# 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H71.50 Gd N4.50 Ni O10.50' _chemical_formula_weight 1383.80 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3208(5) _cell_length_b 15.4148(6) _cell_length_c 17.9987(7) _cell_angle_alpha 88.6950(12) _cell_angle_beta 73.2600(12) _cell_angle_gamma 70.2450(12) _cell_volume 3319.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20143 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1422 _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5761 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_decay_% ? _diffrn_reflns_number 25192 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11546 _reflns_number_gt 10002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _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^)+(0.0811P)^2^+10.1904P] 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 11546 _refine_ls_number_parameters 839 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Gd1 Gd 0.15254(2) 0.100368(17) 0.227482(14) 0.03129(10) Uani 1 1 d . . . Ni2 Ni 0.10939(6) 0.20786(4) 0.40442(4) 0.03210(17) Uani 1 1 d . . . O5 O 0.2389(3) 0.1276(2) 0.3149(2) 0.0324(8) Uani 1 1 d . . . O6 O 0.3744(3) 0.0438(3) 0.1862(2) 0.0377(8) Uani 1 1 d . . . O7 O 0.1978(3) 0.2689(3) 0.4455(2) 0.0379(8) Uani 1 1 d . . . O8 O 0.0721(3) 0.3161(2) 0.3377(2) 0.0365(8) Uani 1 1 d . . . O9 O 0.2173(3) 0.1892(3) 0.1336(2) 0.0414(9) Uani 1 1 d . . . O10 O -0.0021(3) 0.2041(3) 0.2002(2) 0.0417(9) Uani 1 1 d . . . O11 O 0.1892(3) 0.0106(3) 0.1140(2) 0.0392(9) Uani 1 1 d . . . O12 O 0.2191(3) -0.0545(2) 0.2543(2) 0.0379(8) Uani 1 1 d . . . O13 O 0.0305(3) 0.1496(2) 0.3508(2) 0.0330(8) Uani 1 1 d . . . O14 O -0.0182(3) 0.0385(3) 0.2728(2) 0.0365(8) Uani 1 1 d . . . N3 N 0.1568(4) 0.0964(3) 0.4733(3) 0.0357(10) Uani 1 1 d . . . N4 N -0.0388(4) 0.2616(3) 0.4989(3) 0.0400(11) Uani 1 1 d . . . N5 N 0.3811(8) 0.4117(6) 0.1836(6) 0.109(3) Uani 1 1 d . . . C15 C -0.0399(5) -0.0235(5) 0.2270(4) 0.0481(15) Uani 1 1 d . . . H15A H -0.0886 0.0120 0.1970 0.058 Uiso 1 1 calc R . . H15B H -0.0767 -0.0611 0.2613 0.058 Uiso 1 1 calc R . . H15C H 0.0307 -0.0639 0.1913 0.058 Uiso 1 1 calc R . . C16 C -0.1086(4) 0.0974(4) 0.3301(3) 0.0346(11) Uani 1 1 d . . . C17 C -0.2172(5) 0.1008(4) 0.3455(3) 0.0380(12) Uani 1 1 d . . . H17 H -0.2343 0.0594 0.3170 0.046 Uiso 1 1 calc R . . C18 C -0.3031(5) 0.1657(4) 0.4033(3) 0.0418(13) Uani 1 1 d . . . C19 C -0.2729(5) 0.2230(4) 0.4446(3) 0.0420(13) Uani 1 1 d . . . H19 H -0.3294 0.2660 0.4849 0.050 Uiso 1 1 calc R . . C20 C -0.1632(5) 0.2197(4) 0.4292(3) 0.0379(12) Uani 1 1 d . . . C21 C -0.0786(5) 0.1565(4) 0.3713(3) 0.0344(11) Uani 1 1 d . . . C22 C -0.4233(5) 0.1718(5) 0.4190(4) 0.0534(16) Uani 1 1 d . . . H22A H -0.4679 0.2335 0.4092 0.064 Uiso 1 1 calc R . . H22B H -0.4531 0.1605 0.4733 0.064 Uiso 1 1 calc R . . H22C H -0.4267 0.1252 0.3845 0.064 Uiso 1 1 calc R . . C23 C -0.1416(5) 0.2917(4) 0.4728(4) 0.0446(14) Uani 1 1 d . . . H23A H -0.1384 0.3429 0.4390 0.054 Uiso 1 1 calc R . . H23B H -0.2070 0.3175 0.5194 0.054 Uiso 1 1 calc R . . C24 C -0.0428(6) 0.3435(4) 0.5429(4) 0.0510(15) Uani 1 1 d . . . H24A H -0.1125 0.3650 0.5859 0.077 Uiso 1 1 calc R . . H24B H -0.0395 0.3930 0.5082 0.077 Uiso 1 1 calc R . . H24C H 0.0210 0.3265 0.5638 0.077 Uiso 1 1 calc R . . C25 C -0.0363(5) 0.1845(4) 0.5505(3) 0.0470(14) Uani 1 1 d . . . H25A H -0.0644 0.1407 0.5307 0.056 Uiso 1 1 calc R . . H25B H -0.0857 0.2094 0.6037 0.056 Uiso 1 1 calc R . . C26 C 0.0817(5) 0.1343(4) 0.5530(3) 0.0449(14) Uani 1 1 d . . . H26A H 0.1087 0.1776 0.5746 0.054 Uiso 1 1 calc R . . H26B H 0.0825 0.0833 0.5875 0.054 Uiso 1 1 calc R . . C27 C 0.1418(5) 0.0101(4) 0.4512(3) 0.0393(13) Uani 1 1 d . . . H27A H 0.1651 -0.0373 0.4860 0.059 Uiso 1 1 calc R . . H27B H 0.1875 -0.0120 0.3973 0.059 Uiso 1 1 calc R . . H27C H 0.0630 0.0229 0.4556 0.059 Uiso 1 1 calc R . . C28 C 0.2758(5) 0.0742(4) 0.4700(3) 0.0406(13) Uani 1 1 d . . . H28A H 0.2938 0.0279 0.5075 0.049 Uiso 1 1 calc R . . H28B H 0.2856 0.1309 0.4865 0.049 Uiso 1 1 calc R . . C29 C 0.3582(5) 0.0370(4) 0.3899(3) 0.0372(12) Uani 1 1 d . . . C30 C 0.4634(5) -0.0285(4) 0.3859(4) 0.0432(14) Uani 1 1 d . . . H30 H 0.4800 -0.0457 0.4332 0.052 Uiso 1 1 calc R . . C31 C 0.5435(5) -0.0689(4) 0.3168(4) 0.0447(14) Uani 1 1 d . . . C32 C 0.6565(6) -0.1378(5) 0.3144(5) 0.065(2) Uani 1 1 d . . . H32A H 0.7151 -0.1146 0.2848 0.078 Uiso 1 1 calc R . . H32B H 0.6667 -0.1971 0.2892 0.078 Uiso 1 1 calc R . . H32C H 0.6611 -0.1462 0.3676 0.078 Uiso 1 1 calc R . . C33 C 0.5160(5) -0.0452(4) 0.2468(4) 0.0414(13) Uani 1 1 d . . . H33 H 0.5681 -0.0733 0.1980 0.050 Uiso 1 1 calc R . . C34 C 0.4132(5) 0.0188(4) 0.2501(3) 0.0363(12) Uani 1 1 d . . . C35 C 0.3341(5) 0.0648(4) 0.3204(3) 0.0349(12) Uani 1 1 d . . . C36 C 0.4484(5) 0.0047(5) 0.1103(3) 0.0495(15) Uani 1 1 d . . . H36A H 0.4702 -0.0628 0.1081 0.059 Uiso 1 1 calc R . . H36B H 0.5153 0.0220 0.1001 0.059 Uiso 1 1 calc R . . H36C H 0.4104 0.0283 0.0710 0.059 Uiso 1 1 calc R . . C37 C 0.4079(5) -0.2849(4) 0.3443(3) 0.0434(13) Uani 1 1 d . . . H37 H 0.4491 -0.2801 0.3782 0.052 Uiso 1 1 calc R . . C38 C 0.3560(5) -0.2075(4) 0.3097(3) 0.0366(12) Uani 1 1 d . . . H38 H 0.3591 -0.1490 0.3221 0.044 Uiso 1 1 calc R . . C39 C 0.3985(5) -0.3700(4) 0.3285(4) 0.0472(14) Uani 1 1 d . . . H39 H 0.4326 -0.4228 0.3525 0.057 Uiso 1 1 calc R . . C40 C 0.3402(5) -0.3776(4) 0.2787(4) 0.0484(15) Uani 1 1 d . . . H40 H 0.3328 -0.4351 0.2690 0.058 Uiso 1 1 calc R . . C41 C 0.2916(5) -0.2996(4) 0.2419(3) 0.0382(12) Uani 1 1 d . . . H41 H 0.2528 -0.3047 0.2063 0.046 Uiso 1 1 calc R . . C42 C 0.3007(5) -0.2148(4) 0.2579(3) 0.0363(12) Uani 1 1 d . . . C43 C 0.2633(5) -0.1465(4) 0.1375(3) 0.0389(12) Uani 1 1 d . . . H43A H 0.2888 -0.2085 0.1157 0.047 Uiso 1 1 calc R . . C44 C 0.2554(4) -0.1318(4) 0.2165(3) 0.0349(12) Uani 1 1 d . . . C45 C 0.2357(4) -0.0749(4) 0.0895(3) 0.0357(12) Uani 1 1 d . . . C46 C 0.2635(4) -0.0962(4) 0.0038(3) 0.0369(12) Uani 1 1 d . . . C47 C 0.2550(5) -0.0239(5) -0.0447(3) 0.0469(14) Uani 1 1 d . . . H47 H 0.2333 0.0378 -0.0232 0.056 Uiso 1 1 calc R . . C48 C 0.2782(5) -0.0416(5) -0.1249(4) 0.0537(17) Uani 1 1 d . . . H48 H 0.2725 0.0080 -0.1576 0.064 Uiso 1 1 calc R . . C49 C 0.3092(5) -0.1309(6) -0.1567(4) 0.0576(18) Uani 1 1 d . . . H49 H 0.3244 -0.1428 -0.2111 0.069 Uiso 1 1 calc R . . C50 C 0.3181(6) -0.2021(5) -0.1093(4) 0.0586(18) Uani 1 1 d . . . H50 H 0.3392 -0.2635 -0.1313 0.070 Uiso 1 1 calc R . . C51 C 0.2969(5) -0.1864(5) -0.0302(4) 0.0494(15) Uani 1 1 d . . . H51 H 0.3050 -0.2370 0.0015 0.059 Uiso 1 1 calc R . . C52 C 0.3653(5) 0.2480(5) 0.0207(4) 0.0505(15) Uani 1 1 d . . . H52 H 0.3846 0.2272 0.0664 0.061 Uiso 1 1 calc R . . C53 C 0.4433(6) 0.2672(5) -0.0410(5) 0.0624(19) Uani 1 1 d . . . H53 H 0.5147 0.2612 -0.0367 0.075 Uiso 1 1 calc R . . C54 C 0.4170(6) 0.2951(5) -0.1093(4) 0.064(2) Uani 1 1 d . . . H54 H 0.4701 0.3085 -0.1516 0.077 Uiso 1 1 calc R . . C55 C 0.3146(6) 0.3030(6) -0.1151(4) 0.065(2) Uani 1 1 d . . . H55 H 0.2973 0.3204 -0.1621 0.078 Uiso 1 1 calc R . . C56 C 0.2351(6) 0.2860(5) -0.0530(4) 0.0599(18) Uani 1 1 d . . . H56 H 0.1637 0.2927 -0.0576 0.072 Uiso 1 1 calc R . . C57 C 0.2596(5) 0.2589(4) 0.0164(3) 0.0425(13) Uani 1 1 d . . . C58 C 0.1762(5) 0.2419(4) 0.0853(4) 0.0427(13) Uani 1 1 d . . . C59 C 0.0623(5) 0.2835(4) 0.0951(4) 0.0466(14) Uani 1 1 d . . . H59A H 0.0400 0.3259 0.0589 0.056 Uiso 1 1 calc R . . C60 C -0.0212(5) 0.2669(4) 0.1548(3) 0.0408(13) Uani 1 1 d . . . C61 C -0.1431(5) 0.3259(4) 0.1692(4) 0.0447(14) Uani 1 1 d . . . C62 C -0.2192(5) 0.3211(5) 0.2396(4) 0.0486(15) Uani 1 1 d . . . H62 H -0.1946 0.2802 0.2761 0.058 Uiso 1 1 calc R . . C63 C -0.3303(6) 0.3761(5) 0.2561(5) 0.0610(19) Uani 1 1 d . . . H63 H -0.3818 0.3732 0.3044 0.073 Uiso 1 1 calc R . . C64 C -0.3675(6) 0.4350(5) 0.2033(5) 0.067(2) Uani 1 1 d . . . H64 H -0.4439 0.4731 0.2155 0.081 Uiso 1 1 calc R . . C65 C -0.2927(7) 0.4386(6) 0.1322(6) 0.076(2) Uani 1 1 d . . . H65 H -0.3182 0.4783 0.0953 0.092 Uiso 1 1 calc R . . C66 C -0.1806(6) 0.3843(5) 0.1151(5) 0.0634(19) Uani 1 1 d . . . H66 H -0.1295 0.3868 0.0666 0.076 Uiso 1 1 calc R . . C67 C 0.2646(5) 0.3810(4) 0.4790(3) 0.0359(12) Uani 1 1 d . . . C68 C 0.2680(6) 0.3460(5) 0.5506(4) 0.0506(16) Uani 1 1 d . . . H68 H 0.2358 0.3000 0.5681 0.061 Uiso 1 1 calc R . . C69 C 0.3181(6) 0.3780(5) 0.5965(4) 0.0576(17) Uani 1 1 d . . . H69 H 0.3184 0.3547 0.6457 0.069 Uiso 1 1 calc R . . C70 C 0.3666(7) 0.4418(5) 0.5718(5) 0.064(2) Uani 1 1 d . . . H70 H 0.3995 0.4640 0.6041 0.076 Uiso 1 1 calc R . . C71 C 0.3681(8) 0.4750(6) 0.4994(6) 0.087(3) Uani 1 1 d . . . H71 H 0.4036 0.5188 0.4815 0.104 Uiso 1 1 calc R . . C72 C 0.3180(7) 0.4443(5) 0.4533(5) 0.066(2) Uani 1 1 d . . . H72 H 0.3200 0.4668 0.4035 0.079 Uiso 1 1 calc R . . C73 C 0.2048(4) 0.3487(4) 0.4323(3) 0.0343(11) Uani 1 1 d . . . C74 C 0.1564(5) 0.4084(4) 0.3829(3) 0.0387(12) Uani 1 1 d . . . H74A H 0.1678 0.4662 0.3783 0.046 Uiso 1 1 calc R . . C75 C 0.0927(4) 0.3909(4) 0.3396(3) 0.0347(11) Uani 1 1 d . . . C76 C 0.0371(5) 0.4665(4) 0.2952(3) 0.0416(13) Uani 1 1 d . . . C77 C 0.0650(6) 0.5461(4) 0.2805(4) 0.0518(16) Uani 1 1 d . . . H77 H 0.1245 0.5525 0.2963 0.062 Uiso 1 1 calc R . . C78 C 0.0066(7) 0.6156(5) 0.2432(5) 0.066(2) Uani 1 1 d . . . H78 H 0.0251 0.6701 0.2347 0.080 Uiso 1 1 calc R . . C79 C -0.0488(5) 0.4600(4) 0.2704(4) 0.0500(15) Uani 1 1 d . . . H79 H -0.0706 0.4073 0.2808 0.060 Uiso 1 1 calc R . . C80 C -0.1041(6) 0.5285(5) 0.2307(5) 0.064(2) Uani 1 1 d . . . H80 H -0.1608 0.5210 0.2120 0.077 Uiso 1 1 calc R . . C81 C -0.0773(7) 0.6068(5) 0.2184(5) 0.070(2) Uani 1 1 d . . . H81 H -0.1170 0.6549 0.1927 0.084 Uiso 1 1 calc R . . C82 C 0.3847(7) 0.2530(5) 0.2385(5) 0.071(2) Uani 1 1 d . . . H82A H 0.3211 0.2389 0.2321 0.086 Uiso 1 1 calc R . . H82B H 0.3801 0.2551 0.2938 0.086 Uiso 1 1 calc R . . H82C H 0.4545 0.2048 0.2093 0.086 Uiso 1 1 calc R . . C83 C 0.3825(7) 0.3421(6) 0.2091(5) 0.072(2) Uani 1 1 d . . . N6 N 0.9458(17) 0.8135(9) 0.1139(12) 0.095(7) Uani 0.50 1 d P . . C86 C 1.0179(11) 0.8705(15) -0.0069(15) 0.107(10) Uani 0.50 1 d P . . H86A H 0.9740 0.8688 -0.0418 0.160 Uiso 0.50 1 calc PR . . H86B H 1.0963 0.8324 -0.0313 0.160 Uiso 0.50 1 calc PR . . H86C H 1.0124 0.9344 0.0030 0.160 Uiso 0.50 1 calc PR . . C85 C 0.9784(19) 0.8374(9) 0.0604(16) 0.075(7) Uani 0.50 1 d P . . C87 C 0.1802(10) 0.4879(7) 0.0734(6) 0.100(3) Uani 1 1 d . . . C88 C 0.085(2) 0.5010(18) 0.0404(18) 0.116(9) Uani 0.50 1 d P . . C88A C 0.2058(16) 0.5734(10) 0.0761(9) 0.069(4) Uani 0.50 1 d P . . N7A N 0.248(4) 0.6313(15) 0.0735(9) 0.211(18) Uani 0.50 1 d P . . N7 N 0.002(12) 0.511(6) 0.015(5) 0.13(2) Uani 0.50 1 d P . . O2W O 0.436(3) 0.5461(16) 0.0318(19) 0.25(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.03243(16) 0.02728(15) 0.03158(16) 0.00254(10) -0.01132(11) -0.00564(11) Ni2 0.0399(4) 0.0258(3) 0.0323(4) 0.0009(3) -0.0106(3) -0.0135(3) O5 0.0330(18) 0.0287(19) 0.0356(19) 0.0061(15) -0.0123(16) -0.0092(15) O6 0.0321(19) 0.040(2) 0.034(2) 0.0036(16) -0.0091(16) -0.0049(17) O7 0.048(2) 0.031(2) 0.041(2) 0.0043(16) -0.0196(18) -0.0178(18) O8 0.045(2) 0.0294(19) 0.040(2) 0.0027(16) -0.0177(17) -0.0142(17) O9 0.039(2) 0.044(2) 0.040(2) 0.0130(18) -0.0167(18) -0.0089(18) O10 0.035(2) 0.035(2) 0.049(2) 0.0099(18) -0.0153(18) -0.0035(17) O11 0.045(2) 0.039(2) 0.033(2) -0.0012(17) -0.0171(17) -0.0082(18) O12 0.045(2) 0.0263(19) 0.040(2) -0.0020(16) -0.0175(18) -0.0042(17) O13 0.0326(18) 0.0298(19) 0.039(2) 0.0000(15) -0.0116(16) -0.0128(16) O14 0.039(2) 0.033(2) 0.042(2) -0.0040(16) -0.0145(17) -0.0145(17) N3 0.048(3) 0.031(2) 0.031(2) 0.0024(18) -0.010(2) -0.018(2) N4 0.051(3) 0.033(3) 0.034(2) -0.002(2) -0.006(2) -0.018(2) N5 0.121(7) 0.067(5) 0.131(8) -0.006(5) -0.008(6) -0.045(5) C15 0.048(3) 0.054(4) 0.048(4) -0.009(3) -0.015(3) -0.023(3) C16 0.035(3) 0.032(3) 0.033(3) 0.005(2) -0.009(2) -0.009(2) C17 0.038(3) 0.041(3) 0.038(3) 0.004(2) -0.013(2) -0.015(3) C18 0.041(3) 0.041(3) 0.045(3) 0.009(3) -0.014(3) -0.015(3) C19 0.036(3) 0.042(3) 0.041(3) 0.003(3) -0.005(2) -0.010(3) C20 0.040(3) 0.027(3) 0.041(3) 0.002(2) -0.006(2) -0.009(2) C21 0.040(3) 0.031(3) 0.033(3) 0.004(2) -0.012(2) -0.012(2) C22 0.039(3) 0.060(4) 0.060(4) 0.006(3) -0.015(3) -0.016(3) C23 0.046(3) 0.035(3) 0.044(3) -0.007(3) -0.002(3) -0.011(3) C24 0.056(4) 0.043(4) 0.050(4) -0.014(3) -0.006(3) -0.019(3) C25 0.057(4) 0.046(4) 0.037(3) -0.003(3) -0.003(3) -0.025(3) C26 0.062(4) 0.044(3) 0.034(3) 0.005(3) -0.014(3) -0.024(3) C27 0.056(3) 0.033(3) 0.037(3) 0.007(2) -0.017(3) -0.023(3) C28 0.053(3) 0.035(3) 0.043(3) 0.010(2) -0.024(3) -0.019(3) C29 0.046(3) 0.033(3) 0.040(3) 0.009(2) -0.018(3) -0.020(3) C30 0.050(3) 0.039(3) 0.052(4) 0.011(3) -0.029(3) -0.018(3) C31 0.041(3) 0.037(3) 0.059(4) 0.014(3) -0.024(3) -0.011(3) C32 0.047(4) 0.062(5) 0.081(5) 0.024(4) -0.030(4) -0.003(3) C33 0.041(3) 0.034(3) 0.049(3) 0.009(3) -0.016(3) -0.010(3) C34 0.037(3) 0.034(3) 0.042(3) 0.011(2) -0.015(2) -0.014(2) C35 0.041(3) 0.027(3) 0.044(3) 0.011(2) -0.019(3) -0.015(2) C36 0.035(3) 0.066(4) 0.036(3) -0.003(3) -0.003(3) -0.009(3) C37 0.043(3) 0.043(3) 0.042(3) 0.010(3) -0.015(3) -0.010(3) C38 0.040(3) 0.032(3) 0.035(3) 0.003(2) -0.011(2) -0.008(2) C39 0.047(3) 0.037(3) 0.050(4) 0.014(3) -0.016(3) -0.004(3) C40 0.049(3) 0.034(3) 0.055(4) 0.000(3) -0.008(3) -0.011(3) C41 0.040(3) 0.031(3) 0.040(3) -0.001(2) -0.011(2) -0.008(2) C42 0.038(3) 0.032(3) 0.036(3) 0.002(2) -0.007(2) -0.010(2) C43 0.040(3) 0.034(3) 0.037(3) -0.006(2) -0.013(2) -0.002(2) C44 0.030(3) 0.037(3) 0.036(3) 0.003(2) -0.011(2) -0.008(2) C45 0.033(3) 0.038(3) 0.034(3) -0.002(2) -0.010(2) -0.008(2) C46 0.030(3) 0.046(3) 0.033(3) 0.001(2) -0.012(2) -0.009(2) C47 0.042(3) 0.064(4) 0.039(3) 0.005(3) -0.013(3) -0.023(3) C48 0.050(4) 0.083(5) 0.036(3) 0.018(3) -0.017(3) -0.029(4) C49 0.048(4) 0.083(5) 0.033(3) -0.008(3) -0.011(3) -0.012(4) C50 0.058(4) 0.068(5) 0.040(4) -0.016(3) -0.018(3) -0.005(4) C51 0.050(4) 0.051(4) 0.041(3) -0.009(3) -0.018(3) -0.006(3) C52 0.043(3) 0.052(4) 0.049(4) 0.011(3) -0.013(3) -0.007(3) C53 0.039(3) 0.069(5) 0.069(5) 0.009(4) -0.009(3) -0.012(3) C54 0.046(4) 0.066(5) 0.059(4) 0.018(4) 0.003(3) -0.009(3) C55 0.062(4) 0.073(5) 0.051(4) 0.027(4) -0.015(3) -0.015(4) C56 0.053(4) 0.073(5) 0.056(4) 0.019(4) -0.022(3) -0.022(4) C57 0.045(3) 0.039(3) 0.042(3) 0.010(3) -0.014(3) -0.011(3) C58 0.043(3) 0.037(3) 0.049(3) 0.004(3) -0.016(3) -0.013(3) C59 0.041(3) 0.043(3) 0.055(4) 0.016(3) -0.020(3) -0.010(3) C60 0.036(3) 0.041(3) 0.045(3) 0.004(3) -0.017(3) -0.007(3) C61 0.037(3) 0.035(3) 0.060(4) 0.005(3) -0.019(3) -0.005(3) C62 0.042(3) 0.048(4) 0.051(4) -0.006(3) -0.016(3) -0.006(3) C63 0.044(4) 0.061(4) 0.066(5) -0.023(4) -0.013(3) -0.003(3) C64 0.044(4) 0.058(5) 0.087(6) -0.011(4) -0.029(4) 0.007(3) C65 0.055(4) 0.068(5) 0.094(6) 0.016(5) -0.036(5) 0.005(4) C66 0.043(4) 0.069(5) 0.069(5) 0.023(4) -0.021(3) -0.004(3) C67 0.039(3) 0.022(3) 0.050(3) 0.004(2) -0.022(3) -0.009(2) C68 0.065(4) 0.059(4) 0.044(3) 0.007(3) -0.025(3) -0.035(3) C69 0.069(4) 0.063(4) 0.054(4) 0.006(3) -0.034(4) -0.026(4) C70 0.075(5) 0.052(4) 0.088(5) 0.007(4) -0.057(4) -0.026(4) C71 0.108(7) 0.086(6) 0.135(8) 0.064(6) -0.095(7) -0.073(6) C72 0.086(5) 0.068(5) 0.083(5) 0.042(4) -0.057(5) -0.052(4) C73 0.037(3) 0.027(3) 0.037(3) 0.000(2) -0.010(2) -0.010(2) C74 0.044(3) 0.028(3) 0.051(3) 0.007(2) -0.021(3) -0.016(2) C75 0.037(3) 0.031(3) 0.035(3) 0.000(2) -0.012(2) -0.009(2) C76 0.044(3) 0.037(3) 0.045(3) 