# Electronic Supplementary Material (ESI) for CrystEngComm # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H37 Gd N8 Ni O13' _chemical_formula_weight 1065.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5623(5) _cell_length_b 18.0907(5) _cell_length_c 23.0081(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.177(3) _cell_angle_gamma 90.00 _cell_volume 4297.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24713 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 27.31 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2140 _exptl_absorpt_coefficient_mu 2.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3647 _exptl_absorpt_correction_T_max 0.6112 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37378 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.31 _reflns_number_total 9291 _reflns_number_gt 7475 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+8.0637P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9291 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3531(7) 0.2423(4) 0.4633(3) 0.0710(19) Uani 1 1 d . . . H1A H 0.3614 0.2897 0.4825 0.106 Uiso 1 1 calc R . . H1B H 0.4090 0.2074 0.4877 0.106 Uiso 1 1 calc R . . H1C H 0.2650 0.2257 0.4576 0.106 Uiso 1 1 calc R . . C2 C 0.3819(5) 0.1841(3) 0.3731(2) 0.0481(12) Uani 1 1 d . . . C3 C 0.3303(7) 0.1188(3) 0.3881(3) 0.0635(16) Uani 1 1 d . . . H3 H 0.2985 0.1157 0.4228 0.076 Uiso 1 1 calc R . . C4 C 0.3258(7) 0.0576(3) 0.3516(3) 0.0716(19) Uani 1 1 d . . . H4 H 0.2895 0.0136 0.3613 0.086 Uiso 1 1 calc R . . C5 C 0.3751(6) 0.0620(3) 0.3008(3) 0.0594(14) Uani 1 1 d . . . H5 H 0.3715 0.0209 0.2763 0.071 Uiso 1 1 calc R . . C6 C 0.4308(5) 0.1278(3) 0.2858(2) 0.0423(10) Uani 1 1 d . . . C7 C 0.4331(4) 0.1906(2) 0.32202(18) 0.0375(9) Uani 1 1 d . . . C8 C 0.4909(5) 0.1239(3) 0.23445(19) 0.0432(11) Uani 1 1 d . . . H8 H 0.4700 0.0831 0.2097 0.052 Uiso 1 1 calc R . . C9 C 0.6256(6) 0.1529(3) 0.1684(2) 0.0564(14) Uani 1 1 d . . . H9A H 0.5863 0.1842 0.1353 0.068 Uiso 1 1 calc R . . H9B H 0.6062 0.1019 0.1568 0.068 Uiso 1 1 calc R . . C10 C 0.7695(7) 0.1639(3) 0.1815(2) 0.0630(16) Uani 1 1 d . . . H10A H 0.8048 0.1373 0.1519 0.076 Uiso 1 1 calc R . . H10B H 0.8056 0.1421 0.2199 0.076 Uiso 1 1 calc R . . C11 C 0.8135(7) 0.2430(4) 0.1822(3) 0.0688(17) Uani 1 1 d . . . H11A H 0.9068 0.2435 0.1867 0.083 Uiso 1 1 calc R . . H11B H 0.7764 0.2650 0.1440 0.083 Uiso 1 1 calc R . . C12 C 0.8539(5) 0.3462(3) 0.2453(2) 0.0492(12) Uani 1 1 d . . . H12 H 0.9278 0.3486 0.2295 0.059 Uiso 1 1 calc R . . C13 C 0.8369(5) 0.4061(3) 0.2850(2) 0.0463(11) Uani 1 1 d . . . C14 C 0.9291(6) 0.4631(4) 0.2906(3) 0.0674(16) Uani 1 1 d . . . H14 H 0.9963 0.4600 0.2703 0.081 Uiso 1 1 calc R . . C15 C 0.9205(7) 0.5235(4) 0.3259(3) 0.0741(18) Uani 1 1 d . . . H15 H 0.9821 0.5609 0.3293 0.089 Uiso 1 1 calc R . . C16 C 0.8214(6) 0.5292(3) 0.3563(3) 0.0610(15) Uani 1 1 d . . . H16 H 0.8153 0.5706 0.3795 0.073 Uiso 1 1 calc R . . C17 C 0.7328(5) 0.4739(3) 0.3522(2) 0.0428(11) Uani 1 1 d . . . C18 C 0.7363(4) 0.4109(2) 0.31588(18) 0.0373(10) Uani 1 1 d . . . C19 C 0.6345(6) 0.5298(3) 0.4266(2) 0.0628(15) Uani 1 1 d . . . H19A H 0.5604 0.5246 0.4443 0.094 Uiso 1 1 calc R . . H19B H 0.6333 0.5777 0.4086 0.094 Uiso 1 1 calc R . . H19C H 0.7121 0.5244 0.4567 0.094 Uiso 1 1 calc R . . C20 C 0.5326(5) 0.3709(3) 0.1565(2) 0.0455(11) Uani 1 1 d . . . H20 H 0.6190 0.3853 0.1654 0.055 Uiso 1 1 calc R . . C21 C 0.4541(5) 0.4025(3) 0.1080(2) 0.0426(10) Uani 1 1 d . . . H21 H 0.4877 0.4366 0.0850 0.051 Uiso 1 1 calc R . . C22 C 0.3231(5) 0.3833(2) 0.09320(17) 0.0388(10) Uani 1 1 d . . . C23 C 0.2826(5) 0.3318(3) 0.12989(19) 0.0468(11) Uani 1 1 d . . . H23 H 0.1960 0.3176 0.1226 0.056 Uiso 1 1 calc R . . C24 C 0.3694(5) 0.3013(3) 0.17726(19) 0.0446(11) Uani 1 1 d . . . H24 H 0.3395 0.2656 0.2001 0.054 Uiso 1 1 calc R . . C25 C 0.2306(5) 0.4116(2) 0.04061(17) 0.0378(10) Uani 1 1 d . . . C26 C 0.2258(4) 0.4813(2) 0.01237(17) 0.0362(9) Uani 1 1 d . . . C27 C 0.3041(5) 0.5426(3) 0.0328(2) 0.0444(11) Uani 1 1 d . . . H27 H 0.3690 0.5340 0.0663 0.053 Uiso 1 1 calc R . . C28 C 0.2995(6) 0.6138(3) 0.0109(2) 0.0534(13) Uani 1 1 d . . . H28 H 0.3579 0.6470 0.0328 0.064 Uiso 1 1 calc R . . C29 C 0.2188(6) 0.6422(3) -0.0398(2) 0.0568(14) Uani 1 1 d . . . H29 H 0.2288 0.6923 -0.0466 0.068 Uiso 1 1 calc R . . C30 C 0.1264(6) 0.6065(3) -0.0812(2) 0.0550(13) Uani 1 1 d . . . H30 H 0.0874 0.6355 -0.1134 0.066 Uiso 1 1 calc R . . C31 C 0.0820(5) 0.5344(3) -0.0826(2) 0.0462(11) Uani 1 1 d . . . H31 H 0.0198 0.5216 -0.1161 0.055 Uiso 1 1 calc R . . C32 C 0.1177(4) 0.4781(2) -0.04073(16) 0.0349(9) Uani 1 1 d . . . C33 C 0.0623(4) 0.4069(2) -0.04167(17) 0.0351(9) Uani 1 1 d . . . C34 C 0.1298(4) 0.3694(3) 0.00858(17) 0.0366(9) Uani 1 1 d . . . H34 H 0.1096 0.3219 0.0192 0.044 Uiso 1 1 calc R . . C35 C -0.1471(5) 0.2611(3) -0.12908(19) 0.0456(11) Uani 1 1 d . . . H35 H -0.1487 0.2097 -0.1295 0.055 Uiso 1 1 calc R . . C36 C -0.0485(5) 0.2954(3) -0.0898(2) 0.0463(11) Uani 1 1 d . . . H36 H 0.0146 0.2669 -0.0655 0.056 Uiso 1 1 calc R . . C37 C -0.0417(4) 0.3714(3) -0.08573(17) 0.0366(9) Uani 1 1 d . . . C38 C -0.1398(5) 0.4097(3) -0.12432(18) 0.0409(10) Uani 1 1 d . . . H38 H -0.1415 0.4611 -0.1239 0.049 Uiso 1 1 calc R . . C39 C -0.2344(5) 0.3707(3) -0.16314(18) 0.0432(10) Uani 1 1 d . . . H39 H -0.2980 0.3978 -0.1885 0.052 Uiso 1 1 calc R . . C40 C 0.9960(11) 0.6584(6) 0.4664(6) 0.138(5) Uani 1 1 d . . . C41 C 1.0500(10) 0.6055(5) 0.5108(4) 0.110(3) Uani 1 1 d . . . H41A H 1.0884 0.5659 0.4927 0.165 Uiso 1 1 calc R . . H41B H 0.9829 0.5861 0.5288 0.165 Uiso 1 1 calc R . . H41C H 1.1150 0.6288 0.5406 0.165 Uiso 1 1 calc R . . Gd1 Gd 0.46891(2) 0.366399(13) 0.362595(9) 0.03867(9) Uani 1 1 d . . . N1 N 0.5690(4) 0.1704(2) 0.21993(14) 0.0409(9) Uani 1 1 d . . . N2 N 0.7796(4) 0.2901(2) 0.22925(16) 0.0450(9) Uani 1 1 d . . . N3 N 0.6198(5) 0.3395(3) 0.48277(18) 0.0555(11) Uani 1 1 d . . . N4 N 0.2647(5) 0.4518(3) 0.4084(2) 0.0633(13) Uani 1 1 d . . . N5 N 0.2918(6) 0.4270(3) 0.25845(18) 0.0605(13) Uani 1 1 d . . . N6 N 0.4950(4) 0.3209(2) 0.19195(15) 0.0406(9) Uani 1 1 d . . . N7 N -0.2408(4) 0.2970(2) -0.16676(15) 0.0382(8) Uani 1 1 d . . . N8 N 0.9490(15) 0.6980(6) 0.4329(6) 0.256(10) Uani 1 1 d . . . Ni1 Ni 0.62419(6) 0.26564(3) 0.26467(2) 0.03497(14) Uani 1 1 d . . . O1 O 0.3893(4) 0.24836(19) 0.40614(15) 0.0542(9) Uani 1 1 d . . . O2 O 0.4798(3) 0.25561(16) 0.31046(12) 0.0384(7) Uani 1 1 d . . . O3 O 0.6451(3) 0.36019(16) 0.31406(13) 0.0385(7) Uani 1 1 d . . . O4 O 0.6308(4) 0.47334(19) 0.38164(14) 0.0486(8) Uani 1 1 d . . . O5 O 0.6547(4) 0.3112(2) 0.43803(15) 0.0597(10) Uani 1 1 d . . . O6 O 0.5257(4) 0.3837(2) 0.47166(16) 0.0591(10) Uani 1 1 d . . . O7 O 0.6752(5) 0.3238(3) 0.53300(17) 0.0869(15) Uani 1 1 d . . . O8 O 0.2615(5) 0.3828(3) 0.4108(2) 0.0801(13) Uani 1 1 d . . . O9 O 0.3521(4) 0.4776(2) 0.38474(17) 0.0625(10) Uani 1 1 d . . . O10 O 0.1905(5) 0.4910(4) 0.4276(2) 0.1038(19) Uani 1 1 d . . . O11 O 0.2611(4) 0.3717(2) 0.28619(18) 0.0654(10) Uani 1 1 d . . . O12 O 0.4103(5) 0.4475(2) 0.27326(18) 0.0655(11) Uani 1 1 d . . . O13 O 0.2127(6) 0.4573(3) 0.2198(2) 0.1027(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.104(5) 0.056(4) 0.068(4) 0.003(3) 0.051(4) -0.003(4) C2 0.060(3) 0.033(2) 0.055(3) -0.001(2) 0.018(2) -0.004(2) C3 0.085(4) 0.040(3) 0.077(4) 0.004(3) 0.042(3) -0.010(3) C4 0.091(5) 0.034(3) 0.103(5) -0.002(3) 0.050(4) -0.020(3) C5 0.068(4) 0.038(3) 0.074(3) -0.009(3) 0.019(3) -0.014(3) C6 0.052(3) 0.030(2) 0.042(2) 0.0004(18) 0.0036(19) -0.001(2) C7 0.042(2) 0.029(2) 0.040(2) 0.0038(17) 0.0039(18) -0.002(2) C8 0.055(3) 0.032(2) 0.037(2) -0.0052(17) -0.0049(19) -0.003(2) C9 0.088(4) 0.046(3) 0.035(2) -0.008(2) 0.013(2) -0.001(3) C10 0.087(5) 0.061(4) 0.047(3) -0.007(2) 0.029(3) 0.002(3) C11 0.091(5) 0.064(4) 0.063(3) -0.006(3) 0.041(3) -0.007(3) C12 0.052(3) 0.052(3) 0.046(2) 0.010(2) 0.014(2) 0.001(3) C13 0.045(3) 0.043(3) 0.048(2) 0.010(2) 0.002(2) -0.005(2) C14 0.056(4) 0.069(4) 0.076(4) 0.002(3) 0.012(3) -0.015(3) C15 0.062(4) 0.062(4) 0.096(5) -0.009(3) 0.011(3) -0.024(3) C16 0.066(4) 0.044(3) 0.068(3) -0.010(3) 0.003(3) -0.018(3) C17 0.044(3) 0.037(3) 0.042(2) 0.0031(18) -0.0034(19) -0.001(2) C18 0.040(2) 0.030(2) 0.036(2) 0.0053(16) -0.0030(17) -0.002(2) C19 0.082(4) 0.050(3) 0.051(3) -0.016(2) 0.002(3) -0.002(3) C20 0.050(3) 0.038(3) 0.042(2) 0.0083(19) -0.0057(19) -0.010(2) C21 0.040(3) 0.042(3) 0.043(2) 0.0092(19) 0.0029(19) -0.001(2) C22 0.051(3) 0.034(2) 0.0280(18) -0.0019(15) 0.0015(17) 0.000(2) C23 0.050(3) 0.052(3) 0.035(2) 0.0050(19) 0.0002(19) -0.006(2) C24 0.050(3) 0.046(3) 0.035(2) 0.0081(19) 0.0034(19) -0.002(2) C25 0.049(3) 0.034(2) 0.0284(18) 0.0007(16) 0.0034(17) 0.003(2) C26 0.041(2) 0.035(2) 0.0297(18) -0.0017(16) 0.0033(17) 0.000(2) C27 0.049(3) 0.041(3) 