# 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_I-A #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H42 Cu7 N14 Nd3 O22' _chemical_formula_sum 'C58 H42 Cu7 N14 Nd3 O22' _chemical_formula_weight 2164.63 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9085(14) _cell_length_b 17.017(2) _cell_length_c 17.936(2) _cell_angle_alpha 74.992(2) _cell_angle_beta 90.255(2) _cell_angle_gamma 88.732(2) _cell_volume 3509.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 12631 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 25.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2094 _exptl_absorpt_coefficient_mu 4.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.368 _exptl_absorpt_correction_T_max 0.420 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18172 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.40 _reflns_number_total 12631 _reflns_number_gt 9188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0000P)^2^+13.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12631 _refine_ls_number_parameters 931 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.006 _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 -0.0258(7) 1.1011(5) 0.4766(5) 0.049(2) Uani 1 1 d . . . C2 C 0.3286(7) 1.0481(5) 0.5017(4) 0.046(2) Uani 1 1 d . . . C3 C 0.6441(7) 1.1873(6) 0.5144(5) 0.046(2) Uani 1 1 d . . . C4 C -0.1362(8) 0.3156(5) 0.5306(5) 0.050(2) Uani 1 1 d . . . C5 C 0.2754(7) 0.4986(5) 0.5076(5) 0.050(2) Uani 1 1 d U . . C6 C 0.5794(8) 0.6771(7) 0.5038(5) 0.067(2) Uani 1 1 d . A . C7 C 0.7696(7) 1.2810(5) 0.2721(4) 0.044(2) Uani 1 1 d . . . H7 H 0.8438 1.2619 0.2762 0.053 Uiso 1 1 calc R . . C8 C 0.7249(6) 1.3129(5) 0.1999(4) 0.043(2) Uani 1 1 d . . . H8 H 0.7687 1.3173 0.1563 0.051 Uiso 1 1 calc R . . C9 C 0.6141(6) 1.3383(4) 0.1931(4) 0.0340(18) Uani 1 1 d . . . C10 C 0.5536(7) 1.3316(6) 0.2588(4) 0.055(3) Uani 1 1 d . . . H10 H 0.4782 1.3479 0.2563 0.066 Uiso 1 1 calc R . . C11 C 0.6066(7) 1.3004(6) 0.3288(4) 0.058(3) Uani 1 1 d . . . H11 H 0.5648 1.2965 0.3733 0.070 Uiso 1 1 calc R . . C12 C 0.5621(7) 1.3798(4) 0.1143(4) 0.0327(18) Uani 1 1 d . . . C13 C -0.0676(8) 1.0424(6) 0.6674(5) 0.065(3) Uani 1 1 d . . . H13 H -0.1000 1.0842 0.6288 0.078 Uiso 1 1 calc R . . C14 C -0.1151(7) 1.0240(6) 0.7402(4) 0.060(3) Uani 1 1 d . . . H14 H -0.1785 1.0527 0.7496 0.072 Uiso 1 1 calc R . . C15 C -0.0686(6) 0.9635(5) 0.7979(4) 0.0322(18) Uani 1 1 d . . . C16 C 0.0245(7) 0.9224(5) 0.7807(4) 0.047(2) Uani 1 1 d . . . H16 H 0.0587 0.8808 0.8186 0.057 Uiso 1 1 calc R . . C17 C 0.0665(7) 0.9434(5) 0.7072(4) 0.048(2) Uani 1 1 d . . . H17 H 0.1288 0.9144 0.6965 0.057 Uiso 1 1 calc R . . C18 C -0.1211(6) 0.9410(4) 0.8769(4) 0.0286(16) Uani 1 1 d . . . C19 C 0.4097(8) 1.0647(7) 1.3088(5) 0.076(3) Uani 1 1 d . . . H19 H 0.3380 1.0601 1.3297 0.092 Uiso 1 1 calc R . . C20 C 0.4228(7) 1.0548(7) 1.2363(5) 0.065(3) Uani 1 1 d . . . H20 H 0.3610 1.0446 1.2087 0.078 Uiso 1 1 calc R . . C21 C 0.5286(6) 1.0600(5) 1.2040(4) 0.0339(18) Uani 1 1 d . . . C22 C 0.6158(6) 1.0764(5) 1.2478(4) 0.043(2) Uani 1 1 d . . . H22 H 0.6885 1.0804 1.2285 0.051 Uiso 1 1 calc R . . C23 C 0.5955(7) 1.0867(5) 1.3196(4) 0.045(2) Uani 1 1 d . . . H23 H 0.6558 1.0986 1.3477 0.054 Uiso 1 1 calc R . . C24 C 0.5475(6) 1.0429(4) 1.1265(4) 0.0283(16) Uani 1 1 d . . . C25 C 0.7372(7) 1.2254(5) 0.7258(4) 0.050(2) Uani 1 1 d . . . H25 H 0.8130 1.2364 0.7178 0.060 Uiso 1 1 calc R . . C26 C 0.7031(6) 1.1907(5) 0.7999(4) 0.043(2) Uani 1 1 d . . . H26 H 0.7551 1.1782 0.8403 0.052 Uiso 1 1 calc R . . C27 C 0.5911(6) 1.1744(4) 0.8140(4) 0.0315(17) Uani 1 1 d . . . C28 C 0.5188(7) 1.1971(6) 0.7524(4) 0.064(3) Uani 1 1 d . . . H28 H 0.4419 1.1903 0.7596 0.077 Uiso 1 1 calc R . . C29 C 0.5599(8) 1.2301(7) 0.6798(5) 0.086(4) Uani 1 1 d . . . H29 H 0.5091 1.2433 0.6387 0.103 Uiso 1 1 calc R . . C30 C 0.5502(6) 1.1285(4) 0.8924(4) 0.0294(17) Uani 1 1 d . . . C31 C 0.0479(7) 0.5379(6) 0.3070(5) 0.064(3) Uani 1 1 d . . . H31 H 0.1102 0.5608 0.3239 0.077 Uiso 1 1 calc R . . C32 C 0.0140(7) 0.5682(5) 0.2304(4) 0.053(3) Uani 1 1 d . . . H32 H 0.0516 0.6108 0.1979 0.064 Uiso 1 1 calc R . . C33 C -0.0749(6) 0.5345(5) 0.2043(4) 0.0365(19) Uani 1 1 d . . . C34 C -0.1285(9) 0.4744(6) 0.2554(5) 0.081(4) Uani 1 1 d . . . H34 H -0.1906 0.4505 0.2397 0.097 Uiso 1 1 calc R . . C35 C -0.0900(9) 0.4489(7) 0.3315(5) 0.091(4) Uani 1 1 d . . . H35 H -0.1286 0.4083 0.3659 0.110 Uiso 1 1 calc R . . C36 C -0.1183(7) 0.5638(5) 0.1221(4) 0.0355(18) Uani 1 1 d . . . C37 C 0.5690(11) 0.4542(10) 0.6712(7) 0.058(4) Uani 0.6772(18) 1 d P A 1 H37 H 0.6259 0.4575 0.6353 0.070 Uiso 0.6772(18) 1 calc PR A 1 C38 C 0.5982(10) 0.4455(8) 0.7464(6) 0.038(3) Uani 0.6772(18) 1 d P A 1 H38 H 0.6734 0.4429 0.7612 0.046 Uiso 0.6772(18) 1 calc PR A 1 C39 C 0.5158(10) 0.4405(10) 0.7996(7) 0.031(3) Uani 0.6772(18) 1 d P A 1 C40 C 0.4075(11) 0.4349(12) 0.7780(7) 0.058(4) Uani 0.6772(18) 1 d P A 1 H40 H 0.3504 0.4247 0.8142 0.069 Uiso 0.6772(18) 1 calc PR A 1 C41 C 0.3849(12) 0.4447(11) 0.7006(7) 0.075(5) Uani 0.6772(18) 1 d P A 1 H41 H 0.3107 0.4417 0.6852 0.090 Uiso 0.6772(18) 1 calc PR A 1 C42 C 0.5478(7) 0.4467(4) 0.8814(4) 0.0306(17) Uani 1 1 d . . . C43 C 0.7971(9) 0.7193(6) 0.3594(5) 0.0746(17) Uani 1 1 d . . . H43 H 0.8048 0.6666 0.3910 0.090 Uiso 1 1 calc R . . C44 C 0.8234(9) 0.7316(6) 0.2823(5) 0.0746(17) Uani 1 1 d . . . H44 H 0.8502 0.6885 0.2639 0.090 Uiso 1 1 calc R . . C45 C 0.8099(7) 0.8068(5) 0.2337(4) 0.040(2) Uani 1 1 d . . . C46 C 0.7748(7) 0.8679(5) 0.2648(4) 0.049(2) Uani 1 1 d . . . H46 H 0.7661 0.9209 0.2343 0.059 Uiso 1 1 calc R . . C47 C 0.7524(8) 0.8489(6) 0.3432(5) 0.060(3) Uani 1 1 d . . . H47 H 0.7283 0.8914 0.3634 0.072 Uiso 1 1 calc R . . C48 C 0.8304(6) 0.8196(5) 0.1484(4) 0.0366(19) Uani 1 1 d . . . C49 C 0.7425(8) 0.6517(6) 0.6551(5) 0.057(3) Uani 1 1 d . . . H49 H 0.7103 0.6113 0.6362 0.068 Uiso 1 1 calc R . . C50 C 0.7646(7) 0.6355(5) 0.7331(4) 0.049(2) Uani 1 1 d . . . H50 H 0.7474 0.5853 0.7658 0.058 Uiso 1 1 calc R . . C51 C 0.8124(6) 0.6944(5) 0.7620(4) 0.0327(18) Uani 1 1 d . . . C52 C 0.8365(8) 0.7662(5) 0.7108(4) 0.059(3) Uani 1 1 d . . . H52 H 0.8688 0.8075 0.7283 0.070 Uiso 1 1 calc R . . C53 C 0.8131(8) 0.7781(6) 0.6329(5) 0.065(3) Uani 1 1 d . . . H53 H 0.8322 0.8270 0.5988 0.078 Uiso 1 1 calc R . . C54 C 0.8319(6) 0.6806(5) 0.8477(4) 0.0332(18) Uani 1 1 d . . . C55 C 0.6578(6) 0.7557(5) 0.9894(4) 0.0320(17) Uani 1 1 d . . . C56 C 0.5349(6) 0.7601(5) 0.9787(6) 0.064(3) Uani 1 1 d . . . H56A H 0.5064 0.8114 0.9846 0.096 Uiso 1 1 calc R . . H56B H 0.5016 0.7166 1.0165 0.096 Uiso 1 1 calc R . . H56C H 0.5165 0.7553 0.9279 0.096 Uiso 1 1 calc R . . C57 C 1.1443(6) 0.7485(5) 1.0006(6) 0.047(2) Uani 1 1 d . . . C58 C 1.2687(7) 0.7450(7) 1.0038(8) 0.106(5) Uani 1 1 d . . . H58A H 1.2940 0.6903 1.0277 0.159 Uiso 1 1 calc R . . H58B H 1.2950 0.7807 1.0333 0.159 Uiso 1 1 calc R . . H58C H 1.2976 0.7617 0.9524 0.159 Uiso 1 1 calc R . . C37B C 0.6595(12) 0.4268(13) 0.6873(9) 0.058(4) Uani 0.3228(18) 1 d PG A 2 H37B H 0.7282 0.4235 0.6637 0.070 Uiso 0.3228(18) 1 calc PR A 2 C38B C 0.6562(14) 0.4289(15) 0.7642(9) 0.038(3) Uani 0.3228(18) 1 d PG A 2 H38B H 0.7227 0.4270 0.7920 0.046 Uiso 0.3228(18) 1 calc PR A 2 C39B C 0.5536(17) 0.434(2) 0.7994(8) 0.031(3) Uani 0.3228(18) 1 d PG A 2 C40B C 0.4542(13) 0.437(2) 0.7578(11) 0.058(4) Uani 0.3228(18) 1 d PG A 2 H40B H 0.3855 0.4401 0.7814 0.069 Uiso 0.3228(18) 1 calc PR A 2 C41B C 0.4574(12) 0.4347(18) 0.6809(11) 0.075(5) Uani 0.3228(18) 1 d PG A 2 H41B H 0.3909 0.4366 0.6530 0.090 Uiso 0.3228(18) 1 calc PR A 2 N12B N 0.5601(15) 0.4297(14) 0.6456(8) 0.053(3) Uani 0.3228(18) 1 d PG A 2 Cu1 Cu 0.78452(9) 1.22429(7) 0.43891(6) 0.0564(3) Uani 1 1 d . . . Cu2 Cu 0.08014(9) 1.02541(7) 0.53806(6) 0.0529(3) Uani 1 1 d . . . Cu3 Cu 0.46957(9) 1.08415(8) 0.46566(6) 0.0558(3) Uani 1 1 d . . . Cu4 Cu 0.73033(9) 1.25951(7) 0.55842(6) 0.0541(3) Uani 1 1 d . . . Cu5 Cu 0.05321(9) 0.43114(7) 0.47199(6) 0.0506(3) Uani 1 1 d U . . Cu6 Cu 0.41138(13) 0.53286(13) 0.53425(10) 0.0607(5) Uani 0.6772(18) 1 d P . 1 Cu7 Cu 0.71192(10) 0.73979(8) 0.49740(6) 0.0653(4) Uani 1 1 d . . . Cu6B Cu 0.5909(3) 0.4338(3) 0.5236(2) 0.0607(5) Uani 0.3228(18) 1 d P . 2 N1 N -0.0889(7) 1.1537(5) 0.4524(4) 0.062(2) Uani 1 1 d . . . N2 N 0.2368(7) 1.0331(5) 0.5212(4) 0.058(2) Uani 1 1 d . . . N3 N 0.5809(6) 1.1438(5) 0.4990(4) 0.055(2) Uani 1 1 d . . . N4 N -0.0580(6) 0.3532(5) 0.5130(4) 0.057(2) Uani 1 1 d . A . N5 N 0.1910(7) 0.4717(5) 0.4946(4) 0.066(2) Uani 1 1 d U A . N6 N 0.5149(7) 0.6293(6) 0.5071(4) 0.067(2) Uani 1 1 d . . . N7 N 0.7128(6) 1.2757(4) 0.3371(3) 0.0470(18) Uani 1 1 d . . . N8 N 0.0226(6) 1.0029(4) 0.6505(4) 0.0490(19) Uani 1 1 d . . . N9 N 0.4945(6) 1.0807(5) 1.3517(4) 0.0515(19) Uani 1 1 d . . . N10 N 0.6681(6) 1.2442(5) 0.6648(4) 0.054(2) Uani 1 1 d . . . N11 N -0.0016(6) 0.4795(4) 0.3568(4) 0.0487(19) Uani 1 1 d . A . N12 N 0.4636(9) 0.4581(8) 0.6469(6) 0.053(3) Uani 0.6772(18) 1 d P A 1 N13 N 0.7618(8) 0.7770(5) 0.3912(4) 0.0746(17) Uani 1 1 d . . . N14 N 0.7649(6) 0.7225(5) 0.6052(4) 0.051(2) Uani 1 1 d . . . Nd1 Nd 0.68240(3) 0.96150(2) 1.00640(2) 0.02340(10) Uani 1 1 d . . . Nd2 Nd 0.68077(3) 0.54420(2) 0.98929(2) 0.02683(10) Uani 1 1 d . . . Nd3 Nd 0.90591(3) 0.75066(2) 0.99886(2) 0.02530(10) Uani 1 1 d . . . O1 O 0.6318(4) 1.4115(3) 0.0636(3) 0.0404(13) Uani 1 1 d . . . O2 O 0.4591(4) 1.3805(3) 0.1070(3) 0.0372(13) Uani 1 1 d . . . O3 O -0.2116(4) 0.9742(3) 0.8856(3) 0.0375(13) Uani 1 1 d . . . O4 O -0.0673(4) 0.8885(3) 0.9294(3) 0.0362(12) Uani 1 1 d . . . O5 O 0.4652(4) 1.0438(3) 1.0834(3) 0.0367(13) Uani 1 1 d . . . O6 O 0.6473(4) 1.0281(3) 1.1111(3) 0.0380(13) Uani 1 1 d . . . O7 O 0.6273(4) 1.0979(3) 0.9407(3) 0.0321(12) Uani 1 1 d . . . O8 O 0.4476(4) 1.1249(3) 0.9030(3) 0.0334(12) Uani 1 1 d . . . O9 O -0.0583(4) 0.6139(3) 0.0742(3) 0.0384(13) Uani 1 1 d . . . O10 O -0.2101(4) 0.5381(3) 0.1074(3) 0.0431(14) Uani 1 1 d . . . O11 O 0.6436(4) 0.4658(3) 0.8960(3) 0.0402(13) Uani 1 1 d . A . O12 O 0.4657(4) 0.4374(3) 0.9252(3) 0.0422(14) Uani 1 1 d . . . O13 O 0.8634(5) 0.7592(4) 0.1266(3) 0.0560(17) Uani 1 1 d . . . O14 O 0.8133(4) 0.8895(3) 0.1046(3) 0.0388(13) Uani 1 1 d . . . O15 O 0.8098(4) 0.6126(3) 0.8912(3) 0.0395(13) Uani 1 1 d . A . O16 O 0.8702(5) 0.7392(3) 0.8702(3) 0.0470(15) Uani 1 1 d . A . O17 O 0.7112(4) 0.6877(3) 1.0003(3) 0.0353(12) Uani 1 1 d . A . O18 O 0.7121(4) 0.8195(3) 0.9881(3) 0.0309(11) Uani 1 1 d . A . O19 O 1.0936(4) 0.7127(3) 0.9586(3) 0.0405(13) Uani 1 1 d . A . O20 O 1.0923(4) 0.7868(3) 1.0421(3) 0.0473(15) Uani 1 1 d . A . O21W O 0.8546(4) 1.0447(3) 1.0089(3) 0.0474(15) Uani 1 1 d . . . H21A H 0.9009 1.0460 1.0424 0.057 Uiso 1 1 d R . . H21B H 0.8590 1.0871 0.9747 0.057 Uiso 1 1 d R . . O22W O 0.8554(4) 0.4570(3) 0.9919(3) 0.0470(14) Uani 1 1 d . A . H22A H 0.8950 0.4554 0.9550 0.056 Uiso 1 1 d R . . H22B H 0.8618 0.4128 1.0237 0.056 Uiso 1 1 d R . . 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 0.055(6) 0.049(6) 0.035(5) 0.001(4) 0.016(4) 0.009(5) C2 0.051(6) 0.063(6) 0.031(5) -0.020(4) 0.007(4) -0.020(5) C3 0.043(5) 0.059(6) 0.032(5) -0.006(4) 0.010(4) -0.005(4) C4 0.056(6) 0.050(6) 0.045(5) -0.010(4) 0.014(4) -0.018(5) C5 0.048(5) 0.054(6) 0.050(5) -0.014(4) -0.009(4) 0.004(4) C6 0.054(5) 0.107(7) 0.039(3) -0.019(4) -0.005(3) 0.006(4) C7 0.036(5) 0.059(6) 0.033(5) -0.002(4) -0.002(4) 0.003(4) C8 0.040(5) 0.054(6) 0.028(4) 0.000(4) 0.003(4) 0.002(4) C9 0.048(5) 0.030(4) 0.021(4) -0.001(3) -0.003(3) -0.001(4) C10 0.052(6) 0.073(7) 0.031(5) 0.004(4) -0.001(4) 0.015(5) C11 0.060(6) 0.084(7) 0.021(4) 0.001(4) 0.002(4) 0.030(5) C12 0.046(5) 0.024(4) 0.026(4) -0.003(3) -0.002(4) 0.000(4) C13 0.084(7) 0.071(7) 0.026(5) 0.011(4) 0.023(5) 0.033(6) C14 0.069(6) 0.072(7) 0.028(5) 0.006(4) 0.018(4) 0.037(5) C15 0.036(4) 0.040(5) 0.022(4) -0.008(3) 0.009(3) -0.005(4) C16 0.046(5) 0.064(6) 0.027(4) -0.004(4) 0.002(4) 0.010(4) C17 0.041(5) 0.068(6) 0.032(5) -0.010(4) 0.014(4) 0.005(4) C18 0.034(4) 0.028(4) 0.026(4) -0.012(3) 0.006(3) -0.008(3) C19 0.043(6) 0.153(11) 0.052(6) -0.060(7) 0.008(5) -0.016(6) C20 0.031(5) 0.128(10) 0.052(6) -0.054(6) 0.008(4) -0.021(5) C21 0.042(5) 0.043(5) 0.022(4) -0.018(3) -0.004(3) -0.002(4) C22 0.035(5) 0.065(6) 0.033(5) -0.022(4) 0.006(4) -0.003(4) C23 0.045(5) 0.073(6) 0.025(4) -0.025(4) 0.001(4) -0.006(4) C24 0.040(5) 0.023(4) 0.023(4) -0.008(3) 0.004(3) -0.001(3) C25 0.041(5) 0.070(7) 0.035(5) -0.004(4) 0.009(4) -0.022(5) C26 0.039(5) 0.062(6) 0.023(4) -0.001(4) 0.001(3) -0.004(4) C27 0.037(4) 0.036(5) 0.018(4) -0.002(3) 0.000(3) -0.003(3) C28 0.038(5) 0.111(9) 0.025(5) 0.016(5) 0.002(4) -0.010(5) C29 0.054(6) 0.155(12) 0.026(5) 0.017(6) -0.006(4) -0.024(7) C30 0.042(5) 0.023(4) 0.022(4) -0.004(3) 0.004(3) 0.000(3) C31 0.056(6) 0.084(8) 0.040(5) 0.008(5) -0.017(4) -0.034(5) C32 0.059(6) 0.059(6) 0.032(5) 0.009(4) -0.006(4) -0.029(5) C33 0.044(5) 0.040(5) 0.024(4) -0.005(3) -0.009(3) -0.004(4) C34 0.102(8) 0.078(8) 0.043(6) 0.023(5) -0.035(6) -0.051(7) C35 0.106(9) 0.110(10) 0.035(6) 0.026(6) -0.029(6) -0.063(8) C36 0.049(5) 0.028(4) 0.030(4) -0.009(3) -0.007(4) 0.002(4) C37 0.056(8) 0.091(11) 0.028(7) -0.018(7) 0.002(6) -0.002(8) C38 0.043(8) 0.049(8) 0.024(6) -0.013(5) -0.004(6) -0.006(7) C39 0.036(9) 0.036(6) 0.020(4) -0.005(4) -0.001(5) -0.008(7) C40 0.048(10) 0.117(10) 0.012(7) -0.021(7) 0.006(5) -0.030(9) C41 0.048(9) 0.143(14) 0.036(8) -0.021(8) 0.000(7) -0.044(11) C42 0.045(5) 0.025(4) 0.023(4) -0.009(3) 0.001(4) 0.001(3) C43 0.134(5) 0.061(4) 0.024(3) -0.003(2) 0.014(3) 0.013(3) C44 0.134(5) 0.061(4) 0.024(3) -0.003(2) 0.014(3) 0.013(3) C45 0.055(5) 0.052(5) 0.011(4) -0.003(3) -0.002(3) 0.010(4) C46 0.076(6) 0.047(6) 0.026(4) -0.010(4) 0.018(4) -0.011(5) C47 0.087(7) 0.069(7) 0.034(5) -0.032(5) 0.013(5) -0.014(6) C48 0.036(4) 0.057(6) 0.016(4) -0.009(4) 0.000(3) 0.014(4) C49 0.083(7) 0.061(7) 0.034(5) -0.025(5) -0.002(5) -0.016(5) C50 0.074(6) 0.044(5) 0.023(4) 0.002(4) -0.001(4) -0.016(5) C51 0.041(4) 0.042(5) 0.016(4) -0.009(3) 0.005(3) -0.012(4) C52 0.098(7) 0.051(6) 0.022(4) 0.003(4) -0.011(4) -0.034(5) C53 0.093(8) 0.068(7) 0.025(5) 0.009(4) -0.008(5) -0.040(6) C54 0.032(4) 0.041(5) 0.025(4) -0.006(4) 0.001(3) 0.002(4) C55 0.034(4) 0.030(5) 0.032(4) -0.008(3) -0.001(3) -0.004(4) C56 0.028(5) 0.046(6) 0.124(9) -0.034(6) -0.007(5) -0.004(4) C57 0.029(5) 0.035(5) 0.077(7) -0.015(5) -0.001(4) 0.001(4) C58 0.033(6) 0.120(10) 0.210(14) -0.126(10) -0.011(7) 0.009(6) C37B 0.056(8) 0.091(11) 0.028(7) -0.018(7) 0.002(6) -0.002(8) C38B 0.043(8) 0.049(8) 0.024(6) -0.013(5) -0.004(6) -0.006(7) C39B 0.036(9) 0.036(6) 0.020(4) -0.005(4) -0.001(5) -0.008(7) C40B 0.048(10) 0.117(10) 0.012(7) -0.021(7) 0.006(5) -0.030(9) C41B 0.048(9) 0.143(14) 0.036(8) -0.021(8) 0.000(7) -0.044(11) N12B 0.054(6) 0.085(9) 0.025(5) -0.024(5) 0.015(5) -0.026(6) Cu1 0.0538(7) 0.0750(8) 0.0292(6) 0.0058(5) -0.0039(5) 0.0094(6) Cu2 0.0575(7) 0.0650(8) 0.0317(6) -0.0043(5) 0.0146(5) -0.0004(6) Cu3 0.0595(7) 0.0772(9) 0.0373(6) -0.0251(6) 0.0110(5) -0.0222(6) Cu4 0.0665(7) 0.0670(8) 0.0275(5) -0.0075(5) 0.0099(5) -0.0277(6) Cu5 0.0516(7) 0.0600(7) 0.0348(6) -0.0014(5) -0.0069(5) -0.0157(6) Cu6 0.0471(8) 0.1052(14) 0.0366(9) -0.0289(9) 0.0037(8) -0.0229(9) Cu7 0.0812(9) 0.0959(10) 0.0176(5) -0.0106(6) 0.0066(5) -0.0233(7) Cu6B 0.0471(8) 0.1052(14) 0.0366(9) -0.0289(9) 0.0037(8) -0.0229(9) N1 0.069(6) 0.071(6) 0.047(5) -0.014(4) -0.002(4) -0.005(5) N2 0.071(6) 0.054(5) 0.049(5) -0.012(4) 0.006(4) -0.005(4) N3 0.054(5) 0.073(6) 0.040(4) -0.018(4) 0.004(4) -0.016(4) N4 0.062(5) 0.062(5) 0.044(5) -0.007(4) 0.000(4) -0.016(4) N5 0.071(5) 0.068(6) 0.055(5) -0.010(4) -0.012(4) -0.007(4) N6 0.054(5) 0.107(7) 0.039(3) -0.019(4) -0.005(3) 0.006(4) N7 0.056(5) 0.057(5) 0.023(4) -0.002(3) -0.006(3) 0.012(4) N8 0.052(4) 0.061(5) 0.029(4) -0.001(3) 0.016(3) 0.001(4) N9 0.051(5) 0.080(6) 0.030(4) -0.025(4) 0.007(3) -0.008(4) N10 0.055(5) 0.076(6) 0.025(4) 0.000(4) 0.004(3) -0.026(4) N11 0.050(4) 0.064(5) 0.026(4) 0.000(3) -0.013(3) -0.019(4) N12 0.054(6) 0.085(9) 0.025(5) -0.024(5) 0.015(5) -0.026(6) N13 0.134(5) 0.061(4) 0.024(3) -0.003(2) 0.014(3) 0.013(3) N14 0.061(5) 0.070(5) 0.022(4) -0.009(4) 0.007(3) -0.023(4) Nd1 0.0282(2) 0.0269(2) 0.01419(18) -0.00362(15) 0.00212(15) -0.00120(16) Nd2 0.0340(2) 0.0283(2) 0.01613(19) -0.00190(16) -0.00150(16) -0.00218(17) Nd3 0.0265(2) 0.0302(2) 0.01838(19) -0.00482(16) 0.00067(15) -0.00067(17) O1 0.056(4) 0.036(3) 0.025(3) -0.001(2) 0.000(3) -0.007(3) O2 0.044(3) 0.035(3) 0.029(3) -0.001(2) -0.010(2) 0.005(3) O3 0.040(3) 0.045(3) 0.024(3) -0.005(2) 0.013(2) 0.003(3) O4 0.048(3) 0.034(3) 0.024(3) -0.001(2) 0.003(2) -0.006(3) O5 0.045(3) 0.046(3) 0.019(3) -0.008(2) -0.011(2) 0.001(3) O6 0.039(3) 0.057(4) 0.023(3) -0.018(2) 0.003(2) 0.002(3) O7 0.046(3) 0.026(3) 0.022(3) -0.002(2) 0.004(2) -0.003(2) O8 0.034(3) 0.032(3) 0.028(3) 0.004(2) 0.005(2) -0.005(2) O9 0.048(3) 0.031(3) 0.029(3) 0.005(2) -0.001(2) 0.006(3) O10 0.049(3) 0.051(4) 0.028(3) -0.007(3) -0.012(3) -0.003(3) O11 0.045(3) 0.050(4) 0.029(3) -0.015(3) 0.002(2) -0.009(3) O12 0.044(3) 0.055(4) 0.028(3) -0.011(3) 0.009(2) 0.001(3) O13 0.079(4) 0.069(4) 0.018(3) -0.010(3) 0.002(3) 0.035(3) O14 0.037(3) 0.055(4) 0.019(3) 0.001(2) -0.003(2) -0.002(3) O15 0.049(3) 0.041(3) 0.024(3) 0.000(2) 0.008(2) -0.001(3) O16 0.064(4) 0.059(4) 0.019(3) -0.009(3) 0.004(2) -0.026(3) O17 0.041(3) 0.027(3) 0.039(3) -0.008(2) -0.002(2) 0.000(2) O18 0.030(3) 0.028(3) 0.037(3) -0.012(2) 0.000(2) 0.000(2) O19 0.027(3) 0.051(4) 0.053(4) -0.029(3) 0.009(2) -0.007(3) O20 0.038(3) 0.057(4) 0.056(4) -0.031(3) -0.008(3) -0.002(3) O21W 0.040(3) 0.048(4) 0.051(4) -0.006(3) -0.008(3) -0.017(3) O22W 0.048(3) 0.038(3) 0.050(3) -0.003(3) 0.012(3) 0.016(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 N1 1.150(10) . ? C1 Cu2 1.909(9) . ? C1 Cu2 2.340(9) 2_576 ? C2 N2 1.162(10) . ? C2 Cu3 1.861(9) . ? C3 N3 1.148(10) . ? C3 Cu4 1.934(9) . ? C3 Cu1 2.157(8) . ? C4 N4 1.140(9) . ? C4 Cu4 1.874(9) 1_445 ? C5 N5 1.160(10) . ? C5 Cu6 1.836(9) . ? C5 Cu6B 1.982(10) 2_666 ? C6 N6 1.123(12) . ? C6 Cu7 1.911(11) . ? C7 N7 1.334(9) . ? C7 C8 1.368(10) . ? C7 H7 0.9300 . ? C8 C9 1.375(10) . ? C8 H8 0.9300 . ? C9 C10 1.365(10) . ? C9 C12 1.528(9) . ? C10 C11 1.375(10) . ? C10 H10 0.9300 . ? C11 N7 1.320(10) . ? C11 H11 0.9300 . ? C12 O2 1.233(8) . ? C12 O1 1.258(8) . ? C13 N8 1.332(10) . ? C13 C14 1.388(10) . ? C13 H13 0.9300 . ? C14 C15 1.362(10) . ? C14 H14 0.9300 . ? C15 C16 1.375(10) . ? C15 C18 1.511(9) . ? C16 C17 1.373(10) . ? C16 H16 0.9300 . ? C17 N8 1.331(10) . ? C17 H17 0.9300 . ? C18 O3 1.235(8) . ? C18 O4 1.277(8) . ? C19 N9 1.341(10) . ? C19 C20 1.363(11) . ? C19 H19 0.9300 . ? C20 C21 1.384(10) . ? C20 H20 0.9300 . ? C21 C22 1.376(10) . ? C21 C24 1.509(9) . ? C22 C23 1.368(10) . ? C22 H22 0.9300 . ? C23 N9 1.331(9) . ? C23 H23 0.9300 . ? C24 O5 1.243(8) . ? C24 O6 1.257(8) . ? C25 N10 1.333(9) . ? C25 C26 1.374(10) . ? C25 H25 0.9300 . ? C26 C27 1.379(10) . ? C26 H26 0.9300 . ? C27 C28 1.367(10) . ? C27 C30 1.511(9) . ? C28 C29 1.375(11) . ? C28 H28 0.9300 . ? C29 N10 1.332(10) . ? C29 H29 0.9300 . ? C30 O8 1.237(8) . ? C30 O7 1.266(8) . ? C31 N11 1.306(10) . ? C31 C32 1.391(10) . ? C31 H31 0.9300 . ? C32 C33 1.353(10) . ? C32 H32 0.9300 . ? C33 C34 1.358(11) . ? C33 C36 1.514(9) . ? C34 C35 1.392(11) . ? C34 H34 0.9300 . ? C35 N11 1.315(10) . ? C35 H35 0.9300 . ? C36 O10 1.239(8) . ? C36 O9 1.276(8) . ? C37 N12 1.322(15) . ? C37 C38 1.360(15) . ? C37 H37 0.9300 . ? C38 C39 1.361(15) . ? C38 H38 0.9300 . ? C39 C40 1.358(16) . ? C39 C42 1.544(13) . ? C40 C41 1.379(16) . ? C40 H40 0.9300 . ? C41 N12 1.328(15) . ? C41 H41 0.9300 . ? C42 O11 1.238(8) . ? C42 O12 1.245(8) . ? C42 C39B 1.542(15) . ? C43 N13 1.319(12) . ? C43 C44 1.381(11) . ? C43 H43 0.9300 . ? C44 C45 1.355(11) . ? C44 H44 0.9300 . ? C45 C46 1.360(11) . ? C45 C48 1.509(9) . ? C46 C47 1.389(10) . ? C46 H46 0.9300 . ? C47 N13 1.302(11) . ? C47 H47 0.9300 . ? C48 O13 1.248(9) . ? C48 O14 1.255(9) . ? C49 N14 1.334(10) . ? C49 C50 1.377(10) . ? C49 H49 0.9300 . ? C50 C51 1.374(10) . ? C50 H50 0.9300 . ? C51 C52 1.362(10) . ? C51 C54 1.511(9) . ? C52 C53 1.386(10) . ? C52 H52 0.9300 . ? C53 N14 1.317(10) . ? C53 H53 0.9300 . ? C54 O15 1.252(8) . ? C54 O16 1.261(9) . ? C55 O18 1.270(8) . ? C55 O17 1.277(8) . ? C55 C56 1.474(10) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O19 1.246(9) . ? C57 O20 1.263(10) . ? C57 C58 1.482(11) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C37B C38B 1.3900 . ? C37B N12B 1.3900 . ? C37B H37B 0.9300 . ? C38B C39B 1.3900 . ? C38B H38B 0.9300 . ? C39B C40B 1.3900 . ? C40B C41B 1.3900 . ? C40B H40B 0.9300 . ? C41B N12B 1.3900 . ? C41B H41B 0.9300 . ? N12B Cu6B 2.204(14) . ? Cu1 N1 1.881(9) 1_655 ? Cu1 N7 1.989(6) . ? Cu1 Cu4 2.4557(16) . ? Cu2 N2 1.894(8) . ? Cu2 N8 2.075(6) . ? Cu2 C1 2.340(9) 2_576 ? Cu2 Cu2 2.630(2) 2_576 ? Cu3 N3 1.875(8) . ? Cu3 N9 2.082(6) 1_554 ? Cu3 Cu3 2.884(3) 2_676 ? Cu4 C4 1.874(9) 1_665 ? Cu4 N10 2.005(7) . ? Cu5 N5 1.878(8) . ? Cu5 N4 1.907(7) . ? Cu5 N11 2.110(6) . ? Cu5 Cu5 3.034(2) 2_566 ? Cu6 N6 2.033(9) . ? Cu6 N12 2.169(11) . ? Cu6 Cu6 2.801(4) 2_666 ? Cu7 N13 1.946(7) . ? Cu7 N14 1.978(6) . ? Cu6B N6 1.845(9) 2_666 ? Cu6B C5 1.982(10) 2_666 ? Cu6B Cu6B 3.043(8) 2_666 ? N1 Cu1 1.881(9) 1_455 ? N6 Cu6B 1.845(9) 2_666 ? N9 Cu3 2.082(6) 1_556 ? Nd1 O7 2.391(5) . ? Nd1 O5 2.397(5) 2_677 ? Nd1 O14 2.411(5) 1_556 ? Nd1 O6 2.465(5) . ? Nd1 O8 2.467(4) 2_677 ? Nd1 O3 2.476(5) 1_655 ? Nd1 O21W 2.524(5) . ? Nd1 O18 2.539(5) . ? Nd2 O1 2.392(5) 1_546 ? Nd2 O12 2.396(5) 2_667 ? Nd2 O15 2.419(5) . ? Nd2 O11 2.439(5) . ? Nd2 O10 2.458(5) 1_656 ? Nd2 O2 2.476(5) 2_676 ? Nd2 O22W 2.520(5) . ? Nd2 O17 2.535(5) . ? Nd3 O4 2.383(5) 1_655 ? Nd3 O13 2.389(5) 1_556 ? Nd3 O9 2.397(5) 1_656 ? Nd3 O16 2.402(5) . ? Nd3 O19 2.474(5) . ? Nd3 O20 2.490(5) . ? Nd3 O18 2.549(5) . ? Nd3 O17 2.573(5) . ? O1 Nd2 2.392(5) 1_564 ? O2 Nd2 2.476(5) 2_676 ? O3 Nd1 2.476(5) 1_455 ? O4 Nd3 2.383(5) 1_455 ? O5 Nd1 2.397(5) 2_677 ? O8 Nd1 2.467(4) 2_677 ? O9 Nd3 2.397(5) 1_454 ? O10 Nd2 2.458(5) 1_454 ? O12 Nd2 2.396(5) 2_667 ? O13 Nd3 2.389(5) 1_554 ? O14 Nd1 2.411(5) 1_554 ? O21W H21A 0.8200 . ? O21W H21B 0.8199 . ? O22W H22A 0.8201 . ? O22W H22B 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cu2 165.7(8) . . ? N1 C1 Cu2 114.8(8) . 2_576 ? Cu2 C1 Cu2 75.7(3) . 2_576 ? N2 C2 Cu3 173.5(9) . . ? N3 C3 Cu4 168.1(8) . . ? N3 C3 Cu1 118.4(7) . . ? Cu4 C3 Cu1 73.6(3) . . ? N4 C4 Cu4 176.6(9) . 1_445 ? N5 C5 Cu6 175.1(8) . . ? N5 C5 Cu6B 152.5(8) . 2_666 ? Cu6 C5 Cu6B 31.50(18) . 