0.003(3) -0.019(3) -0.011(3) C77 0.066(4) 0.041(3) 0.058(4) 0.014(3) -0.033(3) -0.020(3) C78 0.090(6) 0.052(4) 0.068(5) 0.016(4) -0.035(4) -0.029(4) C79 0.055(4) 0.041(3) 0.063(4) 0.011(3) -0.031(3) -0.017(3) C80 0.063(4) 0.052(4) 0.088(6) 0.013(4) -0.047(4) -0.014(4) C81 0.086(6) 0.048(4) 0.088(6) 0.020(4) -0.056(5) -0.015(4) C82 0.069(5) 0.056(5) 0.077(5) -0.005(4) 0.000(4) -0.024(4) C83 0.065(5) 0.051(5) 0.091(6) -0.015(4) 0.001(4) -0.027(4) N6 0.175(17) 0.025(7) 0.145(16) 0.018(8) -0.139(15) -0.034(8) C86 0.021(6) 0.108(16) 0.18(2) -0.108(17) -0.036(10) 0.007(8) C85 0.110(16) 0.014(6) 0.126(17) -0.011(8) -0.105(16) 0.005(7) C87 0.115(8) 0.080(7) 0.092(7) -0.014(5) -0.016(6) -0.030(6) C88 0.089(16) 0.089(16) 0.15(2) 0.020(15) -0.053(17) 0.000(13) C88A 0.105(13) 0.040(8) 0.049(8) 0.003(6) -0.017(8) -0.014(8) N7A 0.56(6) 0.115(15) 0.043(9) 0.034(9) -0.099(19) -0.21(3) N7 0.154(18) 0.07(3) 0.13(6) 0.01(3) 0.01(5) -0.01(3) O2W 0.45(6) 0.21(3) 0.34(5) 0.21(3) -0.35(5) -0.26(4) _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 O13 2.303(4) . ? Gd1 O9 2.308(4) . ? Gd1 O10 2.316(4) . ? Gd1 O5 2.319(3) . ? Gd1 O11 2.329(4) . ? Gd1 O12 2.341(4) . ? Gd1 O6 2.659(4) . ? Gd1 O14 2.666(4) . ? Gd1 Ni2 3.4293(7) . ? Ni2 O7 2.025(4) . ? Ni2 O13 2.026(3) . ? Ni2 O5 2.037(4) . ? Ni2 O8 2.041(4) . ? Ni2 N4 2.121(5) . ? Ni2 N3 2.124(5) . ? O5 C35 1.339(6) . ? O6 C34 1.388(6) . ? O6 C36 1.436(7) . ? O7 C73 1.276(6) . ? O8 C75 1.277(6) . ? O9 C58 1.288(7) . ? O10 C60 1.260(7) . ? O11 C45 1.278(7) . ? O12 C44 1.255(7) . ? O13 C21 1.360(6) . ? O14 C16 1.387(7) . ? O14 C15 1.427(6) . ? N3 C28 1.488(7) . ? N3 C26 1.489(7) . ? N3 C27 1.489(6) . ? N4 C24 1.484(7) . ? N4 C25 1.489(8) . ? N4 C23 1.497(8) . ? N5 C83 1.154(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.376(7) . ? C16 C21 1.410(8) . ? C17 C18 1.407(8) . ? C17 H17 0.9500 . ? C18 C19 1.392(8) . ? C18 C22 1.514(8) . ? C19 C20 1.389(8) . ? C19 H19 0.9500 . ? C20 C21 1.390(8) . ? C20 C23 1.522(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.513(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.519(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C35 1.403(7) . ? C29 C30 1.406(8) . ? C30 C31 1.378(9) . ? C30 H30 0.9500 . ? C31 C33 1.417(8) . ? C31 C32 1.510(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.377(8) . ? C33 H33 0.9500 . ? C34 C35 1.407(8) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.396(8) . ? C37 C39 1.402(9) . ? C37 H37 0.9500 . ? C38 C42 1.370(8) . ? C38 H38 0.9500 . ? C39 C40 1.375(9) . ? C39 H39 0.9500 . ? C40 C41 1.409(8) . ? C40 H40 0.9500 . ? C41 C42 1.398(8) . ? C41 H41 0.9500 . ? C42 C44 1.501(7) . ? C43 C45 1.403(8) . ? C43 C44 1.411(7) . ? C43 H43A 0.9500 . ? C45 C46 1.495(7) . ? C46 C47 1.394(9) . ? C46 C51 1.404(9) . ? C47 C48 1.399(9) . ? C47 H47 0.9500 . ? C48 C49 1.381(10) . ? C48 H48 0.9500 . ? C49 C50 1.370(11) . ? C49 H49 0.9500 . ? C50 C51 1.380(9) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C57 1.385(9) . ? C52 C53 1.388(9) . ? C52 H52 0.9500 . ? C53 C54 1.393(11) . ? C53 H53 0.9500 . ? C54 C55 1.362(10) . ? C54 H54 0.9500 . ? C55 C56 1.390(10) . ? C55 H55 0.9500 . ? C56 C57 1.399(9) . ? C56 H56 0.9500 . ? C57 C58 1.493(8) . ? C58 C59 1.392(8) . ? C59 C60 1.396(8) . ? C59 H59A 0.9500 . ? C60 C61 1.517(8) . ? C61 C66 1.393(9) . ? C61 C62 1.394(9) . ? C62 C63 1.381(9) . ? C62 H62 0.9500 . ? C63 C64 1.379(11) . ? C63 H63 0.9500 . ? C64 C65 1.390(12) . ? C64 H64 0.9500 . ? C65 C66 1.388(10) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C72 1.390(8) . ? C67 C68 1.392(8) . ? C67 C73 1.504(7) . ? C68 C69 1.390(9) . ? C68 H68 0.9500 . ? C69 C70 1.352(10) . ? C69 H69 0.9500 . ? C70 C71 1.386(11) . ? C70 H70 0.9500 . ? C71 C72 1.383(10) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.396(8) . ? C74 C75 1.394(8) . ? C74 H74A 0.9500 . ? C75 C76 1.504(8) . ? C76 C79 1.375(8) . ? C76 C77 1.396(8) . ? C77 C78 1.382(9) . ? C77 H77 0.9500 . ? C78 C81 1.364(11) . ? C78 H78 0.9500 . ? C79 C80 1.381(9) . ? C79 H79 0.9500 . ? C80 C81 1.367(10) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 C83 1.455(11) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? N6 C85 1.05(3) . ? C86 C85 1.34(3) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88A 1.474(19) . ? C87 C88 1.50(3) . ? C88 N7 1.28(15) . ? C88 N7 1.79(14) 2_565 ? C88A N7A 1.20(3) . ? N7 N7 0.66(15) 2_565 ? N7 C88 1.79(14) 2_565 ? 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 O13 Gd1 O9 127.82(13) . . ? O13 Gd1 O10 78.66(13) . . ? O9 Gd1 O10 73.04(13) . . ? O13 Gd1 O5 67.39(12) . . ? O9 Gd1 O5 96.14(13) . . ? O10 Gd1 O5 126.40(13) . . ? O13 Gd1 O11 143.80(13) . . ? O9 Gd1 O11 78.78(14) . . ? O10 Gd1 O11 88.97(14) . . ? O5 Gd1 O11 141.53(13) . . ? O13 Gd1 O12 94.41(13) . . ? O9 Gd1 O12 134.83(14) . . ? O10 Gd1 O12 139.23(13) . . ? O5 Gd1 O12 85.21(12) . . ? O11 Gd1 O12 73.10(13) . . ? O13 Gd1 O6 127.11(12) . . ? O9 Gd1 O6 69.87(12) . . ? O10 Gd1 O6 142.86(13) . . ? O5 Gd1 O6 60.88(12) . . ? O11 Gd1 O6 82.00(12) . . ? O12 Gd1 O6 71.76(13) . . ? O13 Gd1 O14 62.30(11) . . ? O9 Gd1 O14 138.45(12) . . ? O10 Gd1 O14 70.39(13) . . ? O5 Gd1 O14 121.30(12) . . ? O11 Gd1 O14 81.50(13) . . ? O12 Gd1 O14 70.91(13) . . ? O6 Gd1 O14 142.15(12) . . ? O13 Gd1 Ni2 34.87(8) . . ? O9 Gd1 Ni2 106.76(10) . . ? O10 Gd1 Ni2 96.56(10) . . ? O5 Gd1 Ni2 35.24(9) . . ? O11 Gd1 Ni2 173.09(9) . . ? O12 Gd1 Ni2 99.98(9) . . ? O6 Gd1 Ni2 95.92(8) . . ? O14 Gd1 Ni2 96.41(8) . . ? O7 Ni2 O13 173.31(15) . . ? O7 Ni2 O5 96.99(15) . . ? O13 Ni2 O5 78.28(14) . . ? O7 Ni2 O8 88.73(14) . . ? O13 Ni2 O8 86.78(14) . . ? O5 Ni2 O8 92.74(15) . . ? O7 Ni2 N4 95.08(17) . . ? O13 Ni2 N4 90.33(16) . . ? O5 Ni2 N4 165.25(16) . . ? O8 Ni2 N4 95.97(17) . . ? O7 Ni2 N3 88.48(16) . . ? O13 Ni2 N3 95.85(15) . . ? O5 Ni2 N3 85.99(16) . . ? O8 Ni2 N3 176.78(16) . . ? N4 Ni2 N3 85.89(18) . . ? O7 Ni2 Gd1 133.36(11) . . ? O13 Ni2 Gd1 40.55(10) . . ? O5 Ni2 Gd1 41.07(10) . . ? O8 Ni2 Gd1 77.12(10) . . ? N4 Ni2 Gd1 130.11(13) . . ? N3 Ni2 Gd1 103.70(12) . . ? C35 O5 Ni2 126.6(3) . . ? C35 O5 Gd1 120.7(3) . . ? Ni2 O5 Gd1 103.70(14) . . ? C34 O6 C36 118.3(4) . . ? C34 O6 Gd1 111.0(3) . . ? C36 O6 Gd1 125.7(3) . . ? C73 O7 Ni2 127.3(3) . . ? C75 O8 Ni2 127.3(3) . . ? C58 O9 Gd1 134.5(4) . . ? C60 O10 Gd1 137.2(4) . . ? C45 O11 Gd1 136.8(3) . . ? C44 O12 Gd1 136.1(3) . . ? C21 O13 Ni2 129.7(3) . . ? C21 O13 Gd1 123.8(3) . . ? Ni2 O13 Gd1 104.58(14) . . ? C16 O14 C15 117.3(4) . . ? C16 O14 Gd1 112.9(3) . . ? C15 O14 Gd1 125.2(3) . . ? C28 N3 C26 110.8(4) . . ? C28 N3 C27 108.5(4) . . ? C26 N3 C27 109.9(4) . . ? C28 N3 Ni2 109.7(3) . . ? C26 N3 Ni2 103.0(3) . . ? C27 N3 Ni2 114.9(3) . . ? C24 N4 C25 109.3(5) . . ? C24 N4 C23 106.1(5) . . ? C25 N4 C23 111.8(5) . . ? C24 N4 Ni2 113.0(4) . . ? C25 N4 Ni2 104.5(4) . . ? C23 N4 Ni2 112.3(3) . . ? O14 C15 H15A 109.5 . . ? O14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 O14 124.9(5) . . ? C17 C16 C21 122.2(5) . . ? O14 C16 C21 112.9(4) . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 117.5(5) . . ? C19 C18 C22 122.1(6) . . ? C17 C18 C22 120.3(5) . . ? C20 C19 C18 122.5(6) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C19 C20 C21 119.9(5) . . ? C19 C20 C23 117.9(5) . . ? C21 C20 C23 122.0(5) . . ? O13 C21 C20 124.2(5) . . ? O13 C21 C16 118.0(5) . . ? C20 C21 C16 117.8(5) . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C20 117.9(5) . . ? N4 C23 H23A 107.8 . . ? C20 C23 H23A 107.8 . . ? N4 C23 H23B 107.8 . . ? C20 C23 H23B 107.8 . . ? H23A C23 H23B 107.2 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C26 110.2(5) . . ? N4 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? N4 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? N3 C26 C25 110.1(5) . . ? N3 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? N3 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 114.1(4) . . ? N3 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? N3 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C35 C29 C30 118.8(5) . . ? C35 C29 C28 123.2(5) . . ? C30 C29 C28 118.0(5) . . ? C31 C30 C29 123.2(5) . . ? C31 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? C30 C31 C33 117.8(5) . . ? C30 C31 C32 121.9(6) . . ? C33 C31 C32 120.3(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C31 119.4(6) . . ? C34 C33 H33 120.3 . . ? C31 C33 H33 120.3 . . ? C33 C34 O6 124.7(5) . . ? C33 C34 C35 122.9(5) . . ? O6 C34 C35 112.4(5) . . ? O5 C35 C29 125.6(5) . . ? O5 C35 C34 116.6(5) . . ? C29 C35 C34 117.6(5) . . ? O6 C36 H36A 109.5 . . ? O6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 119.3(5) . . ? C38 C37 H37 120.4 . . ? C39 C37 H37 120.4 . . ? C42 C38 C37 120.7(5) . . ? C42 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C37 120.5(5) . . ? C40 C39 H39 119.7 . . ? C37 C39 H39 119.7 . . ? C39 C40 C41 119.7(6) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 119.7(5) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C38 C42 C41 120.0(5) . . ? C38 C42 C44 119.0(5) . . ? C41 C42 C44 120.9(5) . . ? C45 C43 C44 123.8(5) . . ? C45 C43 H43A 118.1 . . ? C44 C43 H43A 118.1 . . ? O12 C44 C43 125.6(5) . . ? O12 C44 C42 116.5(5) . . ? C43 C44 C42 117.8(5) . . ? O11 C45 C43 123.9(5) . . ? O11 C45 C46 116.0(5) . . ? C43 C45 C46 120.1(5) . . ? C47 C46 C51 118.2(5) . . ? C47 C46 C45 119.1(5) . . ? C51 C46 C45 122.6(5) . . ? C46 C47 C48 120.3(6) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C49 C48 C47 120.3(7) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C50 C49 C48 119.6(6) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 121.1(7) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C50 C51 C46 120.4(7) . . ? C50 C51 H51 119.8 . . ? C46 C51 H51 119.8 . . ? C57 C52 C53 120.9(6) . . ? C57 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C52 C53 C54 120.1(6) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 119.5(6) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C56 120.8(7) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C55 C56 C57 120.5(6) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C52 C57 C56 118.2(6) . . ? C52 C57 C58 119.4(5) . . ? C56 C57 C58 122.5(6) . . ? O9 C58 C59 124.1(6) . . ? O9 C58 C57 115.6(5) . . ? C59 C58 C57 120.3(5) . . ? C58 C59 C60 124.2(5) . . ? C58 C59 H59A 117.9 . . ? C60 C59 H59A 117.9 . . ? O10 C60 C59 123.6(5) . . ? O10 C60 C61 115.5(5) . . ? C59 C60 C61 120.9(5) . . ? C66 C61 C62 119.5(6) . . ? C66 C61 C60 122.4(6) . . ? C62 C61 C60 118.1(5) . . ? C63 C62 C61 119.9(6) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C64 C63 C62 120.8(7) . . ? C64 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C63 C64 C65 119.8(6) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C66 C65 C64 120.1(7) . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 120.0(7) . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C72 C67 C68 118.2(5) . . ? C72 C67 C73 122.6(5) . . ? C68 C67 C73 119.2(5) . . ? C69 C68 C67 120.3(6) . . ? C69 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? C70 C69 C68 120.8(7) . . ? C70 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? C69 C70 C71 119.9(6) . . ? C69 C70 H70 120.1 . . ? C71 C70 H70 120.1 . . ? C72 C71 C70 120.0(7) . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C71 C72 C67 120.7(7) . . ? C71 C72 H72 119.7 . . ? C67 C72 H72 119.7 . . ? O7 C73 C74 125.5(5) . . ? O7 C73 C67 115.4(5) . . ? C74 C73 C67 119.0(5) . . ? C75 C74 C73 125.8(5) . . ? C75 C74 H74A 117.1 . . ? C73 C74 H74A 117.1 . . ? O8 C75 C74 124.9(5) . . ? O8 C75 C76 116.0(5) . . ? C74 C75 C76 119.0(5) . . ? C79 C76 C77 117.7(6) . . ? C79 C76 C75 119.2(5) . . ? C77 C76 C75 123.0(5) . . ? C78 C77 C76 120.4(6) . . ? C78 C77 H77 119.8 . . ? C76 C77 H77 119.8 . . ? C81 C78 C77 120.7(7) . . ? C81 C78 H78 119.6 . . ? C77 C78 H78 119.6 . . ? C76 C79 C80 121.5(6) . . ? C76 C79 H79 119.2 . . ? C80 C79 H79 119.2 . . ? C81 C80 C79 120.1(7) . . ? C81 C80 H80 120.0 . . ? C79 C80 H80 120.0 . . ? C78 C81 C80 119.6(7) . . ? C78 C81 H81 120.2 . . ? C80 C81 H81 120.2 . . ? C83 C82 H82A 109.5 . . ? C83 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C83 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N5 C83 C82 177.9(10) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N6 C85 C86 178(2) . . ? C88A C87 C88 112.1(15) . . ? N7 C88 C87 178(5) . . ? N7 C88 N7 16(6) . 2_565 ? C87 C88 N7 165(3) . 2_565 ? N7A C88A C87 167(2) . . ? N7 N7 C88 132(10) 2_565 . ? N7 N7 C88 33(10) 2_565 2_565 ? C88 N7 C88 164(6) . 2_565 ? 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 O13 Gd1 Ni2 O7 -176.0(2) . . . . ? O9 Gd1 Ni2 O7 -42.52(18) . . . . ? O10 Gd1 Ni2 O7 -116.74(18) . . . . ? O5 Gd1 Ni2 O7 34.0(2) . . . . ? O11 Gd1 Ni2 O7 100.3(8) . . . . ? O12 Gd1 Ni2 O7 100.68(18) . . . . ? O6 Gd1 Ni2 O7 28.21(17) . . . . ? O14 Gd1 Ni2 O7 172.36(17) . . . . ? O9 Gd1 Ni2 O13 133.46(18) . . . . ? O10 Gd1 Ni2 O13 59.25(18) . . . . ? O5 Gd1 Ni2 O13 -150.0(2) . . . . ? O11 Gd1 Ni2 O13 -83.7(8) . . . . ? O12 Gd1 Ni2 O13 -83.34(18) . . . . ? O6 Gd1 Ni2 O13 -155.81(18) . . . . ? O14 Gd1 Ni2 O13 -11.66(18) . . . . ? O13 Gd1 Ni2 O5 150.0(2) . . . . ? O9 Gd1 Ni2 O5 -76.54(17) . . . . ? O10 Gd1 Ni2 O5 -150.76(18) . . . . ? O11 Gd1 Ni2 O5 66.3(8) . . . . ? O12 Gd1 Ni2 O5 66.66(17) . . . . ? O6 Gd1 Ni2 O5 -5.81(17) . . . . ? O14 Gd1 Ni2 O5 138.34(17) . . . . ? O13 Gd1 Ni2 O8 -100.30(19) . . . . ? O9 Gd1 Ni2 O8 33.17(15) . . . . ? O10 Gd1 Ni2 O8 -41.05(15) . . . . ? O5 Gd1 Ni2 O8 109.70(18) . . . . ? O11 Gd1 Ni2 O8 176.0(8) . . . . ? O12 Gd1 Ni2 O8 176.36(14) . . . . ? O6 Gd1 Ni2 O8 103.89(14) . . . . ? O14 Gd1 Ni2 O8 -111.96(14) . . . . ? O13 Gd1 Ni2 N4 -13.3(2) . . . . ? O9 Gd1 Ni2 N4 120.12(19) . . . . ? O10 Gd1 Ni2 N4 45.9(2) . . . . ? O5 Gd1 Ni2 N4 -163.3(2) . . . . ? O11 Gd1 Ni2 N4 -97.0(8) . . . . ? O12 Gd1 Ni2 N4 -96.7(2) . . . . ? O6 Gd1 Ni2 N4 -169.15(19) . . . . ? O14 Gd1 Ni2 N4 -25.00(19) . . . . ? O13 Gd1 Ni2 N3 82.9(2) . . . . ? O9 Gd1 Ni2 N3 -143.63(16) . . . . ? O10 Gd1 Ni2 N3 142.15(16) . . . . ? O5 Gd1 Ni2 N3 -67.09(19) . . . . ? O11 Gd1 Ni2 N3 -0.8(8) . . . . ? O12 Gd1 Ni2 N3 -0.43(16) . . . . ? O6 Gd1 Ni2 N3 -72.90(15) . . . . ? O14 Gd1 Ni2 N3 71.25(15) . . . . ? O7 Ni2 O5 C35 57.6(4) . . . . ? O13 Ni2 O5 C35 -127.2(4) . . . . ? O8 Ni2 O5 C35 146.7(4) . . . . ? N4 Ni2 O5 C35 -87.1(8) . . . . ? N3 Ni2 O5 C35 -30.4(4) . . . . ? Gd1 Ni2 O5 C35 -146.6(4) . . . . ? O7 Ni2 O5 Gd1 -155.81(15) . . . . ? O13 Ni2 O5 Gd1 19.39(14) . . . . ? O8 Ni2 O5 Gd1 -66.75(15) . . . . ? N4 Ni2 O5 Gd1 59.5(7) . . . . ? N3 Ni2 O5 Gd1 116.22(16) . . . . ? O13 Gd1 O5 C35 131.0(4) . . . . ? O9 Gd1 O5 C35 -100.4(4) . . . . ? O10 Gd1 O5 C35 -173.8(3) . . . . ? O11 Gd1 O5 C35 -20.7(4) . . . . ? O12 Gd1 O5 C35 34.2(4) . . . . ? O6 Gd1 O5 C35 -37.5(3) . . . . ? O14 Gd1 O5 C35 98.5(4) . . . . ? Ni2 Gd1 O5 C35 149.1(4) . . . . ? O13 Gd1 O5 Ni2 -18.04(13) . . . . ? O9 Gd1 O5 Ni2 110.52(15) . . . . ? O10 Gd1 O5 Ni2 37.1(2) . . . . ? O11 Gd1 O5 Ni2 -169.80(16) . . . . ? O12 Gd1 O5 Ni2 -114.85(16) . . . . ? O6 Gd1 O5 Ni2 173.38(19) . . . . ? O14 Gd1 O5 Ni2 -50.64(18) . . . . ? O13 Gd1 O6 C34 19.1(4) . . . . ? O9 Gd1 O6 C34 141.9(4) . . . . ? O10 Gd1 O6 C34 145.3(3) . . . . ? O5 Gd1 O6 C34 32.3(3) . . . . ? O11 Gd1 O6 C34 -137.2(3) . . . . ? O12 Gd1 O6 C34 -62.4(3) . . . . ? O14 Gd1 O6 C34 -72.3(4) . . . . ? Ni2 Gd1 O6 C34 36.2(3) . . . . ? O13 Gd1 O6 C36 173.2(4) . . . . ? O9 Gd1 O6 C36 -64.0(4) . . . . ? O10 Gd1 O6 C36 -60.6(5) . . . . ? O5 Gd1 O6 C36 -173.5(5) . . . . ? O11 Gd1 O6 C36 17.0(4) . . . . ? O12 Gd1 O6 C36 91.7(5) . . . . ? O14 Gd1 O6 C36 81.9(5) . . . . ? Ni2 Gd1 