# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Peter Roesky' _publ_contact_author_address ; ; _publ_contact_author_email roesky@chemie.uni-karlsruhe.de loop_ _publ_author_name P.Roesky A.Bhunia A.K.Powell 'Yanhua Lan' S.Kureti data_2 _database_code_depnum_ccdc_archive 'CCDC 794154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H97 Er2 N11 Ni3 O36' _chemical_formula_weight 2167.23 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.682(3) _cell_length_b 15.347(3) _cell_length_c 19.140(4) _cell_angle_alpha 95.82(3) _cell_angle_beta 100.58(3) _cell_angle_gamma 94.33(3) _cell_volume 4197.9(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.259 _exptl_crystal_size_mid 0.143 _exptl_crystal_size_min 0.085 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 2.732 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4926 _exptl_absorpt_correction_T_max 0.7897 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32757 _diffrn_reflns_av_R_equivalents 0.1229 _diffrn_reflns_av_sigmaI/netI 0.1428 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.74 _reflns_number_total 16656 _reflns_number_gt 11087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.1007P)^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 16656 _refine_ls_number_parameters 943 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1806 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1071(7) -0.0538(5) -0.0765(5) 0.027(2) Uani 1 1 d . . . C2 C -0.1988(7) -0.0338(6) -0.0665(6) 0.030(2) Uani 1 1 d . . . H2 H -0.2357 -0.0034 -0.1004 0.036 Uiso 1 1 calc R . . C3 C -0.2328(6) -0.0577(6) -0.0096(6) 0.029(2) Uani 1 1 d . . . C4 C -0.1821(7) -0.1029(6) 0.0427(6) 0.032(2) Uani 1 1 d . . . H4 H -0.2058 -0.1158 0.0838 0.039 Uiso 1 1 calc R . . C5 C -0.0971(7) -0.1276(6) 0.0320(6) 0.035(2) Uani 1 1 d . . . H5 H -0.0629 -0.1605 0.0655 0.042 Uiso 1 1 calc R . . C6 C -0.0596(7) -0.1054(6) -0.0268(6) 0.030(2) Uani 1 1 d . . . C7 C 0.0312(7) -0.1335(6) -0.0339(6) 0.035(2) Uani 1 1 d . . . H7 H 0.0621 -0.1652 0.0020 0.042 Uiso 1 1 calc R . . C8 C 0.1664(7) -0.1512(6) -0.0863(7) 0.038(3) Uani 1 1 d . . . H8A H 0.2150 -0.1130 -0.0514 0.046 Uiso 1 1 calc R . . H8B H 0.1664 -0.2118 -0.0729 0.046 Uiso 1 1 calc R . . C9 C 0.1851(8) -0.1498(6) -0.1589(6) 0.039(3) Uani 1 1 d . . . H9A H 0.1535 -0.2028 -0.1902 0.046 Uiso 1 1 calc R . . H9B H 0.2528 -0.1484 -0.1581 0.046 Uiso 1 1 calc R . . C10 C 0.1928(8) -0.0221(6) -0.2211(6) 0.035(2) Uani 1 1 d . . . H10 H 0.2503 -0.0404 -0.2303 0.042 Uiso 1 1 calc R . . C11 C 0.1623(7) 0.0565(6) -0.2484(6) 0.031(2) Uani 1 1 d . . . C12 C 0.0711(7) 0.0801(6) -0.2488(6) 0.029(2) Uani 1 1 d . . . C13 C 0.0464(7) 0.1568(7) -0.2810(6) 0.033(2) Uani 1 1 d . . . H13 H -0.0147 0.1741 -0.2828 0.040 Uiso 1 1 calc R . . C14 C 0.1084(7) 0.2059(6) -0.3092(6) 0.034(2) Uani 1 1 d . . . C15 C 0.2227(7) 0.1069(7) -0.2815(7) 0.040(3) Uani 1 1 d . . . H15 H 0.2821 0.0874 -0.2841 0.048 Uiso 1 1 calc R . . C16 C 0.1999(7) 0.1827(6) -0.3102(6) 0.035(2) Uani 1 1 d . . . H16 H 0.2431 0.2177 -0.3295 0.042 Uiso 1 1 calc R . . C17 C 0.0845(7) 0.2912(6) -0.3359(6) 0.031(2) Uani 1 1 d . . . C18 C 0.0084(7) 0.5122(6) -0.2470(7) 0.037(2) Uani 1 1 d . . . C19 C -0.0022(8) 0.5453(6) -0.1744(6) 0.037(2) Uani 1 1 d . . . C20 C 0.0685(8) 0.5979(7) -0.1297(7) 0.040(3) Uani 1 1 d . . . H20 H 0.1240 0.6138 -0.1461 0.048 Uiso 1 1 calc R . . C21 C 0.0601(8) 0.6280(6) -0.0611(6) 0.035(2) Uani 1 1 d . . . H21 H 0.1088 0.6664 -0.0313 0.042 Uiso 1 1 calc R . . C22 C -0.0203(8) 0.6024(6) -0.0350(6) 0.035(2) Uani 1 1 d . . . C23 C -0.0917(8) 0.5447(6) -0.0790(6) 0.032(2) Uani 1 1 d . . . C24 C -0.0831(8) 0.5172(6) -0.1492(6) 0.033(2) Uani 1 1 d . . . H24 H -0.1315 0.4796 -0.1801 0.040 Uiso 1 1 calc R . . C25 C -0.0280(8) 0.6382(6) 0.0356(6) 0.033(2) Uani 1 1 d . . . H25 H 0.0230 0.6769 0.0621 0.040 Uiso 1 1 calc R . . C26 C -0.0966(8) 0.6636(7) 0.1398(7) 0.042(3) Uani 1 1 d . . . H26A H -0.0739 0.7268 0.1448 0.050 Uiso 1 1 calc R . . H26B H -0.0546 0.6345 0.1748 0.050 Uiso 1 1 calc R . . C27 C -0.1930(8) 0.6534(6) 0.1532(6) 0.037(2) Uani 1 1 d . . . H27A H -0.1929 0.6598 0.2052 0.044 Uiso 1 1 calc R . . H27B H -0.2305 0.6979 0.1310 0.044 Uiso 1 1 calc R . . C28 C -0.2799(8) 0.5132(6) 0.1524(6) 0.036(2) Uani 1 1 d . . . H28 H -0.2895 0.5349 0.1986 0.043 Uiso 1 1 calc R . . C29 C -0.3211(8) 0.4264(6) 0.1223(6) 0.035(2) Uani 1 1 d . . . C30 C -0.3192(7) 0.3951(6) 0.0507(6) 0.032(2) Uani 1 1 d . . . C31 C -0.3624(7) 0.3084(6) 0.0261(6) 0.031(2) Uani 1 1 d . . . H31 H -0.3666 0.2856 -0.0225 0.038 Uiso 1 1 calc R . . C32 C -0.3984(7) 0.2564(6) 0.0721(6) 0.032(2) Uani 1 1 d . . . C33 C -0.3976(8) 0.2888(6) 0.1421(6) 0.036(2) Uani 1 1 d . . . H33 H -0.4225 0.2525 0.1728 0.043 Uiso 1 1 calc R . . C34 C -0.3610(8) 0.3730(6) 0.1674(7) 0.040(3) Uani 1 1 d . . . H34 H -0.3623 0.3959 0.2152 0.048 Uiso 1 1 calc R . . C35 C -0.4389(8) 0.1615(6) 0.0430(7) 0.038(3) Uani 1 1 d . . . C36 C -0.6688(8) 0.0341(6) 0.0021(7) 0.042(3) Uani 1 1 d . . . C37 C 0.0419(7) 0.3653(6) -0.5520(6) 0.033(2) Uani 1 1 d . . . C38 C 0.0726(7) 0.2850(6) -0.5901(6) 0.033(2) Uani 1 1 d . . . C39 C 0.1321(8) 0.2333(6) -0.5513(6) 0.038(3) Uani 1 1 d . . . H39 H 0.1486 0.2460 -0.5008 0.046 Uiso 1 1 calc R . . C40 C 0.1685(8) 0.1622(6) -0.5862(6) 0.035(2) Uani 1 1 d . A . C41 C 0.0477(8) 0.2661(7) -0.6646(7) 0.042(3) Uani 1 1 d . . . H41 H 0.0065 0.3007 -0.6916 0.051 Uiso 1 1 calc R . . C42 C 0.0831(8) 0.1980(7) -0.6975(7) 0.044(3) Uani 1 1 d . . . H42 H 0.0668 0.1859 -0.7481 0.053 Uiso 1 1 calc R . . C43 C 0.1439(7) 0.1437(7) -0.6592(6) 0.037(2) Uani 1 1 d . . . C44 C 0.1804(8) 0.0743(8) -0.6988(6) 0.044(3) Uani 1 1 d . A . H44 H 0.1598 0.0648 -0.7492 0.053 Uiso 1 1 calc R . . C45A C 0.2950(13) -0.0259(11) -0.7181(10) 0.022(3) Uiso 0.50 1 d P A 1 H45A H 0.2517 -0.0611 -0.7587 0.027 Uiso 0.50 1 calc PR A 1 H45B H 0.3356 0.0161 -0.7374 0.027 Uiso 0.50 1 calc PR A 1 C46A C 0.3486(17) -0.0811(14) -0.6770(12) 0.033(5) Uiso 0.50 1 d P A 1 H46A H 0.4128 -0.0741 -0.6862 0.040 Uiso 0.50 1 calc PR A 1 H46B H 0.3233 -0.1427 -0.6941 0.040 Uiso 0.50 1 calc PR A 1 C45B C 0.259(2) -0.0613(18) -0.7121(16) 0.056(7) Uiso 0.50 1 d P A 2 H45C H 0.1988 -0.0986 -0.7280 0.067 Uiso 0.50 1 calc PR A 2 H45D H 0.2805 -0.0456 -0.7555 0.067 Uiso 0.50 1 calc PR A 2 C46B C 0.3174(14) -0.1058(12) -0.6785(10) 0.020(4) Uiso 0.50 1 d P A 2 H46C H 0.3707 -0.1095 -0.7033 0.024 Uiso 0.50 1 calc PR A 2 H46D H 0.2883 -0.1664 -0.6795 0.024 Uiso 0.50 1 calc PR A 2 C47 C 0.4134(8) -0.1050(6) -0.5571(6) 0.038(3) Uani 1 1 d . A . H47 H 0.4471 -0.1474 -0.5783 0.046 Uiso 1 1 calc R . . C48 C 0.4327(8) -0.0886(6) -0.4811(6) 0.035(2) Uani 1 1 d . . . C49 C 0.4930(7) -0.1408(6) -0.4405(6) 0.035(2) Uani 1 1 d . . . H49 H 0.5245 -0.1827 -0.4646 0.042 Uiso 1 1 calc R . . C50 C 0.5067(9) -0.1320(7) -0.3672(6) 0.042(3) Uani 1 1 d . . . H50 H 0.5484 -0.1665 -0.3407 0.050 Uiso 1 1 calc R . . C51 C 0.4583(7) -0.0713(6) -0.3312(6) 0.032(2) Uani 1 1 d . . . C52 C 0.4005(9) -0.0194(7) -0.3705(6) 0.041(3) Uani 1 1 d . . . H52 H 0.3689 0.0218 -0.3459 0.049 Uiso 1 1 calc R . . C53 C 0.3867(8) -0.0253(7) -0.4457(6) 0.039(3) Uani 1 1 d . A . C54 C 0.4688(8) -0.0583(7) -0.2520(6) 0.038(2) Uani 1 1 d . . . C55 C 0.2071(9) 0.6030(7) -0.3563(7) 0.044(3) Uani 1 1 d . . . H55 H 0.1648 0.6318 -0.3321 0.053 Uiso 1 1 calc R . . C56 C 0.3560(14) 0.6118(13) -0.3911(14) 0.103(7) Uani 1 1 d . . . H56A H 0.4091 0.6565 -0.3853 0.155 Uiso 1 1 calc R . . H56B H 0.3310 0.5950 -0.4422 0.155 Uiso 1 1 calc R . . H56C H 0.3765 0.5600 -0.3690 0.155 Uiso 1 1 calc R . . C57 C 0.3075(13) 0.7388(10) -0.3277(10) 0.077(5) Uani 1 1 d . . . H57A H 0.3696 0.7595 -0.3346 0.116 Uiso 1 1 calc R . . H57B H 0.3062 0.7446 -0.2764 0.116 Uiso 1 1 calc R . . H57C H 0.2615 0.7743 -0.3520 0.116 Uiso 1 1 calc R . . C58 C 0.3984(13) 0.4208(11) 0.1042(10) 0.077(5) Uiso 1 1 d . . . H58A H 0.3714 0.3962 0.1420 0.116 Uiso 1 1 calc R . . H58B H 0.3666 0.4721 0.0903 0.116 Uiso 1 1 calc R . . H58C H 0.4648 0.4388 0.1219 0.116 Uiso 1 1 calc R . . C59 C 0.3438(16) 0.2685(13) 0.0522(13) 0.103(6) Uiso 1 1 d . . . H59A H 0.3267 0.2715 0.0994 0.154 Uiso 1 1 calc R . . H59B H 0.3880 0.2242 0.0486 0.154 Uiso 1 1 calc R . . H59C H 0.2879 0.2523 0.0150 0.154 Uiso 1 1 calc R . . C60 C 0.4186(10) 0.3743(9) -0.0136(8) 0.058(3) Uiso 1 1 d . . . H60 H 0.4487 0.4316 -0.0122 0.070 Uiso 1 1 calc R . . C61 C -0.3548(14) -0.3332(12) -0.4002(11) 0.089(5) Uiso 1 1 d . . . H61A H -0.3829 -0.2933 -0.3688 0.133 Uiso 1 1 calc R . . H61B H -0.4035 -0.3753 -0.4300 0.133 Uiso 1 1 calc R . . H61C H -0.3232 -0.2991 -0.4309 0.133 Uiso 1 1 calc R . . C62 C -0.2707(16) -0.3618(14) -0.2777(13) 0.106(7) Uiso 1 1 d . . . H62A H -0.3116 -0.3178 -0.2648 0.159 Uiso 1 1 calc R . . H62B H -0.2056 -0.3389 -0.2595 0.159 Uiso 1 1 calc R . . H62C H -0.2843 -0.4157 -0.2567 0.159 Uiso 1 1 calc R . . C63 C -0.2422(10) -0.4393(8) -0.3893(8) 0.052(3) Uiso 1 1 d . . . H63 H -0.1999 -0.4705 -0.3600 0.062 Uiso 1 1 calc R . . C64 