 0.0024(19) C10 0.067(3) 0.060(3) 0.052(3) 0.013(2) 0.030(2) -0.006(3) C11 0.108(4) 0.082(4) 0.045(3) -0.008(3) 0.046(3) -0.023(4) C12 0.097(4) 0.070(3) 0.039(3) -0.012(2) 0.026(3) -0.026(3) C13 0.047(3) 0.039(2) 0.043(3) -0.015(2) 0.001(2) -0.006(2) C14 0.047(3) 0.044(2) 0.050(3) -0.021(2) 0.010(2) -0.011(2) C15 0.048(3) 0.038(2) 0.037(2) -0.0098(19) 0.009(2) -0.003(2) C16 0.033(2) 0.042(2) 0.033(2) -0.0070(19) 0.0091(18) 0.001(2) C17 0.031(2) 0.0265(19) 0.028(2) 0.0033(17) 0.0097(17) 0.0005(17) C18 0.026(2) 0.036(2) 0.026(2) 0.0012(17) 0.0067(16) -0.0060(18) C19 0.029(2) 0.031(2) 0.025(2) 0.0077(17) 0.0011(17) 0.0014(18) C20 0.028(2) 0.069(3) 0.046(3) -0.010(2) 0.010(2) -0.011(2) C21 0.033(2) 0.100(4) 0.053(3) -0.030(3) 0.023(2) -0.011(3) C22 0.048(3) 0.067(3) 0.045(3) -0.019(2) 0.020(2) 0.001(3) C23 0.044(2) 0.028(2) 0.025(2) -0.0013(17) 0.0015(18) -0.0014(19) C24 0.036(2) 0.0234(19) 0.028(2) -0.0012(16) 0.0025(17) -0.0039(17) C25 0.026(2) 0.0199(18) 0.026(2) 0.0048(15) 0.0051(16) 0.0072(16) C26 0.027(2) 0.035(2) 0.036(2) -0.0032(18) 0.0041(18) -0.0016(18) C27 0.025(2) 0.050(3) 0.044(3) -0.006(2) 0.0067(19) -0.003(2) C28 0.031(2) 0.057(3) 0.049(3) -0.014(2) 0.018(2) -0.003(2) C29 0.043(3) 0.068(3) 0.055(3) -0.027(2) 0.025(2) -0.001(2) C30 0.044(3) 0.039(2) 0.041(2) -0.014(2) 0.010(2) 0.002(2) N1 0.038(2) 0.0340(19) 0.050(2) 0.0058(17) 0.0011(17) 0.0000(16) N2 0.0323(19) 0.0255(16) 0.044(2) -0.0052(15) 0.0009(16) -0.0050(15) N3 0.0344(19) 0.0287(17) 0.0289(18) -0.0041(14) -0.0011(15) -0.0012(15) N4 0.043(2) 0.0319(18) 0.0353(19) -0.0107(15) 0.0064(16) -0.0095(16) O1 0.0300(15) 0.0372(14) 0.0250(14) 0.0038(12) 0.0025(12) 0.0007(12) O2 0.0397(16) 0.0369(15) 0.0389(16) 0.0063(13) 0.0088(13) -0.0076(13) O3 0.073(2) 0.120(3) 0.071(2) 0.054(2) -0.012(2) -0.058(2) O4 0.0264(14) 0.0295(14) 0.0314(14) -0.0045(11) 0.0065(11) -0.0043(11) O5 0.0220(13) 0.0332(14) 0.0230(13) 0.0016(11) 0.0025(11) -0.0045(12) O6 0.0283(15) 0.0531(17) 0.0331(15) -0.0074(13) 0.0024(12) -0.0140(14) O7 0.0298(15) 0.0444(16) 0.0407(17) -0.0116(13) 0.0069(13) -0.0037(13) O8 0.0255(14) 0.0337(14) 0.0291(14) -0.0094(12) 0.0040(11) -0.0015(12) O9 0.0296(15) 0.0333(14) 0.0395(16) -0.0101(13) 0.0007(13) -0.0018(13) O10 0.0406(17) 0.0490(17) 0.0536(19) -0.0261(15) 0.0086(14) -0.0117(15) O11 0.0269(14) 0.0261(13) 0.0244(13) -0.0003(11) 0.0041(11) -0.0026(11) O1W 0.0413(17) 0.0385(15) 0.0423(17) 0.0021(13) -0.0046(14) 0.0072(14) O2W 0.063(2) 0.097(3) 0.073(2) 0.022(2) -0.001(2) -0.023(2) O3W 0.092(3) 0.126(3) 0.089(3) 0.052(2) 0.030(2) 0.058(2) O4W 0.130(4) 0.043(2) 0.047(3) -0.001(2) -0.010(3) -0.009(3) O5W 0.108(4) 0.125(4) 0.029(3) 0.006(3) -0.009(3) -0.014(4) O12 0.157(7) 0.039(4) 0.034(4) 0.003(3) 0.006(4) 0.017(4) C31 0.069(8) 0.061(7) 0.094(9) 0.000(6) -0.006(7) 0.019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O2 2.271(3) . y Ho1 O1 2.304(2) . y Ho1 O9 2.307(3) . y Ho1 O5 2.343(2) . y Ho1 O8 2.374(3) . y Ho1 O4 2.375(2) . y Ho1 O5 2.382(2) 3_777 y Ho1 O11 2.390(2) . y Ho1 Ni2 3.1352(9) . y Ho1 Ni1 3.4687(9) . y Ni1 N4 1.972(3) . y Ni1 O11 1.981(2) . y Ni1 N1 2.032(3) . y Ni1 O4 2.045(3) . y Ni1 N2 2.171(3) . y Ni2 O1 2.005(3) . y Ni2 N3 2.023(3) . y Ni2 O8 2.028(2) . y Ni2 O11 2.046(2) . y Ni2 O7 2.054(3) . y Ni2 O1W 2.081(3) . y C1 N1 1.480(5) . ? C1 C2 1.497(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.491(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.481(5) . ? C3 C4 1.521(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.472(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.284(5) . ? C5 C6 1.447(6) . ? C5 H5 0.9300 . ? C6 C7 1.402(5) . ? C6 C12 1.402(6) . ? C7 O1 1.317(5) . ? C7 C8 1.412(6) . ? C8 C10 1.391(6) . ? C8 C9 1.514(6) . ? C9 O3 1.240(5) . ? C9 O2 1.265(5) . ? C10 C11 1.361(7) . ? C10 H10 0.9300 . ? C11 C12 1.365(8) . ? C11 H11A 0.9300 . ? C12 H12 0.9300 . ? C13 N2 1.494(5) . ? C13 C14 1.520(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.470(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.279(5) . ? C15 C16 1.441(5) . ? C15 H15 0.9300 . ? C16 C22 1.412(6) . ? C16 C17 1.437(5) . ? C17 O4 1.326(5) . ? C17 C18 1.420(5) . ? C18 C20 1.398(6) . ? C18 C19 1.505(5) . ? C19 O6 1.229(4) . ? C19 O5 1.316(4) . ? C20 C21 1.387(6) . ? C20 H20 0.9300 . ? C21 C22 1.357(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O10 1.255(4) . ? C23 O9 1.279(5) . ? C23 C24 1.505(6) . ? C24 C30 1.388(6) . ? C24 C25 1.432(5) . ? C25 O8 1.307(4) . ? C25 C26 1.421(5) . ? C26 C28 1.405(6) . ? C26 C27 1.432(5) . ? C27 O7 1.245(5) . ? C27 H27 0.9300 . ? C28 C29 1.362(6) . ? C28 H28 0.9300 . ? C29 C30 1.379(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? O5 Ho1 2.382(2) 3_777 y O11 H11 0.8200 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O12 C31 1.272(10) . ? O12 H12A 0.8200 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ho1 O1 72.29(9) . . y O2 Ho1 O9 81.42(10) . . y O1 Ho1 O9 114.84(9) . . y O2 Ho1 O5 77.37(9) . . y O1 Ho1 O5 136.82(9) . . y O9 Ho1 O5 89.59(9) . . y O2 Ho1 O8 112.02(9) . . y O1 Ho1 O8 66.98(9) . . y O9 Ho1 O8 70.20(8) . . y O5 Ho1 O8 155.30(8) . . y O2 Ho1 O4 87.35(9) . . y O1 Ho1 O4 78.16(9) . . y O9 Ho1 O4 158.81(9) . . y O5 Ho1 O4 70.36(8) . . y O8 Ho1 O4 130.93(8) . . y O2 Ho1 O5 142.33(9) . 3_777 y O1 Ho1 O5 144.99(9) . 3_777 y O9 Ho1 O5 83.23(9) . 3_777 y O5 Ho1 O5 68.31(10) . 3_777 y O8 Ho1 O5 94.52(8) . 3_777 y O4 Ho1 O5 95.12(8) . 3_777 y O2 Ho1 O11 138.08(9) . . y O1 Ho1 O11 69.55(9) . . y O9 Ho1 O11 130.64(9) . . y O5 Ho1 O11 121.58(8) . . y O8 Ho1 O11 67.51(8) . . y O4 Ho1 O11 68.54(9) . . y O5 Ho1 O11 75.98(8) 3_777 . y O2 Ho1 Ni2 110.26(7) . . y O1 Ho1 Ni2 39.69(7) . . y O9 Ho1 Ni2 109.60(6) . . y O5 Ho1 Ni2 159.98(6) . . y O8 Ho1 Ni2 40.30(6) . . y O4 Ho1 Ni2 91.12(6) . . y O5 Ho1 Ni2 107.28(6) 3_777 . y O11 Ho1 Ni2 40.73(6) . . y O2 Ho1 Ni1 114.80(7) . . y O1 Ho1 Ni1 69.12(6) . . y O9 Ho1 Ni1 163.24(7) . . y O5 Ho1 Ni1 97.85(6) . . y O8 Ho1 Ni1 98.36(6) . . y O4 Ho1 Ni1 35.04(6) . . y O5 Ho1 Ni1 85.61(6) 3_777 . y O11 Ho1 Ni1 33.54(6) . . y Ni2 Ho1 Ni1 62.130(14) . . y O2 Ho1 Ho1 110.56(7) . 3_777 y O1 Ho1 Ho1 159.37(6) . 3_777 y O9 Ho1 Ho1 85.64(7) . 3_777 y O5 Ho1 Ho1 34.48(6) . 3_777 y O8 Ho1 Ho1 126.33(6) . 3_777 y O4 Ho1 Ho1 81.55(6) . 3_777 y O5 Ho1 Ho1 33.83(6) 3_777 3_777 y O11 Ho1 Ho1 99.57(6) . 3_777 y Ni2 Ho1 Ho1 138.064(13) . 3_777 y Ni1 Ho1 Ho1 92.02(2) . 