O6 C36 -169.7(4) . . . . ? O13 Ni2 O7 C73 53.9(15) . . . . ? O5 Ni2 O7 C73 98.6(4) . . . . ? O8 Ni2 O7 C73 6.0(4) . . . . ? N4 Ni2 O7 C73 -89.9(5) . . . . ? N3 Ni2 O7 C73 -175.6(5) . . . . ? Gd1 Ni2 O7 C73 76.9(5) . . . . ? O7 Ni2 O8 C75 -7.9(4) . . . . ? O13 Ni2 O8 C75 177.1(4) . . . . ? O5 Ni2 O8 C75 -104.8(4) . . . . ? N4 Ni2 O8 C75 87.1(4) . . . . ? N3 Ni2 O8 C75 -38(3) . . . . ? Gd1 Ni2 O8 C75 -143.1(4) . . . . ? O13 Gd1 O9 C58 -78.0(6) . . . . ? O10 Gd1 O9 C58 -17.8(5) . . . . ? O5 Gd1 O9 C58 -144.0(5) . . . . ? O11 Gd1 O9 C58 74.6(5) . . . . ? O12 Gd1 O9 C58 126.6(5) . . . . ? O6 Gd1 O9 C58 160.1(6) . . . . ? O14 Gd1 O9 C58 11.4(6) . . . . ? Ni2 Gd1 O9 C58 -109.7(5) . . . . ? O13 Gd1 O10 C60 137.6(6) . . . . ? O9 Gd1 O10 C60 2.0(5) . . . . ? O5 Gd1 O10 C60 87.0(6) . . . . ? O11 Gd1 O10 C60 -76.6(6) . . . . ? O12 Gd1 O10 C60 -138.8(5) . . . . ? O6 Gd1 O10 C60 -1.3(7) . . . . ? O14 Gd1 O10 C60 -158.0(6) . . . . ? Ni2 Gd1 O10 C60 107.5(6) . . . . ? O13 Gd1 O11 C45 -82.4(6) . . . . ? O9 Gd1 O11 C45 135.6(5) . . . . ? O10 Gd1 O11 C45 -151.4(5) . . . . ? O5 Gd1 O11 C45 49.9(6) . . . . ? O12 Gd1 O11 C45 -8.6(5) . . . . ? O6 Gd1 O11 C45 64.7(5) . . . . ? O14 Gd1 O11 C45 -81.1(5) . . . . ? Ni2 Gd1 O11 C45 -8.2(12) . . . . ? O13 Gd1 O12 C44 148.5(5) . . . . ? O9 Gd1 O12 C44 -50.7(6) . . . . ? O10 Gd1 O12 C44 70.8(6) . . . . ? O5 Gd1 O12 C44 -144.6(5) . . . . ? O11 Gd1 O12 C44 3.2(5) . . . . ? O6 Gd1 O12 C44 -83.8(5) . . . . ? O14 Gd1 O12 C44 89.9(5) . . . . ? Ni2 Gd1 O12 C44 -176.8(5) . . . . ? O7 Ni2 O13 C21 -138.4(12) . . . . ? O5 Ni2 O13 C21 176.0(4) . . . . ? O8 Ni2 O13 C21 -90.5(4) . . . . ? N4 Ni2 O13 C21 5.5(4) . . . . ? N3 Ni2 O13 C21 91.4(4) . . . . ? Gd1 Ni2 O13 C21 -164.4(5) . . . . ? O7 Ni2 O13 Gd1 25.9(14) . . . . ? O5 Ni2 O13 Gd1 -19.60(14) . . . . ? O8 Ni2 O13 Gd1 73.87(16) . . . . ? N4 Ni2 O13 Gd1 169.84(18) . . . . ? N3 Ni2 O13 Gd1 -104.26(17) . . . . ? O9 Gd1 O13 C21 103.9(4) . . . . ? O10 Gd1 O13 C21 46.1(4) . . . . ? O5 Gd1 O13 C21 -176.2(4) . . . . ? O11 Gd1 O13 C21 -26.1(5) . . . . ? O12 Gd1 O13 C21 -93.3(4) . . . . ? O6 Gd1 O13 C21 -163.7(3) . . . . ? O14 Gd1 O13 C21 -27.6(3) . . . . ? Ni2 Gd1 O13 C21 165.6(4) . . . . ? O9 Gd1 O13 Ni2 -61.6(2) . . . . ? O10 Gd1 O13 Ni2 -119.46(17) . . . . ? O5 Gd1 O13 Ni2 18.21(13) . . . . ? O11 Gd1 O13 Ni2 168.31(16) . . . . ? O12 Gd1 O13 Ni2 101.15(16) . . . . ? O6 Gd1 O13 Ni2 30.7(2) . . . . ? O14 Gd1 O13 Ni2 166.9(2) . . . . ? O13 Gd1 O14 C16 25.2(3) . . . . ? O9 Gd1 O14 C16 -91.7(4) . . . . ? O10 Gd1 O14 C16 -62.0(3) . . . . ? O5 Gd1 O14 C16 59.4(3) . . . . ? O11 Gd1 O14 C16 -154.0(3) . . . . ? O12 Gd1 O14 C16 131.1(3) . . . . ? O6 Gd1 O14 C16 141.0(3) . . . . ? Ni2 Gd1 O14 C16 32.7(3) . . . . ? O13 Gd1 O14 C15 -179.5(5) . . . . ? O9 Gd1 O14 C15 63.7(5) . . . . ? O10 Gd1 O14 C15 93.3(4) . . . . ? O5 Gd1 O14 C15 -145.3(4) . . . . ? O11 Gd1 O14 C15 1.4(4) . . . . ? O12 Gd1 O14 C15 -73.6(4) . . . . ? O6 Gd1 O14 C15 -63.7(5) . . . . ? Ni2 Gd1 O14 C15 -172.0(4) . . . . ? O7 Ni2 N3 C28 -40.6(3) . . . . ? O13 Ni2 N3 C28 134.3(3) . . . . ? O5 Ni2 N3 C28 56.5(3) . . . . ? O8 Ni2 N3 C28 -10(3) . . . . ? N4 Ni2 N3 C28 -135.8(4) . . . . ? Gd1 Ni2 N3 C28 93.8(3) . . . . ? O7 Ni2 N3 C26 77.4(3) . . . . ? O13 Ni2 N3 C26 -107.7(3) . . . . ? O5 Ni2 N3 C26 174.5(3) . . . . ? O8 Ni2 N3 C26 108(3) . . . . ? N4 Ni2 N3 C26 -17.8(3) . . . . ? Gd1 Ni2 N3 C26 -148.2(3) . . . . ? O7 Ni2 N3 C27 -163.1(4) . . . . ? O13 Ni2 N3 C27 11.8(4) . . . . ? O5 Ni2 N3 C27 -66.0(4) . . . . ? O8 Ni2 N3 C27 -133(3) . . . . ? N4 Ni2 N3 C27 101.7(4) . . . . ? Gd1 Ni2 N3 C27 -28.7(4) . . . . ? O7 Ni2 N4 C24 19.5(4) . . . . ? O13 Ni2 N4 C24 -156.5(4) . . . . ? O5 Ni2 N4 C24 164.4(6) . . . . ? O8 Ni2 N4 C24 -69.7(4) . . . . ? N3 Ni2 N4 C24 107.6(4) . . . . ? Gd1 Ni2 N4 C24 -147.9(4) . . . . ? O7 Ni2 N4 C25 -99.2(3) . . . . ? O13 Ni2 N4 C25 84.7(3) . . . . ? O5 Ni2 N4 C25 45.6(8) . . . . ? O8 Ni2 N4 C25 171.5(3) . . . . ? N3 Ni2 N4 C25 -11.1(3) . . . . ? Gd1 Ni2 N4 C25 93.3(4) . . . . ? O7 Ni2 N4 C23 139.4(4) . . . . ? O13 Ni2 N4 C23 -36.6(4) . . . . ? O5 Ni2 N4 C23 -75.7(8) . . . . ? O8 Ni2 N4 C23 50.2(4) . . . . ? N3 Ni2 N4 C23 -132.4(4) . . . . ? Gd1 Ni2 N4 C23 -28.0(4) . . . . ? C15 O14 C16 C17 -0.5(8) . . . . ? Gd1 O14 C16 C17 156.9(4) . . . . ? C15 O14 C16 C21 -179.2(5) . . . . ? Gd1 O14 C16 C21 -21.8(5) . . . . ? O14 C16 C17 C18 -177.7(5) . . . . ? C21 C16 C17 C18 0.8(8) . . . . ? C16 C17 C18 C19 -1.7(8) . . . . ? C16 C17 C18 C22 178.3(5) . . . . ? C17 C18 C19 C20 1.8(9) . . . . ? C22 C18 C19 C20 -178.2(6) . . . . ? C18 C19 C20 C21 -0.9(9) . . . . ? C18 C19 C20 C23 174.3(5) . . . . ? Ni2 O13 C21 C20 11.1(7) . . . . ? Gd1 O13 C21 C20 -150.6(4) . . . . ? Ni2 O13 C21 C16 -170.4(3) . . . . ? Gd1 O13 C21 C16 27.9(6) . . . . ? C19 C20 C21 O13 178.4(5) . . . . ? C23 C20 C21 O13 3.4(9) . . . . ? C19 C20 C21 C16 -0.1(8) . . . . ? C23 C20 C21 C16 -175.1(5) . . . . ? C17 C16 C21 O13 -178.5(5) . . . . ? O14 C16 C21 O13 0.3(7) . . . . ? C17 C16 C21 C20 0.1(8) . . . . ? O14 C16 C21 C20 178.8(5) . . . . ? C24 N4 C23 C20 -176.9(5) . . . . ? C25 N4 C23 C20 -57.8(7) . . . . ? Ni2 N4 C23 C20 59.2(6) . . . . ? C19 C20 C23 N4 141.7(5) . . . . ? C21 C20 C23 N4 -43.1(8) . . . . ? C24 N4 C25 C26 -82.4(6) . . . . ? C23 N4 C25 C26 160.5(5) . . . . ? Ni2 N4 C25 C26 38.8(5) . . . . ? C28 N3 C26 C25 161.8(4) . . . . ? C27 N3 C26 C25 -78.3(6) . . . . ? Ni2 N3 C26 C25 44.5(5) . . . . ? N4 C25 C26 N3 -59.4(6) . . . . ? C26 N3 C28 C29 -178.7(4) . . . . ? C27 N3 C28 C29 60.5(6) . . . . ? Ni2 N3 C28 C29 -65.7(5) . . . . ? N3 C28 C29 C35 33.2(7) . . . . ? N3 C28 C29 C30 -146.9(5) . . . . ? C35 C29 C30 C31 -1.9(8) . . . . ? C28 C29 C30 C31 178.2(5) . . . . ? C29 C30 C31 C33 -2.3(9) . . . . ? C29 C30 C31 C32 178.9(6) . . . . ? C30 C31 C33 C34 2.2(8) . . . . ? C32 C31 C33 C34 -178.9(6) . . . . ? C31 C33 C34 O6 -176.3(5) . . . . ? C31 C33 C34 C35 2.1(8) . . . . ? C36 O6 C34 C33 -3.9(8) . . . . ? Gd1 O6 C34 C33 152.4(5) . . . . ? C36 O6 C34 C35 177.6(5) . . . . ? Gd1 O6 C34 C35 -26.1(5) . . . . ? Ni2 O5 C35 C29 5.8(7) . . . . ? Gd1 O5 C35 C29 -135.7(4) . . . . ? Ni2 O5 C35 C34 -178.6(3) . . . . ? Gd1 O5 C35 C34 39.9(6) . . . . ? C30 C29 C35 O5 -178.5(5) . . . . ? C28 C29 C35 O5 1.4(8) . . . . ? C30 C29 C35 C34 5.9(7) . . . . ? C28 C29 C35 C34 -174.1(5) . . . . ? C33 C34 C35 O5 177.9(5) . . . . ? O6 C34 C35 O5 -3.6(7) . . . . ? C33 C34 C35 C29 -6.1(8) . . . . ? O6 C34 C35 C29 172.4(4) . . . . ? C39 C37 C38 C42 -3.0(9) . . . . ? C38 C37 C39 C40 0.9(9) . . . . ? C37 C39 C40 C41 1.3(9) . . . . ? C39 C40 C41 C42 -1.6(9) . . . . ? C37 C38 C42 C41 2.8(8) . . . . ? C37 C38 C42 C44 -174.4(5) . . . . ? C40 C41 C42 C38 -0.5(8) . . . . ? C40 C41 C42 C44 176.6(5) . . . . ? Gd1 O12 C44 C43 -2.1(9) . . . . ? Gd1 O12 C44 C42 173.7(3) . . . . ? C45 C43 C44 O12 3.0(9) . . . . ? C45 C43 C44 C42 -172.8(5) . . . . ? C38 C42 C44 O12 -35.0(7) . . . . ? C41 C42 C44 O12 147.9(5) . . . . ? C38 C42 C44 C43 141.2(6) . . . . ? C41 C42 C44 C43 -35.9(8) . . . . ? Gd1 O11 C45 C43 12.6(9) . . . . ? Gd1 O11 C45 C46 -165.7(4) . . . . ? C44 C43 C45 O11 -7.9(9) . . . . ? C44 C43 C45 C46 170.2(5) . . . . ? O11 C45 C46 C47 10.3(7) . . . . ? C43 C45 C46 C47 -168.0(5) . . . . ? O11 C45 C46 C51 -168.9(5) . . . . ? C43 C45 C46 C51 12.8(8) . . . . ? C51 C46 C47 C48 0.6(8) . . . . ? C45 C46 C47 C48 -178.6(5) . . . . ? C46 C47 C48 C49 0.3(9) . . . . ? C47 C48 C49 C50 -0.5(10) . . . . ? C48 C49 C50 C51 -0.3(11) . . . . ? C49 C50 C51 C46 1.2(10) . . . . ? C47 C46 C51 C50 -1.4(9) . . . . ? C45 C46 C51 C50 177.8(6) . . . . ? C57 C52 C53 C54 -1.9(12) . . . . ? C52 C53 C54 C55 -0.3(12) . . . . ? C53 C54 C55 C56 1.7(13) . . . . ? C54 C55 C56 C57 -1.0(13) . . . . ? C53 C52 C57 C56 2.6(10) . . . . ? C53 C52 C57 C58 -177.2(6) . . . . ? C55 C56 C57 C52 -1.2(11) . . . . ? C55 C56 C57 C58 178.6(7) . . . . ? Gd1 O9 C58 C59 23.0(9) . . . . ? Gd1 O9 C58 C57 -158.6(4) . . . . ? C52 C57 C58 O9 -22.7(8) . . . . ? C56 C57 C58 O9 157.5(6) . . . . ? C52 C57 C58 C59 155.8(6) . . . . ? C56 C57 C58 C59 -24.0(10) . . . . ? O9 C58 C59 C60 -6.0(10) . . . . ? C57 C58 C59 C60 175.7(6) . . . . ? Gd1 O10 C60 C59 8.6(10) . . . . ? Gd1 O10 C60 C61 -170.8(4) . . . . ? C58 C59 C60 O10 -9.2(10) . . . . ? C58 C59 C60 C61 170.2(6) . . . . ? O10 C60 C61 C66 -165.9(6) . . . . ? C59 C60 C61 C66 14.6(10) . . . . ? O10 C60 C61 C62 14.4(8) . . . . ? C59 C60 C61 C62 -165.0(6) . . . . ? C66 C61 C62 C63 -1.8(10) . . . . ? C60 C61 C62 C63 177.8(6) . . . . ? C61 C62 C63 C64 0.8(10) . . . . ? C62 C63 C64 C65 0.8(12) . . . . ? C63 C64 C65 C66 -1.2(13) . . . . ? C64 C65 C66 C61 0.1(13) . . . . ? C62 C61 C66 C65 1.4(12) . . . . ? C60 C61 C66 C65 -178.3(7) . . . . ? C72 C67 C68 C69 3.5(10) . . . . ? C73 C67 C68 C69 -177.0(6) . . . . ? C67 C68 C69 C70 -1.5(11) . . . . ? C68 C69 C70 C71 -1.1(13) . . . . ? C69 C70 C71 C72 1.4(14) . . . . ? C70 C71 C72 C67 0.7(14) . . . . ? C68 C67 C72 C71 -3.1(12) . . . . ? C73 C67 C72 C71 177.4(7) . . . . ? Ni2 O7 C73 C74 -3.5(8) . . . . ? Ni2 O7 C73 C67 172.4(3) . . . . ? C72 C67 C73 O7 154.1(6) . . . . ? C68 C67 C73 O7 -25.4(8) . . . . ? C72 C67 C73 C74 -29.8(9) . . . . ? C68 C67 C73 C74 150.7(6) . . . . ? O7 C73 C74 C75 -0.3(10) . . . . ? C67 C73 C74 C75 -175.9(5) . . . . ? Ni2 O8 C75 C74 7.3(8) . . . . ? Ni2 O8 C75 C76 -168.7(4) . . . . ? C73 C74 C75 O8 -1.8(10) . . . . ? C73 C74 C75 C76 174.0(6) . . . . ? O8 C75 C76 C79 14.0(8) . . . . ? C74 C75 C76 C79 -162.2(6) . . . . ? O8 C75 C76 C77 -169.0(6) . . . . ? C74 C75 C76 C77 14.8(9) . . . . ? C79 C76 C77 C78 0.7(10) . . . . ? C75 C76 C77 C78 -176.3(7) . . . . ? C76 C77 C78 C81 -1.6(12) . . . . ? C77 C76 C79 C80 1.5(11) . . . . ? C75 C76 C79 C80 178.7(6) . . . . ? C76 C79 C80 C81 -3.0(12) . . . . ? C77 C78 C81 C80 0.1(13) . . . . ? C79 C80 C81 C78 2.1(13) . . . . ? C88A C87 C88 N7 -128(100) . . . . ? C88A C87 C88 N7 130(15) . . . 2_565 ? C88 C87 C88A N7A -139(7) . . . . ? C87 C88 N7 N7 -110(100) . . . 2_565 ? C87 C88 N7 C88 -110(100) . . . 2_565 ? N7 C88 N7 C88 0.00(14) 2_565 . . 2_565 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.466 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 930905' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71.50 H71 N4 Ni O10.50 Tb' _chemical_formula_weight 1371.95 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.408(4) _cell_length_b 15.386(6) _cell_length_c 17.909(7) _cell_angle_alpha 88.542(18) _cell_angle_beta 73.370(15) _cell_angle_gamma 70.398(12) _cell_volume 3325(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9403 _cell_measurement_theta_min 3.0548 _cell_measurement_theta_max 27.3775 _exptl_crystal_description Prism _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1410 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8713 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_decay_% ? _diffrn_reflns_number 20705 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11321 _reflns_number_gt 9133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _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. Atoms c85, c89 and N6 of an acetonitrile molecule experienced serious disorder, and ISOR command was used during the refinement. ; _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^)+(0.0655P)^2^+7.3885P] 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 11321 _refine_ls_number_parameters 831 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.041 _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 Tb1 Tb 0.15144(2) 0.102205(19) 0.227877(15) 0.02244(11) Uani 1 1 d . . . Ni2 Ni 0.11044(6) 0.20753(5) 0.40532(4) 0.02208(18) Uani 1 1 d . . . O5 O 0.2390(3) 0.1268(3) 0.3150(2) 0.0232(9) Uani 1 1 d . . . O6 O 0.3735(3) 0.0436(3) 0.1851(2) 0.0260(9) Uani 1 1 d . . . O7 O 0.1994(3) 0.2694(3) 0.4457(2) 0.0262(9) Uani 1 1 d . . . O8 O 0.0729(3) 0.3154(3) 0.3367(2) 0.0276(9) Uani 1 1 d . . . O9 O 0.2173(3) 0.1909(3) 0.1334(2) 0.0271(9) Uani 1 1 d . . . O10 O -0.0006(3) 0.2050(3) 0.1994(2) 0.0307(10) Uani 1 1 d . . . O11 O 0.1860(3) 0.0144(3) 0.1142(2) 0.0314(10) Uani 1 1 d . . . O12 O 0.2163(3) -0.0511(3) 0.2565(2) 0.0242(9) Uani 1 1 d . . . O13 O 0.0310(3) 0.1491(3) 0.3514(2) 0.0240(9) Uani 1 1 d . . . O14 O -0.0188(3) 0.0390(3) 0.2734(2) 0.0272(9) Uani 1 1 d . . . N3 N 0.1573(4) 0.0959(3) 0.4753(3) 0.0240(11) Uani 1 1 d . . . N4 N -0.0372(4) 0.2613(3) 0.5005(3) 0.0276(11) Uani 1 1 d . . . N5 N 0.3924(9) 0.4074(6) 0.1845(7) 0.123(4) Uani 1 1 d . . . C15 C -0.0420(5) -0.0209(5) 0.2257(4) 0.0324(15) Uani 1 1 d . . . H15A H -0.0907 0.0164 0.1964 0.039 Uiso 1 1 calc R . . H15B H -0.0785 -0.0596 0.2591 0.039 Uiso 1 1 calc R . . H15C H 0.0275 -0.0606 0.1890 0.039 Uiso 1 1 calc R . . C16 C -0.1084(5) 0.0984(4) 0.3301(3) 0.0250(13) Uani 1 1 d . . . C17 C -0.2178(5) 0.1032(4) 0.3460(3) 0.0288(14) Uani 1 1 d . . . H17 H -0.2360 0.0628 0.3172 0.035 Uiso 1 1 calc R . . C18 C -0.3024(5) 0.1680(4) 0.4048(3) 0.0292(14) Uani 1 1 d . . . C19 C -0.2716(5) 0.2247(4) 0.4454(4) 0.0318(14) Uani 1 1 d . . . H19 H -0.3276 0.2685 0.4851 0.038 Uiso 1 1 calc R . . C20 C -0.1614(5) 0.2210(4) 0.4309(3) 0.0281(13) Uani 1 1 d . . . C21 C -0.0773(5) 0.1566(4) 0.3721(3) 0.0258(13) Uani 1 1 d . . . C22 C -0.4229(5) 0.1755(5) 0.4188(4) 0.0396(16) Uani 1 1 d . . . H22A H -0.4658 0.2377 0.4087 0.048 Uiso 1 1 calc R . . H22B H -0.4540 0.1640 0.4732 0.048 Uiso 1 1 calc R . . H22C H -0.4264 0.1295 0.3837 0.048 Uiso 1 1 calc R . . C23 C -0.1386(5) 0.2918(4) 0.4735(4) 0.0322(14) Uani 1 1 d . . . H23A H -0.1341 0.3424 0.4389 0.039 Uiso 1 1 calc R . . H23B H -0.2035 0.3185 0.5199 0.039 Uiso 1 1 calc R . . C24 C -0.0392(6) 0.3443(5) 0.5443(4) 0.0399(17) Uani 1 1 d . . . H24A H -0.1081 0.3668 0.5875 0.060 Uiso 1 1 calc R . . H24B H -0.0350 0.3933 0.5088 0.060 Uiso 1 1 calc R . . H24C H 0.0242 0.3269 0.5653 0.060 Uiso 1 1 calc R . . C25 C -0.0337(5) 0.1849(4) 0.5529(3) 0.0303(14) Uani 1 1 d . . . H25A H -0.0622 0.1408 0.5340 0.036 Uiso 1 1 calc R . . H25B H -0.0822 0.2103 0.6062 0.036 Uiso 1 1 calc R . . C26 C 0.0840(5) 0.1341(4) 0.5557(3) 0.0301(14) Uani 1 1 d . . . H26A H 0.1117 0.1773 0.5768 0.036 Uiso 1 1 calc R . . H26B H 0.0846 0.0831 0.5907 0.036 Uiso 1 1 calc R . . C27 C 0.1426(5) 0.0100(4) 0.4536(3) 0.0265(13) Uani 1 1 d . . . H27A H 0.1660 -0.0374 0.4886 0.040 Uiso 1 1 calc R . . H27B H 0.1876 -0.0120 0.3996 0.040 Uiso 1 1 calc R . . H27C H 0.0643 0.0224 0.4582 0.040 Uiso 1 1 calc R . . C28 C 0.2760(5) 0.0736(4) 0.4716(3) 0.0264(13) Uani 1 1 d . . . H28A H 0.2940 0.0270 0.5093 0.032 Uiso 1 1 calc R . . H28B H 0.2860 0.1302 0.4883 0.032 Uiso 1 1 calc R . . C29 C 0.3574(5) 0.0368(4) 0.3914(3) 0.0251(13) Uani 1 1 d . . . C30 C 0.4624(5) -0.0284(4) 0.3872(4) 0.0282(13) Uani 1 1 d . . . H30 H 0.4795 -0.0457 0.4345 0.034 Uiso 1 1 calc R . . C31 C 0.5426(5) -0.0687(4) 0.3163(4) 0.0313(14) Uani 1 1 d . . . C32 C 0.6560(6) -0.1369(5) 0.3155(4) 0.0463(18) Uani 1 1 d . . . H32A H 0.7139 -0.1132 0.2859 0.056 Uiso 1 1 calc R . . H32B H 0.6671 -0.1969 0.2908 0.056 Uiso 1 1 calc R . . H32C H 0.6597 -0.1443 0.3693 0.056 Uiso 1 1 calc R . . C33 C 0.5149(5) -0.0461(4) 0.2468(4) 0.0267(13) Uani 1 1 d . . . H33 H 0.5662 -0.0748 0.1981 0.032 Uiso 1 1 calc R . . C34 C 0.4124(5) 0.0183(4) 0.2493(3) 0.0258(13) Uani 1 1 d . . . C35 C 0.3343(5) 0.0634(4) 0.3199(3) 0.0243(13) Uani 1 1 d . . . C36 C 0.4464(5) 0.0059(5) 0.1095(3) 0.0327(15) Uani 1 1 d . . . H36A H 0.4685 -0.0617 0.1069 0.039 Uiso 1 1 calc R . . H36B H 0.5123 0.0238 0.0995 0.039 Uiso 1 1 calc R . . H36C H 0.4085 0.0297 0.0700 0.039 Uiso 1 1 calc R . . C37 C 0.4089(5) -0.2852(4) 0.3443(3) 0.0297(14) Uani 1 1 d . . . H37 H 0.4501 -0.2808 0.3784 0.036 Uiso 1 1 calc R . . C38 C 0.3556(5) -0.2067(4) 0.3104(3) 0.0255(13) Uani 1 1 d . . . H38 H 0.3590 -0.1484 0.3231 0.031 Uiso 1 1 calc R . . C39 C 0.4002(5) -0.3694(4) 0.3269(4) 0.0331(15) Uani 1 1 d . . . H39 H 0.4357 -0.4231 0.3495 0.040 Uiso 1 1 calc R . . C40 C 0.3405(5) -0.3761(4) 0.2771(4) 0.0322(15) Uani 1 1 d . . . H40 H 0.3342 -0.4339 0.2664 0.039 Uiso 1 1 calc R . . C41 C 0.2900(5) -0.2986(4) 0.2429(3) 0.0272(13) Uani 1 1 d . . . H41 H 0.2497 -0.3035 0.2083 0.033 Uiso 1 1 calc R . . C42 C 0.2981(4) -0.2128(4) 0.2590(3) 0.0224(12) Uani 1 1 d . . . C43 C 0.2597(5) -0.1433(4) 0.1382(3) 0.0271(13) Uani 1 1 d . . . H43A H 0.2855 -0.2053 0.1163 0.032 Uiso 1 1 calc R . . C44 C 0.2519(5) -0.1288(4) 0.2183(3) 0.0268(13) Uani 1 1 d . . . C45 C 0.2317(5) -0.0719(4) 0.0896(3) 0.0250(13) Uani 1 1 d . . . C46 C 0.2602(5) -0.0934(5) 0.0030(3) 0.0296(14) Uani 1 1 d . . . C47 C 0.2550(5) -0.0225(5) -0.0475(4) 0.0376(16) Uani 1 1 d . . . H47 H 0.2346 0.0393 -0.0267 0.045 Uiso 1 1 calc R . . C48 C 0.2788(6) -0.0403(6) -0.1265(4) 0.0456(19) Uani 1 1 d . . . H48 H 0.2754 0.0088 -0.1601 0.055 Uiso 1 1 calc R . . C49 C 0.3076(6) -0.1298(6) -0.1571(4) 0.0471(19) Uani 1 1 d . . . H49 H 0.3228 -0.1419 -0.2117 0.057 Uiso 1 1 calc R . . C50 C 0.3145(6) -0.2009(6) -0.1096(4) 0.052(2) Uani 1 1 d . . . H50 H 0.3355 -0.2624 -0.1313 0.063 Uiso 1 1 calc R . . C51 C 0.2910(6) -0.1836(5) -0.0302(4) 0.0436(18) Uani 1 1 d . . . H51 H 0.2958 -0.2335 0.0026 0.052 Uiso 1 1 calc R . . C52 C 0.3668(5) 0.2495(5) 0.0198(4) 0.0358(15) Uani 1 1 d . . . H52 H 0.3851 0.2296 0.0663 0.043 Uiso 1 1 calc R . . C53 C 0.4455(6) 0.2672(5) -0.0431(4) 0.0460(18) Uani 1 1 d . . . H53 H 0.5165 0.2603 -0.0384 0.055 Uiso 1 1 calc R . . C54 C 0.4219(6) 0.2941(5) -0.1111(5) 0.049(2) Uani 1 1 d . . . H54 H 0.4756 0.3067 -0.1534 0.059 Uiso 1 1 calc R . . C55 C 0.3192(7) 0.3028(6) -0.1174(5) 0.059(2) Uani 1 1 d . . . H55 H 0.3023 0.3203 -0.1648 0.071 Uiso 1 1 calc R . . C56 C 0.2403(6) 0.2861(6) -0.0551(5) 0.058(2) Uani 1 1 d . . . H56 H 0.1698 0.2922 -0.0603 0.069 Uiso 1 1 calc R . . C57 C 0.2628(5) 0.2608(5) 0.0144(4) 0.0346(15) Uani 1 1 d . . . C58 C 0.1775(5) 0.2428(4) 0.0847(4) 0.0303(14) Uani 1 1 d . . . C59 C 0.0656(5) 0.2849(5) 0.0937(4) 0.0356(16) Uani 1 1 d . . . H59A H 0.0446 0.3276 0.0570 0.043 Uiso 1 1 calc R . . C60 C -0.0189(5) 0.2690(4) 0.1530(4) 0.0293(14) Uani 1 1 d . . . C61 C -0.1401(5) 0.3270(4) 0.1664(4) 0.0338(15) Uani 1 1 d . . . C62 C -0.2167(5) 0.3231(5) 0.2380(4) 0.0338(15) Uani 1 1 d . . . H62 H -0.1926 0.2828 0.2752 0.041 Uiso 1 1 calc R . . C63 C -0.3277(6) 0.3783(5) 0.2541(4) 0.0437(18) Uani 1 1 d . . . H63 H -0.3790 0.3749 0.3023 0.052 Uiso 1 1 calc R . . C64 C -0.3643(6) 0.4380(6) 0.2009(5) 0.059(2) Uani 1 1 d . . . H64 H -0.4398 0.4766 0.2127 0.071 Uiso 1 1 calc R . . C65 C -0.2887(7) 0.4408(6) 0.1296(6) 0.074(3) Uani 1 1 d . . . H65 H -0.3133 0.4809 0.0924 0.089 Uiso 1 1 calc R . . C66 C -0.1763(6) 0.3848(6) 0.1121(5) 0.055(2) Uani 1 1 d . . . H66 H -0.1256 0.3867 0.0632 0.066 Uiso 1 1 calc R . . C67 C 0.2651(5) 0.3819(4) 0.4785(4) 0.0265(13) Uani 1 1 d . . . C68 C 0.2700(6) 0.3464(5) 0.5508(4) 0.0364(16) Uani 1 1 d . . . H68 H 0.2399 0.2991 0.5680 0.044 Uiso 1 1 calc R . . C69 C 0.3182(6) 0.3794(5) 0.5974(4) 0.0399(16) Uani 1 1 d . . . H69 H 0.3182 0.3558 0.6469 0.048 Uiso 1 1 calc R . . C70 C 0.3654(6) 0.4449(5) 0.5738(5) 0.0451(18) Uani 1 1 d . . . H70 H 0.3978 0.4670 0.6065 0.054 Uiso 1 1 calc R . . C71 C 0.3656(7) 0.4792(5) 0.5009(5) 0.057(2) Uani 1 1 d . . . H71 H 0.3997 0.5241 0.4835 0.068 Uiso 1 1 calc R . . C72 C 0.3163(6) 0.4482(5) 0.4532(5) 0.0456(19) Uani 1 1 d . . . H72 H 0.3173 0.4718 0.4036 0.055 Uiso 1 1 calc R . . C73 C 0.2061(5) 0.3495(4) 0.4315(3) 0.0256(13) Uani 1 1 d . . . C74 C 0.1601(5) 0.4075(4) 0.3797(4) 0.0288(14) Uani 1 1 d . . . H74A H 0.1741 0.4642 0.3727 0.035 Uiso 1 1 calc R . . C75 C 0.0951(5) 0.3897(4) 0.3372(4) 0.0273(13) Uani 1 1 d . . . C76 C 0.0419(6) 0.4647(4) 0.2899(4) 0.0377(16) Uani 1 1 d . . . C77 C 0.0683(10) 0.5428(7) 0.2756(6) 0.086(4) Uani 1 1 d . . . H77A H 0.1278 0.5489 0.2912 0.104 Uiso 1 1 calc R . . C78 C 0.0098(11) 0.6142(8) 0.2383(7) 0.105(5) Uani 1 1 d . . . H78A H 0.0281 0.6689 0.2303 0.126 Uiso 1 1 calc R . . C79 C -0.0486(5) 0.4622(4) 0.2699(4) 0.0342(15) Uani 1 1 d . . . H79 H -0.0747 0.4122 0.2847 0.041 Uiso 1 1 calc R . . C80 C -0.1028(6) 0.5292(5) 0.2294(5) 0.0487(19) Uani 1 1 d . . . H80 H -0.1609 0.5220 0.2126 0.058 Uiso 1 1 calc R . . C81 C -0.0743(10) 0.6053(7) 0.2132(7) 0.088(4) Uani 1 1 d . . . H81 H -0.1116 0.6518 0.1850 0.106 Uiso 1 1 calc R . . C82 C 0.3891(7) 0.2492(5) 0.2384(4) 0.054(2) Uani 1 1 d . . . H82A H 0.3251 0.2369 0.2314 0.064 Uiso 1 1 calc R . . H82B H 0.3839 0.2508 0.2941 0.064 Uiso 1 1 calc R . . H82C H 0.4574 0.2001 0.2096 0.064 Uiso 1 1 calc R . . C83 C 0.3905(7) 0.3383(6) 0.2089(5) 0.061(2) Uani 1 1 d . . . N6 N 0.9361(13) 0.8145(8) 0.1151(9) 0.057(4) Uani 0.50 1 d PU . . C86 C 1.0152(10) 0.8731(10) -0.0100(10) 0.056(5) Uani 0.50 1 d P . . H86A H 0.9586 0.8927 -0.0375 0.084 Uiso 0.50 1 calc PR . . H86B H 1.0808 0.8244 -0.0425 0.084 Uiso 0.50 1 calc PR . . H86C H 1.0356 0.9261 0.0003 0.084 Uiso 0.50 1 calc PR . . C85 C 0.9734(14) 0.8393(9) 0.0602(11) 0.044(4) Uani 0.50 1 d PU . . C87 C 0.1747(11) 0.4865(7) 0.0744(7) 0.029(3) Uani 0.50 1 d P . . H87A H 0.1137 0.4961 0.0518 0.043 Uiso 0.50 1 calc PR . . H87B H 0.1549 0.4655 0.1270 0.043 Uiso 0.50 1 calc PR . . H87C H 0.2417 0.4396 0.0414 0.043 Uiso 0.50 1 calc PR . . C88 C 0.1948(13) 0.5718(11) 0.0789(9) 0.049(4) Uani 0.50 1 d P . . C89 C 0.522(2) 0.4690(15) -0.0028(18) 0.088(7) Uani 0.50 1 d PU . . N7 N 0.224(2) 0.6354(10) 0.0766(7) 0.104(8) Uani 0.50 1 d P . . O15 O 0.622(2) 0.415(2) -0.0528(9) 0.185(13) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02226(17) 0.02210(16) 0.02135(16) 0.00327(11) -0.00693(12) -0.00526(12) Ni2 0.0264(4) 0.0186(4) 0.0216(4) 0.0013(3) -0.0057(3) -0.0094(3) O5 0.023(2) 0.022(2) 0.024(2) 0.0026(17) -0.0094(17) -0.0057(17) O6 0.024(2) 0.028(2) 0.023(2) 0.0077(17) -0.0090(17) -0.0029(18) O7 0.034(2) 0.018(2) 0.033(2) 0.0049(17) -0.0142(19) -0.0129(18) O8 0.031(2) 0.022(2) 0.033(2) 0.0053(18) -0.0118(19) -0.0122(19) O9 0.025(2) 0.030(2) 0.026(2) 0.0109(18) -0.0084(18) -0.0095(18) O10 0.024(2) 0.030(2) 0.037(2) 0.007(2) -0.0104(19) -0.0062(19) O11 0.033(2) 0.036(2) 0.028(2) 0.0047(19) -0.0122(19) -0.014(2) O12 0.026(2) 0.019(2) 0.022(2) -0.0003(16) -0.0066(17) -0.0009(17) O13 0.023(2) 0.019(2) 0.035(2) 0.0035(17) -0.0164(18) -0.0077(17) O14 0.029(2) 0.027(2) 0.027(2) -0.0035(18) -0.0085(18) -0.0100(19) N3 0.031(3) 0.023(2) 0.021(2) 0.000(2) -0.006(2) -0.015(2) N4 0.034(3) 0.024(3) 0.024(3) 0.000(2) -0.003(2) -0.013(2) N5 0.131(9) 0.056(6) 0.151(10) -0.025(6) 0.038(7) -0.055(6) C15 0.031(3) 0.040(4) 0.032(3) -0.006(3) -0.011(3) -0.018(3) C16 0.027(3) 0.023(3) 0.025(3) 0.007(2) -0.010(3) -0.008(3) C17 0.033(3) 0.031(3) 0.026(3) 0.006(3) -0.013(3) -0.012(3) C18 0.024(3) 0.036(3) 0.024(3) 0.010(3) -0.006(3) -0.007(3) C19 0.026(3) 0.032(3) 0.028(3) 0.005(3) 0.000(3) -0.006(3) C20 0.030(3) 0.028(3) 0.021(3) 0.003(2) -0.002(3) -0.008(3) C21 0.031(3) 0.024(3) 0.023(3) 0.003(2) -0.007(3) -0.011(3) C22 0.025(3) 0.047(4) 0.042(4) 0.005(3) -0.009(3) -0.006(3) C23 0.031(3) 0.027(3) 0.033(3) -0.002(3) -0.004(3) -0.007(3) C24 0.042(4) 0.035(4) 0.036(4) -0.012(3) 0.000(3) -0.013(3) C25 0.036(4) 0.032(3) 0.019(3) -0.003(3) 0.003(3) -0.016(3) C26 0.044(4) 0.028(3) 0.021(3) 0.002(3) -0.008(3) -0.017(3) C27 0.033(3) 0.020(3) 0.028(3) 0.002(2) -0.007(3) -0.011(3) C28 0.035(3) 0.026(3) 0.027(3) 0.008(3) -0.017(3) -0.015(3) C29 0.030(3) 0.025(3) 0.029(3) 0.008(2) -0.011(3) -0.017(3) C30 0.033(3) 0.028(3) 0.029(3) 0.012(3) -0.019(3) -0.011(3) C31 0.025(3) 0.027(3) 0.042(4) 0.010(3) -0.016(3) -0.005(3) C32 0.036(4) 0.048(4) 0.050(4) 0.016(4) -0.019(3) -0.003(3) C33 0.022(3) 0.027(3) 0.030(3) 0.007(3) -0.008(3) -0.008(3) C34 0.023(3) 0.021(3) 0.032(3) 0.006(3) -0.007(3) -0.007(3) C35 0.030(3) 0.024(3) 0.028(3) 0.012(2) -0.017(3) -0.015(3) C36 0.021(3) 0.046(4) 0.024(3) -0.001(3) -0.002(3) -0.006(3) C37 0.028(3) 0.033(3) 0.021(3) 0.004(3) -0.006(3) -0.002(3) C38 0.025(3) 0.022(3) 0.024(3) 0.001(2) -0.002(2) -0.004(3) C39 0.034(4) 0.024(3) 0.031(3) 0.009(3) -0.009(3) 0.001(3) C40 0.036(4) 0.024(3) 0.030(3) 0.001(3) -0.003(3) -0.009(3) C41 0.023(3) 0.029(3) 0.026(3) -0.005(3) -0.003(3) -0.007(3) C42 0.019(3) 0.019(3) 0.022(3) 0.001(2) -0.001(2) -0.003(2) C43 0.029(3) 0.023(3) 0.023(3) -0.006(2) -0.003(3) -0.004(3) C44 0.021(3) 0.031(3) 0.028(3) 0.003(3) -0.008(3) -0.008(3) C45 0.020(3) 0.032(3) 0.025(3) 0.001(3) -0.006(2) -0.011(3) C46 0.020(3) 0.047(4) 0.023(3) 0.002(3) -0.009(3) -0.012(3) C47 0.031(4) 0.059(5) 0.032(4) 0.010(3) -0.012(3) -0.026(3) C48 0.037(4) 0.086(6) 0.027(4) 0.020(4) -0.015(3) -0.034(4) C49 0.031(4) 0.075(6) 0.024(4) -0.005(4) -0.004(3) -0.007(4) C50 0.052(5) 0.057(5) 0.031(4) -0.015(4) -0.018(4) 0.010(4) C51 0.044(4) 0.047(4) 0.031(4) -0.006(3) -0.017(3) 0.002(3) C52 0.028(3) 0.038(4) 0.037(4) 0.007(3) -0.006(3) -0.009(3) C53 0.027(4) 0.053(5) 0.048(4) 0.007(4) -0.002(3) -0.009(3) C54 0.033(4) 0.039(4) 0.055(5) 0.014(4) 0.010(4) -0.006(3) C55 0.049(5) 0.082(6) 0.039(4) 0.033(4) -0.009(4) -0.019(5) C56 0.035(4) 0.083(6) 0.053(5) 0.034(5) -0.015(4) -0.017(4) C57 0.037(4) 0.036(4) 0.033(4) 0.013(3) -0.014(3) -0.012(3) C58 0.035(4) 0.026(3) 0.035(4) 0.009(3) -0.012(3) -0.016(3) C59 0.026(3) 0.038(4) 0.041(4) 0.022(3) -0.015(3) -0.006(3) C60 0.030(3) 0.029(3) 0.029(3) 0.000(3) -0.015(3) -0.004(3) C61 0.028(3) 0.031(3) 0.040(4) 0.004(3) -0.018(3) 0.000(3) C62 0.027(3) 0.035(4) 0.038(4) -0.010(3) -0.009(3) -0.007(3) C63 0.032(4) 0.042(4) 0.048(4) -0.016(3) -0.007(3) -0.003(3) C64 0.029(4) 0.060(5) 0.070(6) -0.020(5) -0.018(4) 0.012(4) C65 0.049(5) 0.052(5) 0.097(8) 0.007(5) -0.033(5) 0.021(4) C66 0.036(4) 0.062(5) 0.058(5) 0.020(4) -0.021(4) 0.000(4) C67 0.025(3) 0.017(3) 0.036(3) 0.003(2) -0.009(3) -0.005(2) C68 0.046(4) 0.038(4) 0.032(4) 0.001(3) -0.014(3) -0.021(3) C69 0.047(4) 0.048(4) 0.030(4) 0.000(3) -0.018(3) -0.016(4) C70 0.051(5) 0.039(4) 0.059(5) 0.001(4) -0.039(4) -0.014(4) C71 0.070(6) 0.049(5) 0.086(6) 0.033(4) -0.053(5) -0.042(4) C72 0.055(5) 0.050(4) 0.056(5) 0.026(4) -0.033(4) -0.035(4) C73 0.030(3) 0.022(3) 0.026(3) 0.000(2) -0.008(3) -0.010(3) C74 0.034(3) 0.024(3) 0.038(4) 0.012(3) -0.017(3) -0.016(3) C75 0.025(3) 0.022(3) 0.031(3) 0.000(3) -0.006(3) -0.006(3) C76 0.048(4) 0.029(3) 0.053(4) 0.017(3) -0.034(4) -0.018(3) C77 0.140(10) 0.073(6) 0.119(9) 0.067(6) -0.111(8) -0.073(7) C78 0.177(13) 0.082(7) 0.135(10) 0.070(7) -0.119(10) -0.088(8) C79 0.031(3) 0.029(3) 0.047(4) 0.004(3) -0.020(3) -0.008(3) C80 0.047(4) 0.037(4) 0.064(5) 0.004(4) -0.033(4) -0.002(4) C81 0.140(10) 0.059(6) 0.116(9) 0.041(6) -0.103(9) -0.046(7) C82 0.052(5) 0.057(5) 0.047(5) 0.000(4) 0.001(4) -0.026(4) C83 0.059(5) 0.044(5) 0.068(6) -0.021(4) 0.017(4) -0.031(4) N6 0.096(8) 0.028(6) 0.064(7) -0.007(5) -0.057(6) -0.014(5) C86 0.009(6) 0.060(10) 0.087(12) -0.065(10) -0.019(7) 0.013(6) C85 0.052(7) 0.020(6) 0.062(8) -0.024(6) -0.038(6) 0.004(5) C87 0.045(8) 0.013(5) 0.027(6) 0.000(5) -0.015(6) -0.004(5) C88 0.052(9) 0.051(10) 0.039(8) 0.002(7) -0.015(7) -0.008(8) C89 0.089(11) 0.089(11) 0.100(11) 0.003(9) -0.037(8) -0.040(9) N7 0.26(3) 0.040(8) 0.026(7) 0.009(6) -0.028(11) -0.079(13) O15 0.30(3) 0.37(4) 0.054(10) 0.107(16) -0.101(15) -0.30(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O13 2.297(4) . ? Tb1 O10 2.303(4) . ? Tb1 O5 2.309(4) . ? Tb1 O9 2.312(4) . ? Tb1 O11 2.316(4) . ? Tb1 O12 2.323(4) . ? Tb1 O6 2.682(4) . ? Tb1 O14 2.685(4) . ? Tb1 Ni2 3.4193(14) . ? Ni2 O7 2.035(4) . ? Ni2 O13 2.038(4) . ? Ni2 O5 2.050(4) . ? Ni2 O8 2.051(4) . ? Ni2 N3 2.130(5) . ? Ni2 N4 2.133(5) . ? O5 C35 1.347(7) . ? O6 C34 1.389(7) . ? O6 C36 1.424(7) . ? O7 C73 1.280(7) . ? O8 C75 1.276(7) . ? O9 C58 1.276(7) . ? O10 C60 1.279(7) . ? O11 C45 1.288(7) . ? O12 C44 1.265(7) . ? O13 C21 1.357(7) . ? O14 C16 1.386(7) . ? O14 C15 1.435(7) . ? N3 C27 1.477(7) . ? N3 C28 1.494(7) . ? N3 C26 1.494(7) . ? N4 C25 1.482(7) . ? N4 C23 1.496(8) . ? N4 C24 1.505(8) . ? N5 C83 1.145(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.388(8) . ? C16 C21 1.417(8) . ? C17 C18 1.414(8) . ? C17 H17 0.9500 . ? C18 C19 1.381(9) . ? C18 C22 1.528(8) . ? C19 C20 1.406(9) . ? C19 H19 0.9500 . ? C20 C21 1.409(8) . ? C20 C23 1.503(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.523(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.518(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.409(8) . ? C29 C35 1.423(8) . ? C30 C31 1.401(9) . ? C30 H30 0.9500 . ? C31 C33 1.402(8) . ? C31 C32 1.526(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.389(8) . ? C33 H33 0.9500 . ? C34 C35 1.405(8) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.392(9) . ? C37 C38 1.403(8) . ? C37 H37 0.9500 . ? C38 C42 1.383(8) . ? C38 H38 0.9500 . ? C39 C40 1.383(9) . ? C39 H39 0.9500 . ? C40 C41 1.384(9) . ? C40 H40 0.9500 . ? C41 C42 1.404(8) . ? C41 H41 0.9500 . ? C42 C44 1.503(8) . ? C43 C45 1.403(8) . ? C43 C44 1.426(8) . ? C43 H43A 0.9500 . ? C45 C46 1.503(8) . ? C46 C47 1.397(9) . ? C46 C51 1.402(9) . ? C47 C48 1.372(9) . ? C47 H47 0.9500 . ? C48 C49 1.381(11) . ? C48 H48 0.9500 . ? C49 C50 1.364(11) . ? C49 H49 0.9500 . ? C50 C51 1.379(9) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C57 1.378(9) . ? C52 C53 1.397(9) . ? C52 H52 0.9500 . ? C53 C54 1.365(10) . ? C53 H53 0.9500 . ? C54 C55 1.376(11) . ? C54 H54 0.9500 . ? C55 C56 1.387(10) . ? C55 H55 0.9500 . ? C56 C57 1.379(10) . ? C56 H56 0.9500 . ? C57 C58 1.529(9) . ? C58 C59 1.384(9) . ? C59 C60 1.398(9) . ? C59 H59A 0.9500 . ? C60 C61 1.519(8) . ? C61 C66 1.382(9) . ? C61 C62 1.408(9) . ? C62 C63 1.392(9) . ? C62 H62 0.9500 . ? C63 C64 1.384(11) . ? C63 H63 0.9500 . ? C64 C65 1.394(12) . ? C64 H64 0.9500 . ? C65 C66 1.409(10) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.402(9) . ? C67 C72 1.408(9) . ? C67 C73 1.500(8) . ? C68 C69 1.387(9) . ? C68 H68 0.9500 . ? C69 C70 1.359(10) . ? C69 H69 0.9500 . ? C70 C71 1.396(10) . ? C70 H70 0.9500 . ? C71 C72 1.396(10) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.398(8) . ? C74 C75 1.401(8) . ? C74 H74A 0.9500 . ? C75 C76 1.516(9) . ? C76 C77 1.362(10) . ? C76 C79 1.373(9) . ? C77 C78 1.397(12) . ? C77 H77A 0.9500 . ? C78 C81 1.374(13) . ? C78 H78A 0.9500 . ? C79 C80 1.371(9) . ? C79 H79 0.9500 . ? C80 C81 1.350(11) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 C83 1.461(11) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? N6 C85 1.09(2) . ? C86 C85 1.39(2) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.43(2) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 N7 1.17(2) . ? C89 C89 0.93(4) 2_665 ? C89 O15 1.37(4) . ? 