C 0.0764(14) -0.0720(11) -0.5423(11) 0.085(5) Uiso 1 1 d . . . H64A H 0.0664 -0.0152 -0.5180 0.127 Uiso 1 1 calc R . . H64B H 0.0170 -0.1005 -0.5702 0.127 Uiso 1 1 calc R . . H64C H 0.1202 -0.0627 -0.5745 0.127 Uiso 1 1 calc R . . C65 C 0.1249(14) -0.0964(12) -0.4150(11) 0.083(5) Uiso 1 1 d . . . H65A H 0.1077 -0.0359 -0.4100 0.125 Uiso 1 1 calc R . . H65B H 0.1898 -0.0976 -0.3912 0.125 Uiso 1 1 calc R . . H65C H 0.0844 -0.1341 -0.3928 0.125 Uiso 1 1 calc R . . C66 C 0.1357(12) -0.2077(10) -0.5079(11) 0.074(4) Uiso 1 1 d . . . H66 H 0.1312 -0.2234 -0.5578 0.088 Uiso 1 1 calc R . . C67 C -0.3140(16) 0.3259(14) -0.4111(14) 0.107(7) Uiso 1 1 d . . . H67A H -0.3395 0.3158 -0.4626 0.161 Uiso 1 1 calc R . . H67B H -0.3107 0.2693 -0.3917 0.161 Uiso 1 1 calc R . . H67C H -0.2514 0.3568 -0.4030 0.161 Uiso 1 1 calc R . . C68 C -0.4534(13) 0.3999(12) -0.4265(11) 0.084(5) Uiso 1 1 d . . . H68A H -0.4497 0.3742 -0.4748 0.126 Uiso 1 1 calc R . . H68B H -0.4532 0.4639 -0.4252 0.126 Uiso 1 1 calc R . . H68C H -0.5110 0.3756 -0.4137 0.126 Uiso 1 1 calc R . . C69 C -0.3552(15) 0.4012(13) -0.3108(13) 0.094(6) Uiso 1 1 d . . . H69 H -0.3979 0.4356 -0.2915 0.113 Uiso 1 1 calc R . . N1 N 0.1483(6) -0.0683(5) -0.1856(5) 0.0318(19) Uani 1 1 d . . . N2 N 0.0721(6) -0.1179(5) -0.0859(5) 0.0315(19) Uani 1 1 d . . . N3 N -0.0976(6) 0.6229(5) 0.0668(5) 0.037(2) Uani 1 1 d . . . N4 N -0.2303(6) 0.5637(5) 0.1199(5) 0.0315(19) Uani 1 1 d . . . N5 N 0.3536(6) -0.0669(5) -0.6001(5) 0.034(2) Uani 1 1 d . . . N6 N 0.2409(7) 0.0230(6) -0.6690(6) 0.044(2) Uani 1 1 d . . . N7 N 0.2854(7) 0.6470(6) -0.3574(6) 0.047(2) Uani 1 1 d . . . N8 N -0.3736(11) 0.3790(11) -0.3756(9) 0.085(4) Uani 1 1 d . . . N9 N 0.3870(8) 0.3547(7) 0.0425(7) 0.058(3) Uiso 1 1 d . . . N10 N -0.2866(9) -0.3813(7) -0.3562(7) 0.060(3) Uiso 1 1 d . . . N11 N 0.1145(9) -0.1279(8) -0.4894(7) 0.064(3) Uiso 1 1 d . . . O1 O -0.0759(5) -0.0257(4) -0.1305(4) 0.0315(15) Uani 1 1 d . . . O2 O 0.0106(5) 0.0390(4) -0.2181(4) 0.0331(16) Uani 1 1 d . . . O3 O -0.2850(5) 0.4407(4) 0.0054(4) 0.0368(17) Uani 1 1 d . . . O4 O -0.1678(5) 0.5129(5) -0.0570(4) 0.0408(18) Uani 1 1 d . . . O5 O 0.3318(6) 0.0273(5) -0.4786(5) 0.047(2) Uani 1 1 d . . . O6 O 0.2283(6) 0.1207(5) -0.5452(4) 0.050(2) Uani 1 1 d . . . O7 O -0.0013(6) 0.3082(5) -0.3497(5) 0.047(2) Uani 1 1 d . . . O8 O 0.1469(5) 0.3487(4) -0.3427(4) 0.0342(16) Uani 1 1 d . . . O9 O -0.0600(5) 0.4768(5) -0.2940(4) 0.0414(18) Uani 1 1 d . . . O10 O 0.0893(6) 0.5203(5) -0.2638(4) 0.0432(19) Uani 1 1 d . . . O11 O -0.4376(7) 0.1103(5) 0.0911(5) 0.056(2) Uani 1 1 d . . . O12 O -0.4670(6) 0.1444(5) -0.0228(5) 0.050(2) Uani 1 1 d . . . O13 O 0.0635(6) 0.3784(5) -0.4840(4) 0.0380(18) Uani 1 1 d . . . O14 O 0.4124(5) -0.0123(5) -0.2254(4) 0.0418(19) Uani 1 1 d . . . O15 O 0.5325(6) -0.0875(7) -0.2131(5) 0.057(2) Uani 1 1 d . . . O16 O 0.1823(5) 0.5247(5) -0.3848(4) 0.0380(17) Uani 1 1 d . . . O17 O 0.0020(5) 0.5843(4) -0.4093(4) 0.0368(18) Uani 1 1 d . . . O18 O -0.1123(5) 0.4209(5) -0.4511(5) 0.0403(19) Uani 1 1 d . . . O19 O -0.5974(6) 0.1515(5) -0.1490(4) 0.0428(19) Uani 1 1 d . . . O20 O -0.6474(6) 0.0407(6) -0.0587(5) 0.051(2) Uani 1 1 d . . . O21 O -0.4145(6) 0.1069(5) -0.1668(5) 0.0439(19) Uani 1 1 d . . . O22 O -0.3808(5) -0.0110(6) -0.0555(4) 0.047(2) Uani 1 1 d . . . O23 O 0.3887(6) 0.2061(5) -0.4110(5) 0.055(2) Uiso 1 1 d . . . O24 O -0.3090(14) -0.1732(11) -0.2049(11) 0.139(6) Uiso 1 1 d . . . O25 O -0.2503(7) -0.4568(6) -0.4545(6) 0.061(2) Uiso 1 1 d . . . O26 O 0.1599(9) -0.2633(8) -0.4710(7) 0.087(3) Uiso 1 1 d . . . O27 O 0.4118(7) 0.3217(6) -0.0701(6) 0.067(3) Uiso 1 1 d . . . O28 O -0.2842(9) 0.3830(7) -0.2660(7) 0.081(3) Uiso 1 1 d . . . O29 O -0.4947(8) 0.3638(7) -0.1766(7) 0.076(3) Uiso 1 1 d . . . O30 O -0.3053(7) 0.3574(6) -0.1317(6) 0.064(3) Uiso 1 1 d . . . O31 O -0.2497(6) 0.1946(5) -0.0967(5) 0.054(2) Uiso 1 1 d . . . O32 O -0.0946(6) 0.1705(5) -0.1529(5) 0.049(2) Uiso 1 1 d . . . O33 O -0.1360(7) 0.2774(6) -0.2627(6) 0.063(2) Uiso 1 1 d . . . O34 O 0.4239(11) 0.4632(9) -0.2857(9) 0.104(4) Uiso 1 1 d . . . O35 O 0.2982(6) 0.3641(5) -0.4150(5) 0.051(2) Uiso 1 1 d . . . O36 O 0.4756(7) 0.2065(6) -0.2663(5) 0.055(2) Uiso 1 1 d . . . Ni1 Ni 0.03874(9) -0.04443(7) -0.15480(7) 0.0290(3) Uani 1 1 d . . . Ni2 Ni -0.19537(10) 0.53573(8) 0.03346(8) 0.0321(3) Uani 1 1 d . . . Ni3 Ni 0.28857(10) 0.02587(8) -0.57354(8) 0.0370(3) Uani 1 1 d . A . Er1 Er -0.51771(3) 0.02840(3) -0.10814(3) 0.02783(13) Uani 1 1 d . . . Er2 Er 0.03654(3) 0.45113(3) -0.38281(3) 0.02978(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(5) 0.025(4) 0.029(6) 0.000(4) 0.009(4) 0.011(3) C2 0.031(5) 0.037(5) 0.026(6) 0.007(4) 0.007(4) 0.019(4) C3 0.022(4) 0.035(4) 0.033(6) 0.003(4) 0.007(4) 0.015(4) C4 0.036(5) 0.036(5) 0.029(6) 0.004(4) 0.015(5) 0.010(4) C5 0.035(5) 0.035(5) 0.037(7) 0.013(4) 0.005(5) 0.016(4) C6 0.031(5) 0.032(4) 0.031(6) 0.002(4) 0.008(4) 0.015(4) C7 0.029(5) 0.035(5) 0.044(7) 0.011(4) 0.004(5) 0.019(4) C8 0.032(5) 0.033(5) 0.054(8) 0.012(5) 0.011(5) 0.019(4) C9 0.051(7) 0.030(5) 0.039(7) 0.005(4) 0.014(5) 0.022(4) C10 0.041(6) 0.030(4) 0.043(7) 0.007(4) 0.021(5) 0.020(4) C11 0.041(6) 0.025(4) 0.032(6) 0.002(4) 0.022(5) 0.009(4) C12 0.024(5) 0.032(4) 0.032(6) -0.001(4) 0.008(4) 0.006(4) C13 0.024(5) 0.047(5) 0.032(6) 0.004(4) 0.007(4) 0.016(4) C14 0.041(6) 0.028(4) 0.036(7) 0.005(4) 0.014(5) 0.016(4) C15 0.031(5) 0.041(5) 0.058(8) 0.015(5) 0.021(5) 0.020(4) C16 0.036(5) 0.032(5) 0.041(7) 0.011(4) 0.014(5) 0.011(4) C17 0.031(5) 0.033(5) 0.033(6) 0.002(4) 0.012(4) 0.010(4) C18 0.034(5) 0.035(5) 0.046(8) 0.006(4) 0.015(5) 0.015(4) C19 0.041(6) 0.035(5) 0.036(7) -0.001(4) 0.010(5) 0.016(4) C20 0.046(6) 0.041(5) 0.037(7) 0.009(5) 0.014(5) 0.007(5) C21 0.042(6) 0.037(5) 0.025(6) 0.003(4) 0.007(5) 0.005(4) C22 0.042(6) 0.034(5) 0.034(7) 0.005(4) 0.020(5) 0.005(4) C23 0.044(6) 0.030(4) 0.025(6) 0.005(4) 0.008(5) 0.020(4) C24 0.041(6) 0.031(4) 0.025(6) -0.002(4) 0.002(5) 0.002(4) C25 0.043(6) 0.025(4) 0.031(6) 0.001(4) 0.007(5) 0.003(4) C26 0.039(6) 0.042(5) 0.040(7) -0.006(5) 0.004(5) 0.000(5) C27 0.050(6) 0.027(4) 0.037(7) -0.004(4) 0.020(5) 0.011(4) C28 0.049(6) 0.034(5) 0.025(6) -0.005(4) 0.013(5) 0.011(4) C29 0.040(6) 0.036(5) 0.032(7) 0.004(4) 0.011(5) 0.012(4) C30 0.037(5) 0.030(4) 0.031(6) 0.004(4) 0.011(5) 0.008(4) C31 0.037(5) 0.036(5) 0.023(6) -0.002(4) 0.010(4) 0.012(4) C32 0.039(5) 0.023(4) 0.036(7) -0.001(4) 0.007(5) 0.013(4) C33 0.048(6) 0.036(5) 0.027(6) 0.006(4) 0.014(5) -0.001(4) C34 0.046(6) 0.037(5) 0.038(7) -0.009(4) 0.018(5) -0.004(5) C35 0.041(6) 0.033(5) 0.045(8) -0.001(5) 0.017(5) 0.016(4) C36 0.038(6) 0.030(5) 0.060(9) -0.007(5) 0.017(6) 0.011(4) C37 0.038(5) 0.025(4) 0.041(7) 0.005(4) 0.012(5) 0.017(4) C38 0.042(6) 0.026(4) 0.033(6) 0.000(4) 0.008(5) 0.016(4) C39 0.058(7) 0.034(5) 0.022(6) -0.004(4) 0.005(5) 0.022(5) C40 0.041(6) 0.033(5) 0.030(7) 0.003(4) -0.001(5) 0.025(4) C41 0.048(7) 0.039(5) 0.041(8) 0.006(5) 0.004(5) 0.019(5) C42 0.047(7) 0.052(6) 0.033(7) 0.000(5) 0.005(5) 0.020(5) C43 0.033(5) 0.043(5) 0.037(7) 0.004(4) 0.009(5) 0.019(4) C44 0.050(7) 0.060(7) 0.024(7) -0.006(5) 0.001(5) 0.032(6) C47 0.043(6) 0.035(5) 0.040(7) -0.001(4) 0.017(5) 0.015(4) C48 0.051(6) 0.037(5) 0.022(6) 0.006(4) 0.009(5) 0.023(5) C49 0.039(6) 0.037(5) 0.032(7) 0.003(4) 0.008(5) 0.020(4) C50 0.056(7) 0.045(6) 0.034(7) 0.017(5) 0.015(6) 0.033(5) C51 0.036(5) 0.041(5) 0.026(6) 0.007(4) 0.016(5) 0.014(4) C52 0.060(7) 0.040(5) 0.027(7) 0.004(4) 0.011(5) 0.030(5) C53 0.050(6) 0.044(5) 0.029(6) -0.003(4) 0.018(5) 0.026(5) C54 0.051(7) 0.042(5) 0.021(6) 0.000(4) 0.007(5) 0.011(5) C55 0.047(7) 0.042(6) 0.048(8) 0.014(5) 0.012(6) 0.012(5) C56 0.075(12) 0.103(13) 0.15(2) 0.009(13) 0.069(14) 0.005(10) C57 0.083(12) 0.066(9) 0.079(13) 0.012(8) 0.011(10) -0.015(8) N1 0.039(5) 0.025(4) 0.034(6) 0.007(3) 0.008(4) 0.013(3) N2 0.032(4) 0.024(3) 0.040(6) 0.004(3) 0.008(4) 0.012(3) N3 0.037(5) 0.033(4) 0.045(6) 0.000(4) 0.018(4) 0.012(4) N4 0.035(4) 0.025(4) 0.036(6) -0.001(3) 0.014(4) 0.008(3) N5 0.038(5) 0.039(4) 0.028(5) -0.001(4) 0.009(4) 0.017(4) N6 0.051(6) 0.045(5) 0.038(6) 0.001(4) 0.005(5) 0.031(4) N7 0.042(6) 0.047(5) 0.052(7) 0.009(5) 0.009(5) -0.001(4) N8 0.079(10) 0.120(12) 0.057(10) 0.009(8) 0.013(8) 0.013(9) O1 0.036(4) 0.040(3) 0.025(4) 0.013(3) 0.012(3) 0.019(3) O2 0.026(3) 0.035(3) 0.044(5) 0.012(3) 0.013(3) 0.013(3) O3 0.049(4) 0.037(3) 0.026(4) 0.000(3) 0.012(4) 0.004(3) O4 0.039(4) 0.045(4) 0.038(5) -0.001(3) 0.015(4) -0.008(3) O5 0.068(6) 0.042(4) 0.038(5) 0.004(3) 0.017(4) 0.033(4) O6 0.072(6) 0.055(4) 0.022(5) -0.002(3) -0.005(4) 0.041(4) O7 0.047(5) 0.041(4) 0.063(6) 0.024(4) 0.021(4) 0.022(3) O8 0.038(4) 0.043(4) 0.025(4) 0.012(3) 0.008(3) 0.010(3) O9 0.039(4) 0.052(4) 0.031(5) -0.008(3) 0.011(4) 0.005(3) O10 0.042(4) 0.059(5) 0.028(5) 0.003(3) 0.005(4) 0.014(4) O11 0.083(7) 0.026(3) 0.062(7) 0.007(4) 0.021(5) 0.001(4) O12 0.063(6) 0.033(4) 0.050(6) -0.006(4) 0.003(4) 0.010(4) O13 