3_777 y N4 Ni1 O11 161.68(12) . . y N4 Ni1 N1 104.09(14) . . y O11 Ni1 N1 94.18(12) . . y N4 Ni1 O4 90.77(12) . . y O11 Ni1 O4 83.55(10) . . y N1 Ni1 O4 103.62(12) . . y N4 Ni1 N2 82.89(13) . . y O11 Ni1 N2 100.19(11) . . y N1 Ni1 N2 85.23(12) . . y O4 Ni1 N2 170.20(11) . . y N4 Ni1 Ho1 129.58(10) . . y O11 Ni1 Ho1 41.80(7) . . y N1 Ni1 Ho1 103.48(10) . . y O4 Ni1 Ho1 41.81(7) . . y N2 Ni1 Ho1 140.78(9) . . y O1 Ni2 N3 88.35(12) . . y O1 Ni2 O8 79.61(10) . . y N3 Ni2 O8 166.94(12) . . y O1 Ni2 O11 82.76(10) . . y N3 Ni2 O11 92.51(11) . . y O8 Ni2 O11 81.05(10) . . y O1 Ni2 O7 168.38(10) . . y N3 Ni2 O7 103.21(12) . . y O8 Ni2 O7 88.77(10) . . y O11 Ni2 O7 95.39(11) . . y O1 Ni2 O1W 93.56(11) . . y N3 Ni2 O1W 88.56(12) . . y O8 Ni2 O1W 97.15(10) . . y O11 Ni2 O1W 176.14(11) . . y O7 Ni2 O1W 87.97(11) . . y O1 Ni2 Ho1 47.21(7) . . y N3 Ni2 Ho1 118.26(9) . . y O8 Ni2 Ho1 49.22(7) . . y O11 Ni2 Ho1 49.66(7) . . y O7 Ni2 Ho1 123.75(8) . . y O1W Ni2 Ho1 126.70(8) . . y N1 C1 C2 108.8(4) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 112.7(3) . . ? N2 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N2 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N2 C3 C4 115.4(3) . . ? N2 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? N2 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? N3 C4 C3 111.5(3) . . ? N3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N3 C5 C6 128.2(4) . . ? N3 C5 H5 115.9 . . ? C6 C5 H5 115.9 . . ? C7 C6 C12 118.3(4) . . ? C7 C6 C5 123.8(4) . . ? C12 C6 C5 117.6(4) . . ? O1 C7 C6 120.6(4) . . ? O1 C7 C8 120.2(3) . . ? C6 C7 C8 119.2(4) . . ? C10 C8 C7 119.4(4) . . ? C10 C8 C9 118.3(4) . . ? C7 C8 C9 122.3(4) . . ? O3 C9 O2 122.2(4) . . ? O3 C9 C8 118.0(4) . . ? O2 C9 C8 119.7(4) . . ? C11 C10 C8 121.7(5) . . ? C11 C10 H10 119.2 . . ? C8 C10 H10 119.2 . . ? C10 C11 C12 119.1(5) . . ? C10 C11 H11A 120.5 . . ? C12 C11 H11A 120.5 . . ? C11 C12 C6 122.4(5) . . ? C11 C12 H12 118.8 . . ? C6 C12 H12 118.8 . . ? N2 C13 C14 112.0(3) . . ? N2 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? N2 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N4 C14 C13 108.5(3) . . ? N4 C14 H14A 110.0 . . ? C13 C14 H14A 110.0 . . ? N4 C14 H14B 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? N4 C15 C16 128.3(4) . . ? N4 C15 H15 115.8 . . ? C16 C15 H15 115.8 . . ? C22 C16 C17 119.8(4) . . ? C22 C16 C15 115.7(4) . . ? C17 C16 C15 124.5(4) . . ? O4 C17 C18 121.8(3) . . ? O4 C17 C16 120.7(3) . . ? C18 C17 C16 117.5(4) . . ? C20 C18 C17 119.4(4) . . ? C20 C18 C19 115.8(3) . . ? C17 C18 C19 124.5(3) . . ? O6 C19 O5 121.6(3) . . ? O6 C19 C18 121.0(4) . . ? O5 C19 C18 117.2(3) . . ? C21 C20 C18 122.5(4) . . ? C21 C20 H20 118.8 . . ? C18 C20 H20 118.8 . . ? C22 C21 C20 118.9(4) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C16 121.8(4) . . ? C21 C22 H22 119.1 . . ? C16 C22 H22 119.1 . . ? O10 C23 O9 122.2(4) . . ? O10 C23 C24 117.8(4) . . ? O9 C23 C24 120.0(3) . . ? C30 C24 C25 118.5(4) . . ? C30 C24 C23 119.6(3) . . ? C25 C24 C23 121.9(3) . . ? O8 C25 C26 121.1(3) . . ? O8 C25 C24 120.7(3) . . ? C26 C25 C24 118.2(3) . . ? C28 C26 C25 119.7(3) . . ? C28 C26 C27 116.0(4) . . ? C25 C26 C27 124.2(4) . . ? O7 C27 C26 129.6(4) . . ? O7 C27 H27 115.2 . . ? C26 C27 H27 115.2 . . ? C29 C28 C26 121.5(4) . . ? C29 C28 H28 119.3 . . ? C26 C28 H28 119.3 . . ? C28 C29 C30 119.1(4) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C24 122.9(4) . . ? C29 C30 H30 118.6 . . ? C24 C30 H30 118.6 . . ? C1 N1 Ni1 106.7(2) . . ? C1 N1 H1C 110.4 . . ? Ni1 N1 H1C 110.4 . . ? C1 N1 H1D 110.4 . . ? Ni1 N1 H1D 110.4 . . ? H1C N1 H1D 108.6 . . ? C3 N2 C2 109.6(3) . . ? C3 N2 C13 111.9(3) . . ? C2 N2 C13 109.5(3) . . ? C3 N2 Ni1 116.4(2) . . ? C2 N2 Ni1 103.3(2) . . ? C13 N2 Ni1 105.6(2) . . ? C5 N3 C4 118.1(3) . . ? C5 N3 Ni2 123.5(3) . . ? C4 N3 Ni2 117.6(3) . . ? C15 N4 C14 117.8(3) . . ? C15 N4 Ni1 125.8(3) . . ? C14 N4 Ni1 115.9(3) . . ? C7 O1 Ni2 130.7(2) . . ? C7 O1 Ho1 129.4(2) . . ? Ni2 O1 Ho1 93.10(10) . . ? C9 O2 Ho1 138.4(3) . . ? C17 O4 Ni1 127.6(2) . . ? C17 O4 Ho1 129.2(2) . . ? Ni1 O4 Ho1 103.16(11) . . ? C19 O5 Ho1 121.4(2) . . ? C19 O5 Ho1 125.3(2) . 3_777 ? Ho1 O5 Ho1 111.69(10) . 3_777 ? C27 O7 Ni2 124.1(3) . . ? C25 O8 Ni2 130.3(2) . . ? C25 O8 Ho1 131.0(2) . . ? Ni2 O8 Ho1 90.48(9) . . ? C23 O9 Ho1 140.6(2) . . ? Ni1 O11 Ni2 116.26(12) . . ? Ni1 O11 Ho1 104.67(11) . . ? Ni2 O11 Ho1 89.61(9) . . ? Ni1 O11 H11 113.5 . . ? Ni2 O11 H11 119.6 . . ? Ho1 O11 H11 108.7 . . ? Ni2 O1W H1WA 130.4 . . ? Ni2 O1W H1WB 104.6 . . ? H1WA O1W H1WB 104.5 . . ? H2WA O2W H2WB 104.5 . . ? H3WA O3W H3WB 104.5 . . ? H4WA O4W H4WB 104.5 . . ? H5WA O5W H5WB 104.5 . . ? C31 O12 H12A 109.5 . . ? O12 C31 H31A 109.5 . . ? O12 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O12 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ho1 Ni1 N4 15.57(14) . . . . ? O1 Ho1 Ni1 N4 73.23(14) . . . . ? O9 Ho1 Ni1 N4 -179.8(2) . . . . ? O5 Ho1 Ni1 N4 -64.09(14) . . . . ? O8 Ho1 Ni1 N4 134.60(14) . . . . ? O4 Ho1 Ni1 N4 -26.06(16) . . . . ? O5 Ho1 Ni1 N4 -131.46(14) 3_777 . . . ? O11 Ho1 Ni1 N4 157.43(16) . . . . ? Ni2 Ho1 Ni1 N4 116.35(13) . . . . ? Ho1 Ho1 Ni1 N4 -98.22(12) 3_777 . . . ? O2 Ho1 Ni1 O11 -141.86(12) . . . . ? O1 Ho1 Ni1 O11 -84.19(12) . . . . ? O9 Ho1 Ni1 O11 22.8(2) . . . . ? O5 Ho1 Ni1 O11 138.48(12) . . . . ? O8 Ho1 Ni1 O11 -22.83(12) . . . . ? O4 Ho1 Ni1 O11 176.51(14) . . . . ? O5 Ho1 Ni1 O11 71.11(11) 3_777 . . . ? Ni2 Ho1 Ni1 O11 -41.07(10) . . . . ? Ho1 Ho1 Ni1 O11 104.35(10) 3_777 . . . ? O2 Ho1 Ni1 N1 137.10(13) . . . . ? O1 Ho1 Ni1 N1 -165.24(12) . . . . ? O9 Ho1 Ni1 N1 -58.2(2) . . . . ? O5 Ho1 Ni1 N1 57.44(12) . . . . ? O8 Ho1 Ni1 N1 -103.87(12) . . . . ? O4 Ho1 Ni1 N1 95.47(14) . . . . ? O5 Ho1 Ni1 N1 -9.93(12) 3_777 . . . ? O11 Ho1 Ni1 N1 -81.04(14) . . . . ? Ni2 Ho1 Ni1 N1 -122.11(10) . . . . ? Ho1 Ho1 Ni1 N1 23.31(10) 3_777 . . . ? O2 Ho1 Ni1 O4 41.63(13) . . . . ? O1 Ho1 Ni1 O4 99.30(12) . . . . ? O9 Ho1 Ni1 O4 -153.7(2) . . . . ? O5 Ho1 Ni1 O4 -38.03(12) . . . . ? O8 Ho1 Ni1 O4 160.66(12) . . . . ? O5 Ho1 Ni1 O4 -105.40(12) 3_777 . . . ? O11 Ho1 Ni1 O4 -176.51(14) . . . . ? Ni2 Ho1 Ni1 O4 142.42(10) . . . . ? Ho1 Ho1 Ni1 O4 -72.15(10) 3_777 . . . ? O2 Ho1 Ni1 N2 -123.79(16) . . . . ? O1 Ho1 Ni1 N2 -66.12(15) . . . . ? O9 Ho1 Ni1 N2 40.9(3) . . . . ? O5 Ho1 Ni1 N2 156.55(15) . . . . ? O8 Ho1 Ni1 N2 -4.76(15) . . . . ? O4 Ho1 Ni1 N2 -165.42(17) . . . . ? O5 Ho1 Ni1 N2 89.18(15) 3_777 . . . ? O11 Ho1 Ni1 N2 18.07(17) . . . . ? Ni2 Ho1 Ni1 N2 -23.00(14) . . . . ? Ho1 Ho1 Ni1 N2 122.42(14) 3_777 . . . ? O2 Ho1 Ni2 O1 17.76(12) . . . . ? O9 Ho1 Ni2 O1 105.62(12) . . . . ? O5 Ho1 Ni2 O1 -91.6(2) . . . . ? O8 Ho1 Ni2 O1 118.29(14) . . . . ? O4 Ho1 Ni2 O1 -69.83(12) . . . . ? O5 Ho1 Ni2 O1 -165.54(12) 3_777 . . . ? O11 Ho1 Ni2 O1 -124.13(13) . . . . ? Ni1 Ho1 Ni2 O1 -90.33(10) . . . . ? Ho1 Ho1 Ni2 O1 -148.39(10) 3_777 . . . ? O2 Ho1 Ni2 N3 74.93(13) . . . . ? O1 Ho1 Ni2 N3 57.16(14) . . . . ? O9 Ho1 Ni2 N3 162.78(12) . . . . ? O5 Ho1 Ni2 N3 -34.5(2) . . . . ? O8 Ho1 Ni2 N3 175.45(14) . . . . ? O4 Ho1 Ni2 N3 -12.66(12) . . . . ? O5 Ho1 Ni2 N3 -108.38(12) 3_777 . . . ? O11 Ho1 Ni2 N3 -66.97(14) . . . . ? Ni1 Ho1 Ni2 N3 -33.17(10) . . . . ? Ho1 Ho1 Ni2 N3 -91.22(11) 3_777 . . . ? O2 Ho1 