0.040(2) -0.0029(19) 0.0023(19) -0.003(2) C28 0.063(3) 0.039(3) 0.056(3) -0.002(2) 0.006(2) -0.010(2) C29 0.079(4) 0.035(3) 0.056(3) 0.009(2) 0.013(3) -0.005(3) C30 0.073(4) 0.041(3) 0.048(3) 0.014(2) 0.008(3) -0.001(3) C31 0.057(3) 0.044(3) 0.037(2) 0.0048(19) 0.006(2) -0.001(2) C32 0.041(2) 0.035(2) 0.0278(17) 0.0014(15) 0.0054(16) 0.0035(19) C33 0.044(3) 0.031(2) 0.0277(18) -0.0008(15) 0.0028(16) 0.002(2) C34 0.046(2) 0.033(2) 0.0294(18) 0.0000(16) 0.0053(17) 0.000(2) C35 0.056(3) 0.034(2) 0.041(2) 0.0011(18) -0.005(2) -0.003(2) C36 0.054(3) 0.037(3) 0.040(2) 0.0032(19) -0.006(2) -0.001(2) C37 0.043(2) 0.038(2) 0.0271(17) -0.0005(16) 0.0037(16) 0.003(2) C38 0.050(3) 0.033(2) 0.035(2) -0.0017(17) -0.0016(18) 0.004(2) C39 0.051(3) 0.039(3) 0.033(2) -0.0024(18) -0.0035(18) 0.006(2) C40 0.137(9) 0.074(6) 0.164(10) -0.062(7) -0.058(8) 0.031(6) C41 0.122(8) 0.074(6) 0.126(7) -0.014(5) 0.010(6) 0.001(5) Gd1 0.05088(15) 0.03049(12) 0.03465(11) 0.00174(8) 0.00907(9) 0.00149(11) N1 0.053(2) 0.039(2) 0.0274(16) -0.0026(14) 0.0004(15) 0.0034(19) N2 0.057(3) 0.042(2) 0.0378(18) 0.0077(16) 0.0141(17) 0.005(2) N3 0.078(3) 0.049(3) 0.038(2) 0.0055(18) 0.009(2) 0.002(3) N4 0.067(3) 0.076(4) 0.047(2) -0.001(2) 0.011(2) 0.025(3) N5 0.078(4) 0.061(3) 0.040(2) 0.006(2) 0.007(2) 0.026(3) N6 0.048(2) 0.036(2) 0.0334(17) 0.0033(15) -0.0012(15) 0.0025(18) N7 0.042(2) 0.038(2) 0.0303(16) -0.0004(14) -0.0007(15) -0.0006(17) N8 0.304(17) 0.111(8) 0.253(14) -0.085(9) -0.167(13) 0.104(10) Ni1 0.0464(3) 0.0304(3) 0.0262(2) 0.00135(19) 0.0034(2) -0.0006(2) O1 0.078(3) 0.0389(19) 0.0547(19) -0.0031(15) 0.0339(19) -0.0094(18) O2 0.0515(19) 0.0299(16) 0.0334(14) 0.0015(11) 0.0077(13) -0.0027(14) O3 0.0495(18) 0.0269(16) 0.0381(14) -0.0027(12) 0.0069(13) -0.0065(14) O4 0.061(2) 0.0372(18) 0.0462(17) -0.0072(14) 0.0068(15) -0.0036(17) O5 0.072(3) 0.064(3) 0.0437(18) -0.0038(17) 0.0132(17) 0.012(2) O6 0.085(3) 0.047(2) 0.0472(19) 0.0016(15) 0.0190(19) 0.015(2) O7 0.117(4) 0.097(4) 0.0383(19) 0.010(2) -0.003(2) 0.023(3) O8 0.081(3) 0.075(3) 0.088(3) 0.021(2) 0.026(3) 0.003(3) O9 0.074(3) 0.051(2) 0.063(2) -0.0010(18) 0.016(2) 0.012(2) O10 0.089(4) 0.142(5) 0.083(3) -0.020(3) 0.022(3) 0.052(4) O11 0.068(3) 0.058(3) 0.065(2) 0.003(2) 0.002(2) 0.004(2) O12 0.077(3) 0.058(3) 0.064(2) 0.0121(19) 0.022(2) 0.010(2) O13 0.124(5) 0.113(4) 0.063(3) 0.024(3) 0.001(3) 0.056(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 C1 O1 1.449(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.377(7) . ? C2 O1 1.382(6) . ? C2 C7 1.398(6) . ? C3 C4 1.384(8) . ? C3 H3 0.9300 . ? C4 C5 1.378(8) . ? C4 H4 0.9300 . ? C5 C6 1.402(7) . ? C5 H5 0.9300 . ? C6 C7 1.407(6) . ? C6 C8 1.455(7) . ? C7 O2 1.324(5) . ? C8 N1 1.272(6) . ? C8 H8 0.9300 . ? C9 N1 1.469(6) . ? C9 C10 1.498(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.503(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.478(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.288(7) . ? C12 C13 1.451(7) . ? C12 H12 0.9300 . ? C13 C18 1.400(7) . ? C13 C14 1.407(8) . ? C14 C15 1.376(9) . ? C14 H14 0.9300 . ? C15 C16 1.380(9) . ? C15 H15 0.9300 . ? C16 C17 1.359(7) . ? C16 H16 0.9300 . ? C17 O4 1.389(6) . ? C17 C18 1.418(6) . ? C18 O3 1.324(5) . ? C19 O4 1.448(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N6 1.333(6) . ? C20 C21 1.368(6) . ? C20 H20 0.9300 . ? C21 C22 1.398(7) . ? C21 H21 0.9300 . ? C22 C23 1.384(6) . ? C22 C25 1.477(6) . ? C23 C24 1.383(6) . ? C23 H23 0.9300 . ? C24 N6 1.346(6) . ? C24 H24 0.9300 . ? C25 C34 1.389(6) . ? C25 C26 1.414(6) . ? C26 C27 1.405(6) . ? C26 C32 1.488(6) . ? C27 C28 1.379(7) . ? C27 H27 0.9300 . ? C28 C29 1.390(8) . ? C28 H28 0.9300 . ? C29 C30 1.371(8) . ? C29 H29 0.9300 . ? C30 C31 1.386(7) . ? C30 H30 0.9300 . ? C31 C32 1.397(6) . ? C31 H31 0.9300 . ? C32 C33 1.412(6) . ? C33 C34 1.399(6) . ? C33 C37 1.477(6) . ? C34 H34 0.9300 . ? C35 N7 1.339(6) . ? C35 C36 1.375(7) . ? C35 H35 0.9300 . ? C36 C37 1.378(6) . ? C36 H36 0.9300 . ? C37 C38 1.398(6) . ? C38 C39 1.384(6) . ? C38 H38 0.9300 . ? C39 N7 1.338(6) . ? C39 H39 0.9300 . ? C40 N8 1.094(15) . ? C40 C41 1.427(15) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? Gd1 O2 2.351(3) . ? Gd1 O3 2.366(3) . ? Gd1 O9 2.469(4) . ? Gd1 O6 2.474(4) . ? Gd1 O12 2.495(4) . ? Gd1 O11 2.508(4) . ? Gd1 O5 2.534(4) . ? Gd1 O4 2.558(4) . ? Gd1 O1 2.574(3) . ? Gd1 O8 2.673(5) . ? Gd1 N5 2.924(4) . ? Gd1 N3 2.926(4) . ? N1 Ni1 2.028(4) . ? N2 Ni1 2.030(4) . ? N3 O7 1.214(5) . ? N3 O6 1.259(6) . ? N3 O5 1.271(5) . ? N4 O10 1.207(6) . ? N4 O8 1.251(7) . ? N4 O9 1.257(6) . ? N5 O13 1.216(6) . ? N5 O11 1.265(6) . ? N5 O12 1.282(7) . ? N6 Ni1 2.167(4) . ? N7 Ni1 2.204(4) 4_465 ? Ni1 O2 2.036(3) . ? Ni1 O3 2.040(3) . ? Ni1 N7 2.204(4) 4_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.3(5) . . ? C3 C2 C7 121.8(5) . . ? O1 C2 C7 113.9(4) . . ? C2 C3 C4 120.0(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.8(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C7 119.6(4) . . ? C5 C6 C8 115.9(4) . . ? C7 C6 C8 124.4(4) . . ? O2 C7 C2 118.0(4) . . ? O2 C7 C6 124.0(4) . . ? C2 C7 C6 118.0(4) . . ? N1 C8 C6 126.8(4) . . ? N1 C8 H8 116.6 . . ? C6 C8 H8 116.6 . . ? N1 C9 C10 112.1(4) . . ? N1 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 115.3(6) . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? N2 C11 C10 115.7(4) . . ? N2 C11 H11A 108.3 . . ? C10 C11 H11A 108.3 . . ? N2 C11 H11B 108.3 . . ? C10 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? N2 C12 C13 128.3(5) . . ? N2 C12 H12 115.8 . . ? C13 C12 H12 115.8 . . ? C18 C13 C14 119.5(5) . . ? C18 C13 C12 125.0(5) . . ? C14 C13 C12 115.5(5) . . ? C15 C14 C13 120.4(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.7(6) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 119.6(6) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 O4 124.4(5) . . ? C16 C17 C18 122.0(5) . . ? O4 C17 C18 113.6(4) . . ? O3 C18 C13 124.4(4) . . ? O3 C18 C17 117.8(4) . . ? C13 C18 C17 117.8(4) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N6 C20 C21 125.2(5) . . ? N6 C20 H20 117.4 . . ? C21 C20 H20 117.4 . . ? C20 C21 C22 119.5(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 115.9(4) . . ? C23 C22 C25 119.8(4) . . ? C21 C22 C25 124.2(4) . . ? C24 C23 C22 120.7(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? N6 C24 C23 123.2(4) . . ? N6 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C34 C25 C26 107.3(4) . . ? C34 C25 C22 123.0(4) . . ? C26 C25 C22 129.7(4) . . ? C27 C26 C25 126.1(4) . . ? C27 C26 C32 127.0(4) . . ? C25 C26 C32 106.9(4) . . ? C28 C27 C26 129.9(5) . . ? C28 C27 H27 115.0 . . ? C26 C27 H27 115.0 . . ? C27 C28 C29 128.3(5) . . ? C27 C28 H28 115.8 . . ? C29 C28 H28 115.8 . . ? C30 C29 C28 129.0(5) . . ? C30 C29 H29 115.5 . . ? C28 C29 H29 115.5 . . ? C29 C30 C31 130.3(5) . . ? C29 C30 H30 114.9 . . ? C31 C30 H30 114.9 . . ? C30 C31 C32 129.0(5) . . ? C30 C31 H31 115.5 . . ? C32 C31 H31 115.5 . . ? C31 C32 C33 127.1(4) . . ? C31 C32 C26 125.9(4) . . ? C33 C32 C26 106.9(4) . . ? C34 C33 C32 107.0(4) . . ? C34 C33 C37 122.1(4) . . ? C32 C33 C37 130.8(4) . . ? C25 C34 C33 111.8(4) . . ? C25 C34 H34 124.1 . . ? C33 C34 H34 124.1 . . ? N7 C35 C36 124.1(5) . . ? N7 C35 H35 118.0 . . ? C36 C35 H35 118.0 . . ? C35 C36 C37 121.1(4) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C36 C37 C38 115.5(4) . . ? C36 C37 C33 120.1(4) . . ? C38 C37 C33 124.4(4) . . ? C39 C38 C37 119.7(4) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? N7 C39 C38 124.6(4) . . ? N7 C39 H39 117.7 . . ? C38 C39 H39 117.7 . . ? N8 C40 C41 176.6(19) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O2 Gd1 O3 65.85(10) . . ? O2 Gd1 O9 151.68(13) . . ? O3 Gd1 O9 127.82(13) . . ? O2 Gd1 O6 126.72(11) . . ? O3 Gd1 O6 115.99(13) . . ? O9 Gd1 O6 73.28(13) . . ? O2 Gd1 O12 96.39(12) . . ? O3 Gd1 O12 73.87(13) . . ? O9 Gd1 O12 69.07(13) . . ? O6 Gd1 O12 136.58(13) . . ? O2 Gd1 O11 78.73(13) . . ? O3 Gd1 O11 109.28(12) . . ? O9 Gd1 O11 73.26(14) . . ? O6 Gd1 O11 134.05(14) . . ? O12 Gd1 O11 51.09(15) . . ? O2 Gd1 O5 84.24(11) . . ? O3 Gd1 O5 74.46(11) . . ? O9 Gd1 O5 121.88(12) . . ? O6 Gd1 O5 50.81(12) . . ? O12 Gd1 O5 144.84(15) . . ? O11 Gd1 O5 158.72(14) . . ? O2 Gd1 O4 129.00(11) . . ? O3 Gd1 O4 63.44(10) . . ? O9 Gd1 O4 72.15(13) . . ? O6 Gd1 O4 73.76(12) . . ? O12 Gd1 O4 74.75(13) . . ? O11 Gd1 O4 123.09(13) . . ? O5 Gd1 O4 77.73(13) . . ? O2 Gd1 O1 63.03(10) . . ? O3 Gd1 O1 119.88(11) . . ? O9 Gd1 O1 112.17(13) . . ? O6 Gd1 O1 74.89(12) . . ? O12 Gd1 O1 139.82(15) . . ? O11 Gd1 O1 89.72(14) . . ? O5 Gd1 O1 71.09(14) . . ? O4 Gd1 O1 145.30(12) . . ? O2 Gd1 O8 116.02(14) . . ? O3 Gd1 O8 175.03(13) . . ? O9 Gd1 O8 48.32(15) . . ? O6 Gd1 O8 67.01(15) . . ? O12 Gd1 O8 101.21(15) . . ? O11 Gd1 O8 67.29(15) . . ? O5 Gd1 O8 110.08(13) . . ? O4 Gd1 O8 114.97(14) . . ? O1 Gd1 O8 64.32(14) . . ? O2 Gd1 N5 89.59(12) . . ? O3 Gd1 N5 93.55(13) . . ? O9 Gd1 N5 66.59(13) . . ? O6 Gd1 N5 139.48(13) . . ? O12 Gd1 N5 25.83(14) . . ? O11 Gd1 N5 25.48(15) . . ? O5 Gd1 N5 167.93(13) . . ? O4 Gd1 N5 98.40(14) . . ? O1 Gd1 N5 115.14(15) . . ? O8 Gd1 N5 81.95(15) . . ? O2 Gd1 N3 105.36(12) . . ? O3 Gd1 N3 96.44(12) . . ? O9 Gd1 N3 97.87(13) . . ? O6 Gd1 N3 25.23(12) . . ? O12 Gd1 N3 150.14(15) . . ? O11 Gd1 N3 152.92(14) . . ? O5 Gd1 N3 25.66(12) . . ? O4 Gd1 N3 75.68(12) . . ? O1 Gd1 N3 69.62(13) . . ? O8 Gd1 N3 87.53(15) . . ? N5 Gd1 N3 164.45(13) . . ? C8 N1 C9 117.7(4) . . ? C8 N1 Ni1 124.2(3) . . ? C9 N1 Ni1 118.1(3) . . ? C12 N2 C11 116.0(4) . . ? C12 N2 Ni1 123.4(3) . . ? C11 N2 Ni1 120.6(4) . . ? O7 N3 O6 122.9(5) . . ? O7 N3 O5 120.9(5) . . ? O6 N3 O5 116.2(4) . . ? O7 N3 Gd1 174.6(4) . . ? O6 N3 Gd1 56.9(2) . . ? O5 N3 Gd1 59.7(2) . . ? O10 N4 O8 123.0(6) . . ? O10 N4 O9 122.2(6) . . ? O8 N4 O9 114.8(5) . . ? O13 N5 O11 121.1(6) . . ? O13 N5 O12 123.1(6) . . ? O11 N5 O12 115.8(4) . . ? O13 N5 Gd1 172.4(4) . . ? O11 N5 Gd1 58.5(3) . . ? O12 N5 Gd1 58.0(2) . . ? C20 N6 C24 115.5(4) . . ? C20 N6 Ni1 124.4(3) . . ? C24 N6 Ni1 119.9(3) . . ? C39 N7 C35 115.1(4) . . ? C39 N7 Ni1 125.0(3) . 