0.059(5) 0.044(4) 0.013(4) 0.004(3) 0.004(3) 0.028(3) O14 0.038(4) 0.049(4) 0.038(5) -0.003(3) 0.009(4) 0.013(3) O15 0.055(5) 0.102(7) 0.019(5) 0.019(4) 0.000(4) 0.040(5) O16 0.033(4) 0.043(4) 0.044(5) 0.006(3) 0.020(4) 0.010(3) O17 0.054(5) 0.028(3) 0.035(5) 0.014(3) 0.012(4) 0.025(3) O18 0.027(4) 0.044(4) 0.046(5) -0.003(3) -0.003(3) 0.015(3) O19 0.050(5) 0.048(4) 0.037(5) 0.009(3) 0.016(4) 0.024(4) O20 0.036(4) 0.082(6) 0.050(6) 0.016(4) 0.034(4) 0.029(4) O21 0.044(4) 0.053(4) 0.046(5) 0.019(4) 0.025(4) 0.019(4) O22 0.035(4) 0.086(6) 0.028(5) 0.025(4) 0.001(3) 0.040(4) Ni1 0.0296(6) 0.0285(5) 0.0332(8) 0.0069(5) 0.0108(6) 0.0143(5) Ni2 0.0397(7) 0.0295(6) 0.0281(8) -0.0016(5) 0.0113(6) 0.0045(5) Ni3 0.0474(8) 0.0375(6) 0.0282(8) -0.0005(5) 0.0067(6) 0.0255(6) Er1 0.0298(2) 0.0298(2) 0.0266(3) 0.00413(16) 0.00884(19) 0.01113(16) Er2 0.0354(2) 0.0282(2) 0.0295(3) 0.00495(17) 0.0106(2) 0.01460(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.304(12) . ? C1 C6 1.418(14) . ? C1 C2 1.446(12) . ? C2 C3 1.350(14) . ? C3 C4 1.406(15) . ? C3 C36 1.545(13) 2_455 ? C4 C5 1.376(14) . ? C5 C6 1.402(15) . ? C6 C7 1.457(12) . ? C7 N2 1.285(14) . ? C8 C9 1.467(16) . ? C8 N2 1.512(12) . ? C9 N1 1.499(12) . ? C10 N1 1.259(13) . ? C10 C11 1.432(13) . ? C11 C15 1.411(14) . ? C11 C12 1.411(13) . ? C12 O2 1.311(12) . ? C12 C13 1.423(14) . ? C13 C14 1.359(15) . ? C14 C16 1.418(14) . ? C14 C17 1.496(13) . ? C15 C16 1.375(14) . ? C17 O8 1.257(12) . ? C17 O7 1.290(12) . ? C17 Er2 2.793(9) . ? C18 O9 1.266(14) . ? C18 O10 1.287(13) . ? C18 C19 1.470(15) . ? C18 Er2 2.787(11) . ? C19 C20 1.367(16) . ? C19 C24 1.414(15) . ? C20 C21 1.378(16) . ? C21 C22 1.408(15) . ? C22 C23 1.406(16) . ? C22 C25 1.434(15) . ? C23 O4 1.340(13) . ? C23 C24 1.398(14) . ? C25 N3 1.293(14) . ? C26 N3 1.468(15) . ? C26 C27 1.484(15) . ? C27 N4 1.477(12) . ? C28 N4 1.303(13) . ? C28 C29 1.438(14) . ? C29 C30 1.411(15) . ? C29 C34 1.421(15) . ? C30 O3 1.311(12) . ? C30 C31 1.425(14) . ? C31 C32 1.392(15) . ? C32 C33 1.380(15) . ? C32 C35 1.540(14) . ? C33 C34 1.367(14) . ? C35 O12 1.245(15) . ? C35 O11 1.269(14) . ? C36 O22 1.241(15) 2_455 ? C36 O20 1.271(15) . ? C36 C3 1.545(13) 2_455 ? C37 O17 1.257(12) 2_564 ? C37 O13 1.273(13) . ? C37 C38 1.509(12) . ? C38 C39 1.390(14) . ? C38 C41 1.399(16) . ? C39 C40 1.411(12) . ? C40 O6 1.315(12) . ? C40 C43 1.372(16) . ? C41 C42 1.353(15) . ? C42 C43 1.422(15) . ? C43 C44 1.438(13) . ? C44 N6 1.320(14) . ? C45A C46A 1.40(3) . ? C45A N6 1.516(19) . ? C46A N5 1.45(2) . ? C45B C46B 1.27(3) . ? C45B N6 1.53(3) . ? C46B N5 1.54(2) . ? C47 N5 1.305(14) . ? C47 C48 1.421(16) . ? C48 C53 1.412(12) . ? C48 C49 1.418(14) . ? C49 C50 1.373(16) . ? C50 C51 1.413(13) . ? C51 C52 1.382(14) . ? C51 C54 1.486(15) . ? C52 C53 1.408(16) . ? C53 O5 1.309(13) . ? C54 O15 1.226(14) . ? C54 O14 1.270(13) . ? C54 Er1 2.900(11) 1_655 ? C55 O16 1.265(13) . ? C55 N7 1.293(15) . ? C56 N7 1.429(19) . ? C57 N7 1.454(18) . ? C58 N9 1.45(2) . ? C59 N9 1.47(2) . ? C60 O27 1.266(17) . ? C60 N9 1.299(18) . ? C61 N10 1.48(2) . ? C62 N10 1.47(3) . ? C63 O25 1.230(16) . ? C63 N10 1.320(17) . ? C64 N11 1.45(2) . ? C65 N11 1.43(2) . ? C66 O26 1.196(19) . ? C66 N11 1.317(19) . ? C67 N8 1.45(3) . ? C68 N8 1.46(2) . ? C69 N8 1.23(3) . ? C69 O28 1.29(2) . ? N1 Ni1 1.860(8) . ? N2 Ni1 1.844(9) . ? N3 Ni2 1.860(9) . ? N4 Ni2 1.840(9) . ? N5 Ni3 1.853(7) . ? N6 Ni3 1.828(10) . ? O1 Ni1 1.861(7) . ? O2 Ni1 1.868(7) . ? O3 Ni2 1.855(7) . ? O4 Ni2 1.855(8) . ? O5 Ni3 1.809(9) . ? O6 Ni3 1.845(7) . ? O7 Er2 2.397(7) . ? O8 Er2 2.421(7) . ? O9 Er2 2.426(7) . ? O10 Er2 2.378(8) . ? O11 Er1 2.253(7) 2_455 ? O12 Er1 2.271(8) . ? O13 Er2 2.250(7) . ? O14 Er1 2.292(8) 1_655 ? O15 Er1 2.786(9) 1_655 ? O16 Er2 2.352(7) . ? O17 C37 1.257(12) 2_564 ? O17 Er2 2.228(6) . ? O18 Er2 2.318(7) . ? O19 Er1 2.418(7) . ? O20 Er1 2.288(7) . ? O21 Er1 2.373(8) . ? O22 C36 1.241(15) 2_455 ? O22 Er1 2.233(7) . ? Er1 O11 2.253(7) 2_455 ? Er1 O14 2.292(8) 1_455 ? Er1 O15 2.786(9) 1_455 ? Er1 C54 2.900(11) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 125.5(8) . . ? O1 C1 C2 118.4(9) . . ? C6 C1 C2 116.1(9) . . ? C3 C2 C1 120.9(9) . . ? C2 C3 C4 122.6(8) . . ? C2 C3 C36 118.1(9) . 2_455 ? C4 C3 C36 119.2(10) . 2_455 ? C5 C4 C3 117.6(10) . . ? C4 C5 C6 121.7(9) . . ? C5 C6 C1 120.8(8) . . ? C5 C6 C7 118.4(9) . . ? C1 C6 C7 120.8(9) . . ? N2 C7 C6 124.0(10) . . ? C9 C8 N2 107.6(9) . . ? C8 C9 N1 106.6(8) . . ? N1 C10 C11 124.1(9) . . ? C15 C11 C12 119.4(9) . . ? C15 C11 C10 118.4(9) . . ? C12 C11 C10 121.9(9) . . ? O2 C12 C11 124.1(9) . . ? O2 C12 C13 118.6(8) . . ? C11 C12 C13 117.2(9) . . ? C14 C13 C12 121.4(9) . . ? C13 C14 C16 122.3(9) . . ? C13 C14 C17 120.6(9) . . ? C16 C14 C17 117.0(9) . . ? C16 C15 C11 123.1(9) . . ? C15 C16 C14 116.3(10) . . ? O8 C17 O7 118.8(9) . . ? O8 C17 C14 121.1(9) . . ? O7 C17 C14 120.0(9) . . ? O8 C17 Er2 59.9(5) . . ? O7 C17 Er2 58.9(5) . . ? C14 C17 Er2 178.4(7) . . ? O9 C18 O10 118.7(10) . . ? O9 C18 C19 122.0(10) . . ? O10 C18 C19 119.3(10) . . ? O9 C18 Er2 60.4(6) . . ? O10 C18 Er2 58.3(6) . . ? C19 C18 Er2 177.6(8) . . ? C20 C19 C24 120.1(10) . . ? C20 C19 C18 120.1(10) . . ? C24 C19 C18 119.6(10) . . ? C19 C20 C21 120.7(11) . . ? C20 C21 C22 120.4(11) . . ? C23 C22 C21 119.6(10) . . ? C23 C22 C25 121.7(10) . . ? C21 C22 C25 118.6(10) . . ? O4 C23 C24 117.5(10) . . ? O4 C23 C22 123.5(10) . . ? C24 C23 C22 119.0(10) . . ? C23 C24 C19 120.1(10) . . ? N3 C25 C22 126.4(10) . . ? N3 C26 C27 108.1(9) . . ? N4 C27 C26 104.8(8) . . ? N4 C28 C29 123.5(10) . . ? C30 C29 C34 121.6(9) . . ? C30 C29 C28 120.6(10) . . ? C34 C29 C28 117.8(10) . . ? O3 C30 C29 125.2(9) . . ? O3 C30 C31 118.7(9) . . ? C29 C30 C31 116.0(9) . . ? C32 C31 C30 121.2(9) . . ? C33 C32 C31 121.1(9) . . ? C33 C32 C35 120.5(10) . . ? C31 C32 C35 118.4(9) . . ? C34 C33 C32 120.0(10) . . ? C33 C34 C29 120.0(10) . . ? O12 C35 O11 128.7(10) . . ? O12 C35 C32 117.7(10) . . ? O11 C35 C32 113.6(10) . . ? O22 C36 O20 127.0(10) 2_455 . ? O22 C36 C3 117.1(10) 2_455 2_455 ? O20 C36 C3 115.9(10) . 2_455 ? O17 C37 O13 124.7(8) 2_564 . ? O17 C37 C38 116.6(10) 2_564 . ? O13 C37 C38 118.6(8) . . ? C39 C38 C41 119.8(9) . . ? C39 C38 C37 119.3(9) . . ? C41 C38 C37 120.7(9) . . ? C38 C39 C40 120.8(10) . . ? O6 C40 C43 124.5(8) . . ? O6 C40 C39 116.0(10) . . ? C43 C40 C39 119.4(9) . . ? C42 C41 C38 119.0(10) . . ? C41 C42 C43 122.6(11) . . ? C40 C43 C42 118.5(9) . . ? C40 C43 C44 122.7(9) . . ? C42 C43 C44 118.7(11) . . ? N6 C44 C43 123.8(11) . . ? C46A C45A N6 106.9(16) . . ? C45A C46A N5 116.5(16) . . ? C46B C45B N6 115(2) . . ? C45B C46B N5 113.3(17) . . ? N5 C47 C48 125.7(9) . . ? C53 C48 C49 119.6(10) . . ? C53 C48 C47 120.5(9) . . ? C49 C48 C47 119.7(9) . . ? C50 C49 C48 121.3(9) . . ? C49 C50 C51 119.6(9) . . ? C52 C51 C50 119.2(10) . . ? C52 C51 C54 117.9(9) . . ? C50 C51 C54 122.9(9) . . ? C51 C52 C53 122.6(9) . . ? O5 C53 C52 118.5(8) . . ? O5 C53 C48 123.8(10) . . ? C52 C53 C48 117.6(10) . . ? O15 C54 O14 120.6(10) . . ? O15 C54 C51 121.3(10) . . ? O14 C54 C51 118.0(10) . . ? O15 C54 Er1 72.4(6) . 1_655 ? O14 C54 Er1 49.7(5) . 1_655 ? C51 C54 Er1 160.3(7) . 1_655 ? O16 C55 N7 125.4(11) . . ? O27 C60 N9 124.1(13) . . ? O25 C63 N10 126.4(14) . . ? O26 C66 N11 129.3(19) . . ? N8 C69 O28 127(2) . . ? C10 N1 C9 120.8(8) . . ? C10 N1 Ni1 127.1(6) . . ? C9 N1 Ni1 112.0(7) . . ? C7 N2 C8 118.2(9) . . ? C7 N2 Ni1 127.6(7) . . ? C8 N2 Ni1 113.5(7) . . ? C25 N3 C26 121.0(9) . . ? C25 N3 Ni2 124.8(8) . . ? C26 N3 Ni2 113.3(7) . . ? C28 N4 C27 120.5(9) . . ? C28 N4 Ni2 127.2(7) . . ? C27 N4 Ni2 112.4(7) . . ? C47 N5 C46A 120.4(11) . . ? C47 N5 C46B 121.7(9) . . ? C46A N5 C46B 21.7(10) . . ? C47 N5 Ni3 125.8(7) . . ? C46A N5 Ni3 112.3(9) . . ? C46B N5 Ni3 111.8(8) . . ? C44 N6 C45A 116.6(11) . . ? C44 N6 C45B 119.6(14) . . ? C45A N6 C45B 29.1(11) . . ? C44 N6 Ni3 126.6(8) . . ? C45A N6 Ni3 114.7(9) . . ? C45B N6 Ni3 112.1(12) . . ? C55 N7 C56 123.4(12) . . ? C55 N7 C57 122.8(12) . . ? C56 N7 C57 113.7(13) . . ? C69 N8 C67 121.5(19) . . ? C69 N8 C68 127.2(18) . . ? C67 N8 C68 111.2(16) . . ? C60 N9 C58 119.1(13) . . ? C60 N9 C59 126.0(14) . . ? C58 N9 C59 114.7(15) . . ? C63 N10 C62 123.2(14) . . ? C63 N10 C61 118.3(14) . . ? C62 N10 C61 118.6(14) . . ? C66 N11 C65 119.3(14) . . ? C66 N11 C64 121.9(15) . . ? C65 N11 C64 118.7(13) . . ? C1 O1 Ni1 126.2(6) . . ? C12 O2 Ni1 124.7(6) . . ? C30 O3 Ni2 123.5(7) . . ? C23 O4 Ni2 126.6(7) . . ? C53 O5 Ni3 128.8(6) . . ? C40 O6 Ni3 127.0(7) . . ? C17 O7 Er2 93.6(6) . . ? C17 O8 Er2 93.4(6) . . ? C18 O9 Er2 92.6(6) . . ? C18 O10 Er2 94.3(7) . . ? C35 O11 Er1 142.2(8) . 2_455 ? C35 O12 Er1 140.9(7) . . ? C37 O13 Er2 146.7(6) . . ? C54 O14 Er1 105.4(7) . 1_655 ? C54 O15 Er1 82.8(6) . 