Ni2 O8 -100.52(12) . . . . ? O1 Ho1 Ni2 O8 -118.29(14) . . . . ? O9 Ho1 Ni2 O8 -12.67(12) . . . . ? O5 Ho1 Ni2 O8 150.1(2) . . . . ? O4 Ho1 Ni2 O8 171.89(11) . . . . ? O5 Ho1 Ni2 O8 76.17(11) 3_777 . . . ? O11 Ho1 Ni2 O8 117.58(13) . . . . ? Ni1 Ho1 Ni2 O8 151.39(10) . . . . ? Ho1 Ho1 Ni2 O8 93.33(10) 3_777 . . . ? O2 Ho1 Ni2 O11 141.89(12) . . . . ? O1 Ho1 Ni2 O11 124.13(13) . . . . ? O9 Ho1 Ni2 O11 -130.25(12) . . . . ? O5 Ho1 Ni2 O11 32.5(2) . . . . ? O8 Ho1 Ni2 O11 -117.58(13) . . . . ? O4 Ho1 Ni2 O11 54.30(11) . . . . ? O5 Ho1 Ni2 O11 -41.41(11) 3_777 . . . ? Ni1 Ho1 Ni2 O11 33.80(9) . . . . ? Ho1 Ho1 Ni2 O11 -24.26(9) 3_777 . . . ? O2 Ho1 Ni2 O7 -152.90(12) . . . . ? O1 Ho1 Ni2 O7 -170.67(14) . . . . ? O9 Ho1 Ni2 O7 -65.05(12) . . . . ? O5 Ho1 Ni2 O7 97.7(2) . . . . ? O8 Ho1 Ni2 O7 -52.38(13) . . . . ? O4 Ho1 Ni2 O7 119.51(11) . . . . ? O5 Ho1 Ni2 O7 23.79(11) 3_777 . . . ? O11 Ho1 Ni2 O7 65.20(13) . . . . ? Ni1 Ho1 Ni2 O7 99.01(9) . . . . ? Ho1 Ho1 Ni2 O7 40.95(9) 3_777 . . . ? O2 Ho1 Ni2 O1W -36.48(13) . . . . ? O1 Ho1 Ni2 O1W -54.25(14) . . . . ? O9 Ho1 Ni2 O1W 51.37(13) . . . . ? O5 Ho1 Ni2 O1W -145.9(2) . . . . ? O8 Ho1 Ni2 O1W 64.04(14) . . . . ? O4 Ho1 Ni2 O1W -124.07(12) . . . . ? O5 Ho1 Ni2 O1W 140.21(12) 3_777 . . . ? O11 Ho1 Ni2 O1W -178.38(14) . . . . ? Ni1 Ho1 Ni2 O1W -144.57(11) . . . . ? Ho1 Ho1 Ni2 O1W 157.37(10) 3_777 . . . ? N1 C1 C2 N2 -54.4(5) . . . . ? N2 C3 C4 N3 -52.7(4) . . . . ? N3 C5 C6 C7 5.0(7) . . . . ? N3 C5 C6 C12 178.3(5) . . . . ? C12 C6 C7 O1 178.0(4) . . . . ? C5 C6 C7 O1 -8.7(6) . . . . ? C12 C6 C7 C8 -0.8(6) . . . . ? C5 C6 C7 C8 172.4(4) . . . . ? O1 C7 C8 C10 -177.2(4) . . . . ? C6 C7 C8 C10 1.6(6) . . . . ? O1 C7 C8 C9 4.0(6) . . . . ? C6 C7 C8 C9 -177.1(4) . . . . ? C10 C8 C9 O3 22.6(6) . . . . ? C7 C8 C9 O3 -158.6(4) . . . . ? C10 C8 C9 O2 -156.8(4) . . . . ? C7 C8 C9 O2 22.0(6) . . . . ? C7 C8 C10 C11 -1.1(7) . . . . ? C9 C8 C10 C11 177.7(4) . . . . ? C8 C10 C11 C12 -0.3(8) . . . . ? C10 C11 C12 C6 1.2(9) . . . . ? C7 C6 C12 C11 -0.6(8) . . . . ? C5 C6 C12 C11 -174.2(5) . . . . ? N2 C13 C14 N4 -43.3(5) . . . . ? N4 C15 C16 C22 176.0(4) . . . . ? N4 C15 C16 C17 -1.3(7) . . . . ? C22 C16 C17 O4 175.5(4) . . . . ? C15 C16 C17 O4 -7.4(6) . . . . ? C22 C16 C17 C18 -2.6(6) . . . . ? C15 C16 C17 C18 174.6(4) . . . . ? O4 C17 C18 C20 -174.0(4) . . . . ? C16 C17 C18 C20 4.0(5) . . . . ? O4 C17 C18 C19 11.9(6) . . . . ? C16 C17 C18 C19 -170.1(3) . . . . ? C20 C18 C19 O6 10.0(5) . . . . ? C17 C18 C19 O6 -175.7(3) . . . . ? C20 C18 C19 O5 -165.9(3) . . . . ? C17 C18 C19 O5 8.4(5) . . . . ? C17 C18 C20 C21 -2.9(7) . . . . ? C19 C18 C20 C21 171.7(4) . . . . ? C18 C20 C21 C22 0.1(8) . . . . ? C20 C21 C22 C16 1.4(8) . . . . ? C17 C16 C22 C21 -0.1(7) . . . . ? C15 C16 C22 C21 -177.6(4) . . . . ? O10 C23 C24 C30 -16.1(5) . . . . ? O9 C23 C24 C30 163.3(4) . . . . ? O10 C23 C24 C25 163.0(3) . . . . ? O9 C23 C24 C25 -17.6(5) . . . . ? C30 C24 C25 O8 173.5(3) . . . . ? C23 C24 C25 O8 -5.6(5) . . . . ? C30 C24 C25 C26 -4.8(5) . . . . ? C23 C24 C25 C26 176.1(3) . . . . ? O8 C25 C26 C28 -175.2(3) . . . . ? C24 C25 C26 C28 3.1(5) . . . . ? O8 C25 C26 C27 9.2(6) . . . . ? C24 C25 C26 C27 -172.5(4) . . . . ? C28 C26 C27 O7 178.4(4) . . . . ? C25 C26 C27 O7 -5.8(7) . . . . ? C25 C26 C28 C29 0.6(6) . . . . ? C27 C26 C28 C29 176.5(4) . . . . ? C26 C28 C29 C30 -2.5(7) . . . . ? C28 C29 C30 C24 0.6(7) . . . . ? C25 C24 C30 C29 3.0(6) . . . . ? C23 C24 C30 C29 -177.9(4) . . . . ? C2 C1 N1 Ni1 45.8(4) . . . . ? N4 Ni1 N1 C1 -103.5(3) . . . . ? O11 Ni1 N1 C1 77.9(3) . . . . ? O4 Ni1 N1 C1 162.2(3) . . . . ? N2 Ni1 N1 C1 -22.0(3) . . . . ? Ho1 Ni1 N1 C1 119.2(2) . . . . ? C4 C3 N2 C2 -173.9(3) . . . . ? C4 C3 N2 C13 -52.2(4) . . . . ? C4 C3 N2 Ni1 69.3(4) . . . . ? C1 C2 N2 C3 -92.3(4) . . . . ? C1 C2 N2 C13 144.6(4) . . . . ? C1 C2 N2 Ni1 32.4(4) . . . . ? C14 C13 N2 C3 163.1(3) . . . . ? C14 C13 N2 C2 -75.1(4) . . . . ? C14 C13 N2 Ni1 35.6(4) . . . . ? N4 Ni1 N2 C3 -140.1(3) . . . . ? O11 Ni1 N2 C3 21.7(3) . . . . ? N1 Ni1 N2 C3 115.1(3) . . . . ? Ho1 Ni1 N2 C3 9.5(3) . . . . ? N4 Ni1 N2 C2 99.7(3) . . . . ? O11 Ni1 N2 C2 -98.6(2) . . . . ? N1 Ni1 N2 C2 -5.2(3) . . . . ? Ho1 Ni1 N2 C2 -110.7(2) . . . . ? N4 Ni1 N2 C13 -15.3(2) . . . . ? O11 Ni1 N2 C13 146.4(2) . . . . ? N1 Ni1 N2 C13 -120.2(2) . . . . ? Ho1 Ni1 N2 C13 134.3(2) . . . . ? C6 C5 N3 C4 -175.8(4) . . . . ? C6 C5 N3 Ni2 14.8(6) . . . . ? C3 C4 N3 C5 121.6(4) . . . . ? C3 C4 N3 Ni2 -68.4(4) . . . . ? O1 Ni2 N3 C5 -21.7(3) . . . . ? O8 Ni2 N3 C5 -44.4(7) . . . . ? O11 Ni2 N3 C5 -104.4(3) . . . . ? O7 Ni2 N3 C5 159.5(3) . . . . ? O1W Ni2 N3 C5 71.9(3) . . . . ? Ho1 Ni2 N3 C5 -59.8(3) . . . . ? O1 Ni2 N3 C4 168.9(3) . . . . ? O8 Ni2 N3 C4 146.2(5) . . . . ? O11 Ni2 N3 C4 86.2(3) . . . . ? O7 Ni2 N3 C4 -9.9(3) . . . . ? O1W Ni2 N3 C4 -97.5(3) . . . . ? Ho1 Ni2 N3 C4 130.8(2) . . . . ? C16 C15 N4 C14 -172.9(4) . . . . ? C16 C15 N4 Ni1 -1.9(6) . . . . ? C13 C14 N4 C15 -158.5(4) . . . . ? C13 C14 N4 Ni1 29.5(4) . . . . ? O11 Ni1 N4 C15 79.7(5) . . . . ? N1 Ni1 N4 C15 -96.0(3) . . . . ? O4 Ni1 N4 C15 8.2(3) . . . . ? N2 Ni1 N4 C15 -179.3(4) . . . . ? Ho1 Ni1 N4 C15 25.2(4) . . . . ? O11 Ni1 N4 C14 -109.0(4) . . . . ? N1 Ni1 N4 C14 75.2(3) . . . . ? O4 Ni1 N4 C14 179.4(3) . . . . ? N2 Ni1 N4 C14 -8.0(3) . . . . ? Ho1 Ni1 N4 C14 -163.5(2) . . . . ? C6 C7 O1 Ni2 -8.6(5) . . . . ? C8 C7 O1 Ni2 170.2(3) . . . . ? C6 C7 O1 Ho1 134.5(3) . . . . ? C8 C7 O1 Ho1 -46.7(5) . . . . ? N3 Ni2 O1 C7 20.1(3) . . . . ? O8 Ni2 O1 C7 -165.0(3) . . . . ? O11 Ni2 O1 C7 112.8(3) . . . . ? O7 Ni2 O1 C7 -165.7(5) . . . . ? O1W Ni2 O1 C7 -68.4(3) . . . . ? Ho1 Ni2 O1 C7 152.3(3) . . . . ? N3 Ni2 O1 Ho1 -132.24(11) . . . . ? O8 Ni2 O1 Ho1 42.68(9) . . . . ? O11 Ni2 O1 Ho1 -39.49(9) . . . . ? O7 Ni2 O1 Ho1 42.0(6) . . . . ? O1W Ni2 O1 Ho1 139.31(10) . . . . ? O2 Ho1 O1 C7 44.6(3) . . . . ? O9 Ho1 O1 C7 116.0(3) . . . . ? O5 Ho1 O1 C7 -2.9(3) . . . . ? O8 Ho1 O1 C7 168.9(3) . . . . ? O4 Ho1 O1 C7 -46.4(3) . . . . ? O5 Ho1 O1 C7 -128.3(3) 3_777 . . . ? O11 Ho1 O1 C7 -117.6(3) . . . . ? Ni2 Ho1 O1 C7 -152.8(3) . . . . ? Ni1 Ho1 O1 C7 -81.7(3) . . . . ? Ho1 Ho1 O1 C7 -56.8(4) 3_777 . . . ? O2 Ho1 O1 Ni2 -162.51(12) . . . . ? O9 Ho1 O1 Ni2 -91.20(11) . . . . ? O5 Ho1 O1 Ni2 149.99(9) . . . . ? O8 Ho1 O1 Ni2 -38.23(9) . . . . ? O4 Ho1 O1 Ni2 106.49(10) . . . . ? O5 Ho1 O1 Ni2 24.55(19) 3_777 . . . ? O11 Ho1 O1 Ni2 35.20(9) . . . . ? Ni1 Ho1 O1 Ni2 71.11(7) . . . . ? Ho1 Ho1 O1 Ni2 96.05(19) 3_777 . . . ? O3 C9 O2 Ho1 174.0(3) . . . . ? C8 C9 O2 Ho1 -6.6(6) . . . . ? O1 Ho1 O2 C9 -17.5(4) . . . . ? O9 Ho1 O2 C9 -137.1(4) . . . . ? O5 Ho1 O2 C9 131.4(4) . . . . ? O8 Ho1 O2 C9 -72.6(4) . . . . ? O4 Ho1 O2 C9 60.9(4) . . . . ? O5 Ho1 O2 C9 155.8(4) 3_777 . . . ? O11 Ho1 O2 C9 7.7(4) . . . . ? Ni2 Ho1 O2 C9 -29.3(4) . . . . ? Ni1 