2_666 ? N6 C6 Cu7 167.5(11) . . ? N7 C7 C8 123.7(8) . . ? N7 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C7 C8 C9 118.8(7) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 118.5(7) . . ? C10 C9 C12 120.3(7) . . ? C8 C9 C12 120.9(7) . . ? C9 C10 C11 118.4(8) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? N7 C11 C10 124.3(8) . . ? N7 C11 H11 117.8 . . ? C10 C11 H11 117.8 . . ? O2 C12 O1 127.0(7) . . ? O2 C12 C9 118.5(7) . . ? O1 C12 C9 114.6(7) . . ? N8 C13 C14 122.9(8) . . ? N8 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 119.6(8) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 117.7(7) . . ? C14 C15 C18 120.4(7) . . ? C16 C15 C18 121.8(7) . . ? C17 C16 C15 119.5(7) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? N8 C17 C16 123.5(8) . . ? N8 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? O3 C18 O4 125.4(6) . . ? O3 C18 C15 118.2(6) . . ? O4 C18 C15 116.5(6) . . ? N9 C19 C20 123.6(8) . . ? N9 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C19 C20 C21 119.7(8) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 116.9(7) . . ? C22 C21 C24 121.9(7) . . ? C20 C21 C24 121.0(7) . . ? C23 C22 C21 119.8(7) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? N9 C23 C22 123.7(7) . . ? N9 C23 H23 118.1 . . ? C22 C23 H23 118.1 . . ? O5 C24 O6 125.1(7) . . ? O5 C24 C21 118.8(7) . . ? O6 C24 C21 116.1(6) . . ? N10 C25 C26 123.8(7) . . ? N10 C25 H25 118.1 . . ? C26 C25 H25 118.1 . . ? C25 C26 C27 119.6(7) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C28 C27 C26 117.0(7) . . ? C28 C27 C30 120.8(7) . . ? C26 C27 C30 122.0(6) . . ? C27 C28 C29 119.8(8) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? N10 C29 C28 124.0(8) . . ? N10 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? O8 C30 O7 127.3(6) . . ? O8 C30 C27 118.1(6) . . ? O7 C30 C27 114.7(6) . . ? N11 C31 C32 124.5(8) . . ? N11 C31 H31 117.7 . . ? C32 C31 H31 117.7 . . ? C33 C32 C31 118.7(7) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C32 C33 C34 117.7(7) . . ? C32 C33 C36 122.4(7) . . ? C34 C33 C36 119.8(7) . . ? C33 C34 C35 119.7(8) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? N11 C35 C34 123.0(8) . . ? N11 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? O10 C36 O9 125.6(7) . . ? O10 C36 C33 117.1(7) . . ? O9 C36 C33 117.3(7) . . ? N12 C37 C38 123.1(13) . . ? N12 C37 H37 118.4 . . ? C38 C37 H37 118.4 . . ? C39 C38 C37 119.1(12) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C40 C39 C38 119.0(11) . . ? C40 C39 C42 122.1(10) . . ? C38 C39 C42 118.8(10) . . ? C39 C40 C41 117.9(11) . . ? C39 C40 H40 121.1 . . ? C41 C40 H40 121.1 . . ? N12 C41 C40 123.3(12) . . ? N12 C41 H41 118.3 . . ? C40 C41 H41 118.3 . . ? O11 C42 O12 126.6(7) . . ? O11 C42 C39B 105.6(10) . . ? O12 C42 C39B 127.7(10) . . ? O11 C42 C39 120.9(7) . . ? O12 C42 C39 112.2(7) . . ? C39B C42 C39 17.2(10) . . ? N13 C43 C44 124.5(9) . . ? N13 C43 H43 117.8 . . ? C44 C43 H43 117.8 . . ? C45 C44 C43 119.8(9) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 117.2(7) . . ? C44 C45 C48 120.1(8) . . ? C46 C45 C48 122.7(7) . . ? C45 C46 C47 118.2(8) . . ? C45 C46 H46 120.9 . . ? C47 C46 H46 120.9 . . ? N13 C47 C46 126.0(9) . . ? N13 C47 H47 117.0 . . ? C46 C47 H47 117.0 . . ? O13 C48 O14 124.7(7) . . ? O13 C48 C45 117.0(7) . . ? O14 C48 C45 118.4(7) . . ? N14 C49 C50 123.3(8) . . ? N14 C49 H49 118.4 . . ? C50 C49 H49 118.4 . . ? C51 C50 C49 119.2(8) . . ? C51 C50 H50 120.4 . . ? C49 C50 H50 120.4 . . ? C52 C51 C50 117.4(7) . . ? C52 C51 C54 121.8(7) . . ? C50 C51 C54 120.7(7) . . ? C51 C52 C53 120.3(8) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? N14 C53 C52 122.4(8) . . ? N14 C53 H53 118.8 . . ? C52 C53 H53 118.8 . . ? O15 C54 O16 124.7(7) . . ? O15 C54 C51 118.3(7) . . ? O16 C54 C51 117.0(7) . . ? O18 C55 O17 119.1(6) . . ? O18 C55 C56 120.5(7) . . ? O17 C55 C56 120.4(7) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O19 C57 O20 121.7(7) . . ? O19 C57 C58 119.6(8) . . ? O20 C57 C58 118.7(8) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C38B C37B N12B 120.0 . . ? C38B C37B H37B 120.0 . . ? N12B C37B H37B 120.0 . . ? C37B C38B C39B 120.0 . . ? C37B C38B H38B 120.0 . . ? C39B C38B H38B 120.0 . . ? C38B C39B C40B 120.0 . . ? C38B C39B C42 120.9(13) . . ? C40B C39B C42 118.7(13) . . ? C41B C40B C39B 120.0 . . ? C41B C40B H40B 120.0 . . ? C39B C40B H40B 120.0 . . ? C40B C41B N12B 120.0 . . ? C40B C41B H41B 120.0 . . ? N12B C41B H41B 120.0 . . ? C41B N12B C37B 120.0 . . ? C41B N12B Cu6B 127.8(9) . . ? C37B N12B Cu6B 112.1(9) . . ? N1 Cu1 N7 124.0(3) 1_655 . ? N1 Cu1 C3 117.6(3) 1_655 . ? N7 Cu1 C3 103.7(3) . . ? N1 Cu1 Cu4 112.6(2) 1_655 . ? N7 Cu1 Cu4 123.0(2) . . ? C3 Cu1 Cu4 49.1(3) . . ? N2 Cu2 C1 122.3(3) . . ? N2 Cu2 N8 118.5(3) . . ? C1 Cu2 N8 105.7(3) . . ? N2 Cu2 C1 107.6(3) . 2_576 ? C1 Cu2 C1 104.3(3) . 2_576 ? N8 Cu2 C1 93.8(3) . 2_576 ? N2 Cu2 Cu2 131.1(2) . 2_576 ? C1 Cu2 Cu2 59.6(3) . 2_576 ? N8 Cu2 Cu2 104.7(2) . 2_576 ? C1 Cu2 Cu2 44.7(2) 2_576 2_576 ? C2 Cu3 N3 134.4(3) . . ? C2 Cu3 N9 112.6(3) . 1_554 ? N3 Cu3 N9 111.3(3) . 1_554 ? C2 Cu3 Cu3 81.8(3) . 2_676 ? N3 Cu3 Cu3 105.1(2) . 2_676 ? N9 Cu3 Cu3 96.3(2) 1_554 2_676 ? C4 Cu4 C3 133.8(4) 1_665 . ? C4 Cu4 N10 120.6(3) 1_665 . ? C3 Cu4 N10 104.1(3) . . ? C4 Cu4 Cu1 76.4(3) 1_665 . ? C3 Cu4 Cu1 57.4(2) . . ? N10 Cu4 Cu1 158.1(2) . . ? N5 Cu5 N4 143.3(3) . . ? N5 Cu5 N11 113.6(3) . . ? N4 Cu5 N11 102.8(3) . . ? N5 Cu5 Cu5 85.6(3) . 2_566 ? N4 Cu5 Cu5 96.1(2) . 2_566 ? N11 Cu5 Cu5 93.8(2) . 2_566 ? C5 Cu6 N6 141.7(4) . . ? C5 Cu6 N12 109.4(4) . . ? N6 Cu6 N12 107.2(4) . . ? C5 Cu6 Cu6 111.1(3) . 2_666 ? N6 Cu6 Cu6 79.5(2) . 2_666 ? N12 Cu6 Cu6 90.2(3) . 2_666 ? C6 Cu7 N13 111.0(4) . . ? C6 Cu7 N14 105.2(3) . . ? N13 Cu7 N14 141.9(3) . . ? N6 Cu6B C5 145.4(4) 2_666 2_666 ? N6 Cu6B N12B 107.8(6) 2_666 . ? C5 Cu6B N12B 106.7(6) 2_666 . ? N6 Cu6B Cu6B 83.2(3) 2_666 2_666 ? C5 Cu6B Cu6B 98.9(3) 2_666 2_666 ? N12B Cu6B Cu6B 89.3(6) . 2_666 ? C1 N1 Cu1 163.1(8) . 1_455 ? C2 N2 Cu2 169.6(7) . . ? C3 N3 Cu3 172.9(8) . . ? C4 N4 Cu5 169.1(8) . . ? C5 N5 Cu5 178.4(8) . . ? C6 N6 Cu6B 160.2(9) . 2_666 ? C6 N6 Cu6 168.7(8) . . ? Cu6B N6 Cu6 30.81(18) 2_666 . ? C11 N7 C7 116.3(7) . . ? C11 N7 Cu1 123.4(5) . . ? C7 N7 Cu1 120.2(6) . . ? C17 N8 C13 116.8(7) . . ? C17 N8 Cu2 121.9(6) . . ? C13 N8 Cu2 120.9(5) . . ? C23 N9 C19 116.2(7) . . ? C23 N9 Cu3 122.6(5) . 1_556 ? C19 N9 Cu3 120.9(6) . 1_556 ? C29 N10 C25 115.7(7) . . ? C29 N10 Cu4 122.0(6) . . ? C25 N10 Cu4 119.8(6) . . ? C31 N11 C35 116.3(7) . . ? C31 N11 Cu5 124.4(5) . . ? C35 N11 Cu5 119.3(6) . . ? C37 N12 C41 116.8(12) . . ? C37 N12 Cu6 122.0(9) . . ? C41 N12 Cu6 115.6(10) . . ? C47 N13 C43 114.3(8) . . ? C47 N13 Cu7 129.6(7) . . ? C43 N13 Cu7 115.5(6) . . ? C53 N14 C49 117.4(7) . . ? C53 N14 Cu7 124.6(6) . . ? C49 N14 Cu7 117.8(6) . . ? O7 Nd1 O5 71.72(17) . 2_677 ? O7 Nd1 O14 139.75(17) . 1_556 ? O5 Nd1 O14 148.53(18) 2_677 1_556 ? O7 Nd1 O6 75.84(16) . . ? O5 Nd1 O6 119.83(17) 2_677 . ? O14 Nd1 O6 78.04(17) 1_556 . ? O7 Nd1 O8 119.98(16) . 2_677 ? O5 Nd1 O8 81.49(16) 2_677 2_677 ? O14 Nd1 O8 79.77(16) 1_556 2_677 ? O6 Nd1 O8 72.92(17) . 2_677 ? O7 Nd1 O3 81.07(16) . 1_655 ? O5 Nd1 O3 78.42(16) 2_677 1_655 ? O14 Nd1 O3 103.07(16) 1_556 1_655 ? O6 Nd1 O3 142.91(17) . 1_655 ? O8 Nd1 O3 144.15(17) 2_677 1_655 ? O7 Nd1 O21W 74.83(17) . . ? O5 Nd1 O21W 137.19(17) 2_677 . ? O14 Nd1 O21W 69.30(17) 1_556 . ? O6 Nd1 O21W 75.52(17) . . ? O8 Nd1 O21W 139.50(16) 2_677 . ? O3 Nd1 O21W 70.61(17) 1_655 . ? O7 Nd1 O18 143.21(15) . . ? O5 Nd1 O18 78.33(16) 2_677 . ? O14 Nd1 O18 72.48(16) 1_556 . ? O6 Nd1 O18 139.33(16) . . ? O8 Nd1 O18 74.76(16) 2_677 . ? O3 Nd1 O18 72.29(16) 1_655 . ? O21W Nd1 O18 117.45(16) . . ? O1 Nd2 O12 73.15(18) 1_546 2_667 ? O1 Nd2 O15 141.73(18) 1_546 . ? O12 Nd2 O15 145.07(18) 2_667 . ? O1 Nd2 O11 74.11(17) 1_546 . ? O12 Nd2 O11 119.03(18) 2_667 . ? O15 Nd2 O11 82.57(17) . . ? O1 Nd2 O10 80.62(17) 1_546 1_656 ? O12 Nd2 O10 79.26(17) 2_667 1_656 ? O15 Nd2 O10 101.03(17) . 1_656 ? O11 Nd2 O10 141.48(18) . 1_656 ? O1 Nd2 O2 117.11(17) 1_546 2_676 ? O12 Nd2 O2 80.63(17) 2_667 2_676 ? O15 Nd2 O2 81.71(17) . 2_676 ? O11 Nd2 O2 70.87(17) . 2_676 ? O10 Nd2 O2 147.61(18) 1_656 2_676 ? O1 Nd2 O22W 74.96(17) 1_546 . ? O12 Nd2 O22W 138.84(17) 2_667 . ? O15 Nd2 O22W 69.91(17) . . ? O11 Nd2 O22W 75.17(17) . . ? O10 Nd2 O22W 70.43(18) 1_656 . ? O2 Nd2 O22W 137.99(17) 2_676 . ? O1 Nd2 O17 142.15(16) 1_546 . ? O12 Nd2 O17 77.37(17) 2_667 . ? O15 Nd2 O17 70.04(17) . . ? O11 Nd2 O17 142.54(16) . . ? O10 Nd2 O17 70.93(17) 1_656 . ? O2 Nd2 O17 80.07(16) 2_676 . ? O22W Nd2 O17 116.07(17) . . ? O4 Nd3 O13 103.87(19) 1_655 1_556 ? O4 Nd3 O9 161.86(17) 1_655 1_656 ? O13 Nd3 O9 77.51(18) 1_556 1_656 ? O4 Nd3 O16 80.73(17) 1_655 . ? O13 Nd3 O16 157.5(2) 1_556 . ? O9 Nd3 O16 105.05(18) 1_656 . ? O4 Nd3 O19 90.05(17) 1_655 . ? O13 Nd3 O19 123.92(18) 1_556 . ? O9 Nd3 O19 74.80(17) 1_656 . ? O16 Nd3 O19 77.54(18) . . ? O4 Nd3 O20 74.48(18) 1_655 . ? O13 Nd3 O20 79.2(2) 1_556 . ? O9 Nd3 O20 88.20(18) 1_656 . ? O16 Nd3 O20 122.90(18) . . ? O19 Nd3 O20 52.40(17) . . ? O4 Nd3 O18 74.43(16) 1_655 . ? O13 Nd3 O18 74.90(17) 1_556 . ? O9 Nd3 O18 122.69(16) 1_656 . ? O16 Nd3 O18 85.49(18) . . ? O19 Nd3 O18 158.70(16) . . ? O20 Nd3 O18 132.83(17) . . ? O4 Nd3 O17 119.99(16) 1_655 . ? O13 Nd3 O17 85.60(19) 1_556 . ? O9 Nd3 O17 78.09(16) 1_656 . ? O16 Nd3 O17 73.38(16) . . ? O19 Nd3 O17 132.99(17) . . ? O20 Nd3 O17 161.43(17) . . ? O18 Nd3 O17 50.78(15) . . ? C12 O1 Nd2 138.5(5) . 1_564 ? C12 O2 Nd2 135.9(5) . 2_676 ? C18 O3 Nd1 128.1(4) . 1_455 ? C18 O4 Nd3 135.7(4) . 1_455 ? C24 O5 Nd1 174.5(5) . 2_677 ? C24 O6 Nd1 118.5(4) . . ? C30 O7 Nd1 133.6(4) . . ? C30 O8 Nd1 137.3(4) . 2_677 ? C36 O9 Nd3 132.2(5) . 1_454 ? C36 O10 Nd2 135.3(5) . 1_454 ? C42 O11 Nd2 122.8(5) . . ? C42 O12 Nd2 164.6(5) . 2_667 ? C48 O13 Nd3 128.6(5) . 1_554 ? C48 O14 Nd1 139.8(5) . 1_554 ? C54 O15 Nd2 142.9(5) . . ? C54 O16 Nd3 129.8(5) . . ? C55 O17 Nd2 139.7(4) . . ? C55 O17 Nd3 94.3(4) . . ? Nd2 O17 Nd3 123.7(2) . . ? C55 O18 Nd1 140.5(5) . . ? C55 O18 Nd3 95.6(4) . . ? Nd1 O18 Nd3 122.04(18) . . ? C57 O19 Nd3 93.5(5) . . ? C57 O20 Nd3 92.4(5) . . ? Nd1 O21W H21A 133.5 . . ? Nd1 O21W H21B 116.6 . . ? H21A O21W H21B 107.7 . . ? Nd2 O22W H22A 126.6 . . ? Nd2 O22W H22B 120.0 . . ? H22A O22W H22B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.446 _refine_diff_density_min -1.401 _refine_diff_density_rms 0.149 _database_code_depnum_ccdc_archive 'CCDC 964391' ####################################################################### # # 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_I-B #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H42 Cu7 Eu3 N14 O22, H2 O' _chemical_formula_sum 'C58 H44 Cu7 Eu3 N14 O23' _chemical_formula_weight 2205.84 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8797(8) _cell_length_b 17.3366(12) _cell_length_c 17.9107(13) _cell_angle_alpha 74.3320(10) _cell_angle_beta 88.4180(10) _cell_angle_gamma 86.2360(10) _cell_volume 3543.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 12532 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2132 _exptl_absorpt_coefficient_mu 4.751 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.333 _exptl_absorpt_correction_T_max 0.387 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18310 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.20 _reflns_number_total 12532 _reflns_number_gt 10514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0327P)^2^+8.8249P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00072(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12532 _refine_ls_number_parameters 949 _refine_ls_number_restraints 340 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9826(6) 1.0969(4) -0.0163(4) 0.0416(14) Uani 1 1 d U . . C2 C 1.3355(6) 1.0471(4) 0.0018(4) 0.0446(16) Uani 1 1 d U . . C3 C 0.6464(6) 1.1880(4) 0.0077(4) 0.0388(11) Uani 1 1 d U . . C4 C 0.9469(5) 1.3479(3) 0.0160(3) 0.0342(13) Uani 1 1 d U . . C5 C 0.7343(5) 0.4944(4) 0.0108(3) 0.0311(11) Uani 1 1 d U . . C6 C 0.4308(5) 0.3349(4) -0.0160(3) 0.0329(12) Uani 1 1 d U . . C7 C 0.2266(5) 0.7205(4) 0.2377(3) 0.0364(14) Uani 1 1 d U . . H7 H 0.1508 0.7382 0.2352 0.044 Uiso 1 1 calc R . . C8 C 0.2724(5) 0.6876(4) 0.3093(4) 0.0368(14) Uani 1 1 d U . . H8 H 0.2280 0.6814 0.3539 0.044 Uiso 1 1 calc R . . C9 C 0.3852(5) 0.6638(3) 0.3143(3) 0.0271(10) Uani 1 1 d U . . C10 C 0.4462(6) 0.6736(4) 0.2461(4) 0.0492(18) Uani 1 1 d U . . H10 H 0.5231 0.6593 0.2472 0.059 Uiso 1 1 calc R . . C11 C 0.3921(6) 0.7047(5) 0.1761(4) 0.055(2) Uani 1 1 d U . . H11 H 0.4334 0.7090 0.1304 0.066 Uiso 1 1 calc R . . C12 C 0.4377(5) 0.6213(3) 0.3909(3) 0.0254(10) Uani 1 1 d U . . C13 C 0.9378(7) 1.0272(5) 0.1764(4) 0.067(3) Uani 1 1 d U . . H13 H 0.9050 1.0699 0.1386 0.080 Uiso 1 1 calc R . . C14 C 0.8878(6) 1.0077(4) 0.2494(4) 0.057(2) Uani 1 1 d U . . H14 H 0.8235 1.0369 0.2597 0.068 Uiso 1 1 calc R . . C15 C 0.9346(5) 0.9446(3) 0.3065(3) 0.0274(11) Uani 1 1 d U . . C16 C 1.0297(5) 0.9032(4) 0.2867(4) 0.0387(14) Uani 1 1 d U . . H16 H 1.0641 0.8601 0.3233 0.046 Uiso 1 1 calc R . . C17 C 1.0725(5) 0.9263(4) 0.2126(4) 0.0397(14) Uani 1 1 d U . . H17 H 1.1352 0.8970 0.2003 0.048 Uiso 1 1 calc R . . C18 C 0.8829(5) 0.9208(3) 0.3858(3) 0.0241(9) Uani 1 1 d U . . C19 C 0.5892(6) 0.9261(6) 0.1937(4) 0.068(3) Uani 1 1 d U . . H19 H 0.6615 0.9262 0.1724 0.081 Uiso 1 1 calc R . . C20 C 0.5768(5) 0.9361(5) 0.2668(4) 0.058(2) Uani 1 1 d U . . H20 H 0.6399 0.9404 0.2947 0.069 Uiso 1 1 calc R . . C21 C 0.4711(5) 0.9399(3) 0.2987(3) 0.0281(11) Uani 1 1 d U . . C22 C 0.3814(5) 0.9296(4) 0.2553(4) 0.0398(15) Uani 1 1 d U . . H22 H 0.3081 0.9316 0.2745 0.048 Uiso 1 1 calc R . . C23 C 0.4017(6) 0.9165(5) 0.1836(4) 0.0472(17) Uani 1 1 d U . . H23 H 0.3409 0.9074 0.1562 0.057 Uiso 1 1 calc R . . C24 C 0.4513(4) 0.9587(3) 0.3758(3) 0.0242(9) Uani 1 1 d U . . C25 C 0.7482(5) 1.2083(4) 0.2211(3) 0.0386(14) Uani 1 1 d U . . H25 H 0.8244 1.2167 0.2116 0.046 Uiso 1 1 calc R . . C26 C 0.7141(5) 1.1749(4) 0.2955(3) 0.0339(13) Uani 1 1 d U . . H26 H 0.7669 1.1598 0.3349 0.041 Uiso 1 1 calc R . . C27 C 0.6018(4) 1.1633(3) 0.3125(3) 0.0265(11) Uani 1 1 d U . . C28 C 0.5284(5) 1.1880(5) 0.2519(4) 0.0490(19) Uani 1 1 d U . . H28 H 0.4513 1.1835 0.2609 0.059 Uiso 1 1 calc R . . C29 C 0.5681(6) 1.2193(5) 0.1781(4) 0.056(2) Uani 1 1 d U . . H29 H 0.5166 1.2342 0.1378 0.067 Uiso 1 1 calc R . . C30 C 0.5612(5) 1.1211(3) 0.3919(3) 0.0240(9) Uani 1 1 d U . . C31 C 1.0293(7) 0.5335(5) 0.8078(4) 0.064(2) Uani 1 1 d U . . H31 H 1.0888 0.5576 0.8233 0.077 Uiso 1 1 calc R . . C32 C 0.9958(6) 0.5608(5) 0.7310(4) 0.054(2) Uani 1 1 d U . . H32 H 1.0337 0.6006 0.6960 0.065 Uiso 1 1 calc R . . C33 C 0.9053(5) 0.5276(3) 0.7078(3) 0.0277(11) Uani 1 1 d U . . C34 C 0.8521(6) 0.4715(4) 0.7628(4) 0.052(2) Uani 1 1 d U . . H34 H 0.7876 0.4503 0.7503 0.063 Uiso 1 1 calc R . . C35 C 0.8934(7) 0.4462(5) 0.8366(4) 0.067(3) Uani 1 1 d U . . H35 H 0.8572 0.4061 0.8725 0.080 Uiso 1 1 calc R . . C36 C 0.8620(5) 0.5558(3) 0.6255(3) 0.0259(9) Uani 1 1 d U . . C37 C 0.6643(5) 0.4170(4) 0.1904(4) 0.0417(14) Uani 1 1 d U . . H37 H 0.7331 0.4061 0.1682 0.050 Uiso 1 1 calc R . . C38 C 0.6631(5) 0.4211(4) 0.2658(4) 0.0398(13) Uani 1 1 d U . . H38 H 0.7300 0.4140 0.2932 0.048 Uiso 1 1 calc R . . C39 C 0.5622(5) 0.4357(3) 0.3004(3) 0.0277(10) Uani 1 1 d U . . C40 C 0.4650(6) 0.4427(5) 0.2577(4) 0.0472(16) Uani 1 1 d U . . H40 H 0.3946 0.4496 0.2797 0.057 Uiso 1 1 calc R . . C41 C 0.4745(6) 0.4392(5) 0.1818(4) 0.0539(19) Uani 1 1 d U . . H41 H 0.4088 0.4450 0.1532 0.065 Uiso 1 1 calc R . . C42 C 0.5602(5) 0.4513(3) 0.3793(3) 0.0257(9) Uani 1 1 d U . . C43 C 0.7551(8) 0.6986(5) 0.8625(4) 0.065(2) Uani 1 1 d U . . H43 H 0.7459 0.6468 0.8933 0.077 Uiso 1 1 calc R . . C44 C 0.7749(7) 0.7091(4) 0.7848(4) 0.0519(19) Uani 1 1 d U . . H44 H 0.7812 0.6652 0.7641 0.062 Uiso 1 1 calc R . . C45 C 0.7854(5) 0.7860(3) 0.7372(3) 0.0277(10) Uani 1 1 d U . . C46 C 0.7757(6) 0.8471(4) 0.7712(4) 0.0470(17) Uani 1 1 d U . . H46 H 0.7812 0.8996 0.7411 0.056 Uiso 1 1 calc R . . C47 C 0.7576(7) 0.8319(5) 0.8508(4) 0.056(2) Uani 1 1 d U . . H47 H 0.7519 0.8748 0.8729 0.067 Uiso 1 1 calc R . . C48 C 0.8032(4) 0.7985(3) 0.6516(3) 0.0248(9) Uani 1 1 d U . . C49 C 0.2598(6) 0.3572(4) -0.1643(4) 0.0447(16) Uani 1 1 d U . . H49 H 0.2931 0.3968 -0.1479 0.054 Uiso 1 1 calc R . . C50 C 0.2369(6) 0.3715(4) -0.2415(3) 0.0372(13) Uani 1 1 d U . . H50 H 0.2536 0.4200 -0.2762 0.045 Uiso 1 1 calc R . . C51 C 0.1889(5) 0.3135(4) -0.2672(3) 0.0288(11) Uani 1 1 d U . . C52 C 0.1622(6) 0.2439(4) -0.2126(3) 0.0470(18) Uani 1 1 d U . . H52 H 0.1276 0.2040 -0.2276 0.056 Uiso 1 1 calc R . . C53 C 0.1870(6) 0.2341(5) -0.1363(4) 0.052(2) Uani 1 1 d U . . H53 H 0.1683 0.1869 -0.1004 0.063 Uiso 1 1 calc R . . C54 C 0.1695(5) 0.3258(4) -0.3523(3) 0.0281(10) Uani 1 1 d U . . C55 C 0.6455(4) 0.7508(3) 0.4929(3) 0.0258(10) Uani 1 1 d U . . C56 C 0.5203(5) 0.7573(4) 0.4887(6) 0.063(3) Uani 1 1 d U . . H56A H 0.4975 0.7468 0.4415 0.094 Uiso 1 1 calc R . . H56B H 0.4929 0.8104 0.4895 0.094 Uiso 1 1 calc R . . H56C H 0.4897 0.7189 0.5323 0.094 Uiso 1 1 calc R . . C57 C 1.1260(5) 0.7338(3) 0.5170(4) 0.0336(11) Uani 1 1 d U . . C58 C 1.2493(5) 0.7407(6) 0.5208(6) 0.078(3) Uani 1 1 d U . . H58A H 1.2886 0.6940 0.5113 0.117 Uiso 1 1 calc R . . H58B H 1.2681 0.7447 0.5714 0.117 Uiso 1 1 calc R . . H58C H 1.2710 0.7877 0.4824 0.117 Uiso 1 1 calc R . . Cu1 Cu 0.78800(7) 1.21609(6) -0.07177(5) 0.0477(2) Uani 1 1 d U . . Cu2 Cu 1.09017(7) 1.01934(5) 0.04433(5) 0.0494(2) Uani 1 1 d U . . Cu3 Cu 1.47478(8) 1.08642(6) -0.03576(5) 0.0515(2) Uani 1 1 d U . . Cu4 Cu 0.73715(7) 1.25293(5) 0.05122(4) 0.0410(2) Uani 1 1 d U . . Cu5 Cu 0.95054(7) 0.57206(5) 0.02605(5) 0.0459(2) Uani 1 1 d U . . Cu6 Cu 0.60104(7) 0.43859(6) 0.02423(5) 0.0462(2) Uani 1 1 d U . . Cu7 Cu 0.29223(8) 0.27387(6) -0.00619(4) 0.0535(3) Uani 1 1 d U . . Eu1 Eu 0.67669(2) 0.950638(15) 0.508151(14) 0.01871(8) Uani 1 1 d U . . Eu2 Eu 0.67622(2) 0.544169(15) 0.493485(15) 0.01996(8) Uani 1 1 d U . . Eu3 Eu 0.88975(2) 0.734600(15) 0.502925(15) 0.01911(8) Uani 1 1 d U . . N1 N 0.9166(5) 1.1460(4) -0.0455(4) 0.0601(15) Uani 1 1 d U . . N2 N 1.2459(5) 1.0292(4) 0.0221(3) 0.0498(14) Uani 1 1 d U . . N3 N 0.5818(5) 1.1476(4) -0.0061(3) 0.0475(13) Uani 1 1 d U . . N4 N 0.8693(5) 1.3114(4) 0.0298(4) 0.0577(15) Uani 1 1 d U . . N5 N 0.8163(5) 0.5249(4) 0.0140(4) 0.0533(16) Uani 1 1 d U . . N6 N 0.4970(5) 0.3768(4) -0.0067(4) 0.0601(17) Uani 1 1 d U . . N7 N 0.2838(4) 0.7285(3) 0.1715(3) 0.0443(13) Uani 1 1 d U . . N8 N 1.0294(5) 0.9886(3) 0.1569(3) 0.0431(12) Uani 1 1 d U . . N9 N 0.5037(5) 0.9162(4) 0.1514(3) 0.0471(14) Uani 1 1 d U . . N10 N 0.6773(4) 1.2295(3) 0.1613(3) 0.0402(11) Uani 1 1 d U . . N11 N 0.9825(5) 0.4759(4) 0.8596(3) 0.0494(15) Uani 1 1 d U . . N12 N 0.5723(5) 0.4280(4) 0.1473(3) 0.0447(12) Uani 1 1 d U . . N13 N 0.7482(5) 0.7583(4) 0.8962(3) 0.0472(13) Uani 1 1 d U . . N14 N 0.2367(5) 0.2892(3) -0.1112(3) 0.0429(13) Uani 1 1 d U . . O1 O 0.3706(3) 0.5864(2) 0.4423(2) 0.0343(9) Uani 1 1 d U . . O2 O 0.5416(3) 0.6222(2) 0.3980(2) 0.0338(8) Uani 1 1 d U . . O3 O 0.7920(3) 0.9580(2) 0.3962(2) 0.0293(6) Uani 1 1 d U . . O4 O 0.9330(3) 0.8657(2) 0.4362(2) 0.0264(6) Uani 1 1 d U . . O5 O 0.5348(3) 0.9539(2) 0.4176(2) 0.0293(7) Uani 1 1 d U . . O6 O 0.3528(3) 0.9800(2) 0.3910(2) 0.0313(9) Uani 1 1 d U . . O7 O 0.6353(3) 1.0868(2) 0.4403(2) 0.0281(7) Uani 1 1 d U . . O8 O 0.4575(3) 1.1234(2) 0.4038(2) 0.0312(9) Uani 1 1 d U . . O9 O 0.9222(3) 0.6003(2) 0.5749(2) 0.0256(5) Uani 1 1 d U . . O10 O 0.7693(3) 0.5313(2) 0.6137(2) 0.0315(6) Uani 1 1 d U . . O11 O 0.6502(3) 0.4743(2) 0.3978(2) 0.0344(8) Uani 1 1 d U . . O12 O 0.4716(3) 0.4416(3) 0.4189(2) 0.0370(9) Uani 1 1 d U . . O13 O 0.8269(3) 0.7374(2) 0.6290(2) 0.0283(5) Uani 1 1 d U . . O14 O 0.7934(3) 0.8686(2) 0.6086(2) 0.0267(6) Uani 1 1 d U . . O15 O 0.1924(3) 0.3913(2) -0.3983(2) 0.0340(9) Uani 1 1 d U . . O16 O 0.1326(4) 0.2682(3) -0.3730(2) 0.0412(10) Uani 1 1 d U . . O17 O 0.7013(3) 0.8127(2) 0.4865(2) 0.0232(5) Uani 1 1 d U . . O18 O 0.6984(3) 0.6832(2) 0.5019(2) 0.0251(6) Uani 1 1 d U . . O19 O 1.0858(3) 0.7058(2) 0.4669(3) 0.0327(6) Uani 1 1 d U . . O20 O 1.0599(3) 0.7547(2) 0.5664(3) 0.0344(6) Uani 1 1 d U . . O21W O 0.8471(3) 1.0208(2) 0.5223(3) 0.0337(7) Uani 1 1 d U . . H21A H 0.8773 1.0482 0.4835 0.040 Uiso 1 1 d R . . H21B H 0.8283 1.0474 0.5527 0.040 Uiso 1 1 d R . . O22W O 0.8547(3) 0.4601(2) 0.4954(3) 0.0355(8) Uani 1 1 d U . . H22A H 0.8541 0.4118 0.5154 0.043 Uiso 1 1 d R . . H22B H 0.8955 0.4701 0.4569 0.043 Uiso 1 1 d R . . O23W O 0.0372(4) 0.9015(3) 0.6027(3) 0.0489(12) Uani 1 1 d . . . H23A H 0.0402 0.8539 0.6053 0.059 Uiso 1 1 d R . . H23B H -0.0261 0.9225 0.5955 0.059 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(3) 0.035(3) 0.035(2) -0.005(2) 0.019(2) 0.003(2) C2 0.049(2) 0.060(4) 0.031(3) -0.022(3) 0.009(3) -0.017(3) C3 0.043(2) 0.040(3) 0.033(2) -0.008(2) -0.0042(17) -0.0043(17) C4 0.041(3) 0.031(3) 0.027(3) 0.001(3) -0.003(3) -0.010(2) C5 0.026(2) 0.037(3) 0.029(3) -0.008(2) -0.0031(18) 0.0009(17) C6 0.039(3) 0.042(3) 0.024(3) -0.019(3) -0.004(2) -0.0012(19) C7 0.027(2) 0.050(4) 0.027(2) -0.004(3) -0.0047(13) 0.009(3) C8 0.0275(19) 0.050(4) 0.0255(18) 0.002(3) -0.0027(15) 0.005(2) C9 0.0268(17) 0.031(3) 0.0218(14) -0.0046(19) -0.0055(11) 0.001(2) C10 0.034(3) 0.074(5) 0.0266(17) 0.004(3) 0.0019(15) 0.013(3) C11 0.044(3) 0.089(5) 0.0226(15) -0.003(3) 0.003(2) 0.025(4) C12 0.0284(13) 0.020(3) 0.0248(17) -0.0017(18) -0.0051(13) 0.0022(18) C13 0.079(5) 0.062(5) 0.038(3) 0.013(3) 0.028(3) 0.034(3) C14 0.063(4) 0.050(4) 0.039(3) 0.010(3) 0.025(3) 0.023(3) C15 0.028(3) 0.028(3) 0.0266(17) -0.0087(16) 0.0097(16) -0.0025(17) C16 0.031(3) 0.055(4) 0.0275(19) -0.0107(19) 0.0072(19) 0.010(2) C17 0.029(3) 0.060(4) 0.0283(17) -0.0115(19) 0.008(2) 0.009(2) C18 0.028(2) 0.0215(15) 0.0258(16) -0.0104(13) 0.0095(12) -0.0076(14) C19 0.031(2) 0.142(8) 0.049(4) -0.058(5) 0.009(2) -0.008(4) C20 0.0243(18) 0.121(7) 0.045(4) -0.050(4) 0.002(2) -0.004(4) C21 0.0245(18) 0.037(3) 0.026(2) -0.015(2) -0.0009(14) 0.001(2) C22 0.025(2) 0.074(5) 0.027(3) -0.025(3) 0.0016(18) -0.007(3) C23 0.036(2) 0.085(5) 0.033(3) -0.034(4) 0.005(2) -0.016(4) C24 0.0257(14) 0.027(3) 0.019(2) -0.005(2) -0.0039(12) 0.002(2) C25 0.0277(19) 0.060(4) 0.0262(10) -0.007(3) 0.0051(13) -0.014(3) C26 0.0226(16) 0.051(4) 0.0250(14) -0.006(2) 0.0026(15) -0.004(2) C27 0.0224(16) 0.028(3) 0.0252(16) 0.000(2) 0.0021(12) -0.001(2) C28 0.0249(19) 0.078(5) 0.0304(18) 0.009(3) -0.0020(12) -0.005(3) C29 0.0309(17) 0.101(6) 0.0253(16) 0.002(3) -0.0015(11) -0.002(4) C30 0.0277(14) 0.0171(18) 0.0257(16) -0.0028(15) 0.0037(12) -0.0033(17) C31 0.057(5) 0.093(6) 