1_655 ? C55 O16 Er2 123.0(7) . . ? C37 O17 Er2 152.2(7) 2_564 . ? C36 O20 Er1 136.8(8) . . ? C36 O22 Er1 149.2(8) 2_455 . ? N2 Ni1 N1 86.3(4) . . ? N2 Ni1 O1 95.2(3) . . ? N1 Ni1 O1 175.5(4) . . ? N2 Ni1 O2 174.5(4) . . ? N1 Ni1 O2 94.0(3) . . ? O1 Ni1 O2 84.9(3) . . ? N4 Ni2 O3 93.9(3) . . ? N4 Ni2 O4 175.3(4) . . ? O3 Ni2 O4 85.6(3) . . ? N4 Ni2 N3 85.4(4) . . ? O3 Ni2 N3 173.9(4) . . ? O4 Ni2 N3 95.5(4) . . ? O5 Ni3 N6 178.0(5) . . ? O5 Ni3 O6 84.0(3) . . ? N6 Ni3 O6 95.4(4) . . ? O5 Ni3 N5 94.8(4) . . ? N6 Ni3 N5 85.9(4) . . ? O6 Ni3 N5 177.7(4) . . ? O22 Er1 O11 80.5(4) . 2_455 ? O22 Er1 O12 78.6(3) . . ? O11 Er1 O12 127.2(3) 2_455 . ? O22 Er1 O20 126.8(3) . . ? O11 Er1 O20 75.5(3) 2_455 . ? O12 Er1 O20 79.4(3) . . ? O22 Er1 O14 125.2(3) . 1_455 ? O11 Er1 O14 85.5(3) 2_455 1_455 ? O12 Er1 O14 144.7(3) . 1_455 ? O20 Er1 O14 99.5(3) . 1_455 ? O22 Er1 O21 78.9(3) . . ? O11 Er1 O21 140.6(3) 2_455 . ? O12 Er1 O21 80.7(3) . . ? O20 Er1 O21 142.7(3) . . ? O14 Er1 O21 79.5(3) 1_455 . ? O22 Er1 O19 143.8(3) . . ? O11 Er1 O19 135.1(3) 2_455 . ? O12 Er1 O19 73.6(3) . . ? O20 Er1 O19 70.0(3) . . ? O14 Er1 O19 73.0(3) 1_455 . ? O21 Er1 O19 74.3(3) . . ? O22 Er1 O15 76.0(3) . 1_455 ? O11 Er1 O15 71.3(3) 2_455 1_455 ? O12 Er1 O15 145.1(3) . 1_455 ? O20 Er1 O15 135.3(3) . 1_455 ? O14 Er1 O15 49.4(2) 1_455 1_455 ? O21 Er1 O15 71.3(3) . 1_455 ? O19 Er1 O15 116.4(3) . 1_455 ? O22 Er1 C54 100.3(3) . 1_455 ? O11 Er1 C54 80.4(3) 2_455 1_455 ? O12 Er1 C54 151.0(3) . 1_455 ? O20 Er1 C54 121.0(3) . 1_455 ? O14 Er1 C54 25.0(3) 1_455 1_455 ? O21 Er1 C54 70.7(3) . 1_455 ? O19 Er1 C54 93.4(3) . 1_455 ? O15 Er1 C54 24.8(3) 1_455 1_455 ? O17 Er2 O13 106.2(3) . . ? O17 Er2 O18 78.1(3) . . ? O13 Er2 O18 77.9(3) . . ? O17 Er2 O16 76.6(3) . . ? O13 Er2 O16 81.4(3) . . ? O18 Er2 O16 141.1(3) . . ? O17 Er2 O10 85.6(3) . . ? O13 Er2 O10 151.0(3) . . ? O18 Er2 O10 130.9(3) . . ? O16 Er2 O10 75.7(3) . . ? O17 Er2 O7 153.0(3) . . ? O13 Er2 O7 85.5(3) . . ? O18 Er2 O7 80.9(3) . . ? O16 Er2 O7 130.0(3) . . ? O10 Er2 O7 95.7(3) . . ? O17 Er2 O8 151.8(3) . . ? O13 Er2 O8 75.2(2) . . ? O18 Er2 O8 128.5(2) . . ? O16 Er2 O8 75.8(2) . . ? O10 Er2 O8 82.1(3) . . ? O7 Er2 O8 54.1(3) . . ? O17 Er2 O9 83.7(3) . . ? O13 Er2 O9 151.1(3) . . ? O18 Er2 O9 77.8(3) . . ? O16 Er2 O9 127.4(3) . . ? O10 Er2 O9 54.4(3) . . ? O7 Er2 O9 75.4(3) . . ? O8 Er2 O9 108.8(3) . . ? O17 Er2 C18 84.3(3) . . ? O13 Er2 C18 169.5(3) . . ? O18 Er2 C18 104.3(3) . . ? O16 Er2 C18 102.0(3) . . ? O10 Er2 C18 27.4(3) . . ? O7 Er2 C18 84.7(3) . . ? O8 Er2 C18 95.8(3) . . ? O9 Er2 C18 27.0(3) . . ? O17 Er2 C17 174.5(3) . . ? O13 Er2 C17 78.9(3) . . ? O18 Er2 C17 105.3(3) . . ? O16 Er2 C17 102.5(3) . . ? O10 Er2 C17 88.9(3) . . ? O7 Er2 C17 27.5(3) . . ? O8 Er2 C17 26.7(3) . . ? O9 Er2 C17 92.7(3) . . ? C18 Er2 C17 90.7(3) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 2.420 _refine_diff_density_min -4.173 _refine_diff_density_rms 0.221 # Attachment '- compound3.cif' data_d:\calc\ab68_ni_lu_salen\ab68t _database_code_depnum_ccdc_archive 'CCDC 794155' #TrackingRef '- compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H42 Lu2 N7 Ni3 O22, 4(C3 H7 N O), 10(H2 O)' _chemical_formula_sum 'C69 H97 Lu2 N11 Ni3 O36' _chemical_formula_weight 2182.65 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.637(3) _cell_length_b 15.373(3) _cell_length_c 19.098(4) _cell_angle_alpha 95.65(3) _cell_angle_beta 100.61(3) _cell_angle_gamma 94.39(3) _cell_volume 4183.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2204 _exptl_absorpt_coefficient_mu 3.095 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5628 _exptl_absorpt_correction_T_max 0.8361 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30288 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.1039 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.75 _reflns_number_total 16731 _reflns_number_gt 11735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0583P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16731 _refine_ls_number_parameters 943 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1083(6) -0.0534(5) -0.0772(4) 0.0193(16) Uani 1 1 d . . . C2 C -0.1989(6) -0.0339(5) -0.0682(4) 0.0209(16) Uani 1 1 d . . . H2 H -0.2356 -0.0041 -0.1028 0.025 Uiso 1 1 calc R . . C3 C -0.2343(6) -0.0575(6) -0.0100(4) 0.0232(17) Uani 1 1 d . . . C4 C -0.1838(6) -0.1044(6) 0.0410(4) 0.0251(18) Uani 1 1 d . . . H4 H -0.2089 -0.1201 0.0810 0.030 Uiso 1 1 calc R . . C5 C -0.0971(6) -0.1272(6) 0.0321(4) 0.0235(17) Uani 1 1 d . . . H5 H -0.0623 -0.1591 0.0662 0.028 Uiso 1 1 calc R . . C6 C -0.0590(6) -0.1037(5) -0.0277(4) 0.0214(16) Uani 1 1 d . . . C7 C 0.0316(6) -0.1331(5) -0.0347(4) 0.0205(16) Uani 1 1 d . . . H7 H 0.0618 -0.1654 0.0013 0.025 Uiso 1 1 calc R . . C8 C 0.1661(6) -0.1500(6) -0.0852(5) 0.0258(18) Uani 1 1 d . . . H8A H 0.1661 -0.2105 -0.0717 0.031 Uiso 1 1 calc R . . H8B H 0.2142 -0.1115 -0.0501 0.031 Uiso 1 1 calc R . . C9 C 0.1856(6) -0.1479(6) -0.1603(5) 0.0278(19) Uani 1 1 d . . . H9A H 0.2534 -0.1469 -0.1597 0.033 Uiso 1 1 calc R . . H9B H 0.1532 -0.2002 -0.1923 0.033 Uiso 1 1 calc R . . C10 C 0.1962(6) -0.0195(5) -0.2215(4) 0.0257(18) Uani 1 1 d . . . H10 H 0.2546 -0.0371 -0.2295 0.031 Uiso 1 1 calc R . . C11 C 0.1634(6) 0.0589(6) -0.2505(5) 0.0256(18) Uani 1 1 d . . . C12 C 0.0723(6) 0.0828(5) -0.2487(4) 0.0194(16) Uani 1 1 d . . . C13 C 0.0467(6) 0.1594(5) -0.2817(4) 0.0206(16) Uani 1 1 d . . . H13 H -0.0150 0.1759 -0.2842 0.025 Uiso 1 1 calc R . . C14 C 0.1099(6) 0.2095(5) -0.3098(4) 0.0238(17) Uani 1 1 d . . . C15 C 0.2249(7) 0.1097(6) -0.2824(5) 0.030(2) Uani 1 1 d . . . H15 H 0.2849 0.0913 -0.2844 0.036 Uiso 1 1 calc R . . C16 C 0.2004(6) 0.1853(6) -0.3110(5) 0.0253(18) Uani 1 1 d . . . H16 H 0.2433 0.2201 -0.3308 0.030 Uiso 1 1 calc R . . C17 C 0.0852(6) 0.2949(6) -0.3355(4) 0.0254(18) Uani 1 1 d . . . C18 C 0.0076(7) 0.5115(6) -0.2489(5) 0.0274(19) Uani 1 1 d . . . C19 C -0.0027(6) 0.5451(6) -0.1750(4) 0.0253(18) Uani 1 1 d . . . C20 C 0.0689(7) 0.6002(6) -0.1304(5) 0.0296(19) Uani 1 1 d . . . H20 H 0.1235 0.6182 -0.1476 0.036 Uiso 1 1 calc R . . C21 C 0.0605(7) 0.6290(6) -0.0612(5) 0.0278(19) Uani 1 1 d . . . H21 H 0.1096 0.6665 -0.0308 0.033 Uiso 1 1 calc R . . C22 C -0.0214(6) 0.6025(5) -0.0352(4) 0.0238(17) Uani 1 1 d . . . C23 C -0.0932(7) 0.5444(5) -0.0794(4) 0.0254(18) Uani 1 1 d . . . C24 C -0.0829(6) 0.5167(6) -0.1497(4) 0.0232(17) Uani 1 1 d . . . H24 H -0.1309 0.4783 -0.1805 0.028 Uiso 1 1 calc R . . C25 C -0.0286(7) 0.6381(5) 0.0355(5) 0.0264(18) Uani 1 1 d . . . H25 H 0.0218 0.6776 0.0620 0.032 Uiso 1 1 calc R . . C26 C -0.0952(7) 0.6628(6) 0.1406(4) 0.0273(18) Uani 1 1 d . . . H26A H -0.0733 0.7260 0.1450 0.033 Uiso 1 1 calc R . . H26B H -0.0525 0.6342 0.1757 0.033 Uiso 1 1 calc R . . C27 C -0.1943(7) 0.6506(6) 0.1534(5) 0.031(2) Uani 1 1 d . . . H27A H -0.1948 0.6562 0.2054 0.038 Uiso 1 1 calc R . . H27B H -0.2321 0.6952 0.1313 0.038 Uiso 1 1 calc R . . C28 C -0.2809(6) 0.5111(6) 0.1524(4) 0.0241(17) Uani 1 1 d . . . H28 H -0.2911 0.5329 0.1984 0.029 Uiso 1 1 calc R . . C29 C -0.3201(6) 0.4249(5) 0.1226(4) 0.0217(16) Uani 1 1 d . . . C30 C -0.3208(6) 0.3926(5) 0.0512(4) 0.0199(16) Uani 1 1 d . . . C31 C -0.3629(6) 0.3065(5) 0.0253(4) 0.0234(17) Uani 1 1 d . . . H31 H -0.3669 0.2844 -0.0235 0.028 Uiso 1 1 calc R . . C32 C -0.3981(6) 0.2551(5) 0.0713(4) 0.0220(16) Uani 1 1 d . . . C33 C -0.3972(7) 0.2870(6) 0.1428(4) 0.0287(19) Uani 1 1 d . . . H33 H -0.4216 0.2506 0.1737 0.034 Uiso 1 1 calc R . . C34 C -0.3611(7) 0.3705(6) 0.1670(4) 0.0272(18) Uani 1 1 d . . . H34 H -0.3632 0.3933 0.2147 0.033 Uiso 1 1 calc R . . C35 C -0.4387(6) 0.1606(6) 0.0432(4) 0.0217(16) Uani 1 1 d . . . C36 C -0.6685(7) 0.0348(6) 0.0019(4) 0.0260(18) Uani 1 1 d . . . C37 C 0.0438(6) 0.3680(5) -0.5503(4) 0.0228(17) Uani 1 1 d . . . C38 C 0.0731(6) 0.2863(5) -0.5885(4) 0.0233(18) Uani 1 1 d . . . C39 C 0.1311(7) 0.2352(6) -0.5492(4) 0.0269(19) Uani 1 1 d . . . H39 H 0.1465 0.2481 -0.4985 0.032 Uiso 1 1 calc R . . C40 C 0.1683(7) 0.1635(6) -0.5829(4) 0.030(2) Uani 1 1 d . A . C41 C 0.0477(7) 0.2672(6) -0.6635(5) 0.032(2) Uani 1 1 d . . . H41 H 0.0077 0.3026 -0.6907 0.038 Uiso 1 1 calc R . . C42 C 0.0809(7) 0.1975(7) -0.6965(5) 0.036(2) Uani 1 1 d . . . H42 H 0.0628 0.1840 -0.7470 0.043 Uiso 1 1 calc R . . C43 C 0.1416(7) 0.1445(6) -0.6578(5) 0.0299(19) Uani 1 1 d . . . C44 C 0.1789(7) 0.0751(6) -0.6978(5) 0.036(2) Uani 1 1 d . A . H44 H 0.1586 0.0656 -0.7484 0.043 Uiso 1 1 calc R . . C45A C 0.2927(12) -0.0256(11) -0.7164(8) 0.021(3) Uiso 0.50 1 d P A 1 H45A H 0.2487 -0.0615 -0.7563 0.025 Uiso 0.50 1 calc PR A 1 H45B H 0.3325 0.0157 -0.7372 0.025 Uiso 0.50 1 calc PR A 1 C46A C 0.3477(15) -0.0797(13) -0.6769(9) 0.024(4) Uiso 0.50 1 d P A 1 H46A H 0.4118 -0.0716 -0.6866 0.028 Uiso 0.50 1 calc PR A 1 H46B H 0.3231 -0.1415 -0.6936 0.028 Uiso 0.50 1 calc PR A 1 C45B C 0.2516(16) -0.0589(14) -0.7108(10) 0.035(4) Uiso 0.50 1 d P A 2 H45C H 0.1918 -0.0968 -0.7223 0.042 Uiso 0.50 1 calc PR A 2 H45D H 0.2687 -0.0454 -0.7566 0.042 Uiso 0.50 1 calc PR A 2 C46B C 0.3183(15) -0.1032(14) -0.6755(9) 0.024(4) Uiso 0.50 1 d P A 2 H46C H 0.3716 -0.1032 -0.7008 0.029 Uiso 0.50 1 calc PR A 2 H46D H 0.2929 -0.1650 -0.6764 0.029 