Ho1 O2 C9 38.4(4) . . . . ? Ho1 Ho1 O2 C9 140.8(4) 3_777 . . . ? C18 C17 O4 Ni1 -163.8(3) . . . . ? C16 C17 O4 Ni1 18.2(5) . . . . ? C18 C17 O4 Ho1 19.9(5) . . . . ? C16 C17 O4 Ho1 -158.0(3) . . . . ? N4 Ni1 O4 C17 -16.8(3) . . . . ? O11 Ni1 O4 C17 -179.4(3) . . . . ? N1 Ni1 O4 C17 87.9(3) . . . . ? Ho1 Ni1 O4 C17 -177.0(3) . . . . ? N4 Ni1 O4 Ho1 160.20(12) . . . . ? O11 Ni1 O4 Ho1 -2.34(10) . . . . ? N1 Ni1 O4 Ho1 -95.09(13) . . . . ? N2 Ni1 O4 Ho1 110.8(6) . . . . ? O2 Ho1 O4 C17 34.1(3) . . . . ? O1 Ho1 O4 C17 106.6(3) . . . . ? O9 Ho1 O4 C17 -23.7(4) . . . . ? O5 Ho1 O4 C17 -43.4(3) . . . . ? O8 Ho1 O4 C17 151.3(3) . . . . ? O5 Ho1 O4 C17 -108.2(3) 3_777 . . . ? O11 Ho1 O4 C17 179.1(3) . . . . ? Ni2 Ho1 O4 C17 144.4(3) . . . . ? Ni1 Ho1 O4 C17 177.0(3) . . . . ? Ho1 Ho1 O4 C17 -77.1(3) 3_777 . . . ? O2 Ho1 O4 Ni1 -142.86(11) . . . . ? O1 Ho1 O4 Ni1 -70.40(10) . . . . ? O9 Ho1 O4 Ni1 159.3(2) . . . . ? O5 Ho1 O4 Ni1 139.61(12) . . . . ? O8 Ho1 O4 Ni1 -25.69(15) . . . . ? O5 Ho1 O4 Ni1 74.82(10) 3_777 . . . ? O11 Ho1 O4 Ni1 2.07(8) . . . . ? Ni2 Ho1 O4 Ni1 -32.63(9) . . . . ? Ho1 Ho1 O4 Ni1 105.90(9) 3_777 . . . ? O6 C19 O5 Ho1 125.1(3) . . . . ? C18 C19 O5 Ho1 -59.0(4) . . . . ? O6 C19 O5 Ho1 -70.4(4) . . . 3_777 ? C18 C19 O5 Ho1 105.4(3) . . . 3_777 ? O2 Ho1 O5 C19 -29.4(2) . . . . ? O1 Ho1 O5 C19 16.6(3) . . . . ? O9 Ho1 O5 C19 -110.7(3) . . . . ? O8 Ho1 O5 C19 -145.0(3) . . . . ? O4 Ho1 O5 C19 62.3(3) . . . . ? O5 Ho1 O5 C19 166.4(3) 3_777 . . . ? O11 Ho1 O5 C19 109.8(3) . . . . ? Ni2 Ho1 O5 C19 85.5(3) . . . . ? Ni1 Ho1 O5 C19 84.3(2) . . . . ? Ho1 Ho1 O5 C19 166.4(3) 3_777 . . . ? O2 Ho1 O5 Ho1 164.17(12) . . . 3_777 ? O1 Ho1 O5 Ho1 -149.80(10) . . . 3_777 ? O9 Ho1 O5 Ho1 82.88(11) . . . 3_777 ? O8 Ho1 O5 Ho1 48.6(2) . . . 3_777 ? O4 Ho1 O5 Ho1 -104.12(11) . . . 3_777 ? O5 Ho1 O5 Ho1 0.0 3_777 . . 3_777 ? O11 Ho1 O5 Ho1 -56.61(13) . . . 3_777 ? Ni2 Ho1 O5 Ho1 -80.9(2) . . . 3_777 ? Ni1 Ho1 O5 Ho1 -82.06(9) . . . 3_777 ? C26 C27 O7 Ni2 -8.7(6) . . . . ? O1 Ni2 O7 C27 14.4(7) . . . . ? N3 Ni2 O7 C27 -171.5(3) . . . . ? O8 Ni2 O7 C27 13.8(3) . . . . ? O11 Ni2 O7 C27 94.6(3) . . . . ? O1W Ni2 O7 C27 -83.4(3) . . . . ? Ho1 Ni2 O7 C27 50.6(3) . . . . ? C26 C25 O8 Ni2 2.4(5) . . . . ? C24 C25 O8 Ni2 -175.9(2) . . . . ? C26 C25 O8 Ho1 -136.2(3) . . . . ? C24 C25 O8 Ho1 45.5(4) . . . . ? O1 Ni2 O8 C25 168.9(3) . . . . ? N3 Ni2 O8 C25 -168.1(5) . . . . ? O11 Ni2 O8 C25 -106.9(3) . . . . ? O7 Ni2 O8 C25 -11.3(3) . . . . ? O1W Ni2 O8 C25 76.5(3) . . . . ? Ho1 Ni2 O8 C25 -150.1(3) . . . . ? O1 Ni2 O8 Ho1 -41.07(9) . . . . ? N3 Ni2 O8 Ho1 -18.0(5) . . . . ? O11 Ni2 O8 Ho1 43.15(9) . . . . ? O7 Ni2 O8 Ho1 138.80(10) . . . . ? O1W Ni2 O8 Ho1 -133.40(10) . . . . ? O2 Ho1 O8 C25 -114.5(3) . . . . ? O1 Ho1 O8 C25 -172.6(3) . . . . ? O9 Ho1 O8 C25 -43.0(3) . . . . ? O5 Ho1 O8 C25 -6.2(4) . . . . ? O4 Ho1 O8 C25 139.0(3) . . . . ? O5 Ho1 O8 C25 38.2(3) 3_777 . . . ? O11 Ho1 O8 C25 111.0(3) . . . . ? Ni2 Ho1 O8 C25 149.7(3) . . . . ? Ni1 Ho1 O8 C25 124.4(3) . . . . ? Ho1 Ho1 O8 C25 25.6(3) 3_777 . . . ? O2 Ho1 O8 Ni2 95.78(10) . . . . ? O1 Ho1 O8 Ni2 37.67(9) . . . . ? O9 Ho1 O8 Ni2 167.32(12) . . . . ? O5 Ho1 O8 Ni2 -155.89(15) . . . . ? O4 Ho1 O8 Ni2 -10.76(15) . . . . ? O5 Ho1 O8 Ni2 -111.55(9) 3_777 . . . ? O11 Ho1 O8 Ni2 -38.75(8) . . . . ? Ni1 Ho1 O8 Ni2 -25.33(8) . . . . ? Ho1 Ho1 O8 Ni2 -124.09(6) 3_777 . . . ? O10 C23 O9 Ho1 -178.5(3) . . . . ? C24 C23 O9 Ho1 2.1(6) . . . . ? O2 Ho1 O9 C23 136.2(4) . . . . ? O1 Ho1 O9 C23 70.3(4) . . . . ? O5 Ho1 O9 C23 -146.5(4) . . . . ? O8 Ho1 O9 C23 19.0(4) . . . . ? O4 Ho1 O9 C23 -165.0(3) . . . . ? O5 Ho1 O9 C23 -78.3(4) 3_777 . . . ? O11 Ho1 O9 C23 -13.4(4) . . . . ? Ni2 Ho1 O9 C23 27.7(4) . . . . ? Ni1 Ho1 O9 C23 -29.7(5) . . . . ? Ho1 Ho1 O9 C23 -112.2(4) 3_777 . . . ? N4 Ni1 O11 Ni2 26.7(4) . . . . ? N1 Ni1 O11 Ni2 -157.43(14) . . . . ? O4 Ni1 O11 Ni2 99.31(13) . . . . ? N2 Ni1 O11 Ni2 -71.53(14) . . . . ? Ho1 Ni1 O11 Ni2 96.97(14) . . . . ? N4 Ni1 O11 Ho1 -70.3(4) . . . . ? N1 Ni1 O11 Ho1 105.60(12) . . . . ? O4 Ni1 O11 Ho1 2.34(10) . . . . ? N2 Ni1 O11 Ho1 -168.51(11) . . . . ? O1 Ni2 O11 Ni1 -68.45(13) . . . . ? N3 Ni2 O11 Ni1 19.57(15) . . . . ? O8 Ni2 O11 Ni1 -149.00(14) . . . . ? O7 Ni2 O11 Ni1 123.10(13) . . . . ? O1W Ni2 O11 Ni1 -86.5(16) . . . . ? Ho1 Ni2 O11 Ni1 -106.20(14) . . . . ? O1 Ni2 O11 Ho1 37.76(9) . . . . ? N3 Ni2 O11 Ho1 125.77(11) . . . . ? O8 Ni2 O11 Ho1 -42.80(9) . . . . ? O7 Ni2 O11 Ho1 -130.70(9) . . . . ? O1W Ni2 O11 Ho1 19.7(16) . . . . ? O2 Ho1 O11 Ni1 57.05(16) . . . . ? O1 Ho1 O11 Ni1 82.75(11) . . . . ? O9 Ho1 O11 Ni1 -171.53(9) . . . . ? O5 Ho1 O11 Ni1 -50.42(13) . . . . ? O8 Ho1 O11 Ni1 155.45(12) . . . . ? O4 Ho1 O11 Ni1 -2.15(9) . . . . ? O5 Ho1 O11 Ni1 -103.52(11) 3_777 . . . ? Ni2 Ho1 O11 Ni1 117.10(13) . . . . ? Ho1 Ho1 O11 Ni1 -79.06(9) 3_777 . . . ? O2 Ho1 O11 Ni2 -60.05(15) . . . . ? O1 Ho1 O11 Ni2 -34.35(9) . . . . ? O9 Ho1 O11 Ni2 71.37(13) . . . . ? O5 Ho1 O11 Ni2 -167.53(8) . . . . ? O8 Ho1 O11 Ni2 38.35(8) . . . . ? O4 Ho1 O11 Ni2 -119.26(11) . . . . ? O5 Ho1 O11 Ni2 139.38(10) 3_777 . . . ? Ni1 Ho1 O11 Ni2 -117.10(13) . . . . ? Ho1 Ho1 O11 Ni2 163.83(6) 3_777 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C O10 0.90 2.47 3.199(4) 137.9 3_777 N1 H1D O9 0.90 2.50 3.091(4) 123.6 3_777 O11 H11 O6 0.82 2.17 2.935(4) 155.6 3_777 O1W H1WA O3W 0.85 1.82 2.647(5) 162.8 1_565 O1W H1WB O5W 0.85 2.00 2.766(5) 149.5 1_565 O2W H2WA O6 0.85 2.14 2.963(5) 161.6 1_445 O2W H2WB O3 0.85 1.91 2.688(5) 151.5 1_445 O3W H3WA O10 0.85 2.19 2.801(5) 128.7 4_575 O4W H4WA O3 0.85 2.36 3.168(6) 158.0 1_445 O4W H4WA O2 0.85 2.56 3.038(5) 116.8 1_445 O4W H4WB O9 0.85 2.43 3.262(5) 165.0 1_445 O5W H5WB O4W 0.85 1.82 2.660(6) 167.3 4_665 O12 H12A O10 0.82 1.95 2.760(7) 167.7 1_544 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.684 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.110 data_1262 _database_code_depnum_ccdc_archive 'CCDC 898024' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C60 H58 Er2 N8 Ni4 O24), 15(H2 O)' _chemical_formula_sum 'C120 H146 Er4 N16 Ni8 O63' _chemical_formula_weight 3959.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.596(2) _cell_length_b 18.121(3) _cell_length_c 15.466(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.104(3) _cell_angle_gamma 90.00 _cell_volume 3485.7(11) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4656 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 26.09 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1978 _exptl_absorpt_coefficient_mu 3.