0.032(3) 0.010(3) -0.021(3) -0.043(4) C32 0.044(4) 0.077(5) 0.031(2) 0.012(3) -0.018(3) -0.031(3) C33 0.027(3) 0.031(3) 0.0234(16) -0.0042(18) -0.0073(16) -0.0013(19) C34 0.060(4) 0.064(5) 0.027(2) 0.006(3) -0.017(3) -0.035(3) C35 0.072(5) 0.087(6) 0.030(3) 0.015(3) -0.022(3) -0.048(4) C36 0.035(2) 0.0227(17) 0.0217(15) -0.0077(14) -0.0072(12) -0.0024(18) C37 0.0345(19) 0.064(4) 0.0323(17) -0.024(3) 0.0064(16) -0.005(3) C38 0.0345(19) 0.059(4) 0.032(2) -0.022(3) 0.0049(17) -0.001(3) C39 0.0303(18) 0.030(3) 0.027(2) -0.016(2) 0.0010(13) -0.004(2) C40 0.0335(19) 0.078(5) 0.038(2) -0.027(4) -0.0028(16) -0.011(3) C41 0.0333(19) 0.098(6) 0.040(2) -0.033(4) -0.0055(14) -0.016(4) C42 0.0343(19) 0.021(3) 0.025(2) -0.0109(19) 0.0032(14) -0.005(2) C43 0.122(7) 0.046(2) 0.0196(19) -0.0013(18) 0.007(4) 0.002(4) C44 0.096(6) 0.036(2) 0.0210(18) -0.0051(15) 0.006(4) 0.002(4) C45 0.032(3) 0.0360(19) 0.0164(12) -0.0091(9) 0.000(2) -0.001(2) C46 0.079(5) 0.043(2) 0.0250(19) -0.0170(17) 0.013(3) -0.018(4) C47 0.093(6) 0.059(2) 0.026(2) -0.025(2) 0.013(4) -0.028(4) C48 0.023(3) 0.0336(13) 0.0164(11) -0.0075(9) -0.0023(17) 0.0097(18) C49 0.063(4) 0.055(3) 0.0211(15) -0.0132(14) 0.001(3) -0.026(3) C50 0.052(4) 0.041(3) 0.0214(14) -0.0088(16) 0.000(3) -0.016(3) C51 0.031(3) 0.039(2) 0.0184(14) -0.0100(14) 0.003(2) -0.009(2) C52 0.069(5) 0.053(3) 0.0200(15) -0.0046(19) -0.005(3) -0.033(3) C53 0.073(5) 0.064(4) 0.0198(16) -0.004(2) -0.005(3) -0.040(4) C54 0.024(3) 0.042(2) 0.0182(14) -0.0075(14) 0.002(2) -0.009(2) C55 0.0176(7) 0.0260(12) 0.035(3) -0.011(2) -0.001(2) -0.0019(10) C56 0.0177(11) 0.041(3) 0.142(8) -0.047(5) -0.003(4) -0.0008(13) C57 0.0182(7) 0.027(3) 0.059(4) -0.016(3) -0.0050(17) 0.000(2) C58 0.0205(14) 0.103(7) 0.133(8) -0.069(6) -0.001(3) -0.012(4) Cu1 0.0428(5) 0.0680(6) 0.0241(4) -0.0007(4) -0.0061(4) 0.0085(4) Cu2 0.0477(5) 0.0574(5) 0.0356(5) -0.0024(4) 0.0169(4) 0.0019(4) Cu3 0.0514(5) 0.0754(6) 0.0369(5) -0.0269(5) 0.0080(4) -0.0257(5) Cu4 0.0476(5) 0.0497(5) 0.0257(4) -0.0067(3) 0.0068(3) -0.0205(4) Cu5 0.0425(5) 0.0596(5) 0.0334(4) -0.0039(4) -0.0061(4) -0.0209(4) Cu6 0.0412(5) 0.0662(6) 0.0352(4) -0.0162(4) -0.0023(4) -0.0208(4) Cu7 0.0617(6) 0.0869(7) 0.0160(4) -0.0144(4) 0.0020(4) -0.0322(5) Eu1 0.01817(13) 0.02358(14) 0.01366(13) -0.00422(11) 0.00191(10) -0.00025(10) Eu2 0.02174(14) 0.02298(14) 0.01477(14) -0.00407(11) -0.00137(10) -0.00243(10) Eu3 0.01722(13) 0.02527(14) 0.01513(14) -0.00608(11) -0.00018(10) -0.00071(10) N1 0.045(2) 0.069(4) 0.067(4) -0.023(3) -0.008(2) 0.0110(19) N2 0.0461(12) 0.058(4) 0.044(3) -0.012(3) 0.014(2) -0.0051(19) N3 0.057(3) 0.056(4) 0.035(3) -0.019(3) -0.003(2) -0.014(2) N4 0.052(3) 0.069(4) 0.049(3) -0.007(3) 0.014(2) -0.030(3) N5 0.045(3) 0.060(4) 0.052(4) -0.004(3) -0.007(3) -0.021(2) N6 0.057(3) 0.080(4) 0.054(3) -0.031(3) -0.013(3) -0.022(3) N7 0.039(2) 0.060(4) 0.0255(18) -0.001(3) -0.0020(18) 0.012(3) N8 0.047(3) 0.048(3) 0.0317(15) -0.0089(16) 0.0116(17) 0.006(2) N9 0.039(2) 0.080(4) 0.035(3) -0.036(3) 0.0078(18) -0.010(3) N10 0.0372(19) 0.055(3) 0.0251(10) -0.0030(16) 0.0017(10) -0.014(2) N11 0.043(3) 0.074(4) 0.025(2) 0.003(2) -0.013(2) -0.022(3) N12 0.0396(19) 0.064(4) 0.0357(13) -0.019(2) 0.0034(11) -0.022(2) N13 0.061(4) 0.067(3) 0.018(2) -0.0144(16) 0.003(3) -0.019(3) N14 0.052(3) 0.063(3) 0.0173(14) -0.0099(14) 0.000(2) -0.027(3) O1 0.0448(19) 0.030(2) 0.0257(17) -0.0013(16) -0.0009(16) -0.0100(18) O2 0.0318(12) 0.0380(18) 0.0299(18) -0.0046(14) -0.0142(11) -0.0034(10) O3 0.0356(13) 0.0280(11) 0.0208(11) -0.0025(10) 0.0119(10) 0.0007(9) O4 0.0241(11) 0.0271(8) 0.0287(14) -0.0086(9) 0.0089(10) -0.0049(6) O5 0.0307(11) 0.0311(15) 0.0269(17) -0.0098(15) -0.0100(11) 0.0057(9) O6 0.0269(12) 0.046(2) 0.025(2) -0.0177(18) 0.0001(14) 0.0010(17) O7 0.0342(15) 0.0238(7) 0.0239(15) -0.0030(10) 0.0023(13) 0.0012(9) O8 0.0288(12) 0.033(2) 0.028(2) -0.0029(17) 0.0077(13) -0.0036(16) O9 0.0268(11) 0.0264(7) 0.0233(14) -0.0067(8) -0.0060(9) 0.0027(6) O10 0.0378(16) 0.0357(15) 0.0191(14) -0.0013(10) -0.0085(11) -0.0096(12) O11 0.0400(16) 0.0424(17) 0.0286(17) -0.0210(16) 0.0058(14) -0.0129(13) O12 0.0321(17) 0.053(3) 0.029(2) -0.016(2) 0.0038(15) -0.0007(18) O13 0.0391(15) 0.0309(10) 0.0153(9) -0.0078(8) -0.0012(8) 0.0035(10) O14 0.0282(18) 0.0323(10) 0.0188(11) -0.0068(7) -0.0032(10) 0.0056(11) O15 0.036(2) 0.0401(18) 0.0228(16) -0.0042(14) 0.0055(18) -0.0038(17) O16 0.053(3) 0.056(2) 0.0182(19) -0.0115(17) 0.0026(19) -0.027(2) O17 0.0182(7) 0.0237(6) 0.0278(15) -0.0068(9) -0.0016(10) -0.0007(6) O18 0.0192(7) 0.0247(6) 0.0328(17) -0.0098(10) -0.0018(11) -0.0021(7) O19 0.0191(8) 0.0347(14) 0.048(2) -0.0185(15) 0.0051(12) -0.0011(7) O20 0.0233(9) 0.0380(14) 0.0481(18) -0.0219(13) -0.0138(10) 0.0027(8) O21W 0.0270(14) 0.0303(10) 0.047(2) -0.0154(12) -0.0011(15) -0.0055(9) O22W 0.0303(15) 0.0257(12) 0.049(2) -0.0089(17) 0.0018(14) 0.0029(11) O23W 0.034(2) 0.052(3) 0.062(3) -0.017(2) -0.004(2) -0.010(2) _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 N1 1.144(8) . ? C1 Cu2 1.919(7) . ? C1 Cu2 2.421(7) 2_775 ? C2 N2 1.149(8) . ? C2 Cu3 1.869(7) . ? C3 N3 1.147(8) . ? C3 Cu4 1.928(7) . ? C3 Cu1 2.167(7) . ? C4 N4 1.137(8) . ? C4 Cu5 1.893(6) 2_775 ? C5 N5 1.148(7) . ? C5 Cu6 1.886(6) . ? C6 N6 1.150(8) . ? C6 Cu7 1.993(6) . ? C7 N7 1.328(8) . ? C7 C8 1.367(8) . ? C8 C9 1.374(8) . ? C9 C10 1.379(8) . ? C9 C12 1.501(7) . ? C10 C11 1.382(9) . ? C11 N7 1.323(8) . ? C12 O2 1.246(6) . ? C12 O1 1.253(7) . ? C13 N8 1.328(8) . ? C13 C14 1.387(9) . ? C14 C15 1.378(8) . ? C15 C16 1.389(8) . ? C15 C18 1.494(7) . ? C16 C17 1.371(8) . ? C17 N8 1.341(8) . ? C18 O4 1.254(6) . ? C18 O3 1.256(6) . ? C19 N9 1.331(9) . ? C19 C20 1.370(10) . ? C20 C21 1.370(8) . ? C21 C22 1.384(8) . ? C21 C24 1.512(8) . ? C22 C23 1.377(9) . ? C23 N9 1.327(8) . ? C24 O5 1.244(6) . ? C24 O6 1.249(6) . ? C24 Eu1 3.222(5) 2_676 ? C25 N10 1.338(8) . ? C25 C26 1.363(8) . ? C26 C27 1.375(8) . ? C27 C28 1.369(8) . ? C27 C30 1.496(7) . ? C28 C29 1.369(9) . ? C29 N10 1.336(8) . ? C30 O8 1.244(6) . ? C30 O7 1.256(6) . ? C31 N11 1.309(8) . ? C31 C32 1.388(9) . ? C32 C33 1.375(8) . ? C33 C34 1.358(8) . ? C33 C36 1.516(7) . ? C34 C35 1.369(9) . ? C35 N11 1.328(8) . ? C36 O10 1.249(6) . ? C36 O9 1.260(6) . ? C37 N12 1.329(8) . ? C37 C38 1.371(9) . ? C38 C39 1.376(8) . ? C39 C40 1.383(8) . ? C39 C42 1.507(8) . ? C40 C41 1.378(9) . ? C41 N12 1.329(9) . ? C42 O12 1.247(7) . ? C42 O11 1.249(6) . ? C43 N13 1.331(9) . ? C43 C44 1.369(9) . ? C44 C45 1.386(8) . ? C45 C46 1.354(9) . ? C45 C48 1.502(7) . ? C46 C47 1.391(9) . ? C47 N13 1.324(9) . ? C48 O13 1.246(6) . ? C48 O14 1.251(6) . ? C49 N14 1.340(8) . ? C49 C50 1.368(8) . ? C50 C51 1.375(8) . ? C51 C52 1.381(8) . ? C51 C54 1.503(8) . ? C52 C53 1.368(9) . ? C53 N14 1.335(8) . ? C54 O15 1.250(6) . ? C54 O16 1.262(7) . ? C54 Eu3 3.255(6) 2_665 ? C55 O18 1.266(6) . ? C55 O17 1.276(6) . ? C55 C56 1.486(8) . ? C57 O19 1.248(7) . ? C57 O20 1.277(7) . ? C57 C58 1.482(8) . ? Cu1 N1 1.875(6) . ? Cu1 N7 1.972(5) 2_675 ? Cu1 Cu4 2.5022(12) . ? Cu2 N2 1.891(6) . ? Cu2 N8 2.064(5) . ? Cu2 C1 2.421(7) 2_775 ? Cu2 Cu2 2.9176(19) 2_775 ? Cu3 N3 1.882(6) 1_655 ? Cu3 N9 2.093(5) 2_775 ? Cu3 Cu3 2.952(2) 2_875 ? Cu4 N4 1.898(6) . ? Cu4 N10 2.021(5) . ? Cu5 N5 1.882(6) . ? Cu5 C4 1.893(6) 2_775 ? Cu5 N11 2.146(5) 2_766 ? Cu5 Cu5 3.051(2) 2_765 ? Cu6 N6 1.875(6) . ? Cu6 N12 2.181(6) . ? Cu7 N13 1.952(5) 2_666 ? Cu7 N14 1.954(5) . ? Eu1 O5 2.358(4) . ? Eu1 O7 2.371(4) . ? Eu1 O3 2.377(4) . ? Eu1 O14 2.382(3) . ? Eu1 O8 2.390(4) 2_676 ? Eu1 O6 2.432(4) 2_676 ? Eu1 O21W 2.482(4) . ? Eu1 O17 2.521(4) . ? Eu1 C24 3.222(6) 2_676 ? Eu1 Eu3 4.4017(4) . ? Eu1 Eu1 4.4150(6) 2_676 ? Eu2 O1 2.341(4) 2_666 ? Eu2 O12 2.369(4) 2_666 ? Eu2 O15 2.376(4) 2_665 ? Eu2 O11 2.387(4) . ? Eu2 O10 2.398(4) . ? Eu2 O2 2.434(4) . ? Eu2 O18 2.486(4) . ? Eu2 O22W 2.489(4) . ? Eu2 Eu3 4.3345(4) . ? Eu3 O4 2.347(4) . ? Eu3 O9 2.350(3) . ? Eu3 O16 2.364(4) 2_665 ? Eu3 O13 2.370(4) . ? Eu3 O20 2.436(4) . ? Eu3 O19 2.455(4) . ? Eu3 O18 2.498(3) . ? Eu3 O17 2.521(3) . ? Eu3 C54 3.255(6) 2_665 ? N3 Cu3 1.882(6) 1_455 ? N7 Cu1 1.972(5) 2_675 ? N9 Cu3 2.093(5) 2_775 ? N11 Cu5 2.146(5) 2_766 ? N13 Cu7 1.952(5) 2_666 ? O1 Eu2 2.341(4) 2_666 ? O6 Eu1 2.432(4) 2_676 ? O8 Eu1 2.390(4) 2_676 ? O12 Eu2 2.369(4) 2_666 ? O15 Eu2 2.376(4) 2_665 ? O16 Eu3 2.364(4) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cu2 172.7(7) . . ? N1 C1 Cu2 100.9(6) . 2_775 ? Cu2 C1 Cu2 83.6(2) . 2_775 ? N2 C2 Cu3 174.2(7) . . ? N3 C3 Cu4 167.8(6) . . ? N3 C3 Cu1 117.0(5) . . ? Cu4 C3 Cu1 75.1(2) . . ? N4 C4 Cu5 164.5(6) . 2_775 ? N5 C5 Cu6 170.2(6) . . ? N6 C6 Cu7 162.3(6) . . ? N7 C7 C8 123.9(6) . . ? C7 C8 C9 118.9(6) . . ? C8 C9 C10 117.8(5) . . ? C8 C9 C12 121.0(5) . . ? C10 C9 C12 121.0(5) . . ? C9 C10 C11 119.5(6) . . ? N7 C11 C10 122.5(6) . . ? O2 C12 O1 125.8(5) . . ? O2 C12 C9 118.9(5) . . ? O1 C12 C9 115.3(5) . . ? N8 C13 C14 124.2(6) . . ? C15 C14 C13 119.1(6) . . ? C14 C15 C16 117.3(6) . . ? C14 C15 C18 121.1(5) . . ? C16 C15 C18 121.6(5) . . ? C17 C16 C15 119.4(6) . . ? N8 C17 C16 124.1(6) . . ? O4 C18 O3 125.4(5) . . ? O4 C18 C15 117.8(5) . . ? O3 C18 C15 116.8(5) . . ? N9 C19 C20 123.7(6) . . ? C21 C20 C19 119.7(6) . . ? C20 C21 C22 117.1(6) . . ? C20 C21 C24 122.1(5) . . ? C22 C21 C24 120.8(5) . . ? C23 C22 C21 119.4(6) . . ? N9 C23 C22 123.4(6) . . ? O5 C24 O6 125.6(5) . . ? O5 C24 C21 117.4(5) . . ? O6 C24 C21 117.0(5) . . ? O5 C24 Eu1 85.4(3) . 2_676 ? O6 C24 Eu1 41.5(3) . 2_676 ? C21 C24 Eu1 154.1(3) . 2_676 ? N10 C25 C26 123.1(6) . . ? C25 C26 C27 120.4(6) . . ? C28 C27 C26 116.8(5) . . ? C28 C27 C30 120.8(5) . . ? C26 C27 C30 122.4(5) . . ? C27 C28 C29 120.2(6) . . ? N10 C29 C28 123.1(6) . . ? O8 C30 O7 126.1(5) . . ? O8 C30 C27 117.2(5) . . ? O7 C30 C27 116.7(5) . . ? N11 C31 C32 124.0(6) . . ? C33 C32 C31 118.7(6) . . ? C34 C33 C32 117.3(5) . . ? C34 C33 C36 121.0(5) . . ? C32 C33 C36 121.6(5) . . ? C33 C34 C35 120.1(6) . . ? N11 C35 C34 123.5(6) . . ? O10 C36 O9 125.5(5) . . ? O10 C36 C33 116.3(5) . . ? O9 C36 C33 118.1(5) . . ? N12 C37 C38 123.5(6) . . ? C37 C38 C39 119.4(6) . . ? C38 C39 C40 117.7(6) . . ? C38 C39 C42 120.3(5) . . ? C40 C39 C42 121.7(5) . . ? C41 C40 C39 118.8(6) . . ? N12 C41 C40 123.6(6) . . ? O12 C42 O11 126.3(5) . . ? O12 C42 C39 118.9(5) . . ? O11 C42 C39 114.7(5) . . ? N13 C43 C44 123.6(7) . . ? C43 C44 C45 119.2(7) . . ? C46 C45 C44 117.2(6) . . ? C46 C45 C48 123.1(5) . . ? C44 C45 C48 119.7(5) . . ? C45 C46 C47 120.5(6) . . ? N13 C47 C46 122.2(7) . . ? O13 C48 O14 125.1(5) . . ? O13 C48 C45 116.7(5) . . ? O14 C48 C45 118.2(5) . . ? N14 C49 C50 123.4(6) . . ? C49 C50 C51 119.3(6) . . ? C50 C51 C52 117.7(5) . . ? C50 C51 C54 120.2(5) . . ? C52 C51 C54 122.1(5) . . ? C53 C52 C51 119.6(6) . . ? N14 C53 C52 123.0(6) . . ? O15 C54 O16 124.0(5) . . ? O15 C54 C51 118.7(5) . . ? O16 C54 C51 117.3(5) . . ? O15 C54 Eu3 87.6(3) . 2_665 ? O16 C54 Eu3 36.5(3) . 2_665 ? C51 C54 Eu3 153.5(4) . 2_665 ? O18 C55 O17 119.0(5) . . ? O18 C55 C56 119.9(5) . . ? O17 C55 C56 121.1(5) . . ? O19 C57 O20 119.2(5) . . ? O19 C57 C58 120.7(6) . . ? O20 C57 C58 120.1(6) . . ? N1 Cu1 N7 133.0(3) . 2_675 ? N1 Cu1 C3 115.0(3) . . ? N7 Cu1 C3 103.5(2) 2_675 . ? N1 Cu1 Cu4 103.7(2) . . ? N7 Cu1 Cu4 122.33(17) 2_675 . ? C3 Cu1 Cu4 48.11(18) . . ? N2 Cu2 C1 119.5(3) . . ? N2 Cu2 N8 121.6(2) . . ? C1 Cu2 N8 107.1(2) . . ? N2 Cu2 C1 113.5(2) . 2_775 ? C1 Cu2 C1 96.4(2) . 2_775 ? N8 Cu2 C1 92.9(2) . 2_775 ? N2 Cu2 Cu2 130.9(2) . 2_775 ? C1 Cu2 Cu2 55.6(2) . 2_775 ? N8 Cu2 Cu2 103.58(17) . 2_775 ? C1 Cu2 Cu2 40.81(16) 2_775 2_775 ? C2 Cu3 N3 136.4(3) . 1_655 ? C2 Cu3 N9 109.7(3) . 2_775 ? N3 Cu3 N9 112.1(2) 1_655 2_775 ? C2 Cu3 Cu3 75.5(2) . 2_875 ? N3 Cu3 Cu3 110.57(19) 1_655 2_875 ? N9 Cu3 Cu3 97.28(18) 2_775 2_875 ? N4 Cu4 C3 140.9(3) . . ? N4 Cu4 N10 116.3(3) . . ? C3 Cu4 N10 101.7(2) . . ? N4 Cu4 Cu1 84.2(2) . . ? C3 Cu4 Cu1 56.8(2) . . ? N10 Cu4 Cu1 153.39(16) . . ? N5 Cu5 C4 147.8(3) . 2_775 ? N5 Cu5 N11 111.6(2) . 2_766 ? C4 Cu5 N11 100.4(2) 2_775 2_766 ? N5 Cu5 Cu5 80.4(2) . 2_765 ? C4 Cu5 Cu5 103.2(2) 2_775 2_765 ? N11 Cu5 Cu5 91.94(19) 2_766 2_765 ? N6 Cu6 C5 152.7(3) . . ? N6 Cu6 N12 107.7(2) . . ? C5 Cu6 N12 98.4(2) . . ? N13 Cu7 N14 144.5(2) 2_666 . ? N13 Cu7 C6 107.1(2) 2_666 . ? N14 Cu7 C6 106.8(2) . . ? O5 Eu1 O7 72.37(13) . . ? O5 Eu1 O3 80.90(14) . . ? O7 Eu1 O3 80.48(13) . . ? O5 Eu1 O14 146.15(13) . . ? O7 Eu1 O14 141.48(13) . . ? O3 Eu1 O14 102.05(13) . . ? O5 Eu1 O8 82.05(14) . 2_676 ? O7 Eu1 O8 120.88(13) . 2_676 ? O3 Eu1 O8 146.59(14) . 2_676 ? O14 Eu1 O8 77.48(13) . 2_676 ? O5 Eu1 O6 121.22(13) . 2_676 ? O7 Eu1 O6 75.22(13) . 2_676 ? O3 Eu1 O6 138.72(13) . 2_676 ? O14 Eu1 O6 78.68(13) . 2_676 ? O8 Eu1 O6 74.49(14) 2_676 2_676 ? O5 Eu1 O21W 140.45(14) . . ? O7 Eu1 O21W 74.89(13) . . ? O3 Eu1 O21W 72.30(14) . . ? O14 Eu1 O21W 69.63(13) . . ? O8 Eu1 O21W 134.80(14) 2_676 . ? O6 Eu1 O21W 69.44(13) 2_676 . ? O5 Eu1 O17 77.24(12) . . ? O7 Eu1 O17 141.27(12) . . ? O3 Eu1 O17 71.41(12) . . ? O14 Eu1 O17 72.06(12) . . ? O8 Eu1 O17 76.91(13) 2_676 . ? O6 Eu1 O17 142.66(13) 2_676 . ? O21W Eu1 O17 118.87(12) . . ? O5 Eu1 C24 102.03(13) . 2_676 ? O7 Eu1 C24 71.04(13) . 2_676 ? O3 Eu1 C24 148.64(13) . 2_676 ? O14 Eu1 C24 92.62(13) . 2_676 ? O8 Eu1 C24 63.50(14) 2_676 2_676 ? O6 Eu1 C24 19.91(13) 2_676 2_676 ? O21W Eu1 C24 87.51(14) . 2_676 ? O17 Eu1 C24 139.91(13) . 2_676 ? O5 Eu1 Eu3 103.20(9) . . ? O7 Eu1 Eu3 143.37(9) . . ? O3 Eu1 Eu3 63.04(9) . . ? O14 Eu1 Eu3 52.20(9) . . ? O8 Eu1 Eu3 93.50(9) 2_676 . ? O6 Eu1 Eu3 130.88(9) 2_676 . ? O21W Eu1 Eu3 90.15(9) . . ? O17 Eu1 Eu3 29.19(8) . . ? C24 Eu1 Eu3 142.76(9) 2_676 . ? O5 Eu1 Eu1 48.59(9) . 2_676 ? O7 Eu1 Eu1 60.52(9) . 2_676 ? O3 Eu1 Eu1 121.89(9) . 2_676 ? O14 Eu1 Eu1 135.54(9) . 2_676 ? O8 Eu1 Eu1 62.52(9) 2_676 2_676 ? O6 Eu1 Eu1 72.86(9) 2_676 2_676 ? O21W Eu1 Eu1 127.17(9) . 2_676 ? O17 Eu1 Eu1 113.64(8) . 2_676 ? C24 Eu1 Eu1 53.45(9) 2_676 2_676 ? Eu3 Eu1 Eu1 142.655(10) . 2_676 ? O1 Eu2 O12 74.14(15) 2_666 2_666 ? O1 Eu2 O15 138.57(15) 2_666 2_665 ? O12 Eu2 O15 147.25(15) 2_666 2_665 ? O1 Eu2 O11 72.07(14) 2_666 . ? O12 Eu2 O11 120.50(14) 2_666 . ? O15 Eu2 O11 80.71(14) 2_665 . ? O1 Eu2 O10 81.53(13) 2_666 . ? O12 Eu2 O10 75.54(14) 2_666 . ? O15 Eu2 O10 103.61(14) 2_665 . ? O11 Eu2 O10 142.09(14) . . ? O1 Eu2 O2 116.12(14) 2_666 . ? O12 Eu2 O2 82.53(14) 2_666 . ? O15 Eu2 O2 81.90(14) 2_665 . ? O11 Eu2 O2 70.84(14) . . ? O10 Eu2 O2 146.86(14) . . ? O1 Eu2 O18 147.20(14) 2_666 . ? O12 Eu2 O18 78.94(13) 2_666 . ? O15 Eu2 O18 69.71(13) 2_665 . ? O11 Eu2 O18 139.42(13) . . ? O10 Eu2 O18 73.81(13) . . ? O2 Eu2 O18 77.85(12) . . ? O1 Eu2 O22W 75.19(14) 2_666 . ? O12 Eu2 O22W 137.60(14) 2_666 . ? O15 Eu2 O22W 68.06(14) 2_665 . ? O11 Eu2 O22W 75.61(14) . . ? O10 Eu2 O22W 71.58(14) . . ? O2 Eu2 O22W 137.90(14) . . ? O18 Eu2 O22W 115.52(12) . . ? O1 Eu2 Eu3 143.78(10) 2_666 . ? O12 Eu2 Eu3 102.39(10) 2_666 . ? O15 Eu2 Eu3 52.22(10) 2_665 . ? O11 Eu2 Eu3 132.93(10) . . ? O10 Eu2 Eu3 63.09(9) . . ? O2 Eu2 Eu3 98.68(9) . . ? O18 Eu2 Eu3 29.66(8) . . ? O22W Eu2 Eu3 85.93(9) . . ? O4 Eu3 O9 157.84(13) . . ? O4 Eu3 O16 79.00(14) . 2_665 ? O9 Eu3 O16 106.05(14) . 2_665 ? O4 Eu3 O13 107.32(13) . . ? O9 Eu3 O13 77.37(13) . . ? O16 Eu3 O13 155.21(14) 2_665 . ? O4 Eu3 O20 76.66(13) . . ? O9 Eu3 O20 83.77(13) . . ? O16 Eu3 O20 128.52(15) 2_665 . ? O13 Eu3 O20 76.01(14) . . ? O4 Eu3 O19 81.61(13) . . ? O9 Eu3 O19 78.30(13) . . ? O16 Eu3 O19 79.22(15) 2_665 . ? O13 Eu3 O19 125.04(14) . . ? O20 Eu3 O19 52.89(14) . . ? O4 Eu3 O18 122.94(12) . . ? O9 Eu3 O18 78.99(12) . . ? O16 Eu3 O18 76.08(13) 2_665 . ? O13 Eu3 O18 80.64(13) . . ? O20 Eu3 O18 153.49(14) . . ? O19 Eu3 O18 140.04(13) . . ? O4 Eu3 O17 75.89(12) . . ? O9 Eu3 O17 125.56(12) . . ? O16 Eu3 O17 85.24(14) 2_665 . ? O13 Eu3 O17 73.59(12) . . ? O20 Eu3 O17 130.10(12) . . ? O19 Eu3 O17 154.71(13) . . ? O18 Eu3 O17 51.73(11) . . ? O4 Eu3 C54 97.43(14) . 2_665 ? O9 Eu3 C54 89.62(14) . 2_665 ? O16 Eu3 C54 18.53(14) 2_665 2_665 ? O13 Eu3 C54 143.82(14) . 2_665 ? O20 Eu3 C54 136.60(14) . 2_665 ? O19 Eu3 C54 83.74(14) . 2_665 ? O18 Eu3 C54 63.67(13) . 2_665 ? O17 Eu3 C54 87.82(13) . 2_665 ? O4 Eu3 Eu2 142.29(9) . . ? O9 Eu3 Eu2 56.22(9) . . ? O16 Eu3 Eu2 69.82(10) 2_665 . ? O13 Eu3 Eu2 93.71(10) . . ? O20 Eu3 Eu2 139.99(10) . . ? O19 Eu3 Eu2 111.71(9) . . ? O18 Eu3 Eu2 29.51(8) . . ? O17 Eu3 Eu2 80.79(8) . . ? C54 Eu3 Eu2 52.08(10) 2_665 . ? O4 Eu3 Eu1 55.98(9) . . ? O9 Eu3 Eu1 140.15(9) . . ? O16 Eu3 Eu1 100.97(12) 2_665 . ? O13 Eu3 Eu1 66.16(9) . . ? O20 Eu3 Eu1 101.71(9) . . ? O19 Eu3 Eu1 136.09(9) . . ? O18 Eu3 Eu1 79.75(8) . . ? O17 Eu3 Eu1 29.19(8) . . ? C54 Eu3 Eu1 110.25(10) 2_665 . ? Eu2 Eu3 Eu1 109.232(9) . . ? C1 N1 Cu1 166.2(6) . . ? C2 N2 Cu2 169.4(6) . . ? C3 N3 Cu3 175.9(6) . 1_455 ? C4 N4 Cu4 178.4(7) . . ? C5 N5 Cu5 176.4(6) . . ? C6 N6 Cu6 171.5(6) . . ? C11 N7 C7 117.3(5) . . ? C11 N7 Cu1 122.0(4) . 2_675 ? C7 N7 Cu1 120.4(4) . 2_675 ? C13 N8 C17 115.9(6) . . ? C13 N8 Cu2 120.3(5) . . ? C17 N8 Cu2 123.6(4) . . ? C23 N9 C19 116.5(6) . . ? C23 N9 Cu3 121.1(4) . 2_775 ? C19 N9 Cu3 122.0(4) . 2_775 ? C29 N10 C25 116.4(5) . . ? C29 N10 Cu4 121.9(4) . . ? C25 N10 Cu4 120.4(4) . . ? C31 N11 C35 116.3(6) . . ? C31 N11 Cu5 122.1(4) . 2_766 ? C35 N11 Cu5 121.5(4) . 2_766 ? C41 N12 C37 116.9(6) . . ? C41 N12 Cu6 126.9(5) . . ? C37 N12 Cu6 115.8(4) . . ? C47 N13 C43 117.2(6) . . ? C47 N13 Cu7 128.1(5) . 2_666 ? C43 N13 Cu7 114.3(5) . 2_666 ? C53 N14 C49 116.9(5) . . ? C53 N14 Cu7 125.2(4) . . ? C49 N14 Cu7 117.6(4) . . ? C12 O1 Eu2 139.3(4) . 2_666 ? C12 O2 Eu2 133.5(4) . . ? C18 O3 Eu1 132.0(3) . . ? C18 O4 Eu3 133.7(3) . . ? C24 O5 Eu1 172.5(4) . . ? C24 O6 Eu1 118.6(3) . 2_676 ? C30 O7 Eu1 132.9(3) . . ? C30 O8 Eu1 138.6(3) . 2_676 ? C36 O9 Eu3 130.5(3) . . ? C36 O10 Eu2 129.4(4) . . ? C42 O11 Eu2 127.7(4) . . ? C42 O12 Eu2 162.5(4) . 2_666 ? C48 O13 Eu3 126.3(3) . . ? C48 O14 Eu1 140.6(4) . . ? C54 O15 Eu2 144.4(4) . 2_665 ? C54 O16 Eu3 124.9(4) . 2_665 ? C55 O17 Eu3 94.0(3) . . ? C55 O17 Eu1 139.8(3) . . ? Eu3 O17 Eu1 121.62(14) . . ? C55 O18 Eu2 142.4(3) . . ? C55 O18 Eu3 95.3(3) . . ? Eu2 O18 Eu3 120.84(14) . . ? C57 O19 Eu3 93.6(3) . . ? C57 O20 Eu3 93.8(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.847 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 964392' ####################################################################### # # 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_I-C #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H42 Cu7 Gd3 N14 O22, H2 O' _chemical_formula_sum 'C58 H44 Cu7 Gd3 N14 O23' _chemical_formula_weight 2221.68 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8653(11) _cell_length_b 17.3600(16) _cell_length_c 17.9132(16) _cell_angle_alpha 74.3680(10) _cell_angle_beta 88.4170(10) _cell_angle_gamma 86.1580(10) _cell_volume 3545.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 12823 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 25.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2138 _exptl_absorpt_coefficient_mu 4.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.321 _exptl_absorpt_correction_T_max 0.375 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18717 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.40 _reflns_number_total 12823 _reflns_number_gt 10640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0368P)^2^+3.6835P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00119(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12823 _refine_ls_number_parameters 949 _refine_ls_number_restraints 346 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0167(6) -0.0968(4) 1.0152(4) 0.0428(14) Uani 1 1 d U . . C2 C -0.3362(6) -0.0463(4) 0.9980(4) 0.0455(17) Uani 1 1 d U . . C3 C 0.6447(6) 0.1879(4) 1.0079(4) 0.0401(12) Uani 1 1 d U . . C4 C 0.9466(5) 0.3479(4) 1.0158(3) 0.0334(13) Uani 1 1 d U . . C5 C 0.7341(5) 0.4945(4) 0.0112(3) 0.0314(12) Uani 1 1 d U . . C6 C 0.4308(5) 0.3356(4) -0.0159(3) 0.0343(13) Uani 1 1 d U . . C7 C 0.7743(5) 0.2797(4) 0.7623(3) 0.0372(14) Uani 1 1 d U . . H7 H 0.8504 0.2625 0.7647 0.045 Uiso 1 1 calc R . . C8 C 0.7273(5) 0.3130(4) 0.6904(3) 0.0357(13) Uani 1 1 d U . . H8 H 0.7715 0.3194 0.6457 0.043 Uiso 1 1 calc R . . C9 C 0.6145(5) 0.3365(3) 0.6854(3) 0.0275(11) Uani 1 1 d U . . C10 C 0.5534(6) 0.3259(5) 0.7530(4) 0.0510(19) Uani 1 1 d U . . H10 H 0.4761 0.3393 0.7518 0.061 Uiso 1 1 calc R . . C11 C 0.6071(6) 0.2951(5) 0.8230(4) 0.060(2) Uani 1 1 d U . . H11 H 0.5650 0.2910 0.8684 0.072 Uiso 1 1 calc R . . C12 C 0.5622(5) 0.3791(3) 0.6091(3) 0.0247(10) Uani 1 1 d U . . C13 C 0.0616(7) -0.0277(5) 0.8232(4) 0.067(3) Uani 1 1 d U . . H13 H 0.0938 -0.0713 0.8603 0.080 Uiso 1 1 calc R . . C14 C 0.1106(7) -0.0072(4) 0.7495(4) 0.058(2) Uani 1 1 d U . . H14 H 0.1744 -0.0364 0.7382 0.070 Uiso 1 1 calc R . . C15 C 0.0641(5) 0.0563(3) 0.6938(3) 0.0268(11) Uani 1 1 d U . . C16 C -0.0298(5) 0.0981(4) 0.7130(4) 0.0366(13) Uani 1 1 d U . . H16 H -0.0637 0.1416 0.6766 0.044 Uiso 1 1 calc R . . C17 C -0.0721(5) 0.0741(4) 0.7871(4) 0.0431(16) Uani 1 1 d U . . H17 H -0.1354 0.1031 0.7995 0.052 Uiso 1 1 calc R . . C18 C 0.1173(5) 0.0802(3) 0.6139(3) 0.0228(9) Uani 1 1 d U . . C19 C 0.4107(6) 0.0739(6) 0.8065(4) 0.069(3) Uani 1 1 d U . . H19 H 0.3384 0.0734 0.8280 0.083 Uiso 1 1 calc R . . C20 C 0.4230(6) 0.0636(5) 0.7329(4) 0.058(2) Uani 1 1 d U . . H20 H 0.3599 0.0593 0.7050 0.070 Uiso 1 1 calc R . . C21 C 0.5292(5) 0.0599(4) 0.7011(3) 0.0277(11) Uani 1 1 d U . . C22 C 0.6187(5) 0.0694(4) 0.7444(4) 0.0414(15) Uani 1 1 d U . . H22 H 0.6920 0.0672 0.7251 0.050 Uiso 1 1 calc R . . C23 C 0.5992(6) 0.0823(5) 0.8167(4) 0.0471(17) Uani 1 1 d U . . H23 H 0.6606 0.0898 0.8446 0.056 Uiso 1 1 calc R . . C24 C 0.5483(5) 0.0410(3) 0.6243(3) 0.0256(10) Uani 1 1 d U . . C25 C 0.7483(5) 0.2080(4) 1.2212(3) 0.0387(14) Uani 1 1 d U . . H25 H 0.8246 0.2161 1.2117 0.046 Uiso 1 1 calc R . . C26 C 0.7139(5) 0.1741(4) 1.2961(4) 0.0368(14) Uani 1 1 d U . . H26 H 0.7668 0.1587 1.3356 0.044 Uiso 1 1 calc R . . C27 C 0.6027(5) 0.1629(3) 1.3127(3) 0.0277(11) Uani 1 1 d U . . C28 C 0.5278(5) 0.1878(5) 1.2525(4) 0.0482(18) Uani 1 1 d U . . H28 H 0.4506 0.1830 1.2615 0.058 Uiso 1 1 calc R . . C29 C 0.5690(6) 0.2201(5) 1.1784(4) 0.060(2) Uani 1 1 d U . . H29 H 0.5176 0.2358 1.1381 0.072 Uiso 1 1 calc R . . C30 C 0.5619(5) 0.1204(3) 1.3930(3) 0.0242(10) Uani 1 1 d U . . C31 C -0.0289(7) 0.4661(5) 0.1926(4) 0.064(3) Uani 1 1 d U . . H31 H -0.0880 0.4418 0.1768 0.077 Uiso 1 1 calc R . . C32 C 0.0039(6) 0.4383(5) 0.2692(4) 0.059(2) Uani 1 1 d U . . H32 H -0.0340 0.3980 0.3035 0.071 Uiso 1 1 calc R . . C33 C 0.0933(5) 0.4713(4) 0.2937(3) 0.0289(11) Uani 1 1 d U . . C34 C 0.1474(7) 0.5286(5) 