Uiso 0.50 1 calc PR A 2 C47 C 0.4127(7) -0.1037(6) -0.5582(4) 0.030(2) Uani 1 1 d . A . H47 H 0.4467 -0.1448 -0.5806 0.036 Uiso 1 1 calc R . . C48 C 0.4310(7) -0.0895(6) -0.4818(5) 0.0269(19) Uani 1 1 d . . . C49 C 0.4940(6) -0.1407(6) -0.4406(4) 0.0273(19) Uani 1 1 d . . . H49 H 0.5271 -0.1809 -0.4649 0.033 Uiso 1 1 calc R . . C50 C 0.5079(7) -0.1334(6) -0.3669(5) 0.030(2) Uani 1 1 d . . . H50 H 0.5494 -0.1685 -0.3407 0.036 Uiso 1 1 calc R . . C51 C 0.4596(6) -0.0733(6) -0.3311(4) 0.0263(18) Uani 1 1 d . . . C52 C 0.4012(7) -0.0212(6) -0.3693(5) 0.030(2) Uani 1 1 d . . . H52 H 0.3693 0.0192 -0.3441 0.036 Uiso 1 1 calc R . . C53 C 0.3873(7) -0.0260(6) -0.4444(4) 0.0288(19) Uani 1 1 d . A . C54 C 0.4729(7) -0.0626(7) -0.2505(4) 0.031(2) Uani 1 1 d . . . C55 C 0.2060(8) 0.6028(7) -0.3577(5) 0.038(2) Uani 1 1 d . . . H55 H 0.1642 0.6315 -0.3327 0.045 Uiso 1 1 calc R . . C56 C 0.3519(10) 0.6092(11) -0.3974(9) 0.074(4) Uani 1 1 d . . . H56A H 0.4066 0.6517 -0.3930 0.111 Uiso 1 1 calc R . . H56B H 0.3230 0.5944 -0.4481 0.111 Uiso 1 1 calc R . . H56C H 0.3713 0.5559 -0.3771 0.111 Uiso 1 1 calc R . . C57 C 0.3059(12) 0.7392(9) -0.3276(7) 0.067(4) Uani 1 1 d . . . H57A H 0.3681 0.7611 -0.3341 0.100 Uiso 1 1 calc R . . H57B H 0.3043 0.7435 -0.2763 0.100 Uiso 1 1 calc R . . H57C H 0.2592 0.7745 -0.3515 0.100 Uiso 1 1 calc R . . C58 C 0.3996(11) 0.4214(10) 0.1048(8) 0.064(3) Uiso 1 1 d . . . H58A H 0.3726 0.3966 0.1427 0.096 Uiso 1 1 calc R . . H58B H 0.3675 0.4724 0.0907 0.096 Uiso 1 1 calc R . . H58C H 0.4662 0.4395 0.1227 0.096 Uiso 1 1 calc R . . C59 C 0.3427(14) 0.2699(12) 0.0473(10) 0.087(5) Uiso 1 1 d . . . H59A H 0.3243 0.2697 0.0940 0.131 Uiso 1 1 calc R . . H59B H 0.3856 0.2248 0.0419 0.131 Uiso 1 1 calc R . . H59C H 0.2871 0.2574 0.0091 0.131 Uiso 1 1 calc R . . C60 C 0.4175(9) 0.3723(9) -0.0150(7) 0.054(3) Uiso 1 1 d . . . H60 H 0.4468 0.4296 -0.0150 0.064 Uiso 1 1 calc R . . C61 C -0.3537(12) -0.3308(12) -0.3968(9) 0.080(4) Uiso 1 1 d . . . H61A H -0.3801 -0.2918 -0.3637 0.120 Uiso 1 1 calc R . . H61B H -0.4039 -0.3705 -0.4275 0.120 Uiso 1 1 calc R . . H61C H -0.3214 -0.2956 -0.4266 0.120 Uiso 1 1 calc R . . C62 C -0.2700(14) -0.3655(13) -0.2771(10) 0.094(5) Uiso 1 1 d . . . H62A H -0.3100 -0.3216 -0.2624 0.140 Uiso 1 1 calc R . . H62B H -0.2043 -0.3437 -0.2591 0.140 Uiso 1 1 calc R . . H62C H -0.2840 -0.4203 -0.2572 0.140 Uiso 1 1 calc R . . C63 C -0.2414(9) -0.4391(8) -0.3896(6) 0.049(3) Uiso 1 1 d . . . H63 H -0.1972 -0.4688 -0.3602 0.058 Uiso 1 1 calc R . . C64 C 0.0760(13) -0.0709(12) -0.5417(9) 0.080(4) Uiso 1 1 d . . . H64A H 0.0666 -0.0147 -0.5163 0.120 Uiso 1 1 calc R . . H64B H 0.0162 -0.0981 -0.5700 0.120 Uiso 1 1 calc R . . H64C H 0.1202 -0.0608 -0.5735 0.120 Uiso 1 1 calc R . . C65 C 0.1202(12) -0.0992(11) -0.4146(8) 0.073(4) Uiso 1 1 d . . . H65A H 0.1030 -0.0388 -0.4096 0.109 Uiso 1 1 calc R . . H65B H 0.1844 -0.1010 -0.3890 0.109 Uiso 1 1 calc R . . H65C H 0.0776 -0.1374 -0.3943 0.109 Uiso 1 1 calc R . . C66 C 0.1334(11) -0.2077(10) -0.5108(8) 0.068(4) Uiso 1 1 d . . . H66 H 0.1279 -0.2232 -0.5609 0.082 Uiso 1 1 calc R . . C67 C -0.3133(14) 0.3255(13) -0.4106(10) 0.091(5) Uiso 1 1 d . . . H67A H -0.3380 0.3148 -0.4623 0.137 Uiso 1 1 calc R . . H67B H -0.3105 0.2693 -0.3905 0.137 Uiso 1 1 calc R . . H67C H -0.2504 0.3563 -0.4021 0.137 Uiso 1 1 calc R . . C68 C -0.4524(12) 0.4022(12) -0.4262(9) 0.078(4) Uiso 1 1 d . . . H68A H -0.4496 0.3769 -0.4748 0.117 Uiso 1 1 calc R . . H68B H -0.4503 0.4663 -0.4243 0.117 Uiso 1 1 calc R . . H68C H -0.5106 0.3791 -0.4133 0.117 Uiso 1 1 calc R . . C69 C -0.3544(12) 0.4008(11) -0.3085(9) 0.072(4) Uiso 1 1 d . . . H69 H -0.3969 0.4346 -0.2884 0.087 Uiso 1 1 calc R . . N1 N 0.1495(5) -0.0662(4) -0.1853(4) 0.0223(14) Uani 1 1 d . . . N2 N 0.0729(5) -0.1180(5) -0.0867(4) 0.0218(14) Uani 1 1 d . . . N3 N -0.0983(5) 0.6206(5) 0.0658(3) 0.0225(14) Uani 1 1 d . . . N4 N -0.2319(5) 0.5612(5) 0.1195(4) 0.0246(15) Uani 1 1 d . . . N5 N 0.3527(6) -0.0642(5) -0.5987(4) 0.0287(16) Uani 1 1 d . . . N6 N 0.2380(6) 0.0259(6) -0.6683(4) 0.0346(19) Uani 1 1 d . . . N7 N 0.2849(7) 0.6470(6) -0.3589(5) 0.041(2) Uani 1 1 d . . . N8 N -0.3741(8) 0.3790(9) -0.3764(7) 0.069(3) Uani 1 1 d . . . N9 N 0.3886(7) 0.3548(7) 0.0424(5) 0.050(2) Uiso 1 1 d . . . N10 N -0.2877(8) -0.3819(7) -0.3562(6) 0.054(2) Uiso 1 1 d . . . N11 N 0.1135(8) -0.1291(8) -0.4895(6) 0.058(3) Uiso 1 1 d . . . O1 O -0.0757(4) -0.0249(4) -0.1310(3) 0.0248(12) Uani 1 1 d . . . O2 O 0.0111(4) 0.0405(4) -0.2179(3) 0.0240(12) Uani 1 1 d . . . O3 O -0.2857(5) 0.4397(4) 0.0055(3) 0.0282(13) Uani 1 1 d . . . O4 O -0.1678(5) 0.5125(4) -0.0579(3) 0.0289(14) Uani 1 1 d . . . O5 O 0.3312(5) 0.0270(5) -0.4765(3) 0.0371(17) Uani 1 1 d . . . O6 O 0.2271(5) 0.1202(5) -0.5433(3) 0.0422(19) Uani 1 1 d . . . O7 O -0.0007(5) 0.3109(4) -0.3501(4) 0.0321(15) Uani 1 1 d . . . O8 O 0.1478(4) 0.3524(4) -0.3423(3) 0.0284(13) Uani 1 1 d . . . O9 O -0.0604(5) 0.4758(5) -0.2948(3) 0.0328(14) Uani 1 1 d . . . O10 O 0.0885(5) 0.5211(4) -0.2652(3) 0.0310(15) Uani 1 1 d . . . O11 O -0.4374(6) 0.1086(4) 0.0895(4) 0.0381(17) Uani 1 1 d . . . O12 O -0.4678(5) 0.1426(4) -0.0223(3) 0.0344(16) Uani 1 1 d . . . O13 O 0.0651(5) 0.3812(4) -0.4830(3) 0.0296(14) Uani 1 1 d . . . O14 O 0.4174(5) -0.0135(4) -0.2227(3) 0.0284(14) Uani 1 1 d . . . O15 O 0.5335(6) -0.0966(7) -0.2131(4) 0.057(2) Uani 1 1 d . . . O16 O 0.1797(4) 0.5251(4) -0.3867(3) 0.0285(13) Uani 1 1 d . . . O17 O 0.0003(5) 0.5816(4) -0.4111(3) 0.0280(14) Uani 1 1 d . . . O18 O -0.1123(4) 0.4208(4) -0.4517(3) 0.0305(14) Uani 1 1 d . . . O19 O -0.5960(5) 0.1488(4) -0.1500(3) 0.0323(15) Uani 1 1 d . . . O20 O -0.6463(4) 0.0415(5) -0.0574(4) 0.0349(16) Uani 1 1 d . . . O21 O -0.4131(5) 0.1025(4) -0.1650(3) 0.0344(15) Uani 1 1 d . . . O22 O -0.3815(4) -0.0119(5) -0.0548(3) 0.0367(17) Uani 1 1 d . . . O23 O 0.3895(5) 0.2060(5) -0.4100(4) 0.0438(17) Uiso 1 1 d . . . O24 O -0.3047(15) -0.1765(14) -0.2044(11) 0.155(7) Uiso 1 1 d . . . O25 O -0.2506(7) -0.4566(6) -0.4540(5) 0.061(2) Uiso 1 1 d . . . O26 O 0.1588(8) -0.2636(7) -0.4708(6) 0.077(3) Uiso 1 1 d . . . O27 O 0.4099(7) 0.3191(6) -0.0714(5) 0.058(2) Uiso 1 1 d . . . O28 O -0.2857(7) 0.3823(7) -0.2665(5) 0.067(2) Uiso 1 1 d . . . O29 O -0.4965(7) 0.3622(6) -0.1763(5) 0.064(2) Uiso 1 1 d . . . O30 O -0.3052(6) 0.3568(6) -0.1323(5) 0.056(2) Uiso 1 1 d . . . O31 O -0.2502(6) 0.1935(5) -0.0958(4) 0.0491(19) Uiso 1 1 d . . . O32 O -0.0927(5) 0.1724(5) -0.1522(4) 0.0367(15) Uiso 1 1 d . . . O33 O -0.1365(6) 0.2790(6) -0.2624(4) 0.0507(19) Uiso 1 1 d . . . O34 O 0.4241(8) 0.4644(7) -0.2839(6) 0.074(3) Uiso 1 1 d . . . O35 O 0.3012(6) 0.3644(5) -0.4142(4) 0.0457(18) Uiso 1 1 d . . . O36 O 0.4773(6) 0.2047(5) -0.2658(4) 0.0470(18) Uiso 1 1 d . . . Ni1 Ni 0.03929(7) -0.04310(7) -0.15553(5) 0.0194(2) Uani 1 1 d . . . Ni2 Ni -0.19584(8) 0.53437(7) 0.03301(5) 0.0218(2) Uani 1 1 d . . . Ni3 Ni 0.28762(9) 0.02669(7) -0.57221(6) 0.0271(3) Uani 1 1 d . A . Lu1 Lu -0.51763(2) 0.02883(2) -0.107059(16) 0.01764(9) Uani 1 1 d . . . Lu2 Lu 0.03675(2) 0.45191(2) -0.382766(17) 0.01927(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(4) 0.020(4) 0.019(4) -0.001(3) 0.008(3) -0.001(3) C2 0.017(4) 0.026(4) 0.020(4) 0.008(3) -0.002(3) 0.007(4) C3 0.015(4) 0.028(4) 0.027(4) 0.002(3) 0.003(3) 0.001(4) C4 0.026(4) 0.030(4) 0.021(4) 0.005(3) 0.007(3) 0.008(4) C5 0.021(4) 0.025(4) 0.025(4) 0.010(3) 0.000(3) 0.005(4) C6 0.024(4) 0.023(4) 0.019(4) 0.002(3) 0.009(3) 0.003(4) C7 0.024(4) 0.020(4) 0.018(3) 0.007(3) 0.003(3) 0.004(3) C8 0.018(4) 0.025(4) 0.040(5) 0.012(4) 0.010(4) 0.009(4) C9 0.026(5) 0.028(4) 0.035(5) 0.010(4) 0.015(4) 0.015(4) C10 0.031(5) 0.021(4) 0.029(4) 0.003(3) 0.013(4) 0.007(4) C11 0.032(5) 0.022(4) 0.027(4) 0.003(3) 0.013(4) 0.012(4) C12 0.020(4) 0.014(3) 0.024(4) -0.003(3) 0.007(3) 0.002(3) C13 0.023(4) 0.023(4) 0.018(3) 0.001(3) 0.007(3) 0.008(4) C14 0.032(5) 0.021(4) 0.020(4) 0.004(3) 0.007(3) 0.004(4) C15 0.026(5) 0.032(5) 0.036(5) 0.008(4) 0.015(4) 0.005(4) C16 0.024(4) 0.026(4) 0.031(4) 0.006(3) 0.016(4) 0.002(4) C17 0.022(4) 0.031(4) 0.026(4) 0.009(4) 0.010(3) 0.002(4) C18 0.031(5) 0.020(4) 0.035(5) 0.009(4) 0.012(4) 0.005(4) C19 0.033(5) 0.024(4) 0.025(4) 0.011(3) 0.015(4) 0.007(4) C20 0.034(5) 0.025(4) 0.032(4) 0.001(4) 0.014(4) -0.005(4) C21 0.034(5) 0.022(4) 0.029(4) -0.001(3) 0.015(4) -0.004(4) C22 0.032(5) 0.018(4) 0.023(4) 0.005(3) 0.009(3) 0.001(4) C23 0.037(5) 0.016(4) 0.024(4) 0.001(3) 0.009(4) 0.005(4) C24 0.029(5) 0.028(4) 0.013(3) 0.003(3) 0.003(3) 0.001(4) C25 0.034(5) 0.015(4) 0.027(4) -0.003(3) 0.006(4) -0.006(4) C26 0.032(5) 0.026(4) 0.023(4) -0.004(3) 0.010(4) -0.007(4) C27 0.045(6) 0.026(4) 0.026(4) -0.006(3) 0.020(4) -0.006(4) C28 0.027(4) 0.029(4) 0.018(4) -0.004(3) 0.014(3) 0.000(4) C29 0.022(4) 0.021(4) 0.022(4) -0.001(3) 0.008(3) -0.007(4) C30 0.024(4) 0.018(4) 0.020(4) 0.001(3) 0.009(3) 0.000(3) C31 0.027(4) 0.025(4) 0.021(4) 0.007(3) 0.009(3) -0.001(4) C32 0.022(4) 0.022(4) 