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3394 _exptl_absorpt_correction_T_max 0.7189 _exptl_absorpt_process_details 'SADABS(Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17154 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6131 _reflns_number_gt 4549 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2005)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2005)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^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 6131 _refine_ls_number_parameters 487 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.082875(11) 1.053841(8) 0.596556(10) 0.02343(4) Uani 1 1 d . . . Ni1 Ni 0.31226(3) 1.04849(2) 0.70768(3) 0.02666(11) Uani 1 1 d . . . Ni2 Ni 0.15993(3) 0.89367(2) 0.70900(3) 0.02779(12) Uani 1 1 d . . . C1 C 0.2546(3) 0.7850(2) 0.6161(3) 0.0439(12) Uani 1 1 d . . . H1A H 0.2993 0.8199 0.5908 0.053 Uiso 1 1 calc R . . H1B H 0.2501 0.7400 0.5818 0.053 Uiso 1 1 calc R . . C2 C 0.3029(3) 0.7689(2) 0.7090(3) 0.0440(12) Uani 1 1 d . . . H2A H 0.2624 0.7297 0.7313 0.053 Uiso 1 1 calc R . . H2B H 0.3761 0.7517 0.7106 0.053 Uiso 1 1 calc R . . C3 C 0.4072(3) 0.87359(19) 0.7700(3) 0.0386(11) Uani 1 1 d . . . H3A H 0.4120 0.8916 0.7117 0.046 Uiso 1 1 calc R . . H3B H 0.4647 0.8381 0.7854 0.046 Uiso 1 1 calc R . . C4 C 0.4266(3) 0.9381(2) 0.8335(3) 0.0399(11) Uani 1 1 d . . . H4A H 0.4368 0.9198 0.8931 0.048 Uiso 1 1 calc R . . H4B H 0.4915 0.9640 0.8247 0.048 Uiso 1 1 calc R . . C5 C 0.2861(3) 1.0015(2) 0.8846(3) 0.0449(12) Uani 1 1 d . . . H5 H 0.3155 0.9802 0.9377 0.054 Uiso 1 1 calc R . . C6 C 0.1900(3) 1.0446(2) 0.8848(3) 0.0454(12) Uani 1 1 d . . . C7 C 0.1311(3) 1.07781(18) 0.8103(2) 0.0322(10) Uani 1 1 d . . . C8 C 0.0307(3) 1.1109(2) 0.8167(3) 0.0391(11) Uani 1 1 d . . . C9 C -0.0390(3) 1.1444(2) 0.7387(3) 0.0488(12) Uani 1 1 d . . . C10 C -0.0058(3) 1.1119(2) 0.8966(3) 0.0625(14) Uani 1 1 d . . . H10 H -0.0712 1.1343 0.9010 0.075 Uiso 1 1 calc R . . C11 C 0.0532(4) 1.0803(3) 0.9697(4) 0.0835(18) Uani 1 1 d . . . H11 H 0.0276 1.0814 1.0229 0.100 Uiso 1 1 calc R . . C12 C 0.1493(4) 1.0476(3) 0.9640(3) 0.0715(16) Uani 1 1 d . . . H12 H 0.1887 1.0266 1.0139 0.086 Uiso 1 1 calc R . . C13 C 0.2850(3) 0.8113(2) 0.8548(3) 0.0412(11) Uani 1 1 d . . . H13A H 0.3047 0.8511 0.8962 0.049 Uiso 1 1 calc R . . H13B H 0.3303 0.7692 0.8737 0.049 Uiso 1 1 calc R . . C14 C 0.1691(3) 0.7909(2) 0.8541(3) 0.0474(12) Uani 1 1 d . . . H14A H 0.1550 0.7425 0.8280 0.057 Uiso 1 1 calc R . . H14B H 0.1541 0.7890 0.9137 0.057 Uiso 1 1 calc R . . C15 C 0.0033(3) 0.8524(2) 0.8183(3) 0.0413(11) Uani 1 1 d . . . H15 H -0.0146 0.8240 0.8640 0.050 Uiso 1 1 calc R . . C16 C -0.0815(3) 0.8983(2) 0.7731(2) 0.0349(10) Uani 1 1 d . . . C17 C -0.0706(2) 0.94571(18) 0.7013(2) 0.0280(9) Uani 1 1 d . . . C18 C -0.1631(2) 0.98213(19) 0.6581(2) 0.0298(9) Uani 1 1 d . . . C19 C -0.1702(2) 1.02154(19) 0.5734(2) 0.0295(9) Uani 1 1 d . . . C20 C -0.2584(3) 0.9761(2) 0.6928(3) 0.0480(12) Uani 1 1 d . . . H20 H -0.3185 1.0021 0.6662 0.058 Uiso 1 1 calc R . . C21 C -0.2671(3) 0.9339(3) 0.7640(3) 0.0599(14) Uani 1 1 d . . . H21 H -0.3317 0.9319 0.7859 0.072 Uiso 1 1 calc R . . C22 C -0.1799(3) 0.8941(2) 0.8032(3) 0.0515(13) Uani 1 1 d . . . H22 H -0.1866 0.8638 0.8507 0.062 Uiso 1 1 calc R . . C23 C 0.4732(3) 1.0607(2) 0.5914(3) 0.0386(11) Uani 1 1 d . . . H23 H 0.5419 1.0509 0.5794 0.046 Uiso 1 1 calc R . . C24 C 0.4127(2) 1.11116(19) 0.5330(3) 0.0322(10) Uani 1 1 d . . . C25 C 0.3019(2) 1.12804(17) 0.5343(2) 0.0266(9) Uani 1 1 d . . . C26 C 0.2460(2) 1.17212(18) 0.4656(2) 0.0287(9) Uani 1 1 d . . . C27 C 0.1292(3) 1.18993(18) 0.4588(2) 0.0316(10) Uani 1 1 d . . . C28 C 0.3037(3) 1.2010(2) 0.4042(3) 0.0413(11) Uani 1 1 d . . . H28 H 0.2682 1.2315 0.3606 0.050 Uiso 1 1 calc R . . C29 C 0.4127(3) 1.1864(2) 0.4050(3) 0.0508(12) Uani 1 1 d . . . H29 H 0.4491 1.2078 0.3635 0.061 Uiso 1 1 calc R . . C30 C 0.4647(3) 1.1406(2) 0.4671(3) 0.0474(12) Uani 1 1 d . . . H30 H 0.5362 1.1284 0.4659 0.057 Uiso 1 1 calc R . . N1 N 0.1471(2) 0.81584(16) 0.6149(2) 0.0409(10) Uani 1 1 d . . . H1C H 0.1010 0.7803 0.6256 0.049 Uiso 1 1 calc R . . H1D H 0.1228 0.8359 0.5622 0.049 Uiso 1 1 calc R . . N2 N 0.3035(2) 0.83480(15) 0.7668(2) 0.0336(8) Uani 1 1 d . . . N3 N 0.3358(2) 0.98899(16) 0.8201(2) 0.0342(8) Uani 1 1 d . . . N4 N 0.0992(2) 0.84602(16) 0.8037(2) 0.0392(9) Uani 1 1 d . . . O1 O 0.16929(16) 1.07874(12) 0.73541(16) 0.0293(6) Uani 1 1 d . . . O2 O -0.02501(18) 1.12860(13) 0.66124(17) 0.0378(7) Uani 1 1 d . . . O3 O -0.1112(2) 1.1863(2) 0.7542(2) 0.0936(12) Uani 1 1 d . . . O4 O 0.02472(16) 0.95567(11) 0.67692(16) 0.0288(6) Uani 1 1 d . . . O5 O -0.08882(15) 1.01656(12) 0.53134(15) 0.0260(6) Uani 1 1 d . . . O6 O -0.25317(17) 1.05463(13) 0.54135(17) 0.0372(7) Uani 1 1 d . . . O7 O 0.44937(17) 1.02770(13) 0.65576(17) 0.0364(7) Uani 1 1 d . . . O8 O 0.25425(15) 1.10525(12) 0.59807(15) 0.0282(6) Uani 1 1 d . . . O9 O 0.07074(16) 1.15100(12) 0.50107(17) 0.0336(7) Uani 1 1 d . . . O10 O 0.09305(19) 1.24173(15) 0.41007(19) 0.0509(8) Uani 1 1 d . . . O11 O 0.22349(16) 0.96748(11) 0.63913(15) 0.0247(6) Uani 1 1 d D . . H11A H 0.2553 0.9469 0.5905 0.030 Uiso 1 1 calc RD . . O1W O 0.39439(18) 1.13650(13) 0.77571(18) 0.0426(8) Uani 1 1 d . . . H1WA H 0.3641 1.1693 0.8027 0.051 Uiso 1 1 d R . . H1WB H 0.4106 1.1006 0.8107 0.051 Uiso 1 1 d R . . O2W O 0.7140(2) 0.19243(19) 0.6321(2) 0.0812(12) Uani 1 1 d . . . H2WA H 0.7211 0.1567 0.5979 0.097 Uiso 1 1 d R . . H2WB H 0.7757 0.2024 0.6604 0.097 Uiso 1 1 d R . . O3W O 0.4688(3) 0.1356(2) 0.9536(3) 0.1088(16) Uani 1 1 d . . . H3WA H 0.4281 0.1450 0.9056 0.131 Uiso 1 1 d R . . H3WB H 0.4451 0.1594 0.9939 0.131 Uiso 1 1 d R . . O4W O 0.5755(3) 0.1902(2) 0.7481(3) 0.0791(13) Uani 0.75 1 d P . . H4WA H 0.5957 0.2349 0.7551 0.095 Uiso 0.75 1 d PR . . H4WB H 0.6289 0.1630 0.7673 0.095 Uiso 0.75 1 d PR . . O5W O 0.9053(3) 0.2733(2) 0.5768(3) 0.0716(15) Uani 0.75 1 d P . . H5WA H 0.9649 0.2754 0.5578 0.086 Uiso 0.75 1 d PR . . H5WB H 0.8906 0.2281 0.5831 0.086 Uiso 0.75 1 d PR . . O6W O 0.3004(10) 0.8950(7) 0.0848(8) 0.077(4) Uani 0.25 1 d P . . H6WA H 0.2661 0.8590 0.0585 0.092 Uiso 0.25 1 d PR . . H6WB H 0.3464 0.9094 0.0538 0.092 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01915(7) 0.02558(7) 0.02460(9) -0.00030(7) 0.00054(6) 0.00135(6) Ni1 0.0222(2) 0.0308(2) 0.0252(3) 0.0019(2) -0.00168(18) 0.00013(17) Ni2 0.0250(2) 0.0271(2) 0.0308(3) 0.0045(2) 0.00287(19) 0.00393(17) C1 0.043(2) 0.0364(19) 0.053(3) -0.010(2) 0.0105(19) 0.0092(17) C2 0.0329(19) 0.0355(19) 0.062(3) 0.000(2) 0.0046(19) 0.0049(16) C3 0.0246(17) 0.042(2) 0.046(3) 0.0103(19) -0.0027(17) 0.0068(15) C4 0.040(2) 0.044(2) 0.032(2) 0.0112(19) -0.0075(18) 0.0022(17) C5 0.057(2) 0.043(2) 0.033(2) 0.005(2) 0.0022(19) 0.0039(18) C6 0.064(2) 0.043(2) 0.031(2) -0.0031(19) 0.0131(19) 0.0025(19) C7 0.045(2) 0.0264(16) 0.027(2) -0.0049(16) 0.0125(17) -0.0097(15) C8 0.0391(19) 0.0412(19) 0.039(2) -0.0150(18) 0.0116(17) -0.0058(16) C9 0.035(2) 0.053(2) 0.059(3) -0.031(2) 0.0089(19) 0.0000(17) C10 0.067(3) 0.064(3) 