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 O13 Tb1 O10 79.33(14) . . ? O13 Tb1 O5 68.10(13) . . ? O10 Tb1 O5 127.65(14) . . ? O13 Tb1 O9 128.76(14) . . ? O10 Tb1 O9 73.32(14) . . ? O5 Tb1 O9 96.15(14) . . ? O13 Tb1 O11 143.21(14) . . ? O10 Tb1 O11 88.07(15) . . ? O5 Tb1 O11 141.16(14) . . ? O9 Tb1 O11 78.49(15) . . ? O13 Tb1 O12 93.14(13) . . ? O10 Tb1 O12 139.42(14) . . ? O5 Tb1 O12 83.76(13) . . ? O9 Tb1 O12 134.91(14) . . ? O11 Tb1 O12 74.35(14) . . ? O13 Tb1 O6 127.73(12) . . ? O10 Tb1 O6 142.70(13) . . ? O5 Tb1 O6 60.89(13) . . ? O9 Tb1 O6 69.52(13) . . ? O11 Tb1 O6 81.63(14) . . ? O12 Tb1 O6 71.44(13) . . ? O13 Tb1 O14 61.93(12) . . ? O10 Tb1 O14 70.58(14) . . ? O5 Tb1 O14 121.36(13) . . ? O9 Tb1 O14 138.90(13) . . ? O11 Tb1 O14 81.30(13) . . ? O12 Tb1 O14 70.77(13) . . ? O6 Tb1 O14 141.46(12) . . ? O13 Tb1 Ni2 35.34(9) . . ? O10 Tb1 Ni2 97.31(11) . . ? O5 Tb1 Ni2 35.71(10) . . ? O9 Tb1 Ni2 107.00(11) . . ? O11 Tb1 Ni2 173.20(10) . . ? O12 Tb1 Ni2 98.85(10) . . ? O6 Tb1 Ni2 96.40(9) . . ? O14 Tb1 Ni2 96.52(8) . . ? O7 Ni2 O13 172.85(16) . . ? O7 Ni2 O5 96.87(16) . . ? O13 Ni2 O5 78.23(16) . . ? O7 Ni2 O8 89.03(16) . . ? O13 Ni2 O8 86.01(16) . . ? O5 Ni2 O8 92.39(16) . . ? O7 Ni2 N3 88.80(17) . . ? O13 Ni2 N3 96.00(17) . . ? O5 Ni2 N3 86.15(17) . . ? O8 Ni2 N3 177.22(17) . . ? O7 Ni2 N4 95.50(18) . . ? O13 Ni2 N4 90.15(18) . . ? O5 Ni2 N4 165.07(17) . . ? O8 Ni2 N4 96.15(18) . . ? N3 Ni2 N4 85.78(19) . . ? O7 Ni2 Tb1 132.86(12) . . ? O13 Ni2 Tb1 40.68(11) . . ? O5 Ni2 Tb1 41.11(11) . . ? O8 Ni2 Tb1 75.97(12) . . ? N3 Ni2 Tb1 104.31(13) . . ? N4 Ni2 Tb1 129.96(14) . . ? C35 O5 Ni2 127.1(3) . . ? C35 O5 Tb1 121.1(3) . . ? Ni2 O5 Tb1 103.18(16) . . ? C34 O6 C36 118.2(4) . . ? C34 O6 Tb1 110.8(3) . . ? C36 O6 Tb1 126.4(3) . . ? C73 O7 Ni2 127.0(4) . . ? C75 O8 Ni2 126.8(4) . . ? C58 O9 Tb1 134.3(4) . . ? C60 O10 Tb1 137.0(4) . . ? C45 O11 Tb1 136.4(4) . . ? C44 O12 Tb1 135.2(4) . . ? C21 O13 Ni2 129.5(4) . . ? C21 O13 Tb1 124.4(3) . . ? Ni2 O13 Tb1 103.99(16) . . ? C16 O14 C15 116.9(5) . . ? C16 O14 Tb1 112.5(3) . . ? C15 O14 Tb1 124.9(3) . . ? C27 N3 C28 108.1(4) . . ? C27 N3 C26 110.5(4) . . ? C28 N3 C26 110.3(4) . . ? C27 N3 Ni2 115.0(4) . . ? C28 N3 Ni2 109.6(3) . . ? C26 N3 Ni2 103.3(3) . . ? C25 N4 C23 113.1(5) . . ? C25 N4 C24 108.9(5) . . ? C23 N4 C24 106.5(5) . . ? C25 N4 Ni2 104.4(3) . . ? C23 N4 Ni2 111.9(4) . . ? C24 N4 Ni2 112.1(4) . . ? O14 C15 H15A 109.5 . . ? O14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O14 C16 C17 125.8(5) . . ? O14 C16 C21 112.5(5) . . ? C17 C16 C21 121.7(6) . . ? C16 C17 C18 120.4(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 117.6(6) . . ? C19 C18 C22 122.7(6) . . ? C17 C18 C22 119.6(6) . . ? C18 C19 C20 123.3(6) . . ? C18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C19 C20 C21 119.0(6) . . ? C19 C20 C23 118.7(5) . . ? C21 C20 C23 122.0(6) . . ? O13 C21 C20 124.1(5) . . ? O13 C21 C16 117.9(5) . . ? C20 C21 C16 117.9(6) . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C20 118.3(5) . . ? N4 C23 H23A 107.7 . . ? C20 C23 H23A 107.7 . . ? N4 C23 H23B 107.7 . . ? C20 C23 H23B 107.7 . . ? H23A C23 H23B 107.1 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C26 111.1(5) . . ? N4 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? N4 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? N3 C26 C25 109.5(5) . . ? N3 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? N3 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 114.4(5) . . ? N3 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? N3 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C30 C29 C35 117.6(5) . . ? C30 C29 C28 118.3(5) . . ? C35 C29 C28 124.1(5) . . ? C31 C30 C29 123.1(5) . . ? C31 C30 H30 118.5 . . ? C29 C30 H30 118.5 . . ? C30 C31 C33 118.2(5) . . ? C30 C31 C32 120.6(6) . . ? C33 C31 C32 121.2(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C31 119.9(6) . . ? C34 C33 H33 120.1 . . ? C31 C33 H33 120.1 . . ? C33 C34 O6 125.3(5) . . ? C33 C34 C35 122.1(5) . . ? O6 C34 C35 112.5(5) . . ? O5 C35 C34 117.0(5) . . ? O5 C35 C29 124.1(5) . . ? C34 C35 C29 118.8(5) . . ? O6 C36 H36A 109.5 . . ? O6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 118.5(6) . . ? C39 C37 H37 120.7 . . ? C38 C37 H37 120.7 . . ? C42 C38 C37 121.1(6) . . ? C42 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C40 C39 C37 120.9(6) . . ? C40 C39 H39 119.5 . . ? C37 C39 H39 119.5 . . ? C39 C40 C41 120.0(6) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C40 C41 C42 120.3(6) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C38 C42 C41 119.1(5) . . ? C38 C42 C44 119.0(5) . . ? C41 C42 C44 121.8(5) . . ? C45 C43 C44 124.2(5) . . ? C45 C43 H43A 117.9 . . ? C44 C43 H43A 117.9 . . ? O12 C44 C43 125.7(5) . . ? O12 C44 C42 117.1(5) . . ? C43 C44 C42 117.0(5) . . ? O11 C45 C43 123.6(5) . . ? O11 C45 C46 116.2(5) . . ? C43 C45 C46 120.1(5) . . ? C47 C46 C51 117.4(6) . . ? C47 C46 C45 120.2(6) . . ? C51 C46 C45 122.3(6) . . ? C48 C47 C46 121.3(7) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C47 C48 C49 119.7(7) . . ? C47 C48 H48 120.1 . . ? C49 C48 H48 120.1 . . ? C50 C49 C48 120.6(7) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 120.0(7) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C46 121.0(7) . . ? C50 C51 H51 119.5 . . ? C46 C51 H51 119.5 . . ? C57 C52 C53 120.2(7) . . ? C57 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 121.0(7) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 C55 118.9(7) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C54 C55 C56 120.5(7) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C57 C56 C55 120.9(7) . . ? C57 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? C52 C57 C56 118.5(6) . . ? C52 C57 C58 119.1(6) . . ? C56 C57 C58 122.5(6) . . ? O9 C58 C59 124.5(6) . . ? O9 C58 C57 115.5(5) . . ? C59 C58 C57 120.0(6) . . ? C58 C59 C60 124.6(6) . . ? C58 C59 H59A 117.7 . . ? C60 C59 H59A 117.7 . . ? O10 C60 C59 123.0(6) . . ? O10 C60 C61 115.1(6) . . ? C59 C60 C61 121.9(6) . . ? C66 C61 C62 119.5(6) . . ? C66 C61 C60 122.2(6) . . ? C62 C61 C60 118.2(6) . . ? C63 C62 C61 120.1(7) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C64 C63 C62 120.8(7) . . ? C64 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C63 C64 C65 119.0(7) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? C64 C65 C66 120.8(8) . . ? C64 C65 H65 119.6 . . ? C66 C65 H65 119.6 . . ? C61 C66 C65 119.7(8) . . ? C61 C66 H66 120.2 . . ? C65 C66 H66 120.2 . . ? C68 C67 C72 117.6(6) . . ? C68 C67 C73 119.9(5) . . ? C72 C67 C73 122.5(6) . . ? C69 C68 C67 120.9(6) . . ? C69 C68 H68 119.5 . . ? C67 C68 H68 119.5 . . ? C70 C69 C68 121.5(7) . . ? C70 C69 H69 119.3 . . ? C68 C69 H69 119.3 . . ? C69 C70 C71 119.0(6) . . ? C69 C70 H70 120.5 . . ? C71 C70 H70 120.5 . . ? C72 C71 C70 120.7(7) . . ? C72 C71 H71 119.6 . . ? C70 C71 H71 119.6 . . ? C71 C72 C67 120.2(7) . . ? C71 C72 H72 119.9 . . ? C67 C72 H72 119.9 . . ? O7 C73 C74 125.4(5) . . ? O7 C73 C67 114.6(5) . . ? C74 C73 C67 119.9(5) . . ? C73 C74 C75 126.0(5) . . ? C73 C74 H74A 117.0 . . ? C75 C74 H74A 117.0 . . ? O8 C75 C74 125.2(6) . . ? O8 C75 C76 115.9(5) . . ? C74 C75 C76 118.9(5) . . ? C77 C76 C79 116.5(7) . . ? C77 C76 C75 123.4(6) . . ? C79 C76 C75 119.4(6) . . ? C76 C77 C78 121.3(8) . . ? C76 C77 H77A 119.3 . . ? C78 C77 H77A 119.3 . . ? C81 C78 C77 120.1(9) . . ? C81 C78 H78A 119.9 . . ? C77 C78 H78A 119.9 . . ? C80 C79 C76 122.5(7) . . ? C80 C79 H79 118.8 . . ? C76 C79 H79 118.8 . . ? C81 C80 C79 120.5(7) . . ? C81 C80 H80 119.8 . . ? C79 C80 H80 119.8 . . ? C80 C81 C78 118.6(8) . . ? C80 C81 H81 120.7 . . ? C78 C81 H81 120.7 . . ? C83 C82 H82A 109.5 . . ? C83 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C83 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N5 C83 C82 178.9(10) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N6 C85 C86 176.9(18) . . ? C88 C87 H87A 109.5 . . ? C88 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C88 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N7 C88 C87 171.6(19) . . ? C89 C89 O15 136(5) 2_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Tb1 Ni2 O7 -175.6(2) . . . . ? O10 Tb1 Ni2 O7 -115.85(18) . . . . ? O5 Tb1 Ni2 O7 35.4(2) . . . . ? O9 Tb1 Ni2 O7 -41.12(18) . . . . ? O11 Tb1 Ni2 O7 102.1(9) . . . . ? O12 Tb1 Ni2 O7 101.51(18) . . . . ? O6 Tb1 Ni2 O7 29.37(17) . . . . ? O14 Tb1 Ni2 O7 172.98(17) . . . . ? O10 Tb1 Ni2 O13 59.75(19) . . . . ? O5 Tb1 Ni2 O13 -149.0(2) . . . . ? O9 Tb1 Ni2 O13 134.48(19) . . . . ? O11 Tb1 Ni2 O13 -82.3(9) . . . . ? O12 Tb1 Ni2 O13 -82.90(19) . . . . ? O6 Tb1 Ni2 O13 -155.03(18) . . . . ? O14 Tb1 Ni2 O13 -11.42(18) . . . . ? O13 Tb1 Ni2 O5 149.0(2) . . . . ? O10 Tb1 Ni2 O5 -151.24(19) . . . . ? O9 Tb1 Ni2 O5 -76.51(19) . . . . ? O11 Tb1 Ni2 O5 66.7(9) . . . . ? O12 Tb1 Ni2 O5 66.12(19) . . . . ? O6 Tb1 Ni2 O5 -6.02(18) . . . . ? O14 Tb1 Ni2 O5 137.59(18) . . . . ? O13 Tb1 Ni2 O8 -100.4(2) . . . . ? O10 Tb1 Ni2 O8 -40.66(16) . . . . ? O5 Tb1 Ni2 O8 110.6(2) . . . . ? O9 Tb1 Ni2 O8 34.07(16) . . . . ? O11 Tb1 Ni2 O8 177.3(9) . . . . ? O12 Tb1 Ni2 O8 176.70(15) . . . . ? O6 Tb1 Ni2 O8 104.57(14) . . . . ? O14 Tb1 Ni2 O8 -111.83(15) . . . . ? O13 Tb1 Ni2 N3 82.4(2) . . . . ? O10 Tb1 Ni2 N3 142.19(17) . . . . ? O5 Tb1 Ni2 N3 -66.6(2) . . . . ? O9 Tb1 Ni2 N3 -143.08(17) . . . . ? O11 Tb1 Ni2 N3 0.1(9) . . . . ? O12 Tb1 Ni2 N3 -0.45(17) . . . . ? O6 Tb1 Ni2 N3 -72.58(16) . . . . ? O14 Tb1 Ni2 N3 71.02(16) . . . . ? O13 Tb1 Ni2 N4 -14.1(2) . . . . ? O10 Tb1 Ni2 N4 45.6(2) . . . . ? O5 Tb1 Ni2 N4 -163.2(2) . . . . ? O9 Tb1 Ni2 N4 120.3(2) . . . . ? O11 Tb1 Ni2 N4 -96.4(9) . . . . ? O12 Tb1 Ni2 N4 -97.0(2) . . . . ? O6 Tb1 Ni2 N4 -169.17(19) . . . . ? O14 Tb1 Ni2 N4 -25.56(19) . . . . ? O7 Ni2 O5 C35 57.9(4) . . . . ? O13 Ni2 O5 C35 -127.3(4) . . . . ? O8 Ni2 O5 C35 147.2(4) . . . . ? N3 Ni2 O5 C35 -30.4(4) . . . . ? N4 Ni2 O5 C35 -87.8(8) . . . . ? Tb1 Ni2 O5 C35 -147.4(5) . . . . ? O7 Ni2 O5 Tb1 -154.68(16) . . . . ? O13 Ni2 O5 Tb1 20.05(15) . . . . ? O8 Ni2 O5 Tb1 -65.37(17) . . . . ? N3 Ni2 O5 Tb1 117.00(18) . . . . ? N4 Ni2 O5 Tb1 59.6(7) . . . . ? O13 Tb1 O5 C35 131.1(4) . . . . ? O10 Tb1 O5 C35 -173.1(4) . . . . ? O9 Tb1 O5 C35 -99.4(4) . . . . ? O11 Tb1 O5 C35 -20.1(5) . . . . ? O12 Tb1 O5 C35 35.2(4) . . . . ? O6 Tb1 O5 C35 -37.0(4) . . . . ? O14 Tb1 O5 C35 98.2(4) . . . . ? Ni2 Tb1 O5 C35 149.9(5) . . . . ? O13 Tb1 O5 Ni2 -18.72(14) . . . . ? O10 Tb1 O5 Ni2 37.1(2) . . . . ? O9 Tb1 O5 Ni2 110.72(16) . . . . ? O11 Tb1 O5 Ni2 -170.01(17) . . . . ? O12 Tb1 O5 Ni2 -114.65(17) . . . . ? O6 Tb1 O5 Ni2 173.1(2) . . . . ? O14 Tb1 O5 Ni2 -51.7(2) . . . . ? O13 Tb1 O6 C34 17.6(4) . . . . ? O10 Tb1 O6 C34 146.6(3) . . . . ? O5 Tb1 O6 C34 31.6(3) . . . . ? O9 Tb1 O6 C34 141.4(4) . . . . ? O11 Tb1 O6 C34 -137.8(3) . . . . ? O12 Tb1 O6 C34 -61.6(3) . . . . ? O14 Tb1 O6 C34 -73.3(4) . . . . ? Ni2 Tb1 O6 C34 35.6(3) . . . . ? O13 Tb1 O6 C36 173.0(4) . . . . ? O10 Tb1 O6 C36 -58.0(5) . . . . ? O5 Tb1 O6 C36 -173.0(5) . . . . ? O9 Tb1 O6 C36 -63.2(4) . . . . ? O11 Tb1 O6 C36 17.5(4) . . . . ? O12 Tb1 O6 C36 93.8(5) . . . . ? O14 Tb1 O6 C36 82.1(5) . . . . ? Ni2 Tb1 O6 C36 -169.0(4) . . . . ? O13 Ni2 O7 C73 52.3(15) . . . . ? O5 Ni2 O7 C73 98.6(5) . . . . ? O8 Ni2 O7 C73 6.3(5) . . . . ? N3 Ni2 O7 C73 -175.4(5) . . . . ? N4 Ni2 O7 C73 -89.8(5) . . . . ? Tb1 Ni2 O7 C73 76.1(5) . . . . ? O7 Ni2 O8 C75 -7.0(5) . . . . ? O13 Ni2 O8 C75 178.2(5) . . . . ? O5 Ni2 O8 C75 -103.8(5) . . . . ? N3 Ni2 O8 C75 -46(4) . . . . ? N4 Ni2 O8 C75 88.4(5) . . . . ? Tb1 Ni2 O8 C75 -141.8(5) . . . . ? O13 Tb1 O9 C58 -78.6(6) . . . . ? O10 Tb1 O9 C58 -17.9(5) . . . . ? O5 Tb1 O9 C58 -145.4(5) . . . . ? O11 Tb1 O9 C58 73.6(5) . . . . ? O12 Tb1 O9 C58 127.3(5) . . . . ? O6 Tb1 O9 C58 158.8(6) . . . . ? O14 Tb1 O9 C58 11.5(6) . . . . ? Ni2 Tb1 O9 C58 -110.6(5) . . . . ? O13 Tb1 O10 C60 137.6(6) . . . . ? O5 Tb1 O10 C60 86.3(6) . . . . ? O9 Tb1 O10 C60 1.4(5) . . . . ? O11 Tb1 O10 C60 -77.1(6) . . . . ? O12 Tb1 O10 C60 -140.1(5) . . . . ? O6 Tb1 O10 C60 -3.7(7) . . . . ? O14 Tb1 O10 C60 -158.6(6) . . . . ? Ni2 Tb1 O10 C60 107.1(6) . . . . ? O13 Tb1 O11 C45 -82.0(6) . . . . ? O10 Tb1 O11 C45 -151.3(5) . . . . ? O5 Tb1 O11 C45 49.9(6) . . . . ? O9 Tb1 O11 C45 135.4(5) . . . . ? O12 Tb1 O11 C45 -8.3(5) . . . . ? O6 Tb1 O11 C45 64.7(5) . . . . ? O14 Tb1 O11 C45 -80.6(5) . . . . ? Ni2 Tb1 O11 C45 -8.9(13) . . . . ? O13 Tb1 O12 C44 147.9(5) . . . . ? O10 Tb1 O12 C44 70.7(6) . . . . ? O5 Tb1 O12 C44 -144.5(5) . . . . ? O9 Tb1 O12 C44 -52.1(6) . . . . ? O11 Tb1 O12 C44 3.1(5) . . . . ? O6 Tb1 O12 C44 -83.2(5) . . . . ? O14 Tb1 O12 C44 89.1(5) . . . . ? Ni2 Tb1 O12 C44 -177.0(5) . . . . ? O7 Ni2 O13 C21 -136.6(12) . . . . ? O5 Ni2 O13 C21 176.3(5) . . . . ? O8 Ni2 O13 C21 -90.4(4) . . . . ? N3 Ni2 O13 C21 91.5(4) . . . . ? N4 Ni2 O13 C21 5.7(5) . . . . ? Tb1 Ni2 O13 C21 -163.5(5) . . . . ? O7 Ni2 O13 Tb1 26.9(13) . . . . ? O5 Ni2 O13 Tb1 -20.23(15) . . . . ? O8 Ni2 O13 Tb1 73.05(17) . . . . ? N3 Ni2 O13 Tb1 -105.02(18) . . . . ? N4 Ni2 O13 Tb1 169.21(18) . . . . ? O10 Tb1 O13 C21 45.3(4) . . . . ? O5 Tb1 O13 C21 -176.5(4) . . . . ? O9 Tb1 O13 C21 103.5(4) . . . . ? O11 Tb1 O13 C21 -26.7(5) . . . . ? O12 Tb1 O13 C21 -94.5(4) . . . . ? O6 Tb1 O13 C21 -163.4(4) . . . . ? O14 Tb1 O13 C21 -28.3(4) . . . . ? Ni2 Tb1 O13 C21 164.6(5) . . . . ? O10 Tb1 O13 Ni2 -119.32(18) . . . . ? O5 Tb1 O13 Ni2 18.90(14) . . . . ? O9 Tb1 O13 Ni2 -61.0(2) . . . . ? O11 Tb1 O13 Ni2 168.70(18) . . . . ? O12 Tb1 O13 Ni2 100.89(16) . . . . ? O6 Tb1 O13 Ni2 32.0(2) . . . . ? O14 Tb1 O13 Ni2 167.1(2) . . . . ? O13 Tb1 O14 C16 26.3(3) . . . . ? O10 Tb1 O14 C16 -61.7(3) . . . . ? O5 Tb1 O14 C16 61.3(4) . . . . ? O9 Tb1 O14 C16 -91.6(4) . . . . ? O11 Tb1 O14 C16 -152.7(4) . . . . ? O12 Tb1 O14 C16 130.9(4) . . . . ? O6 Tb1 O14 C16 142.7(3) . . . . ? Ni2 Tb1 O14 C16 33.8(3) . . . . ? O13 Tb1 O14 C15 178.8(5) . . . . ? O10 Tb1 O14 C15 90.7(4) . . . . ? O5 Tb1 O14 C15 -146.3(4) . . . . ? O9 Tb1 O14 C15 60.9(5) . . . . ? O11 Tb1 O14 C15 -0.3(4) . . . . ? O12 Tb1 O14 C15 -76.7(4) . . . . ? O6 Tb1 O14 C15 -64.9(5) . . . . ? Ni2 Tb1 O14 C15 -173.8(4) . . . . ? O7 Ni2 N3 C27 -162.6(4) . . . . ? O13 Ni2 N3 C27 12.1(4) . . . . ? O5 Ni2 N3 C27 -65.7(4) . . . . ? O8 Ni2 N3 C27 -124(3) . . . . ? N4 Ni2 N3 C27 101.8(4) . . . . ? Tb1 Ni2 N3 C27 -28.5(4) . . . . ? O7 Ni2 N3 C28 -40.6(3) . . . . ? O13 Ni2 N3 C28 134.1(3) . . . . ? O5 Ni2 N3 C28 56.4(3) . . . . ? O8 Ni2 N3 C28 -2(4) . . . . ? N4 Ni2 N3 C28 -136.2(4) . . . . ? Tb1 Ni2 N3 C28 93.6(3) . . . . ? O7 Ni2 N3 C26 77.0(3) . . . . ? O13 Ni2 N3 C26 -108.4(3) . . . . ? O5 Ni2 N3 C26 173.9(3) . . . . ? O8 Ni2 N3 C26 116(3) . . . . ? N4 Ni2 N3 C26 -18.7(3) . . . . ? Tb1 Ni2 N3 C26 -148.9(3) . . . . ? O7 Ni2 N4 C25 -98.6(4) . . . . ? O13 Ni2 N4 C25 85.8(4) . . . . ? O5 Ni2 N4 C25 47.2(9) . . . . ? O8 Ni2 N4 C25 171.8(4) . . . . ? N3 Ni2 N4 C25 -10.2(4) . . . . ? Tb1 Ni2 N4 C25 94.9(4) . . . . ? O7 Ni2 N4 C23 138.7(4) . . . . ? O13 Ni2 N4 C23 -36.9(4) . . . . ? O5 Ni2 N4 C23 -75.5(8) . . . . ? O8 Ni2 N4 C23 49.1(4) . . . . ? N3 Ni2 N4 C23 -132.9(4) . . . . ? Tb1 Ni2 N4 C23 -27.8(4) . . . . ? O7 Ni2 N4 C24 19.1(4) . . . . ? O13 Ni2 N4 C24 -156.5(4) . . . . ? O5 Ni2 N4 C24 165.0(6) . . . . ? O8 Ni2 N4 C24 -70.5(4) . . . . ? N3 Ni2 N4 C24 107.5(4) . . . . ? Tb1 Ni2 N4 C24 -147.3(4) . . . . ? C15 O14 C16 C17 1.7(8) . . . . ? Tb1 O14 C16 C17 156.5(5) . . . . ? C15 O14 C16 C21 -178.1(5) . . . . ? Tb1 O14 C16 C21 -23.3(6) . . . . ? O14 C16 C17 C18 -179.0(5) . . . . ? C21 C16 C17 C18 0.8(9) . . . . ? C16 C17 C18 C19 -0.5(9) . . . . ? C16 C17 C18 C22 177.2(6) . . . . ? C17 C18 C19 C20 0.1(9) . . . . ? C22 C18 C19 C20 -177.5(6) . . . . ? C18 C19 C20 C21 0.1(9) . . . . ? C18 C19 C20 C23 174.4(6) . . . . ? Ni2 O13 C21 C20 11.0(8) . . . . ? Tb1 O13 C21 C20 -149.4(5) . . . . ? Ni2 O13 C21 C16 -171.5(4) . . . . ? Tb1 O13 C21 C16 28.1(7) . . . . ? C19 C20 C21 O13 177.6(5) . . . . ? C23 C20 C21 O13 3.5(9) . . . . ? C19 C20 C21 C16 0.1(8) . . . . ? C23 C20 C21 C16 -174.0(5) . . . . ? O14 C16 C21 O13 1.6(7) . . . . ? C17 C16 C21 O13 -178.2(5) . . . . ? O14 C16 C21 C20 179.3(5) . . . . ? C17 C16 C21 C20 -0.5(9) . . . . ? C25 N4 C23 C20 -57.4(7) . . . . ? C24 N4 C23 