0.2380(4) 0.057(2) Uani 1 1 d U . . H34 H 0.2114 0.5502 0.2509 0.068 Uiso 1 1 calc R . . C35 C 0.1069(7) 0.5537(5) 0.1635(4) 0.062(2) Uani 1 1 d U . . H35 H 0.1441 0.5931 0.1275 0.075 Uiso 1 1 calc R . . C36 C 0.1379(5) 0.4442(3) 0.3748(3) 0.0254(9) Uani 1 1 d U . . C37 C 0.6644(6) 0.4174(4) 0.1909(4) 0.0436(15) Uani 1 1 d U . . H37 H 0.7337 0.4071 0.1688 0.052 Uiso 1 1 calc R . . C38 C 0.6632(5) 0.4207(4) 0.2664(4) 0.0380(13) Uani 1 1 d U . . H38 H 0.7300 0.4130 0.2940 0.046 Uiso 1 1 calc R . . C39 C 0.5618(5) 0.4355(3) 0.3011(3) 0.0272(10) Uani 1 1 d U . . C40 C 0.4653(5) 0.4431(4) 0.2581(4) 0.0443(15) Uani 1 1 d U . . H40 H 0.3950 0.4504 0.2803 0.053 Uiso 1 1 calc R . . C41 C 0.4732(6) 0.4400(5) 0.1816(4) 0.056(2) Uani 1 1 d U . . H41 H 0.4073 0.4465 0.1530 0.067 Uiso 1 1 calc R . . C42 C 0.5601(5) 0.4503(3) 0.3798(3) 0.0248(9) Uani 1 1 d U . . C43 C 0.2431(8) 0.3015(5) 0.1380(4) 0.061(2) Uani 1 1 d U . . H43 H 0.2501 0.3534 0.1071 0.074 Uiso 1 1 calc R . . C44 C 0.2239(7) 0.2909(4) 0.2159(4) 0.0520(19) Uani 1 1 d U . . H44 H 0.2175 0.3348 0.2365 0.062 Uiso 1 1 calc R . . C45 C 0.2142(5) 0.2147(4) 0.2632(3) 0.0286(11) Uani 1 1 d U . . C46 C 0.2240(6) 0.1527(4) 0.2286(4) 0.0453(16) Uani 1 1 d U . . H46 H 0.2177 0.1003 0.2585 0.054 Uiso 1 1 calc R . . C47 C 0.2430(7) 0.1681(5) 0.1501(4) 0.056(2) Uani 1 1 d U . . H47 H 0.2496 0.1251 0.1282 0.067 Uiso 1 1 calc R . . C48 C 0.1974(4) 0.2012(3) 0.3489(3) 0.0235(9) Uani 1 1 d U . . C49 C 0.2591(6) 0.3578(4) 0.8364(3) 0.0421(15) Uani 1 1 d U . . H49 H 0.2908 0.3976 0.8533 0.051 Uiso 1 1 calc R . . C50 C 0.2370(5) 0.3721(4) 0.7581(3) 0.0357(13) Uani 1 1 d U . . H50 H 0.2544 0.4202 0.7233 0.043 Uiso 1 1 calc R . . C51 C 0.1890(5) 0.3140(4) 0.7326(3) 0.0277(11) Uani 1 1 d U . . C52 C 0.1629(6) 0.2446(4) 0.7861(3) 0.0469(18) Uani 1 1 d U . . H52 H 0.1295 0.2046 0.7705 0.056 Uiso 1 1 calc R . . C53 C 0.1863(7) 0.2342(5) 0.8632(4) 0.053(2) Uani 1 1 d U . . H53 H 0.1663 0.1873 0.8988 0.064 Uiso 1 1 calc R . . C54 C 0.1709(5) 0.3261(4) 0.6472(3) 0.0278(10) Uani 1 1 d U . . C55 C 0.3546(5) 0.2493(3) 0.5070(4) 0.0300(7) Uani 1 1 d U . . C56 C 0.4788(5) 0.2430(4) 0.5121(5) 0.059(2) Uani 1 1 d U . . H56A H 0.5092 0.2046 0.4859 0.089 Uiso 1 1 calc R . . H56B H 0.5005 0.2260 0.5656 0.089 Uiso 1 1 calc R . . H56C H 0.5076 0.2943 0.4882 0.089 Uiso 1 1 calc R . . C57 C -0.1241(5) 0.2665(4) 0.4816(4) 0.0384(8) Uani 1 1 d U . . C58 C -0.2493(6) 0.2594(6) 0.4795(6) 0.076(3) Uani 1 1 d U . . H58A H -0.2678 0.2441 0.4339 0.114 Uiso 1 1 calc R . . H58B H -0.2879 0.3100 0.4786 0.114 Uiso 1 1 calc R . . H58C H -0.2724 0.2195 0.5247 0.114 Uiso 1 1 calc R . . Cu1 Cu 0.78759(7) 0.21599(6) 0.92842(5) 0.0488(2) Uani 1 1 d U . . Cu2 Cu -0.08991(8) -0.01894(6) 0.95531(5) 0.0505(2) Uani 1 1 d U . . Cu3 Cu 0.47490(8) 0.08614(6) 0.96431(5) 0.0522(2) Uani 1 1 d U . . Cu4 Cu 0.73679(7) 0.25304(5) 1.05147(4) 0.0419(2) Uani 1 1 d U . . Cu5 Cu 1.04938(7) 0.42797(6) 0.97376(5) 0.0467(2) Uani 1 1 d U . . Cu6 Cu 0.60113(7) 0.43864(6) 0.02431(5) 0.0469(2) Uani 1 1 d U . . Cu7 Cu 0.29193(8) 0.27415(6) -0.00620(5) 0.0543(3) Uani 1 1 d U . . Gd1 Gd 0.32330(2) 0.049931(15) 0.491782(14) 0.01882(8) Uani 1 1 d U . . Gd2 Gd 0.32398(2) 0.455784(16) 0.506497(15) 0.02013(8) Uani 1 1 d U . . Gd3 Gd 0.11079(2) 0.265893(16) 0.496995(15) 0.01896(8) Uani 1 1 d U . . N1 N 0.0829(5) -0.1455(4) 1.0455(4) 0.0601(17) Uani 1 1 d U . . N2 N -0.2468(5) -0.0291(4) 0.9772(3) 0.0518(15) Uani 1 1 d U . . N3 N 0.5816(5) 0.1478(4) 0.9932(3) 0.0442(13) Uani 1 1 d U . . N4 N 0.8703(5) 0.3106(4) 1.0303(4) 0.0589(15) Uani 1 1 d U . . N5 N 0.8158(5) 0.5249(4) 0.0144(4) 0.0552(17) Uani 1 1 d U . . N6 N 0.4967(5) 0.3766(4) -0.0064(4) 0.0625(18) Uani 1 1 d U . . N7 N 0.7161(5) 0.2709(4) 0.8290(3) 0.0450(13) Uani 1 1 d U . . N8 N -0.0293(5) 0.0122(3) 0.8429(3) 0.0428(12) Uani 1 1 d U . . N9 N 0.4960(5) 0.0843(4) 0.8483(3) 0.0486(14) Uani 1 1 d U . . N10 N 0.6776(4) 0.2300(3) 1.1615(3) 0.0419(12) Uani 1 1 d U . . N11 N 0.0173(5) 0.5244(4) 0.1403(3) 0.0509(16) Uani 1 1 d U . . N12 N 0.5725(5) 0.4279(4) 0.1471(3) 0.0437(12) Uani 1 1 d U . . N13 N 0.2523(5) 0.2415(4) 0.1038(3) 0.0461(12) Uani 1 1 d U . . N14 N 0.2366(5) 0.2887(4) 0.8892(3) 0.0441(14) Uani 1 1 d U . . O1 O 0.6304(4) 0.4140(2) 0.5576(2) 0.0341(9) Uani 1 1 d U . . O2 O 0.4584(3) 0.3778(2) 0.6010(2) 0.0340(8) Uani 1 1 d U . . O3 O 0.2070(3) 0.0430(2) 0.6028(2) 0.0307(6) Uani 1 1 d U . . O4 O 0.0673(3) 0.1354(2) 0.5631(2) 0.0283(6) Uani 1 1 d U . . O5 O 0.4636(3) 0.0465(2) 0.5817(2) 0.0291(8) Uani 1 1 d U . . O6 O 0.6466(3) 0.0200(2) 0.6087(2) 0.0317(9) Uani 1 1 d U . . O7 O 0.6360(3) 0.0862(2) 1.4408(2) 0.0284(8) Uani 1 1 d U . . O8 O 0.4575(3) 0.1231(2) 1.4044(2) 0.0312(9) Uani 1 1 d U . . O9 O 0.0780(3) 0.3993(2) 0.4257(2) 0.0303(6) Uani 1 1 d U . . O10 O 0.2306(3) 0.4684(2) 0.3865(2) 0.0335(7) Uani 1 1 d U . . O11 O 0.6493(3) 0.4749(2) 0.3980(2) 0.0329(9) Uani 1 1 d U . . O12 O 0.4710(3) 0.4414(2) 0.4185(2) 0.0325(8) Uani 1 1 d U . . O13 O 0.1742(3) 0.2630(2) 0.3718(2) 0.0328(6) Uani 1 1 d U . . O14 O 0.2075(3) 0.1313(2) 0.3919(2) 0.0303(7) Uani 1 1 d U . . O15 O 0.1931(3) 0.3920(2) 0.6020(2) 0.0316(7) Uani 1 1 d U . . O16 O 0.1334(3) 0.2695(3) 0.6264(2) 0.0336(6) Uani 1 1 d U . . O17 O 0.3019(3) 0.3173(2) 0.4980(2) 0.0278(5) Uani 1 1 d U . . O18 O 0.2987(3) 0.1873(2) 0.5130(2) 0.0261(5) Uani 1 1 d U . . O19 O -0.0854(3) 0.2951(2) 0.5333(2) 0.0342(7) Uani 1 1 d U . . O20 O -0.0593(3) 0.2456(3) 0.4334(2) 0.0353(7) Uani 1 1 d U . . O21W O 0.1535(3) -0.0202(2) 0.4769(2) 0.0342(8) Uani 1 1 d U . . H21A H 0.1929 -0.0423 0.4491 0.041 Uiso 1 1 d R . . H21B H 0.1208 -0.0537 0.5100 0.041 Uiso 1 1 d R . . O22W O 0.1463(3) 0.5398(2) 0.5041(3) 0.0394(9) Uani 1 1 d U . . H22A H 0.1559 0.5880 0.4934 0.047 Uiso 1 1 d R . . H22B H 0.1008 0.5265 0.5395 0.047 Uiso 1 1 d R . . O23W O 0.0373(4) 0.9022(3) 0.6014(3) 0.0480(12) Uani 1 1 d . . . H23A H -0.0303 0.9149 0.6026 0.058 Uiso 1 1 d R . . H23B H 0.0494 0.8558 0.5996 0.058 Uiso 1 1 d R . . 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 0.051(3) 0.040(3) 0.033(2) -0.003(2) 0.017(3) -0.008(2) C2 0.051(2) 0.059(5) 0.036(4) -0.028(3) 0.009(3) -0.014(3) C3 0.045(3) 0.039(4) 0.037(3) -0.009(3) -0.0043(19) -0.004(2) C4 0.034(3) 0.035(3) 0.029(3) -0.004(2) -0.006(2) -0.0045(19) C5 0.032(3) 0.035(3) 0.028(3) -0.010(2) -0.0040(19) 0.0029(19) C6 0.039(3) 0.050(4) 0.020(3) -0.019(3) -0.007(2) 0.001(2) C7 0.030(2) 0.050(4) 0.0263(11) -0.003(3) -0.0054(13) 0.010(3) C8 0.0284(19) 0.049(4) 0.0243(12) -0.002(3) -0.0035(14) 0.006(2) C9 0.0282(17) 0.030(3) 0.0211(15) -0.0024(19) -0.0044(11) 0.002(2) C10 0.035(2) 0.079(5) 0.0244(17) 0.006(3) 0.0010(13) 0.018(3) C11 0.044(3) 0.101(6) 0.0213(16) -0.001(4) 0.0002(16) 0.029(4) C12 0.0310(13) 0.021(3) 0.0213(17) -0.0055(17) -0.0061(12) 0.0041(18) C13 0.078(5) 0.061(5) 0.040(3) 0.014(3) 0.029(3) 0.033(3) C14 0.068(5) 0.052(4) 0.037(3) 0.010(3) 0.024(3) 0.027(3) C15 0.025(3) 0.034(3) 0.0223(17) -0.0105(16) 0.0052(16) 0.0005(18) C16 0.028(3) 0.053(4) 0.0277(19) -0.0116(19) 0.0060(19) 0.009(2) C17 0.034(3) 0.062(4) 0.0297(19) -0.011(2) 0.010(2) 0.013(2) C18 0.027(2) 0.0213(15) 0.0233(16) -0.0109(12) 0.0077(12) -0.0068(14) C19 0.029(2) 0.148(8) 0.050(3) -0.061(5) 0.008(2) -0.010(4) C20 0.0262(18) 0.119(7) 0.046(3) -0.050(5) 0.002(2) -0.001(4) C21 0.0241(18) 0.037(3) 0.026(2) -0.016(2) -0.0029(14) 0.004(2) C22 0.030(2) 0.070(5) 0.035(3) -0.029(3) -0.0018(17) -0.009(3) C23 0.034(2) 0.083(5) 0.036(3) -0.034(4) -0.0027(17) -0.011(4) C24 0.0256(15) 0.031(3) 0.021(2) -0.010(2) -0.0041(12) 0.003(2) C25 0.028(2) 0.060(4) 0.0278(10) -0.010(3) 0.0065(13) -0.009(3) C26 0.0255(17) 0.054(4) 0.0273(15) -0.005(3) 0.0018(15) -0.006(3) C27 0.0240(17) 0.034(3) 0.0227(17) -0.005(2) 0.0021(12) 0.001(2) C28 0.029(2) 0.078(5) 0.0275(19) 0.005(3) -0.0029(12) -0.006(3) C29 0.0343(18) 0.107(6) 0.0250(17) 0.005(3) -0.0020(12) -0.005(4) C30 0.0271(15) 0.024(3) 0.0224(17) -0.0086(18) 0.0018(12) -0.002(2) C31 0.058(5) 0.091(6) 0.036(3) 0.009(3) -0.024(3) -0.041(4) C32 0.057(5) 0.082(6) 0.033(3) 0.003(3) -0.019(3) -0.037(4) C33 0.028(3) 0.034(3) 0.0248(16) -0.0072(18) -0.0075(16) -0.001(2) C34 0.069(5) 0.068(5) 0.028(2) 0.004(3) -0.016(3) -0.037(4) C35 0.068(5) 0.079(6) 0.032(2) 0.011(3) -0.020(3) -0.041(4) C36 0.033(2) 0.0212(17) 0.0232(15) -0.0081(14) -0.0077(12) 0.0010(18) C37 0.037(2) 0.069(5) 0.0333(17) -0.026(3) 0.0058(15) -0.007(3) C38 0.0328(19) 0.055(4) 0.031(2) -0.021(3) 0.0042(16) 0.001(3) C39 0.0287(18) 0.028(3) 0.0268(19) -0.011(2) 0.0028(12) -0.005(2) C40 0.032(2) 0.068(5) 0.036(2) -0.020(3) -0.0032(16) -0.003(3) C41 0.035(2) 0.102(6) 0.039(2) -0.030(4) -0.0031(15) -0.017(4) C42 0.0260(17) 0.023(3) 0.025(2) -0.007(2) 0.0034(13) 0.001(2) C43 0.115(7) 0.045(2) 0.0190(17) -0.0023(14) 0.007(4) 0.006(4) C44 0.095(6) 0.036(2) 0.0205(15) -0.0049(14) 0.010(3) 0.006(4) C45 0.033(3) 0.0359(19) 0.0170(12) -0.0088(9) 0.002(2) 0.003(3) C46 0.075(5) 0.043(2) 0.0236(14) -0.0162(13) 0.010(3) -0.015(4) C47 0.095(6) 0.057(2) 0.0250(17) -0.0232(15) 0.014(4) -0.030(4) C48 0.018(2) 0.0356(15) 0.0155(11) -0.0070(8) -0.0017(16) 0.0066(17) C49 0.053(4) 0.058(3) 0.022(2) -0.019(2) 0.001(3) -0.021(3) C50 0.048(4) 0.042(3) 0.0213(17) -0.0132(17) 0.001(3) -0.015(3) C51 0.027(3) 0.041(3) 0.0176(11) -0.0106(12) 0.000(2) -0.009(2) C52 0.068(5) 0.053(3) 0.0201(16) -0.0042(19) -0.008(3) -0.032(4) C53 0.075(5) 0.063(4) 0.0200(17) -0.002(2) -0.010(3) -0.033(4) C54 0.030(3) 0.040(2) 0.0158(11) -0.0111(12) 0.0055(18) -0.0094(19) C55 0.0181(5) 0.0261(11) 0.048(2) -0.014(2) -0.0023(10) 0.0007(7) C56 0.0182(9) 0.043(3) 0.127(7) -0.042(5) -0.009(4) 0.0021(13) C57 0.0183(5) 0.040(2) 0.064(3) -0.027(2) -0.0054(9) 0.0028(10) C58 0.0199(10) 0.092(6) 0.136(8) -0.064(6) -0.003(3) -0.009(4) Cu1 0.0428(5) 0.0695(6) 0.0262(4) -0.0020(4) -0.0077(3) 0.0115(4) Cu2 0.0509(5) 0.0574(6) 0.0365(5) -0.0044(4) 0.0179(4) 0.0026(4) Cu3 0.0525(5) 0.0767(7) 0.0377(5) -0.0289(5) 0.0082(4) -0.0237(5) Cu4 0.0490(5) 0.0508(5) 0.0268(4) -0.0088(4) 0.0072(3) -0.0201(4) Cu5 0.0426(5) 0.0608(6) 0.0351(5) -0.0056(4) -0.0063(4) -0.0199(4) Cu6 0.0410(5) 0.0687(6) 0.0356(5) -0.0183(4) -0.0026(4) -0.0172(4) Cu7 0.0623(6) 0.0875(7) 0.0180(4) -0.0164(4) 0.0009(4) -0.0293(5) Gd1 0.01779(14) 0.02366(15) 0.01488(14) -0.00569(10) 0.00122(10) 0.00114(10) Gd2 0.02144(14) 0.02322(15) 0.01595(15) -0.00549(11) -0.00189(10) -0.00134(10) Gd3 0.01732(14) 0.02445(15) 0.01589(14) -0.00713(11) -0.00070(10) 0.00041(10) N1 0.055(4) 0.073(5) 0.052(4) -0.018(3) -0.006(3) 0.006(3) N2 0.0507(13) 0.063(4) 0.041(3) -0.013(3) 0.014(2) -0.006(2) N3 0.049(3) 0.059(4) 0.031(3) -0.021(3) 0.005(2) -0.015(2) N4 0.048(3) 0.073(4) 0.055(3) -0.013(3) 0.014(2) -0.026(3) N5 0.048(3) 0.065(4) 0.050(4) -0.006(3) -0.006(3) -0.019(3) N6 0.051(4) 0.098(5) 0.051(3) -0.036(3) -0.010(3) -0.023(3) N7 0.039(2) 0.064(4) 0.0243(9) -0.0024(18) -0.0048(13) 0.014(3) N8 0.044(3) 0.051(3) 0.0309(15) -0.0094(16) 0.0090(17) 0.006(2) N9 0.039(2) 0.078(4) 0.0403(19) -0.035(3) 0.0031(16) -0.009(3) N10 0.039(2) 0.056(3) 0.0272(10) -0.0036(17) 0.0021(10) -0.011(2) N11 0.042(3) 0.075(4) 0.031(3) -0.001(2) -0.010(2) -0.022(3) N12 0.042(2) 0.060(4) 0.0352(13) -0.020(2) 0.0020(11) -0.016(3) N13 0.063(3) 0.061(2) 0.0167(13) -0.0128(11) -0.002(2) -0.011(3) N14 0.051(3) 0.069(3) 0.016(2) -0.0142(17) 0.002(2) -0.023(3) O1 0.0464(19) 0.029(2) 0.0235(18) -0.0006(15) -0.0032(16) -0.0066(18) O2 0.0332(11) 0.039(2) 0.0276(14) -0.0057(14) -0.0110(10) 0.0036(13) O3 0.0365(14) 0.0321(16) 0.0216(12) -0.0061(11) 0.0119(10) 0.0018(11) O4 0.0279(12) 0.0292(9) 0.0280(14) -0.0068(8) 0.0018(12) -0.0064(8) O5 0.0323(12) 0.0301(18) 0.0253(18) -0.0092(15) -0.0105(11) 0.0058(12) O6 0.0286(13) 0.042(2) 0.028(2) -0.0178(18) 0.0004(14) 0.0040(17) O7 0.0303(17) 0.027(2) 0.0245(17) -0.0024(15) 0.0017(14) 0.0002(16) O8 0.0280(13) 0.035(2) 0.026(2) -0.0017(17) 0.0057(13) -0.0010(17) O9 0.0299(12) 0.0279(9) 0.0298(14) -0.0042(8) 0.0000(12) 0.0068(8) O10 0.0373(14) 0.0419(19) 0.0209(11) -0.0059(11) -0.0098(9) -0.0063(13) O11 0.0328(16) 0.044(3) 0.027(2) -0.0172(19) 0.0048(16) -0.0088(18) O12 0.0301(11) 0.038(2) 0.0291(14) -0.0089(16) 0.0084(10) -0.0041(12) O13 0.0410(14) 0.0399(14) 0.0170(9) -0.0096(10) 0.0029(8) 0.0080(14) O14 0.0295(19) 0.0368(12) 0.0217(12) -0.0030(10) -0.0073(11) 0.0013(14) O15 0.0326(13) 0.0374(14) 0.0232(12) -0.0059(10) 0.0068(10) -0.0019(13) O16 0.0428(15) 0.0449(16) 0.0176(8) -0.0143(10) 0.0011(9) -0.0106(15) O17 0.0191(7) 0.0258(7) 0.0403(16) -0.0125(11) 0.0018(9) -0.0005(7) O18 0.0195(7) 0.0247(7) 0.0345(16) -0.0090(10) -0.0044(10) 0.0010(6) O19 0.0205(7) 0.0406(17) 0.046(2) -0.0212(14) 0.0074(9) -0.0014(10) O20 0.0257(9) 0.0465(18) 0.0386(18) -0.0199(13) -0.0133(10) 0.0032(12) O21W 0.0272(16) 0.0354(16) 0.044(2) -0.0156(14) 0.0033(16) -0.0093(15) O22W 0.0333(16) 0.0315(15) 0.051(2) -0.0096(14) 0.0040(15) 0.0097(13) O23W 0.033(3) 0.051(3) 0.062(3) -0.018(2) -0.003(2) -0.009(2) _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 N1 1.146(9) . ? C1 Cu2 1.909(7) . ? C1 Cu2 2.430(7) 2_557 ? C2 N2 1.145(8) . ? C2 Cu3 1.866(7) 2_557 ? C3 N3 1.139(8) . ? C3 Cu4 1.941(7) . ? C4 N4 1.132(8) . ? C4 Cu5 1.897(6) . ? C5 N5 1.144(7) . ? C5 Cu6 1.883(6) . ? C6 N6 1.137(8) . ? C6 Cu7 2.001(6) . ? C7 N7 1.340(8) . ? C7 C8 1.379(8) . ? C7 H7 0.9300 . ? C8 C9 1.371(8) . ? C8 H8 0.9300 . ? C9 C10 1.370(8) . ? C9 C12 1.496(7) . ? C10 C11 1.379(9) . ? C10 H10 0.9300 . ? C11 N7 1.330(8) . ? C11 H11 0.9300 . ? C12 O2 1.246(6) . ? C12 O1 1.264(7) . ? C13 N8 1.334(9) . ? C13 C14 1.393(9) . ? C13 H13 0.9300 . ? C14 C15 1.368(9) . ? C14 H14 0.9300 . ? C15 C16 1.375(8) . ? C15 C18 1.512(7) . ? C16 C17 1.372(8) . ? C16 H16 0.9300 . ? C17 N8 1.337(8) . ? C17 H17 0.9300 . ? C18 O3 1.246(6) . ? C18 O4 1.258(6) . ? C19 N9 1.325(9) . ? C19 C20 1.380(9) . ? C19 H19 0.9300 . ? C20 C21 1.373(8) . ? C20 H20 0.9300 . ? C21 C22 1.377(8) . ? C21 C24 1.506(8) . ? C22 C23 1.383(9) . ? C22 H22 0.9300 . ? C23 N9 1.337(8) . ? C23 H23 0.9300 . ? C24 O6 1.246(6) . ? C24 O5 1.262(6) . ? C25 N10 1.334(8) . ? C25 C26 1.374(8) . ? C25 H25 0.9300 . ? C26 C27 1.359(8) . ? C26 H26 0.9300 . ? C27 C28 1.374(8) . ? C27 C30 1.512(7) . ? C28 C29 1.384(9) . ? C28 H28 0.9300 . ? C29 N10 1.327(8) . ? C29 H29 0.9300 . ? C30 O7 1.247(6) . ? C30 O8 1.251(6) . ? C31 N11 1.318(8) . ? C31 C32 1.383(9) . ? C31 H31 0.9300 . ? C32 C33 1.374(8) . ? C32 H32 0.9300 . ? C33 C34 1.382(8) . ? C33 C36 1.501(8) . ? C34 C35 1.377(9) . ? C34 H34 0.9300 . ? C35 N11 1.331(8) . ? C35 H35 0.9300 . ? C36 O10 1.245(6) . ? C36 O9 1.265(6) . ? C37 N12 1.335(8) . ? C37 C38 1.368(8) . ? C37 H37 0.9300 . ? C38 C39 1.380(8) . ? C38 H38 0.9300 . ? C39 C40 1.377(8) . ? C39 C42 1.499(8) . ? C40 C41 1.386(9) . ? C40 H40 0.9300 . ? C41 N12 1.346(9) . ? C41 H41 0.9300 . ? C42 O12 1.243(6) . ? C42 O11 1.251(6) . ? C43 N13 1.340(9) . ? C43 C44 1.372(9) . ? C43 H43 0.9300 . ? C44 C45 1.375(9) . ? C44 H44 0.9300 . ? C45 C46 1.376(8) . ? C45 C48 1.500(7) . ? C46 C47 1.375(9) . ? C46 H46 0.9300 . ? C47 N13 1.330(9) . ? C47 H47 0.9300 . ? C48 O14 1.250(6) . ? C48 O13 1.260(7) . ? C49 N14 1.350(8) . ? C49 C50 1.386(8) . ? C49 H49 0.9300 . ? C50 C51 1.374(8) . ? C50 H50 0.9300 . ? C51 C52 1.371(8) . ? C51 C54 1.507(7) . ? C52 C53 1.376(8) . ? C52 H52 0.9300 . ? C53 N14 1.340(8) . ? C53 H53 0.9300 . ? C54 O15 1.250(7) . ? C54 O16 1.252(7) . ? C55 O17 1.271(7) . ? C55 O18 1.280(6) . ? C55 C56 1.474(8) . ? C55 Gd3 2.894(5) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O20 1.249(7) . ? C57 O19 1.272(7) . ? C57 C58 1.501(8) . ? C57 Gd3 2.808(6) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? Cu1 N1 1.886(7) 2_657 ? Cu1 N7 1.965(5) . ? Cu1 Cu4 2.5049(12) . ? Cu2 N2 1.902(6) . ? Cu2 N8 2.061(5) . ? Cu2 C1 2.430(7) 2_557 ? Cu2 Cu2 2.914(2) 2_557 ? Cu3 C2 1.866(7) 2_557 ? Cu3 N3 1.879(6) . ? Cu3 N9 2.095(5) . ? Cu3 Cu3 2.946(2) 2_657 ? Cu4 N4 1.905(6) . ? Cu4 N10 2.018(5) . ? Cu5 N5 1.887(6) 2_766 ? Cu5 N11 2.139(5) 2_666 ? Cu5 Cu5 3.053(2) 2_767 ? Cu6 N6 1.880(6) . ? Cu6 N12 2.176(5) . ? Cu7 N14 1.949(5) 1_554 ? Cu7 N13 1.951(5) . ? Gd1 O5 2.334(4) . ? Gd1 O14 2.366(4) . ? Gd1 O3 2.370(4) . ? Gd1 O7 2.371(4) 2_657 ? Gd1 O8 2.379(4) 1_554 ? Gd1 O6 2.433(4) 2_656 ? Gd1 O21W 2.479(4) . ? Gd1 O18 2.511(4) . ? Gd1 H21A 2.5690 . ? Gd2 O1 2.335(4) 2_666 ? Gd2 O12 2.365(4) . ? Gd2 O15 2.372(4) . ? Gd2 O11 2.380(4) 2_666 ? Gd2 O10 2.396(4) . ? Gd2 O2 2.422(4) . ? Gd2 O22W 2.476(4) . ? Gd2 O17 2.481(4) . ? Gd3 O9 2.336(4) . ? Gd3 O4 2.341(4) . ? Gd3 O16 2.358(4) . ? Gd3 O13 2.359(4) . ? Gd3 O20 2.435(4) . ? Gd3 O19 2.456(4) . ? Gd3 O17 2.494(4) . ? Gd3 O18 2.517(4) . ? N1 Cu1 1.886(7) 2_657 ? N5 Cu5 1.887(6) 2_766 ? N11 Cu5 2.139(5) 2_666 ? N14 Cu7 1.949(5) 1_556 ? O1 Gd2 2.335(4) 2_666 ? O6 Gd1 2.433(4) 2_656 ? O7 Gd1 2.371(4) 2_657 ? O8 Gd1 2.379(4) 1_556 ? O11 Gd2 2.380(4) 2_666 ? O21W H21A 0.8254 . ? O21W H21B 0.8201 . ? O22W H22A 0.8204 . ? O22W H22B 0.8165 . ? O23W H23A 0.8187 . ? O23W H23B 0.8167 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cu2 174.1(7) . . ? N1 C1 Cu2 99.9(6) . 2_557 ? Cu2 C1 Cu2 83.5(3) . 2_557 ? N2 C2 Cu3 173.5(7) . 2_557 ? N3 C3 Cu4 169.2(6) . . ? N4 C4 Cu5 165.6(6) . . ? N5 C5 Cu6 170.4(6) . . ? N6 C6 Cu7 162.6(6) . . ? N7 C7 C8 123.4(6) . . ? N7 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C9 C8 C7 119.2(6) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 117.9(5) . . ? C10 C9 C12 120.9(5) . . ? C8 C9 C12 120.9(5) . . ? C9 C10 C11 119.6(6) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N7 C11 C10 123.3(6) . . ? N7 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? O2 C12 O1 125.6(5) . . ? O2 C12 C9 119.4(5) . . ? O1 C12 C9 115.0(5) . . ? N8 C13 C14 123.1(7) . . ? N8 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C15 C14 C13 119.3(6) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 118.4(6) . . ? C14 C15 C18 120.0(5) . . ? C16 C15 C18 121.5(5) . . ? C17 C16 C15 118.4(6) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? N8 C17 C16 124.9(6) . . ? N8 C17 H17 117.6 . . ? C16 C17 H17 117.6 . . ? O3 C18 O4 124.7(5) . . ? O3 C18 C15 117.6(5) . . ? O4 C18 C15 117.8(5) . . ? N9 C19 C20 123.7(7) . . ? N9 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C21 C20 C19 119.5(6) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 117.2(6) . . ? C20 C21 C24 121.7(5) . . ? C22 C21 C24 121.0(5) . . ? C21 C22 C23 119.9(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? N9 C23 C22 122.8(6) . . ? N9 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? O6 C24 O5 125.4(5) . . ? O6 C24 C21 117.0(5) . . ? O5 C24 C21 117.6(5) . . ? N10 C25 C26 123.3(6) . . ? N10 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C27 C26 C25 120.1(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 117.7(5) . . ? C26 C27 C30 122.0(5) . . ? C28 C27 C30 120.2(5) . . ? C27 C28 C29 118.8(6) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? N10 C29 C28 123.9(6) . . ? N10 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? O7 C30 O8 126.9(5) . . ? O7 C30 C27 116.6(5) . . ? O8 C30 C27 116.5(5) . . ? N11 C31 C32 125.0(6) . . ? N11 C31 H31 117.5 . . ? C32 C31 H31 117.5 . . ? C33 C32 C31 118.9(6) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 116.6(6) . . ? C32 C33 C36 123.4(5) . . ? C34 C33 C36 119.9(5) . . ? C35 C34 C33 120.2(6) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? N11 C35 C34 123.3(6) . . ? N11 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? O10 C36 O9 125.4(5) . . ? O10 C36 C33 117.2(5) . . ? O9 C36 C33 117.4(5) . . ? N12 C37 C38 124.1(6) . . ? N12 C37 H37 117.9 . . ? C38 C37 H37 117.9 . . ? C37 C38 C39 119.4(6) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C40 C39 C38 117.5(6) . . ? C40 C39 C42 122.1(5) . . ? C38 C39 C42 120.2(5) . . ? C39 C40 C41 119.9(6) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? N12 C41 C40 122.5(6) . . ? N12 C41 H41 118.8 . . ? C40 C41 H41 118.8 . . ? O12 C42 O11 126.4(5) . . ? O12 C42 C39 118.5(5) . . ? O11 C42 C39 115.0(5) . . ? N13 C43 C44 124.0(7) . . ? N13 C43 H43 118.0 . . ? C44 C43 H43 118.0 . . ? C43 C44 C45 119.3(7) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C44 C45 C46 117.2(6) . . ? C44 C45 C48 120.4(5) . . ? C46 C45 C48 122.4(5) . . ? C47 C46 C45 120.1(6) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? N13 C47 C46 123.2(7) . . ? N13 C47 H47 118.4 . . ? C46 C47 H47 118.4 . . ? O14 C48 O13 125.1(5) . . ? O14 C48 C45 119.0(5) . . ? O13 C48 C45 115.9(5) . . ? N14 C49 C50 122.9(6) . . ? N14 C49 H49 118.5 . . ? C50 C49 H49 118.5 . . ? C51 C50 C49 119.0(6) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C52 C51 C50 118.4(5) . . ? C52 C51 C54 121.6(5) . . ? C50 C51 C54 120.0(5) . . ? C51 C52 C53 119.8(6) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? N14 C53 C52 123.0(6) . . ? N14 C53 H53 118.5 . . ? C52 C53 H53 118.5 . . ? O15 C54 O16 124.4(5) . . ? O15 C54 C51 118.0(5) . . ? O16 C54 C51 117.6(5) . . ? O17 C55 O18 119.4(5) . . ? O17 C55 C56 119.4(5) . . ? O18 C55 C56 121.2(5) . . ? O17 C55 Gd3 59.2(3) . . ? O18 C55 Gd3 60.2(3) . . ? C56 C55 Gd3 178.5(4) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O20 C57 O19 120.5(5) . . ? O20 C57 C58 121.1(6) . . ? O19 C57 C58 118.4(6) . . ? O20 C57 Gd3 59.9(3) . . ? O19 C57 Gd3 60.9(3) . . ? C58 C57 Gd3 174.5(6) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N1 Cu1 N7 132.7(3) 2_657 . ? N1 Cu1 Cu4 103.8(2) 2_657 . ? N7 Cu1 Cu4 122.46(17) . . ? N2 Cu2 C1 119.3(3) . . ? N2 Cu2 N8 121.3(2) . . ? C1 Cu2 N8 107.1(2) . . ? N2 Cu2 C1 113.7(3) . 2_557 ? C1 Cu2 C1 96.5(3) . 2_557 ? N8 Cu2 C1 93.1(2) . 2_557 ? N2 Cu2 Cu2 130.95(19) . 2_557 ? C1 Cu2 Cu2 55.9(2) . 2_557 ? N8 Cu2 Cu2 103.80(17) . 2_557 ? C1 Cu2 Cu2 40.60(18) 2_557 2_557 ? C2 Cu3 N3 136.7(3) 2_557 . ? C2 Cu3 N9 109.8(3) 2_557 . ? N3 Cu3 N9 111.6(2) . . ? C2 Cu3 Cu3 75.0(2) 2_557 2_657 ? N3 Cu3 Cu3 111.07(19) . 2_657 ? N9 Cu3 Cu3 97.70(18) . 2_657 ? N4 Cu4 C3 141.1(3) . . ? N4 Cu4 N10 116.0(3) . . ? C3 Cu4 N10 101.7(2) . . ? N4 Cu4 Cu1 84.1(2) . . ? C3 Cu4 Cu1 57.0(2) . . ? N10 Cu4 Cu1 153.48(17) . . ? N5 Cu5 C4 147.9(3) 2_766 . ? N5 Cu5 N11 111.4(2) 2_766 2_666 ? C4 Cu5 N11 100.4(2) . 2_666 ? N5 Cu5 Cu5 80.4(2) 2_766 2_767 ? C4 Cu5 Cu5 103.3(2) . 2_767 ? N11 Cu5 Cu5 92.17(19) 2_666 2_767 ? N6 Cu6 C5 153.1(3) . . ? N6 Cu6 N12 107.5(2) . . ? C5 Cu6 N12 98.3(2) . . ? N14 Cu7 N13 144.7(2) 1_554 . ? N14 Cu7 C6 107.0(2) 1_554 . ? N13 Cu7 C6 106.9(2) . . ? O5 Gd1 O14 146.22(13) . . ? O5 Gd1 O3 81.16(14) . . ? O14 Gd1 O3 101.74(14) . . ? O5 Gd1 O7 72.58(13) . 2_657 ? O14 Gd1 O7 141.19(14) . 2_657 ? O3 Gd1 O7 80.71(13) . 2_657 ? O5 Gd1 O8 82.11(14) . 1_554 ? O14 Gd1 O8 77.55(13) . 1_554 ? O3 Gd1 O8 146.75(14) . 1_554 ? O7 Gd1 O8 120.84(13) 2_657 1_554 ? O5 Gd1 O6 121.07(13) . 