4_465 ? C35 N7 Ni1 119.5(3) . 4_465 ? N1 Ni1 N2 98.69(17) . . ? N1 Ni1 O2 91.18(14) . . ? N2 Ni1 O2 169.96(15) . . ? N1 Ni1 O3 168.76(15) . . ? N2 Ni1 O3 92.26(15) . . ? O2 Ni1 O3 77.96(12) . . ? N1 Ni1 N6 86.18(15) . . ? N2 Ni1 N6 91.17(15) . . ? O2 Ni1 N6 91.28(14) . . ? O3 Ni1 N6 91.13(13) . . ? N1 Ni1 N7 89.99(14) . 4_666 ? N2 Ni1 N7 86.74(15) . 4_666 ? O2 Ni1 N7 91.50(13) . 4_666 ? O3 Ni1 N7 93.14(13) . 4_666 ? N6 Ni1 N7 175.31(14) . 4_666 ? C2 O1 C1 116.1(4) . . ? C2 O1 Gd1 118.0(3) . . ? C1 O1 Gd1 125.9(3) . . ? C7 O2 Ni1 122.3(3) . . ? C7 O2 Gd1 126.5(3) . . ? Ni1 O2 Gd1 108.09(13) . . ? C18 O3 Ni1 126.2(3) . . ? C18 O3 Gd1 126.3(3) . . ? Ni1 O3 Gd1 107.41(13) . . ? C17 O4 C19 115.9(4) . . ? C17 O4 Gd1 118.8(3) . . ? C19 O4 Gd1 124.9(3) . . ? N3 O5 Gd1 94.7(3) . . ? N3 O6 Gd1 97.9(3) . . ? N4 O8 Gd1 93.5(3) . . ? N4 O9 Gd1 103.4(3) . . ? N5 O11 Gd1 96.0(3) . . ? N5 O12 Gd1 96.1(3) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.31 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.359 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 949947' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H36 Eu N7 O14 Zn' _chemical_formula_weight 1044.08 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4060(14) _cell_length_b 13.526(3) _cell_length_c 18.568(3) _cell_angle_alpha 74.727(13) _cell_angle_beta 81.420(12) _cell_angle_gamma 80.592(13) _cell_volume 2234.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12922 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 24.91 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6551 _exptl_absorpt_correction_T_max 0.8684 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16057 _diffrn_reflns_av_R_equivalents 0.1006 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.91 _reflns_number_total 7624 _reflns_number_gt 4451 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7624 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1402 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.2390 _refine_ls_wR_factor_gt 0.2089 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.3223(19) 0.7028(17) 0.2234(12) 0.114(7) Uani 1 1 d . . . H1A H -0.2875 0.7367 0.2554 0.172 Uiso 1 1 calc R . . H1B H -0.4031 0.6684 0.2500 0.172 Uiso 1 1 calc R . . H1C H -0.3525 0.7531 0.1795 0.172 Uiso 1 1 calc R . . C2 C -0.2388(14) 0.5700(10) 0.1543(7) 0.061(3) Uani 1 1 d . . . C3 C -0.3746(15) 0.5819(12) 0.1289(8) 0.073(4) Uani 1 1 d . . . H3 H -0.4507 0.6277 0.1443 0.088 Uiso 1 1 calc R . . C4 C -0.394(2) 0.5250(16) 0.0806(11) 0.102(6) Uani 1 1 d . . . H4 H -0.4817 0.5351 0.0608 0.123 Uiso 1 1 calc R . . C5 C -0.284(2) 0.4534(13) 0.0613(8) 0.084(5) Uani 1 1 d . . . H5 H -0.3003 0.4141 0.0297 0.101 Uiso 1 1 calc R . . C6 C -0.1454(16) 0.4377(10) 0.0889(7) 0.063(3) Uani 1 1 d . . . C7 C -0.1292(15) 0.4983(10) 0.1369(7) 0.058(3) Uani 1 1 d . . . C8 C -0.0403(17) 0.3645(11) 0.0627(7) 0.067(4) Uani 1 1 d . . . H8 H -0.0658 0.3386 0.0254 0.080 Uiso 1 1 calc R . . C9 C 0.174(2) 0.2513(17) 0.0495(11) 0.108(6) Uani 1 1 d . . . H9A H 0.1084 0.2112 0.0372 0.130 Uiso 1 1 calc R . . H9B H 0.2227 0.2871 0.0024 0.130 Uiso 1 1 calc R . . C10 C 0.281(3) 0.1803(18) 0.0900(13) 0.121(7) Uani 1 1 d . . . H10A H 0.3199 0.1282 0.0625 0.145 Uiso 1 1 calc R . . H10B H 0.2344 0.1455 0.1382 0.145 Uiso 1 1 calc R . . C11 C 0.401(3) 0.228(2) 0.1030(14) 0.136(9) Uani 1 1 d . . . H11A H 0.4387 0.2691 0.0551 0.163 Uiso 1 1 calc R . . H11B H 0.4770 0.1730 0.1204 0.163 Uiso 1 1 calc R . . C12 C 0.4698(19) 0.3035(16) 0.1915(11) 0.096(5) Uani 1 1 d . . . H12 H 0.5586 0.2656 0.1807 0.115 Uiso 1 1 calc R . . C13 C 0.4702(14) 0.3638(13) 0.2455(11) 0.087(5) Uani 1 1 d . . . C14 C 0.5939(17) 0.3496(16) 0.2828(12) 0.103(7) Uani 1 1 d . . . H14 H 0.6726 0.3015 0.2735 0.123 Uiso 1 1 calc R . . C15 C 0.598(2) 0.407(2) 0.3330(15) 0.129(9) Uani 1 1 d . . . H15 H 0.6809 0.3981 0.3571 0.155 Uiso 1 1 calc R . . C16 C 0.487(2) 0.4754(14) 0.3482(10) 0.094(6) Uani 1 1 d . . . H16 H 0.4929 0.5128 0.3828 0.113 Uiso 1 1 calc R . . C17 C 0.3621(17) 0.4920(12) 0.3137(8) 0.075(4) Uani 1 1 d . . . C18 C 0.3522(14) 0.4363(11) 0.2618(8) 0.068(4) Uani 1 1 d . . . C19 C 0.234(3) 0.6150(16) 0.3840(11) 0.117(7) Uani 1 1 d . . . H19A H 0.1448 0.6603 0.3862 0.176 Uiso 1 1 calc R . . H19B H 0.3142 0.6546 0.3735 0.176 Uiso 1 1 calc R . . H19C H 0.2410 0.5652 0.4314 0.176 Uiso 1 1 calc R . . C20 C 0.0784(15) 0.2594(11) 0.3360(8) 0.069(4) Uani 1 1 d . . . H20 H 0.1413 0.3015 0.3432 0.083 Uiso 1 1 calc R . . C21 C 0.0033(15) 0.2005(11) 0.3983(7) 0.063(3) Uani 1 1 d . . . H21 H 0.0136 0.2052 0.4463 0.076 Uiso 1 1 calc R . . C22 C -0.0890(13) 0.1333(10) 0.3887(7) 0.063(3) Uani 1 1 d . . . C23 C -0.1005(16) 0.1323(11) 0.3159(7) 0.069(4) Uani 1 1 d . . . H23 H -0.1591 0.0888 0.3066 0.083 Uiso 1 1 calc R . . C24 C -0.0276(15) 0.1938(10) 0.2578(7) 0.065(3) Uani 1 1 d . . . H24 H -0.0413 0.1918 0.2097 0.077 Uiso 1 1 calc R . . C25 C -0.1711(15) 0.0743(10) 0.4540(7) 0.064(3) Uani 1 1 d . . . C26 C -0.2157(14) -0.0225(11) 0.4629(7) 0.061(3) Uani 1 1 d . . . C27 C -0.1674(17) -0.0893(13) 0.4168(8) 0.077(4) Uani 1 1 d . . . H27 H -0.1042 -0.0639 0.3748 0.092 Uiso 1 1 calc R . . C28 C -0.198(2) -0.1881(13) 0.4232(8) 0.101(6) Uani 1 1 d . . . H28 H -0.1490 -0.2209 0.3869 0.122 Uiso 1 1 calc R . . C29 C -0.295(2) -0.2454(14) 0.4775(10) 0.097(5) Uani 1 1 d . . . H29 H -0.3099 -0.3078 0.4695 0.116 Uiso 1 1 calc R . . C30 C -0.370(2) -0.2196(14) 0.5408(10) 0.091(5) Uani 1 1 d . . . H30 H -0.4292 -0.2679 0.5691 0.109 Uiso 1 1 calc R . . C31 C -0.3735(16) -0.1366(12) 0.5700(8) 0.071(4) Uani 1 1 d . . . H31 H -0.4277 -0.1392 0.6165 0.085 Uiso 1 1 calc R . . C32 C -0.3040(14) -0.0456(11) 0.5377(7) 0.061(3) Uani 1 1 d . . . C33 C -0.3066(15) 0.0358(11) 0.5717(7) 0.065(3) Uani 1 1 d . . . C34 C -0.2242(15) 0.1089(12) 0.5222(7) 0.071(4) Uani 1 1 d . . . H34 H -0.2065 0.1697 0.5316 0.085 Uiso 1 1 calc R . . C35 C -0.3713(15) 0.0428(11) 0.6459(8) 0.068(4) Uani 1 1 d . . . C36 C -0.296(2) 0.0761(14) 0.6924(9) 0.089(5) Uani 1 1 d . . . H36 H -0.2036 0.0942 0.6756 0.107 Uiso 1 1 calc R . . C37 C -0.361(2) 0.0824(16) 0.7652(10) 0.106(6) Uani 1 1 d . . . H37 H -0.3065 0.1021 0.7957 0.128 Uiso 1 1 calc R . . C38 C -0.562(2) 0.0311(15) 0.7472(10) 0.094(5) Uani 1 1 d . . . H38 H -0.6562 0.0167 0.7650 0.113 Uiso 1 1 calc R . . C39 C -0.5102(17) 0.0185(13) 0.6787(9) 0.080(4) Uani 1 1 d . . . H39 H -0.5668 -0.0067 0.6523 0.096 Uiso 1 1 calc R . . N1 N 0.0862(14) 0.3289(9) 0.0837(6) 0.071(3) Uani 1 1 d . . . N2 N 0.3686(14) 0.2935(10) 0.1566(8) 0.081(4) Uani 1 1 d . . . N3 N 0.0625(11) 0.2573(9) 0.2636(6) 0.061(3) Uani 1 1 d . . . N4 N -0.4913(17) 0.0622(12) 0.7919(8) 0.092(4) Uani 1 1 d . . . N5 N -0.1178(17) 0.5249(13) 0.3745(7) 0.085(4) Uani 1 1 d . . . N6 N -0.0017(15) 0.8375(12) 0.2198(11) 0.090(4) Uani 1 1 d . . . N7 N 0.2579(15) 0.6980(11) 0.1041(8) 0.083(4) Uani 1 1 d . . . O1 O -0.2072(10) 0.6277(8) 0.2011(6) 0.075(3) Uani 1 1 d . . . O2 O -0.0008(9) 0.4922(7) 0.1652(5) 0.062(2) Uani 1 1 d . . . O3 O 0.2283(9) 0.4577(7) 0.2288(5) 0.068(2) Uani 1 1 d . . . O4 O 0.2389(12) 0.5626(9) 0.3259(5) 0.082(3) Uani 1 1 d . . . O5 O -0.0572(13) 0.4670(8) 0.3364(6) 0.084(3) Uani 1 1 d . . . O6 O -0.1082(14) 0.6214(10) 0.3483(6) 0.100(4) Uani 1 1 d . . . O7 O -0.197(2) 0.4956(14) 0.4324(7) 0.152(7) Uani 1 1 d . . . O8 O -0.0348(15) 0.7923(10) 0.1754(9) 0.115(4) Uani 1 1 d . . . O9 O 0.0559(15) 0.7731(11) 0.2741(7) 0.104(4) Uani 1 1 d . . . O10 O -0.0218(18) 0.9216(12) 0.2236(10) 0.134(5) Uani 1 1 d . . . O11 O 0.1496(15) 0.6588(10) 0.0954(5) 0.099(4) Uani 1 1 d . . . O12 O 0.2741(11) 0.6937(9) 