C20 -177.0(5) . . . . ? Ni2 N4 C23 C20 60.2(6) . . . . ? C19 C20 C23 N4 141.9(6) . . . . ? C21 C20 C23 N4 -43.9(8) . . . . ? C23 N4 C25 C26 160.0(5) . . . . ? C24 N4 C25 C26 -81.7(6) . . . . ? Ni2 N4 C25 C26 38.1(5) . . . . ? C27 N3 C26 C25 -78.9(6) . . . . ? C28 N3 C26 C25 161.6(5) . . . . ? Ni2 N3 C26 C25 44.5(5) . . . . ? N4 C25 C26 N3 -59.0(6) . . . . ? C27 N3 C28 C29 60.8(6) . . . . ? C26 N3 C28 C29 -178.3(5) . . . . ? Ni2 N3 C28 C29 -65.2(5) . . . . ? N3 C28 C29 C30 -147.3(5) . . . . ? N3 C28 C29 C35 32.2(8) . . . . ? C35 C29 C30 C31 -1.3(9) . . . . ? C28 C29 C30 C31 178.2(6) . . . . ? C29 C30 C31 C33 -3.0(9) . . . . ? C29 C30 C31 C32 178.4(6) . . . . ? C30 C31 C33 C34 3.3(9) . . . . ? C32 C31 C33 C34 -178.0(6) . . . . ? C31 C33 C34 O6 -177.2(5) . . . . ? C31 C33 C34 C35 0.7(9) . . . . ? C36 O6 C34 C33 -4.6(8) . . . . ? Tb1 O6 C34 C33 153.1(5) . . . . ? C36 O6 C34 C35 177.3(5) . . . . ? Tb1 O6 C34 C35 -25.0(5) . . . . ? Ni2 O5 C35 C34 -177.9(4) . . . . ? Tb1 O5 C35 C34 39.9(6) . . . . ? Ni2 O5 C35 C29 5.3(8) . . . . ? Tb1 O5 C35 C29 -137.0(5) . . . . ? C33 C34 C35 O5 177.9(5) . . . . ? O6 C34 C35 O5 -4.0(7) . . . . ? C33 C34 C35 C29 -5.1(9) . . . . ? O6 C34 C35 C29 173.0(5) . . . . ? C30 C29 C35 O5 -178.0(5) . . . . ? C28 C29 C35 O5 2.5(9) . . . . ? C30 C29 C35 C34 5.3(8) . . . . ? C28 C29 C35 C34 -174.2(5) . . . . ? C39 C37 C38 C42 -1.9(9) . . . . ? C38 C37 C39 C40 0.2(9) . . . . ? C37 C39 C40 C41 1.1(9) . . . . ? C39 C40 C41 C42 -0.6(9) . . . . ? C37 C38 C42 C41 2.4(8) . . . . ? C37 C38 C42 C44 -174.1(5) . . . . ? C40 C41 C42 C38 -1.1(8) . . . . ? C40 C41 C42 C44 175.2(5) . . . . ? Tb1 O12 C44 C43 -1.6(9) . . . . ? Tb1 O12 C44 C42 173.3(4) . . . . ? C45 C43 C44 O12 2.1(10) . . . . ? C45 C43 C44 C42 -172.8(5) . . . . ? C38 C42 C44 O12 -35.2(8) . . . . ? C41 C42 C44 O12 148.4(5) . . . . ? C38 C42 C44 C43 140.2(6) . . . . ? C41 C42 C44 C43 -36.2(8) . . . . ? Tb1 O11 C45 C43 11.6(9) . . . . ? Tb1 O11 C45 C46 -165.2(4) . . . . ? C44 C43 C45 O11 -6.8(9) . . . . ? C44 C43 C45 C46 169.9(5) . . . . ? O11 C45 C46 C47 11.0(8) . . . . ? C43 C45 C46 C47 -166.0(6) . . . . ? O11 C45 C46 C51 -168.0(6) . . . . ? C43 C45 C46 C51 15.0(9) . . . . ? C51 C46 C47 C48 0.2(9) . . . . ? C45 C46 C47 C48 -178.8(6) . . . . ? C46 C47 C48 C49 0.5(10) . . . . ? C47 C48 C49 C50 -1.1(11) . . . . ? C48 C49 C50 C51 0.9(12) . . . . ? C49 C50 C51 C46 -0.2(12) . . . . ? C47 C46 C51 C50 -0.4(10) . . . . ? C45 C46 C51 C50 178.7(6) . . . . ? C57 C52 C53 C54 -1.2(11) . . . . ? C52 C53 C54 C55 -0.7(12) . . . . ? C53 C54 C55 C56 1.2(13) . . . . ? C54 C55 C56 C57 0.1(14) . . . . ? C53 C52 C57 C56 2.6(11) . . . . ? C53 C52 C57 C58 -178.7(6) . . . . ? C55 C56 C57 C52 -2.0(12) . . . . ? C55 C56 C57 C58 179.3(8) . . . . ? Tb1 O9 C58 C59 23.7(10) . . . . ? Tb1 O9 C58 C57 -159.0(4) . . . . ? C52 C57 C58 O9 -21.9(9) . . . . ? C56 C57 C58 O9 156.8(7) . . . . ? C52 C57 C58 C59 155.6(7) . . . . ? C56 C57 C58 C59 -25.8(10) . . . . ? O9 C58 C59 C60 -6.8(11) . . . . ? C57 C58 C59 C60 175.9(6) . . . . ? Tb1 O10 C60 C59 9.1(10) . . . . ? Tb1 O10 C60 C61 -171.2(4) . . . . ? C58 C59 C60 O10 -9.0(11) . . . . ? C58 C59 C60 C61 171.4(6) . . . . ? O10 C60 C61 C66 -165.7(7) . . . . ? C59 C60 C61 C66 14.0(10) . . . . ? O10 C60 C61 C62 16.3(8) . . . . ? C59 C60 C61 C62 -164.0(6) . . . . ? C66 C61 C62 C63 -1.0(10) . . . . ? C60 C61 C62 C63 177.1(6) . . . . ? C61 C62 C63 C64 -0.6(10) . . . . ? C62 C63 C64 C65 1.5(12) . . . . ? C63 C64 C65 C66 -0.9(14) . . . . ? C62 C61 C66 C65 1.6(12) . . . . ? C60 C61 C66 C65 -176.4(8) . . . . ? C64 C65 C66 C61 -0.6(14) . . . . ? C72 C67 C68 C69 3.5(10) . . . . ? C73 C67 C68 C69 -176.0(6) . . . . ? C67 C68 C69 C70 -2.1(11) . . . . ? C68 C69 C70 C71 -0.3(11) . . . . ? C69 C70 C71 C72 1.2(13) . . . . ? C70 C71 C72 C67 0.3(13) . . . . ? C68 C67 C72 C71 -2.6(11) . . . . ? C73 C67 C72 C71 177.0(7) . . . . ? Ni2 O7 C73 C74 -5.6(9) . . . . ? Ni2 O7 C73 C67 171.7(4) . . . . ? C68 C67 C73 O7 -24.5(8) . . . . ? C72 C67 C73 O7 156.0(6) . . . . ? C68 C67 C73 C74 153.0(6) . . . . ? C72 C67 C73 C74 -26.5(9) . . . . ? O7 C73 C74 C75 2.9(10) . . . . ? C67 C73 C74 C75 -174.3(6) . . . . ? Ni2 O8 C75 C74 6.9(9) . . . . ? Ni2 O8 C75 C76 -170.5(4) . . . . ? C73 C74 C75 O8 -3.6(10) . . . . ? C73 C74 C75 C76 173.8(6) . . . . ? O8 C75 C76 C77 -170.9(8) . . . . ? C74 C75 C76 C77 11.5(12) . . . . ? O8 C75 C76 C79 19.2(9) . . . . ? C74 C75 C76 C79 -158.4(6) . . . . ? C79 C76 C77 C78 -3.5(16) . . . . ? C75 C76 C77 C78 -173.7(10) . . . . ? C76 C77 C78 C81 -2(2) . . . . ? C77 C76 C79 C80 7.4(12) . . . . ? C75 C76 C79 C80 178.0(6) . . . . ? C76 C79 C80 C81 -5.7(13) . . . . ? C79 C80 C81 C78 -0.1(17) . . . . ? C77 C78 C81 C80 4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.442 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 930906' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71.50 H72 Dy N4 Ni O11' _chemical_formula_weight 1384.54 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3097(15) _cell_length_b 15.3831(19) _cell_length_c 17.944(2) _cell_angle_alpha 88.64(5) _cell_angle_beta 73.25(3) _cell_angle_gamma 70.27(4) _cell_volume 3300.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 12040 _cell_measurement_theta_min 2.4791 _cell_measurement_theta_max 31.5022 _exptl_crystal_description Prism _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1422 _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8360 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_decay_% ? _diffrn_reflns_number 33776 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12927 _reflns_number_gt 12335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _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. The acetonitrile and acetone solvents experienced serious disorder and site instability, and therefore bond constraints (DFIX) and ISOR commands were used during the refinement. ; _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^)+(0.0547P)^2^+7.7102P] 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 12927 _refine_ls_number_parameters 838 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.041 _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 Dy1 Dy 0.152139(15) 0.100659(12) 0.227594(10) 0.02232(7) Uani 1 1 d . . . Ni2 Ni 0.10989(4) 0.20753(3) 0.40425(3) 0.02182(12) Uani 1 1 d . . . O5 O 0.2391(2) 0.12658(18) 0.31429(16) 0.0222(6) Uani 1 1 d . . . O6 O 0.3752(2) 0.0432(2) 0.18492(16) 0.0270(6) Uani 1 1 d . . . O7 O 0.1987(2) 0.26904(19) 0.44498(17) 0.0275(6) Uani 1 1 d . . . O8 O 0.0725(2) 0.31589(19) 0.33740(17) 0.0265(6) Uani 1 1 d . . . O9 O 0.2170(2) 0.1893(2) 0.13334(17) 0.0288(6) Uani 1 1 d . . . O10 O -0.0016(2) 0.2029(2) 0.19995(18) 0.0298(7) Uani 1 1 d . . . O11 O 0.1877(2) 0.0122(2) 0.11404(16) 0.0282(6) Uani 1 1 d . . . O12 O 0.2185(2) -0.05284(18) 0.25558(16) 0.0243(6) Uani 1 1 d . . . O13 O 0.0294(2) 0.14858(19) 0.35121(16) 0.0225(6) Uani 1 1 d . . . O14 O -0.0182(2) 0.03752(19) 0.27306(17) 0.0265(6) Uani 1 1 d . . . N3 N 0.1573(3) 0.0959(2) 0.47350(19) 0.0241(7) Uani 1 1 d . . . N4 N -0.0384(3) 0.2616(2) 0.4991(2) 0.0271(7) Uani 1 1 d . . . N5 N 0.3807(6) 0.4113(4) 0.1838(4) 0.090(2) Uani 1 1 d . . . C15 C -0.0407(4) -0.0235(3) 0.2262(3) 0.0347(10) Uani 1 1 d . . . H15A H -0.0895 0.0130 0.1965 0.042 Uiso 1 1 calc R . . H15B H -0.0777 -0.0616 0.2600 0.042 Uiso 1 1 calc R . . H15C H 0.0297 -0.0637 0.1900 0.042 Uiso 1 1 calc R . . C16 C -0.1086(3) 0.0969(3) 0.3301(2) 0.0237(8) Uani 1 1 d . . . C17 C -0.2181(3) 0.1007(3) 0.3458(2) 0.0267(9) Uani 1 1 d . . . H17 H -0.2357 0.0594 0.3174 0.032 Uiso 1 1 calc R . . C18 C -0.3030(4) 0.1658(3) 0.4036(3) 0.0294(9) Uani 1 1 d . . . C19 C -0.2726(4) 0.2230(3) 0.4445(3) 0.0301(9) Uani 1 1 d . . . H19 H -0.3294 0.2664 0.4846 0.036 Uiso 1 1 calc R . . C20 C -0.1627(3) 0.2201(3) 0.4298(2) 0.0264(8) Uani 1 1 d . . . C21 C -0.0776(3) 0.1561(3) 0.3710(2) 0.0221(8) Uani 1 1 d . . . C22 C -0.4234(4) 0.1735(4) 0.4194(3) 0.0424(12) Uani 1 1 d . . . H22A H -0.4669 0.2357 0.4093 0.051 Uiso 1 1 calc R . . H22B H -0.4536 0.1627 0.4740 0.051 Uiso 1 1 calc R . . H22C H -0.4278 0.1273 0.3850 0.051 Uiso 1 1 calc R . . C23 C -0.1412(4) 0.2924(3) 0.4723(3) 0.0314(9) Uani 1 1 d . . . H23A H -0.1367 0.3428 0.4375 0.038 Uiso 1 1 calc R . . H23B H -0.2068 0.3192 0.5186 0.038 Uiso 1 1 calc R . . C24 C -0.0418(4) 0.3441(3) 0.5423(3) 0.0366(11) Uani 1 1 d . . . H24A H -0.1114 0.3662 0.5855 0.055 Uiso 1 1 calc R . . H24B H -0.0384 0.3932 0.5068 0.055 Uiso 1 1 calc R . . H24C H 0.0222 0.3274 0.5630 0.055 Uiso 1 1 calc R . . C25 C -0.0362(4) 0.1848(3) 0.5507(3) 0.0330(10) Uani 1 1 d . . . H25A H -0.0646 0.1410 0.5310 0.040 Uiso 1 1 calc R . . H25B H -0.0856 0.2097 0.6040 0.040 Uiso 1 1 calc R . . C26 C 0.0823(4) 0.1342(3) 0.5532(2) 0.0308(9) Uani 1 1 d . . . H26A H 0.1095 0.1775 0.5746 0.037 Uiso 1 1 calc R . . H26B H 0.0829 0.0831 0.5879 0.037 Uiso 1 1 calc R . . C27 C 0.1419(4) 0.0098(3) 0.4518(2) 0.0267(9) Uani 1 1 d . . . H27A H 0.1652 -0.0376 0.4867 0.040 Uiso 1 1 calc R . . H27B H 0.1873 -0.0125 0.3978 0.040 Uiso 1 1 calc R . . H27C H 0.0629 0.0228 0.4565 0.040 Uiso 1 1 calc R . . C28 C 0.2770(4) 0.0737(3) 0.4698(2) 0.0268(9) Uani 1 1 d . . . H28A H 0.2952 0.0271 0.5073 0.032 Uiso 1 1 calc R . . H28B H 0.2868 0.1304 0.4864 0.032 Uiso 1 1 calc R . . C29 C 0.3586(4) 0.0369(3) 0.3898(2) 0.0261(8) Uani 1 1 d . . . C30 C 0.4644(4) -0.0287(3) 0.3854(3) 0.0298(9) Uani 1 1 d . . . H30 H 0.4813 -0.0461 0.4327 0.036 Uiso 1 1 calc R . . C31 C 0.5444(4) -0.0686(3) 0.3159(3) 0.0317(10) Uani 1 1 d . . . C32 C 0.6582(4) -0.1374(4) 0.3132(3) 0.0481(13) Uani 1 1 d . . . H32A H 0.7165 -0.1137 0.2836 0.058 Uiso 1 1 calc R . . H32B H 0.6687 -0.1968 0.2879 0.058 Uiso 1 1 calc R . . H32C H 0.6631 -0.1461 0.3665 0.058 Uiso 1 1 calc R . . C33 C 0.5172(3) -0.0465(3) 0.2463(3) 0.0289(9) Uani 1 1 d . . . H33 H 0.5692 -0.0755 0.1976 0.035 Uiso 1 1 calc R . . C34 C 0.4143(3) 0.0177(3) 0.2489(2) 0.0253(8) Uani 1 1 d . . . C35 C 0.3355(3) 0.0633(3) 0.3195(2) 0.0226(8) Uani 1 1 d . . . C36 C 0.4487(4) 0.0037(4) 0.1095(3) 0.0368(10) Uani 1 1 d . . . H36A H 0.4702 -0.0639 0.1077 0.044 Uiso 1 1 calc R . . H36B H 0.5158 0.0208 0.0990 0.044 Uiso 1 1 calc R . . H36C H 0.4108 0.0271 0.0699 0.044 Uiso 1 1 calc R . . C37 C 0.4084(4) -0.2844(3) 0.3445(3) 0.0314(9) Uani 1 1 d . . . H37 H 0.4497 -0.2799 0.3786 0.038 Uiso 1 1 calc R . . C38 C 0.3572(3) -0.2067(3) 0.3105(2) 0.0248(8) Uani 1 1 d . . . H38 H 0.3610 -0.1484 0.3229 0.030 Uiso 1 1 calc R . . C39 C 0.3989(4) -0.3693(3) 0.3287(3) 0.0357(10) Uani 1 1 d . . . H39 H 0.4331 -0.4224 0.3525 0.043 Uiso 1 1 calc R . . C40 C 0.3399(4) -0.3762(3) 0.2784(3) 0.0341(10) Uani 1 1 d . . . H40 H 0.3331 -0.4339 0.2682 0.041 Uiso 1 1 calc R . . C41 C 0.2907(4) -0.2991(3) 0.2427(3) 0.0291(9) Uani 1 1 d . . . H41 H 0.2506 -0.3042 0.2080 0.035 Uiso 1 1 calc R . . C42 C 0.3002(3) -0.2138(3) 0.2581(2) 0.0231(8) Uani 1 1 d . . . C43 C 0.2623(4) -0.1447(3) 0.1380(2) 0.0276(9) Uani 1 1 d . . . H43A H 0.2876 -0.2067 0.1160 0.033 Uiso 1 1 calc R . . C44 C 0.2552(3) -0.1311(3) 0.2173(2) 0.0233(8) Uani 1 1 d . . . C45 C 0.2347(3) -0.0731(3) 0.0898(2) 0.0257(8) Uani 1 1 d . . . C46 C 0.2625(3) -0.0954(3) 0.0038(2) 0.0276(9) Uani 1 1 d . . . C47 C 0.2546(4) -0.0228(4) -0.0450(3) 0.0332(10) Uani 1 1 d . . . H47 H 0.2337 0.0388 -0.0235 0.040 Uiso 1 1 calc R . . C48 C 0.2771(4) -0.0405(4) -0.1251(3) 0.0423(12) Uani 1 1 d . . . H48 H 0.2708 0.0093 -0.1580 0.051 Uiso 1 1 calc R . . C49 C 0.3087(4) -0.1299(4) -0.1569(3) 0.0460(13) Uani 1 1 d . . . H49 H 0.3235 -0.1416 -0.2114 0.055 Uiso 1 1 calc R . . C50 C 0.3188(4) -0.2018(4) -0.1098(3) 0.0461(13) Uani 1 1 d . . . H50 H 0.3415 -0.2634 -0.1319 0.055 Uiso 1 1 calc R . . C51 C 0.2962(4) -0.1853(4) -0.0301(3) 0.0384(11) Uani 1 1 d . . . H51 H 0.3036 -0.2358 0.0019 0.046 Uiso 1 1 calc R . . C52 C 0.3655(4) 0.2486(3) 0.0213(3) 0.0367(10) Uani 1 1 d . . . H52 H 0.3841 0.2280 0.0675 0.044 Uiso 1 1 calc R . . C53 C 0.4439(4) 0.2678(4) -0.0398(3) 0.0475(13) Uani 1 1 d . . . H53 H 0.5152 0.2613 -0.0348 0.057 Uiso 1 1 calc R . . C54 C 0.4187(4) 0.2966(4) -0.1085(3) 0.0485(13) Uani 1 1 d . . . H54 H 0.4715 0.3119 -0.1500 0.058 Uiso 1 1 calc R . . C55 C 0.3162(5) 0.3027(4) -0.1154(3) 0.0536(15) Uani 1 1 d . . . H55 H 0.2996 0.3193 -0.1629 0.064 Uiso 1 1 calc R . . C56 C 0.2368(4) 0.2849(4) -0.0535(3) 0.0447(12) Uani 1 1 d . . . H56 H 0.1659 0.2906 -0.0589 0.054 Uiso 1 1 calc R . . C57 C 0.2599(4) 0.2588(3) 0.0163(3) 0.0311(9) Uani 1 1 d . . . C58 C 0.1772(4) 0.2408(3) 0.0851(3) 0.0289(9) Uani 1 1 d . . . C59 C 0.0626(4) 0.2827(3) 0.0942(3) 0.0362(10) Uani 1 1 d . . . H59A H 0.0403 0.3249 0.0576 0.043 Uiso 1 1 calc R . . C60 C -0.0210(4) 0.2654(3) 0.1546(3) 0.0300(9) Uani 1 1 d . . . C61 C -0.1428(4) 0.3242(3) 0.1686(3) 0.0330(10) Uani 1 1 d . . . C62 C -0.2188(4) 0.3203(3) 0.2391(3) 0.0346(10) Uani 1 1 d . . . H62 H -0.1943 0.2795 0.2760 0.042 Uiso 1 1 calc R . . C63 C -0.3308(4) 0.3759(4) 0.2560(3) 0.0452(13) Uani 1 1 d . . . H63 H -0.3823 0.3739 0.3046 0.054 Uiso 1 1 calc R . . C64 C -0.3669(5) 0.4339(4) 0.2023(4) 0.0531(15) Uani 1 1 d . . . H64 H -0.4436 0.4712 0.2139 0.064 Uiso 1 1 calc R . . C65 C -0.2928(5) 0.4383(4) 0.1320(4) 0.0616(17) Uani 1 1 d . . . H65 H -0.3182 0.4794 0.0956 0.074 Uiso 1 1 calc R . . C66 C -0.1802(4) 0.3823(4) 0.1140(4) 0.0516(14) Uani 1 1 d . . . H66 H -0.1294 0.3839 0.0648 0.062 Uiso 1 1 calc R . . C67 C 0.2648(3) 0.3816(3) 0.4788(2) 0.0256(8) Uani 1 1 d . . . C68 C 0.2672(4) 0.3471(3) 0.5511(3) 0.0353(10) Uani 1 1 d . . . H68 H 0.2342 0.3016 0.5688 0.042 Uiso 1 1 calc R . . C69 C 0.3171(4) 0.3784(4) 0.5973(3) 0.0432(12) Uani 1 1 d . . . H69 H 0.3170 0.3550 0.6468 0.052 Uiso 1 1 calc R . . C70 C 0.3667(5) 0.4433(4) 0.5720(3) 0.0476(14) Uani 1 1 d . . . H70 H 0.4005 0.4651 0.6039 0.057 Uiso 1 1 calc R . . C71 C 0.3671(5) 0.4762(4) 0.5004(4) 0.0622(19) Uani 1 1 d . . . H71 H 0.4025 0.5203 0.4824 0.075 Uiso 1 1 calc R . . C72 C 0.3168(5) 0.4461(4) 0.4539(3) 0.0473(14) Uani 1 1 d . . . H72 H 0.3177 0.4698 0.4045 0.057 Uiso 1 1 calc R . . C73 C 0.2051(3) 0.3485(3) 0.4322(2) 0.0240(8) Uani 1 1 d . . . C74 C 0.1568(3) 0.4088(3) 0.3823(3) 0.0271(9) Uani 1 1 d . . . H74A H 0.1686 0.4665 0.3773 0.032 Uiso 1 1 calc R . . C75 C 0.0925(3) 0.3907(3) 0.3391(2) 0.0252(8) Uani 1 1 d . . . C76 C 0.0381(4) 0.4662(3) 0.2939(3) 0.0305(9) Uani 1 1 d . . . C77 C 0.0656(5) 0.5457(4) 0.2794(3) 0.0424(12) Uani 1 1 d . . . H77 H 0.1253 0.5520 0.2951 0.051 Uiso 1 1 calc R . . C78 C 0.0062(5) 0.6166(4) 0.2418(3) 0.0514(14) Uani 1 1 d . . . H78 H 0.0235 0.6718 0.2343 0.062 Uiso 1 1 calc R . . C79 C -0.0490(4) 0.4598(3) 0.2697(3) 0.0366(11) Uani 1 1 d . . . H79 H -0.0709 0.4070 0.2804 0.044 Uiso 1 1 calc R . . C80 C -0.1051(5) 0.5287(4) 0.2300(3) 0.0488(14) Uani 1 1 d . . . H80 H -0.1633 0.5221 0.2126 0.059 Uiso 1 1 calc R . . C81 C -0.0763(5) 0.6066(4) 0.2160(4) 0.0551(15) Uani 1 1 d . . . H81 H -0.1139 0.6535 0.1883 0.066 Uiso 1 1 calc R . . C82 C 0.3848(5) 0.2536(4) 0.2379(4) 0.0554(15) Uani 1 1 d . . . H82A H 0.3210 0.2396 0.2315 0.067 Uiso 1 1 calc R . . H82B H 0.3800 0.2557 0.2934 0.067 Uiso 1 1 calc R . . H82C H 0.4545 0.2053 0.2088 0.067 Uiso 1 1 calc R . . C83 C 0.3829(5) 0.3423(4) 0.2086(4) 0.0565(16) Uani 1 1 d . . . N6 N 0.9440(12) 0.8139(6) 0.1120(9) 0.080(5) Uani 0.50 1 d P . . C85 C 0.9804(10) 0.8390(7) 0.0564(8) 0.045(3) Uani 0.50 1 d PU . . C86 C 1.0181(7) 0.8742(9) -0.0101(7) 0.058(4) Uani 0.50 1 d P . . H86A H 0.9632 0.8879 -0.0392 0.087 Uiso 0.50 1 calc PR . . H86B H 1.0891 0.8293 -0.0416 0.087 Uiso 0.50 1 calc PR . . H86C H 1.0296 0.9314 0.0016 0.087 Uiso 0.50 1 calc PR . . C87 C 0.1834(8) 0.4883(5) 0.0727(5) 0.0297(19) Uani 0.50 1 d PD . . H87A H 0.1936 0.4701 0.0183 0.045 Uiso 0.50 1 calc PR . . H87B H 0.1058 0.4994 0.1037 0.045 Uiso 0.50 1 calc PR . . H87C H 0.2337 0.4387 0.0938 0.045 Uiso 0.50 1 calc PR . . C88 C 0.2091(11) 0.5732(8) 0.0762(6) 0.061(3) Uani 0.50 1 d PD . . O1W O 0.436(3) 0.5484(13) 0.0301(15) 0.26(2) Uani 0.50 1 d P . . N7 N 0.246(2) 0.6321(11) 0.0738(7) 0.204(15) Uani 0.50 1 d PD . . O15 O 0.0000 0.5000 0.0000 0.187(6) Uani 1 2 d SDU . . C90 C 0.0855(12) 0.5015(11) 0.0415(9) 0.080(4) Uani 0.50 1 d PDU . . 