2_656 ? O14 Gd1 O6 78.89(14) . 2_656 ? O3 Gd1 O6 138.53(14) . 2_656 ? O7 Gd1 O6 74.81(13) 2_657 2_656 ? O8 Gd1 O6 74.49(14) 1_554 2_656 ? O5 Gd1 O21W 140.45(14) . . ? O14 Gd1 O21W 69.64(13) . . ? O3 Gd1 O21W 72.34(14) . . ? O7 Gd1 O21W 74.55(13) 2_657 . ? O8 Gd1 O21W 134.59(14) 1_554 . ? O6 Gd1 O21W 69.17(13) 2_656 . ? O5 Gd1 O18 77.36(12) . . ? O14 Gd1 O18 71.97(13) . . ? O3 Gd1 O18 71.49(13) . . ? O7 Gd1 O18 141.63(13) 2_657 . ? O8 Gd1 O18 76.91(13) 1_554 . ? O6 Gd1 O18 142.73(13) 2_656 . ? O21W Gd1 O18 119.12(12) . . ? O5 Gd1 H21A 141.1 . . ? O14 Gd1 H21A 72.6 . . ? O3 Gd1 H21A 89.3 . . ? O7 Gd1 H21A 68.7 2_657 . ? O8 Gd1 H21A 121.1 1_554 . ? O6 Gd1 H21A 50.8 2_656 . ? O21W Gd1 H21A 18.7 . . ? O18 Gd1 H21A 134.7 . . ? O1 Gd2 O12 74.42(14) 2_666 . ? O1 Gd2 O15 138.15(15) 2_666 . ? O12 Gd2 O15 147.40(14) . . ? O1 Gd2 O11 72.17(14) 2_666 2_666 ? O12 Gd2 O11 120.62(14) . 2_666 ? O15 Gd2 O11 80.42(14) . 2_666 ? O1 Gd2 O10 81.47(14) 2_666 . ? O12 Gd2 O10 75.29(14) . . ? O15 Gd2 O10 103.81(14) . . ? O11 Gd2 O10 142.38(14) 2_666 . ? O1 Gd2 O2 116.49(14) 2_666 . ? O12 Gd2 O2 82.56(14) . . ? O15 Gd2 O2 81.85(14) . . ? O11 Gd2 O2 70.87(14) 2_666 . ? O10 Gd2 O2 146.53(14) . . ? O1 Gd2 O22W 74.68(15) 2_666 . ? O12 Gd2 O22W 137.18(14) . . ? O15 Gd2 O22W 68.27(14) . . ? O11 Gd2 O22W 75.93(14) 2_666 . ? O10 Gd2 O22W 71.44(14) . . ? O2 Gd2 O22W 138.35(14) . . ? O1 Gd2 O17 147.21(14) 2_666 . ? O12 Gd2 O17 78.77(13) . . ? O15 Gd2 O17 70.02(13) . . ? O11 Gd2 O17 139.34(13) 2_666 . ? O10 Gd2 O17 73.67(13) . . ? O2 Gd2 O17 77.67(13) . . ? O22W Gd2 O17 115.61(13) . . ? O9 Gd3 O4 157.57(13) . . ? O9 Gd3 O16 105.69(14) . . ? O4 Gd3 O16 79.55(14) . . ? O9 Gd3 O13 77.52(14) . . ? O4 Gd3 O13 107.21(14) . . ? O16 Gd3 O13 154.84(14) . . ? O9 Gd3 O20 83.78(14) . . ? O4 Gd3 O20 76.37(14) . . ? O16 Gd3 O20 128.73(14) . . ? O13 Gd3 O20 76.21(14) . . ? O9 Gd3 O19 78.10(14) . . ? O4 Gd3 O19 81.64(14) . . ? O16 Gd3 O19 79.10(14) . . ? O13 Gd3 O19 125.44(14) . . ? O20 Gd3 O19 53.17(14) . . ? O9 Gd3 O17 78.98(13) . . ? O4 Gd3 O17 123.24(13) . . ? O16 Gd3 O17 75.89(13) . . ? O13 Gd3 O17 80.41(14) . . ? O20 Gd3 O17 153.43(14) . . ? O19 Gd3 O17 139.76(13) . . ? O9 Gd3 O18 125.87(13) . . ? O4 Gd3 O18 75.79(12) . . ? O16 Gd3 O18 85.56(14) . . ? O13 Gd3 O18 73.19(13) . . ? O20 Gd3 O18 129.64(13) . . ? O19 Gd3 O18 154.66(13) . . ? O17 Gd3 O18 52.15(12) . . ? O9 Gd3 C57 81.64(17) . . ? O4 Gd3 C57 75.93(17) . . ? O16 Gd3 C57 103.78(18) . . ? O13 Gd3 C57 101.38(18) . . ? O20 Gd3 C57 26.36(16) . . ? O19 Gd3 C57 26.92(16) . . ? O17 Gd3 C57 159.66(16) . . ? O18 Gd3 C57 147.96(15) . . ? O9 Gd3 C55 102.46(15) . . ? O4 Gd3 C55 99.92(15) . . ? O16 Gd3 C55 79.95(16) . . ? O13 Gd3 C55 75.04(16) . . ? O20 Gd3 C55 148.38(16) . . ? O19 Gd3 C55 158.33(16) . . ? O17 Gd3 C55 25.96(14) . . ? O18 Gd3 C55 26.20(13) . . ? C57 Gd3 C55 173.63(17) . . ? C1 N1 Cu1 165.4(6) . 2_657 ? C2 N2 Cu2 169.5(6) . . ? C3 N3 Cu3 176.9(6) . . ? C4 N4 Cu4 176.8(7) . . ? C5 N5 Cu5 176.5(6) . 2_766 ? C6 N6 Cu6 171.9(6) . . ? C11 N7 C7 116.5(5) . . ? C11 N7 Cu1 122.8(4) . . ? C7 N7 Cu1 120.5(4) . . ? C13 N8 C17 115.9(6) . . ? C13 N8 Cu2 120.0(5) . . ? C17 N8 Cu2 124.0(4) . . ? C19 N9 C23 116.8(6) . . ? C19 N9 Cu3 121.9(5) . . ? C23 N9 Cu3 120.7(4) . . ? C29 N10 C25 116.1(5) . . ? C29 N10 Cu4 121.9(4) . . ? C25 N10 Cu4 120.7(4) . . ? C31 N11 C35 115.8(6) . . ? C31 N11 Cu5 122.6(4) . 2_666 ? C35 N11 Cu5 121.6(5) . 2_666 ? C37 N12 C41 116.5(6) . . ? C37 N12 Cu6 116.4(4) . . ? C41 N12 Cu6 126.6(5) . . ? C47 N13 C43 116.2(6) . . ? C47 N13 Cu7 129.0(5) . . ? C43 N13 Cu7 114.5(5) . . ? C53 N14 C49 116.8(5) . . ? C53 N14 Cu7 126.2(5) . 1_556 ? C49 N14 Cu7 116.8(4) . 1_556 ? C12 O1 Gd2 138.9(4) . 2_666 ? C12 O2 Gd2 133.9(4) . . ? C18 O3 Gd1 132.8(4) . . ? C18 O4 Gd3 133.6(3) . . ? C24 O5 Gd1 172.3(4) . . ? C24 O6 Gd1 118.9(4) . 2_656 ? C30 O7 Gd1 132.6(4) . 2_657 ? C30 O8 Gd1 138.3(4) . 1_556 ? C36 O9 Gd3 130.8(3) . . ? C36 O10 Gd2 129.4(4) . . ? C42 O11 Gd2 128.6(4) . 2_666 ? C42 O12 Gd2 162.3(4) . . ? C48 O13 Gd3 126.1(3) . . ? C48 O14 Gd1 140.8(4) . . ? C54 O15 Gd2 143.5(4) . . ? C54 O16 Gd3 125.5(4) . . ? C55 O17 Gd2 142.7(3) . . ? C55 O17 Gd3 94.9(3) . . ? Gd2 O17 Gd3 120.96(15) . . ? C55 O18 Gd1 140.1(3) . . ? C55 O18 Gd3 93.6(3) . . ? Gd1 O18 Gd3 121.97(14) . . ? C57 O19 Gd3 92.1(3) . . ? C57 O20 Gd3 93.7(3) . . ? Gd1 O21W H21A 86.8 . . ? Gd1 O21W H21B 128.3 . . ? H21A O21W H21B 110.1 . . ? Gd2 O22W H22A 113.4 . . ? Gd2 O22W H22B 118.6 . . ? H22A O22W H22B 111.6 . . ? H23A O23W H23B 112.4 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.241 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 964393' ####################################################################### # # 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_I-D #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H42 Cu7 N14 O22 Tb3, H2 O' _chemical_formula_sum 'C58 H44 Cu7 N14 O23 Tb3' _chemical_formula_weight 2226.72 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8612(4) _cell_length_b 17.3255(5) _cell_length_c 17.9096(5) _cell_angle_alpha 74.402(2) _cell_angle_beta 88.414(2) _cell_angle_gamma 86.095(2) _cell_volume 3536.50(19) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 13000 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 25.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 5.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.306 _exptl_absorpt_correction_T_max 0.361 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25858 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.40 _reflns_number_total 13000 _reflns_number_gt 10992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0206P)^2^+6.5493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00033(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13000 _refine_ls_number_parameters 943 _refine_ls_number_restraints 317 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.004 _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 0.4822(5) 0.5967(3) 0.4844(3) 0.0403(11) Uani 1 1 d U . . C2 C 0.8373(5) 0.5463(3) 0.5019(3) 0.0438(13) Uani 1 1 d U . . C3 C 0.1459(5) 0.6881(3) 0.5082(3) 0.0371(9) Uani 1 1 d U . . C4 C 0.4472(4) 0.8476(3) 0.5154(3) 0.0314(10) Uani 1 1 d U . . C5 C 0.7658(4) 1.0056(3) 0.4888(3) 0.0265(9) Uani 1 1 d U . . C6 C 0.0700(5) 0.1650(3) 0.5162(3) 0.0328(10) Uani 1 1 d U . . C7 C -0.2745(4) 0.2201(3) 0.7374(3) 0.0352(11) Uani 1 1 d U . . H7 H -0.3509 0.2367 0.7346 0.042 Uiso 1 1 calc R . . C8 C -0.2276(4) 0.1873(3) 0.8094(3) 0.0345(11) Uani 1 1 d U . . H8 H -0.2720 0.1814 0.8539 0.041 Uiso 1 1 calc R . . C9 C -0.1147(4) 0.1632(3) 0.8148(2) 0.0244(8) Uani 1 1 d U . . C10 C -0.0525(5) 0.1744(4) 0.7470(3) 0.0477(15) Uani 1 1 d U . . H10 H 0.0248 0.1609 0.7485 0.057 Uiso 1 1 calc R . . C11 C -0.1061(5) 0.2059(4) 0.6769(3) 0.0537(17) Uani 1 1 d U . . H11 H -0.0639 0.2109 0.6315 0.064 Uiso 1 1 calc R . . C12 C -0.0624(4) 0.1203(2) 0.8919(2) 0.0212(7) Uani 1 1 d U . . C17 C 0.5765(3) 0.4223(2) 0.7138(2) 0.0407(12) Uani 1 1 d GU . . H17 H 0.6397 0.3932 0.7013 0.049 Uiso 1 1 calc R . . C16 C 0.5301(3) 0.40043(18) 0.78803(16) 0.0346(10) Uani 1 1 d GU . . H16 H 0.5628 0.3572 0.8254 0.042 Uiso 1 1 calc R . . C15 C 0.4349(3) 0.44327(19) 0.80645(14) 0.0246(8) Uani 1 1 d GU . . C14 C 0.3861(3) 0.5079(2) 0.75061(19) 0.0532(17) Uani 1 1 d GU . . H14 H 0.3224 0.5366 0.7629 0.064 Uiso 1 1 calc R . . C13 C 0.4325(4) 0.5298(2) 0.67634(18) 0.067(2) Uani 1 1 d GU . . H13 H 0.3994 0.5726 0.6387 0.080 Uiso 1 1 calc R . . C18 C 0.3822(4) 0.4191(3) 0.8871(2) 0.0216(7) Uani 1 1 d U . . C19 C 0.0902(5) 0.4256(5) 0.6932(3) 0.068(2) Uani 1 1 d U . . H19 H 0.1623 0.4257 0.6714 0.081 Uiso 1 1 calc R . . C20 C 0.0777(5) 0.4358(4) 0.7678(3) 0.0562(18) Uani 1 1 d U . . H20 H 0.1407 0.4398 0.7960 0.067 Uiso 1 1 calc R . . C21 C -0.0294(4) 0.4397(3) 0.7990(3) 0.0267(9) Uani 1 1 d U . . C22 C -0.1183(5) 0.4302(3) 0.7561(3) 0.0389(12) Uani 1 1 d U . . H22 H -0.1916 0.4322 0.7756 0.047 Uiso 1 1 calc R . . C23 C -0.0988(5) 0.4177(4) 0.6839(3) 0.0448(14) Uani 1 1 d U . . H23 H -0.1603 0.4103 0.6560 0.054 Uiso 1 1 calc R . . C24 C -0.0476(4) 0.4583(3) 0.8765(2) 0.0218(8) Uani 1 1 d U . . C25 C 0.2489(5) 0.7086(3) 0.7216(3) 0.0374(11) Uani 1 1 d U . . H25 H 0.3249 0.7176 0.7117 0.045 Uiso 1 1 calc R . . C26 C 0.2151(4) 0.6741(3) 0.7968(3) 0.0322(10) Uani 1 1 d U . . H26 H 0.2682 0.6586 0.8362 0.039 Uiso 1 1 calc R . . C27 C 0.1024(4) 0.6626(3) 0.8132(2) 0.0234(8) Uani 1 1 d U . . C28 C 0.0277(5) 0.6873(4) 0.7532(3) 0.0485(15) Uani 1 1 d U . . H28 H -0.0494 0.6826 0.7623 0.058 Uiso 1 1 calc R . . C29 C 0.0686(5) 0.7192(4) 0.6790(3) 0.0568(17) Uani 1 1 d U . . H29 H 0.0172 0.7342 0.6386 0.068 Uiso 1 1 calc R . . C30 C 0.0622(4) 0.6202(2) 0.8933(2) 0.0211(7) Uani 1 1 d U . . C31 C 0.5288(6) 0.0343(4) 1.3066(3) 0.063(2) Uani 1 1 d U . . H31 H 0.5891 0.0580 1.3218 0.076 Uiso 1 1 calc R . . C32 C 0.4943(5) 0.0620(4) 1.2298(3) 0.0510(16) Uani 1 1 d U . . H32 H 0.5314 0.1024 1.1949 0.061 Uiso 1 1 calc R . . C33 C 0.4047(4) 0.0285(3) 1.2067(2) 0.0249(9) Uani 1 1 d U . . C34 C 0.3516(5) -0.0282(3) 1.2616(3) 0.0533(17) Uani 1 1 d U . . H34 H 0.2877 -0.0500 1.2488 0.064 Uiso 1 1 calc R . . C35 C 0.3928(6) -0.0534(4) 1.3363(3) 0.062(2) Uani 1 1 d U . . H35 H 0.3565 -0.0933 1.3723 0.074 Uiso 1 1 calc R . . C36 C 0.3608(4) 0.0558(2) 1.1246(2) 0.0220(7) Uani 1 1 d U . . C37 C 0.1650(5) -0.0837(3) 0.6909(3) 0.0413(12) Uani 1 1 d U . . H37 H 0.2337 -0.0957 0.6690 0.050 Uiso 1 1 calc R . . C38 C 0.1639(4) -0.0789(3) 0.7665(3) 0.0337(11) Uani 1 1 d U . . H38 H 0.2310 -0.0850 0.7938 0.040 Uiso 1 1 calc R . . C39 C 0.0621(4) -0.0648(3) 0.8013(3) 0.0243(8) Uani 1 1 d U . . C40 C -0.0350(5) -0.0576(4) 0.7589(3) 0.0418(13) Uani 1 1 d U . . H40 H -0.1055 -0.0507 0.7811 0.050 Uiso 1 1 calc R . . C41 C -0.0254(5) -0.0610(4) 0.6824(3) 0.0518(16) Uani 1 1 d U . . H41 H -0.0913 -0.0552 0.6539 0.062 Uiso 1 1 calc R . . C42 C 0.0599(4) -0.0493(2) 0.8804(2) 0.0231(8) Uani 1 1 d U . . C43 C 0.2570(7) 0.1984(4) 1.3621(3) 0.063(2) Uani 1 1 d U . . H43 H 0.2496 0.1465 1.3930 0.075 Uiso 1 1 calc R . . C44 C 0.2756(6) 0.2088(3) 1.2840(3) 0.0497(16) Uani 1 1 d U . . H44 H 0.2808 0.1648 1.2633 0.060 Uiso 1 1 calc R . . C45 C 0.2863(4) 0.2855(3) 1.2366(2) 0.0246(9) Uani 1 1 d U . . C46 C 0.2767(5) 0.3474(3) 1.2705(3) 0.0453(14) Uani 1 1 d U . . H46 H 0.2814 0.4001 1.2405 0.054 Uiso 1 1 calc R . . C47 C 0.2597(6) 0.3312(4) 1.3499(3) 0.0547(17) Uani 1 1 d U . . H47 H 0.2557 0.3740 1.3722 0.066 Uiso 1 1 calc R . . C48 C 0.3022(4) 0.2983(3) 1.1508(2) 0.0217(8) Uani 1 1 d U . . C49 C 0.2411(5) 0.1423(3) 0.6640(3) 0.0400(13) Uani 1 1 d U . . H49 H 0.2083 0.1029 0.6470 0.048 Uiso 1 1 calc R . . C50 C 0.2633(5) 0.1271(3) 0.7422(3) 0.0353(12) Uani 1 1 d U . . H50 H 0.2470 0.0784 0.7766 0.042 Uiso 1 1 calc R . . C51 C 0.3101(4) 0.1858(3) 0.7678(2) 0.0250(9) Uani 1 1 d U . . C52 C 0.3364(5) 0.2558(3) 0.7141(3) 0.0451(15) Uani 1 1 d U . . H52 H 0.3694 0.2961 0.7297 0.054 Uiso 1 1 calc R . . C53 C 0.3133(6) 0.2655(4) 0.6370(3) 0.0509(17) Uani 1 1 d U . . H53 H 0.3329 0.3125 0.6012 0.061 Uiso 1 1 calc R . . C54 C 0.3283(4) 0.1736(3) 0.8536(2) 0.0227(8) Uani 1 1 d U . . C55 C 0.1449(4) 0.2502(2) 0.9933(2) 0.0196(7) Uani 1 1 d U . . C56 C 0.0196(4) 0.2575(3) 0.9884(4) 0.0567(18) Uani 1 1 d U . . H56A H -0.0031 0.2456 0.9419 0.085 Uiso 1 1 calc R . . H56B H -0.0073 0.3113 0.9876 0.085 Uiso 1 1 calc R . . H56C H -0.0119 0.2204 1.0326 0.085 Uiso 1 1 calc R . . C57 C 0.6226(4) 0.2328(3) 1.0175(3) 0.0295(9) Uani 1 1 d U . . C58 C 0.7459(5) 0.2409(4) 1.0199(5) 0.072(2) Uani 1 1 d U . . H58A H 0.7617 0.2963 0.9994 0.108 Uiso 1 1 calc R . . H58B H 0.7846 0.2095 0.9892 0.108 Uiso 1 1 calc R . . H58C H 0.7712 0.2222 1.0725 0.108 Uiso 1 1 calc R . . Cu1 Cu 0.28736(6) 0.71619(5) 0.42861(4) 0.04673(18) Uani 1 1 d U . . Cu2 Cu 0.58960(7) 0.51858(4) 0.54512(4) 0.04781(18) Uani 1 1 d U . . Cu3 Cu 0.97510(7) 0.58596(5) 0.46422(4) 0.04976(19) Uani 1 1 d U . . Cu4 Cu 0.23660(6) 0.75314(4) 0.55186(3) 0.03896(16) Uani 1 1 d U . . Cu5 Cu 0.54913(6) 0.92827(4) 0.47336(4) 0.04370(18) Uani 1 1 d U . . Cu6 Cu -0.10083(6) 0.06172(4) 0.47543(4) 0.04441(18) Uani 1 1 d U . . Cu7 Cu 0.20937(7) 0.22585(5) 0.50615(3) 0.0512(2) Uani 1 1 d U . . N1 N 0.4178(4) 0.6455(3) 0.4555(3) 0.0564(13) Uani 1 1 d U . . N2 N 0.7466(4) 0.5294(3) 0.5224(3) 0.0456(10) Uani 1 1 d U . . N3 N 0.0819(4) 0.6472(3) 0.4941(2) 0.0440(10) Uani 1 1 d U . . N4 N 0.3702(4) 0.8108(3) 0.5303(3) 0.0558(13) Uani 1 1 d U . . N5 N 0.6843(4) 0.9760(3) 0.4852(3) 0.0480(12) Uani 1 1 d U . . N6 N 0.0034(5) 0.1245(3) 0.5063(3) 0.0565(14) Uani 1 1 d U . . N7 N -0.2152(4) 0.2293(3) 0.6714(2) 0.0397(10) Uani 1 1 d U . . N8 N 0.5289(4) 0.4870(3) 0.6585(2) 0.0419(10) Uani 1 1 d GU . . N9 N 0.0037(4) 0.4158(3) 0.6521(2) 0.0461(12) Uani 1 1 d U . . N10 N 0.1770(4) 0.7295(3) 0.6625(2) 0.0382(9) Uani 1 1 d U . . N11 N 0.4814(4) -0.0233(3) 1.3590(2) 0.0439(11) Uani 1 1 d U . . N12 N 0.0725(4) -0.0719(3) 0.6475(2) 0.0414(10) Uani 1 1 d U . . N13 N 0.2490(4) 0.2577(3) 1.3960(2) 0.0463(12) Uani 1 1 d U . . N14 N 0.2641(4) 0.2107(3) 0.6113(2) 0.0391(10) Uani 1 1 d U . . O1 O -0.1308(3) 0.08505(18) 0.94220(17) 0.0315(7) Uani 1 1 d U . . O2 O 0.0416(3) 0.12159(19) 0.89961(17) 0.0314(6) Uani 1 1 d U . . O3 O 0.2921(3) 0.45690(18) 0.89770(17) 0.0281(5) Uani 1 1 d U . . O4 O 0.4320(3) 0.36312(17) 0.93736(17) 0.0251(5) Uani 1 1 d U . . O5 O 0.0374(3) 0.45269(18) 0.91853(16) 0.0259(6) Uani 1 1 d U . . O6 O -0.1462(3) 0.48143(19) 0.89176(17) 0.0292(7) Uani 1 1 d U . . O7 O 0.1366(3) 0.58482(17) 0.94121(17) 0.0258(5) Uani 1 1 d U . . O8 O -0.0427(3) 0.62253(18) 0.90534(17) 0.0278(7) Uani 1 1 d U . . O9 O 0.4211(3) 0.10126(17) 1.07371(17) 0.0268(5) Uani 1 1 d U . . O10 O 0.2686(3) 0.03190(19) 1.11268(17) 0.0302(6) Uani 1 1 d U . . O11 O 0.1493(3) -0.02496(19) 0.89889(17) 0.0312(6) Uani 1 1 d U . . O12 O -0.0292(3) -0.0592(2) 0.91982(18) 0.0335(7) Uani 1 1 d U . . O13 O 0.3258(3) 0.23691(19) 1.12767(16) 0.0307(5) Uani 1 1 d U . . O14 O 0.2916(3) 0.36849(18) 1.10804(17) 0.0280(6) Uani 1 1 d U . . O15 O 0.3049(3) 0.10724(18) 0.89851(16) 0.0272(5) Uani 1 1 d U . . O16 O 0.3653(3) 0.23040(19) 0.87454(16) 0.0305(5) Uani 1 1 d U . . O17 O 0.1982(3) 0.18216(17) 1.00265(18) 0.0249(4) Uani 1 1 d U . . O18 O 0.2007(3) 0.31204(17) 0.98678(17) 0.0244(4) Uani 1 1 d U . . O19 O 0.5832(3) 0.20552(19) 0.96619(19) 0.0310(5) Uani 1 1 d U . . O20 O 0.5571(3) 0.2539(2) 1.06659(18) 0.0319(5) Uani 1 1 d U . . O21W O 0.3454(3) 0.51916(18) 1.02345(19) 0.0303(6) Uani 1 1 d U . . H21B H 0.3810 0.5466 0.9875 0.036 Uiso 1 1 d R . . H21A H 0.3208 0.5455 1.0528 0.036 Uiso 1 1 d R . . O22W O 0.3532(3) -0.03933(19) 0.99594(19) 0.0338(7) Uani 1 1 d U . . H22A H 0.3551 -0.0886 1.0122 0.041 Uiso 1 1 d R . . H22B H 0.4042 -0.0263 0.9640 0.041 Uiso 1 1 d R . . O23W O 0.4624(3) 0.5975(2) 0.8992(2) 0.0439(9) Uani 1 1 d . . . H23B H 0.5288 0.5822 0.9039 0.053 Uiso 1 1 d R . . H23A H 0.4519 0.6456 0.8942 0.053 Uiso 1 1 d R . . Tb1 Tb 0.176492(17) 0.449532(12) 1.008312(11) 0.01608(6) Uani 1 1 d U . . Tb2 Tb 0.175630(18) 0.044282(12) 0.993614(11) 0.01744(6) Uani 1 1 d U . . Tb3 Tb 0.388033(17) 0.233785(12) 1.003136(11) 0.01611(6) Uani 1 1 d U . . 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 0.047(2) 0.032(3) 0.0367(18) -0.0036(18) 0.022(2) 0.0023(17) C2 0.0496(19) 0.056(3) 0.034(3) -0.023(3) 0.009(2) -0.020(2) C3 0.044(2) 0.039(3) 0.028(2) -0.009(2) -0.0022(16) -0.0042(16) C4 0.033(2) 0.031(2) 0.027(2) -0.0009(19) -0.005(2) -0.0056(16) C5 0.027(2) 0.033(3) 0.020(2) -0.009(2) 0.002(2) -0.0042(18) C6 0.036(2) 0.043(3) 0.024(2) -0.018(2) -0.0058(17) -0.0001(17) C7 0.026(2) 0.047(3) 0.0252(17) 0.000(2) -0.0042(11) 0.008(2) C8 0.0282(18) 0.046(3) 0.0219(15) 0.001(2) -0.0019(13) 0.007(2) C9 0.0249(16) 0.024(2) 0.0206(12) 0.0000(15) -0.0041(10) -0.0015(17) C10 0.032(2) 0.072(4) 0.0238(14) 0.008(2) 0.0009(13) 0.017(3) C11 0.040(2) 0.087(4) 0.0208(13) 0.003(3) 0.0018(17) 0.024(3) C12 0.0273(12) 0.015(2) 0.0207(14) -0.0035(14) -0.0045(11) 0.0010(14) C17 0.032(3) 0.056(3) 0.0297(15) -0.0085(16) 0.0142(17) 0.007(2) C16 0.026(3) 0.049(3) 0.0272(15) -0.0102(15) 0.0093(16) 0.0045(18) C15 0.028(2) 0.024(2) 0.0213(13) -0.0057(12) 0.0110(13) -0.0037(15) C14 0.066(4) 0.045(3) 0.032(2) 0.0105(18) 0.024(2) 0.021(2) C13 0.082(5) 0.063(4) 0.032(2) 0.015(2) 0.028(2) 0.033(3) C18 0.024(2) 0.0211(13) 0.0201(13) -0.0058(10) 0.0093(11) -0.0070(13) C19 0.030(2) 0.145(6) 0.048(3) -0.062(4) 0.005(2) -0.003(4) C20 0.0256(18) 0.117(5) 0.044(3) -0.052(4) 0.0001(19) 0.000(3) C21 0.0259(17) 0.035(2) 0.0229(18) -0.0144(19) -0.0021(12) 0.002(2) C22 0.0269(19) 0.072(4) 0.025(2) -0.024(3) 0.0000(15) -0.005(3) C23 0.0341(19) 0.082(4) 0.028(2) -0.030(3) 0.0002(18) -0.009(3) C24 0.0236(13) 0.024(2) 0.0177(17) -0.0054(17) -0.0024(11) -0.0003(18) C25 0.0297(18) 0.057(3) 0.0241(9) -0.006(2) 0.0068(12) -0.014(2) C26 0.0238(16) 0.048(3) 0.0231(12) -0.0048(19) 0.0031(13) -0.009(2) C27 0.0211(15) 0.025(2) 0.0217(13) -0.0037(15) 0.0043(10) 0.0016(17) C28 0.0243(18) 0.084(4) 0.0252(15) 0.006(2) 0.0008(11) -0.004(3) C29 0.0330(17) 0.101(5) 0.0236(13) 0.006(3) 0.0007(10) -0.009(3) C30 0.0250(13) 0.0136(15) 0.0232(13) -0.0029(12) 0.0040(10) -0.0016(14) C31 0.060(4) 0.087(5) 0.033(2) 0.014(3) -0.024(3) -0.047(3) C32 0.044(4) 0.073(4) 0.028(2) 0.011(2) -0.014(2) -0.034(3) C33 0.024(2) 0.029(2) 0.0206(12) -0.0040(14) -0.0048(13) -0.0023(16) C34 0.063(4) 0.060(4) 0.0294(19) 0.012(2) -0.021(2) -0.040(3) C35 0.065(4) 0.084(5) 0.0266(19) 0.014(2) -0.017(3) -0.047(3) C36 0.029(2) 0.0172(14) 0.0202(13) -0.0053(11) -0.0055(11) 0.0010(15) C37 0.0365(19) 0.064(4) 0.030(2) -0.024(3) 0.0049(16) -0.004(3) C38 0.0276(18) 0.051(3) 0.0279(19) -0.020(2) 0.0003(15) 0.000(2) C39 0.0267(17) 0.025(2) 0.0244(16) -0.0109(17) 0.0016(11) -0.0052(19) C40 0.0260(18) 0.074(4) 0.030(2) -0.021(3) 0.0016(14) -0.007(3) C41 0.0343(19) 0.098(5) 0.030(2) -0.027(3) -0.0001(17) -0.018(3) C42 0.0317(17) 0.016(2) 0.0233(16) -0.0086(16) 0.0023(12) -0.0025(17) C43 0.119(6) 0.044(2) 0.0182(16) -0.0001(15) 0.012(3) -0.004(4) C44 0.096(5) 0.0307(16) 0.0187(15) -0.0023(12) 0.010(3) 0.001(3) C45 0.029(3) 0.0301(16) 0.0139(10) -0.0052(8) -0.0002(18) 0.003(2) C46 0.078(4) 0.0373(19) 0.0254(16) -0.0149(14) 0.010(3) -0.017(3) C47 0.089(5) 0.059(2) 0.0287(18) -0.0272(18) 0.017(3) -0.036(3) C48 0.017(2) 0.0318(12) 0.0134(10) -0.0034(8) 0.0007(14) 0.0053(15) C49 0.057(4) 0.048(2) 0.0202(12) -0.0139(12) -0.002(2) -0.022(3) C50 0.055(4) 0.035(2) 0.0196(12) -0.0099(13) -0.001(2) -0.016(2) C51 0.029(3) 0.033(2) 0.0146(10) -0.0076(10) 0.0003(18) -0.0095(19) C52 0.071(4) 0.049(3) 0.0165(12) -0.0020(15) -0.005(2) -0.036(3) C53 0.077(5) 0.060(3) 0.0159(13) -0.0007(16) -0.005(2) -0.041(3) C54 0.024(2) 0.0316(16) 0.0135(9) -0.0063(10) 0.0029(14) -0.0082(15) C55 0.0155(7) 0.0229(10) 0.022(2) -0.0089(17) 0.0024(18) -0.0024(9) C56 0.0162(10) 0.035(3) 0.128(6) -0.038(4) -0.001(3) -0.0015(12) C57 0.0164(7) 0.023(2) 0.050(3) -0.010(2) -0.0024(15) -0.0016(19) C58 0.0187(13) 0.089(5) 0.126(6) -0.058(5) -0.001(3) -0.010(3) Cu1 0.0414(4) 0.0661(5) 0.0236(3) 0.0012(3) -0.0057(3) 0.0087(3) Cu2 0.0477(4) 0.0541(4) 0.0342(4) -0.0018(3) 0.0179(3) 0.0011(3) Cu3 0.0516(5) 0.0725(5) 0.0347(4) -0.0262(4) 0.0094(3) -0.0264(4) Cu4 0.0468(4) 0.0472(4) 0.0228(3) -0.0056(3) 0.0082(3) -0.0213(3) Cu5 0.0404(4) 0.0565(4) 0.0317(3) -0.0026(3) -0.0051(3) -0.0212(3) Cu6 0.0395(4) 0.0635(5) 0.0340(4) -0.0154(3) -0.0012(3) -0.0197(3) Cu7 0.0606(5) 0.0827(5) 0.0141(3) -0.0134(3) 0.0020(3) -0.0309(4) N1 0.043(2) 0.064(3) 0.064(3) -0.023(2) -0.008(2) 0.0086(18) N2 0.0455(11) 0.054(3) 0.035(2) -0.009(2) 0.0110(16) -0.0075(17) N3 0.052(3) 0.053(3) 0.033(2) -0.020(2) -0.0023(17) -0.0090(18) N4 0.048(3) 0.068(3) 0.050(3) -0.010(2) 0.0160(19) -0.028(2) N5 0.037(2) 0.058(3) 0.045(3) -0.004(2) -0.002(2) -0.0184(19) N6 0.052(3) 0.081(4) 0.045(3) -0.026(3) -0.005(2) -0.023(2) N7 0.035(2) 0.055(3) 0.0215(15) -0.0007(19) -0.0047(15) 0.010(2) N8 0.046(2) 0.046(2) 0.0308(12) -0.0086(13) 0.0130(14) 0.0017(17) N9 0.039(2) 0.080(3) 0.030(2) -0.034(2) 0.0067(15) -0.012(3) N10 0.0361(18) 0.055(3) 0.0216(9) -0.0065(16) 0.0049(9) -0.011(2) N11 0.040(3) 0.064(3) 0.0219(18) 0.0032(17) -0.0108(17) -0.021(2) N12 0.042(2) 0.064(3) 0.0254(19) -0.022(2) 0.0036(13) -0.016(2) N13 0.062(3) 0.065(2) 0.0154(17) -0.0130(13) -0.003(2) -0.017(3) N14 0.046(3) 0.060(2) 0.0146(12) -0.0109(11) 0.0024(16) -0.024(2) O1 0.0405(17) 0.0260(17) 0.0236(14) 0.0039(12) -0.0045(13) -0.0115(14) O2 0.0286(10) 0.0366(16) 0.0246(15) -0.0007(12) -0.0088(9) 0.0006(10) O3 0.0325(12) 0.0295(13) 0.0192(10) -0.0029(9) 0.0136(9) -0.0010(9) O4 0.0271(12) 0.0248(8) 0.0228(11) -0.0042(7) 0.0031(10) -0.0085(7) O5 0.0291(11) 0.0275(12) 0.0205(13) -0.0058(12) -0.0075(9) 0.0015(10) O6 0.0255(12) 0.0413(19) 0.0248(16) -0.0164(15) 0.0005(12) 0.0009(14) O7 0.0294(14) 0.0202(7) 0.0243(13) -0.0006(9) 0.0027(11) -0.0003(9) O8 0.0256(11) 0.0293(17) 0.0245(16) -0.0009(13) 0.0076(11) -0.0022(13) O9 0.0295(12) 0.0238(8) 0.0238(11) -0.0017(7) -0.0007(10) 0.0032(7) O10 0.0331(15) 0.0381(15) 0.0181(9) -0.0031(9) -0.0077(8) -0.0068(11) O11 0.0380(14) 0.0380(14) 0.0232(14) -0.0163(13) 0.0054(11) -0.0109(11) O12 0.0325(15) 0.043(2) 0.0250(15) -0.0098(15) 0.0051(12) -0.0028(15) O13 0.0397(14) 0.0366(11) 0.0140(8) -0.0064(8) 0.0051(8) 0.0057(12) O14 0.0277(17) 0.0328(10) 0.0192(10) 0.0010(8) -0.0057(10) -0.0020(11) O15 0.0286(12) 0.0316(11) 0.0194(10) -0.0030(8) 0.0059(9) -0.0059(10) O16 0.0407(15) 0.0402(13) 0.0139(7) -0.0095(9) 0.0021(8) -0.0166(12) O17 0.0177(7) 0.0213(7) 0.0361(13) -0.0083(9) 0.0040(8) -0.0035(7) O18 0.0185(7) 0.0208(6) 0.0336(13) -0.0065(9) -0.0037(9) -0.0016(6) O19 0.0193(7) 0.0358(14) 0.0412(16) -0.0165(12) 0.0082(8) -0.0024(9) O20 0.0245(9) 0.0416(15) 0.0330(14) -0.0147(11) -0.0106(9) -0.0011(11) O21W 0.0234(13) 0.0286(12) 0.0403(17) -0.0103(11) 0.0002(12) -0.0073(10) O22W 0.0280(14) 0.0270(12) 0.0436(17) -0.0064(11) 0.0022(12) 0.0056(11) O23W 0.030(2) 0.045(2) 0.059(2) -0.0146(19) 0.0004(18) -0.0120(17) Tb1 0.01610(11) 0.01964(11) 0.01152(10) -0.00293(8) 0.00260(8) -0.00052(8) Tb2 0.01976(12) 0.01928(11) 0.01276(10) -0.00293(8) -0.00060(8) -0.00304(8) Tb3 0.01519(11) 0.02051(11) 0.01266(10) -0.00450(8) 0.00048(8) -0.00133(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.124(7) . ? C1 Cu2 1.920(6) . ? C1 Cu2 2.413(6) 2_666 ? C2 N2 1.158(7) . ? C2 Cu3 1.856(6) . ? C3 N3 1.151(6) . ? C3 Cu4 1.930(5) . ? C3 Cu1 2.165(6) . ? C4 N4 1.135(7) . ? C4 Cu5 1.896(5) . ? C5 N5 1.136(6) . ? C5 Cu6 1.889(5) 1_665 ? C6 N6 1.139(7) . ? C6 Cu7 1.999(5) . ? C7 N7 1.337(6) . ? C7 C8 1.377(6) . ? C7 H7 0.9300 . ? C8 C9 1.372(7) . ? C8 H8 0.9300 . ? C9 C10 1.378(7) . ? C9 