0.1706(5) 0.081(3) Uani 1 1 d . . . O13 O 0.3371(16) 0.7409(12) 0.0511(7) 0.133(5) Uani 1 1 d . . . O14W O -0.1885(19) 1.1254(17) 0.1082(12) 0.219(12) Uani 1 1 d . . . Zn1 Zn 0.15628(15) 0.36297(12) 0.17417(8) 0.0586(4) Uani 1 1 d . . . Eu Eu 0.05514(7) 0.60594(6) 0.23006(4) 0.0572(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.070(11) 0.127(17) 0.141(17) -0.037(14) -0.005(11) 0.006(11) C2 0.057(8) 0.061(8) 0.063(8) -0.005(6) -0.019(6) -0.010(6) C3 0.050(7) 0.071(10) 0.082(9) 0.010(8) -0.009(7) -0.005(7) C4 0.080(11) 0.114(15) 0.126(15) -0.027(12) -0.062(11) -0.008(11) C5 0.111(13) 0.083(12) 0.068(9) -0.001(8) -0.039(9) -0.042(10) C6 0.084(9) 0.049(8) 0.051(7) 0.006(6) -0.017(7) -0.015(7) C7 0.070(8) 0.044(7) 0.055(7) 0.010(6) -0.016(6) -0.020(6) C8 0.085(10) 0.070(9) 0.045(7) -0.013(6) -0.002(7) -0.012(8) C9 0.128(17) 0.115(16) 0.089(12) -0.049(12) 0.011(12) -0.018(13) C10 0.123(18) 0.113(17) 0.115(16) -0.038(14) 0.038(14) -0.007(15) C11 0.100(16) 0.130(19) 0.16(2) -0.056(17) 0.035(15) 0.024(14) C12 0.060(10) 0.109(15) 0.103(13) -0.009(11) 0.011(9) -0.011(9) C13 0.041(8) 0.080(11) 0.116(13) 0.027(10) -0.018(8) -0.011(7) C14 0.048(9) 0.101(15) 0.135(17) 0.026(12) -0.030(10) -0.013(9) C15 0.070(12) 0.122(19) 0.17(2) 0.045(16) -0.054(14) -0.039(13) C16 0.095(13) 0.085(12) 0.097(12) 0.031(9) -0.042(10) -0.056(11) C17 0.073(10) 0.077(10) 0.068(9) 0.020(8) -0.023(7) -0.033(8) C18 0.049(7) 0.072(9) 0.068(8) 0.023(7) -0.017(6) -0.026(7) C19 0.150(19) 0.117(16) 0.099(13) -0.036(12) -0.045(13) -0.014(14) C20 0.059(8) 0.071(9) 0.070(9) 0.000(7) -0.005(6) -0.018(7) C21 0.066(8) 0.066(9) 0.054(7) -0.004(6) -0.005(6) -0.018(7) C22 0.050(7) 0.062(8) 0.054(7) 0.012(6) -0.001(5) 0.003(6) C23 0.072(9) 0.069(9) 0.063(8) -0.001(7) -0.022(7) -0.012(7) C24 0.073(9) 0.053(8) 0.052(7) 0.009(6) 0.009(6) -0.015(7) C25 0.069(8) 0.048(8) 0.062(8) 0.009(6) -0.010(6) -0.006(6) C26 0.057(7) 0.062(9) 0.058(7) -0.003(6) -0.010(6) -0.006(6) C27 0.089(11) 0.084(11) 0.051(7) -0.005(7) -0.005(7) -0.017(8) C28 0.18(2) 0.068(11) 0.055(8) -0.014(8) 0.009(10) -0.027(12) C29 0.125(15) 0.079(12) 0.089(12) -0.002(9) -0.010(11) -0.052(11) C30 0.098(12) 0.091(13) 0.079(10) -0.007(9) 0.009(9) -0.034(10) C31 0.071(9) 0.075(10) 0.064(8) -0.009(7) 0.001(7) -0.019(7) C32 0.060(7) 0.066(9) 0.047(6) 0.009(6) -0.001(5) -0.019(6) C33 0.073(9) 0.061(9) 0.050(7) 0.002(6) 0.001(6) -0.014(7) C34 0.072(9) 0.074(10) 0.062(8) -0.010(7) 0.006(7) -0.018(7) C35 0.069(9) 0.070(9) 0.061(8) -0.015(7) 0.004(7) -0.010(7) C36 0.095(12) 0.094(13) 0.077(10) -0.018(9) 0.002(9) -0.020(9) C37 0.124(17) 0.113(16) 0.074(11) -0.013(10) -0.003(11) -0.017(12) C38 0.077(11) 0.105(14) 0.089(12) -0.025(10) 0.014(9) 0.003(10) C39 0.074(10) 0.089(12) 0.076(10) -0.018(8) -0.001(8) -0.017(8) N1 0.084(9) 0.070(8) 0.057(6) -0.012(6) 0.012(6) -0.029(7) N2 0.070(8) 0.069(8) 0.090(9) -0.004(7) 0.008(7) -0.007(6) N3 0.048(6) 0.070(7) 0.056(6) -0.002(5) 0.001(5) -0.007(5) N4 0.092(10) 0.104(11) 0.071(8) -0.020(8) 0.008(8) -0.009(8) N5 0.112(11) 0.089(11) 0.060(7) -0.007(7) -0.005(7) -0.052(9) N6 0.076(9) 0.058(9) 0.142(14) -0.046(10) 0.015(9) -0.020(7) N7 0.071(8) 0.101(11) 0.073(9) -0.014(7) 0.003(7) -0.023(7) O1 0.065(6) 0.075(7) 0.089(7) -0.031(5) -0.018(5) 0.008(5) O2 0.053(5) 0.063(6) 0.073(5) -0.015(4) -0.017(4) -0.012(4) O3 0.047(5) 0.085(7) 0.068(5) -0.002(5) -0.019(4) -0.016(4) O4 0.093(8) 0.097(8) 0.062(6) -0.004(5) -0.035(5) -0.028(6) O5 0.106(8) 0.064(7) 0.081(7) -0.018(6) 0.002(6) -0.017(6) O6 0.115(9) 0.098(9) 0.085(7) -0.031(7) 0.032(7) -0.036(7) O7 0.201(17) 0.188(16) 0.072(8) -0.028(9) 0.052(9) -0.108(13) O8 0.109(10) 0.073(8) 0.164(13) -0.026(8) -0.015(9) -0.018(7) O9 0.117(10) 0.098(10) 0.091(8) 0.000(7) -0.012(7) -0.028(8) O10 0.138(13) 0.074(9) 0.191(16) -0.029(10) -0.022(11) -0.015(8) O11 0.133(10) 0.121(10) 0.049(5) -0.016(6) -0.002(6) -0.049(8) O12 0.071(6) 0.106(8) 0.064(6) -0.003(5) -0.005(5) -0.034(6) O13 0.118(10) 0.166(14) 0.081(8) 0.021(8) 0.036(7) -0.050(10) O14W 0.109(12) 0.23(2) 0.23(2) 0.131(18) -0.045(13) -0.040(13) Zn1 0.0511(8) 0.0576(10) 0.0578(8) -0.0015(7) 0.0020(6) -0.0090(7) Eu 0.0545(4) 0.0630(5) 0.0520(4) -0.0071(3) -0.0061(3) -0.0131(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 C1 O1 1.45(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.359(19) . ? C2 C3 1.398(18) . ? C2 O1 1.400(16) . ? C3 C4 1.37(2) . ? C3 H3 0.9300 . ? C4 C5 1.37(3) . ? C4 H4 0.9300 . ? C5 C6 1.44(2) . ? C5 H5 0.9300 . ? C6 C7 1.398(18) . ? C6 C8 1.41(2) . ? C7 O2 1.370(15) . ? C8 N1 1.285(18) . ? C8 H8 0.9300 . ? C9 C10 1.42(3) . ? C9 N1 1.45(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.46(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.47(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.27(2) . ? C12 C13 1.45(3) . ? C12 H12 0.9300 . ? C13 C14 1.40(2) . ? C13 C18 1.41(2) . ? C14 C15 1.37(3) . ? C14 H14 0.9300 . ? C15 C16 1.33(3) . ? C15 H15 0.9300 . ? C16 C17 1.38(2) . ? C16 H16 0.9300 . ? C17 C18 1.39(2) . ? C17 O4 1.41(2) . ? C18 O3 1.351(15) . ? C19 O4 1.43(2) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 1.383(17) . ? C20 C21 1.388(18) . ? C20 H20 0.9300 . ? C21 C22 1.42(2) . ? C21 H21 0.9300 . ? C22 C23 1.376(18) . ? C22 C25 1.455(18) . ? C23 C24 1.348(18) . ? C23 H23 0.9300 . ? C24 N3 1.336(18) . ? C24 H24 0.9300 . ? C25 C26 1.401(19) . ? C25 C34 1.456(19) . ? C26 C27 1.38(2) . ? C26 C32 1.493(17) . ? C27 C28 1.38(2) . ? C27 H27 0.9300 . ? C28 C29 1.41(2) . ? C28 H28 0.9300 . ? C29 C30 1.37(2) . ? C29 H29 0.9300 . ? C30 C31 1.36(2) . ? C30 H30 0.9300 . ? C31 C32 1.434(19) . ? C31 H31 0.9300 . ? C32 C33 1.402(19) . ? C33 C34 1.407(19) . ? C33 C35 1.441(18) . ? C34 H34 0.9300 . ? C35 C36 1.39(2) . ? C35 C39 1.41(2) . ? C36 C37 1.41(2) . ? C36 H36 0.9300 . ? C37 N4 1.30(2) . ? C37 H37 0.9300 . ? C38 N4 1.32(2) . ? C38 C39 1.34(2) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? N1 Zn1 2.075(12) . ? N2 Zn1 2.081(13) . ? N3 Zn1 2.074(11) . ? N5 O5 1.211(17) . ? N5 O7 1.224(17) . ? N5 O6 1.280(17) . ? N5 Eu 2.962(13) . ? N6 O10 1.142(17) . ? N6 O8 1.246(19) . ? N6 O9 1.271(19) . ? N6 Eu 3.050(15) . ? N7 O13 1.217(16) . ? N7 O12 1.251(15) . ? N7 O11 1.271(17) . ? N7 Eu 2.927(13) . ? O1 Eu 2.557(9) . ? O2 Zn1 2.084(9) . ? O2 Eu 2.350(8) . ? O3 Zn1 2.075(10) . ? O3 Eu 2.370(9) . ? O4 Eu 2.556(9) . ? O5 Eu 2.573(11) . ? O6 Eu 2.522(10) . ? O8 Eu 2.513(13) . ? O9 Eu 2.601(14) . ? O11 Eu 2.482(10) . ? O12 Eu 2.510(10) . ? Zn1 Eu 3.6418(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 121.5(13) . . ? C7 C2 O1 115.4(11) . . ? C3 C2 O1 123.0(13) . . ? C4 C3 C2 118.9(15) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 120.5(14) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 121.3(14) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C8 127.7(13) . . ? C7 C6 C5 116.5(14) . . ? C8 C6 C5 115.8(13) . . ? C2 C7 O2 116.9(11) . . ? C2 C7 C6 121.1(12) . . ? O2 C7 C6 121.9(12) . . ? N1 C8 C6 128.4(13) . . ? N1 C8 H8 115.8 . . ? C6 C8 H8 115.8 . . ? C10 C9 N1 119.2(16) . . ? C10 C9 H9A 107.5 . . ? N1 C9 H9A 107.5 . . ? C10 C9 H9B 107.5 . . ? N1 C9 H9B 107.5 . . ? H9A C9 H9B 107.0 . . ? C9 C10 C11 114(2) . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 N2 117.3(17) . . ? C10 C11 H11A 108.0 . . ? N2 C11 H11A 108.0 . . ? C10 C11 H11B 108.0 . . ? N2 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? N2 C12 C13 131.0(16) . . ? N2 C12 H12 114.5 . . ? C13 C12 H12 114.5 . . ? C14 C13 C18 119(2) . . ? C14 C13 C12 118.5(18) . . ? C18 C13 C12 122.9(14) . . ? C15 C14 C13 120(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C14 121.6(19) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 121(2) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C18 119.6(17) . . ? C16 C17 O4 125.5(17) . . ? C18 C17 O4 114.9(12) . . ? O3 C18 C17 116.7(14) . . ? O3 C18 C13 124.0(15) . . ? C17 C18 C13 119.3(14) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 121.9(13) . . ? N3 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C22 119.9(13) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 116.5(12) . . ? C23 C22 C25 123.8(14) . . ? C21 C22 C25 119.6(12) . . ? C24 C23 C22 120.5(14) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? N3 C24 C23 125.5(14) . . ? N3 C24 H24 117.2 . . ? C23 C24 H24 117.2 . . ? C26 C25 C22 127.5(13) . . ? C26 C25 C34 107.9(12) . . ? C22 C25 C34 124.6(13) . . ? C27 C26 C25 125.9(13) . . ? C27 C26 C32 127.0(13) . . ? C25 C26 C32 106.3(12) . . ? C28 C27 C26 130.1(15) . . ? C28 C27 H27 114.9 . . ? C26 C27 H27 114.9 . . ? C27 C28 C29 128.6(16) . . ? C27 C28 H28 115.7 . . ? C29 C28 H28 115.7 . . ? C30 C29 C28 127.4(17) . . ? C30 C29 H29 116.3 . . ? C28 C29 H29 116.3 . . ? C31 C30 C29 132.1(16) . . ? C31 C30 H30 114.0 . . ? C29 C30 H30 114.0 . . ? C30 C31 C32 128.0(14) . . ? C30 C31 H31 116.0 . . ? C32 C31 H31 116.0 . . ? C33 C32 