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 Dy1 0.02281(11) 0.02154(11) 0.02138(11) 0.00263(7) -0.00884(8) -0.00427(7) Ni2 0.0269(3) 0.0186(3) 0.0218(3) 0.00094(19) -0.0079(2) -0.0095(2) O5 0.0240(14) 0.0203(14) 0.0239(14) 0.0037(11) -0.0111(11) -0.0064(11) O6 0.0226(14) 0.0318(16) 0.0226(14) 0.0038(12) -0.0074(12) -0.0038(12) O7 0.0374(17) 0.0209(14) 0.0306(16) 0.0051(12) -0.0170(13) -0.0127(12) O8 0.0314(16) 0.0228(15) 0.0296(15) 0.0031(12) -0.0133(13) -0.0112(12) O9 0.0249(15) 0.0328(16) 0.0291(16) 0.0122(12) -0.0118(12) -0.0079(12) O10 0.0220(15) 0.0303(16) 0.0342(17) 0.0093(13) -0.0118(13) -0.0030(12) O11 0.0330(16) 0.0251(15) 0.0250(15) -0.0001(12) -0.0136(13) -0.0040(12) O12 0.0299(15) 0.0205(14) 0.0219(14) 0.0001(11) -0.0103(12) -0.0058(11) O13 0.0222(14) 0.0228(14) 0.0231(14) -0.0017(11) -0.0061(11) -0.0087(11) O14 0.0274(15) 0.0247(15) 0.0285(15) -0.0043(12) -0.0099(12) -0.0087(12) N3 0.0328(19) 0.0200(17) 0.0225(17) 0.0019(13) -0.0092(14) -0.0121(14) N4 0.0335(19) 0.0235(18) 0.0235(17) -0.0015(14) -0.0054(15) -0.0113(15) N5 0.097(5) 0.050(4) 0.112(6) -0.009(3) 0.005(4) -0.041(3) C15 0.031(2) 0.038(3) 0.037(3) -0.010(2) -0.011(2) -0.013(2) C16 0.025(2) 0.023(2) 0.024(2) 0.0035(15) -0.0082(16) -0.0086(16) C17 0.028(2) 0.027(2) 0.030(2) 0.0063(17) -0.0115(18) -0.0127(17) C18 0.026(2) 0.033(2) 0.027(2) 0.0076(17) -0.0066(17) -0.0098(18) C19 0.029(2) 0.030(2) 0.026(2) 0.0016(17) -0.0036(17) -0.0072(18) C20 0.027(2) 0.023(2) 0.025(2) 0.0013(16) -0.0045(17) -0.0060(16) C21 0.026(2) 0.0190(19) 0.0224(19) 0.0038(15) -0.0075(16) -0.0095(16) C22 0.027(2) 0.055(3) 0.044(3) 0.005(2) -0.008(2) -0.015(2) C23 0.029(2) 0.028(2) 0.032(2) -0.0067(18) -0.0023(18) -0.0075(18) C24 0.041(3) 0.030(2) 0.032(2) -0.0138(19) 0.000(2) -0.012(2) C25 0.043(3) 0.034(2) 0.022(2) -0.0013(18) -0.0029(19) -0.019(2) C26 0.043(3) 0.031(2) 0.022(2) 0.0043(17) -0.0088(19) -0.018(2) C27 0.036(2) 0.023(2) 0.026(2) 0.0048(16) -0.0097(18) -0.0168(18) C28 0.035(2) 0.025(2) 0.027(2) 0.0079(16) -0.0167(18) -0.0132(18) C29 0.032(2) 0.021(2) 0.029(2) 0.0048(16) -0.0120(18) -0.0121(17) C30 0.035(2) 0.028(2) 0.037(2) 0.0136(18) -0.024(2) -0.0139(18) C31 0.025(2) 0.029(2) 0.044(3) 0.0096(19) -0.017(2) -0.0090(18) C32 0.034(3) 0.047(3) 0.061(4) 0.019(3) -0.024(3) -0.004(2) C33 0.023(2) 0.028(2) 0.035(2) 0.0063(18) -0.0087(18) -0.0077(17) C34 0.024(2) 0.027(2) 0.028(2) 0.0080(16) -0.0124(17) -0.0088(16) C35 0.0236(19) 0.0204(19) 0.029(2) 0.0075(16) -0.0127(16) -0.0110(16) C36 0.027(2) 0.047(3) 0.028(2) 0.001(2) -0.0050(18) -0.006(2) C37 0.030(2) 0.035(2) 0.027(2) 0.0067(18) -0.0106(18) -0.0069(18) C38 0.027(2) 0.023(2) 0.022(2) 0.0018(15) -0.0064(16) -0.0078(16) C39 0.036(2) 0.029(2) 0.034(2) 0.0100(19) -0.011(2) -0.0019(19) C40 0.036(2) 0.023(2) 0.039(3) 0.0024(18) -0.009(2) -0.0066(18) C41 0.030(2) 0.026(2) 0.031(2) 0.0004(17) -0.0097(18) -0.0079(17) C42 0.0207(19) 0.024(2) 0.0203(19) -0.0001(15) -0.0042(15) -0.0033(15) C43 0.031(2) 0.026(2) 0.023(2) -0.0031(16) -0.0091(17) -0.0051(17) C44 0.0192(19) 0.023(2) 0.026(2) 0.0019(16) -0.0069(16) -0.0049(15) C45 0.0172(19) 0.034(2) 0.025(2) 0.0003(17) -0.0083(16) -0.0063(16) C46 0.024(2) 0.038(2) 0.022(2) 0.0018(17) -0.0095(17) -0.0107(18) C47 0.030(2) 0.050(3) 0.028(2) 0.009(2) -0.0131(19) -0.020(2) C48 0.036(3) 0.071(4) 0.029(2) 0.013(2) -0.015(2) -0.026(3) C49 0.035(3) 0.079(4) 0.020(2) -0.006(2) -0.010(2) -0.012(3) C50 0.044(3) 0.054(3) 0.031(3) -0.015(2) -0.014(2) -0.002(2) C51 0.038(3) 0.043(3) 0.031(2) -0.003(2) -0.016(2) -0.004(2) C52 0.026(2) 0.043(3) 0.035(3) 0.006(2) -0.0096(19) -0.005(2) C53 0.025(2) 0.059(3) 0.051(3) 0.009(3) -0.008(2) -0.009(2) C54 0.033(3) 0.051(3) 0.048(3) 0.010(2) 0.002(2) -0.010(2) C55 0.042(3) 0.077(4) 0.037(3) 0.024(3) -0.011(2) -0.016(3) C56 0.033(3) 0.061(3) 0.042(3) 0.018(2) -0.015(2) -0.015(2) C57 0.030(2) 0.026(2) 0.036(2) 0.0086(18) -0.0118(19) -0.0070(18) C58 0.030(2) 0.028(2) 0.031(2) 0.0071(17) -0.0138(18) -0.0089(17) C59 0.029(2) 0.039(3) 0.041(3) 0.016(2) -0.014(2) -0.009(2) C60 0.027(2) 0.031(2) 0.033(2) 0.0040(18) -0.0147(18) -0.0064(18) C61 0.027(2) 0.028(2) 0.043(3) 0.0038(19) -0.017(2) -0.0023(18) C62 0.028(2) 0.035(3) 0.038(3) -0.002(2) -0.012(2) -0.0059(19) C63 0.030(3) 0.050(3) 0.047(3) -0.014(2) -0.007(2) -0.006(2) C64 0.032(3) 0.044(3) 0.073(4) -0.008(3) -0.022(3) 0.006(2) C65 0.043(3) 0.054(4) 0.080(5) 0.025(3) -0.031(3) 0.002(3) C66 0.032(3) 0.057(4) 0.060(4) 0.019(3) -0.017(3) -0.005(2) C67 0.026(2) 0.0194(19) 0.033(2) 0.0026(16) -0.0146(18) -0.0052(16) C68 0.042(3) 0.036(3) 0.037(3) 0.006(2) -0.018(2) -0.020(2) C69 0.050(3) 0.053(3) 0.038(3) 0.006(2) -0.024(2) -0.023(3) C70 0.056(3) 0.040(3) 0.066(4) 0.006(2) -0.046(3) -0.017(2) C71 0.075(4) 0.062(4) 0.096(5) 0.043(4) -0.064(4) -0.052(3) C72 0.058(3) 0.052(3) 0.061(3) 0.031(3) -0.042(3) -0.037(3) C73 0.024(2) 0.020(2) 0.027(2) 0.0013(16) -0.0086(17) -0.0069(16) C74 0.031(2) 0.019(2) 0.037(2) 0.0054(17) -0.0168(19) -0.0107(17) C75 0.026(2) 0.024(2) 0.026(2) 0.0030(16) -0.0097(17) -0.0072(16) C76 0.035(2) 0.024(2) 0.035(2) 0.0053(18) -0.0170(19) -0.0079(18) C77 0.058(3) 0.041(3) 0.044(3) 0.016(2) -0.031(3) -0.024(2) C78 0.073(4) 0.038(3) 0.055(3) 0.018(2) -0.034(3) -0.023(3) C79 0.037(3) 0.031(2) 0.048(3) 0.009(2) -0.023(2) -0.011(2) C80 0.047(3) 0.040(3) 0.067(4) 0.009(3) -0.038(3) -0.006(2) C81 0.071(4) 0.037(3) 0.062(4) 0.016(3) -0.043(3) -0.005(3) C82 0.051(3) 0.046(3) 0.059(4) -0.005(3) -0.001(3) -0.017(3) C83 0.049(3) 0.046(3) 0.069(4) -0.017(3) 0.002(3) -0.025(3) N6 0.149(12) 0.015(4) 0.125(11) 0.007(5) -0.121(10) -0.021(6) C85 0.065(6) 0.017(4) 0.069(6) -0.011(4) -0.062(5) 0.004(4) C86 0.009(4) 0.080(8) 0.078(8) -0.059(7) -0.009(5) -0.004(4) C87 0.042(5) 0.016(4) 0.019(4) -0.010(3) 0.004(3) -0.003(3) C88 0.075(9) 0.070(9) 0.024(5) -0.002(5) -0.011(5) -0.011(7) O1W 0.52(5) 0.22(2) 0.33(3) 0.22(3) -0.38(4) -0.30(3) N7 0.56(5) 0.097(11) 0.034(7) 0.033(7) -0.092(14) -0.21(2) O15 0.179(9) 0.162(9) 0.199(9) 0.052(7) -0.035(7) -0.052(7) C90 0.089(8) 0.070(7) 0.077(8) 0.020(6) -0.020(6) -0.026(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 Dy1 O10 2.298(3) . ? Dy1 O5 2.301(3) . ? Dy1 O9 2.304(3) . ? Dy1 O13 2.304(3) . ? Dy1 O11 2.317(3) . ? Dy1 O12 2.324(3) . ? Dy1 O14 2.670(3) . ? Dy1 O6 2.670(3) . ? Dy1 Ni2 3.4151(7) . ? Ni2 O7 2.028(3) . ? Ni2 O8 2.038(3) . ? Ni2 O5 2.040(3) . ? Ni2 O13 2.040(3) . ? Ni2 N4 2.123(4) . ? Ni2 N3 2.123(3) . ? O5 C35 1.351(5) . ? O6 C34 1.389(5) . ? O6 C36 1.426(5) . ? O7 C73 1.266(5) . ? O8 C75 1.268(5) . ? O9 C58 1.268(5) . ? O10 C60 1.253(5) . ? O11 C45 1.273(5) . ? O12 C44 1.269(5) . ? O13 C21 1.329(5) . ? O14 C16 1.387(5) . ? O14 C15 1.432(5) . ? N3 C27 1.485(5) . ? N3 C26 1.486(5) . ? N3 C28 1.493(5) . ? N4 C25 1.482(6) . ? N4 C24 1.484(5) . ? N4 C23 1.503(6) . ? N5 C83 1.136(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.383(6) . ? C16 C21 1.414(5) . ? C17 C18 1.402(6) . ? C17 H17 0.9500 . ? C18 C19 1.385(6) . ? C18 C22 1.508(6) . ? C19 C20 1.395(6) . ? C19 H19 0.9500 . ? C20 C21 1.404(6) . ? C20 C23 1.510(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.519(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.511(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C35 1.402(6) . ? C29 C30 1.410(6) . ? C30 C31 1.377(7) . ? C30 H30 0.9500 . ? C31 C33 1.402(6) . ? C31 C32 1.514(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.379(6) . ? C33 H33 0.9500 . ? C34 C35 1.407(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.386(6) . ? C37 C39 1.397(7) . ? C37 H37 0.9500 . ? C38 C42 1.394(5) . ? C38 H38 0.9500 . ? C39 C40 1.382(7) . ? C39 H39 0.9500 . ? C40 C41 1.387(6) . ? C40 H40 0.9500 . ? C41 C42 1.401(6) . ? C41 H41 0.9500 . ? C42 C44 1.485(5) . ? C43 C45 1.401(6) . ? C43 C44 1.413(6) . ? C43 H43A 0.9500 . ? C45 C46 1.498(6) . ? C46 C47 1.397(6) . ? C46 C51 1.397(6) . ? C47 C48 1.395(6) . ? C47 H47 0.9500 . ? C48 C49 1.379(8) . ? C48 H48 0.9500 . ? C49 C50 1.370(8) . ? C49 H49 0.9500 . ? C50 C51 1.384(6) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.383(7) . ? C52 C57 1.389(6) . ? C52 H52 0.9500 . ? C53 C54 1.394(8) . ? C53 H53 0.9500 . ? C54 C55 1.378(8) . ? C54 H54 0.9500 . ? C55 C56 1.389(7) . ? C55 H55 0.9500 . ? C56 C57 1.394(7) . ? C56 H56 0.9500 . ? C57 C58 1.489(6) . ? C58 C59 1.402(6) . ? C59 C60 1.404(6) . ? C59 H59A 0.9500 . ? C60 C61 1.515(6) . ? C61 C62 1.389(7) . ? C61 C66 1.396(7) . ? C62 C63 1.392(6) . ? C62 H62 0.9500 . ? C63 C64 1.375(8) . ? C63 H63 0.9500 . ? C64 C65 1.376(9) . ? C64 H64 0.9500 . ? C65 C66 1.398(7) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C72 1.388(6) . ? C67 C68 1.395(6) . ? C67 C73 1.505(5) . ? C68 C69 1.383(6) . ? C68 H68 0.9500 . ? C69 C70 1.375(7) . ? C69 H69 0.9500 . ? C70 C71 1.369(8) . ? C70 H70 0.9500 . ? C71 C72 1.380(7) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.402(6) . ? C74 C75 1.401(5) . ? C74 H74A 0.9500 . ? C75 C76 1.502(6) . ? C76 C79 1.384(6) . ? C76 C77 1.388(6) . ? C77 C78 1.400(7) . ? C77 H77 0.9500 . ? C78 C81 1.362(8) . ? C78 H78 0.9500 . ? C79 C80 1.388(7) . ? C79 H79 0.9500 . ? C80 C81 1.373(8) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 C83 1.447(8) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? N6 C85 1.100(18) . ? C85 C86 1.332(18) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.464(11) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 N7 1.161(9) . ? O15 C90 1.535(9) 2_565 ? O15 C90 1.535(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Dy1 O5 127.26(10) . . ? O10 Dy1 O9 73.23(10) . . ? O5 Dy1 O9 96.30(10) . . ? O10 Dy1 O13 78.83(10) . . ? O5 Dy1 O13 68.11(9) . . ? O9 Dy1 O13 128.49(10) . . ? O10 Dy1 O11 88.19(10) . . ? O5 Dy1 O11 141.45(10) . . ? O9 Dy1 O11 78.41(11) . . ? O13 Dy1 O11 143.17(10) . . ? O10 Dy1 O12 139.27(10) . . ? O5 Dy1 O12 84.21(9) . . ? O9 Dy1 O12 134.94(10) . . ? O13 Dy1 O12 93.59(10) . . ? O11 Dy1 O12 74.14(10) . . ? O10 Dy1 O14 70.41(10) . . ? O5 Dy1 O14 121.36(9) . . ? O9 Dy1 O14 138.60(9) . . ? O13 Dy1 O14 61.89(9) . . ? O11 Dy1 O14 81.30(10) . . ? O12 Dy1 O14 70.80(9) . . ? O10 Dy1 O6 142.82(10) . . ? O5 Dy1 O6 60.99(9) . . ? O9 Dy1 O6 69.70(9) . . ? O13 Dy1 O6 127.86(9) . . ? O11 Dy1 O6 81.79(10) . . ? O12 Dy1 O6 71.55(9) . . ? O14 Dy1 O6 141.66(9) . . ? O10 Dy1 Ni2 97.02(8) . . ? O5 Dy1 Ni2 35.50(7) . . ? O9 Dy1 Ni2 106.88(8) . . ? O13 Dy1 Ni2 35.51(6) . . ? O11 Dy1 Ni2 173.43(7) . . ? O12 Dy1 Ni2 99.29(7) . . ? O14 Dy1 Ni2 96.64(6) . . ? O6 Dy1 Ni2 96.27(6) . . ? O7 Ni2 O8 88.51(11) . . ? O7 Ni2 O5 97.22(12) . . ? O8 Ni2 O5 92.89(11) . . ? O7 Ni2 O13 173.65(12) . . ? O8 Ni2 O13 87.14(11) . . ? O5 Ni2 O13 78.40(11) . . ? O7 Ni2 N4 95.11(13) . . ? O8 Ni2 N4 95.85(13) . . ? O5 Ni2 N4 165.05(12) . . ? O13 Ni2 N4 89.93(12) . . ? O7 Ni2 N3 88.65(12) . . ? O8 Ni2 N3 176.76(12) . . ? O5 Ni2 N3 85.94(12) . . ? O13 Ni2 N3 95.57(12) . . ? N4 Ni2 N3 85.94(14) . . ? O7 Ni2 Dy1 133.26(9) . . ? O8 Ni2 Dy1 77.08(8) . . ? O5 Ni2 Dy1 40.92(7) . . ? O13 Ni2 Dy1 41.00(8) . . ? N4 Ni2 Dy1 130.09(10) . . ? N3 Ni2 Dy1 103.83(9) . . ? C35 O5 Ni2 126.7(2) . . ? C35 O5 Dy1 121.1(2) . . ? Ni2 O5 Dy1 103.58(11) . . ? C34 O6 C36 117.9(3) . . ? C34 O6 Dy1 110.8(2) . . ? C36 O6 Dy1 126.1(2) . . ? C73 O7 Ni2 127.5(3) . . ? C75 O8 Ni2 127.6(3) . . ? C58 O9 Dy1 134.8(3) . . ? C60 O10 Dy1 137.4(3) . . ? C45 O11 Dy1 136.0(3) . . ? C44 O12 Dy1 135.4(3) . . ? C21 O13 Ni2 130.1(2) . . ? C21 O13 Dy1 124.1(2) . . ? Ni2 O13 Dy1 103.48(11) . . ? C16 O14 C15 117.1(3) . . ? C16 O14 Dy1 112.5(2) . . ? C15 O14 Dy1 125.2(3) . . ? C27 N3 C26 109.8(3) . . ? C27 N3 C28 108.6(3) . . ? C26 N3 C28 111.0(3) . . ? C27 N3 Ni2 114.9(2) . . ? C26 N3 Ni2 102.9(2) . . ? C28 N3 Ni2 109.6(2) . . ? C25 N4 C24 110.1(3) . . ? C25 N4 C23 112.2(3) . . ? C24 N4 C23 105.8(3) . . ? C25 N4 Ni2 104.5(3) . . ? C24 N4 Ni2 112.6(3) . . ? C23 N4 Ni2 111.9(3) . . ? O14 C15 H15A 109.5 . . ? O14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 O14 125.1(4) . . ? C17 C16 C21 122.4(4) . . ? O14 C16 C21 112.5(3) . . ? C16 C17 C18 119.8(4) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 117.9(4) . . ? C19 C18 C22 121.6(4) . . ? C17 C18 C22 120.5(4) . . ? C18 C19 C20 123.2(4) . . ? C18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C19 C20 C21 119.1(4) . . ? C19 C20 C23 118.5(4) . . ? C21 C20 C23 122.2(4) . . ? O13 C21 C20 124.1(3) . . ? O13 C21 C16 118.3(3) . . ? C20 C21 C16 117.6(4) . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C20 117.4(3) . . ? N4 C23 H23A 108.0 . . ? C20 C23 H23A 108.0 . . ? N4 C23 H23B 108.0 . . ? C20 C23 H23B 108.0 . . ? H23A C23 H23B 107.2 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C26 110.1(4) . . ? N4 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? N4 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.2 . . ? N3 C26 C25 110.3(3) . . ? N3 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? N3 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 114.1(3) . . ? N3 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? N3 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C35 C29 C30 117.7(4) . . ? C35 C29 C28 124.1(4) . . ? C30 C29 C28 118.1(4) . . ? C31 C30 C29 123.3(4) . . ? C31 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? C30 C31 C33 118.2(4) . . ? C30 C31 C32 121.9(4) . . ? C33 C31 C32 119.8(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C31 119.6(4) . . ? C34 C33 H33 120.2 . . ? C31 C33 H33 120.2 . . ? C33 C34 O6 125.5(4) . . ? C33 C34 C35 122.1(4) . . ? O6 C34 C35 112.4(3) . . ? O5 C35 C29 124.6(4) . . ? O5 C35 C34 116.5(3) . . ? C29 C35 C34 118.7(4) . . ? O6 C36 H36A 109.5 . . ? O6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 119.8(4) . . ? C38 C37 H37 120.1 . . ? C39 C37 H37 120.1 . . ? C37 C38 C42 120.2(4) . . ? C37 C38 H38 119.9 . . ? C42 C38 H38 119.9 . . ? C40 C39 C37 120.1(4) . . ? C40 C39 H39 119.9 . . ? C37 C39 H39 119.9 . . ? C39 C40 C41 120.3(4) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C42 119.9(4) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C38 C42 C41 119.5(4) . . ? C38 C42 C44 118.8(4) . . ? C41 C42 C44 121.6(4) . . ? C45 C43 C44 124.5(4) . . ? C45 C43 H43A 117.8 . . ? C44 C43 H43A 117.8 . . ? O12 C44 C43 125.0(4) . . ? O12 C44 C42 116.8(3) . . ? C43 C44 C42 118.1(4) . . ? O11 C45 C43 124.1(4) . . ? O11 C45 C46 116.2(4) . . ? C43 C45 C46 119.7(4) . . ? C47 C46 C51 118.2(4) . . ? C47 C46 C45 118.6(4) . . ? C51 C46 C45 123.2(4) . . ? C48 C47 C46 120.3(5) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C49 C48 C47 120.2(5) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C50 C49 C48 120.1(4) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.4(5) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C50 C51 C46 120.8(5) . . ? C50 C51 H51 119.6 . . ? C46 C51 H51 119.6 . . ? C53 C52 C57 121.2(5) . . ? C53 C52 H52 119.4 . . ? C57 C52 H52 119.4 . . ? C52 C53 C54 120.2(5) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C55 C54 C53 119.0(5) . . ? C55 