C12 1.509(6) . ? C10 C11 1.381(7) . ? C10 H10 0.9300 . ? C11 N7 1.327(7) . ? C11 H11 0.9300 . ? C12 O2 1.248(5) . ? C12 O1 1.255(5) . ? C17 C16 1.3900 . ? C17 N8 1.380(5) . ? C17 H17 0.9300 . ? C16 C15 1.3900 . ? C16 H16 0.9300 . ? C15 C14 1.3900 . ? C15 C18 1.521(5) . ? C14 C13 1.3900 . ? C14 H14 0.9300 . ? C13 N8 1.397(5) . ? C13 H13 0.9300 . ? C18 O3 1.253(5) . ? C18 O4 1.257(5) . ? C19 N9 1.325(7) . ? C19 C20 1.396(7) . ? C19 H19 0.9300 . ? C20 C21 1.379(7) . ? C20 H20 0.9300 . ? C21 C22 1.365(6) . ? C21 C24 1.514(6) . ? C22 C23 1.379(6) . ? C22 H22 0.9300 . ? C23 N9 1.330(7) . ? C23 H23 0.9300 . ? C24 O6 1.257(5) . ? C24 O5 1.257(5) . ? C25 N10 1.334(6) . ? C25 C26 1.378(6) . ? C25 H25 0.9300 . ? C26 C27 1.377(7) . ? C26 H26 0.9300 . ? C27 C28 1.369(7) . ? C27 C30 1.506(6) . ? C28 C29 1.383(7) . ? C28 H28 0.9300 . ? C29 N10 1.325(7) . ? C29 H29 0.9300 . ? C30 O8 1.256(5) . ? C30 O7 1.255(5) . ? C31 N11 1.318(7) . ? C31 C32 1.393(7) . ? C31 H31 0.9300 . ? C32 C33 1.368(7) . ? C32 H32 0.9300 . ? C33 C34 1.363(7) . ? C33 C36 1.514(6) . ? C34 C35 1.382(7) . ? C34 H34 0.9300 . ? C35 N11 1.325(7) . ? C35 H35 0.9300 . ? C36 O10 1.238(5) . ? C36 O9 1.273(5) . ? C37 N12 1.335(7) . ? C37 C38 1.379(6) . ? C37 H37 0.9300 . ? C38 C39 1.380(7) . ? C38 H38 0.9300 . ? C39 C40 1.377(7) . ? C39 C42 1.510(6) . ? C40 C41 1.388(7) . ? C40 H40 0.9300 . ? C41 N12 1.330(7) . ? C41 H41 0.9300 . ? C42 O12 1.250(6) . ? C42 O11 1.252(5) . ? C43 N13 1.324(7) . ? C43 C44 1.375(7) . ? C43 H43 0.9300 . ? C44 C45 1.382(7) . ? C44 H44 0.9300 . ? C45 C46 1.365(6) . ? C45 C48 1.501(6) . ? C46 C47 1.385(7) . ? C46 H46 0.9300 . ? C47 N13 1.330(7) . ? C47 H47 0.9300 . ? C48 O14 1.251(5) . ? C48 O13 1.253(5) . ? C49 N14 1.340(6) . ? C49 C50 1.383(6) . ? C49 H49 0.9300 . ? C50 C51 1.376(6) . ? C50 H50 0.9300 . ? C51 C52 1.380(6) . ? C51 C54 1.513(6) . ? C52 C53 1.378(6) . ? C52 H52 0.9300 . ? C53 N14 1.335(6) . ? C53 H53 0.9300 . ? C54 O16 1.252(5) . ? C54 O15 1.258(5) . ? C55 O17 1.271(5) . ? C55 O18 1.275(5) . ? C55 C56 1.486(6) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O19 1.255(5) . ? C57 O20 1.266(6) . ? C57 C58 1.481(7) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? Cu1 N1 1.896(5) . ? Cu1 N7 1.974(4) 2_566 ? Cu2 N2 1.906(5) . ? Cu2 N8 2.078(4) . ? Cu2 C1 2.413(6) 2_666 ? Cu2 Cu2 2.9120(16) 2_666 ? Cu3 N3 1.881(5) 1_655 ? Cu3 N9 2.100(4) 2_666 ? Cu3 Cu3 2.9349(16) 2_766 ? Cu4 N4 1.905(5) . ? Cu4 N10 2.030(4) . ? Cu5 N5 1.895(5) . ? Cu5 N11 2.148(4) 1_564 ? Cu5 Cu5 3.0440(15) 2_676 ? Cu6 C5 1.889(5) 1_445 ? Cu6 N6 1.888(5) . ? Cu6 N12 2.179(4) 2_556 ? Cu7 N14 1.953(4) . ? Cu7 N13 1.953(4) 1_554 ? N3 Cu3 1.881(4) 1_455 ? N7 Cu1 1.974(4) 2_566 ? N9 Cu3 2.100(4) 2_666 ? N11 Cu5 2.148(4) 1_546 ? N12 Cu6 2.179(4) 2_556 ? N13 Cu7 1.953(4) 1_556 ? O1 Tb2 2.317(3) 2_557 ? O2 Tb2 2.409(3) . ? O3 Tb1 2.357(3) . ? O4 Tb3 2.321(3) . ? O5 Tb1 2.324(3) . ? O6 Tb1 2.412(3) 2_567 ? O7 Tb1 2.351(3) . ? O8 Tb1 2.359(3) 2_567 ? O9 Tb3 2.317(3) . ? O10 Tb2 2.379(3) . ? O11 Tb2 2.364(3) . ? O12 Tb2 2.344(3) 2_557 ? O13 Tb3 2.343(3) . ? O14 Tb1 2.356(3) . ? O15 Tb2 2.351(3) . ? O16 Tb3 2.343(3) . ? O17 Tb2 2.470(3) . ? O17 Tb3 2.480(3) . ? O18 Tb3 2.505(3) . ? O18 Tb1 2.510(3) . ? O19 Tb3 2.443(3) . ? O20 Tb3 2.423(3) . ? O21W Tb1 2.466(3) . ? O21W H21B 0.8158 . ? O21W H21A 0.8193 . ? O22W Tb2 2.468(3) . ? O22W H22A 0.8242 . ? O22W H22B 0.8210 . ? O23W H23B 0.8125 . ? O23W H23A 0.8146 . ? Tb1 O8 2.359(3) 2_567 ? Tb1 O6 2.412(3) 2_567 ? Tb2 O1 2.317(3) 2_557 ? Tb2 O12 2.344(3) 2_557 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cu2 172.7(5) . . ? N1 C1 Cu2 101.2(5) . 2_666 ? Cu2 C1 Cu2 83.63(18) . 2_666 ? N2 C2 Cu3 173.0(6) . . ? N3 C3 Cu4 168.2(5) . . ? N3 C3 Cu1 116.4(4) . . ? Cu4 C3 Cu1 75.21(19) . . ? N4 C4 Cu5 165.1(5) . . ? N5 C5 Cu6 169.8(4) . 1_665 ? N6 C6 Cu7 162.2(5) . . ? N7 C7 C8 122.9(5) . . ? N7 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? C9 C8 C7 119.4(5) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 117.9(4) . . ? C8 C9 C12 121.0(4) . . ? C10 C9 C12 120.9(4) . . ? C9 C10 C11 119.3(5) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N7 C11 C10 123.0(5) . . ? N7 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? O2 C12 O1 126.5(4) . . ? O2 C12 C9 118.8(4) . . ? O1 C12 C9 114.6(4) . . ? C16 C17 N8 120.1(2) . . ? C16 C17 H17 120.0 . . ? N8 C17 H17 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 C18 119.5(3) . . ? C16 C15 C18 120.5(3) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N8 C13 C14 119.7(2) . . ? N8 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? O3 C18 O4 125.5(4) . . ? O3 C18 C15 116.7(4) . . ? O4 C18 C15 117.8(4) . . ? N9 C19 C20 122.8(6) . . ? N9 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C21 C20 C19 119.0(5) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C22 C21 C20 117.9(4) . . ? C22 C21 C24 121.4(4) . . ? C20 C21 C24 120.7(4) . . ? C21 C22 C23 119.7(5) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? N9 C23 C22 123.1(5) . . ? N9 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? O6 C24 O5 125.6(4) . . ? O6 C24 C21 116.7(4) . . ? O5 C24 C21 117.6(4) . . ? N10 C25 C26 122.7(5) . . ? N10 C25 H25 118.7 . . ? C26 C25 H25 118.7 . . ? C27 C26 C25 119.6(5) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C28 C27 C26 117.8(4) . . ? C28 C27 C30 120.5(4) . . ? C26 C27 C30 121.6(4) . . ? C27 C28 C29 119.1(5) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? N10 C29 C28 123.4(5) . . ? N10 C29 H29 118.3 . . ? C28 C29 H29 118.3 . . ? O8 C30 O7 126.3(4) . . ? O8 C30 C27 116.8(4) . . ? O7 C30 C27 116.8(4) . . ? N11 C31 C32 124.2(5) . . ? N11 C31 H31 117.9 . . ? C32 C31 H31 117.9 . . ? C33 C32 C31 118.6(5) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C32 C33 C34 117.6(4) . . ? C32 C33 C36 122.1(4) . . ? C34 C33 C36 120.3(4) . . ? C33 C34 C35 120.0(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? N11 C35 C34 123.2(5) . . ? N11 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? O10 C36 O9 125.4(4) . . ? O10 C36 C33 117.1(4) . . ? O9 C36 C33 117.5(4) . . ? N12 C37 C38 123.3(5) . . ? N12 C37 H37 118.3 . . ? C38 C37 H37 118.3 . . ? C39 C38 C37 119.3(5) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C40 C39 C38 118.1(4) . . ? C40 C39 C42 121.4(4) . . ? C38 C39 C42 120.1(4) . . ? C39 C40 C41 118.5(5) . . ? C39 C40 H40 120.7 . . ? C41 C40 H40 120.7 . . ? N12 C41 C40 123.8(5) . . ? N12 C41 H41 118.1 . . ? C40 C41 H41 118.1 . . ? O12 C42 O11 126.2(4) . . ? O12 C42 C39 118.8(4) . . ? O11 C42 C39 115.0(4) . . ? N13 C43 C44 124.2(5) . . ? N13 C43 H43 117.9 . . ? C44 C43 H43 117.9 . . ? C43 C44 C45 119.1(5) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C46 C45 C44 117.5(4) . . ? C46 C45 C48 122.6(4) . . ? C44 C45 C48 119.8(4) . . ? C45 C46 C47 119.4(5) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? N13 C47 C46 123.6(5) . . ? N13 C47 H47 118.2 . . ? C46 C47 H47 118.2 . . ? O14 C48 O13 125.1(4) . . ? O14 C48 C45 118.3(4) . . ? O13 C48 C45 116.6(4) . . ? N14 C49 C50 123.8(4) . . ? N14 C49 H49 118.1 . . ? C50 C49 H49 118.1 . . ? C51 C50 C49 118.3(5) . . ? C51 C50 H50 120.8 . . ? C49 C50 H50 120.8 . . ? C50 C51 C52 118.7(4) . . ? C50 C51 C54 119.9(4) . . ? C52 C51 C54 121.4(4) . . ? C51 C52 C53 119.2(5) . . ? C51 C52 H52 120.4 . . ? C53 C52 H52 120.4 . . ? N14 C53 C52 123.1(5) . . ? N14 C53 H53 118.4 . . ? C52 C53 H53 118.4 . . ? O16 C54 O15 124.9(4) . . ? O16 C54 C51 117.7(4) . . ? O15 C54 C51 117.4(4) . . ? O17 C55 O18 119.0(4) . . ? O17 C55 C56 120.4(4) . . ? O18 C55 C56 120.6(4) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O19 C57 O20 120.1(4) . . ? O19 C57 C58 119.6(5) . . ? O20 C57 C58 120.3(5) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N1 Cu1 N7 133.0(2) . 2_566 ? N1 Cu1 C3 114.8(2) . . ? N7 Cu1 C3 103.63(19) 2_566 . ? C1 Cu2 N2 118.8(2) . . ? C1 Cu2 N8 107.5(2) . . ? N2 Cu2 N8 121.54(19) . . ? C1 Cu2 C1 96.37(19) . 2_666 ? N2 Cu2 C1 113.54(19) . 2_666 ? N8 Cu2 C1 93.31(18) . 2_666 ? C1 Cu2 Cu2 55.43(17) . 2_666 ? N2 Cu2 Cu2 130.45(14) . 2_666 ? N8 Cu2 Cu2 104.27(14) . 2_666 ? C1 Cu2 Cu2 40.94(14) 2_666 2_666 ? C2 Cu3 N3 136.3(2) . 1_655 ? C2 Cu3 N9 109.9(2) . 2_666 ? N3 Cu3 N9 112.03(19) 1_655 2_666 ? C2 Cu3 Cu3 74.82(19) . 2_766 ? N3 Cu3 Cu3 110.66(15) 1_655 2_766 ? N9 Cu3 Cu3 97.91(14) 2_666 2_766 ? C3 Cu4 N4 140.5(2) . . ? C3 Cu4 N10 101.8(2) . . ? N4 Cu4 N10 116.38(19) . . ? C4 Cu5 N5 147.8(2) . . ? C4 Cu5 N11 100.55(19) . 1_564 ? N5 Cu5 N11 111.37(19) . 1_564 ? C4 Cu5 Cu5 103.51(16) . 2_676 ? N5 Cu5 Cu5 80.21(16) . 2_676 ? N11 Cu5 Cu5 92.14(14) 1_564 2_676 ? C5 Cu6 N6 152.8(2) 1_445 . ? C5 Cu6 N12 98.18(18) 1_445 2_556 ? N6 Cu6 N12 107.8(2) . 2_556 ? N14 Cu7 N13 145.2(2) . 1_554 ? N14 Cu7 C6 106.40(18) . . ? N13 Cu7 C6 106.85(19) 1_554 . ? C1 N1 Cu1 165.8(5) . . ? C2 N2 Cu2 170.5(5) . . ? C3 N3 Cu3 175.8(5) . 1_455 ? C4 N4 Cu4 177.2(5) . . ? C5 N5 Cu5 177.0(5) . . ? C6 N6 Cu6 172.2(5) . . ? C11 N7 C7 117.4(4) . . ? C11 N7 Cu1 122.5(4) . 2_566 ? C7 N7 Cu1 120.0(3) . 2_566 ? C13 N8 C17 120.2(3) . . ? C13 N8 Cu2 117.9(3) . . ? C17 N8 Cu2 121.7(3) . . ? C19 N9 C23 117.4(4) . . ? C19 N9 Cu3 121.0(4) . 2_666 ? C23 N9 Cu3 121.0(4) . 2_666 ? C29 N10 C25 117.2(4) . . ? C29 N10 Cu4 121.6(4) . . ? C25 N10 Cu4 120.0(4) . . ? C31 N11 C35 116.3(4) . . ? C31 N11 Cu5 122.3(4) . 1_546 ? C35 N11 Cu5 121.2(4) . 1_546 ? C41 N12 C37 116.7(4) . . ? C41 N12 Cu6 127.1(4) . 2_556 ? C37 N12 Cu6 115.9(4) . 2_556 ? C47 N13 C43 116.2(4) . . ? C47 N13 Cu7 128.6(4) . 1_556 ? C43 N13 Cu7 114.9(4) . 1_556 ? C53 N14 C49 116.8(4) . . ? C53 N14 Cu7 125.5(4) . . ? C49 N14 Cu7 117.3(3) . . ? C12 O1 Tb2 139.5(3) . 2_557 ? C12 O2 Tb2 133.7(3) . . ? C18 O3 Tb1 132.2(3) . . ? C18 O4 Tb3 134.0(3) . . ? C24 O5 Tb1 171.6(3) . . ? C24 O6 Tb1 119.7(3) . 2_567 ? C30 O7 Tb1 133.4(3) . . ? C30 O8 Tb1 139.1(3) . 2_567 ? C36 O9 Tb3 130.8(3) . . ? C36 O10 Tb2 129.7(3) . . ? C42 O11 Tb2 128.6(3) . . ? C42 O12 Tb2 162.0(3) . 2_557 ? C48 O13 Tb3 126.6(3) . . ? C48 O14 Tb1 140.7(3) . . ? C54 O15 Tb2 143.7(3) . . ? C54 O16 Tb3 125.6(3) . . ? C55 O17 Tb2 142.1(3) . . ? C55 O17 Tb3 95.1(2) . . ? Tb2 O17 Tb3 121.25(12) . . ? C55 O18 Tb3 93.8(2) . . ? C55 O18 Tb1 139.9(3) . . ? Tb3 O18 Tb1 121.64(12) . . ? C57 O19 Tb3 92.7(3) . . ? C57 O20 Tb3 93.4(3) . . ? Tb1 O21W H21B 124.3 . . ? Tb1 O21W H21A 100.7 . . ? H21B O21W H21A 111.3 . . ? Tb2 O22W H22A 121.6 . . ? Tb2 O22W H22B 122.5 . . ? H22A O22W H22B 109.6 . . ? H23B O23W H23A 112.9 . . ? O5 Tb1 O7 72.73(11) . . ? O5 Tb1 O3 80.90(11) . . ? O7 Tb1 O3 80.28(10) . . ? O5 Tb1 O14 146.18(11) . . ? O7 Tb1 O14 141.08(11) . . ? O3 Tb1 O14 102.08(11) . . ? O5 Tb1 O8 82.03(11) . 2_567 ? O7 Tb1 O8 120.75(11) . 2_567 ? O3 Tb1 O8 147.02(11) . 2_567 ? O14 Tb1 O8 77.74(11) . 2_567 ? O5 Tb1 O6 121.29(11) . 2_567 ? O7 Tb1 O6 75.11(10) . 2_567 ? O3 Tb1 O6 138.59(11) . 2_567 ? O14 Tb1 O6 78.64(11) . 2_567 ? O8 Tb1 O6 74.21(11) 2_567 2_567 ? O5 Tb1 O21W 140.55(11) . . ? O7 Tb1 O21W 74.55(11) . . ? O3 Tb1 O21W 72.37(11) . . ? O14 Tb1 O21W 69.50(11) . . ? O8 Tb1 O21W 134.58(11) 2_567 . ? O6 Tb1 O21W 69.27(11) 2_567 . ? O5 Tb1 O18 76.97(10) . . ? O7 Tb1 O18 141.38(10) . . ? O3 Tb1 O18 71.69(10) . . ? O14 Tb1 O18 72.29(10) . . ? O8 Tb1 O18 77.08(10) 2_567 . ? O6 Tb1 O18 142.65(10) 2_567 . ? O21W Tb1 O18 119.24(10) . . ? O1 Tb2 O12 74.51(12) 2_557 2_557 ? O1 Tb2 O15 138.09(11) 2_557 . ? O12 Tb2 O15 147.38(11) 2_557 . ? O1 Tb2 O11 72.34(11) 2_557 . ? O12 Tb2 O11 120.47(12) 2_557 . ? O15 Tb2 O11 80.18(11) . . ? O1 Tb2 O10 81.25(11) 2_557 . ? O12 Tb2 O10 75.64(11) 2_557 . ? O15 Tb2 O10 104.02(11) . . ? O11 Tb2 O10 142.30(11) . . ? O1 Tb2 O2 116.56(11) 2_557 . ? O12 Tb2 O2 82.21(11) 2_557 . ? O15 Tb2 O2 81.78(11) . . ? O11 Tb2 O2 70.84(11) . . ? O10 Tb2 O2 146.64(11) . . ? O1 Tb2 O22W 74.81(12) 2_557 . ? O12 Tb2 O22W 137.61(11) 2_557 . ? O15 Tb2 O22W 68.13(11) . . ? O11 Tb2 O22W 75.96(11) . . ? O10 Tb2 O22W 71.38(11) . . ? O2 Tb2 O22W 138.30(11) . . ? O1 Tb2 O17 146.81(11) 2_557 . ? O12 Tb2 O17 78.69(11) 2_557 . ? O15 Tb2 O17 70.30(10) . . ? O11 Tb2 O17 139.67(11) . . ? O10 Tb2 O17 73.35(10) . . ? O2 Tb2 O17 78.12(10) . . ? O22W Tb2 O17 115.25(10) . . ? O9 Tb3 O4 157.19(11) . . ? O9 Tb3 O13 77.65(11) . . ? O4 Tb3 O13 107.32(11) . . ? O9 Tb3 O16 105.75(11) . . ? O4 Tb3 O16 79.36(10) . . ? O13 Tb3 O16 155.04(12) . . ? O9 Tb3 O20 83.66(11) . . ? O4 Tb3 O20 76.31(11) . . ? O13 Tb3 O20 75.85(12) . . ? O16 Tb3 O20 128.86(12) . . ? O9 Tb3 O19 78.40(11) . . ? O4 Tb3 O19 80.91(11) . . ? O13 Tb3 O19 125.51(11) . . ? O16 Tb3 O19 78.92(12) . . ? O20 Tb3 O19 53.36(11) . . ? O9 Tb3 O17 78.87(11) . . ? O4 Tb3 O17 123.68(10) . . ? O13 Tb3 O17 80.53(11) . . ? O16 Tb3 O17 76.04(11) . . ? O20 Tb3 O17 153.11(11) . . ? O19 Tb3 O17 139.87(10) . . ? O9 Tb3 O18 126.00(11) . . ? O4 Tb3 O18 76.11(10) . . ? O13 Tb3 O18 73.55(11) . . ? O16 Tb3 O18 85.25(11) . . ? O20 Tb3 O18 129.81(10) . . ? O19 Tb3 O18 154.12(11) . . ? O17 Tb3 O18 52.20(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 C7 C8 C9 0.6(8) . . . . ? C7 C8 C9 C10 1.0(8) . . . . ? C7 C8 C9 C12 -174.5(4) . . . . ? C8 C9 C10 C11 -2.6(8) . . . . ? C12 C9 C10 C11 172.9(5) . . . . ? C9 C10 C11 N7 2.8(10) . . . . ? C8 C9 C12 O2 -157.8(4) . . . . ? C10 C9 C12 O2 26.9(7) . . . . ? C8 C9 C12 O1 23.3(6) . . . . ? C10 C9 C12 O1 -152.0(5) . . . . ? N8 C17 C16 C15 0.8(4) . . . . ? C17 C16 C15 C14 0.0 . . . . ? C17 C16 C15 C18 178.9(4) . . . . ? C16 C15 C14 C13 0.0 . . . . ? C18 C15 C14 C13 -178.9(4) . . . . ? C15 C14 C13 N8 -0.7(4) . . . . ? C14 C15 C18 O3 3.9(5) . . . . ? C16 C15 C18 O3 -175.1(3) . . . . ? C14 C15 C18 O4 -176.2(3) . . . . ? C16 C15 C18 O4 4.8(5) . . . . ? N9 C19 C20 C21 -3.2(11) . . . . ? C19 C20 C21 C22 2.5(9) . . . . ? C19 C20 C21 C24 -174.3(6) . . . . ? C20 C21 C22 C23 -0.4(8) . . . . ? C24 C21 C22 C23 176.3(5) . . . . ? C21 C22 C23 N9 -1.3(9) . . . . ? C22 C21 C24 O6 -14.7(7) . . . . ? C20 C21 C24 O6 161.9(5) . . . . ? C22 C21 C24 O5 168.1(5) . . . . ? C20 C21 C24 O5 -15.2(7) . . . . ? N10 C25 C26 C27 -2.2(8) . . . . ? C25 C26 C27 C28 -0.7(7) . . . . ? C25 C26 C27 C30 175.8(4) . . . . ? C26 C27 C28 C29 2.6(8) . . . . ? C30 C27 C28 C29 -173.9(5) . . . . ? C27 C28 C29 N10 -1.9(10) . . . . ? C28 C27 C30 O8 -13.3(6) . . . . ? C26 C27 C30 O8 170.3(4) . . . . ? C28 C27 C30 O7 165.6(4) . . . . ? C26 C27 C30 O7 -10.8(6) . . . . ? N11 C31 C32 C33 0.9(11) . . . . ? C31 C32 C33 C34 2.4(9) . . . . ? C31 C32 C33 C36 179.2(6) . . . . ? C32 C33 C34 C35 -3.8(9) . . . . ? C36 C33 C34 C35 179.4(6) . . . . ? C33 C34 C35 N11 1.9(11) . . . . ? C32 C33 C36 O10 -168.1(5) . . . . ? C34 C33 C36 O10 8.6(7) . . . . ? C32 C33 C36 O9 11.7(7) . . . . ? C34 C33 C36 O9 -171.5(5) . . . . ? N12 C37 C38 C39 3.1(8) . . . . ? C37 C38 C39 C40 1.2(8) . . . . ? C37 C38 C39 C42 -172.6(4) . . . . ? C38 C39 C40 C41 -3.1(8) . . . . ? C42 C39 C40 C41 170.6(5) . . . . ? C39 C40 C41 N12 1.0(10) . . . . ? C40 C39 C42 O12 26.4(7) . . . . ? C38 C39 C42 O12 -160.0(5) . . . . ? C40 C39 C42 O11 -151.6(5) . . . . ? C38 C39 C42 O11 22.0(6) . . . . ? N13 C43 C44 C45 -0.3(12) . . . . ? C43 C44 C45 C46 -0.6(9) . . . . ? C43 C44 C45 C48 -177.6(6) . . . . ? C44 C45 C46 C47 1.7(9) . . . . ? C48 C45 C46 C47 178.6(5) . . . . ? C45 C46 C47 N13 -1.9(11) . . . . ? C46 C45 C48 O14 -9.3(7) . . . . ? C44 C45 C48 O14 167.5(5) . . . . ? C46 C45 C48 O13 170.3(5) . . . . ? C44 C45 C48 O13 -12.9(7) . . . . ? N14 C49 C50 C51 1.0(9) . . . . ? C49 C50 C51 C52 -2.3(8) . . . . ? C49 C50 C51 C54 175.9(5) . . . . ? C50 C51 C52 C53 1.2(9) . . . . ? C54 C51 C52 C53 -177.0(5) . . . . ? C51 C52 C53 N14 1.4(10) . . . . ? C50 C51 C54 O16 -176.2(5) . . . . ? C52 C51 C54 O16 2.0(7) . . . . ? C50 C51 C54 O15 3.7(7) . . . . ? C52 C51 C54 O15 -178.2(5) . . . . ? N3 C3 Cu1 N1 -92.0(5) . . . . ? Cu4 C3 Cu1 N1 85.8(2) . . . . ? N3 C3 Cu1 N7 60.2(5) . . . 2_566 ? Cu4 C3 Cu1 N7 -122.07(18) . . . 2_566 ? N1 C1 Cu2 N2 -107(4) . . . . ? Cu2 C1 Cu2 N2 121.34(19) 2_666 . . . ? N1 C1 Cu2 N8 36(4) . . . . ? Cu2 C1 Cu2 N8 -95.52(18) 2_666 . . . ? N1 C1 Cu2 C1 132(4) . . . 2_666 ? Cu2 C1 Cu2 C1 0.0 2_666 . . 2_666 ? N1 C1 Cu2 Cu2 132(4) . . . 2_666 ? N2 C2 Cu3 N3 76(4) . . . 1_655 ? N2 C2 Cu3 N9 -87(4) . . . 2_666 ? N2 C2 Cu3 Cu3 180(100) . . . 2_766 ? N3 C3 Cu4 N4 173(2) . . . . ? Cu1 C3 Cu4 N4 2.6(4) . . . . ? N3 C3 Cu4 N10 7(2) . . . . ? Cu1 C3 Cu4 N10 -162.78(15) . . . . ? N4 C4 Cu5 N5 156.3(17) . . . . ? N4 C4 Cu5 N11 -31.5(19) . . . 1_564 ? N4 C4 Cu5 Cu5 63.3(19) . . . 2_676 ? N6 C6 Cu7 N14 -136.2(16) . . . . ? N6 C6 Cu7 N13 33.3(17) . . . 1_554 ? Cu2 C1 N1 Cu1 -54(6) . . . . ? Cu2 C1 N1 Cu1 77(2) 2_666 . . . ? N7 Cu1 N1 C1 -145(2) 2_566 . . . ? C3 Cu1 N1 C1 -3(2) . . . . ? Cu3 C2 N2 Cu2 14(6) . . . . ? C1 Cu2 N2 C2 9(3) . . . . ? N8 Cu2 N2 C2 -129(3) . . . . ? C1 Cu2 N2 C2 121(3) 2_666 . . . ? Cu2 Cu2 N2 C2 77(3) 2_666 . . . ? Cu4 C3 N3 Cu3 130(6) . . . 1_455 ? Cu1 C3 N3 Cu3 -61(7) . . . 1_455 ? Cu5 C4 N4 Cu4 -2(12) . . . . ? C3 Cu4 N4 C4 80(10) . . . . ? N10 Cu4 N4 C4 -116(10) . . . . ? Cu6 C5 N5 Cu5 7(12) 1_665 . . . ? C4 Cu5 N5 C5 152(9) . . . . ? N11 Cu5 N5 C5 -19(9) 1_564 . . . ? Cu5 Cu5 N5 C5 -108(9) 2_676 . . . ? Cu7 C6 N6 Cu6 -31(5) . . . . ? C5 Cu6 N6 C6 -158(4) 1_445 . . . ? N12 Cu6 N6 C6 4(4) 2_556 . . . ? C10 C11 N7 C7 -1.2(9) . . . . ? C10 C11 N7 Cu1 173.9(5) . . . 2_566 ? C8 C7 N7 C11 -0.6(8) . . . . ? C8 C7 N7 Cu1 -175.8(4) . . . 2_566 ? C14 C13 N8 C17 1.5(8) . . . . ? C14 C13 N8 Cu2 176.9(2) . . . . ? C16 C17 N8 C13 -1.5(8) . . . . ? C16 C17 N8 Cu2 -176.7(3) . . . . ? C1 Cu2 N8 C13 -6.6(5) . . . . ? N2 Cu2 N8 C13 135.3(4) . . . . ? C1 Cu2 N8 C13 -104.4(4) 2_666 . . . ? Cu2 Cu2 N8 C13 -64.4(4) 2_666 . . . ? C1 Cu2 N8 C17 168.7(4) . . . . ? N2 Cu2 N8 C17 -49.4(5) . . . . ? C1 Cu2 N8 C17 71.0(4) 2_666 . . . ? Cu2 Cu2 N8 C17 111.0(4) 2_666 . . . ? C20 C19 N9 C23 1.5(11) . . . . ? C20 C19 N9 Cu3 173.0(6) . . . 2_666 ? C22 C23 N9 C19 0.8(10) . . . . ? C22 C23 N9 Cu3 -170.7(4) . . . 2_666 ? C28 C29 N10 C25 -1.0(10) . . . . ? C28 C29 N10 Cu4 166.4(5) . . . . ? C26 C25 N10 C29 3.0(8) . . . . ? C26 C25 N10 Cu4 -164.6(4) . . . . ? C3 Cu4 N10 C29 -36.8(5) . . . . ? N4 Cu4 N10 C29 153.5(5) . . . . ? C3 Cu4 N10 C25 130.2(4) . . . . ? N4 Cu4 N10 C25 -39.5(5) . . . . ? C32 C31 N11 C35 -2.8(11) . . . . ? C32 C31 N11 Cu5 173.5(6) . . . 1_546 ? C34 C35 N11 C31 1.3(11) . . . . ? C34 C35 N11 Cu5 -175.0(5) . . . 1_546 ? C40 C41 N12 C37 3.0(9) . . . . ? C40 C41 N12 Cu6 -170.8(5) . . . 2_556 ? C38 C37 N12 C41 -5.1(8) . . . . ? C38 C37 N12 Cu6 169.5(4) . . . 2_556 ? C46 C47 N13 C43 1.0(10) . . . . ? C46 C47 N13 Cu7 -173.0(5) . . . 1_556 ? C44 C43 N13 C47 0.2(11) . . . . ? C44 C43 N13 Cu7 174.9(6) . . . 1_556 ? C52 C53 N14 C49 -2.6(10) . . . . ? C52 C53 N14 Cu7 170.8(5) . . . . ? C50 C49 N14 C53 1.4(9) . . . . ? C50 C49 N14 Cu7 -172.6(5) . . . . ? N13 Cu7 N14 C53 53.3(7) 1_554 . . . ? C6 Cu7 N14 C53 -144.6(5) . . . . ? N13 Cu7 N14 C49 -133.3(4) 1_554 . . . ? C6 Cu7 N14 C49 28.9(5) . . . . ? O2 C12 O1 Tb2 -69.3(6) . . . 2_557 ? C9 C12 O1 Tb2 109.5(4) . . . 2_557 ? O1 C12 O2 Tb2 14.5(7) . . . . ? C9 C12 O2 Tb2 -164.2(3) . . . . ? O4 C18 O3 Tb1 2.2(7) . . . . ? C15 C18 O3 Tb1 -177.9(2) . . . . ? O3 C18 O4 Tb3 66.6(6) . . . . ? C15 C18 O4 Tb3 -113.3(4) . . . . ? O6 C24 O5 Tb1 -2(2) . . . . ? C21 C24 O5 Tb1 175.2(18) . . . . ? O5 C24 O6 Tb1 15.5(6) . . . 2_567 ? C21 C24 O6 Tb1 -161.4(3) . . . 2_567 ? O8 C30 O7 Tb1 61.9(6) . . . . ? C27 C30 O7 Tb1 -116.9(4) . . . . ? O7 C30 O8 Tb1 -20.3(7) . . . 2_567 ? C27 C30 O8 Tb1 158.4(3) . . . 2_567 ? O10 C36 O9 Tb3 65.8(6) . . . . ? C33 C36 O9 Tb3 -114.0(4) . . . . ? O9 C36 O10 Tb2 8.4(7) . . . . ? C33 C36 O10 Tb2 -171.8(3) . . . . ? O12 C42 O11 Tb2 -18.2(7) . . . . ? C39 C42 O11 Tb2 159.5(3) . . . . ? O11 C42 O12 Tb2 31.0(13) . . . 2_557 ? C39 C42 O12 Tb2 -146.7(8) . . . 2_557 ? O14 C48 O13 Tb3 11.4(7) . . . . ? C45 C48 O13 Tb3 -168.2(3) . . . . ? O13 C48 O14 Tb1 64.5(7) . . . . ? C45 C48 O14 Tb1 -115.9(4) . . . . ? O16 C54 O15 Tb2 71.2(7) . . . . ? C51 C54 O15 Tb2 -108.6(5) . . . . ? O15 C54 O16 Tb3 -5.2(7) . . . . ? C51 C54 O16 Tb3 174.7(3) . . . . ? O18 C55 O17 Tb2 -162.7(3) . . . . ? C56 C55 O17 Tb2 16.0(7) . . . . ? O18 C55 O17 Tb3 1.3(4) . . . . ? C56 C55 O17 Tb3 -180.0(4) . . . . ? O17 C55 O18 Tb3 -1.3(4) . . . . ? C56 C55 O18 Tb3 180.0(4) . . . . ? O17 C55 O18 Tb1 -154.8(3) . . . . ? C56 C55 O18 Tb1 26.5(7) . . . . ? O20 C57 O19 Tb3 6.3(5) . . . . ? C58 C57 O19 Tb3 -173.2(5) . . . . ? O19 C57 O20 Tb3 -6.3(5) . . . . ? C58 C57 O20 Tb3 173.1(5) . . . . ? C24 O5 Tb1 O7 -74(2) . . . . ? C24 O5 Tb1 O3 -156(2) . . . . ? C24 O5 Tb1 O14 106(2) . . . . ? C24 O5 Tb1 O8 52(2) . . . 2_567 ? C24 O5 Tb1 O6 -14(2) . . . 2_567 ? C24 O5 Tb1 O21W -109(2) . . . . ? C24 O5 Tb1 O18 131(2) . . . . ? C30 O7 Tb1 O5 8.4(4) . . . . ? C30 O7 Tb1 O3 91.8(4) . . . . ? C30 O7 Tb1 O14 -171.0(3) . . . . ? C30 O7 Tb1 O8 -60.9(4) . . . 2_567 ? C30 O7 Tb1 O6 -121.8(4) . . . 2_567 ? C30 O7 Tb1 O21W 166.0(4) . . . . ? C30 O7 Tb1 O18 48.3(4) . . . . ? C18 O3 Tb1 O5 -134.2(4) . . . . ? C18 O3 Tb1 O7 151.9(4) . . . . ? C18 O3 Tb1 O14 11.5(4) . . . . ? C18 O3 Tb1 O8 -74.5(5) . . . 2_567 ? C18 O3 Tb1 O6 98.0(4) . . . 2_567 ? C18 O3 Tb1 O21W 75.2(4) . . . . ? C18 O3 Tb1 O18 -55.0(4) . . . . ? C48 O14 Tb1 O5 -12.2(6) . . . . ? C48 O14 Tb1 O7 166.7(4) . . . . ? C48 O14 Tb1 O3 -103.9(5) . . . . ? C48 O14 Tb1 O8 42.3(4) . . . 2_567 ? C48 O14 Tb1 O6 118.4(5) . . . 2_567 ? C48 O14 Tb1 O21W -169.6(5) . . . . ? C48 O14 Tb1 O18 -37.8(4) . . . . ? C55 O18 Tb1 O5 -59.5(4) . . . . ? Tb3 O18 Tb1 O5 151.98(16) . . . . ? C55 O18 Tb1 O7 -98.5(4) . . . . ? Tb3 O18 Tb1 O7 113.05(17) . . . . ? C55 O18 Tb1 O3 -144.1(4) . . . . ? Tb3 O18 Tb1 O3 67.40(15) . . . . ? C55 O18 Tb1 O14 106.2(4) . . . . ? Tb3 O18 Tb1 O14 -42.30(14) . . . . ? C55 O18 Tb1 O8 25.1(4) . . . 2_567 ? Tb3 O18 Tb1 O8 -123.35(16) . . . 2_567 ? C55 O18 Tb1 O6 65.6(5) . . . 2_567 ? Tb3 O18 Tb1 O6 -82.9(2) . . . 2_567 ? C55 O18 Tb1 O21W 159.3(4) . . . . ? Tb3 O18 Tb1 O21W 10.83(19) . . . . ? C54 O15 Tb2 O1 167.7(4) . . . 2_557 ? C54 O15 Tb2 O12 -14.6(6) . . . 2_557 ? C54 O15 Tb2 O11 118.5(5) . . . . ? C54 O15 Tb2 O10 -99.8(5) . . . . ? C54 O15 Tb2 O2 46.7(5) . . . . ? C54 O15 Tb2 O22W -162.7(5) . . . . ? C54 O15 Tb2 O17 -33.6(5) . . . . ? C42 O11 Tb2 O1 68.4(4) . . . 2_557 ? C42 O11 Tb2 O12 9.2(4) . . . 2_557 ? C42 O11 Tb2 O15 -143.7(4) . . . . ? C42 O11 Tb2 O10 116.1(4) . . . . ? C42 O11 Tb2 O2 -59.0(4) . . . . ? C42 O11 Tb2 O22W 146.6(4) . . . . ? C42 O11 Tb2 O17 -100.8(4) . . . . ? C36 O10 Tb2 O1 140.9(4) . . . 2_557 ? C36 O10 Tb2 O12 -143.0(4) . . . 2_557 ? C36 O10 Tb2 O15 3.3(4) . . . . ? C36 O10 Tb2 O11 95.4(4) . . . . ? C36 O10 Tb2 O2 -93.1(4) . . . . ? C36 O10 Tb2 O22W 64.0(4) . . . . ? C36 O10 Tb2 O17 -60.7(4) . . . . ? C12 O2 Tb2 O1 26.7(4) . . . 2_557 ? C12 O2 Tb2 O12 -41.6(4) . . . 