C31 125.5(12) . . ? C33 C32 C26 108.7(11) . . ? C31 C32 C26 125.8(13) . . ? C32 C33 C34 107.7(11) . . ? C32 C33 C35 127.5(12) . . ? C34 C33 C35 124.6(14) . . ? C33 C34 C25 109.4(13) . . ? C33 C34 H34 125.3 . . ? C25 C34 H34 125.3 . . ? C36 C35 C39 113.6(13) . . ? C36 C35 C33 120.5(14) . . ? C39 C35 C33 125.9(14) . . ? C35 C36 C37 120.0(18) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? N4 C37 C36 124(2) . . ? N4 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? N4 C38 C39 125.6(17) . . ? N4 C38 H38 117.2 . . ? C39 C38 H38 117.2 . . ? C38 C39 C35 121.1(16) . . ? C38 C39 H39 119.4 . . ? C35 C39 H39 119.4 . . ? C8 N1 C9 118.1(14) . . ? C8 N1 Zn1 122.3(10) . . ? C9 N1 Zn1 119.0(12) . . ? C12 N2 C11 119.2(16) . . ? C12 N2 Zn1 122.8(13) . . ? C11 N2 Zn1 118.0(13) . . ? C24 N3 C20 115.6(11) . . ? C24 N3 Zn1 125.0(9) . . ? C20 N3 Zn1 119.0(9) . . ? C37 N4 C38 115.6(15) . . ? O5 N5 O7 122.3(16) . . ? O5 N5 O6 117.3(13) . . ? O7 N5 O6 120.0(17) . . ? O5 N5 Eu 59.7(7) . . ? O7 N5 Eu 175.9(15) . . ? O6 N5 Eu 57.7(7) . . ? O10 N6 O8 133(2) . . ? O10 N6 O9 115.7(19) . . ? O8 N6 O9 110.9(14) . . ? O10 N6 Eu 173.0(16) . . ? O8 N6 Eu 53.3(9) . . ? O9 N6 Eu 57.6(8) . . ? O13 N7 O12 122.1(15) . . ? O13 N7 O11 122.2(15) . . ? O12 N7 O11 115.7(12) . . ? O13 N7 Eu 176.7(12) . . ? O12 N7 Eu 58.4(7) . . ? O11 N7 Eu 57.2(7) . . ? C2 O1 C1 117.5(12) . . ? C2 O1 Eu 117.6(7) . . ? C1 O1 Eu 124.7(10) . . ? C7 O2 Zn1 122.9(8) . . ? C7 O2 Eu 125.8(8) . . ? Zn1 O2 Eu 110.3(3) . . ? C18 O3 Zn1 125.3(9) . . ? C18 O3 Eu 124.8(9) . . ? Zn1 O3 Eu 109.8(3) . . ? C17 O4 C19 118.3(13) . . ? C17 O4 Eu 116.7(8) . . ? C19 O4 Eu 124.4(11) . . ? N5 O5 Eu 96.3(9) . . ? N5 O6 Eu 96.9(9) . . ? N6 O8 Eu 103.2(12) . . ? N6 O9 Eu 98.0(10) . . ? N7 O11 Eu 97.2(8) . . ? N7 O12 Eu 96.4(8) . . ? N3 Zn1 N1 101.3(4) . . ? N3 Zn1 O3 101.7(4) . . ? N1 Zn1 O3 154.6(4) . . ? N3 Zn1 N2 104.0(4) . . ? N1 Zn1 N2 95.3(6) . . ? O3 Zn1 N2 89.5(5) . . ? N3 Zn1 O2 101.9(4) . . ? N1 Zn1 O2 89.9(4) . . ? O3 Zn1 O2 74.9(3) . . ? N2 Zn1 O2 152.0(4) . . ? N3 Zn1 Eu 103.1(3) . . ? N1 Zn1 Eu 125.2(4) . . ? O3 Zn1 Eu 37.8(2) . . ? N2 Zn1 Eu 124.5(4) . . ? O2 Zn1 Eu 37.2(2) . . ? O2 Eu O3 64.8(3) . . ? O2 Eu O11 70.2(4) . . ? O3 Eu O11 83.4(4) . . ? O2 Eu O12 114.1(3) . . ? O3 Eu O12 80.9(3) . . ? O11 Eu O12 50.6(4) . . ? O2 Eu O8 113.7(4) . . ? O3 Eu O8 150.5(4) . . ? O11 Eu O8 69.5(5) . . ? O12 Eu O8 73.1(4) . . ? O2 Eu O6 116.5(4) . . ? O3 Eu O6 120.5(4) . . ? O11 Eu O6 156.0(5) . . ? O12 Eu O6 129.4(4) . . ? O8 Eu O6 87.3(5) . . ? O2 Eu O4 125.9(3) . . ? O3 Eu O4 63.4(3) . . ? O11 Eu O4 117.3(4) . . ? O12 Eu O4 71.6(3) . . ? O8 Eu O4 118.9(4) . . ? O6 Eu O4 78.8(4) . . ? O2 Eu O1 63.3(3) . . ? O3 Eu O1 125.9(3) . . ? O11 Eu O1 93.0(4) . . ? O12 Eu O1 134.9(3) . . ? O8 Eu O1 68.8(4) . . ? O6 Eu O1 72.2(4) . . ? O4 Eu O1 149.7(4) . . ? O2 Eu O5 77.3(3) . . ? O3 Eu O5 77.7(3) . . ? O11 Eu O5 146.9(4) . . ? O12 Eu O5 148.1(4) . . ? O8 Eu O5 131.7(4) . . ? O6 Eu O5 49.4(4) . . ? O4 Eu O5 77.7(4) . . ? O1 Eu O5 77.0(4) . . ? O2 Eu O9 161.0(4) . . ? O3 Eu O9 132.8(4) . . ? O11 Eu O9 101.8(4) . . ? O12 Eu O9 68.4(4) . . ? O8 Eu O9 47.8(4) . . ? O6 Eu O9 64.1(4) . . ? O4 Eu O9 73.2(4) . . ? O1 Eu O9 100.9(4) . . ? O5 Eu O9 110.9(4) . . ? O2 Eu N7 92.5(4) . . ? O3 Eu N7 81.5(4) . . ? O11 Eu N7 25.5(4) . . ? O12 Eu N7 25.1(3) . . ? O8 Eu N7 69.0(4) . . ? O6 Eu N7 148.6(4) . . ? O4 Eu N7 94.4(4) . . ? O1 Eu N7 114.8(4) . . ? O5 Eu N7 159.2(4) . . ? O9 Eu N7 84.5(4) . . ? O2 Eu N5 96.9(4) . . ? O3 Eu N5 98.4(4) . . ? O11 Eu N5 164.9(4) . . ? O12 Eu N5 144.4(3) . . ? O8 Eu N5 110.8(5) . . ? O6 Eu N5 25.4(4) . . ? O4 Eu N5 76.4(4) . . ? O1 Eu N5 73.7(4) . . ? O5 Eu N5 24.0(3) . . ? O9 Eu N5 88.0(4) . . ? N7 Eu N5 169.5(4) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.91 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.478 _refine_diff_density_min -1.619 _refine_diff_density_rms 0.171 _database_code_depnum_ccdc_archive 'CCDC 949948' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Cu2 Gd N7 O14' _chemical_formula_weight 964.86 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' Cu Cu 0.3201 1.2651 '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 9.0187(18) _cell_length_b 9.5438(19) _cell_length_c 10.835(2) _cell_angle_alpha 87.160(17) _cell_angle_beta 89.548(17) _cell_angle_gamma 61.353(15) _cell_volume 817.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6349 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.21 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 473 _exptl_absorpt_coefficient_mu 3.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0841 _exptl_absorpt_correction_T_max 0.2210 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7726 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 28.21 _reflns_number_total 3894 _reflns_number_gt 2939 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3894 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.6565(9) -0.0638(10) 0.6219(7) 0.0772(19) Uani 1 1 d . . . H1A H 1.6935 -0.1454 0.5630 0.116 Uiso 1 1 calc R . . H1B H 1.7478 -0.0867 0.6783 0.116 Uiso 1 1 calc R . . H1C H 1.6217 0.0381 0.5792 0.116 Uiso 1 1 calc R . . C2 C 1.5110(7) -0.0595(8) 0.6920(6) 0.0618(14) Uani 1 1 d . . . C3 C 1.4379(8) 0.0523(8) 0.7836(6) 0.0688(16) Uani 1 1 d . . . H3 H 1.4812 0.1223 0.7931 0.083 Uiso 1 1 calc R . . C4 C 1.3095(7) 0.0688(7) 0.8605(5) 0.0548(12) Uani 1 1 d . A . C5 C 1.2554(7) 0.1886(6) 0.9560(5) 0.0544(12) Uani 1 1 d . . . C6 C 1.3314(9) 0.2818(8) 0.9734(7) 0.0752(18) Uani 1 1 d . . . H6 H 1.4179 0.2744 0.9223 0.090 Uiso 1 1 calc R . . C7 C 1.2779(10) 0.3850(8) 1.0667(7) 0.0792(19) Uani 1 1 d . . . H7 H 1.3297 0.4469 1.0806 0.095 Uiso 1 1 calc R . . C8 C 1.1500(9) 0.3976(7) 1.1390(7) 0.0721(17) Uani 1 1 d . . . H8 H 1.1112 0.4699 1.2013 0.087 Uiso 1 1 calc R . . C9 C 1.0775(7) 0.3013(6) 1.1191(6) 0.0560(13) Uani 1 1 d . . . C10 C 0.9394(7) 0.3006(7) 1.1959(6) 0.0576(13) Uani 1 1 d . A . C11 C 0.8727(9) 0.4066(8) 1.2868(7) 0.0715(17) Uani 1 1 d . . . H11 H 0.9165 0.4763 1.2953 0.086 Uiso 1 1 calc R . . C12 C 0.7444(9) 0.4220(8) 1.3693(7) 0.0703(17) Uani 1 1 d . . . C13 C 0.6846(11) 0.5516(10) 1.4584(8) 0.098(3) Uani 1 1 d . . . H13A H 0.5966 0.5496 1.5077 0.147 Uiso 1 1 calc R . . H13B H 0.6416 0.6532 1.4137 0.147 Uiso 1 1 calc R . . H13C H 0.7771 0.5354 1.5111 0.147 Uiso 1 1 calc R . . C14 C 1.0323(19) 0.1868(16) 0.6135(13) 0.073(3) Uani 0.50 1 d P . . C15 C 1.0000 0.0000 0.5000 0.074(2) Uani 1 2 d S . . N1 N 1.1299(6) 0.1960(5) 1.0287(4) 0.0539(10) Uani 1 1 d . . . N2 N 1.2610(7) -0.2426(7) 1.1637(6) 0.0708(14) Uani 1 1 d . . . N3 N 1.012(2) 0.3061(16) 0.6417(16) 0.110(5) Uani 0.50 1 d P . . N4 N 1.0680(8) 0.0258(8) 0.5885(6) 0.0809(16) Uani 1 1 d . . . O1 O 1.4589(5) -0.1549(5) 0.6635(4) 0.0679(11) Uani 1 1 d . . . O2 O 1.2289(5) -0.0119(5) 0.8576(4) 0.0587(9) Uani 1 1 d . . . O3 O 0.8945(5) 0.1964(5) 1.1697(4) 0.0651(11) Uani 1 1 d . . . O4 O 0.6790(6) 0.3344(6) 1.3714(5) 0.0757(13) Uani 1 1 d . . . O6 O 1.3741(8) -0.3415(7) 1.2265(6) 0.108(2) Uani 1 1 d . A . O5 O 1.2670(13) -0.1319(14) 1.1167(12) 0.090(3) Uani 0.57 1 d P A 1 O7 O 1.1141(13) -0.2405(12) 1.1495(12) 0.096(3) Uani 0.57 1 d P A 1 O5A O 1.183(2) -0.0996(16) 1.1824(14) 0.092(4) Uani 0.43 1 d P A 2 O7A O 1.223(2) -0.2661(13) 1.0546(14) 0.102(5) Uani 0.43 1 d P A 2 Cu1 Cu 1.26370(8) -0.15959(8) 0.73082(6) 0.0582(2) Uani 1 1 d . . . Gd1 Gd 1.0000 0.0000 1.0000 0.04953(14) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.071(4) 0.117(5) 0.067(4) -0.016(4) 0.016(3) -0.062(4) C2 0.053(3) 0.083(4) 0.058(3) -0.008(3) 0.010(2) -0.039(3) C3 0.074(4) 0.094(4) 0.066(4) -0.017(3) 0.014(3) -0.061(3) C4 0.055(3) 0.065(3) 0.054(3) -0.002(2) 0.001(2) -0.037(2) C5 0.059(3) 0.061(3) 0.054(3) -0.007(2) 0.006(2) -0.036(2) C6 0.077(4) 0.080(4) 0.093(5) -0.022(3) 0.026(4) -0.056(3) C7 0.096(5) 0.086(4) 0.087(5) -0.028(4) 0.023(4) -0.067(4) C8 0.080(4) 0.068(3) 0.086(5) -0.028(3) 0.020(3) -0.048(3) C9 0.061(3) 0.057(3) 0.061(3) -0.010(2) 0.006(3) -0.037(2) C10 0.064(3) 0.060(3) 0.059(3) -0.009(2) 0.006(3) -0.038(3) C11 0.084(4) 0.072(4) 0.074(4) -0.026(3) 0.021(3) -0.048(3) C12 0.071(4) 0.072(4) 0.076(4) -0.028(3) 0.024(3) -0.039(3) C13 0.113(6) 0.105(5) 0.102(6) -0.051(5) 0.053(5) -0.069(5) C14 0.081(8) 0.076(8) 0.068(8) -0.009(6) 0.000(7) -0.042(7) C15 0.079(6) 0.097(7) 0.064(6) -0.011(5) 0.011(5) -0.055(5) N1 0.055(2) 0.058(2) 0.059(3) -0.013(2) 0.007(2) -0.034(2) N2 0.062(3) 0.068(3) 0.086(4) 0.001(3) -0.011(3) -0.035(3) N3 0.116(11) 0.083(8) 0.132(13) -0.032(8) -0.030(10) -0.046(8) N4 0.078(4) 0.099(4) 0.073(4) -0.004(3) -0.006(3) -0.048(3) O1 0.065(2) 0.089(3) 0.068(3) -0.024(2) 0.021(2) -0.050(2) O2 0.064(2) 0.069(2) 0.059(2) -0.0138(18) 0.0118(18) -0.0442(19) O3 0.072(2) 0.078(2) 0.068(3) -0.028(2) 0.025(2) -0.054(2) O4 0.084(3) 0.081(3) 0.085(3) -0.038(2) 