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? C54 C55 C56 120.7(5) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C55 C56 C57 120.7(5) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C52 C57 C56 118.1(4) . . ? C52 C57 C58 118.9(4) . . ? C56 C57 C58 123.0(4) . . ? O9 C58 C59 124.2(4) . . ? O9 C58 C57 116.2(4) . . ? C59 C58 C57 119.6(4) . . ? C58 C59 C60 123.4(4) . . ? C58 C59 H59A 118.3 . . ? C60 C59 H59A 118.3 . . ? O10 C60 C59 123.8(4) . . ? O10 C60 C61 115.9(4) . . ? C59 C60 C61 120.4(4) . . ? C62 C61 C66 119.4(4) . . ? C62 C61 C60 118.1(4) . . ? C66 C61 C60 122.5(4) . . ? C61 C62 C63 120.1(5) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C64 C63 C62 120.1(5) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C63 C64 C65 120.5(5) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C64 C65 C66 120.1(5) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C61 C66 C65 119.7(5) . . ? C61 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? C72 C67 C68 117.9(4) . . ? C72 C67 C73 123.2(4) . . ? C68 C67 C73 118.9(4) . . ? C69 C68 C67 120.9(4) . . ? C69 C68 H68 119.6 . . ? C67 C68 H68 119.6 . . ? C70 C69 C68 120.2(5) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C71 C70 C69 119.5(5) . . ? C71 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? C70 C71 C72 120.8(5) . . ? C70 C71 H71 119.6 . . ? C72 C71 H71 119.6 . . ? C71 C72 C67 120.7(5) . . ? C71 C72 H72 119.7 . . ? C67 C72 H72 119.7 . . ? O7 C73 C74 125.7(4) . . ? O7 C73 C67 115.8(3) . . ? C74 C73 C67 118.4(3) . . ? C75 C74 C73 125.2(4) . . ? C75 C74 H74A 117.4 . . ? C73 C74 H74A 117.4 . . ? O8 C75 C74 125.0(4) . . ? O8 C75 C76 116.6(4) . . ? C74 C75 C76 118.4(4) . . ? C79 C76 C77 117.7(4) . . ? C79 C76 C75 118.7(4) . . ? C77 C76 C75 123.5(4) . . ? C76 C77 C78 120.7(5) . . ? C76 C77 H77 119.7 . . ? C78 C77 H77 119.7 . . ? C81 C78 C77 120.2(5) . . ? C81 C78 H78 119.9 . . ? C77 C78 H78 119.9 . . ? C76 C79 C80 121.5(5) . . ? C76 C79 H79 119.2 . . ? C80 C79 H79 119.2 . . ? C81 C80 C79 119.8(5) . . ? C81 C80 H80 120.1 . . ? C79 C80 H80 120.1 . . ? C78 C81 C80 120.1(5) . . ? C78 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C83 C82 H82A 109.5 . . ? C83 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C83 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N5 C83 C82 178.1(8) . . ? N6 C85 C86 176.1(13) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 H87A 109.5 . . ? C88 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C88 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N7 C88 C87 169.7(18) . . ? C90 O15 C90 180.0(9) 2_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Dy1 Ni2 O7 -116.65(13) . . . . ? O5 Dy1 Ni2 O7 34.71(16) . . . . ? O9 Dy1 Ni2 O7 -42.10(13) . . . . ? O13 Dy1 Ni2 O7 -176.08(16) . . . . ? O11 Dy1 Ni2 O7 101.0(7) . . . . ? O12 Dy1 Ni2 O7 100.81(13) . . . . ? O14 Dy1 Ni2 O7 172.36(13) . . . . ? O6 Dy1 Ni2 O7 28.54(13) . . . . ? O10 Dy1 Ni2 O8 -41.28(11) . . . . ? O5 Dy1 Ni2 O8 110.09(14) . . . . ? O9 Dy1 Ni2 O8 33.28(11) . . . . ? O13 Dy1 Ni2 O8 -100.70(14) . . . . ? O11 Dy1 Ni2 O8 176.4(7) . . . . ? O12 Dy1 Ni2 O8 176.18(11) . . . . ? O14 Dy1 Ni2 O8 -112.26(10) . . . . ? O6 Dy1 Ni2 O8 103.92(10) . . . . ? O10 Dy1 Ni2 O5 -151.37(14) . . . . ? O9 Dy1 Ni2 O5 -76.81(14) . . . . ? O13 Dy1 Ni2 O5 149.21(17) . . . . ? O11 Dy1 Ni2 O5 66.3(7) . . . . ? O12 Dy1 Ni2 O5 66.09(13) . . . . ? O14 Dy1 Ni2 O5 137.64(13) . . . . ? O6 Dy1 Ni2 O5 -6.17(13) . . . . ? O10 Dy1 Ni2 O13 59.42(14) . . . . ? O5 Dy1 Ni2 O13 -149.21(17) . . . . ? O9 Dy1 Ni2 O13 133.98(14) . . . . ? O11 Dy1 Ni2 O13 -82.9(7) . . . . ? O12 Dy1 Ni2 O13 -83.12(14) . . . . ? O14 Dy1 Ni2 O13 -11.56(13) . . . . ? O6 Dy1 Ni2 O13 -155.38(13) . . . . ? O10 Dy1 Ni2 N4 45.49(15) . . . . ? O5 Dy1 Ni2 N4 -163.14(17) . . . . ? O9 Dy1 Ni2 N4 120.05(15) . . . . ? O13 Dy1 Ni2 N4 -13.93(17) . . . . ? O11 Dy1 Ni2 N4 -96.9(7) . . . . ? O12 Dy1 Ni2 N4 -97.05(15) . . . . ? O14 Dy1 Ni2 N4 -25.50(14) . . . . ? O6 Dy1 Ni2 N4 -169.31(14) . . . . ? O10 Dy1 Ni2 N3 141.92(12) . . . . ? O5 Dy1 Ni2 N3 -66.72(15) . . . . ? O9 Dy1 Ni2 N3 -143.53(12) . . . . ? O13 Dy1 Ni2 N3 82.49(15) . . . . ? O11 Dy1 Ni2 N3 -0.4(7) . . . . ? O12 Dy1 Ni2 N3 -0.62(12) . . . . ? O14 Dy1 Ni2 N3 70.93(12) . . . . ? O6 Dy1 Ni2 N3 -72.89(12) . . . . ? O7 Ni2 O5 C35 57.3(3) . . . . ? O8 Ni2 O5 C35 146.2(3) . . . . ? O13 Ni2 O5 C35 -127.4(3) . . . . ? N4 Ni2 O5 C35 -88.1(6) . . . . ? N3 Ni2 O5 C35 -30.8(3) . . . . ? Dy1 Ni2 O5 C35 -147.4(3) . . . . ? O7 Ni2 O5 Dy1 -155.29(11) . . . . ? O8 Ni2 O5 Dy1 -66.43(12) . . . . ? O13 Ni2 O5 Dy1 20.05(11) . . . . ? N4 Ni2 O5 Dy1 59.3(5) . . . . ? N3 Ni2 O5 Dy1 116.60(13) . . . . ? O10 Dy1 O5 C35 -173.6(2) . . . . ? O9 Dy1 O5 C35 -99.9(3) . . . . ? O13 Dy1 O5 C35 131.0(3) . . . . ? O11 Dy1 O5 C35 -20.6(3) . . . . ? O12 Dy1 O5 C35 34.8(3) . . . . ? O14 Dy1 O5 C35 98.1(3) . . . . ? O6 Dy1 O5 C35 -37.3(3) . . . . ? Ni2 Dy1 O5 C35 149.7(3) . . . . ? O10 Dy1 O5 Ni2 36.69(17) . . . . ? O9 Dy1 O5 Ni2 110.39(12) . . . . ? O13 Dy1 O5 Ni2 -18.69(10) . . . . ? O11 Dy1 O5 Ni2 -170.32(12) . . . . ? O12 Dy1 O5 Ni2 -114.93(12) . . . . ? O14 Dy1 O5 Ni2 -51.60(14) . . . . ? O6 Dy1 O5 Ni2 172.98(15) . . . . ? O10 Dy1 O6 C34 146.6(2) . . . . ? O5 Dy1 O6 C34 32.2(2) . . . . ? O9 Dy1 O6 C34 142.0(3) . . . . ? O13 Dy1 O6 C34 18.4(3) . . . . ? O11 Dy1 O6 C34 -137.4(3) . . . . ? O12 Dy1 O6 C34 -61.5(2) . . . . ? O14 Dy1 O6 C34 -72.8(3) . . . . ? Ni2 Dy1 O6 C34 36.3(2) . . . . ? O10 Dy1 O6 C36 -59.7(4) . . . . ? O5 Dy1 O6 C36 -174.2(4) . . . . ? O9 Dy1 O6 C36 -64.4(3) . . . . ? O13 Dy1 O6 C36 172.0(3) . . . . ? O11 Dy1 O6 C36 16.2(3) . . . . ? O12 Dy1 O6 C36 92.2(3) . . . . ? O14 Dy1 O6 C36 80.8(4) . . . . ? Ni2 Dy1 O6 C36 -170.1(3) . . . . ? O8 Ni2 O7 C73 6.5(3) . . . . ? O5 Ni2 O7 C73 99.3(3) . . . . ? O13 Ni2 O7 C73 53.2(12) . . . . ? N4 Ni2 O7 C73 -89.2(3) . . . . ? N3 Ni2 O7 C73 -175.0(3) . . . . ? Dy1 Ni2 O7 C73 77.2(4) . . . . ? O7 Ni2 O8 C75 -8.3(3) . . . . ? O5 Ni2 O8 C75 -105.4(3) . . . . ? O13 Ni2 O8 C75 176.4(3) . . . . ? N4 Ni2 O8 C75 86.7(3) . . . . ? N3 Ni2 O8 C75 -37(2) . . . . ? Dy1 Ni2 O8 C75 -143.4(3) . . . . ? O10 Dy1 O9 C58 -17.9(4) . . . . ? O5 Dy1 O9 C58 -145.0(4) . . . . ? O13 Dy1 O9 C58 -78.1(4) . . . . ? O11 Dy1 O9 C58 73.7(4) . . . . ? O12 Dy1 O9 C58 126.9(4) . . . . ? O14 Dy1 O9 C58 11.5(5) . . . . ? O6 Dy1 O9 C58 159.1(4) . . . . ? Ni2 Dy1 O9 C58 -110.3(4) . . . . ? O5 Dy1 O10 C60 86.9(4) . . . . ? O9 Dy1 O10 C60 1.8(4) . . . . ? O13 Dy1 O10 C60 138.1(4) . . . . ? O11 Dy1 O10 C60 -76.6(4) . . . . ? O12 Dy1 O10 C60 -139.5(4) . . . . ? O14 Dy1 O10 C60 -158.0(4) . . . . ? O6 Dy1 O10 C60 -2.7(5) . . . . ? Ni2 Dy1 O10 C60 107.4(4) . . . . ? O10 Dy1 O11 C45 -151.9(4) . . . . ? O5 Dy1 O11 C45 49.3(4) . . . . ? O9 Dy1 O11 C45 134.9(4) . . . . ? O13 Dy1 O11 C45 -83.3(4) . . . . ? O12 Dy1 O11 C45 -9.0(4) . . . . ? O14 Dy1 O11 C45 -81.4(4) . . . . ? O6 Dy1 O11 C45 64.1(4) . . . . ? Ni2 Dy1 O11 C45 -9.2(10) . . . . ? O10 Dy1 O12 C44 70.9(4) . . . . ? O5 Dy1 O12 C44 -144.6(4) . . . . ? O9 Dy1 O12 C44 -51.4(4) . . . . ? O13 Dy1 O12 C44 147.9(4) . . . . ? O11 Dy1 O12 C44 3.2(4) . . . . ? O14 Dy1 O12 C44 89.3(4) . . . . ? O6 Dy1 O12 C44 -83.3(4) . . . . ? Ni2 Dy1 O12 C44 -176.8(3) . . . . ? O7 Ni2 O13 C21 -136.3(10) . . . . ? O8 Ni2 O13 C21 -89.5(3) . . . . ? O5 Ni2 O13 C21 177.0(3) . . . . ? N4 Ni2 O13 C21 6.4(3) . . . . ? N3 Ni2 O13 C21 92.3(3) . . . . ? Dy1 Ni2 O13 C21 -163.0(4) . . . . ? O7 Ni2 O13 Dy1 26.8(11) . . . . ? O8 Ni2 O13 Dy1 73.53(12) . . . . ? O5 Ni2 O13 Dy1 -20.02(11) . . . . ? N4 Ni2 O13 Dy1 169.38(13) . . . . ? N3 Ni2 O13 Dy1 -104.70(13) . . . . ? O10 Dy1 O13 C21 44.9(3) . . . . ? O5 Dy1 O13 C21 -177.0(3) . . . . ? O9 Dy1 O13 C21 102.7(3) . . . . ? O11 Dy1 O13 C21 -26.6(4) . . . . ? O12 Dy1 O13 C21 -94.7(3) . . . . ? O14 Dy1 O13 C21 -28.7(3) . . . . ? O6 Dy1 O13 C21 -164.0(3) . . . . ? Ni2 Dy1 O13 C21 164.4(3) . . . . ? O10 Dy1 O13 Ni2 -119.43(13) . . . . ? O5 Dy1 O13 Ni2 18.69(10) . . . . ? O9 Dy1 O13 Ni2 -61.61(16) . . . . ? O11 Dy1 O13 Ni2 169.07(12) . . . . ? O12 Dy1 O13 Ni2 100.98(12) . . . . ? O14 Dy1 O13 Ni2 166.95(15) . . . . ? O6 Dy1 O13 Ni2 31.64(17) . . . . ? O10 Dy1 O14 C16 -61.9(2) . . . . ? O5 Dy1 O14 C16 60.5(3) . . . . ? O9 Dy1 O14 C16 -91.8(3) . . . . ? O13 Dy1 O14 C16 25.7(2) . . . . ? O11 Dy1 O14 C16 -153.0(3) . . . . ? O12 Dy1 O14 C16 130.8(3) . . . . ? O6 Dy1 O14 C16 142.2(2) . . . . ? Ni2 Dy1 O14 C16 33.3(2) . . . . ? O10 Dy1 O14 C15 91.7(3) . . . . ? O5 Dy1 O14 C15 -145.9(3) . . . . ? O9 Dy1 O14 C15 61.8(4) . . . . ? O13 Dy1 O14 C15 179.2(3) . . . . ? O11 Dy1 O14 C15 0.5(3) . . . . ? O12 Dy1 O14 C15 -75.6(3) . . . . ? O6 Dy1 O14 C15 -64.3(4) . . . . ? Ni2 Dy1 O14 C15 -173.2(3) . . . . ? O7 Ni2 N3 C27 -163.3(3) . . . . ? O8 Ni2 N3 C27 -135(2) . . . . ? O5 Ni2 N3 C27 -65.9(3) . . . . ? O13 Ni2 N3 C27 12.0(3) . . . . ? N4 Ni2 N3 C27 101.5(3) . . . . ? Dy1 Ni2 N3 C27 -28.8(3) . . . . ? O7 Ni2 N3 C26 77.4(2) . . . . ? O8 Ni2 N3 C26 106(2) . . . . ? O5 Ni2 N3 C26 174.8(2) . . . . ? O13 Ni2 N3 C26 -107.3(2) . . . . ? N4 Ni2 N3 C26 -17.8(2) . . . . ? Dy1 Ni2 N3 C26 -148.1(2) . . . . ? O7 Ni2 N3 C28 -40.7(3) . . . . ? O8 Ni2 N3 C28 -12(2) . . . . ? O5 Ni2 N3 C28 56.7(2) . . . . ? O13 Ni2 N3 C28 134.6(2) . . . . ? N4 Ni2 N3 C28 -135.9(3) . . . . ? Dy1 Ni2 N3 C28 93.8(2) . . . . ? O7 Ni2 N4 C25 -99.6(3) . . . . ? O8 Ni2 N4 C25 171.4(3) . . . . ? O5 Ni2 N4 C25 46.0(6) . . . . ? O13 Ni2 N4 C25 84.3(3) . . . . ? N3 Ni2 N4 C25 -11.3(3) . . . . ? Dy1 Ni2 N4 C25 93.4(3) . . . . ? O7 Ni2 N4 C24 19.9(3) . . . . ? O8 Ni2 N4 C24 -69.2(3) . . . . ? O5 Ni2 N4 C24 165.4(4) . . . . ? O13 Ni2 N4 C24 -156.3(3) . . . . ? N3 Ni2 N4 C24 108.1(3) . . . . ? Dy1 Ni2 N4 C24 -147.2(3) . . . . ? O7 Ni2 N4 C23 138.9(3) . . . . ? O8 Ni2 N4 C23 49.8(3) . . . . ? O5 Ni2 N4 C23 -75.6(6) . . . . ? O13 Ni2 N4 C23 -37.3(3) . . . . ? N3 Ni2 N4 C23 -132.9(3) . . . . ? Dy1 Ni2 N4 C23 -28.2(3) . . . . ? C15 O14 C16 C17 0.9(6) . . . . ? Dy1 O14 C16 C17 156.7(3) . . . . ? C15 O14 C16 C21 -178.0(4) . . . . ? Dy1 O14 C16 C21 -22.1(4) . . . . ? O14 C16 C17 C18 -178.1(4) . . . . ? C21 C16 C17 C18 0.6(6) . . . . ? C16 C17 C18 C19 -1.4(6) . . . . ? C16 C17 C18 C22 177.6(4) . . . . ? C17 C18 C19 C20 1.3(7) . . . . ? C22 C18 C19 C20 -177.7(4) . . . . ? C18 C19 C20 C21 -0.3(7) . . . . ? C18 C19 C20 C23 173.8(4) . . . . ? Ni2 O13 C21 C20 9.9(6) . . . . ? Dy1 O13 C21 C20 -150.1(3) . . . . ? Ni2 O13 C21 C16 -170.9(3) . . . . ? Dy1 O13 C21 C16 29.2(5) . . . . ? C19 C20 C21 O13 178.7(4) . . . . ? C23 C20 C21 O13 4.9(6) . . . . ? C19 C20 C21 C16 -0.6(6) . . . . ? C23 C20 C21 C16 -174.4(4) . . . . ? C17 C16 C21 O13 -178.9(4) . . . . ? O14 C16 C21 O13 0.0(5) . . . . ? C17 C16 C21 C20 0.4(6) . . . . ? O14 C16 C21 C20 179.3(3) . . . . ? C25 N4 C23 C20 -56.9(5) . . . . ? C24 N4 C23 C20 -176.9(4) . . . . ? Ni2 N4 C23 C20 60.2(4) . . . . ? C19 C20 C23 N4 141.6(4) . . . . ? C21 C20 C23 N4 -44.5(6) . . . . ? C24 N4 C25 C26 -82.3(4) . . . . ? C23 N4 C25 C26 160.2(3) . . . . ? Ni2 N4 C25 C26 38.8(4) . . . . ? C27 N3 C26 C25 -78.4(4) . . . . ? C28 N3 C26 C25 161.6(3) . . . . ? Ni2 N3 C26 C25 44.4(4) . . . . ? N4 C25 C26 N3 -59.5(4) . . . . ? C27 N3 C28 C29 60.8(4) . . . . ? C26 N3 C28 C29 -178.4(3) . . . . ? Ni2 N3 C28 C29 -65.5(4) . . . . ? N3 C28 C29 C35 32.5(5) . . . . ? N3 C28 C29 C30 -147.0(4) . . . . ? C35 C29 C30 C31 -1.1(6) . . . . ? C28 C29 C30 C31 178.4(4) . . . . ? C29 C30 C31 C33 -3.3(7) . . . . ? C29 C30 C31 C32 178.7(4) . . . . ? C30 C31 C33 C34 3.4(6) . . . . ? C32 C31 C33 C34 -178.6(4) . . . . ? C31 C33 C34 O6 -177.4(4) . . . . ? C31 C33 C34 C35 0.9(6) . . . . ? C36 O6 C34 C33 -3.4(6) . . . . ? Dy1 O6 C34 C33 152.7(4) . . . . ? C36 O6 C34 C35 178.2(4) . . . . ? Dy1 O6 C34 C35 -25.7(4) . . . . ? Ni2 O5 C35 C29 5.8(5) . . . . ? Dy1 O5 C35 C29 -136.5(3) . . . . ? Ni2 O5 C35 C34 -178.0(3) . . . . ? Dy1 O5 C35 C34 39.7(4) . . . . ? C30 C29 C35 O5 -178.5(4) . . . . ? C28 C29 C35 O5 2.0(6) . . . . ? C30 C29 C35 C34 5.4(6) . . . . ? C28 C29 C35 C34 -174.1(4) . . . . ? C33 C34 C35 O5 178.1(4) . . . . ? O6 C34 C35 O5 -3.4(5) . . . . ? C33 C34 C35 C29 -5.4(6) . . . . ? O6 C34 C35 C29 173.1(3) . . . . ? C39 C37 C38 C42 -2.6(6) . . . . ? C38 C37 C39 C40 0.8(7) . . . . ? C37 C39 C40 C41 0.7(7) . . . . ? C39 C40 C41 C42 -0.4(7) . . . . ? C37 C38 C42 C41 2.8(6) . . . . ? C37 C38 C42 C44 -174.5(4) . . . . ? C40 C41 C42 C38 -1.4(6) . . . . ? C40 C41 C42 C44 175.9(4) . . . . ? Dy1 O12 C44 C43 -2.0(6) . . . . ? Dy1 O12 C44 C42 174.1(2) . . . . ? C45 C43 C44 O12 3.2(7) . . . . ? C45 C43 C44 C42 -172.8(4) . . . . ? C38 C42 C44 O12 -35.3(5) . . . . ? C41 C42 C44 O12 147.4(4) . . . . ? C38 C42 C44 C43 141.0(4) . . . . ? C41 C42 C44 C43 -36.3(6) . . . . ? Dy1 O11 C45 C43 13.3(6) . . . . ? Dy1 O11 C45 C46 -165.6(3) . . . . ? C44 C43 C45 O11 -8.6(7) . . . . ? C44 C43 C45 C46 170.3(4) . . . . ? O11 C45 C46 C47 11.3(6) . . . . ? C43 C45 C46 C47 -167.6(4) . . . . ? O11 C45 C46 C51 -168.7(4) . . . . ? C43 C45 C46 C51 12.4(6) . . . . ? C51 C46 C47 C48 1.5(6) . . . . ? C45 C46 C47 C48 -178.4(4) . . . . ? C46 C47 C48 C49 -0.7(7) . . . . ? C47 C48 C49 C50 -0.5(7) . . . . ? C48 C49 C50 C51 0.8(8) . . . . ? C49 C50 C51 C46 0.1(8) . . . . ? C47 C46 C51 C50 -1.3(7) . . . . ? C45 C46 C51 C50 178.7(4) . . . . ? C57 C52 C53 C54 -1.0(8) . . . . ? C52 C53 C54 C55 -2.0(9) . . . . ? C53 C54 C55 C56 3.1(9) . . . . ? C54 C55 C56 C57 -1.2(10) . . . . ? C53 C52 C57 C56 2.9(8) . . . . ? C53 C52 C57 C58 -177.5(5) . . . . ? C55 C56 C57 C52 -1.8(8) . . . . ? C55 C56 C57 C58 178.6(5) . . . . ? Dy1 O9 C58 C59 23.0(7) . . . . ? Dy1 O9 C58 C57 -159.0(3) . . . . ? C52 C57 C58 O9 -22.4(6) . . . . ? C56 C57 C58 O9 157.1(5) . . . . ? C52 C57 C58 C59 155.6(5) . . . . ? C56 C57 C58 C59 -24.8(7) . . . . ? O9 C58 C59 C60 -5.9(8) . . . . ? C57 C58 C59 C60 176.1(4) . . . . ? Dy1 O10 C60 C59 8.8(7) . . . . ? Dy1 O10 C60 C61 -170.6(3) . . . . ? C58 C59 C60 O10 -9.3(8) . . . . ? C58 C59 C60 C61 170.1(4) . . . . ? O10 C60 C61 C62 14.9(6) . . . . ? C59 C60 C61 C62 -164.5(4) . . . . ? O10 C60 C61 C66 -165.8(5) . . . . ? C59 C60 C61 C66 14.7(7) . . . . ? C66 C61 C62 C63 -1.9(7) . . . . ? C60 C61 C62 C63 177.4(4) . . . . ? C61 C62 C63 C64 1.1(8) . . . . ? C62 C63 C64 C65 -0.7(9) . . . . ? C63 C64 C65 C66 1.2(10) . . . . ? C62 C61 C66 C65 2.3(9) . . . . ? C60 C61 C66 C65 -176.9(5) . . . . ? C64 C65 C66 C61 -2.0(10) . . . . ? C72 C67 C68 C69 1.8(7) . . . . ? C73 C67 C68 C69 -177.3(4) . . . . ? C67 C68 C69 C70 -1.0(8) . . . . ? C68 C69 C70 C71 -0.4(9) . . . . ? C69 C70 C71 C72 1.0(10) . . . . ? C70 C71 C72 C67 -0.1(10) . . . . ? C68 C67 C72 C71 -1.2(8) . . . . ? C73 C67 C72 C71 177.8(5) . . . . ? Ni2 O7 C73 C74 -4.4(6) . . . . ? Ni2 O7 C73 C67 172.0(3) . . . . ? C72 C67 C73 O7 154.6(5) . . . . ? C68 C67 C73 O7 -26.3(6) . . . . ? C72 C67 C73 C74 -28.7(6) . . . . ? C68 C67 C73 C74 150.3(4) . . . . ? O7 C73 C74 C75 0.7(7) . . . . ? C67 C73 C74 C75 -175.6(4) . . . . ? Ni2 O8 C75 C74 7.8(6) . . . . ? Ni2 O8 C75 C76 -169.4(3) . . . . ? C73 C74 C75 O8 -2.5(7) . . . . ? C73 C74 C75 C76 174.6(4) . . . . ? O8 C75 C76 C79 15.3(6) . . . . ? C74 C75 C76 C79 -162.1(4) . . . . ? O8 C75 C76 C77 -169.0(5) . . . . ? C74 C75 C76 C77 13.6(7) . . . . ? C79 C76 C77 C78 0.4(8) . . . . ? C75 C76 C77 C78 -175.3(5) . . . . ? C76 C77 C78 C81 -2.9(9) . . . . ? C77 C76 C79 C80 1.9(8) . . . . ? C75 C76 C79 C80 177.8(5) . . . . ? C76 C79 C80 C81 -1.8(9) . . . . ? C77 C78 C81 C80 3.1(10) . . . . ? C79 C80 C81 C78 -0.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.149 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 930907'