2_557 ? C12 O2 Tb2 O15 166.9(4) . . . . ? C12 O2 Tb2 O11 84.5(4) . . . . ? C12 O2 Tb2 O10 -90.1(4) . . . . ? C12 O2 Tb2 O22W 123.6(4) . . . . ? C12 O2 Tb2 O17 -121.7(4) . . . . ? C55 O17 Tb2 O1 -93.0(5) . . . 2_557 ? Tb3 O17 Tb2 O1 105.7(2) . . . 2_557 ? C55 O17 Tb2 O12 -56.4(4) . . . 2_557 ? Tb3 O17 Tb2 O12 142.30(16) . . . 2_557 ? C55 O17 Tb2 O15 113.3(5) . . . . ? Tb3 O17 Tb2 O15 -47.98(14) . . . . ? C55 O17 Tb2 O11 67.9(5) . . . . ? Tb3 O17 Tb2 O11 -93.4(2) . . . . ? C55 O17 Tb2 O10 -134.6(5) . . . . ? Tb3 O17 Tb2 O10 64.08(15) . . . . ? C55 O17 Tb2 O2 27.9(4) . . . . ? Tb3 O17 Tb2 O2 -133.39(16) . . . . ? C55 O17 Tb2 O22W 166.0(4) . . . . ? Tb3 O17 Tb2 O22W 4.71(18) . . . . ? C36 O9 Tb3 O4 148.2(3) . . . . ? C36 O9 Tb3 O13 42.8(3) . . . . ? C36 O9 Tb3 O16 -111.7(4) . . . . ? C36 O9 Tb3 O20 119.7(4) . . . . ? C36 O9 Tb3 O19 173.5(4) . . . . ? C36 O9 Tb3 O17 -39.8(3) . . . . ? C36 O9 Tb3 O18 -16.0(4) . . . . ? C18 O4 Tb3 O9 158.9(3) . . . . ? C18 O4 Tb3 O13 -101.7(4) . . . . ? C18 O4 Tb3 O16 53.5(4) . . . . ? C18 O4 Tb3 O20 -171.9(4) . . . . ? C18 O4 Tb3 O19 133.8(4) . . . . ? C18 O4 Tb3 O17 -11.7(4) . . . . ? C18 O4 Tb3 O18 -34.2(4) . . . . ? C48 O13 Tb3 O9 167.9(4) . . . . ? C48 O13 Tb3 O4 10.9(4) . . . . ? C48 O13 Tb3 O16 -91.3(4) . . . . ? C48 O13 Tb3 O20 81.4(4) . . . . ? C48 O13 Tb3 O19 102.0(4) . . . . ? C48 O13 Tb3 O17 -111.5(4) . . . . ? C48 O13 Tb3 O18 -58.3(4) . . . . ? C54 O16 Tb3 O9 28.8(4) . . . . ? C54 O16 Tb3 O4 -174.0(4) . . . . ? C54 O16 Tb3 O13 -65.7(5) . . . . ? C54 O16 Tb3 O20 123.4(4) . . . . ? C54 O16 Tb3 O19 103.3(4) . . . . ? C54 O16 Tb3 O17 -45.1(4) . . . . ? C54 O16 Tb3 O18 -97.3(4) . . . . ? C57 O20 Tb3 O9 83.7(3) . . . . ? C57 O20 Tb3 O4 -85.3(3) . . . . ? C57 O20 Tb3 O13 162.6(3) . . . . ? C57 O20 Tb3 O16 -21.4(3) . . . . ? C57 O20 Tb3 O19 3.5(3) . . . . ? C57 O20 Tb3 O17 133.3(3) . . . . ? C57 O20 Tb3 O18 -143.6(3) . . . . ? C57 O19 Tb3 O9 -94.2(3) . . . . ? C57 O19 Tb3 O4 76.1(3) . . . . ? C57 O19 Tb3 O13 -28.7(3) . . . . ? C57 O19 Tb3 O16 157.0(3) . . . . ? C57 O19 Tb3 O20 -3.5(3) . . . . ? C57 O19 Tb3 O17 -150.9(3) . . . . ? C57 O19 Tb3 O18 103.6(3) . . . . ? C55 O17 Tb3 O9 154.9(3) . . . . ? Tb2 O17 Tb3 O9 -36.53(14) . . . . ? C55 O17 Tb3 O4 -28.8(3) . . . . ? Tb2 O17 Tb3 O4 139.75(13) . . . . ? C55 O17 Tb3 O13 75.7(2) . . . . ? Tb2 O17 Tb3 O13 -115.69(15) . . . . ? C55 O17 Tb3 O16 -95.6(3) . . . . ? Tb2 O17 Tb3 O16 72.98(15) . . . . ? C55 O17 Tb3 O20 104.5(3) . . . . ? Tb2 O17 Tb3 O20 -87.0(2) . . . . ? C55 O17 Tb3 O19 -148.6(2) . . . . ? Tb2 O17 Tb3 O19 20.0(2) . . . . ? C55 O17 Tb3 O18 -0.7(2) . . . . ? Tb2 O17 Tb3 O18 167.8(2) . . . . ? C55 O18 Tb3 O9 -29.3(3) . . . . ? Tb1 O18 Tb3 O9 130.99(13) . . . . ? C55 O18 Tb3 O4 156.9(3) . . . . ? Tb1 O18 Tb3 O4 -42.77(13) . . . . ? C55 O18 Tb3 O13 -89.9(3) . . . . ? Tb1 O18 Tb3 O13 70.35(15) . . . . ? C55 O18 Tb3 O16 76.7(2) . . . . ? Tb1 O18 Tb3 O16 -122.96(15) . . . . ? C55 O18 Tb3 O20 -144.6(2) . . . . ? Tb1 O18 Tb3 O20 15.7(2) . . . . ? C55 O18 Tb3 O19 128.9(3) . . . . ? Tb1 O18 Tb3 O19 -70.8(3) . . . . ? C55 O18 Tb3 O17 0.7(2) . . . . ? Tb1 O18 Tb3 O17 161.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.836 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 964394' ####################################################################### # # 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_I-E #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H42 Cu7 Dy3 N14 O22, H2 O' _chemical_formula_sum 'C58 H44 Cu7 Dy3 N14 O23' _chemical_formula_weight 2237.43 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8300(8) _cell_length_b 17.3115(11) _cell_length_c 17.8851(12) _cell_angle_alpha 74.4250(10) _cell_angle_beta 88.4240(10) _cell_angle_gamma 86.0630(10) _cell_volume 3519.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10062 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 25.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2150 _exptl_absorpt_coefficient_mu 5.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.292 _exptl_absorpt_correction_T_max 0.347 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18633 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.40 _reflns_number_total 12736 _reflns_number_gt 10062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0295P)^2^+0.8294P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00108(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12736 _refine_ls_number_parameters 949 _refine_ls_number_restraints 321 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.076 _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 0.0178(7) -0.0965(5) 1.0147(4) 0.0432(16) Uani 1 1 d U . . C2 C -0.3365(7) -0.0457(5) 0.9975(5) 0.052(2) Uani 1 1 d U . . C3 C 0.6464(6) 0.1877(5) 1.0082(4) 0.0401(15) Uani 1 1 d U . . C4 C 0.9469(6) 0.3482(4) 1.0149(4) 0.0318(15) Uani 1 1 d U . . C5 C 0.7341(6) 0.4947(4) 0.0110(4) 0.0295(14) Uani 1 1 d U . . C6 C 0.4291(6) 0.3349(4) -0.0165(4) 0.0314(14) Uani 1 1 d U . . C7 C 0.7741(6) 0.2806(5) 0.7630(4) 0.0393(17) Uani 1 1 d U . . H7 H 0.8510 0.2649 0.7661 0.047 Uiso 1 1 calc R . . C8 C 0.7283(6) 0.3125(4) 0.6907(4) 0.0369(16) Uani 1 1 d U . . H8 H 0.7733 0.3179 0.6463 0.044 Uiso 1 1 calc R . . C9 C 0.6140(5) 0.3365(4) 0.6849(4) 0.0271(12) Uani 1 1 d U . . C10 C 0.5520(6) 0.3249(5) 0.7531(4) 0.049(2) Uani 1 1 d U . . H10 H 0.4744 0.3379 0.7519 0.059 Uiso 1 1 calc R . . C11 C 0.6062(6) 0.2937(6) 0.8234(4) 0.057(2) Uani 1 1 d U . . H11 H 0.5643 0.2885 0.8690 0.069 Uiso 1 1 calc R . . C12 C 0.5616(5) 0.3798(4) 0.6085(4) 0.0245(11) Uani 1 1 d U . . C13 C 0.0621(8) -0.0268(5) 0.8217(5) 0.069(3) Uani 1 1 d U . . H13 H 0.0944 -0.0706 0.8588 0.082 Uiso 1 1 calc R . . C14 C 0.1109(7) -0.0059(5) 0.7481(4) 0.057(2) Uani 1 1 d U . . H14 H 0.1750 -0.0353 0.7371 0.068 Uiso 1 1 calc R . . C15 C 0.0653(5) 0.0576(4) 0.6917(4) 0.0254(12) Uani 1 1 d U . . C16 C -0.0290(6) 0.0995(5) 0.7124(4) 0.0383(16) Uani 1 1 d U . . H16 H -0.0626 0.1437 0.6764 0.046 Uiso 1 1 calc R . . C17 C -0.0724(6) 0.0758(4) 0.7861(4) 0.0368(15) Uani 1 1 d U . . H17 H -0.1358 0.1049 0.7985 0.044 Uiso 1 1 calc R . . C18 C 0.1180(5) 0.0815(4) 0.6122(4) 0.0232(10) Uani 1 1 d U . . C19 C 0.4108(6) 0.0757(6) 0.8055(5) 0.065(3) Uani 1 1 d U . . H19 H 0.3381 0.0772 0.8264 0.079 Uiso 1 1 calc R . . C20 C 0.4224(6) 0.0650(6) 0.7322(5) 0.056(3) Uani 1 1 d U . . H20 H 0.3586 0.0610 0.7045 0.067 Uiso 1 1 calc R . . C21 C 0.5284(5) 0.0603(4) 0.7001(4) 0.0289(14) Uani 1 1 d U . . C22 C 0.6185(6) 0.0693(5) 0.7439(4) 0.0418(19) Uani 1 1 d U . . H22 H 0.6921 0.0666 0.7248 0.050 Uiso 1 1 calc R . . C23 C 0.5987(6) 0.0824(5) 0.8161(4) 0.0454(19) Uani 1 1 d U . . H23 H 0.6604 0.0905 0.8436 0.054 Uiso 1 1 calc R . . C24 C 0.5474(5) 0.0419(4) 0.6233(4) 0.0244(12) Uani 1 1 d U . . C25 C 0.7482(6) 0.2088(5) 1.2225(4) 0.0387(16) Uani 1 1 d U . . H25 H 0.8241 0.2190 1.2128 0.046 Uiso 1 1 calc R . . C26 C 0.7151(6) 0.1732(4) 1.2971(4) 0.0352(15) Uani 1 1 d U . . H26 H 0.7684 0.1562 1.3363 0.042 Uiso 1 1 calc R . . C27 C 0.6022(5) 0.1632(4) 1.3131(4) 0.0237(12) Uani 1 1 d U . . C28 C 0.5284(6) 0.1869(5) 1.2532(4) 0.053(2) Uani 1 1 d U . . H28 H 0.4512 0.1810 1.2622 0.064 Uiso 1 1 calc R . . C29 C 0.5673(6) 0.2190(6) 1.1801(4) 0.057(2) Uani 1 1 d U . . H29 H 0.5152 0.2346 1.1400 0.069 Uiso 1 1 calc R . . C30 C 0.5620(5) 0.1187(4) 1.3942(4) 0.0240(12) Uani 1 1 d U . . C31 C -0.0274(7) 0.4651(6) 0.1935(4) 0.063(3) Uani 1 1 d U . . H31 H -0.0858 0.4399 0.1778 0.075 Uiso 1 1 calc R . . C32 C 0.0052(6) 0.4385(5) 0.2702(4) 0.053(2) Uani 1 1 d U . . H32 H -0.0331 0.3988 0.3051 0.064 Uiso 1 1 calc R . . C33 C 0.0949(5) 0.4718(4) 0.2938(4) 0.0284(13) Uani 1 1 d U . . C34 C 0.1465(7) 0.5287(5) 0.2392(4) 0.058(2) Uani 1 1 d U . . H34 H 0.2094 0.5514 0.2526 0.070 Uiso 1 1 calc R . . C35 C 0.1078(7) 0.5535(6) 0.1646(4) 0.065(3) Uani 1 1 d U . . H35 H 0.1454 0.5929 0.1289 0.078 Uiso 1 1 calc R . . C36 C 0.1385(5) 0.4433(4) 0.3760(3) 0.0226(10) Uani 1 1 d U . . C37 C 0.6647(6) 0.4168(5) 0.1911(4) 0.0408(17) Uani 1 1 d U . . H37 H 0.7337 0.4058 0.1686 0.049 Uiso 1 1 calc R . . C38 C 0.6644(6) 0.4208(4) 0.2669(4) 0.0385(16) Uani 1 1 d U . . H38 H 0.7318 0.4138 0.2942 0.046 Uiso 1 1 calc R . . C39 C 0.5615(5) 0.4354(4) 0.3021(4) 0.0268(13) Uani 1 1 d U . . C40 C 0.4650(6) 0.4423(5) 0.2595(4) 0.0455(19) Uani 1 1 d U . . H40 H 0.3944 0.4492 0.2819 0.055 Uiso 1 1 calc R . . C41 C 0.4732(6) 0.4391(6) 0.1821(5) 0.054(2) Uani 1 1 d U . . H41 H 0.4073 0.4452 0.1534 0.065 Uiso 1 1 calc R . . C42 C 0.5603(5) 0.4509(4) 0.3813(4) 0.0246(12) Uani 1 1 d U . . C43 C 0.2415(8) 0.3024(5) 0.1376(4) 0.060(2) Uani 1 1 d U . . H43 H 0.2463 0.3546 0.1064 0.072 Uiso 1 1 calc R . . C44 C 0.2253(8) 0.2908(5) 0.2164(4) 0.052(2) Uani 1 1 d U . . H44 H 0.2222 0.3345 0.2375 0.062 Uiso 1 1 calc R . . C45 C 0.2138(5) 0.2140(4) 0.2643(4) 0.0262(12) Uani 1 1 d U . . C46 C 0.2233(7) 0.1526(5) 0.2297(4) 0.051(2) Uani 1 1 d U . . H46 H 0.2182 0.0998 0.2593 0.061 Uiso 1 1 calc R . . C47 C 0.2408(8) 0.1695(5) 0.1494(4) 0.057(2) Uani 1 1 d U . . H47 H 0.2460 0.1267 0.1269 0.068 Uiso 1 1 calc R . . C48 C 0.1985(5) 0.2007(4) 0.3495(3) 0.0235(11) Uani 1 1 d U . . C49 C 0.2589(6) 0.3580(5) 0.8353(4) 0.0414(17) Uani 1 1 d U . . H49 H 0.2924 0.3972 0.8522 0.050 Uiso 1 1 calc R . . C50 C 0.2360(6) 0.3731(4) 0.7577(4) 0.0398(17) Uani 1 1 d U . . H50 H 0.2528 0.4217 0.7232 0.048 Uiso 1 1 calc R . . C51 C 0.1878(5) 0.3149(4) 0.7316(4) 0.0282(13) Uani 1 1 d U . . C52 C 0.1626(7) 0.2443(5) 0.7853(4) 0.0447(19) Uani 1 1 d U . . H52 H 0.1303 0.2039 0.7694 0.054 Uiso 1 1 calc R . . C53 C 0.1861(7) 0.2342(5) 0.8625(4) 0.055(2) Uani 1 1 d U . . H53 H 0.1668 0.1871 0.8983 0.066 Uiso 1 1 calc R . . C54 C 0.1719(5) 0.3272(4) 0.6457(3) 0.0247(11) Uani 1 1 d U . . C55 C 0.3549(5) 0.2497(4) 0.5068(4) 0.0227(11) Uani 1 1 d U . . C56 C 0.4812(5) 0.2438(5) 0.5113(6) 0.061(3) Uani 1 1 d U . . H56A H 0.5095 0.1905 0.5112 0.092 Uiso 1 1 calc R . . H56B H 0.5036 0.2552 0.5582 0.092 Uiso 1 1 calc R . . H56C H 0.5116 0.2819 0.4673 0.092 Uiso 1 1 calc R . . C57 C -0.1220(5) 0.2673(4) 0.4822(4) 0.0308(13) Uani 1 1 d U . . C58 C -0.2451(6) 0.2598(6) 0.4799(6) 0.071(3) Uani 1 1 d U . . H58A H -0.2648 0.2535 0.4303 0.107 Uiso 1 1 calc R . . H58B H -0.2847 0.3073 0.4879 0.107 Uiso 1 1 calc R . . H58C H -0.2661 0.2138 0.5201 0.107 Uiso 1 1 calc R . . Cu1 Cu 0.78685(8) 0.21645(7) 0.92870(5) 0.0482(3) Uani 1 1 d U . . Cu2 Cu -0.08937(8) -0.01835(6) 0.95463(6) 0.0501(3) Uani 1 1 d U . . Cu3 Cu 0.47529(8) 0.08571(7) 0.96426(6) 0.0516(3) Uani 1 1 d U . . Cu4 Cu 0.73605(8) 0.25339(6) 1.05211(5) 0.0412(2) Uani 1 1 d U . . Cu5 Cu 1.04898(8) 0.42834(6) 0.97331(5) 0.0462(3) Uani 1 1 d U . . Cu6 Cu 0.60066(8) 0.43809(6) 0.02470(5) 0.0460(3) Uani 1 1 d U . . Cu7 Cu 0.28994(9) 0.27416(7) -0.00624(5) 0.0533(3) Uani 1 1 d U . . Dy1 Dy 0.32345(2) 0.050897(18) 0.491592(16) 0.01894(8) Uani 1 1 d U . . Dy2 Dy 0.32448(2) 0.455606(18) 0.506309(16) 0.02007(8) Uani 1 1 d U . . Dy3 Dy 0.11232(2) 0.266490(18) 0.496675(16) 0.01892(8) Uani 1 1 d U . . N1 N 0.0821(6) -0.1456(5) 1.0450(4) 0.0593(19) Uani 1 1 d U . . N2 N -0.2468(6) -0.0291(4) 0.9778(4) 0.0496(16) Uani 1 1 d U . . N3 N 0.5815(5) 0.1484(4) 0.9937(4) 0.0458(16) Uani 1 1 d U . . N4 N 0.8694(6) 0.3112(5) 1.0305(4) 0.0611(19) Uani 1 1 d U . . N5 N 0.8162(6) 0.5239(4) 0.0144(4) 0.0549(18) Uani 1 1 d U . . N6 N 0.4957(6) 0.3748(4) -0.0060(4) 0.0572(19) Uani 1 1 d U . . N7 N 0.7156(5) 0.2710(4) 0.8279(3) 0.0416(14) Uani 1 1 d U . . N8 N -0.0292(5) 0.0131(4) 0.8414(3) 0.0424(14) Uani 1 1 d U . . N9 N 0.4964(5) 0.0840(4) 0.8484(4) 0.0501(17) Uani 1 1 d U . . N10 N 0.6767(5) 0.2294(4) 1.1631(3) 0.0388(13) Uani 1 1 d U . . N11 N 0.0184(5) 0.5236(4) 0.1408(3) 0.0463(16) Uani 1 1 d U . . N12 N 0.5719(5) 0.4277(4) 0.1482(4) 0.0432(14) Uani 1 1 d U . . N13 N 0.2504(5) 0.2423(4) 0.1041(3) 0.0435(14) Uani 1 1 d U . . N14 N 0.2351(5) 0.2892(4) 0.8881(3) 0.0425(15) Uani 1 1 d U . . O1 O 0.6306(4) 0.4159(3) 0.5578(3) 0.0335(10) Uani 1 1 d U . . O2 O 0.4580(4) 0.3789(3) 0.5995(3) 0.0332(9) Uani 1 1 d U . . O3 O 0.2074(4) 0.0441(3) 0.6015(2) 0.0297(7) Uani 1 1 d U . . O4 O 0.0684(4) 0.1378(3) 0.5623(2) 0.0279(6) Uani 1 1 d U . . O5 O 0.4622(4) 0.0477(3) 0.5813(2) 0.0296(9) Uani 1 1 d U . . O6 O 0.6448(4) 0.0187(3) 0.6077(3) 0.0312(10) Uani 1 1 d U . . O7 O 0.6375(4) 0.0842(3) 1.4416(2) 0.0287(10) Uani 1 1 d U . . O8 O 0.4572(3) 0.1216(3) 1.4062(2) 0.0292(10) Uani 1 1 d U . . O9 O 0.0791(4) 0.3983(3) 0.4267(2) 0.0282(6) Uani 1 1 d U . . O10 O 0.2320(4) 0.4680(3) 0.3882(2) 0.0326(8) Uani 1 1 d U . . O11 O 0.6493(4) 0.4756(3) 0.3990(2) 0.0310(10) Uani 1 1 d U . . O12 O 0.4702(4) 0.4406(3) 0.4203(3) 0.0321(9) Uani 1 1 d U . . O13 O 0.1745(4) 0.2627(3) 0.3729(2) 0.0312(7) Uani 1 1 d U . . O14 O 0.2102(4) 0.1317(3) 0.3923(2) 0.0293(8) Uani 1 1 d U . . O15 O 0.1953(4) 0.3932(3) 0.6013(2) 0.0301(7) Uani 1 1 d U . . O16 O 0.1349(4) 0.2701(3) 0.6243(2) 0.0324(7) Uani 1 1 d U . . O17 O 0.3015(3) 0.3180(3) 0.4977(3) 0.0265(6) Uani 1 1 d U . . O18 O 0.2988(3) 0.1886(2) 0.5127(3) 0.0263(6) Uani 1 1 d U . . O19 O -0.0818(3) 0.2952(3) 0.5341(3) 0.0327(7) Uani 1 1 d U . . O20 O -0.0565(4) 0.2460(3) 0.4338(3) 0.0345(8) Uani 1 1 d U . . O21W O 0.1554(4) -0.0183(3) 0.4762(3) 0.0340(10) Uani 1 1 d U . . H21A H 0.1949 -0.0404 0.4483 0.041 Uiso 1 1 d R . . H21B H 0.1227 -0.0518 0.5093 0.041 Uiso 1 1 d R . . O22W O 0.1475(4) 0.5390(3) 0.5041(3) 0.0375(10) Uani 1 1 d U . . H22A H 0.1570 0.5871 0.4935 0.045 Uiso 1 1 d R . . H22B H 0.1020 0.5257 0.5396 0.045 Uiso 1 1 d R . . O23W O 0.0372(4) 0.9030(3) 0.6002(3) 0.0463(14) Uani 1 1 d . . . H23A H -0.0304 0.9157 0.6014 0.056 Uiso 1 1 d R . . H23B H 0.0493 0.8566 0.5984 0.056 Uiso 1 1 d R . . 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 0.055(3) 0.041(4) 0.030(2) -0.005(2) 0.015(3) -0.005(3) C2 0.053(3) 0.076(6) 0.038(5) -0.031(5) 0.008(4) -0.024(4) C3 0.042(4) 0.044(5) 0.035(3) -0.009(3) -0.004(2) -0.005(3) C4 0.032(3) 0.034(4) 0.026(4) -0.002(3) -0.009(3) -0.005(2) C5 0.032(3) 0.033(4) 0.023(3) -0.007(3) -0.003(2) 0.002(2) C6 0.038(3) 0.040(4) 0.019(3) -0.014(3) -0.006(2) 0.001(2) C7 0.028(2) 0.058(5) 0.0249(12) 0.000(3) -0.0044(14) 0.007(3) C8 0.028(2) 0.050(5) 0.0239(12) 0.003(3) -0.0021(16) 0.008(3) C9 0.0259(19) 0.032(4) 0.0205(16) -0.002(2) -0.0037(12) 0.000(3) C10 0.032(3) 0.076(6) 0.0244(19) 0.007(4) 0.0017(13) 0.012(4) C11 0.040(3) 0.096(7) 0.0215(17) 0.003(4) 0.0022(17) 0.021(4) C12 0.0304(15) 0.018(3) 0.0227(19) -0.002(2) -0.0055(14) 0.004(2) C13 0.074(6) 0.070(6) 0.036(3) 0.018(3) 0.024(4) 0.037(4) C14 0.063(5) 0.047(5) 0.039(3) 0.015(3) 0.026(3) 0.023(3) C15 0.027(3) 0.024(3) 0.025(2) -0.0059(17) 0.0096(19) -0.002(2) C16 0.031(4) 0.054(4) 0.026(2) -0.009(2) 0.007(2) 0.012(3) C17 0.030(4) 0.049(4) 0.029(2) -0.011(2) 0.009(2) 0.007(3) C18 0.026(3) 0.0211(17) 0.0237(18) -0.0076(14) 0.0085(14) -0.0065(17) C19 0.030(2) 0.133(9) 0.048(4) -0.054(6) -0.001(2) 0.006(5) C20 0.025(2) 0.110(7) 0.045(4) -0.045(5) -0.003(2) 0.004(5) C21 0.025(2) 0.037(4) 0.029(3) -0.017(3) -0.0058(17) 0.004(3) C22 0.027(2) 0.071(5) 0.035(3) -0.028(4) -0.006(2) -0.001(4) C23 0.037(2) 0.077(6) 0.028(3) -0.022(4) -0.0035(19) -0.014(4) C24 0.0255(17) 0.024(3) 0.023(2) -0.006(3) -0.0055(15) 0.002(3) C25 0.029(2) 0.057(5) 0.0246(10) 0.000(3) 0.0041(15) -0.010(3) C26 0.0262(19) 0.049(5) 0.0245(17) 0.000(3) 0.0031(17) -0.004(3) C27 0.0244(19) 0.024(3) 0.0205(18) -0.004(2) 0.0036(13) 0.004(3) C28 0.029(2) 0.090(7) 0.026(2) 0.009(4) -0.0016(14) -0.002(4) C29 0.034(2) 0.104(7) 0.0230(19) 0.005(4) -0.0020(12) -0.009(4) C30 0.0271(17) 0.019(3) 0.023(2) -0.002(2) 0.0039(14) 0.001(2) C31 0.062(5) 0.091(7) 0.027(3) 0.011(4) -0.020(3) -0.044(4) C32 0.047(5) 0.080(6) 0.025(3) 0.006(3) -0.015(3) -0.029(4) C33 0.025(3) 0.036(4) 0.0205(17) -0.001(2) -0.0071(18) 0.001(2) C34 0.075(6) 0.062(6) 0.028(3) 0.015(3) -0.023(3) -0.037(4) C35 0.067(6) 0.094(7) 0.025(3) 0.014(3) -0.017(4) -0.048(5) C36 0.027(3) 0.0222(19) 0.0176(16) -0.0045(15) -0.0046(13) 0.003(2) C37 0.036(2) 0.061(5) 0.0323(19) -0.025(4) 0.0051(18) -0.005(4) C38 0.036(2) 0.052(5) 0.034(3) -0.026(4) 0.0013(19) 0.007(4) C39 0.028(2) 0.032(4) 0.023(2) -0.010(3) 0.0016(14) -0.008(3) C40 0.034(2) 0.074(6) 0.031(3) -0.016(4) -0.0057(19) -0.008(4) C41 0.035(2) 0.100(7) 0.036(3) -0.029(5) -0.0073(17) -0.013(4) C42 0.025(2) 0.028(3) 0.020(2) -0.006(3) 0.0026(15) -0.002(3) C43 0.113(7) 0.044(3) 0.0160(18) -0.0002(16) 0.003(4) 0.001(5) C44 0.099(6) 0.035(2) 0.0172(17) -0.0028(16) 0.006(4) -0.001(5) C45 0.028(3) 0.034(2) 0.0162(13) -0.0065(11) 0.004(3) 0.000(3) C46 0.090(6) 0.043(3) 0.0245(16) -0.0154(15) 0.020(4) -0.023(5) C47 0.102(7) 0.057(3) 0.0225(18) -0.0209(17) 0.012(4) -0.037(5) C48 0.020(3) 0.0340(16) 0.0146(12) -0.0048(9) -0.0009(18) 0.005(2) C49 0.053(5) 0.057(4) 0.021(2) -0.016(2) 0.001(3) -0.021(4) C50 0.061(5) 0.041(4) 0.020(2) -0.009(2) -0.003(3) -0.018(4) C51 0.030(3) 0.039(3) 0.0158(12) -0.0058(14) -0.003(3) -0.010(3) C52 0.066(5) 0.050(4) 0.0176(18) -0.001(2) -0.011(4) -0.030(4) C53 0.078(6) 0.073(5) 0.0141(18) -0.002(2) -0.001(4) -0.046(5) C54 0.023(3) 0.037(2) 0.0144(12) -0.0065(13) 0.003(2) -0.008(2) C55 0.0181(8) 0.0266(14) 0.025(3) -0.010(3) -0.001(3) -0.0016(11) C56 0.0183(12) 0.046(4) 0.135(9) -0.051(6) -0.008(4) 0.0001(15) C57 0.0189(8) 0.020(3) 0.054(4) -0.010(3) -0.006(2) 0.002(3) C58 0.0222(16) 0.085(7) 0.125(9) -0.056(7) 0.000(3) -0.013(4) Cu1 0.0431(5) 0.0681(7) 0.0246(5) 0.0006(5) -0.0059(4) 0.0083(5) Cu2 0.0513(6) 0.0566(7) 0.0349(5) -0.0017(5) 0.0171(5) -0.0001(5) Cu3 0.0539(6) 0.0747(8) 0.0349(6) -0.0252(5) 0.0078(5) -0.0255(6) Cu4 0.0494(6) 0.0498(6) 0.0240(5) -0.0052(4) 0.0070(4) -0.0219(5) Cu5 0.0431(5) 0.0603(7) 0.0330(5) -0.0031(5) -0.0053(4) -0.0226(5) Cu6 0.0417(5) 0.0656(7) 0.0339(5) -0.0151(5) -0.0024(4) -0.0183(5) Cu7 0.0632(6) 0.0844(8) 0.0160(5) -0.0136(5) 0.0009(5) -0.0308(6) Dy1 0.01855(15) 0.02329(17) 0.01379(16) -0.00326(12) 0.00173(11) -0.00074(12) Dy2 0.02198(16) 0.02301(17) 0.01451(16) -0.00314(12) -0.00139(12) -0.00354(13) Dy3 0.01790(15) 0.02407(17) 0.01457(16) -0.00474(12) -0.00010(12) -0.00153(12) N1 0.054(4) 0.074(5) 0.050(5) -0.018(4) -0.011(3) 0.004(3) N2 0.0518(14) 0.058(4) 0.037(4) -0.009(3) 0.013(2) -0.010(3) N3 0.049(4) 0.060(4) 0.035(3) -0.021(3) 0.000(3) -0.013(3) N4 0.054(3) 0.076(5) 0.053(4) -0.011(3) 0.016(3) -0.034(3) N5 0.052(4) 0.057(5) 0.053(4) -0.006(4) -0.003(3) -0.023(3) N6 0.066(4) 0.076(5) 0.038(3) -0.022(4) -0.005(3) -0.029(3) N7 0.039(2) 0.056(4) 0.0233(9) -0.004(2) -0.0039(13) 0.015(3) N8 0.044(3) 0.050(4) 0.0296(16) -0.0077(17) 0.008(2) 0.006(2) N9 0.040(2) 0.082(5) 0.038(2) -0.033(3) 0.0009(18) -0.007(4) N10 0.037(2) 0.051(4) 0.0244(11) -0.0006(19) 0.0006(11) -0.011(3) N11 0.041(4) 0.069(5) 0.024(3) 0.001(2) -0.007(2) -0.021(3) N12 0.040(2) 0.061(4) 0.0358(15) -0.019(3) 0.0032(13) -0.026(3) N13 0.057(4) 0.059(3) 0.0157(14) -0.0104(12) -0.001(2) -0.011(3) N14 0.047(4) 0.069(4) 0.014(2) -0.0102(19) -0.001(3) -0.024(3) O1 0.045(2) 0.029(3) 0.024(2) 0.0010(18) -0.0043(19) -0.009(2) O2 0.0334(13) 0.040(3) 0.0234(15) -0.0038(16) -0.0105(11) 0.0012(14) O3 0.0355(16) 0.0295(18) 0.0214(13) -0.0043(13) 0.0126(11) 0.0007(12) O4 0.0281(14) 0.0273(10) 0.0270(15) -0.0043(9) 0.0029(14) -0.0069(9) O5 0.0312(14) 0.033(2) 0.024(2) -0.0071(18) -0.0103(12) 0.0053(14) O6 0.0269(15) 0.041(3) 0.027(2) -0.012(2) -0.0004(17) 0.002(2) O7 0.0298(19) 0.024(3) 0.026(2) 0.0030(17) 0.0010(17) -0.0012(19) O8 0.0278(16) 0.035(3) 0.021(2) -0.002(2) 0.0055(15) 0.001(2) O9 0.0303(15) 0.0269(9) 0.0237(15) -0.0019(9) 0.0010(13) 0.0037(9) O10 0.0368(16) 0.042(2) 0.0166(11) -0.0010(12) -0.0082(10) -0.0087(15) O11 0.0333(18) 0.042(3) 0.021(2) -0.013(2) 0.0025(18) -0.011(2) O12 0.0303(13) 0.039(2) 0.0251(16) -0.0045(18) 0.0087(11) -0.0055(14) O13 0.0399(17) 0.0373(16) 0.0159(9) -0.0079(11) 0.0022(10) 0.0040(16) O14 0.029(2) 0.0348(14) 0.0210(14) -0.0016(11) -0.0073(12) -0.0003(16) O15 0.0335(14) 0.0361(16) 0.0189(13) -0.0041(11) 0.0072(11) -0.0054(15) O16 0.0430(18) 0.0410(18) 0.0150(9) -0.0084(11) 0.0009(10) -0.0124(16) O17 0.0207(9) 0.0252(8) 0.0347(18) -0.0096(12) 0.0016(10) -0.0027(8) O18 0.0202(9) 0.0242(8) 0.0340(19) -0.0068(12) -0.0052(11) -0.0013(7) O19 0.0216(8) 0.0361(19) 0.042(2) -0.0145(16) 0.0075(11) -0.0034(11) O20 0.0256(10) 0.042(2) 0.040(2) -0.0166(16) -0.0131(11) 0.0020(14) O21W 0.0283(18) 0.0334(18) 0.044(2) -0.0139(16) 0.0024(19) -0.0101(18) O22W 0.0319(17) 0.0286(16) 0.050(3) -0.0080(16) 0.0030(17) 0.0051(15) O23W 0.028(3) 0.053(3) 0.060(4) -0.017(3) -0.003(3) -0.010(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 N1 1.131(9) . ? C1 Cu2 1.911(9) . ? C1 Cu2 2.411(8) 2_557 ? C2 N2 1.141(9) . ? C2 Cu3 1.865(8) 2_557 ? C3 N3 1.139(8) . ? C3 Cu4 1.930(7) . ? C4 N4 1.139(8) . ? C4 Cu5 1.888(7) . ? C5 N5 1.135(8) . ? C5 Cu6 1.890(7) . ? C6 N6 1.135(8) . ? C6 Cu7 1.992(7) . ? C7 N7 1.312(8) . ? C7 C8 1.373(9) . ? C8 C9 1.386(9) . ? C9 C10 1.381(9) . ? C9 C12 1.499(8) . ? C10 C11 1.383(10) . ? C11 N7 1.325(9) . ? C12 O2 1.242(7) . ? C12 O1 1.266(7) . ? C13 N8 1.332(9) . ? C13 C14 1.389(10) . ? C14 C15 1.367(10) . ? C15 C16 1.386(8) . ? C15 C18 1.501(8) . ? C16 C17 1.368(9) . ? C17 N8 1.339(9) . ? C18 O3 1.240(7) . ? C18 O4 1.255(7) . ? C19 N9 1.325(9) . ? C19 C20 1.375(10) . ? C20 C21 1.371(9) . ? C21 C22 1.382(9) . ? C21 C24 1.499(8) . ? C22 C23 1.381(9) . ? C23 N9 1.329(9) . ? C24 O6 1.243(7) . ? C24 O5 1.256(7) . ? C25 N10 1.332(8) . ? C25 C26 1.370(9) . ? C26 C27 1.371(9) . ? C27 C28 1.359(9) . ? C27 C30 1.527(8) . ? C28 C29 1.357(10) . ? C29 N10 1.335(9) . ? C30 O7 1.254(7) . ? C30 O8 1.252(7) . ? C31 N11 1.321(9) . ? C31 C32 1.381(10) . ? C32 C33 1.370(9) . ? C33 C34 1.353(10) . ? C33 C36 1.512(8) . ? C34 C35 1.369(10) . ? C35 N11 1.336(9) . ? C36 O9 1.258(7) . ? C36 O10 1.258(7) . ? C37 N12 1.331(9) . ? C37 C38 1.376(9) . ? C38 C39 1.395(9) . ? C39 C40 1.371(9) . ? C39 C42 1.511(8) . ? C40 C41 1.402(10) . ? C41 N12 1.327(9) . ? C42 O11 1.242(7) . ? C42 O12 1.255(7) . ? C43 N13 1.331(9) . ? C43 C44 1.380(10) . ? C44 C45 1.388(10) . ? C45 C46 1.363(9) . ? C45 C48 1.487(8) . ? C46 C47 1.399(10) . ? C47 N13 1.314(10) . ? C48 O14 1.235(7) . ? C48 O13 1.265(7) . ? C49 N14 1.348(9) . ? C49 C50 1.372(9) . ? C50 C51 1.380(9) . ? C51 C52 1.382(9) . ? C51 C54 1.508(8) . ? C52 C53 1.379(9) . ? C53 N14 1.334(9) . ? C54 O15 1.248(7) . ? C54 O16 1.260(7) . ? C55 O18 1.266(7) . ? C55 O17 1.275(7) . ? C55 C56 1.493(8) . ? C57 O20 1.257(8) . ? C57 O19 1.271(7) . ? C57 C58 1.474(9) . ? Cu1 N1 1.897(7) 2_657 ? Cu1 N7 1.978(6) . ? Cu1 Cu4 2.5048(13) . ? Cu2 N2 1.907(7) . ? Cu2 N8 2.070(6) . ? Cu2 C1 2.411(8) 2_557 ? Cu2 Cu2 2.905(2) 2_557 ? Cu3 C2 1.865(8) 2_557 ? Cu3 N3 1.888(6) . ? Cu3 N9 2.089(6) . ? Cu3 Cu3 2.924(2) 2_657 ? Cu4 N4 1.902(7) . ? Cu4 N10 2.031(6) . ? Cu5 N5 1.891(6) 2_766 ? Cu5 N11 2.139(6) 2_666 ? Cu5 Cu5 3.038(2) 2_767 ? Cu6 N6 1.895(6) . ? Cu6 N12 2.186(6) . ? Cu7 N13 1.953(6) . ? Cu7 N14 1.959(5) 1_554 ? Dy1 O5 2.314(4) . ? Dy1 O14 2.333(4) . ? Dy1 O8 2.337(4) 1_554 ? Dy1 O7 2.343(4) 2_657 ? Dy1 O3 2.348(4) . ? Dy1 O6 2.408(4) 2_656 ? Dy1 O21W 2.448(4) . ? Dy1 O18 2.508(4) . ? Dy2 O1 2.303(4) 2_666 ? Dy2 O12 2.326(4) . ? Dy2 O15 2.343(4) . ? Dy2 O11 2.354(4) 2_666 ? Dy2 O10 2.358(4) . ? Dy2 O2 2.388(4) . ? Dy2 O22W 2.455(4) . ? Dy2 O17 2.462(4) . ? Dy3 O9 2.302(4) . ? Dy3 O4 2.308(4) . ? Dy3 O16 2.323(4) . ? Dy3 O13 2.329(4) . ? Dy3 O20 2.411(4) . ? Dy3 O19 2.430(4) . ? Dy3 O17 2.468(4) . ? Dy3 O18 2.487(4) . ? N1 Cu1 1.897(7) 2_657 ? N5 Cu5 1.891(6) 2_766 ? N11 Cu5 2.139(6) 2_666 ? N14 Cu7 1.959(5) 1_556 ? O1 Dy2 2.303(4) 2_666 ? O6 Dy1 2.408(4) 2_656 ? O7 Dy1 2.343(4) 2_657 ? O8 Dy1 2.337(4) 1_556 ? O11 Dy2 2.354(4) 2_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 N1 C1 Cu2 174.1(7) . . ? N1 C1 Cu2 100.7(7) . 