0.037(2) -0.054(2) O6 0.097(4) 0.094(4) 0.125(5) 0.027(3) -0.044(4) -0.042(3) O5 0.067(5) 0.103(7) 0.118(9) 0.041(7) -0.022(5) -0.060(5) O7 0.092(6) 0.090(6) 0.131(9) 0.017(6) -0.030(6) -0.065(5) O5A 0.098(10) 0.077(8) 0.088(9) 0.000(7) -0.024(8) -0.031(8) O7A 0.123(11) 0.062(6) 0.103(10) -0.020(6) -0.040(9) -0.027(7) Cu1 0.0594(4) 0.0684(4) 0.0598(4) -0.0191(3) 0.0150(3) -0.0398(3) Gd1 0.0496(2) 0.0546(2) 0.0537(2) -0.00937(15) 0.00474(15) -0.03193(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.496(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.259(7) . ? C2 C3 1.407(9) . ? C3 C4 1.372(9) . ? C3 H3 0.9300 . ? C4 O2 1.290(7) . ? C4 C5 1.480(8) . ? C5 N1 1.350(8) . ? C5 C6 1.378(8) . ? C6 C7 1.364(9) . ? C6 H6 0.9300 . ? C7 C8 1.349(10) . ? C7 H7 0.9300 . ? C8 C9 1.385(8) . ? C8 H8 0.9300 . ? C9 N1 1.351(7) . ? C9 C10 1.496(9) . ? C10 O3 1.284(7) . ? C10 C11 1.364(8) . ? C11 C12 1.413(10) . ? C11 H11 0.9300 . ? C12 O4 1.231(8) . ? C12 C13 1.491(9) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N3 1.120(17) . ? C14 N4 1.450(15) . ? C15 N4 1.239(6) 2_756 ? C15 N4 1.239(6) . ? N1 Gd1 2.671(4) . ? N2 O5 1.175(11) . ? N2 O6 1.191(7) . ? N2 O5A 1.226(14) . ? N2 O7A 1.294(13) . ? N2 O7 1.325(11) . ? N2 Gd1 2.912(6) . ? N4 Cu1 2.324(6) . ? O1 Cu1 1.920(4) . ? O2 Cu1 1.932(4) . ? O2 Gd1 2.529(4) . ? O3 Cu1 1.934(4) 2_757 ? O3 Gd1 2.530(4) . ? O4 Cu1 1.904(4) 2_757 ? O5 Gd1 2.443(9) . ? O7 Gd1 2.518(10) . ? O5A Gd1 2.428(13) . ? O7A Gd1 2.411(11) . ? Cu1 O4 1.904(4) 2_757 ? Cu1 O3 1.934(4) 2_757 ? Gd1 O7A 2.411(11) 2_757 ? Gd1 O5A 2.428(13) 2_757 ? Gd1 O5 2.443(9) 2_757 ? Gd1 O7 2.518(10) 2_757 ? Gd1 O2 2.529(4) 2_757 ? Gd1 O3 2.530(4) 2_757 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.8(5) . . ? O1 C2 C1 117.7(6) . . ? C3 C2 C1 118.5(6) . . ? C4 C3 C2 126.7(6) . . ? C4 C3 H3 116.7 . . ? C2 C3 H3 116.7 . . ? O2 C4 C3 125.7(5) . . ? O2 C4 C5 115.6(5) . . ? C3 C4 C5 118.8(5) . . ? N1 C5 C6 122.0(5) . . ? N1 C5 C4 115.1(5) . . ? C6 C5 C4 122.8(5) . . ? C7 C6 C5 119.0(6) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C8 C7 C6 120.3(6) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 119.0(6) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? N1 C9 C8 122.0(5) . . ? N1 C9 C10 114.2(5) . . ? C8 C9 C10 123.8(5) . . ? O3 C10 C11 125.5(6) . . ? O3 C10 C9 115.5(5) . . ? C11 C10 C9 119.0(5) . . ? C10 C11 C12 127.0(6) . . ? C10 C11 H11 116.5 . . ? C12 C11 H11 116.5 . . ? O4 C12 C11 123.5(5) . . ? O4 C12 C13 118.3(6) . . ? C11 C12 C13 118.1(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 N4 174.3(16) . . ? N4 C15 N4 180.000(1) 2_756 . ? C5 N1 C9 117.7(5) . . ? C5 N1 Gd1 120.8(3) . . ? C9 N1 Gd1 121.5(4) . . ? O5 N2 O6 122.0(7) . . ? O5 N2 O5A 48.3(9) . . ? O6 N2 O5A 125.5(9) . . ? O5 N2 O7A 85.8(10) . . ? O6 N2 O7A 124.0(8) . . ? O5A N2 O7A 109.5(9) . . ? O5 N2 O7 114.5(8) . . ? O6 N2 O7 123.3(8) . . ? O5A N2 O7 88.5(10) . . ? O7A N2 O7 62.6(9) . . ? O5 N2 Gd1 55.3(5) . . ? O6 N2 Gd1 176.5(6) . . ? O5A N2 Gd1 55.0(7) . . ? O7A N2 Gd1 54.8(5) . . ? O7 N2 Gd1 59.7(5) . . ? C15 N4 C14 121.1(7) . . ? C15 N4 Cu1 127.9(4) . . ? C14 N4 Cu1 110.9(7) . . ? C2 O1 Cu1 125.1(4) . . ? C4 O2 Cu1 122.5(4) . . ? C4 O2 Gd1 128.3(3) . . ? Cu1 O2 Gd1 109.19(17) . . ? C10 O3 Cu1 122.1(4) . 2_757 ? C10 O3 Gd1 128.7(4) . . ? Cu1 O3 Gd1 109.07(17) 2_757 . ? C12 O4 Cu1 126.0(4) . 2_757 ? N2 O5 Gd1 101.4(6) . . ? N2 O7 Gd1 93.3(6) . . ? N2 O5A Gd1 100.5(8) . . ? N2 O7A Gd1 99.2(6) . . ? O4 Cu1 O1 85.53(19) 2_757 . ? O4 Cu1 O2 169.6(2) 2_757 . ? O1 Cu1 O2 95.20(18) . . ? O4 Cu1 O3 95.36(19) 2_757 2_757 ? O1 Cu1 O3 166.0(2) . 2_757 ? O2 Cu1 O3 81.44(17) . 2_757 ? O4 Cu1 N4 93.5(2) 2_757 . ? O1 Cu1 N4 96.8(2) . . ? O2 Cu1 N4 96.8(2) . . ? O3 Cu1 N4 97.1(2) 2_757 . ? O7A Gd1 O7A 180.000(2) . 2_757 ? O7A Gd1 O5A 129.7(4) . 2_757 ? O7A Gd1 O5A 50.3(4) 2_757 2_757 ? O7A Gd1 O5A 50.3(4) . . ? O7A Gd1 O5A 129.7(4) 2_757 . ? O5A Gd1 O5A 180.000(2) 2_757 . ? O7A Gd1 O5 139.4(4) . 2_757 ? O7A Gd1 O5 40.6(4) 2_757 2_757 ? O5A Gd1 O5 23.3(4) 2_757 2_757 ? O5A Gd1 O5 156.7(4) . 2_757 ? O7A Gd1 O5 40.6(4) . . ? O7A Gd1 O5 139.4(4) 2_757 . ? O5A Gd1 O5 156.7(4) 2_757 . ? O5A Gd1 O5 23.3(4) . . ? O5 Gd1 O5 180.000(1) 2_757 . ? O7A Gd1 O7 32.0(5) . . ? O7A Gd1 O7 148.0(5) 2_757 . ? O5A Gd1 O7 137.8(5) 2_757 . ? O5A Gd1 O7 42.2(5) . . ? O5 Gd1 O7 129.8(3) 2_757 . ? O5 Gd1 O7 50.2(3) . . ? O7A Gd1 O7 148.0(5) . 2_757 ? O7A Gd1 O7 32.0(5) 2_757 2_757 ? O5A Gd1 O7 42.2(5) 2_757 2_757 ? O5A Gd1 O7 137.8(5) . 2_757 ? O5 Gd1 O7 50.2(3) 2_757 2_757 ? O5 Gd1 O7 129.8(3) . 2_757 ? O7 Gd1 O7 180.000(1) . 2_757 ? O7A Gd1 O2 100.2(5) . 2_757 ? O7A Gd1 O2 79.8(5) 2_757 2_757 ? O5A Gd1 O2 94.6(5) 2_757 2_757 ? O5A Gd1 O2 85.4(5) . 2_757 ? O5 Gd1 O2 72.4(3) 2_757 2_757 ? O5 Gd1 O2 107.6(3) . 2_757 ? O7 Gd1 O2 69.2(3) . 2_757 ? O7 Gd1 O2 110.8(3) 2_757 2_757 ? O7A Gd1 O2 79.8(5) . . ? O7A Gd1 O2 100.2(5) 2_757 . ? O5A Gd1 O2 85.4(5) 2_757 . ? O5A Gd1 O2 94.6(5) . . ? O5 Gd1 O2 107.6(3) 2_757 . ? O5 Gd1 O2 72.4(3) . . ? O7 Gd1 O2 110.8(3) . . ? O7 Gd1 O2 69.2(3) 2_757 . ? O2 Gd1 O2 180.0 2_757 . ? O7A Gd1 O3 117.0(3) . . ? O7A Gd1 O3 63.0(3) 2_757 . ? O5A Gd1 O3 112.0(3) 2_757 . ? O5A Gd1 O3 68.0(3) . . ? O5 Gd1 O3 94.1(4) 2_757 . ? O5 Gd1 O3 85.9(4) . . ? O7 Gd1 O3 93.5(3) . . ? O7 Gd1 O3 86.5(3) 2_757 . ? O2 Gd1 O3 59.79(13) 2_757 . ? O2 Gd1 O3 120.21(13) . . ? O7A Gd1 O3 63.0(3) . 2_757 ? O7A Gd1 O3 117.0(3) 2_757 2_757 ? O5A Gd1 O3 68.0(3) 2_757 2_757 ? O5A Gd1 O3 112.0(3) . 2_757 ? O5 Gd1 O3 85.9(4) 2_757 2_757 ? O5 Gd1 O3 94.1(4) . 2_757 ? O7 Gd1 O3 86.5(3) . 2_757 ? O7 Gd1 O3 93.5(3) 2_757 2_757 ? O2 Gd1 O3 120.21(13) 2_757 2_757 ? O2 Gd1 O3 59.79(13) . 2_757 ? O3 Gd1 O3 180.000(1) . 2_757 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.736 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 949949' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 Dy N3 Ni2 O23' _chemical_formula_weight 1200.59 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.051(3) _cell_length_b 30.966(6) _cell_length_c 16.201(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.23(3) _cell_angle_gamma 90.00 _cell_volume 7539(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50889 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 33.5 _exptl_crystal_description prism _exptl_crystal_colour green-yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 1.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe ipds II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73858 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13228 _reflns_number_gt 8311 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-area _computing_cell_refinement X-area _computing_data_reduction X-area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13228 _refine_ls_number_parameters 644 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1515 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2833(5) 0.4452(3) 0.7228(4) 0.0633(17) Uani 1 1 d . . . C2 C 0.3108(5) 0.4018(2) 0.6960(4) 0.0609(17) Uani 1 1 d . . . C3 C 0.2797(7) 0.3862(3) 0.6211(6) 0.096(3) Uani 1 1 d . . . H3 H 0.2378 0.4017 0.5886 0.115 Uiso 1 1 calc R . . C4 C 0.3116(9) 0.3469(4) 0.5940(7) 0.121(4) Uani 1 1 d . . . H4 H 0.2924 0.3363 0.5424 0.145 Uiso 1 1 calc R . . C5 C 0.3704(9) 0.3242(3) 0.6425(8) 0.106(4) Uani 1 1 d . . . C6 C 0.4044(8) 0.3384(3) 0.7163(8) 0.113(3) Uani 1 1 d . . . H6 H 0.4469 0.3225 0.7471 0.135 Uiso 1 1 calc R . . C7 C 0.3734(6) 0.3779(3) 0.7450(6) 0.091(3) Uani 1 1 d . . . H7 H 0.3941 0.3884 0.7963 0.109 Uiso 1 1 calc R . . C8 C 0.4126(7) 0.2117(3) 0.5946(7) 0.114(4) Uani 1 1 d . . . H8 H 0.4518 0.2162 0.5531 0.137 Uiso 1 1 calc R . . C9 C 0.3895(6) 0.1706(3) 0.6176(6) 0.095(3) Uani 1 1 d . . . H9 H 0.4160 0.1473 0.5927 0.114 Uiso 1 1 calc R . . C10 C 0.3290(5) 0.1629(2) 0.6756(5) 0.0691(18) Uani 1 1 d . . . C11 C 0.2904(6) 0.1985(2) 0.7122(6) 0.084(2) Uani 1 1 d . . . H11 H 0.2478 0.1943 0.7508 0.100 Uiso 1 1 calc R . . C12 C 0.3147(7) 0.2398(3) 0.6918(6) 0.101(3) Uani 1 1 d . . . H12 H 0.2893 0.2634 0.7170 0.122 Uiso 1 1 calc R . . C13 C 0.3043(5) 0.1181(2) 0.6975(4) 0.0622(17) Uani 1 1 d . . . C14 C -0.0527(5) 0.0514(4) 0.7819(5) 0.096(3) Uani 1 1 d . . . H14 H -0.0846 0.0504 0.8293 0.115 Uiso 1 1 calc R . . C15 C -0.0965(6) 0.0553(4) 0.7066(6) 0.113(4) Uani 1 1 d . . . H15 H -0.1581 0.0577 0.7020 0.135 Uiso 1 1 calc R . . C16 C -0.0474(5) 0.0555(4) 0.6372(5) 0.096(3) Uani 1 1 d . . . H16 H -0.0756 0.0582 0.5848 0.116 Uiso 1 1 calc R . . C17 C 0.0395(5) 0.0490(3) 0.7884(4) 0.0689(19) Uani 1 1 d . . . C18 C 0.0935(5) 0.0486(3) 0.8680(4) 0.0666(18) Uani 1 1 d . . . C19 C 0.0521(6) 0.0541(3) 0.9414(5) 0.086(2) Uani 1 1 d . . . H19 H -0.0098 0.0548 0.9379 0.104 Uiso 1 1 calc R . . C20 C 0.0940(7) 0.0587(3) 1.0205(5) 0.087(2) Uani 1 1 d . . . C21 C 0.0338(7) 0.0627(4) 1.0933(5) 0.122(4) Uani 