0.022(4) 0.005(3) 0.003(3) 0.003(4) C33 0.037(5) 0.030(4) 0.021(4) 0.008(3) 0.012(4) -0.002(4) C34 0.034(5) 0.025(4) 0.021(4) -0.005(3) 0.012(4) -0.007(4) C35 0.014(4) 0.027(4) 0.024(4) 0.001(3) 0.003(3) 0.006(4) C36 0.030(5) 0.021(4) 0.026(4) 0.000(3) 0.003(4) -0.002(4) C37 0.022(4) 0.021(4) 0.027(4) 0.005(3) 0.007(3) 0.001(4) C38 0.033(5) 0.025(4) 0.014(3) 0.004(3) 0.004(3) 0.011(4) C39 0.037(5) 0.026(4) 0.019(4) 0.000(3) 0.005(3) 0.012(4) C40 0.039(5) 0.027(4) 0.021(4) -0.006(3) 0.002(4) 0.007(4) C41 0.039(6) 0.029(5) 0.024(4) 0.003(4) -0.004(4) 0.009(4) C42 0.039(6) 0.042(5) 0.024(4) -0.003(4) -0.003(4) 0.021(5) C43 0.032(5) 0.030(5) 0.026(4) 0.001(4) 0.002(4) 0.006(4) C44 0.044(6) 0.033(5) 0.025(4) -0.014(4) -0.002(4) 0.015(5) C47 0.038(5) 0.035(5) 0.019(4) -0.004(3) 0.011(4) 0.014(4) C48 0.033(5) 0.025(4) 0.027(4) -0.002(3) 0.016(4) 0.011(4) C49 0.029(5) 0.030(4) 0.026(4) 0.000(4) 0.012(4) 0.013(4) C50 0.027(5) 0.031(5) 0.032(5) 0.005(4) 0.006(4) 0.010(4) C51 0.025(5) 0.034(5) 0.021(4) 0.001(4) 0.008(3) -0.002(4) C52 0.036(5) 0.031(5) 0.025(4) -0.001(4) 0.011(4) 0.014(4) C53 0.039(5) 0.029(4) 0.021(4) 0.002(3) 0.010(4) 0.010(4) C54 0.029(5) 0.045(5) 0.018(4) 0.000(4) 0.005(3) 0.001(5) C55 0.043(6) 0.038(5) 0.037(5) 0.008(4) 0.013(4) 0.011(5) C56 0.049(8) 0.084(11) 0.096(11) 0.012(9) 0.036(8) -0.006(8) C57 0.091(11) 0.046(7) 0.054(7) 0.002(6) 0.001(7) -0.022(8) N1 0.018(3) 0.020(3) 0.029(3) 0.005(3) 0.003(3) 0.002(3) N2 0.014(3) 0.022(3) 0.031(4) 0.005(3) 0.005(3) 0.005(3) N3 0.029(4) 0.021(3) 0.018(3) 0.004(3) 0.006(3) 0.002(3) N4 0.030(4) 0.019(3) 0.023(3) -0.003(3) 0.006(3) -0.001(3) N5 0.032(4) 0.028(4) 0.029(4) 0.004(3) 0.010(3) 0.010(4) N6 0.039(5) 0.039(4) 0.023(4) -0.008(3) 0.001(3) 0.019(4) N7 0.042(5) 0.037(5) 0.039(5) 0.003(4) 0.006(4) -0.015(4) N8 0.045(6) 0.094(9) 0.069(7) 0.026(7) 0.005(5) 0.004(7) O1 0.023(3) 0.029(3) 0.025(3) 0.010(2) 0.006(2) 0.005(3) O2 0.023(3) 0.025(3) 0.029(3) 0.012(2) 0.012(2) 0.008(3) O3 0.038(4) 0.023(3) 0.023(3) -0.001(2) 0.009(3) -0.005(3) O4 0.030(3) 0.033(3) 0.024(3) -0.002(3) 0.013(3) -0.009(3) O5 0.058(5) 0.038(4) 0.019(3) 0.004(3) 0.006(3) 0.030(4) O6 0.057(5) 0.045(4) 0.024(3) -0.004(3) -0.001(3) 0.036(4) O7 0.030(4) 0.033(3) 0.041(4) 0.017(3) 0.016(3) 0.011(3) O8 0.028(3) 0.024(3) 0.034(3) 0.009(3) 0.004(3) -0.001(3) O9 0.031(4) 0.042(4) 0.023(3) -0.005(3) 0.009(3) -0.008(3) O10 0.033(4) 0.038(4) 0.022(3) -0.002(3) 0.008(3) 0.005(3) O11 0.060(5) 0.020(3) 0.034(3) 0.007(3) 0.016(3) -0.012(3) O12 0.052(4) 0.016(3) 0.027(3) -0.004(2) -0.007(3) -0.002(3) O13 0.041(4) 0.035(3) 0.014(3) -0.003(2) 0.007(2) 0.015(3) O14 0.035(4) 0.033(3) 0.016(3) -0.004(2) 0.008(3) -0.004(3) O15 0.046(5) 0.100(7) 0.033(4) 0.029(4) 0.009(3) 0.040(5) O16 0.023(3) 0.026(3) 0.039(3) 0.004(3) 0.015(3) -0.002(3) O17 0.036(4) 0.020(3) 0.029(3) 0.008(2) 0.004(3) 0.010(3) O18 0.026(3) 0.032(3) 0.030(3) -0.002(3) 0.000(3) 0.002(3) O19 0.034(4) 0.037(4) 0.028(3) 0.007(3) 0.006(3) 0.014(3) O20 0.018(3) 0.056(4) 0.039(4) 0.015(3) 0.020(3) 0.007(3) O21 0.038(4) 0.037(4) 0.035(3) 0.012(3) 0.020(3) 0.002(3) O22 0.021(3) 0.058(5) 0.033(3) 0.011(3) 0.000(3) 0.020(3) Ni1 0.0189(5) 0.0188(5) 0.0227(5) 0.0063(4) 0.0064(4) 0.0051(4) Ni2 0.0288(6) 0.0197(5) 0.0164(5) -0.0020(4) 0.0075(4) -0.0043(5) Ni3 0.0360(7) 0.0268(6) 0.0181(5) -0.0023(4) 0.0023(4) 0.0147(5) Lu1 0.01934(18) 0.01974(17) 0.01465(15) 0.00293(13) 0.00496(13) 0.00171(15) Lu2 0.0243(2) 0.01787(17) 0.01751(16) 0.00436(13) 0.00652(13) 0.00496(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.309(9) . ? C1 C6 1.412(11) . ? C1 C2 1.418(11) . ? C2 C3 1.377(11) . ? C3 C4 1.405(11) . ? C3 C36 1.521(12) 2_455 ? C4 C5 1.378(11) . ? C5 C6 1.425(11) . ? C6 C7 1.457(11) . ? C7 N2 1.285(10) . ? C8 N2 1.480(10) . ? C8 C9 1.517(12) . ? C9 N1 1.487(10) . ? C10 N1 1.287(11) . ? C10 C11 1.454(11) . ? C11 C15 1.407(12) . ? C11 C12 1.416(11) . ? C12 O2 1.322(10) . ? C12 C13 1.432(11) . ? C13 C14 1.377(12) . ? C14 C16 1.406(12) . ? C14 C17 1.492(11) . ? C15 C16 1.376(12) . ? C17 O8 1.257(11) . ? C17 O7 1.285(10) . ? C17 Lu2 2.757(8) . ? C18 O9 1.249(12) . ? C18 O10 1.281(11) . ? C18 C19 1.492(12) . ? C18 Lu2 2.749(9) . ? C19 C20 1.391(14) . ? C19 C24 1.405(12) . ? C20 C21 1.382(12) . ? C21 C22 1.426(12) . ? C22 C23 1.413(13) . ? C22 C25 1.432(12) . ? C23 O4 1.313(11) . ? C23 C24 1.407(11) . ? C25 N3 1.287(12) . ? C26 N3 1.500(10) . ? C26 C27 1.516(13) . ? C27 N4 1.480(11) . ? C28 N4 1.297(11) . ? C28 C29 1.423(12) . ? C29 C30 1.402(11) . ? C29 C34 1.424(11) . ? C30 O3 1.336(9) . ? C30 C31 1.418(12) . ? C31 C32 1.378(11) . ? C32 C33 1.402(12) . ? C32 C35 1.534(12) . ? C33 C34 1.352(13) . ? C35 O12 1.240(10) . ? C35 O11 1.248(10) . ? C36 O22 1.233(10) 2_455 ? C36 O20 1.246(10) . ? C36 C3 1.521(12) 2_455 ? C37 O17 1.255(9) 2_564 ? C37 O13 1.257(10) . ? C37 C38 1.519(11) . ? C38 C39 1.374(11) . ? C38 C41 1.407(11) . ? C39 C40 1.418(11) . ? C40 O6 1.305(10) . ? C40 C43 1.407(12) . ? C41 C42 1.357(13) . ? C42 C43 1.409(12) . ? C43 C44 1.450(12) . ? C44 N6 1.282(12) . ? C45A C46A 1.38(2) . ? C45A N6 1.529(17) . ? C46A N5 1.476(19) . ? C45B C46B 1.35(3) . ? C45B N6 1.51(2) . ? C46B N5 1.51(2) . ? C47 N5 1.290(11) . ? C47 C48 1.425(12) . ? C48 C53 1.414(11) . ? C48 C49 1.434(12) . ? C49 C50 1.376(12) . ? C50 C51 1.405(12) . ? C51 C52 1.377(12) . ? C51 C54 1.506(11) . ? C52 C53 1.404(12) . ? C53 O5 1.316(10) . ? C54 O15 1.216(11) . ? C54 O14 1.298(11) . ? C54 Lu1 2.928(9) 1_655 ? C55 O16 1.266(12) . ? C55 N7 1.299(14) . ? C56 N7 1.452(17) . ? C57 N7 1.470(15) . ? C58 N9 1.469(17) . ? C59 N9 1.44(2) . ? C60 O27 1.269(15) . ? C60 N9 1.291(16) . ? C61 N10 1.452(18) . ? C62 N10 1.48(2) . ? C63 O25 1.214(14) . ? C63 N10 1.334(15) . ? C64 N11 1.465(18) . ? C65 N11 1.442(18) . ? C66 O26 1.238(16) . ? C66 N11 1.307(18) . ? C67 N8 1.45(2) . ? C68 N8 1.440(18) . ? C69 O28 1.237(17) . ? C69 N8 1.280(19) . ? N1 Ni1 1.854(7) . ? N2 Ni1 1.856(6) . ? N3 Ni2 1.845(8) . ? N4 Ni2 1.843(7) . ? N5 Ni3 1.833(7) . ? N6 Ni3 1.843(7) . ? O1 Ni1 1.862(6) . ? O2 Ni1 1.856(5) . ? O3 Ni2 1.851(7) . ? O4 Ni2 1.861(6) . ? O5 Ni3 1.820(6) . ? O6 Ni3 1.837(6) . ? O7 Lu2 2.366(6) . ? O8 Lu2 2.394(6) . ? O9 Lu2 2.412(6) . ? O10 Lu2 2.351(6) . ? O11 Lu1 2.240(6) 2_455 ? O12 Lu1 2.242(6) . ? O13 Lu2 2.229(5) . ? O14 Lu1 2.249(6) 1_655 ? O16 Lu2 2.316(6) . ? O17 C37 1.255(9) 2_564 ? O17 Lu2 2.196(5) . ? O18 Lu2 2.319(6) . ? O19 Lu1 2.380(6) . ? O20 Lu1 2.272(6) . ? O21 Lu1 2.336(6) . ? O22 C36 1.233(10) 2_455 ? O22 Lu1 2.223(6) . ? Lu1 O11 2.240(6) 2_455 ? Lu1 O14 2.249(6) 1_455 ? Lu1 C54 2.928(9) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 123.8(7) . . ? O1 C1 C2 118.6(7) . . ? C6 C1 C2 117.6(7) . . ? C3 C2 C1 121.1(7) . . ? C2 C3 C4 121.4(7) . . ? C2 C3 C36 119.5(7) . 2_455 ? C4 C3 C36 119.1(7) . 2_455 ? C5 C4 C3 118.8(7) . . ? C4 C5 C6 120.9(7) . . ? C1 C6 C5 120.1(7) . . ? C1 C6 C7 122.5(7) . . ? C5 C6 C7 117.4(7) . . ? N2 C7 C6 123.8(7) . . ? N2 C8 C9 106.3(6) . . ? N1 C9 C8 105.7(6) . . ? N1 C10 C11 122.8(8) . . ? C15 C11 C12 120.7(7) . . ? C15 C11 C10 117.6(8) . . ? C12 C11 C10 121.7(8) . . ? O2 C12 C11 124.7(7) . . ? O2 C12 C13 118.7(7) . . ? C11 C12 C13 116.6(7) . . ? C14 C13 C12 121.1(7) . . ? C13 C14 C16 121.6(7) . . ? C13 C14 C17 119.9(7) . . ? C16 C14 C17 118.4(8) . . ? C16 C15 C11 121.8(8) . . ? C15 C16 C14 118.1(8) . . ? O8 C17 O7 119.1(8) . . ? O8 C17 C14 120.7(8) . . ? O7 C17 C14 120.1(8) . . ? O8 C17 Lu2 60.2(4) . . ? O7 C17 Lu2 59.0(4) . . ? C14 C17 Lu2 179.1(6) . . ? O9 C18 O10 119.8(8) . . ? O9 C18 C19 121.8(8) . . ? O10 C18 C19 118.3(9) . . ? O9 C18 Lu2 61.3(5) . . ? O10 C18 Lu2 58.6(4) . . ? C19 C18 Lu2 176.9(7) . . ? C20 C19 C24 120.4(8) . . ? C20 C19 C18 120.1(8) . . ? C24 C19 C18 119.4(8) . . ? C21 C20 C19 120.0(8) . . ? C20 C21 C22 120.3(9) . . ? C23 C22 C21 120.1(8) . . ? C23 C22 C25 122.0(8) . . ? C21 C22 C25 117.9(8) . . ? O4 C23 C24 118.0(8) . . ? O4 C23 C22 123.7(7) . . ? C24 C23 C22 118.2(8) . . ? C19 C24 C23 120.9(8) . . ? N3 C25 C22 124.8(9) . . ? N3 C26 C27 106.0(7) . . ? N4 C27 C26 105.7(7) . . ? N4 C28 C29 122.8(7) . . ? C30 C29 C28 122.3(7) . . ? C30 C29 C34 119.4(8) . . ? C28 C29 C34 118.4(7) . . ? O3 C30 C29 123.3(7) . . ? O3 C30 C31 118.0(7) . . ? C29 C30 C31 118.7(7) . . ? C32 C31 C30 119.7(7) . . ? C31 C32 C33 121.7(8) . . ? C31 C32 C35 118.8(7) . . ? C33 C32 C35 119.5(7) . . ? C34 C33 C32 119.0(8) . . ? C33 C34 C29 121.4(8) . . ? O12 C35 O11 126.5(8) . . ? O12 C35 C32 118.0(7) . . ? O11 C35 C32 115.5(7) . . ? O22 C36 O20 125.8(8) 2_455 . ? O22 C36 C3 117.0(8) 2_455 2_455 ? O20 C36 C3 117.3(7) . 