0.065(3) -0.022(2) 0.033(2) 0.004(2) C11 0.116(4) 0.095(4) 0.050(3) 0.003(3) 0.047(3) 0.018(3) C12 0.101(4) 0.085(3) 0.031(3) 0.013(3) 0.017(3) 0.023(3) C13 0.040(2) 0.0380(19) 0.045(3) 0.0194(18) 0.0043(19) 0.0084(16) C14 0.046(2) 0.049(2) 0.047(3) 0.022(2) 0.0068(19) 0.0127(18) C15 0.042(2) 0.044(2) 0.039(2) 0.0155(19) 0.0099(18) 0.0030(17) C16 0.0320(18) 0.046(2) 0.027(2) 0.0024(18) 0.0067(16) 0.0033(16) C17 0.0235(16) 0.0330(17) 0.029(2) -0.0044(17) 0.0085(14) -0.0026(14) C18 0.0225(16) 0.0404(19) 0.029(2) 0.0001(17) 0.0102(15) 0.0004(14) C19 0.0194(16) 0.0375(18) 0.030(2) -0.0061(17) -0.0001(15) -0.0020(14) C20 0.0298(19) 0.074(3) 0.042(3) 0.011(2) 0.0111(18) 0.0092(19) C21 0.0296(19) 0.100(3) 0.054(3) 0.019(3) 0.0219(19) 0.008(2) C22 0.035(2) 0.073(3) 0.049(3) 0.024(2) 0.0153(19) 0.0031(19) C23 0.0216(17) 0.046(2) 0.049(3) 0.007(2) 0.0068(17) 0.0033(16) C24 0.0227(16) 0.0356(18) 0.037(2) 0.0029(17) 0.0020(16) -0.0006(14) C25 0.0300(17) 0.0217(15) 0.028(2) -0.0089(15) 0.0028(15) -0.0043(13) C26 0.0274(17) 0.0275(16) 0.031(2) 0.0022(16) 0.0041(15) -0.0005(14) C27 0.0315(18) 0.0306(17) 0.030(2) 0.0042(17) -0.0025(16) 0.0030(14) C28 0.038(2) 0.046(2) 0.040(2) 0.0177(19) 0.0048(18) -0.0014(17) C29 0.039(2) 0.065(3) 0.052(3) 0.025(2) 0.0198(19) 0.0011(19) C30 0.0280(18) 0.064(2) 0.052(3) 0.017(2) 0.0138(18) 0.0050(18) N1 0.0319(16) 0.0414(17) 0.047(2) -0.0081(16) -0.0028(15) 0.0003(13) N2 0.0327(15) 0.0333(15) 0.0340(19) 0.0075(14) 0.0025(14) 0.0064(13) N3 0.0341(15) 0.0347(16) 0.0308(19) 0.0045(15) -0.0037(14) -0.0010(13) N4 0.0353(16) 0.0392(16) 0.044(2) 0.0179(16) 0.0093(15) 0.0087(13) O1 0.0234(11) 0.0403(13) 0.0236(14) -0.0020(11) 0.0017(10) -0.0015(10) O2 0.0337(13) 0.0404(13) 0.0386(16) -0.0080(13) 0.0035(12) 0.0081(11) O3 0.0661(18) 0.135(3) 0.071(2) -0.055(2) -0.0146(17) 0.0586(18) O4 0.0208(11) 0.0298(12) 0.0354(15) 0.0058(11) 0.0031(10) 0.0020(9) O5 0.0196(11) 0.0357(12) 0.0224(13) -0.0024(11) 0.0026(10) 0.0024(9) O6 0.0245(12) 0.0512(14) 0.0365(16) 0.0043(13) 0.0060(11) 0.0101(11) O7 0.0246(12) 0.0426(13) 0.0419(17) 0.0097(13) 0.0044(11) 0.0059(10) O8 0.0181(10) 0.0379(12) 0.0286(14) 0.0069(11) 0.0037(10) 0.0007(9) O9 0.0205(11) 0.0377(12) 0.0397(16) 0.0116(12) -0.0039(11) 0.0005(10) O10 0.0417(14) 0.0539(15) 0.0583(19) 0.0311(15) 0.0113(13) 0.0162(12) O11 0.0194(10) 0.0286(11) 0.0252(14) -0.0017(10) 0.0009(10) 0.0006(9) O1W 0.0403(14) 0.0351(13) 0.0489(18) -0.0052(13) -0.0039(13) 0.0011(11) O2W 0.0612(19) 0.096(2) 0.085(3) -0.031(2) 0.0070(18) 0.0133(17) O3W 0.132(3) 0.131(3) 0.052(3) -0.003(3) -0.020(2) 0.000(3) O4W 0.0507(19) 0.109(3) 0.086(3) -0.067(2) 0.0394(19) -0.0563(19) O5W 0.102(3) 0.047(2) 0.058(3) 0.008(2) -0.010(3) -0.007(2) O6W 0.104(9) 0.077(8) 0.044(8) 0.037(7) -0.002(7) 0.019(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O2 2.261(2) . ? Er1 O9 2.287(2) . ? Er1 O1 2.294(2) . ? Er1 O5 2.337(2) . ? Er1 O8 2.348(2) . ? Er1 O4 2.353(2) . ? Er1 O5 2.365(2) 3_576 ? Er1 O11 2.377(2) . ? Er1 Er1 3.8876(5) 3_576 ? Ni1 O1 1.993(2) . ? Ni1 O8 2.018(2) . ? Ni1 N3 2.027(3) . ? Ni1 O11 2.038(2) . ? Ni1 O7 2.051(2) . ? Ni1 O1W 2.092(2) . ? Ni2 N4 1.957(3) . ? Ni2 O11 1.968(2) . ? Ni2 N1 2.015(3) . ? Ni2 O4 2.035(2) . ? Ni2 N2 2.167(3) . ? C1 N1 1.462(4) . ? C1 C2 1.497(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.491(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.477(4) . ? C3 C4 1.521(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.458(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.279(5) . ? C5 C6 1.441(6) . ? C5 H5 0.9300 . ? C6 C7 1.403(5) . ? C6 C12 1.403(6) . ? C7 O1 1.322(4) . ? C7 C8 1.418(5) . ? C8 C10 1.386(6) . ? C8 C9 1.502(6) . ? C9 O3 1.238(5) . ? C9 O2 1.271(5) . ? C10 C11 1.375(7) . ? C10 H10 0.9300 . ? C11 C12 1.363(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N2 1.478(5) . ? C13 C14 1.505(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.470(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.269(4) . ? C15 C16 1.444(5) . ? C15 H15 0.9300 . ? C16 C22 1.393(5) . ? C16 C17 1.427(5) . ? C17 O4 1.327(4) . ? C17 C18 1.411(4) . ? C18 C20 1.395(5) . ? C18 C19 1.482(5) . ? C19 O6 1.239(4) . ? C19 O5 1.301(4) . ? C20 C21 1.359(6) . ? C20 H20 0.9300 . ? C21 C22 1.373(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O7 1.239(5) . ? C23 C24 1.420(5) . ? C23 H23 0.9300 . ? C24 C30 1.401(5) . ? C24 C25 1.432(4) . ? C25 O8 1.300(4) . ? C25 C26 1.423(5) . ? C26 C28 1.387(5) . ? C26 C27 1.494(4) . ? C27 O10 1.244(4) . ? C27 O9 1.272(4) . ? C28 C29 1.397(5) . ? C28 H28 0.9300 . ? C29 C30 1.358(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? O5 Er1 2.365(2) 3_576 ? O11 H11A 0.9800 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8501 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8493 . ? O5W H5WB 0.8496 . ? O6W H6WA 0.8501 . ? O6W H6WB 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Er1 O9 80.86(9) . . ? O2 Er1 O1 72.38(8) . . ? O9 Er1 O1 115.24(8) . . ? O2 Er1 O5 77.54(8) . . ? O9 Er1 O5 88.92(8) . . ? O1 Er1 O5 136.95(8) . . ? O2 Er1 O8 111.96(8) . . ? O9 Er1 O8 70.64(7) . . ? O1 Er1 O8 67.25(8) . . ? O5 Er1 O8 154.91(8) . . ? O2 Er1 O4 87.71(9) . . ? O9 Er1 O4 158.21(7) . . ? O1 Er1 O4 78.19(8) . . ? O5 Er1 O4 70.44(8) . . ? O8 Er1 O4 131.11(7) . . ? O2 Er1 O5 142.57(8) . 3_576 ? O9 Er1 O5 83.28(8) . 3_576 ? O1 Er1 O5 144.70(7) . 3_576 ? O5 Er1 O5 68.45(8) . 3_576 ? O8 Er1 O5 94.11(8) . 3_576 ? O4 Er1 O5 95.03(8) . 3_576 ? O2 Er1 O11 138.20(9) . . ? O9 Er1 O11 131.02(8) . . ? O1 Er1 O11 69.37(8) . . ? O5 Er1 O11 121.83(7) . . ? O8 Er1 O11 67.34(7) . . ? O4 Er1 O11 68.69(7) . . ? O5 Er1 O11 75.86(7) 3_576 . ? O2 Er1 Er1 110.69(6) . 3_576 ? O9 Er1 Er1 85.26(6) . 3_576 ? O1 Er1 Er1 159.34(6) . 3_576 ? O5 Er1 Er1 34.46(6) . 3_576 ? O8 Er1 Er1 126.01(6) . 3_576 ? O4 Er1 Er1 81.49(6) . 3_576 ? O5 Er1 Er1 33.99(5) 3_576 3_576 ? O11 Er1 Er1 99.70(5) . 