1 1 d . . . H21A H 0.0698 0.0660 1.1437 0.184 Uiso 1 1 calc R . . H21B H -0.0022 0.0372 1.0965 0.184 Uiso 1 1 calc R . . H21C H -0.0040 0.0875 1.0853 0.184 Uiso 1 1 calc R . . C22 C 0.1030(5) 0.0480(2) 0.5757(4) 0.0629(17) Uani 1 1 d . . . C23 C 0.0665(5) 0.0526(3) 0.4957(5) 0.082(2) Uani 1 1 d . . . H23 H 0.0072 0.0612 0.4902 0.098 Uiso 1 1 calc R . . C24 C 0.1099(6) 0.0456(3) 0.4216(5) 0.081(2) Uani 1 1 d . . . C25 C 0.0640(7) 0.0600(4) 0.3421(5) 0.118(4) Uani 1 1 d . . . H25A H 0.1012 0.0539 0.2973 0.178 Uiso 1 1 calc R . . H25B H 0.0527 0.0905 0.3444 0.178 Uiso 1 1 calc R . . H25C H 0.0087 0.0448 0.3336 0.178 Uiso 1 1 calc R . . C26 C 0.4325(7) -0.0820(4) 0.4100(6) 0.113(3) Uani 1 1 d . . . H26A H 0.3935 -0.0838 0.3611 0.169 Uiso 1 1 calc R . . H26B H 0.4387 -0.1101 0.4348 0.169 Uiso 1 1 calc R . . H26C H 0.4898 -0.0718 0.3956 0.169 Uiso 1 1 calc R . . C27 C 0.3937(6) -0.0511(3) 0.4708(5) 0.081(2) Uani 1 1 d . . . C28 C 0.4391(5) -0.0437(3) 0.5488(5) 0.080(2) Uani 1 1 d . . . H28 H 0.4957 -0.0556 0.5559 0.095 Uiso 1 1 calc R . . C29 C 0.4096(5) -0.0210(2) 0.6153(5) 0.0644(18) Uani 1 1 d . . . C30 C 0.4702(5) -0.0120(3) 0.6881(5) 0.0675(18) Uani 1 1 d . . . C31 C 0.5613(5) -0.0215(3) 0.6933(6) 0.091(3) Uani 1 1 d . . . H31 H 0.5867 -0.0367 0.6511 0.109 Uiso 1 1 calc R . . C32 C 0.6123(6) -0.0082(4) 0.7600(7) 0.112(3) Uani 1 1 d . . . H32 H 0.6728 -0.0144 0.7640 0.135 Uiso 1 1 calc R . . C33 C 0.5745(6) 0.0143(3) 0.8219(6) 0.098(3) Uani 1 1 d . . . H33 H 0.6092 0.0237 0.8677 0.117 Uiso 1 1 calc R . . C34 C 0.4832(5) 0.0228(3) 0.8152(5) 0.072(2) Uani 1 1 d . . . C35 C 0.4350(5) 0.0450(3) 0.8801(5) 0.0705(19) Uani 1 1 d . . . C40 C 0.0448(5) 0.0516(3) 0.6464(4) 0.0662(18) Uani 1 1 d . . . C36 C 0.4791(6) 0.0557(3) 0.9532(5) 0.086(2) Uani 1 1 d . . . H36 H 0.5399 0.0502 0.9567 0.103 Uiso 1 1 calc R . . C37 C 0.4437(6) 0.0741(3) 1.0245(5) 0.086(2) Uani 1 1 d . . . C38 C 0.5064(7) 0.0877(4) 1.0940(5) 0.113(3) Uani 1 1 d . . . H38A H 0.4734 0.0994 1.1378 0.170 Uiso 1 1 calc R . . H38B H 0.5461 0.1093 1.0748 0.170 Uiso 1 1 calc R . . H38C H 0.5402 0.0632 1.1141 0.170 Uiso 1 1 calc R . . N1 N 0.4320(4) 0.01046(19) 0.7484(4) 0.0629(14) Uani 1 1 d . . . N2 N 0.0885(3) 0.04766(19) 0.7210(3) 0.0587(13) Uani 1 1 d . . . O1 O 0.3514(3) 0.05174(16) 0.8611(3) 0.0665(12) Uani 1 1 d . . . O2 O 0.3623(4) 0.0791(2) 1.0345(3) 0.0938(18) Uani 1 1 d . . . O3 O 0.1767(4) 0.0608(2) 1.0382(3) 0.0953(18) Uani 1 1 d . . . O4 O 0.1781(3) 0.04229(16) 0.8603(3) 0.0670(12) Uani 1 1 d . . . O6 O 0.3303(3) -0.00586(16) 0.6205(3) 0.0637(12) Uani 1 1 d . . . O7 O 0.3230(4) -0.0331(2) 0.4469(3) 0.0864(16) Uani 1 1 d . . . O8 O 0.1854(3) 0.03908(15) 0.5967(3) 0.0624(12) Uani 1 1 d . . . O9 O 0.2444(3) 0.11060(15) 0.7460(3) 0.0696(13) Uani 1 1 d . . . O10 O 0.3436(3) 0.08701(15) 0.6652(3) 0.0690(12) Uani 1 1 d . . . O11 O 0.2220(3) 0.46492(16) 0.6837(3) 0.0693(12) Uani 1 1 d . . . O12 O 0.4073(5) 0.28573(18) 0.6098(5) 0.125(2) Uani 1 1 d U . . O13 O 0.2430(4) 0.1243(2) 0.9168(4) 0.1021(19) Uani 1 1 d . . . O14 O 0.2944(4) -0.00579(19) 0.9800(3) 0.0805(15) Uani 1 1 d . . . O15 O 0.1734(3) -0.04709(18) 0.5419(3) 0.0784(14) Uani 1 1 d . . . C39 C 0.3758(8) 0.2458(3) 0.6347(7) 0.125(2) Uani 1 1 d U . . O16 O 0.3382(3) 0.06029(19) 0.5005(3) 0.0802(15) Uani 1 1 d . . . O17 O 0.3224(3) 0.46300(16) 0.7874(3) 0.0719(13) Uani 1 1 d . . . O18 O 0.1847(4) 0.0272(2) 0.4174(3) 0.0859(16) Uani 1 1 d . . . Ni1 Ni 0.25587(6) 0.00640(3) 0.51593(5) 0.0670(3) Uani 1 1 d . . . Ni2 Ni 0.26652(7) 0.05895(4) 0.95270(6) 0.0742(3) Uani 1 1 d . . . Dy Dy 0.26123(2) 0.031423(10) 0.73445(2) 0.05716(12) Uani 1 1 d . . . O2A O 0.2040(7) -0.0563(4) 1.0827(7) 0.185(4) Uani 1 1 d U . . O3A O 0.3104(6) -0.0993(3) 1.0668(6) 0.154(3) Uani 1 1 d U . . N3 N 0.2394(11) -0.0899(5) 1.0978(9) 0.182(4) Uani 1 1 d U . . O1A O 0.2051(11) -0.1174(5) 1.1361(10) 0.279(6) Uani 1 1 d U . . O1W O 0.3055(19) 0.1274(7) 0.3896(11) 0.260(13) Uani 0.69(2) 1 d P A 1 O1AW O 0.408(3) 0.1429(10) 0.4049(17) 0.19(2) Uani 0.31(2) 1 d P A 1 O2W O 0.3836(19) -0.1776(13) 0.641(2) 0.36(2) Uani 0.69(2) 1 d P A 2 O2AW O 0.380(3) -0.141(2) 0.709(3) 0.26(3) Uani 0.31(2) 1 d P A 2 O3W O 0.2354(16) -0.1282(5) 0.513(2) 0.314(18) Uani 0.69(2) 1 d P A 3 O3AW O 0.122(4) -0.1452(12) 0.524(3) 0.30(4) Uani 0.31(2) 1 d P A 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.053(4) 0.074(4) 0.064(4) 0.004(4) 0.010(4) -0.001(3) C2 0.067(4) 0.055(4) 0.060(4) 0.004(3) 0.000(3) -0.003(3) C3 0.124(8) 0.074(5) 0.090(6) -0.019(5) 0.006(5) 0.014(5) C4 0.175(12) 0.085(7) 0.102(7) -0.008(6) 0.018(7) 0.017(7) C5 0.140(9) 0.050(5) 0.133(9) 0.002(6) 0.069(8) -0.003(5) C6 0.117(8) 0.068(6) 0.153(10) 0.006(6) 0.011(7) 0.013(5) C7 0.089(6) 0.065(5) 0.119(7) -0.001(5) -0.003(5) 0.004(4) C8 0.135(9) 0.065(5) 0.150(9) 0.000(6) 0.078(8) 0.008(5) C9 0.114(7) 0.056(4) 0.121(7) -0.006(5) 0.050(6) 0.005(4) C10 0.065(4) 0.064(4) 0.079(5) 0.003(4) 0.010(4) 0.003(3) C11 0.089(6) 0.060(4) 0.105(6) -0.009(4) 0.032(5) 0.000(4) C12 0.109(7) 0.065(5) 0.135(8) -0.008(5) 0.050(6) 0.011(5) C13 0.064(4) 0.051(4) 0.070(4) 0.002(3) -0.001(4) 0.007(3) C14 0.050(4) 0.162(9) 0.078(5) -0.013(6) 0.014(4) 0.008(5) C15 0.047(5) 0.211(12) 0.080(6) -0.017(7) -0.003(4) 0.014(6) C16 0.053(5) 0.163(9) 0.071(5) -0.009(6) -0.005(4) 0.017(5) C17 0.055(4) 0.090(5) 0.062(4) -0.001(4) 0.008(3) 0.003(4) C18 0.057(4) 0.084(5) 0.061(4) -0.006(4) 0.015(3) -0.001(4) C19 0.072(5) 0.117(7) 0.071(5) -0.008(5) 0.021(4) 0.004(5) C20 0.085(6) 0.107(7) 0.071(5) -0.007(5) 0.017(5) 0.003(5) C21 0.112(8) 0.186(12) 0.073(6) -0.020(7) 0.035(6) -0.014(8) C22 0.055(4) 0.072(4) 0.061(4) 0.000(3) 0.002(3) 0.007(3) C23 0.060(5) 0.122(7) 0.064(5) 0.006(5) -0.001(4) 0.025(5) C24 0.068(5) 0.113(7) 0.061(5) 0.006(4) -0.001(4) 0.007(5) C25 0.106(8) 0.188(12) 0.060(5) 0.016(6) -0.005(5) 0.044(8) C26 0.103(7) 0.120(8) 0.119(8) -0.032(6) 0.037(6) 0.025(6) C27 0.075(5) 0.082(5) 0.088(6) -0.011(5) 0.024(5) 0.005(4) C28 0.060(5) 0.085(5) 0.093(6) -0.013(4) 0.006(4) 0.022(4) C29 0.055(4) 0.065(4) 0.074(5) 0.002(3) 0.011(3) 0.006(3) C30 0.051(4) 0.077(5) 0.074(5) 0.001(4) 0.008(3) 0.010(3) C31 0.058(5) 0.118(7) 0.096(6) -0.008(5) 0.002(4) 0.025(5) C32 0.057(5) 0.162(10) 0.116(8) -0.014(7) -0.014(5) 0.024(6) C33 0.060(5) 0.123(8) 0.109(7) -0.012(6) -0.013(5) 0.009(5) C34 0.051(4) 0.080(5) 0.084(5) -0.002(4) -0.003(4) 0.000(3) C35 0.055(4) 0.079(5) 0.078(5) 0.001(4) -0.002(4) -0.002(4) C40 0.056(4) 0.080(5) 0.062(4) -0.004(4) 0.002(3) 0.011(4) C36 0.063(5) 0.107(7) 0.088(6) 0.001(5) -0.006(4) 0.002(5) C37 0.080(6) 0.096(6) 0.081(6) -0.004(5) -0.007(5) -0.011(5) C38 0.098(7) 0.156(10) 0.082(6) -0.019(6) -0.026(5) -0.021(7) N1 0.050(3) 0.069(4) 0.069(4) 0.004(3) 0.002(3) 0.005(3) N2 0.048(3) 0.070(3) 0.058(3) -0.003(3) 0.006(3) 0.007(3) O1 0.056(3) 0.075(3) 0.068(3) -0.006(2) -0.002(2) 0.000(2) O2 0.081(4) 0.124(5) 0.075(3) -0.019(3) -0.005(3) 0.000(4) O3 0.084(4) 0.133(5) 0.070(3) -0.016(3) 0.010(3) 0.008(4) O4 0.059(3) 0.080(3) 0.062(3) -0.002(2) 0.005(2) 0.002(2) O6 0.047(3) 0.073(3) 0.072(3) -0.006(2) 0.006(2) 0.011(2) O7 0.078(4) 0.109(4) 0.073(3) -0.021(3) 0.008(3) 0.018(3) O8 0.051(3) 0.076(3) 0.061(3) 0.002(2) 0.007(2) 0.008(2) O9 0.072(3) 0.063(3) 0.076(3) 0.005(2) 0.022(3) 0.002(2) O10 0.070(3) 0.056(3) 0.082(3) -0.001(2) 0.012(3) 0.005(2) O11 0.065(3) 0.068(3) 0.075(3) 0.000(3) 0.001(2) 0.007(3) O12 0.171(5) 0.051(2) 0.161(5) 0.004(3) 0.089(4) 0.007(3) O13 0.115(5) 0.086(4) 0.107(4) -0.009(3) 0.016(4) 0.013(4) O14 0.079(3) 0.094(4) 0.067(3) 0.012(3) -0.015(3) 0.000(3) O15 0.072(3) 0.082(3) 0.081(3) -0.008(3) -0.001(3) -0.002(3) C39 0.171(5) 0.051(2) 0.161(5) 0.004(3) 0.089(4) 0.007(3) O16 0.066(3) 0.094(4) 0.082(3) -0.002(3) 0.023(3) 0.007(3) O17 0.074(3) 0.067(3) 0.074(3) -0.004(3) -0.001(3) 0.002(3) O18 0.071(3) 0.121(5) 0.066(3) -0.005(3) 0.008(3) 0.015(3) Ni1 0.0585(5) 0.0832(6) 0.0597(5) -0.0053(5) 0.0052(4) 0.0114(5) Ni2 0.0696(6) 0.0913(7) 0.0614(5) -0.0086(5) 0.0001(5) 0.0024(5) Dy 0.05259(18) 0.05736(18) 0.0618(2) 0.00011(16) 0.00562(13) 0.00230(16) O2A 0.182(9) 0.167(9) 0.219(9) 0.056(8) 0.123(7) 0.045(7) O3A 0.138(7) 0.182(8) 0.144(7) 0.015(6) 0.013(6) 0.007(6) N3 0.185(9) 0.175(10) 0.198(9) 0.044(8) 0.128(8) 0.004(8) O1A 0.296(13) 0.231(13) 0.329(14) 0.060(11) 0.195(11) 0.012(11) O1W 0.36(3) 0.22(2) 0.192(16) 0.107(15) -0.070(17) -0.03(2) O1AW 0.31(5) 0.16(3) 0.12(2) -0.054(19) 0.14(3) -0.09(3) O2W 0.27(3) 0.43(5) 0.40(5) 0.18(4) 0.13(3) 0.08(3) O2AW 0.19(4) 0.38(8) 0.23(4) -0.04(5) 0.08(3) 0.10(4) O3W 0.23(2) 0.084(10) 0.65(5) 0.026(18) 0.18(3) 0.036(12) O3AW 0.43(9) 0.11(3) 0.34(6) -0.03(3) -0.24(6) 0.00(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 C1 O11 1.249(8) . ? C1 O17 1.295(8) . ? C1 C2 1.478(10) . ? C1 Dy 2.848(8) 2_556 ? C2 C3 1.365(11) . ? C2 C7 1.407(11) . ? C3 C4 1.388(13) . ? C3 