2_455 ? O17 C37 O13 124.3(8) 2_564 . ? O17 C37 C38 116.8(7) 2_564 . ? O13 C37 C38 118.9(7) . . ? C39 C38 C41 120.3(7) . . ? C39 C38 C37 118.7(7) . . ? C41 C38 C37 120.8(7) . . ? C38 C39 C40 121.2(8) . . ? O6 C40 C43 123.6(8) . . ? O6 C40 C39 118.5(7) . . ? C43 C40 C39 117.9(8) . . ? C42 C41 C38 119.2(8) . . ? C41 C42 C43 121.8(8) . . ? C40 C43 C42 119.5(8) . . ? C40 C43 C44 122.2(8) . . ? C42 C43 C44 118.2(8) . . ? N6 C44 C43 123.2(8) . . ? C46A C45A N6 109.8(13) . . ? C45A C46A N5 114.6(13) . . ? C46B C45B N6 113.0(16) . . ? C45B C46B N5 112.7(15) . . ? N5 C47 C48 124.0(7) . . ? C53 C48 C47 121.6(8) . . ? C53 C48 C49 118.0(8) . . ? C47 C48 C49 120.4(7) . . ? C50 C49 C48 121.9(7) . . ? C49 C50 C51 119.0(8) . . ? C52 C51 C50 120.2(8) . . ? C52 C51 C54 118.8(8) . . ? C50 C51 C54 120.9(8) . . ? C51 C52 C53 121.9(8) . . ? O5 C53 C52 117.9(7) . . ? O5 C53 C48 123.3(7) . . ? C52 C53 C48 118.8(8) . . ? O15 C54 O14 121.5(8) . . ? O15 C54 C51 122.0(8) . . ? O14 C54 C51 116.4(8) . . ? O15 C54 Lu1 76.5(6) . 1_655 ? O14 C54 Lu1 46.8(4) . 1_655 ? C51 C54 Lu1 157.0(7) . 1_655 ? O16 C55 N7 126.0(9) . . ? O27 C60 N9 125.2(13) . . ? O25 C63 N10 125.9(12) . . ? O26 C66 N11 125.2(15) . . ? O28 C69 N8 126.5(16) . . ? C10 N1 C9 119.6(7) . . ? C10 N1 Ni1 127.8(6) . . ? C9 N1 Ni1 112.6(5) . . ? C7 N2 C8 117.5(6) . . ? C7 N2 Ni1 126.8(5) . . ? C8 N2 Ni1 114.7(5) . . ? C25 N3 C26 118.5(8) . . ? C25 N3 Ni2 126.5(6) . . ? C26 N3 Ni2 114.3(5) . . ? C28 N4 C27 119.8(7) . . ? C28 N4 Ni2 128.0(6) . . ? C27 N4 Ni2 112.2(5) . . ? C47 N5 C46A 117.6(9) . . ? C47 N5 C46B 118.6(9) . . ? C46A N5 C46B 21.1(9) . . ? C47 N5 Ni3 127.9(6) . . ? C46A N5 Ni3 113.2(8) . . ? C46B N5 Ni3 112.7(8) . . ? C44 N6 C45B 118.3(10) . . ? C44 N6 C45A 117.7(9) . . ? C45B N6 C45A 30.0(9) . . ? C44 N6 Ni3 128.3(6) . . ? C45B N6 Ni3 111.3(8) . . ? C45A N6 Ni3 112.4(7) . . ? C55 N7 C56 120.7(10) . . ? C55 N7 C57 121.6(11) . . ? C56 N7 C57 117.5(11) . . ? C69 N8 C68 127.1(14) . . ? C69 N8 C67 119.7(13) . . ? C68 N8 C67 113.2(14) . . ? C60 N9 C59 121.3(13) . . ? C60 N9 C58 121.1(12) . . ? C59 N9 C58 117.5(12) . . ? C63 N10 C61 120.7(12) . . ? C63 N10 C62 121.0(12) . . ? C61 N10 C62 118.2(13) . . ? C66 N11 C65 121.7(12) . . ? C66 N11 C64 120.7(13) . . ? C65 N11 C64 117.4(12) . . ? C1 O1 Ni1 127.0(5) . . ? C12 O2 Ni1 124.8(5) . . ? C30 O3 Ni2 124.2(5) . . ? C23 O4 Ni2 126.7(6) . . ? C53 O5 Ni3 128.2(5) . . ? C40 O6 Ni3 128.0(6) . . ? C17 O7 Lu2 93.3(5) . . ? C17 O8 Lu2 92.7(5) . . ? C18 O9 Lu2 91.7(5) . . ? C18 O10 Lu2 93.7(6) . . ? C35 O11 Lu1 143.7(6) . 2_455 ? C35 O12 Lu1 142.0(6) . . ? C37 O13 Lu2 146.7(5) . . ? C54 O14 Lu1 108.2(5) . 1_655 ? C55 O16 Lu2 123.6(6) . . ? C37 O17 Lu2 153.5(6) 2_564 . ? C36 O20 Lu1 137.7(6) . . ? C36 O22 Lu1 149.8(6) 2_455 . ? N1 Ni1 N2 85.8(3) . . ? N1 Ni1 O2 94.6(3) . . ? N2 Ni1 O2 174.6(3) . . ? N1 Ni1 O1 176.1(3) . . ? N2 Ni1 O1 95.2(3) . . ? O2 Ni1 O1 84.9(2) . . ? N4 Ni2 N3 86.2(3) . . ? N4 Ni2 O3 93.1(3) . . ? N3 Ni2 O3 173.8(3) . . ? N4 Ni2 O4 175.0(3) . . ? N3 Ni2 O4 94.9(3) . . ? O3 Ni2 O4 86.2(3) . . ? O5 Ni3 N5 94.6(3) . . ? O5 Ni3 O6 83.9(3) . . ? N5 Ni3 O6 177.6(4) . . ? O5 Ni3 N6 177.4(4) . . ? N5 Ni3 N6 87.0(3) . . ? O6 Ni3 N6 94.6(3) . . ? O22 Lu1 O11 80.0(3) . 2_455 ? O22 Lu1 O12 79.1(3) . . ? O11 Lu1 O12 126.6(2) 2_455 . ? O22 Lu1 O14 123.1(2) . 1_455 ? O11 Lu1 O14 85.2(2) 2_455 1_455 ? O12 Lu1 O14 146.0(2) . 1_455 ? O22 Lu1 O20 126.6(2) . . ? O11 Lu1 O20 75.5(3) 2_455 . ? O12 Lu1 O20 78.9(3) . . ? O14 Lu1 O20 101.4(2) 1_455 . ? O22 Lu1 O21 78.0(2) . . ? O11 Lu1 O21 139.2(2) 2_455 . ? O12 Lu1 O21 81.9(3) . . ? O14 Lu1 O21 78.9(2) 1_455 . ? O20 Lu1 O21 144.2(2) . . ? O22 Lu1 O19 144.6(3) . . ? O11 Lu1 O19 135.0(3) 2_455 . ? O12 Lu1 O19 74.6(2) . . ? O14 Lu1 O19 73.5(2) 1_455 . ? O20 Lu1 O19 70.7(2) . . ? O21 Lu1 O19 75.3(2) . . ? O22 Lu1 C54 98.1(3) . 1_455 ? O11 Lu1 C54 79.5(3) 2_455 1_455 ? O12 Lu1 C54 151.9(3) . 1_455 ? O14 Lu1 C54 24.9(2) 1_455 1_455 ? O20 Lu1 C54 122.3(3) . 1_455 ? O21 Lu1 C54 70.3(3) . 1_455 ? O19 Lu1 C54 94.2(2) . 1_455 ? O17 Lu2 O13 105.3(2) . . ? O17 Lu2 O16 76.7(2) . . ? O13 Lu2 O16 80.3(2) . . ? O17 Lu2 O18 77.3(2) . . ? O13 Lu2 O18 78.1(2) . . ? O16 Lu2 O18 140.1(2) . . ? O17 Lu2 O10 86.2(2) . . ? O13 Lu2 O10 150.8(2) . . ? O16 Lu2 O10 76.4(2) . . ? O18 Lu2 O10 131.1(2) . . ? O17 Lu2 O7 152.4(2) . . ? O13 Lu2 O7 85.9(2) . . ? O16 Lu2 O7 130.7(2) . . ? O18 Lu2 O7 80.6(2) . . ? O10 Lu2 O7 96.1(2) . . ? O17 Lu2 O8 152.0(2) . . ? O13 Lu2 O8 75.3(2) . . ? O16 Lu2 O8 75.9(2) . . ? O18 Lu2 O8 128.9(2) . . ? O10 Lu2 O8 82.1(2) . . ? O7 Lu2 O8 54.8(2) . . ? O17 Lu2 O9 84.3(2) . . ? O13 Lu2 O9 151.3(3) . . ? O16 Lu2 O9 128.5(2) . . ? O18 Lu2 O9 77.8(2) . . ? O10 Lu2 O9 54.7(2) . . ? O7 Lu2 O9 75.0(2) . . ? O8 Lu2 O9 108.8(2) . . ? O17 Lu2 C18 85.0(2) . . ? O13 Lu2 C18 169.7(2) . . ? O16 Lu2 C18 103.0(3) . . ? O18 Lu2 C18 104.3(3) . . ? O10 Lu2 C18 27.7(3) . . ? O7 Lu2 C18 84.6(2) . . ? O8 Lu2 C18 95.9(2) . . ? O9 Lu2 C18 27.0(2) . . ? O17 Lu2 C17 175.3(2) . . ? O13 Lu2 C17 79.2(2) . . ? O16 Lu2 C17 103.0(2) . . ? O18 Lu2 C17 105.4(3) . . ? O10 Lu2 C17 89.1(2) . . ? O7 Lu2 C17 27.7(2) . . ? O8 Lu2 C17 27.1(2) . . ? O9 Lu2 C17 92.4(2) . . ? C18 Lu2 C17 90.5(2) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.556 _refine_diff_density_min -1.750 _refine_diff_density_rms 0.165 #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 794156' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Dy Ni N3 O10 S, C2 H10 O3 S' _chemical_formula_sum 'C22 H28 Dy N3 Ni O13 S2' _chemical_formula_weight 827.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.5226(15) _cell_length_b 22.668(5) _cell_length_c 17.349(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.88(3) _cell_angle_gamma 90.00 _cell_volume 2942.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 19806 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 27.13 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1644 _exptl_absorpt_coefficient_mu 3.369 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5533 _exptl_absorpt_correction_T_max 0.7515 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20559 _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.75 _reflns_number_total 6252 _reflns_number_gt 4665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0645P)^2^+7.7292P] 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 6252 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1323(12) 0.3592(3) -0.0498(5) 0.0428(18) Uani 1 1 d . A . C2 C -0.0984(11) 0.2993(3) -0.0299(5) 0.0426(18) Uani 1 1 d . . . H2 H -0.1211 0.2859 0.0200 0.051 Uiso 1 1 calc R . . C3 C -0.0334(11) 0.2598(4) -0.0809(5) 0.0431(18) Uani 1 1 d . . . C4 C -0.0007(12) 0.2789(4) -0.1561(5) 0.049(2) Uani 1 1 d . . . H4 H 0.0410 0.2523 -0.1925 0.059 Uiso 1 1 calc R . . C5 C -0.0316(13) 0.3373(4) -0.1743(5) 0.051(2) Uani 1 1 d . . . H5 H -0.0066 0.3507 -0.2240 0.061 Uiso 1 1 calc R . . C6 C -0.0969(11) 0.3778(4) -0.1245(5) 0.0432(18) Uani 1 1 d . . . C7 C -0.1218(12) 0.4373(4) -0.1497(5) 0.0461(19) Uani 1 1 d . A . H7 H -0.0998 0.4463 -0.2014 0.055 Uiso 1 1 calc R . . C8A C -0.157(2) 0.5422(7) -0.1349(9) 0.031(3) Uiso 0.50 1 d P A 1 H8A1 H -0.0310 0.5500 -0.1439 0.037 Uiso 0.50 1 calc PR A 1 H8A2 H -0.2310 0.5468 -0.1851 0.037 Uiso 0.50 1 calc PR A 1 C9A C -0.207(3) 0.5816(9) -0.0857(11) 0.055(4) Uiso 0.50 1 d P A 1 H9A1 H -0.3028 0.6063 -0.1125 0.066 Uiso 0.50 1 calc PR A 1 H9A2 H -0.1046 0.6077 -0.0695 0.066 Uiso 0.50 1 calc PR A 1 C8B C -0.218(3) 0.5377(8) -0.1492(11) 0.043(4) Uiso 0.50 1 d P A 2 H8B1 H -0.3028 0.5306 -0.1956 0.051 Uiso 0.50 1 calc PR A 2 H8B2 H -0.1082 0.5560 -0.1659 0.051 Uiso 0.50 1 calc PR A 2 C9B C -0.301(2) 0.5778(7) -0.0924(8) 0.035(3) Uiso 0.50 1 d P A 2 H9B1 H -0.2465 0.6176 -0.0937 0.043 Uiso 0.50 1 calc PR A 2 H9B2 H -0.4304 0.5817 -0.1084 0.043 Uiso 0.50 1 calc PR A 2 C10 C -0.3262(12) 0.5896(3) 0.0389(5) 0.0467(19) Uani 1 1 d . A . H10 H -0.3465 0.6299 0.0260 0.056 Uiso 1 1 calc R . . C11 C -0.3224(10) 0.5122(3) 0.1410(5) 0.0369(16) Uani 1 1 d . A . C12 C -0.3548(11) 0.5712(3) 0.1156(5) 0.0421(17) Uani 1 1 d . . . C13 C -0.4109(12) 0.6143(3) 0.1670(5) 0.0440(19) Uani 1 1 d . . . H13 H -0.4310 0.6537 0.1495 0.053 Uiso 1 1 calc R . . C14 C -0.4366(12) 0.5998(4) 0.2418(5) 0.0469(19) Uani 1 1 d . . . H14 H -0.4761 0.6289 0.2756 0.056 Uiso 1 1 calc R . . C15 C -0.4043(11) 0.5420(3) 0.2681(5) 0.0411(17) Uani 1 1 d . . . C16 C -0.3513(10) 0.4994(3) 0.2185(5) 0.0408(17) Uani 1 1 d . . . H16 H -0.3335 0.4602 0.2370 0.049 Uiso 1 1 calc R . . C17 C 0.0007(11) 0.1981(3) -0.0578(5) 0.0409(17) Uani 1 1 d . . . C18 C -0.4344(11) 0.5259(3) 0.3507(5) 0.0411(17) Uani 1 1 d . . . C19 C 0.6151(14) 0.1553(5) 0.1048(7) 0.073(3) Uani 1 1 d . . . H19A H 0.5995 0.1271 0.1464 0.109 Uiso 1 1 calc R . . H19B H 0.6738 0.1910 0.1269 0.109 Uiso 1 1 calc R . . H19C H 0.6891 0.1375 0.0677 0.109 Uiso 1 1 calc R . . C20 C 0.481(2) 0.2130(7) -0.0224(11) 0.117(6) Uani 1 1 d . . . H20A H 0.5834 0.1922 -0.0399 0.175 Uiso 1 1 calc R . . H20B H 0.5166 0.2529 -0.0057 0.175 Uiso 1 1 calc R . . H20C H 0.3849 0.2153 -0.0651 0.175 Uiso 1 1 calc R . . C21 C -0.109(3) -0.2699(11) -0.1884(13) 0.166(9) Uani 1 1 d . . . H21A H -0.0691 -0.2945 -0.1435 0.249 Uiso 1 1 calc R . . H21B H -0.2229 -0.2852 -0.2132 0.249 Uiso 1 1 calc R . . H21C H -0.1257 -0.2292 -0.1714 0.249 Uiso 1 1 calc R . . C22 C 0.046(2) -0.3480(7) -0.2709(11) 0.127(6) Uani 1 1 d . . . H22A H 0.1087 -0.3565 -0.3165 0.190 Uiso 1 1 calc R . . H22B H -0.0780 -0.3616 -0.2803 0.190 Uiso 1 1 calc R . . H22C H 0.1057 -0.3684 -0.2257 0.190 Uiso 1 1 calc R . . N1 N -0.2746(10) 0.5551(3) -0.0142(4) 0.0459(16) Uani 1 1 d . . . N2 N -0.1721(9) 0.4803(3) -0.1074(4) 0.0426(15) Uani 1 1 d . . . N3 N -0.2967(11) 0.0383(4) -0.0697(5) 0.063(2) Uani 1 1 d . . . O1 O -0.1892(9) 0.3944(2) 0.0027(3) 0.0500(15) Uani 1 1 d . . . O2 O -0.2740(8) 0.4701(2) 0.0969(3) 0.0416(12) Uani 1 1 d . . . O3 O -0.0265(8) 0.1807(2) 0.0095(3) 0.0450(13) Uani 1 1 d . . . O4 O 0.0648(8) 0.1624(2) -0.1048(3) 0.0459(13) Uani 1 1 d . . . O5 O -0.4164(7) 0.4729(2) 0.3711(3) 0.0416(12) Uani 1 1 d . . . O6 O -0.4728(9) 0.5682(2) 0.3935(3) 0.0485(14) Uani 1 1 d . . . O7 O -0.2552(8) 0.0912(2) -0.0795(4) 0.0522(15) Uani 1 1 d . . . O8 O -0.1920(7) 0.0056(2) -0.0255(3) 0.0406(12) Uani 1 1 d . . . O9 O -0.4670(14) 0.0116(5) -0.1118(7) 0.121(4) Uani 1 1 d . . . O10 O 0.3275(8) 0.1159(3) 0.0247(4) 0.0512(14) Uani 1 1 d . . . O11 O 0.2254(16) -0.2598(5) -0.2056(6) 0.116(4) Uani 1 1 d . . . O12 O 0.091(2) -0.1397(7) 0.2581(8) 0.163(5) Uani 1 1 d . . . O13 O 0.0911(14) 0.1697(5) -0.3967(7) 0.116(4) Uani 1 1 d . . . S1 S 0.4027(3) 0.17417(12) 0.05658(19) 0.0666(7) Uani 1 1 d . . . S2 S 0.0489(7) -0.27144(17) -0.2537(2) 0.1072(13) Uani 1 1 d . . . Ni1 Ni -0.22823(14) 0.47541(4) -0.00592(6) 0.0366(2) Uani 1 1 d . A . Dy1 Dy 0.04809(5) 0.080680(15) -0.01760(2) 0.03726(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(5) 0.029(4) 0.042(4) 0.003(3) 0.013(4) 0.002(4) C2 0.055(5) 0.032(4) 0.041(4) 0.003(3) 0.011(4) 0.004(4) C3 0.050(4) 0.034(4) 0.046(4) -0.003(3) 0.009(3) -0.001(4) C4 0.067(5) 0.031(4) 0.054(5) -0.004(3) 0.018(4) 0.002(4) C5 0.075(6) 0.034(4) 0.049(5) 0.004(3) 0.026(4) 0.001(4) C6 0.055(5) 0.035(4) 0.041(4) 0.006(3) 0.011(4) 0.001(4) C7 0.062(5) 0.037(4) 0.039(4) 0.006(3) 0.009(4) 0.005(4) C10 0.067(5) 0.023(4) 0.051(5) 0.004(3) 0.008(4) 0.000(4) C11 0.039(4) 0.026(3) 0.046(4) 0.000(3) 0.004(3) 0.003(3) C12 0.051(4) 0.025(4) 0.051(5) 0.002(3) 0.009(4) 0.002(3) C13 0.069(5) 0.022(3) 0.042(4) 0.004(3) 0.009(4) 0.010(4) C14 0.060(5) 0.031(4) 0.052(5) -0.005(3) 0.016(4) 0.007(4) C15 0.054(5) 0.028(4) 0.041(4) 0.002(3) 0.008(3) 0.003(3) C16 0.048(4) 0.029(4) 0.047(4) 0.004(3) 0.011(3) 0.005(3) C17 0.045(4) 0.035(4) 0.045(4) -0.001(3) 0.012(3) -0.004(3) C18 0.044(4) 0.033(4) 0.048(4) -0.003(3) 0.015(3) -0.004(3) C19 0.063(6) 0.066(7) 0.087(8) -0.010(6) -0.001(6) -0.004(5) C20 0.095(9) 0.076(9) 0.176(16) 0.046(10) -0.003(10) -0.036(8) C21 0.164(19) 0.18(2) 0.16(2) 0.021(17) 0.058(16) -0.048(17) C22 0.136(14) 0.091(11) 0.150(16) -0.008(11) -0.004(12) -0.035(11) N1 0.065(5) 0.033(3) 0.041(4) 0.001(3) 0.008(3) 0.000(3) N2 0.052(4) 0.029(3) 0.047(4) 0.007(3) 0.008(3) 0.003(3) N3 0.061(5) 0.063(5) 0.065(5) 0.001(4) 0.013(4) 0.008(4) O1 0.083(4) 0.026(3) 0.044(3) 0.005(2) 0.023(3) 0.005(3) O2 0.059(3) 0.024(2) 0.043(3) 0.003(2) 0.012(2) 0.002(2) O3 0.061(4) 0.031(3) 0.046(3) 0.003(2) 0.018(3) 0.002(3) O4 0.066(4) 0.030(3) 0.046(3) -0.001(2) 0.024(3) -0.001(3) O5 0.054(3) 0.027(3) 0.045(3) 0.001(2) 0.014(2) 0.000(2) O6 0.080(4) 0.031(3) 0.038(3) 0.001(2) 0.024(3) 0.003(3) O7 0.056(3) 0.027(3) 0.073(4) 0.012(3) 0.001(3) 0.000(3) O8 0.041(3) 0.032(3) 0.049(3) 0.012(2) 0.005(2) 0.007(2) O9 0.103(7) 0.111(8) 0.142(10) 0.005(7) -0.014(7) -0.013(6) O10 0.048(3) 0.040(3) 0.066(4) 0.000(3) 0.004(3) -0.007(3) O11 0.154(10) 0.088(7) 0.105(7) -0.022(6) 0.002(7) -0.038(7) O12 0.202(14) 0.156(13) 0.125(10) -0.030(9) -0.015(9) -0.004(11) O13 0.110(7) 0.096(7) 0.147(10) -0.034(7) 0.037(7) 0.006(6) S1 0.0547(14) 0.0498(14) 0.096(2) -0.0209(13) 0.0113(13) -0.0017(11) S2 0.170(4) 0.069(2) 0.087(2) 0.0091(18) 0.034(3) -0.020(2) Ni1 0.0477(5) 0.0250(4) 0.0381(5) 0.0041(4) 0.0090(4) 0.0011(4) Dy1 0.0450(2) 0.02522(17) 0.0430(2) 0.00158(15) 0.01136(13) 0.00054(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.315(9) . ? C1 C6 1.414(11) . ? C1 C2 1.416(11) . ? C2 C3 1.383(11) . ? C3 C4 1.420(12) . ? C3 C17 1.471(11) . ? C4 C5 1.374(11) . ? C5 C6 1.385(11) . ? C6 C7 1.426(11) . ? C7 N2 1.299(11) . ? C8A C9A 1.32(2) . ? C8A N2 1.492(17) . ? C9A N1 1.51(2) . ? C8B N2 1.512(19) . ? C8B C9B 1.52(2) . ? C9B N1 1.445(16) . ? C10 N1 1.299(11) . ? C10 C12 1.431(12) . ? C11 O2 1.299(9) . ? C11 C16 1.415(11) . ? C11 C12 1.421(10) . ? C12 C13 1.418(11) . ? C13 C14 1.371(12) . ? C14 C15 1.402(11) . ? C15 C16 1.379(11) . ? C15 C18 1.517(11) . ? C17 O3 1.268(9) . ? C17 O4 1.278(9) . ? C17 Dy1 2.766(8) . ? C18 O5 1.255(9) . ? C18 O6 1.265(9) . ? C19 S1 1.778(11) . ? C20 S1 1.778(15) . ? C21 S2 1.725(19) . ? C22 S2 1.761(16) . ? N1 Ni1 1.842(7) . ? N2 Ni1 1.855(7) . ? N3 O7 1.254(10) . ? N3 O8 1.278(10) . ? N3 O9 1.533(13) . ? N3 Dy1 2.826(9) . ? O1 Ni1 1.864(5) . ? O2 Ni1 1.855(5) . ? O3 Dy1 2.395(5) . ? O4 Dy1 2.403(5) . ? O5 Dy1 2.319(5) 4_566 ? O6 Dy1 2.299(5) 2_455 ? O7 Dy1 2.432(6) . ? O8 Dy1 2.323(5) 3 ? O8 Dy1 2.475(5) . ? O10 S1 1.519(6) . ? O10 Dy1 2.298(6) . ? O11 S2 1.518(11) . ? Dy1 O6 2.299(5) 2_445 ? Dy1 O5 2.319(5) 4_665 ? Dy1 O8 2.323(5) 3 ? Dy1 Dy1 3.7902(10) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 124.0(7) . . ? O1 C1 C2 118.5(7) . . ? C6 C1 C2 117.5(7) . . ? C3 C2 C1 122.1(7) . . ? C2 C3 C4 119.7(7) . . ? C2 C3 C17 120.3(7) . . ? C4 C3 C17 120.0(7) . . ? C5 C4 C3 117.7(8) . . ? C4 C5 C6 123.8(8) . . ? C5 C6 C1 119.2(7) . . ? C5 C6 C7 118.6(7) . . ? C1 C6 C7 122.2(7) . . ? N2 C7 C6 125.0(8) . . ? C9A C8A N2 113.2(14) . . ? C8A C9A N1 113.8(16) . . ? N2 C8B C9B 106.9(13) . . ? N1 C9B C8B 111.6(12) . . ? N1 C10 C12 124.7(7) . . ? O2 C11 C16 119.3(7) . . ? O2 C11 C12 124.0(7) . . ? C16 C11 C12 116.7(7) . . ? C13 C12 C11 120.4(7) . . ? C13 C12 C10 117.8(7) . . ? C11 C12 C10 121.7(7) . . ? C14 C13 C12 120.8(7) . . ? C13 C14 C15 119.7(7) . . ? C16 C15 C14 120.2(7) . . ? C16 C15 C18 120.1(7) . . ? C14 C15 C18 119.7(7) . . ? C15 C16 C11 122.3(7) . . ? O3 C17 O4 119.8(7) . . ? O3 C17 C3 120.4(7) . . ? O4 C17 C3 119.7(7) . . ? O3 C17 Dy1 59.9(4) . . ? O4 C17 Dy1 60.2(4) . . ? C3 C17 Dy1 177.2(6) . . ? O5 C18 O6 125.7(8) . . ? O5 C18 C15 118.4(7) . . ? O6 C18 C15 115.9(7) . . ? C10 N1 C9B 115.4(9) . . ? C10 N1 C9A 119.5(10) . . ? C9B N1 C9A 27.6(8) . . ? C10 N1 Ni1 127.1(6) . . ? C9B N1 Ni1 115.5(8) . . ? C9A N1 Ni1 112.2(9) . . ? C7 N2 C8A 119.2(8) . . ? C7 N2 C8B 116.0(9) . . ? C8A N2 C8B 19.5(8) . . ? C7 N2 Ni1 126.9(6) . . ? C8A N2 Ni1 113.1(7) . . ? C8B N2 Ni1 116.4(8) . . ? O7 N3 O8 119.3(8) . . ? O7 N3 O9 121.4(8) . . ? O8 N3 O9 119.3(8) . . ? O7 N3 Dy1 59.1(4) . . ? O8 N3 Dy1 61.1(4) . . ? O9 N3 Dy1 168.9(7) . . ? C1 O1 Ni1 127.0(5) . . ? C11 O2 Ni1 127.5(5) . . ? C17 O3 Dy1 92.9(5) . . ? C17 O4 Dy1 92.3(4) . . ? C18 O5 Dy1 135.9(5) . 4_566 ? C18 O6 Dy1 137.5(5) . 2_455 ? N3 O7 Dy1 94.7(5) . . ? N3 O8 Dy1 157.0(6) . 3 ? N3 O8 Dy1 92.1(5) . . ? Dy1 O8 Dy1 104.3(2) 3 . ? S1 O10 Dy1 135.5(4) . . ? O10 S1 C20 106.9(6) . . ? O10 S1 C19 104.2(5) . . ? C20 S1 C19 97.5(7) . . ? O11 S2 C21 105.0(9) . . ? O11 S2 C22 105.0(8) . . ? C21 S2 C22 97.7(10) . . ? N1 Ni1 O2 95.0(3) . . ? N1 Ni1 N2 85.8(3) . . ? O2 Ni1 N2 177.5(3) . . ? N1 Ni1 O1 178.1(3) . . ? O2 Ni1 O1 84.3(2) . . ? N2 Ni1 O1 94.9(3) . . ? O10 Dy1 O6 92.8(2) . 2_445 ? O10 Dy1 O5 105.6(2) . 4_665 ? O6 Dy1 O5 140.82(18) 2_445 4_665 ? O10 Dy1 O8 79.0(2) . 3 ? O6 Dy1 O8 75.3(2) 2_445 3 ? O5 Dy1 O8 74.8(2) 4_665 3 ? O10 Dy1 O3 80.4(2) . . ? O6 Dy1 O3 81.25(18) 2_445 . ? O5 Dy1 O3 135.13(18) 4_665 . ? O8 Dy1 O3 147.7(2) 3 . ? O10 Dy1 O4 80.1(2) . . ? O6 Dy1 O4 135.92(18) 2_445 . ? O5 Dy1 O4 82.06(18) 4_665 . ? O8 Dy1 O4 143.08(19) 3 . ? O3 Dy1 O4 54.68(17) . . ? O10 Dy1 O7 153.3(2) . . ? O6 Dy1 O7 96.7(2) 2_445 . ? O5 Dy1 O7 82.3(2) 4_665 . ? O8 Dy1 O7 127.59(19) 3 . ? O3 Dy1 O7 76.5(2) . . ? O4 Dy1 O7 75.7(2) . . ? O10 Dy1 O8 153.53(19) . . ? O6 Dy1 O8 73.7(2) 2_445 . ? O5 Dy1 O8 74.88(19) 4_665 . ? O8 Dy1 O8 75.7(2) 3 . ? O3 Dy1 O8 118.53(18) . . ? O4 Dy1 O8 125.44(19) . . ? O7 Dy1 O8 52.86(17) . . ? O10 Dy1 C17 80.6(2) . . ? O6 Dy1 C17 108.5(2) 2_445 . ? O5 Dy1 C17 108.5(2) 4_665 . ? O8 Dy1 C17 159.4(2) 3 . ? O3 Dy1 C17 27.3(2) . . ? O4 Dy1 C17 27.5(2) . . ? O7 Dy1 C17 72.8(2) . . ? O8 Dy1 C17 125.0(2) . . ? O10 Dy1 N3 179.5(2) . . ? O6 Dy1 N3 87.2(2) 2_445 . ? O5 Dy1 N3 74.7(2) 4_665 . ? O8 Dy1 N3 101.5(2) 3 . ? O3 Dy1 N3 99.1(2) . . ? O4 Dy1 N3 99.6(2) . . ? O7 Dy1 N3 26.2(2) . . ? O8 Dy1 N3 26.9(2) . . ? C17 Dy1 N3 99.0(2) . . ? O10 Dy1 Dy1 117.85(15) . 3 ? O6 Dy1 Dy1 70.16(13) 2_445 3 ? O5 Dy1 Dy1 70.66(13) 4_665 3 ? O8 Dy1 Dy1 39.25(13) 3 3 ? O3 Dy1 Dy1 146.09(13) . 3 ? O4 Dy1 Dy1 150.29(14) . 3 ? O7 Dy1 Dy1 88.83(13) . 3 ? O8 Dy1 Dy1 36.42(11) . 3 ? C17 Dy1 Dy1 161.39(17) . 3 ? N3 Dy1 Dy1 62.59(18) . 3 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.992 _refine_diff_density_min -1.779 _refine_diff_density_rms 0.153 _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END========================================================================