3_576 ? O1 Ni1 O8 79.70(9) . . ? O1 Ni1 N3 88.65(11) . . ? O8 Ni1 N3 167.36(10) . . ? O1 Ni1 O11 82.53(9) . . ? O8 Ni1 O11 80.45(9) . . ? N3 Ni1 O11 93.26(11) . . ? O1 Ni1 O7 168.55(10) . . ? O8 Ni1 O7 88.86(9) . . ? N3 Ni1 O7 102.70(11) . . ? O11 Ni1 O7 95.20(9) . . ? O1 Ni1 O1W 94.24(9) . . ? O8 Ni1 O1W 96.81(10) . . ? N3 Ni1 O1W 88.88(11) . . ? O11 Ni1 O1W 176.07(9) . . ? O7 Ni1 O1W 87.53(10) . . ? N4 Ni2 O11 162.19(11) . . ? N4 Ni2 N1 103.64(13) . . ? O11 Ni2 N1 94.14(11) . . ? N4 Ni2 O4 90.86(11) . . ? O11 Ni2 O4 83.59(9) . . ? N1 Ni2 O4 104.00(10) . . ? N4 Ni2 N2 82.73(12) . . ? O11 Ni2 N2 100.12(10) . . ? N1 Ni2 N2 85.41(11) . . ? O4 Ni2 N2 169.70(11) . . ? N1 C1 C2 108.8(3) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 112.5(3) . . ? N2 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N2 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N2 C3 C4 116.0(3) . . ? N2 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? N2 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? N3 C4 C3 110.6(3) . . ? N3 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 127.8(4) . . ? N3 C5 H5 116.1 . . ? C6 C5 H5 116.1 . . ? C7 C6 C12 118.8(4) . . ? C7 C6 C5 124.5(4) . . ? C12 C6 C5 116.5(4) . . ? O1 C7 C6 120.4(3) . . ? O1 C7 C8 120.5(3) . . ? C6 C7 C8 119.1(4) . . ? C10 C8 C7 119.5(4) . . ? C10 C8 C9 118.5(3) . . ? C7 C8 C9 122.0(4) . . ? O3 C9 O2 122.4(4) . . ? O3 C9 C8 116.5(4) . . ? O2 C9 C8 121.0(3) . . ? C11 C10 C8 121.1(4) . . ? C11 C10 H10 119.5 . . ? C8 C10 H10 119.5 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C6 121.6(4) . . ? C11 C12 H12 119.2 . . ? C6 C12 H12 119.2 . . ? N2 C13 C14 111.0(3) . . ? N2 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N2 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N4 C14 C13 109.6(3) . . ? N4 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? N4 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N4 C15 C16 128.2(4) . . ? N4 C15 H15 115.9 . . ? C16 C15 H15 115.9 . . ? C22 C16 C17 119.6(3) . . ? C22 C16 C15 115.8(4) . . ? C17 C16 C15 124.6(3) . . ? O4 C17 C18 121.2(3) . . ? O4 C17 C16 120.4(3) . . ? C18 C17 C16 118.4(3) . . ? C20 C18 C17 118.6(3) . . ? C20 C18 C19 116.2(3) . . ? C17 C18 C19 125.0(3) . . ? O6 C19 O5 121.0(3) . . ? O6 C19 C18 121.1(3) . . ? O5 C19 C18 117.8(3) . . ? C21 C20 C18 122.7(4) . . ? C21 C20 H20 118.7 . . ? C18 C20 H20 118.7 . . ? C20 C21 C22 119.5(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C16 121.0(4) . . ? C21 C22 H22 119.5 . . ? C16 C22 H22 119.5 . . ? O7 C23 C24 130.4(3) . . ? O7 C23 H23 114.8 . . ? C24 C23 H23 114.8 . . ? C30 C24 C23 116.2(3) . . ? C30 C24 C25 119.9(3) . . ? C23 C24 C25 123.7(3) . . ? O8 C25 C26 120.7(3) . . ? O8 C25 C24 120.7(3) . . ? C26 C25 C24 118.5(3) . . ? C28 C26 C25 118.2(3) . . ? C28 C26 C27 119.1(3) . . ? C25 C26 C27 122.7(3) . . ? O10 C27 O9 122.9(3) . . ? O10 C27 C26 117.9(3) . . ? O9 C27 C26 119.2(3) . . ? C26 C28 C29 122.9(3) . . ? C26 C28 H28 118.5 . . ? C29 C28 H28 118.5 . . ? C30 C29 C28 119.1(4) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C24 121.2(3) . . ? C29 C30 H30 119.4 . . ? C24 C30 H30 119.4 . . ? C1 N1 Ni2 106.8(2) . . ? C1 N1 H1C 110.4 . . ? Ni2 N1 H1C 110.4 . . ? C1 N1 H1D 110.4 . . ? Ni2 N1 H1D 110.4 . . ? H1C N1 H1D 108.6 . . ? C3 N2 C13 111.9(3) . . ? C3 N2 C2 108.8(3) . . ? C13 N2 C2 109.6(3) . . ? C3 N2 Ni2 117.1(2) . . ? C13 N2 Ni2 106.2(2) . . ? C2 N2 Ni2 102.8(2) . . ? C5 N3 C4 118.1(3) . . ? C5 N3 Ni1 123.4(3) . . ? C4 N3 Ni1 117.6(2) . . ? C15 N4 C14 118.3(3) . . ? C15 N4 Ni2 126.0(3) . . ? C14 N4 Ni2 115.1(2) . . ? C7 O1 Ni1 130.6(2) . . ? C7 O1 Er1 129.3(2) . . ? Ni1 O1 Er1 93.18(10) . . ? C9 O2 Er1 137.3(2) . . ? C17 O4 Ni2 128.0(2) . . ? C17 O4 Er1 128.66(19) . . ? Ni2 O4 Er1 103.16(9) . . ? C19 O5 Er1 120.8(2) . . ? C19 O5 Er1 126.0(2) . 3_576 ? Er1 O5 Er1 111.55(8) . 3_576 ? C23 O7 Ni1 123.5(2) . . ? C25 O8 Ni1 130.52(19) . . ? C25 O8 Er1 130.7(2) . . ? Ni1 O8 Er1 90.94(9) . . ? C27 O9 Er1 140.7(2) . . ? Ni2 O11 Ni1 116.19(12) . . ? Ni2 O11 Er1 104.45(9) . . ? Ni1 O11 Er1 89.62(8) . . ? Ni2 O11 H11A 114.5 . . ? Ni1 O11 H11A 114.5 . . ? Er1 O11 H11A 114.5 . . ? Ni1 O1W H1WA 123.7 . . ? Ni1 O1W H1WB 77.7 . . ? H1WA O1W H1WB 107.7 . . ? H2WA O2W H2WB 107.7 . . ? H3WA O3W H3WB 107.7 . . ? H4WA O4W H4WB 107.7 . . ? H5WA O5W H5WB 107.8 . . ? H6WA O6W H6WB 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -54.8(4) . . . . ? N2 C3 C4 N3 -51.2(4) . . . . ? N3 C5 C6 C7 3.4(7) . . . . ? N3 C5 C6 C12 177.8(4) . . . . ? C12 C6 C7 O1 177.2(4) . . . . ? C5 C6 C7 O1 -8.5(6) . . . . ? C12 C6 C7 C8 -2.2(6) . . . . ? C5 C6 C7 C8 172.1(4) . . . . ? O1 C7 C8 C10 -177.5(3) . . . . ? C6 C7 C8 C10 1.9(5) . . . . ? O1 C7 C8 C9 3.5(5) . . . . ? C6 C7 C8 C9 -177.1(3) . . . . ? C10 C8 C9 O3 17.2(6) . . . . ? C7 C8 C9 O3 -163.7(4) . . . . ? C10 C8 C9 O2 -161.3(4) . . . . ? C7 C8 C9 O2 17.8(5) . . . . ? C7 C8 C10 C11 -0.9(6) . . . . ? C9 C8 C10 C11 178.2(4) . . . . ? C8 C10 C11 C12 0.1(8) . . . . ? C10 C11 C12 C6 -0.4(8) . . . . ? C7 C6 C12 C11 1.4(7) . . . . ? C5 C6 C12 C11 -173.3(5) . . . . ? N2 C13 C14 N4 -43.7(4) . . . . ? N4 C15 C16 C22 179.8(4) . . . . ? N4 C15 C16 C17 0.2(6) . . . . ? C22 C16 C17 O4 173.8(3) . . . . ? C15 C16 C17 O4 -6.7(5) . . . . ? C22 C16 C17 C18 -5.4(5) . . . . ? C15 C16 C17 C18 174.2(3) . . . . ? O4 C17 C18 C20 -172.8(3) . . . . ? C16 C17 C18 C20 6.4(5) . . . . ? O4 C17 C18 C19 12.9(5) . . . . ? C16 C17 C18 C19 -168.0(3) . . . . ? C20 C18 C19 O6 8.4(5) . . . . ? C17 C18 C19 O6 -177.2(3) . . . . ? C20 C18 C19 O5 -167.6(3) . . . . ? C17 C18 C19 O5 6.9(5) . . . . ? C17 C18 C20 C21 -3.2(6) . . . . ? C19 C18 C20 C21 171.6(4) . . . . ? C18 C20 C21 C22 -1.1(7) . . . . ? C20 C21 C22 C16 2.2(7) . . . . ? C17 C16 C22 C21 1.1(6) . . . . ? C15 C16 C22 C21 -178.5(4) . . . . ? O7 C23 C24 C30 178.4(4) . . . . ? O7 C23 C24 C25 -6.6(6) . . . . ? C30 C24 C25 O8 -175.5(3) . . . . ? C23 C24 C25 O8 9.7(5) . . . . ? C30 C24 C25 C26 2.7(5) . . . . ? C23 C24 C25 C26 -172.1(3) . . . . ? O8 C25 C26 C28 173.6(3) . . . . ? C24 C25 C26 C28 -4.6(5) . . . . ? O8 C25 C26 C27 -4.7(5) . . . . ? C24 C25 C26 C27 177.1(3) . . . . ? C28 C26 C27 O10 -14.7(5) . . . . ? C25 C26 C27 O10 163.5(3) . . . . ? C28 C26 C27 O9 163.8(3) . . . . ? C25 C26 C27 O9 -18.0(5) . . . . ? C25 C26 C28 C29 2.6(6) . . . . ? C27 C26 C28 C29 -179.1(4) . . . . ? C26 C28 C29 C30 1.6(6) . . . . ? C28 C29 C30 C24 -3.6(6) . . . . ? C23 C24 C30 C29 176.6(4) . . . . ? C25 C24 C30 C29 1.4(6) . . . . ? C2 C1 N1 Ni2 46.5(3) . . . . ? N4 Ni2 N1 C1 -103.9(2) . . . . ? O11 Ni2 N1 C1 77.3(2) . . . . ? O4 Ni2 N1 C1 161.7(2) . . . . ? N2 Ni2 N1 C1 -22.6(2) . . . . ? C4 C3 N2 C13 -52.9(4) . . . . ? C4 C3 N2 C2 -174.1(3) . . . . ? C4 C3 N2 Ni2 70.0(4) . . . . ? C14 C13 N2 C3 164.7(3) . . . . ? C14 C13 N2 C2 -74.6(4) . . . . ? C14 C13 N2 Ni2 35.8(3) . . . . ? C1 C2 N2 C3 -92.6(3) . . . . ? C1 C2 N2 C13 144.8(3) . . . . ? C1 C2 N2 Ni2 32.2(3) . . . . ? N4 Ni2 N2 C3 -141.5(3) . . . . ? O11 Ni2 N2 C3 20.7(3) . . . . ? N1 Ni2 N2 C3 114.1(3) . . . . ? O4 Ni2 N2 C3 -89.6(6) . . . . ? N4 Ni2 N2 C13 -15.6(2) . . . . ? O11 Ni2 N2 C13 146.6(2) . . . . ? N1 Ni2 N2 C13 -120.0(2) . . . . ? O4 Ni2 N2 C13 36.2(7) . . . . ? N4 Ni2 N2 C2 99.4(2) . . . . ? O11 Ni2 N2 C2 -98.4(2) . . . . ? N1 Ni2 N2 C2 -5.0(2) . . . . ? O4 Ni2 N2 C2 151.3(5) . . . . ? C6 C5 N3 C4 -174.7(4) . . . . ? C6 C5 N3 Ni1 16.2(6) . . . . ? C3 C4 N3 C5 121.0(4) . . . . ? C3 C4 N3 Ni1 -69.2(3) . . . . ? O1 Ni1 N3 C5 -21.9(3) . . . . ? O8 Ni1 N3 C5 -44.6(7) . . . . ? O11 Ni1 N3 C5 -104.3(3) . . . . ? O7 Ni1 N3 C5 159.6(3) . . . . ? O1W Ni1 N3 C5 72.4(3) . . . . ? O1 Ni1 N3 C4 168.9(2) . . . . ? O8 Ni1 N3 C4 146.1(4) . . . . ? O11 Ni1 N3 C4 86.5(2) . . . . ? O7 Ni1 N3 C4 -9.6(3) . . . . ? O1W Ni1 N3 C4 -96.8(2) . . . . ? C16 