H3 0.9300 . ? C4 C5 1.348(15) . ? C4 H4 0.9300 . ? C5 C6 1.347(15) . ? C5 O12 1.430(10) . ? C6 C7 1.398(13) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C39 1.372(12) . ? C8 C9 1.375(12) . ? C8 H8 0.9300 . ? C9 C10 1.367(10) . ? C9 H9 0.9300 . ? C10 C11 1.393(10) . ? C10 C13 1.485(10) . ? C11 C12 1.377(11) . ? C11 H11 0.9300 . ? C12 C39 1.354(12) . ? C12 H12 0.9300 . ? C13 O9 1.250(8) . ? C13 O10 1.258(8) . ? C13 Dy 2.832(7) . ? C14 C15 1.358(12) . ? C14 C17 1.387(10) . ? C14 H14 0.9300 . ? C15 C16 1.380(11) . ? C15 H15 0.9300 . ? C16 C40 1.394(10) . ? C16 H16 0.9300 . ? C17 N2 1.352(8) . ? C17 C18 1.485(10) . ? C18 O4 1.302(8) . ? C18 C19 1.384(10) . ? C19 C20 1.404(12) . ? C19 H19 0.9300 . ? C20 O3 1.263(10) . ? C20 C21 1.533(11) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O8 1.297(8) . ? C22 C23 1.385(10) . ? C22 C40 1.485(9) . ? C23 C24 1.416(11) . ? C23 H23 0.9300 . ? C24 O18 1.268(9) . ? C24 C25 1.495(11) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.514(11) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O7 1.244(10) . ? C27 C28 1.421(12) . ? C28 C29 1.381(10) . ? C28 H28 0.9300 . ? C29 O6 1.289(8) . ? C29 C30 1.476(10) . ? C30 N1 1.353(9) . ? C30 C31 1.401(10) . ? C31 C32 1.354(12) . ? C31 H31 0.9300 . ? C32 C33 1.369(13) . ? C32 H32 0.9300 . ? C33 C34 1.398(11) . ? C33 H33 0.9300 . ? C34 N1 1.347(9) . ? C34 C35 1.479(11) . ? C35 O1 1.295(8) . ? C35 C36 1.365(11) . ? C40 N2 1.349(9) . ? C36 C37 1.419(12) . ? C36 H36 0.9300 . ? C37 O2 1.254(10) . ? C37 C38 1.489(11) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? N1 Dy 2.649(5) . ? N2 Dy 2.644(5) . ? O1 Ni2 2.025(5) . ? O1 Dy 2.477(5) . ? O2 Ni2 2.002(6) . ? O3 Ni2 1.991(6) . ? O4 Ni2 2.013(5) . ? O4 Dy 2.475(5) . ? O6 Ni1 2.014(5) . ? O6 Dy 2.457(4) . ? O7 Ni1 1.974(5) . ? O8 Ni1 2.005(4) . ? O8 Dy 2.461(5) . ? O9 Dy 2.473(5) . ? O10 Dy 2.432(5) . ? O11 Dy 2.455(5) 2_556 ? O12 C39 1.393(10) . ? O13 Ni2 2.130(6) . ? O14 Ni2 2.090(6) . ? O15 Ni1 2.126(5) . ? O16 Ni1 2.102(6) . ? O17 Dy 2.480(5) 2_556 ? O18 Ni1 1.979(5) . ? Dy O11 2.455(5) 2_546 ? Dy O17 2.480(5) 2_546 ? Dy C1 2.848(8) 2_546 ? O2A N3 1.188(15) . ? O3A N3 1.240(14) . ? N3 O1A 1.188(15) . ? O1W O1AW 1.62(4) . ? O2W O2AW 1.59(6) . ? O3W O3AW 1.80(7) . ? 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 O11 C1 O17 119.4(7) . . ? O11 C1 C2 120.4(7) . . ? O17 C1 C2 120.1(6) . . ? O11 C1 Dy 59.2(4) . 2_556 ? O17 C1 Dy 60.5(4) . 2_556 ? C2 C1 Dy 175.7(5) . 2_556 ? C3 C2 C7 120.0(8) . . ? C3 C2 C1 119.7(7) . . ? C7 C2 C1 120.1(7) . . ? C2 C3 C4 118.9(10) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.0(10) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 123.4(9) . . ? C6 C5 O12 117.7(12) . . ? C4 C5 O12 118.4(12) . . ? C5 C6 C7 117.6(10) . . ? C5 C6 H6 121.2 . . ? C7 C6 H6 121.2 . . ? C6 C7 C2 119.9(9) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C39 C8 C9 117.9(8) . . ? C39 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? C10 C9 C8 122.5(8) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 117.6(7) . . ? C9 C10 C13 120.9(7) . . ? C11 C10 C13 121.5(7) . . ? C12 C11 C10 120.7(8) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C39 C12 C11 119.3(8) . . ? C39 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? O9 C13 O10 119.5(6) . . ? O9 C13 C10 121.5(6) . . ? O10 C13 C10 119.0(7) . . ? O9 C13 Dy 60.7(3) . . ? O10 C13 Dy 58.8(4) . . ? C10 C13 Dy 177.8(5) . . ? C15 C14 C17 120.4(8) . . ? C15 C14 H14 119.8 . . ? C17 C14 H14 119.8 . . ? C14 C15 C16 118.5(8) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C15 C16 C40 119.2(7) . . ? C15 C16 H16 120.4 . . ? C40 C16 H16 120.4 . . ? N2 C17 C14 122.0(7) . . ? N2 C17 C18 113.8(6) . . ? C14 C17 C18 124.2(7) . . ? O4 C18 C19 126.3(7) . . ? O4 C18 C17 114.1(6) . . ? C19 C18 C17 119.6(7) . . ? C18 C19 C20 126.6(8) . . ? C18 C19 H19 116.7 . . ? C20 C19 H19 116.7 . . ? O3 C20 C19 126.8(8) . . ? O3 C20 C21 116.0(8) . . ? C19 C20 C21 117.1(8) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O8 C22 C23 126.2(7) . . ? O8 C22 C40 114.2(6) . . ? C23 C22 C40 119.6(6) . . ? C22 C23 C24 126.8(7) . . ? C22 C23 H23 116.6 . . ? C24 C23 H23 116.6 . . ? O18 C24 C23 124.6(7) . . ? O18 C24 C25 117.2(7) . . ? C23 C24 C25 118.2(8) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O7 C27 C28 124.4(7) . . ? O7 C27 C26 115.8(8) . . ? C28 C27 C26 119.7(8) . . ? C29 C28 C27 128.1(7) . . ? C29 C28 H28 116.0 . . ? C27 C28 H28 116.0 . . ? O6 C29 C28 125.2(7) . . ? O6 C29 C30 114.3(6) . . ? C28 C29 C30 120.6(6) . . ? N1 C30 C31 121.2(7) . . ? N1 C30 C29 113.9(6) . . ? C31 C30 C29 124.5(7) . . ? C32 C31 C30 119.6(8) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.9(8) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 119.1(8) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? N1 C34 C33 121.5(8) . . ? N1 C34 C35 115.0(6) . . ? C33 C34 C35 123.5(7) . . ? O1 C35 C36 125.8(8) . . ? O1 C35 C34 114.5(6) . . ? C36 C35 C34 119.7(7) . . ? N2 C40 C16 122.5(7) . . ? N2 C40 C22 114.0(6) . . ? C16 C40 C22 123.4(7) . . ? C35 C36 C37 128.1(8) . . ? C35 C36 H36 115.9 . . ? C37 C36 H36 115.9 . . ? O2 C37 C36 124.7(8) . . ? O2 C37 C38 116.7(8) . . ? C36 C37 C38 118.6(9) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 N1 C30 118.6(6) . . ? C34 N1 Dy 120.4(5) . . ? C30 N1 Dy 120.9(4) . . ? C17 N2 C40 117.4(6) . . ? C17 N2 Dy 121.2(4) . . ? C40 N2 Dy 121.2(4) . . ? C35 O1 Ni2 119.2(5) . . ? C35 O1 Dy 129.4(5) . . ? Ni2 O1 Dy 107.23(19) . . ? C37 O2 Ni2 123.2(5) . . ? C20 O3 Ni2 122.7(5) . . ? C18 O4 Ni2 120.0(4) . . ? C18 O4 Dy 130.0(4) . . ? Ni2 O4 Dy 107.7(2) . . ? C29 O6 Ni1 119.1(4) . . ? C29 O6 Dy 130.7(4) . . ? Ni1 O6 Dy 107.74(18) . . ? C27 O7 Ni1 123.9(5) . . ? C22 O8 Ni1 118.0(4) . . ? C22 O8 Dy 130.3(4) . . ? Ni1 O8 Dy 107.91(19) . . ? C13 O9 Dy 93.2(4) . . ? C13 O10 Dy 94.9(4) . . ? C1 O11 Dy 94.9(4) . 2_556 ? C39 O12 C5 119.1(7) . . ? C12 C39 C8 121.8(8) . . ? C12 C39 O12 125.1(8) . . ? C8 C39 O12 113.1(8) . . ? C1 O17 Dy 92.5(4) . 2_556 ? C24 O18 Ni1 123.0(5) . . ? O7 Ni1 O18 90.9(2) . . ? O7 Ni1 O8 171.7(2) . . ? O18 Ni1 O8 94.6(2) . . ? O7 Ni1 O6 94.7(2) . . ? O18 Ni1 O6 171.8(2) . . ? O8 Ni1 O6 80.56(18) . . ? O7 Ni1 O16 95.8(2) . . ? O18 Ni1 O16 86.6(2) . . ? O8 Ni1 O16 90.8(2) . . ? O6 Ni1 O16 86.9(2) . . ? O7 Ni1 O15 87.2(2) . . ? O18 Ni1 O15 96.8(2) . . ? O8 Ni1 O15 85.9(2) . . ? O6 Ni1 O15 89.4(2) . . ? O16 Ni1 O15 175.4(2) . . ? O3 Ni2 O2 91.3(3) . . ? O3 Ni2 O4 94.5(2) . . ? O2 Ni2 O4 173.3(2) . . ? O3 Ni2 O1 174.2(2) . . ? O2 Ni2 O1 93.4(2) . . ? O4 Ni2 O1 81.08(19) . . ? O3 Ni2 O14 90.9(3) . . ? O2 Ni2 O14 91.8(2) . . ? O4 Ni2 O14 91.6(2) . . ? O1 Ni2 O14 85.5(2) . . ? O3 Ni2 O13 93.1(3) . . ? O2 Ni2 O13 89.2(3) . . ? O4 Ni2 O13 87.0(2) . . ? O1 Ni2 O13 90.4(2) . . ? O14 Ni2 O13 175.8(2) . . ? O10 Dy O11 143.46(16) . 2_546 ? O10 Dy O6 74.80(16) . . ? O11 Dy O6 88.67(16) 2_546 . ? O10 Dy O8 74.69(16) . . ? O11 Dy O8 126.83(16) 2_546 . ? O6 Dy O8 63.78(15) . . ? O10 Dy O9 52.42(15) . . ? O11 Dy O9 143.00(16) 2_546 . ? O6 Dy O9 124.90(16) . . ? O8 Dy O9 85.91(16) . . ? O10 Dy O4 125.33(16) . . ? O11 Dy O4 73.16(16) 2_546 . ? O6 Dy O4 159.70(16) . . ? O8 Dy O4 120.25(15) . . ? O9 Dy O4 75.17(16) . . ? O10 Dy O1 86.14(17) . . ? O11 Dy O1 74.36(17) 2_546 . ? O6 Dy O1 120.42(15) . . ? O8 Dy O1 158.69(17) . . ? O9 Dy O1 74.89(17) . . ? O4 Dy O1 64.02(15) . . ? O10 Dy O17 143.77(16) . 2_546 ? O11 Dy O17 52.88(17) 2_546 2_546 ? O6 Dy O17 73.98(16) . 2_546 ? O8 Dy O17 75.33(16) . 2_546 ? O9 Dy O17 143.56(16) . 2_546 ? O4 Dy O17 87.58(17) . 2_546 ? O1 Dy O17 125.84(16) . 2_546 ? O10 Dy N2 110.59(17) . . ? O11 Dy N2 105.94(17) 2_546 . ? O6 Dy N2 118.90(16) . . ? O8 Dy N2 60.23(15) . . ? O9 Dy N2 73.34(17) . . ? O4 Dy N2 60.09(16) . . ? O1 Dy N2 120.66(16) . . ? O17 Dy N2 70.24(17) 2_546 . ? O10 Dy N1 72.26(17) . . ? O11 Dy N1 71.25(17) 2_546 . ? O6 Dy N1 59.94(17) . . ? O8 Dy N1 119.96(16) . . ? O9 Dy N1 109.86(17) . . ? O4 Dy N1 119.78(17) . . ? O1 Dy N1 60.51(17) . . ? O17 Dy N1 106.58(18) 2_546 . ? N2 Dy N1 176.77(18) . . ? O10 Dy C13 26.28(17) . . ? O11 Dy C13 153.01(19) 2_546 . ? O6 Dy C13 100.08(19) . . ? O8 Dy C13 79.46(18) . . ? O9 Dy C13 26.15(17) . . ? O4 Dy C13 100.22(19) . . ? O1 Dy C13 79.23(18) . . ? O17 Dy C13 154.11(19) 2_546 . ? N2 Dy C13 92.18(19) . . ? N1 Dy C13 91.01(19) . . ? O10 Dy C1 155.35(17) . 2_546 ? O11 Dy C1 25.92(17) 2_546 2_546 ? O6 Dy C1 81.81(18) . 2_546 ? O8 Dy C1 101.97(19) . 2_546 ? O9 Dy C1 152.20(17) . 2_546 ? O4 Dy C1 77.90(18) . 2_546 ? O1 Dy C1 99.33(19) . 2_546 ? O17 Dy C1 27.03(17) 2_546 2_546 ? N2 Dy C1 87.40(19) . 2_546 ? N1 Dy C1 89.43(19) . 2_546 ? C13 Dy C1 178.0(2) . 2_546 ? O1A N3 O2A 122.1(16) . . ? O1A N3 O3A 116.9(17) . . ? O2A N3 O3A 120.5(13) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.804 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 949950'