C15 N4 C14 -175.1(4) . . . . ? C16 C15 N4 Ni2 -3.6(6) . . . . ? C13 C14 N4 C15 -157.7(4) . . . . ? C13 C14 N4 Ni2 29.9(4) . . . . ? O11 Ni2 N4 C15 79.9(5) . . . . ? N1 Ni2 N4 C15 -96.2(3) . . . . ? O4 Ni2 N4 C15 8.5(3) . . . . ? N2 Ni2 N4 C15 -179.6(3) . . . . ? O11 Ni2 N4 C14 -108.4(4) . . . . ? N1 Ni2 N4 C14 75.6(3) . . . . ? O4 Ni2 N4 C14 -179.8(3) . . . . ? N2 Ni2 N4 C14 -7.9(3) . . . . ? C6 C7 O1 Ni1 -7.4(5) . . . . ? C8 C7 O1 Ni1 172.0(2) . . . . ? C6 C7 O1 Er1 135.3(3) . . . . ? C8 C7 O1 Er1 -45.3(4) . . . . ? O8 Ni1 O1 C7 -166.1(3) . . . . ? N3 Ni1 O1 C7 18.8(3) . . . . ? O11 Ni1 O1 C7 112.3(3) . . . . ? O7 Ni1 O1 C7 -168.5(4) . . . . ? O1W Ni1 O1 C7 -69.9(3) . . . . ? O8 Ni1 O1 Er1 41.88(8) . . . . ? N3 Ni1 O1 Er1 -133.18(10) . . . . ? O11 Ni1 O1 Er1 -39.72(8) . . . . ? O7 Ni1 O1 Er1 39.5(5) . . . . ? O1W Ni1 O1 Er1 138.04(9) . . . . ? O2 Er1 O1 C7 45.7(3) . . . . ? O9 Er1 O1 C7 116.2(3) . . . . ? O5 Er1 O1 C7 -2.1(3) . . . . ? O8 Er1 O1 C7 169.6(3) . . . . ? O4 Er1 O1 C7 -45.7(3) . . . . ? O5 Er1 O1 C7 -127.6(2) 3_576 . . . ? O11 Er1 O1 C7 -117.1(3) . . . . ? Er1 Er1 O1 C7 -56.3(3) 3_576 . . . ? O2 Er1 O1 Ni1 -161.72(11) . . . . ? O9 Er1 O1 Ni1 -91.23(10) . . . . ? O5 Er1 O1 Ni1 150.48(9) . . . . ? O8 Er1 O1 Ni1 -37.75(8) . . . . ? O4 Er1 O1 Ni1 106.93(9) . . . . ? O5 Er1 O1 Ni1 24.99(17) 3_576 . . . ? O11 Er1 O1 Ni1 35.48(8) . . . . ? Er1 Er1 O1 Ni1 96.26(16) 3_576 . . . ? O3 C9 O2 Er1 -175.8(3) . . . . ? C8 C9 O2 Er1 2.6(6) . . . . ? O9 Er1 O2 C9 -144.8(3) . . . . ? O1 Er1 O2 C9 -24.5(3) . . . . ? O5 Er1 O2 C9 124.3(4) . . . . ? O8 Er1 O2 C9 -80.0(3) . . . . ? O4 Er1 O2 C9 53.9(3) . . . . ? O5 Er1 O2 C9 149.1(3) 3_576 . . . ? O11 Er1 O2 C9 0.0(4) . . . . ? Er1 Er1 O2 C9 133.9(3) 3_576 . . . ? C18 C17 O4 Ni2 -164.9(2) . . . . ? C16 C17 O4 Ni2 16.0(4) . . . . ? C18 C17 O4 Er1 20.7(4) . . . . ? C16 C17 O4 Er1 -158.4(2) . . . . ? N4 Ni2 O4 C17 -15.2(3) . . . . ? O11 Ni2 O4 C17 -178.2(3) . . . . ? N1 Ni2 O4 C17 89.1(3) . . . . ? N2 Ni2 O4 C17 -66.4(6) . . . . ? N4 Ni2 O4 Er1 160.33(12) . . . . ? O11 Ni2 O4 Er1 -2.70(9) . . . . ? N1 Ni2 O4 Er1 -95.38(12) . . . . ? N2 Ni2 O4 Er1 109.1(5) . . . . ? O2 Er1 O4 C17 33.1(3) . . . . ? O9 Er1 O4 C17 -25.0(4) . . . . ? O1 Er1 O4 C17 105.6(3) . . . . ? O5 Er1 O4 C17 -44.5(3) . . . . ? O8 Er1 O4 C17 150.6(2) . . . . ? O5 Er1 O4 C17 -109.5(3) 3_576 . . . ? O11 Er1 O4 C17 177.8(3) . . . . ? Er1 Er1 O4 C17 -78.2(3) 3_576 . . . ? O2 Er1 O4 Ni2 -142.35(10) . . . . ? O9 Er1 O4 Ni2 159.55(18) . . . . ? O1 Er1 O4 Ni2 -69.87(10) . . . . ? O5 Er1 O4 Ni2 140.07(12) . . . . ? O8 Er1 O4 Ni2 -24.85(15) . . . . ? O5 Er1 O4 Ni2 75.07(10) 3_576 . . . ? O11 Er1 O4 Ni2 2.38(8) . . . . ? Er1 Er1 O4 Ni2 106.34(9) 3_576 . . . ? O6 C19 O5 Er1 126.1(3) . . . . ? C18 C19 O5 Er1 -57.9(4) . . . . ? O6 C19 O5 Er1 -69.8(4) . . . 3_576 ? C18 C19 O5 Er1 106.2(3) . . . 3_576 ? O2 Er1 O5 C19 -29.7(2) . . . . ? O9 Er1 O5 C19 -110.6(2) . . . . ? O1 Er1 O5 C19 16.6(3) . . . . ? O8 Er1 O5 C19 -145.2(2) . . . . ? O4 Er1 O5 C19 62.3(2) . . . . ? O5 Er1 O5 C19 166.2(3) 3_576 . . . ? O11 Er1 O5 C19 109.9(2) . . . . ? Er1 Er1 O5 C19 166.2(3) 3_576 . . . ? O2 Er1 O5 Er1 164.08(11) . . . 3_576 ? O9 Er1 O5 Er1 83.20(10) . . . 3_576 ? O1 Er1 O5 Er1 -149.61(9) . . . 3_576 ? O8 Er1 O5 Er1 48.5(2) . . . 3_576 ? O4 Er1 O5 Er1 -103.91(11) . . . 3_576 ? O5 Er1 O5 Er1 0.0 3_576 . . 3_576 ? O11 Er1 O5 Er1 -56.34(12) . . . 3_576 ? C24 C23 O7 Ni1 -8.4(6) . . . . ? O1 Ni1 O7 C23 16.4(7) . . . . ? O8 Ni1 O7 C23 14.0(3) . . . . ? N3 Ni1 O7 C23 -171.1(3) . . . . ? O11 Ni1 O7 C23 94.3(3) . . . . ? O1W Ni1 O7 C23 -82.8(3) . . . . ? C26 C25 O8 Ni1 -175.6(2) . . . . ? C24 C25 O8 Ni1 2.6(4) . . . . ? C26 C25 O8 Er1 44.6(4) . . . . ? C24 C25 O8 Er1 -137.2(3) . . . . ? O1 Ni1 O8 C25 168.6(3) . . . . ? N3 Ni1 O8 C25 -168.2(5) . . . . ? O11 Ni1 O8 C25 -107.3(3) . . . . ? O7 Ni1 O8 C25 -11.8(3) . . . . ? O1W Ni1 O8 C25 75.5(3) . . . . ? O1 Ni1 O8 Er1 -40.63(8) . . . . ? N3 Ni1 O8 Er1 -17.5(5) . . . . ? O11 Ni1 O8 Er1 43.43(8) . . . . ? O7 Ni1 O8 Er1 138.89(9) . . . . ? O1W Ni1 O8 Er1 -133.73(9) . . . . ? O2 Er1 O8 C25 -113.8(3) . . . . ? O9 Er1 O8 C25 -42.6(2) . . . . ? O1 Er1 O8 C25 -172.2(3) . . . . ? O5 Er1 O8 C25 -5.6(4) . . . . ? O4 Er1 O8 C25 139.1(2) . . . . ? O5 Er1 O8 C25 38.8(3) 3_576 . . . ? O11 Er1 O8 C25 111.6(3) . . . . ? Er1 Er1 O8 C25 26.1(3) 3_576 . . . ? O2 Er1 O8 Ni1 95.61(10) . . . . ? O9 Er1 O8 Ni1 166.74(11) . . . . ? O1 Er1 O8 Ni1 37.14(8) . . . . ? O5 Er1 O8 Ni1 -156.19(14) . . . . ? O4 Er1 O8 Ni1 -11.53(14) . . . . ? O5 Er1 O8 Ni1 -111.86(9) 3_576 . . . ? O11 Er1 O8 Ni1 -39.04(8) . . . . ? Er1 Er1 O8 Ni1 -124.58(6) 3_576 . . . ? O10 C27 O9 Er1 -179.8(2) . . . . ? C26 C27 O9 Er1 1.8(5) . . . . ? O2 Er1 O9 C27 136.6(4) . . . . ? O1 Er1 O9 C27 71.1(4) . . . . ? O5 Er1 O9 C27 -145.8(4) . . . . ? O8 Er1 O9 C27 19.4(3) . . . . ? O4 Er1 O9 C27 -164.1(3) . . . . ? O5 Er1 O9 C27 -77.4(4) 3_576 . . . ? O11 Er1 O9 C27 -12.8(4) . . . . ? Er1 Er1 O9 C27 -111.5(4) 3_576 . . . ? N4 Ni2 O11 Ni1 27.0(4) . . . . ? N1 Ni2 O11 Ni1 -156.83(12) . . . . ? O4 Ni2 O11 Ni1 99.52(12) . . . . ? N2 Ni2 O11 Ni1 -70.77(13) . . . . ? N4 Ni2 O11 Er1 -69.8(3) . . . . ? N1 Ni2 O11 Er1 106.33(11) . . . . ? O4 Ni2 O11 Er1 2.69(9) . . . . ? N2 Ni2 O11 Er1 -167.60(10) . . . . ? O1 Ni1 O11 Ni2 -67.96(12) . . . . ? O8 Ni1 O11 Ni2 -148.70(12) . . . . ? N3 Ni1 O11 Ni2 20.25(13) . . . . ? O7 Ni1 O11 Ni2 123.33(12) . . . . ? O1 Ni1 O11 Er1 37.99(9) . . . . ? O8 Ni1 O11 Er1 -42.76(8) . . . . ? N3 Ni1 O11 Er1 126.20(10) . . . . ? O7 Ni1 O11 Er1 -130.72(9) . . . . ? O2 Er1 O11 Ni2 57.47(15) . . . . ? O9 Er1 O11 Ni2 -171.47(9) . . . . ? O1 Er1 O11 Ni2 82.48(10) . . . . ? O5 Er1 O11 Ni2 -50.78(13) . . . . ? O8 Er1 O11 Ni2 155.58(12) . . . . ? O4 Er1 O11 Ni2 -2.48(9) . . . . ? O5 Er1 O11 Ni2 -103.75(10) 3_576 . . . ? Er1 Er1 O11 Ni2 -79.31(9) 3_576 . . . ? O2 Er1 O11 Ni1 -59.53(14) . . . . ? O9 Er1 O11 Ni1 71.53(13) . . . . ? O1 Er1 O11 Ni1 -34.52(8) . . . . ? O5 Er1 O11 Ni1 -167.78(8) . . . . ? O8 Er1 O11 Ni1 38.58(8) . . . . ? O4 Er1 O11 Ni1 -119.48(10) . . . . ? O5 Er1 O11 Ni1 139.25(9) 3_576 . . . ? Er1 Er1 O11 Ni1 163.69(6) 3_576 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C O10 0.90 2.45 3.165(4) 136.5 3_576 N1 H1D O9 0.90 2.49 3.090(3) 124.4 3_576 O11 H11A O6 0.98 2.04 2.902(4) 146.3 3_576 O1W H1WB N3 0.85 2.25 2.885(4) 132.1 . O2W H2WA O6 0.85 2.09 2.925(4) 166.5 1_645 O2W H2WB O3 0.85 1.89 2.667(4) 151.9 1_645 O3W H3WA O1W 0.85 1.99 2.763(5) 150.2 1_545 O3W H3WB O5W 0.85 1.89 2.734(6) 169.9 4_566 O4W H4WB O6W 0.85 2.55 3.199(12) 134.4 3_666 O5W H5WA O3W 0.85 2.28 2.734(6) 113.3 4_665 O5W H5WB O2 0.85 2.33 2.998(5) 135.7 1_645 O6W H6WB O3W 0.85 2.49 3.108(14) 130.8 3_666 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.761 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.139