2_557 ? Cu2 C1 Cu2 83.6(3) . 2_557 ? N2 C2 Cu3 172.8(9) . 2_557 ? N3 C3 Cu4 167.7(7) . . ? N4 C4 Cu5 165.6(7) . . ? N5 C5 Cu6 169.7(7) . . ? N6 C6 Cu7 161.9(6) . . ? N7 C7 C8 123.8(7) . . ? C7 C8 C9 118.9(7) . . ? C10 C9 C8 117.3(6) . . ? C10 C9 C12 121.0(6) . . ? C8 C9 C12 121.5(6) . . ? C9 C10 C11 119.5(7) . . ? N7 C11 C10 122.3(7) . . ? O2 C12 O1 125.5(6) . . ? O2 C12 C9 119.9(6) . . ? O1 C12 C9 114.5(6) . . ? N8 C13 C14 122.8(8) . . ? C15 C14 C13 120.4(7) . . ? C14 C15 C16 116.7(6) . . ? C14 C15 C18 121.0(6) . . ? C16 C15 C18 122.2(6) . . ? C17 C16 C15 119.7(7) . . ? N8 C17 C16 124.0(6) . . ? O3 C18 O4 125.5(6) . . ? O3 C18 C15 117.1(6) . . ? O4 C18 C15 117.5(5) . . ? N9 C19 C20 124.3(7) . . ? C21 C20 C19 119.6(7) . . ? C20 C21 C22 116.7(6) . . ? C20 C21 C24 122.2(6) . . ? C22 C21 C24 121.0(6) . . ? C21 C22 C23 119.7(7) . . ? N9 C23 C22 123.5(7) . . ? O6 C24 O5 125.1(6) . . ? O6 C24 C21 117.7(5) . . ? O5 C24 C21 117.1(5) . . ? N10 C25 C26 123.1(6) . . ? C25 C26 C27 119.0(7) . . ? C28 C27 C26 118.0(6) . . ? C28 C27 C30 120.7(6) . . ? C26 C27 C30 121.0(6) . . ? C29 C28 C27 120.0(7) . . ? N10 C29 C28 123.1(7) . . ? O7 C30 O8 127.1(6) . . ? O7 C30 C27 116.5(5) . . ? O8 C30 C27 116.4(6) . . ? N11 C31 C32 124.8(7) . . ? C33 C32 C31 118.8(7) . . ? C34 C33 C32 116.9(7) . . ? C34 C33 C36 121.3(6) . . ? C32 C33 C36 121.7(6) . . ? C33 C34 C35 121.1(7) . . ? N11 C35 C34 123.1(8) . . ? O9 C36 O10 125.1(6) . . ? O9 C36 C33 118.5(5) . . ? O10 C36 C33 116.4(6) . . ? N12 C37 C38 123.7(7) . . ? C37 C38 C39 118.9(7) . . ? C40 C39 C38 117.6(6) . . ? C40 C39 C42 122.3(6) . . ? C38 C39 C42 119.9(6) . . ? C39 C40 C41 119.7(7) . . ? N12 C41 C40 122.3(7) . . ? O11 C42 O12 127.4(6) . . ? O11 C42 C39 115.0(5) . . ? O12 C42 C39 117.6(6) . . ? N13 C43 C44 122.9(8) . . ? C43 C44 C45 120.1(7) . . ? C46 C45 C44 116.7(6) . . ? C46 C45 C48 122.7(6) . . ? C44 C45 C48 120.5(6) . . ? C45 C46 C47 119.5(7) . . ? N13 C47 C46 123.7(7) . . ? O14 C48 O13 124.4(6) . . ? O14 C48 C45 119.2(6) . . ? O13 C48 C45 116.3(6) . . ? N14 C49 C50 123.3(7) . . ? C49 C50 C51 118.9(7) . . ? C50 C51 C52 118.3(6) . . ? C50 C51 C54 119.7(6) . . ? C52 C51 C54 121.8(6) . . ? C53 C52 C51 119.4(7) . . ? N14 C53 C52 122.8(7) . . ? O15 C54 O16 125.0(6) . . ? O15 C54 C51 117.6(6) . . ? O16 C54 C51 117.4(6) . . ? O18 C55 O17 118.8(5) . . ? O18 C55 C56 122.0(6) . . ? O17 C55 C56 119.2(6) . . ? O20 C57 O19 119.8(6) . . ? O20 C57 C58 120.7(7) . . ? O19 C57 C58 119.4(7) . . ? N1 Cu1 N7 132.1(3) 2_657 . ? N1 Cu1 Cu4 103.6(2) 2_657 . ? N7 Cu1 Cu4 123.26(17) . . ? C1 Cu2 N2 118.7(3) . . ? C1 Cu2 N8 107.4(3) . . ? N2 Cu2 N8 121.7(3) . . ? C1 Cu2 C1 96.4(3) . 2_557 ? N2 Cu2 C1 113.2(3) . 2_557 ? N8 Cu2 C1 93.8(2) . 2_557 ? C1 Cu2 Cu2 55.6(2) . 2_557 ? N2 Cu2 Cu2 130.0(2) . 2_557 ? N8 Cu2 Cu2 104.62(18) . 2_557 ? C1 Cu2 Cu2 40.8(2) 2_557 2_557 ? C2 Cu3 N3 136.0(3) 2_557 . ? C2 Cu3 N9 110.0(3) 2_557 . ? N3 Cu3 N9 111.9(3) . . ? C2 Cu3 Cu3 74.6(3) 2_557 2_657 ? N3 Cu3 Cu3 111.5(2) . 2_657 ? N9 Cu3 Cu3 98.0(2) . 2_657 ? N4 Cu4 C3 140.2(3) . . ? N4 Cu4 N10 116.3(3) . . ? C3 Cu4 N10 102.1(3) . . ? N4 Cu4 Cu1 83.9(2) . . ? C3 Cu4 Cu1 56.3(2) . . ? N10 Cu4 Cu1 153.26(18) . . ? C4 Cu5 N5 147.9(3) . 2_766 ? C4 Cu5 N11 100.3(3) . 2_666 ? N5 Cu5 N11 111.6(3) 2_766 2_666 ? C4 Cu5 Cu5 103.5(2) . 2_767 ? N5 Cu5 Cu5 79.8(2) 2_766 2_767 ? N11 Cu5 Cu5 92.33(19) 2_666 2_767 ? C5 Cu6 N6 152.9(3) . . ? C5 Cu6 N12 98.4(2) . . ? N6 Cu6 N12 107.5(3) . . ? N13 Cu7 N14 145.3(3) . 1_554 ? N13 Cu7 C6 106.9(3) . . ? N14 Cu7 C6 106.3(3) 1_554 . ? O5 Dy1 O14 145.90(16) . . ? O5 Dy1 O8 81.86(15) . 1_554 ? O14 Dy1 O8 77.67(15) . 1_554 ? O5 Dy1 O7 72.98(15) . 2_657 ? O14 Dy1 O7 141.11(15) . 2_657 ? O8 Dy1 O7 120.59(15) 1_554 2_657 ? O5 Dy1 O3 81.04(15) . . ? O14 Dy1 O3 102.11(15) . . ? O8 Dy1 O3 147.12(15) 1_554 . ? O7 Dy1 O3 80.42(15) 2_657 . ? O5 Dy1 O6 120.86(15) . 2_656 ? O14 Dy1 O6 79.07(15) . 2_656 ? O8 Dy1 O6 74.02(15) 1_554 2_656 ? O7 Dy1 O6 74.70(15) 2_657 2_656 ? O3 Dy1 O6 138.71(15) . 2_656 ? O5 Dy1 O21W 140.61(16) . . ? O14 Dy1 O21W 69.83(15) . . ? O8 Dy1 O21W 134.57(15) 1_554 . ? O7 Dy1 O21W 74.28(15) 2_657 . ? O3 Dy1 O21W 72.42(15) . . ? O6 Dy1 O21W 69.42(14) 2_656 . ? O5 Dy1 O18 77.17(14) . . ? O14 Dy1 O18 71.93(14) . . ? O8 Dy1 O18 77.29(14) 1_554 . ? O7 Dy1 O18 141.71(14) 2_657 . ? O3 Dy1 O18 71.64(14) . . ? O6 Dy1 O18 142.74(15) 2_656 . ? O21W Dy1 O18 119.18(13) . . ? O1 Dy2 O12 74.39(16) 2_666 . ? O1 Dy2 O15 138.11(16) 2_666 . ? O12 Dy2 O15 147.49(16) . . ? O1 Dy2 O11 72.59(15) 2_666 2_666 ? O12 Dy2 O11 120.56(15) . 2_666 ? O15 Dy2 O11 79.93(15) . 2_666 ? O1 Dy2 O10 81.17(15) 2_666 . ? O12 Dy2 O10 75.67(15) . . ? O15 Dy2 O10 104.08(15) . . ? O11 Dy2 O10 142.33(16) 2_666 . ? O1 Dy2 O2 116.50(16) 2_666 . ? O12 Dy2 O2 82.09(16) . . ? O15 Dy2 O2 81.88(16) . . ? O11 Dy2 O2 70.82(15) 2_666 . ? O10 Dy2 O2 146.63(16) . . ? O1 Dy2 O22W 74.91(16) 2_666 . ? O12 Dy2 O22W 137.66(16) . . ? O15 Dy2 O22W 68.04(16) . . ? O11 Dy2 O22W 75.91(15) 2_666 . ? O10 Dy2 O22W 71.40(15) . . ? O2 Dy2 O22W 138.33(15) . . ? O1 Dy2 O17 146.85(15) 2_666 . ? O12 Dy2 O17 78.85(15) . . ? O15 Dy2 O17 70.26(14) . . ? O11 Dy2 O17 139.40(15) 2_666 . ? O10 Dy2 O17 73.49(15) . . ? O2 Dy2 O17 78.07(15) . . ? O22W Dy2 O17 115.20(14) . . ? O9 Dy3 O4 157.13(15) . . ? O9 Dy3 O16 105.57(15) . . ? O4 Dy3 O16 79.38(15) . . ? O9 Dy3 O13 78.04(15) . . ? O4 Dy3 O13 107.13(15) . . ? O16 Dy3 O13 155.01(16) . . ? O9 Dy3 O20 83.90(16) . . ? O4 Dy3 O20 76.09(16) . . ? O16 Dy3 O20 128.75(16) . . ? O13 Dy3 O20 75.96(16) . . ? O9 Dy3 O19 78.23(15) . . ? O4 Dy3 O19 81.01(15) . . ? O16 Dy3 O19 78.54(16) . . ? O13 Dy3 O19 125.94(16) . . ? O20 Dy3 O19 53.73(15) . . ? O9 Dy3 O17 78.89(15) . . ? O4 Dy3 O17 123.68(15) . . ? O16 Dy3 O17 75.78(15) . . ? O13 Dy3 O17 80.83(15) . . ? O20 Dy3 O17 153.50(16) . . ? O19 Dy3 O17 139.27(14) . . ? O9 Dy3 O18 126.08(15) . . ? O4 Dy3 O18 76.12(14) . . ? O16 Dy3 O18 85.42(15) . . ? O13 Dy3 O18 73.27(15) . . ? O20 Dy3 O18 129.59(14) . . ? O19 Dy3 O18 154.12(15) . . ? O17 Dy3 O18 52.38(14) . . ? C1 N1 Cu1 164.5(7) . 2_657 ? C2 N2 Cu2 170.7(8) . . ? C3 N3 Cu3 177.1(7) . . ? C4 N4 Cu4 177.0(7) . . ? C5 N5 Cu5 176.4(7) . 2_766 ? C6 N6 Cu6 172.9(6) . . ? C7 N7 C11 118.1(6) . . ? C7 N7 Cu1 120.6(5) . . ? C11 N7 Cu1 121.2(5) . . ? C13 N8 C17 116.4(6) . . ? C13 N8 Cu2 119.8(5) . . ? C17 N8 Cu2 123.7(5) . . ? C19 N9 C23 116.0(6) . . ? C19 N9 Cu3 122.3(5) . . ? C23 N9 Cu3 121.3(5) . . ? C29 N10 C25 116.6(6) . . ? C29 N10 Cu4 121.7(5) . . ? C25 N10 Cu4 120.5(5) . . ? C31 N11 C35 115.2(7) . . ? C31 N11 Cu5 122.9(5) . 2_666 ? C35 N11 Cu5 121.9(5) . 2_666 ? C41 N12 C37 117.7(6) . . ? C41 N12 Cu6 126.4(5) . . ? C37 N12 Cu6 115.6(5) . . ? C47 N13 C43 117.0(6) . . ? C47 N13 Cu7 128.3(5) . . ? C43 N13 Cu7 114.5(5) . . ? C53 N14 C49 117.2(6) . . ? C53 N14 Cu7 125.4(5) . 1_556 ? C49 N14 Cu7 117.0(5) . 1_556 ? C12 O1 Dy2 140.1(4) . 2_666 ? C12 O2 Dy2 134.7(4) . . ? C18 O3 Dy1 132.6(4) . . ? C18 O4 Dy3 134.3(4) . . ? C24 O5 Dy1 171.4(4) . . ? C24 O6 Dy1 120.7(4) . 2_656 ? C30 O7 Dy1 132.3(4) . 2_657 ? C30 O8 Dy1 139.3(4) . 1_556 ? C36 O9 Dy3 130.8(4) . . ? C36 O10 Dy2 129.7(4) . . ? C42 O11 Dy2 128.3(4) . 2_666 ? C42 O12 Dy2 161.3(4) . . ? C48 O13 Dy3 127.0(4) . . ? C48 O14 Dy1 142.1(4) . . ? C54 O15 Dy2 143.5(4) . . ? C54 O16 Dy3 125.8(4) . . ? C55 O17 Dy2 142.3(4) . . ? C55 O17 Dy3 94.8(3) . . ? Dy2 O17 Dy3 121.52(16) . . ? C55 O18 Dy3 94.1(3) . . ? C55 O18 Dy1 139.7(4) . . ? Dy3 O18 Dy1 121.91(16) . . ? C57 O19 Dy3 92.4(4) . . ? C57 O20 Dy3 93.7(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.020 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.156 _database_code_depnum_ccdc_archive 'CCDC 964395' ####################################################################### # # 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_II-A #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C89 H80 Cl6 Cu13 N19 O40 Tb4, 4(H2 O)' _chemical_formula_sum 'C89 H88 Cl6 Cu13 N19 O44 Tb4' _chemical_formula_weight 3802.49 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' Cl Cl 0.1484 0.1585 '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' 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.896(2) _cell_length_b 16.210(4) _cell_length_c 18.443(4) _cell_angle_alpha 92.002(3) _cell_angle_beta 103.580(3) _cell_angle_gamma 92.510(3) _cell_volume 2869.9(11) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10365 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 25.40 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1846 _exptl_absorpt_coefficient_mu 5.014 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.312 _exptl_absorpt_correction_T_max 0.367 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15094 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.40 _reflns_number_total 10365 _reflns_number_gt 7970 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0000P)^2^+17.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10365 _refine_ls_number_parameters 798 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 0.0195(9) 0.0324(4) -0.0062(5) 0.048(2) Uani 0.50 1 d P . . C2 C 0.6636(14) 0.0631(8) 0.0294(7) 0.048(3) Uani 1 1 d . . . C3 C 1.0591(9) 0.3082(5) -0.0047(4) 0.036(2) Uani 1 1 d . . . C4 C -0.0405(9) 0.1085(6) 0.7993(5) 0.047(2) Uani 1 1 d . . . H4 H -0.1192 0.1005 0.8181 0.056 Uiso 1 1 calc R . . C5 C -0.0535(8) 0.0921(5) 0.7237(4) 0.038(2) Uani 1 1 d . . . H5 H -0.1393 0.0753 0.6927 0.045 Uiso 1 1 calc R . . C6 C 0.0635(8) 0.1013(4) 0.6952(4) 0.0256(16) Uani 1 1 d . . . C7 C 0.1842(8) 0.1330(5) 0.7430(4) 0.0293(18) Uani 1 1 d . . . H7 H 0.2635 0.1435 0.7252 0.035 Uiso 1 1 calc R . . C8 C 0.1879(9) 0.1493(5) 0.8172(4) 0.041(2) Uani 1 1 d . . . H8 H 0.2705 0.1714 0.8484 0.049 Uiso 1 1 calc R . . C9 C 0.0630(8) 0.0749(4) 0.6154(4) 0.0253(17) Uani 1 1 d . . . C10 C 0.5604(8) 0.0205(5) 0.1939(4) 0.036(2) Uani 1 1 d . . . H10 H 0.6408 0.0100 0.1781 0.043 Uiso 1 1 calc R . . C11 C 0.5646(8) 0.0175(5) 0.2688(4) 0.0349(19) Uani 1 1 d . . . H11 H 0.6466 0.0055 0.3024 0.042 Uiso 1 1 calc R . . C12 C 0.4477(7) 0.0323(4) 0.2939(4) 0.0241(16) Uani 1 1 d . . . C13 C 0.3287(8) 0.0506(5) 0.2409(4) 0.037(2) Uani 1 1 d . . . H13 H 0.2473 0.0619 0.2554 0.045 Uiso 1 1 calc R . . C14 C 0.3325(9) 0.0519(6) 0.1669(4) 0.045(2) Uani 1 1 d . . . H14 H 0.2520 0.0631 0.1319 0.054 Uiso 1 1 calc R . . C15 C 0.4444(8) 0.0288(4) 0.3747(4) 0.0231(16) Uani 1 1 d . . . C16 C 0.1037(10) 0.2227(6) 0.1946(5) 0.052(3) Uani 1 1 d . . . H16 H 0.1439 0.2564 0.1647 0.063 Uiso 1 1 calc R . . C17 C 0.1512(10) 0.2344(6) 0.2707(4) 0.048(2) Uani 1 1 d . . . H17 H 0.2202 0.2750 0.2913 0.058 Uiso 1 1 calc R . . C18 C 0.0928(8) 0.1836(5) 0.3161(4) 0.0321(18) Uani 1 1 d . . . C19 C -0.0074(9) 0.1246(5) 0.2818(4) 0.039(2) Uani 1 1 d . . . H19 H -0.0470 0.0888 0.3103 0.047 Uiso 1 1 calc R . . C20 C -0.0493(9) 0.1186(6) 0.2051(5) 0.046(2) Uani 1 1 d . . . H20 H -0.1187 0.0787 0.1832 0.055 Uiso 1 1 calc R . . C21 C 0.1484(9) 0.1905(5) 0.4000(4) 0.0339(19) Uani 1 1 d . . . C22 C 1.1401(9) 0.4693(5) 0.1997(4) 0.039(2) Uani 1 1 d . . . H22 H 1.0490 0.4858 0.1874 0.047 Uiso 1 1 calc R . . C23 C 1.2107(8) 0.4758(5) 0.2733(4) 0.0344(19) Uani 1 1 d . . . H23 H 1.1661 0.4939 0.3096 0.041 Uiso 1 1 calc R . . C24 C 1.3486(8) 0.4553(4) 0.2936(4) 0.0272(17) Uani 1 1 d . . . C25 C 1.4061(9) 0.4259(6) 0.2362(4) 0.046(2) Uani 1 1 d . . . H25 H 1.4978 0.4105 0.2465 0.055 Uiso 1 1 calc R . . C26 C 1.3265(10) 0.4199(6) 0.1646(5) 0.057(3) Uani 1 1 d . . . H26 H 1.3668 0.4001 0.1271 0.068 Uiso 1 1 calc R . . C27 C 1.4337(8) 0.4637(4) 0.3729(4) 0.0255(17) Uani 1 1 d . . . C28 C 0.9586(10) 0.6642(5) 0.2053(5) 0.043(2) Uani 1 1 d . . . H28 H 1.0203 0.6945 0.1842 0.052 Uiso 1 1 calc R . . C29 C 1.0021(9) 0.6436(5) 0.2783(5) 0.037(2) Uani 1 1 d . . . H29 H 1.0917 0.6595 0.3054 0.045 Uiso 1 1 calc R . . C30 C 0.9122(8) 0.5992(5) 0.3117(4) 0.0292(17) Uani 1 1 d . . . C31 C 0.7806(9) 0.5791(6) 0.2692(5) 0.047(2) Uani 1 1 d . . . H31 H 0.7166 0.5498 0.2896 0.056 Uiso 1 1 calc R . . C32 C 0.7433(10) 0.6023(7) 0.1963(5) 0.058(3) Uani 1 1 d . . . H32 H 0.6531 0.5895 0.1685 0.069 Uiso 1 1 calc R . . C33 C 0.9591(8) 0.5698(4) 0.3883(4) 0.0258(17) Uani 1 1 d . . . C34 C 1.2000(11) 0.6564(7) 0.8130(5) 0.062(3) Uani 1 1 d . . . H34 H 1.1414 0.6219 0.8326 0.075 Uiso 1 1 calc R . . C35 C 1.1867(10) 0.6532(6) 0.7367(5) 0.052(3) Uani 1 1 d . . . H35 H 1.1207 0.6163 0.7065 0.062 Uiso 1 1 calc R . . C36 C 1.2684(8) 0.7030(4) 0.7050(4) 0.0280(17) Uani 1 1 d . . . C37 C 1.3644(10) 0.7553(6) 0.7530(5) 0.048(2) Uani 1 1 d . . . H37 H 1.4231 0.7907 0.7342 0.058 Uiso 1 1 calc R . . C38 C 1.3744(10) 0.7557(6) 0.8297(5) 0.055(3) Uani 1 1 d . . . H38 H 1.4404 0.7915 0.8610 0.065 Uiso 1 1 calc R . . C39 C 1.2591(8) 0.6991(5) 0.6214(4) 0.0321(18) Uani 1 1 d . . . C40 C 1.3969(10) 0.7903(7) 1.1085(5) 0.060(3) Uani 1 1 d . . . H40 H 1.4209 0.8335 1.0812 0.072 Uiso 1 1 calc R . . C41 C 1.4276(10) 0.8010(6) 1.1861(5) 0.052(3) Uani 1 1 d . . . H41 H 1.4727 0.8496 1.2099 0.062 Uiso 1 1 calc R . . C42 C 1.3898(8) 0.7382(5) 1.2263(4) 0.0347(19) Uani 1 1 d . . . C43 C 1.3241(10) 0.6689(6) 1.1882(5) 0.052(3) Uani 1 1 d . . . H43 H 1.2963 0.6255 1.2140 0.063 Uiso 1 1 calc R . . C44 C 1.2990(11) 0.6629(6) 1.1120(5) 0.061(3) Uani 1 1 d . . . H44 H 1.2540 0.6148 1.0871 0.073 Uiso 1 1 calc R . . C45 C 1.4258(11) 0.7464(7) 1.3116(5) 0.056(3) Uani 1 1 d . . . Cl1 Cl 0.3385(2) 0.16912(14) 0.00691(12) 0.0507(6) Uani 1 1 d . . . Cl2 Cl 0.8527(2) 0.47145(13) 0.04238(11) 0.0411(5) Uani 1 1 d . . . Cl3 Cl 1.4350(3) 0.37739(18) -0.00480(16) 0.0701(8) Uani 1 1 d . . . Cu1 Cu 0.10626(14) 0.12446(8) -0.04067(6) 0.0570(3) Uani 1 1 d . . . Cu2 Cu 0.44255(11) 0.04696(7) 0.03253(5) 0.0406(3) Uani 1 1 d . . . Cu3 Cu 0.91772(13) 0.15961(8) 0.04561(6) 0.0596(4) Uani 1 1 d . . . Cu4 Cu 1.08054(13) 0.42572(7) 0.03792(6) 0.0527(3) Uani 1 1 d . . . Cu5 Cu 1.19812(15) 0.35593(10) -0.05194(7) 0.0746(4) Uani 1 1 d . . . Cu6 Cu 1.5000 0.5000 0.0000 0.064(3) Uani 0.589(15) 2 d SP . 1 Cu7 Cu 1.31467(16) 0.70929(10) 0.96570(6) 0.0772(5) Uani 1 1 d . . . Cu6B Cu 1.624(2) 0.4826(7) 0.0184(6) 0.096(5) Uani 0.206(7) 1 d P . 2 N1 N 0.0195(9) 0.0324(4) -0.0062(5) 0.048(2) Uani 0.50 1 d P . . N2 N 0.7323(11) 0.0951(6) 0.0369(5) 0.050(3) Uani 1 1 d . . . N3 N 1.0011(9) 0.2481(5) 0.0042(4) 0.0496(19) Uani 1 1 d . . . N4 N 0.0782(7) 0.1349(4) 0.8466(4) 0.0389(17) Uani 1 1 d . . . N5 N 0.4479(7) 0.0376(4) 0.1432(3) 0.0352(16) Uani 1 1 d . . . N6 N 0.0040(8) 0.1665(5) 0.1602(4) 0.0475(19) Uani 1 1 d . . . N7 N 1.1942(7) 0.4408(4) 0.1453(3) 0.0396(17) Uani 1 1 d . . . N8 N 0.8341(8) 0.6432(5) 0.1639(4) 0.0461(19) Uani 1 1 d . . . N9 N 1.2932(8) 0.7067(5) 0.8596(4) 0.048(2) Uani 1 1 d . . . N10 N 1.3361(8) 0.7230(5) 1.0718(4) 0.0428(18) Uani 1 1 d . . . O1 O -0.0464(5) 0.0393(3) 0.5767(3) 0.0358(13) Uani 1 1 d . . . O2 O 0.1738(5) 0.0866(3) 0.5953(3) 0.0301(12) Uani 1 1 d . . . O3 O 0.5518(5) 0.0091(3) 0.4195(3) 0.0313(12) Uani 1 1 d . . . O4 O 0.3316(5) 0.0451(3) 0.3904(3) 0.0336(13) Uani 1 1 d . . . O5 O 0.2233(7) 0.2520(3) 0.4271(3) 0.0521(17) Uani 1 1 d . . . O6 O 0.1130(5) 0.1318(3) 0.4367(3) 0.0368(13) Uani 1 1 d . . . O7 O 1.3733(5) 0.4937(3) 0.4200(3) 0.0315(12) Uani 1 1 d . . . O8 O 1.5546(5) 0.4423(3) 0.3852(3) 0.0338(13) Uani 1 1 d . . . O9 O 1.0842(5) 0.5863(3) 0.4225(3) 0.0326(13) Uani 1 1 d . . . O10 O 0.8745(5) 0.5281(3) 0.4146(3) 0.0332(13) Uani 1 1 d . . . O11 O 1.1881(5) 0.6389(3) 0.5830(3) 0.0332(13) Uani 1 1 d . . . O12 O 1.3242(7) 0.7546(3) 0.5971(3) 0.0469(16) Uani 1 1 d . . . O13 O 1.5264(9) 0.7955(5) 1.3399(3) 0.089(3) Uani 1 1 d . . . O14 O 1.3541(8) 0.7024(5) 1.3435(3) 0.077(2) Uani 1 1 d . . . O15W O 1.3771(5) 0.6546(3) 0.4812(3) 0.0325(13) Uani 1 1 d . . . H15A H 1.3936 0.6962 0.5117 0.039 Uiso 1 1 d R . . H15B H 1.3668 0.6739 0.4383 0.039 Uiso 1 1 d R . . O16W O 1.3574(4) 0.3986(2) 0.5458(2) 0.0446(15) Uani 1 1 d . . . H16A H 1.2996 0.3574 0.5420 0.054 Uiso 1 1 d R . . H16B H 1.4342 0.3805 0.5408 0.054 Uiso 1 1 d R . . O17W O 1.1090(4) 0.4122(2) 0.4297(2) 0.0350(13) Uani 1 1 d R . . H17A H 1.0425 0.3848 0.4412 0.042 Uiso 1 1 d R . . H17B H 1.1839 0.3891 0.4485 0.042 Uiso 1 1 d R . . O18W O 0.4023(5) 0.1472(3) 0.5249(3) 0.0345(13) Uani 1 1 d . . . H18A H 0.3780 0.1895 0.5002 0.041 Uiso 1 1 d R . . H18B H 0.4352 0.1655 0.5696 0.041 Uiso 1 1 d R . . O19W O 0.3075(6) -0.1115(3) 0.4508(3) 0.0448(15) Uani 1 1 d . . . H19A H 0.2773 -0.1591 0.4589 0.054 Uiso 1 1 d R . . H19B H 0.3578 -0.0924 0.4922 0.054 Uiso 1 1 d R . . O20W O 0.1775(5) -0.0884(3) 0.5740(3) 0.0339(13) Uani 1 1 d . . . H20A H 0.0920 -0.1016 0.5707 0.041 Uiso 1 1 d R . . H20B H 0.2183 -0.1337 0.5804 0.041 Uiso 1 1 d R . . O21W O 0.1972(8) 0.2718(4) 0.5860(4) 0.077(2) Uani 1 1 d . . . H21A H 0.1985 0.2333 0.5561 0.093 Uiso 1 1 d R . . H21B H 0.2605 0.2691 0.6237 0.093 Uiso 1 1 d R . . O22W O 0.0995(9) 0.7682(4) 0.4457(5) 0.100(3) Uani 1 1 d . . . H22A H 0.0553 0.7465 0.4753 0.120 Uiso 1 1 d R . . H22B H 0.0952 0.7313 0.4111 0.120 Uiso 1 1 d R . . Tb1 Tb 1.25840(4) 0.52773(2) 0.510387(18) 0.02237(10) Uani 1 1 d . . . Tb2 Tb 0.24893(4) 0.02120(2) 0.496984(18) 0.02226(10) 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 0.050(5) 0.039(5) 0.058(5) 0.009(5) 0.019(4) 0.012(4) C2 0.072(10) 0.049(8) 0.039(7) 0.022(6) 0.041(7) 0.020(6) C3 0.046(5) 0.038(5) 0.026(4) 0.009(4) 0.010(4) 0.007(4) C4 0.044(6) 0.068(6) 0.031(5) -0.007(5) 0.019(4) -0.006(5) C5 0.026(4) 0.058(6) 0.029(4) -0.002(4) 0.007(3) -0.004(4) C6 0.028(4) 0.030(4) 0.021(4) -0.001(3) 0.011(3) 0.004(3) C7 0.028(4) 0.041(5) 0.017(4) -0.007(3) 0.005(3) -0.005(3) C8 0.042(5) 0.048(5) 0.029(5) -0.006(4) 0.004(4) -0.006(4) C9 0.037(5) 0.021(4) 0.019(4) 0.001(3) 0.010(3) 0.004(3) C10 0.033(5) 0.057(5) 0.021(4) 0.004(4) 0.013(4) 0.004(4) C11 0.026(4) 0.051(5) 0.027(4) 0.008(4) 0.005(3) 0.005(4) C12 0.028(4) 0.029(4) 0.015(4) 0.004(3) 0.006(3) -0.001(3) C13 0.035(5) 0.063(6) 0.016(4) 0.012(4) 0.008(3) 0.011(4) C14 0.037(5) 0.083(7) 0.017(4) 0.006(4) 0.005(4) 0.014(5) C15 0.029(4) 0.028(4) 0.016(4) 0.004(3) 0.013(3) 0.002(3) C16 0.061(6) 0.054(6) 0.039(5) 0.014(5) 0.008(5) -0.021(5) C17 0.059(6) 0.053(6) 0.025(5) 0.008(4) -0.002(4) -0.020(5) C18 0.034(5) 0.034(4) 0.029(4) 0.003(4) 0.008(4) 0.008(4) C19 0.043(5) 0.047(5) 0.030(5) 0.003(4) 0.016(4) -0.013(4) C20 0.042(5) 0.060(6) 0.030(5) 0.002(4) 0.000(4) -0.019(5) C21 0.043(5) 0.034(5) 0.027(4) 0.006(4) 0.010(4) 0.011(4) C22 0.037(5) 0.052(5) 0.027(5) 0.000(4) 0.006(4) 0.002(4) C23 0.033(5) 0.045(5) 0.023(4) -0.004(4) 0.004(3) 0.004(4) C24 0.033(4) 0.027(4) 0.019(4) 0.001(3) 0.002(3) -0.001(3) C25 0.037(5) 0.076(7) 0.023(4) -0.006(4) 0.004(4) 0.016(5) C26 0.050(6) 0.091(8) 0.028(5) -0.013(5) 0.008(4) 0.019(6) C27 0.026(4) 0.025(4) 0.023(4) -0.002(3) 0.003(3) -0.009(3) C28 0.049(6) 0.047(5) 0.037(5) 0.011(4) 0.017(4) -0.004(4) C29 0.041(5) 0.037(5) 0.036(5) 0.003(4) 0.013(4) 0.007(4) C30 0.032(4) 0.032(4) 0.026(4) 0.003(3) 0.012(3) 0.003(3) C31 0.039(5) 0.069(6) 0.031(5) 0.006(4) 0.007(4) -0.013(5) C32 0.050(6) 0.089(8) 0.027(5) -0.005(5) -0.003(4) -0.005(6) C33 0.034(5) 0.022(4) 0.021(4) -0.006(3) 0.007(3) 0.000(3) C34 0.067(7) 0.093(8) 0.024(5) 0.002(5) 0.013(5) -0.027(6) C35 0.059(6) 0.065(6) 0.029(5) 0.000(4) 0.011(4) -0.025(5) C36 0.030(4) 0.029(4) 0.025(4) -0.005(3) 0.006(3) 0.003(3) C37 0.065(7) 0.051(6) 0.029(5) -0.006(4) 0.014(4) -0.015(5) C38 0.060(7) 0.065(7) 0.028(5) -0.017(5) -0.005(4) -0.012(5) C39 0.039(5) 0.030(4) 0.026(4) 0.001(4) 0.006(4) 0.005(4) C40 0.057(7) 0.090(8) 0.031(5) 0.027(5) 0.004(5) -0.007(6) C41 0.065(7) 0.053(6) 0.031(5) 0.002(4) 0.005(4) -0.026(5) C42 0.038(5) 0.042(5) 0.022(4) -0.001(4) 0.005(3) -0.014(4) C43 0.076(7) 0.046(5) 0.029(5) 0.004(4) 0.006(5) -0.028(5) C44 0.086(8) 0.054(6) 0.033(6) -0.007(5) 0.000(5) -0.018(6) C45 0.060(7) 0.078(7) 0.024(5) -0.005(5) 0.001(4) -0.027(6) Cl1 0.0540(15) 0.0507(14) 0.0435(13) 0.0012(11) 0.0038(11) 0.0039(11) Cl2 0.0506(13) 0.0394(12) 0.0328(11) 0.0042(9) 0.0090(9) 0.0018(10) Cl3 0.074(2) 0.0712(18) 0.0694(18) 0.0072(15) 0.0228(15) 0.0154(15) Cu1 0.0771(9) 0.0645(8) 0.0314(6) -0.0014(6) 0.0214(6) -0.0182(7) Cu2 0.0479(7) 0.0520(7) 0.0246(5) -0.0022(5) 0.0156(5) -0.0035(5) Cu3 0.0544(8) 0.0868(10) 0.0331(6) 0.0096(6) 0.0057(5) -0.0272(7) Cu4 0.0702(8) 0.0482(7) 0.0304(6) -0.0034(5) -0.0062(5) 0.0037(6) Cu5 0.0744(10) 0.1158(12) 0.0317(7) 0.0015(7) 0.0141(6) -0.0233(9) Cu6 0.082(6) 0.058(2) 0.054(2) 0.0003(16) 0.020(2) -0.009(2) Cu7 0.0917(11) 0.1220(13) 0.0178(6) 0.0002(7) 0.0101(6) 0.0214(9) Cu6B 0.119(15) 0.103(7) 0.070(6) -0.020(5) 0.042(7) -0.027(7) N1 0.050(5) 0.039(5) 0.058(5) 0.009(5) 0.019(4) 0.012(4) N2 0.071(8) 0.062(8) 0.016(4) -0.010(5) 0.002(5) 0.029(5) N3 0.063(5) 0.046(5) 0.040(5) 0.002(4) 0.009(4) 0.009(4) N4 0.042(4) 0.048(4) 0.029(4) -0.001(3) 0.016(3) -0.005(3) N5 0.036(4) 0.053(4) 0.019(3) 0.005(3) 0.010(3) 0.007(3) N6 0.051(5) 0.058(5) 0.030(4) 0.006(4) 0.006(3) -0.015(4) N7 0.047(5) 0.047(4) 0.022(4) -0.001(3) 0.002(3) 0.004(4) N8 0.060(5) 0.062(5) 0.019(4) 0.010(3) 0.014(4) 0.006(4) N9 0.060(5) 0.057(5) 0.026(4) 0.000(4) 0.006(4) 0.007(4) N10 0.047(5) 0.062(5) 0.018(4) -0.001(4) 0.004(3) 0.006(4) O1 0.030(3) 0.048(3) 0.026(3) -0.009(3) 0.001(2) -0.002(3) O2 0.034(3) 0.039(3) 0.022(3) -0.003(2) 0.019(2) -0.002(2) O3 0.026(3) 0.049(3) 0.018(3) 0.006(2) 0.003(2) 0.004(3) O4 0.030(3) 0.055(4) 0.020(3) 0.003(3) 0.013(2) 0.004(3) O5 0.076(5) 0.034(3) 0.035(4) -0.004(3) -0.006(3) -0.007(3) O6 0.034(3) 0.042(3) 0.037(3) 0.009(3) 0.014(3) 0.005(3) O7 0.031(3) 0.047(3) 0.019(3) -0.006(2) 0.010(2) 0.002(3) O8 0.030(3) 0.047(3) 0.024(3) -0.003(2) 0.005(2) 0.004(3) O9 0.029(3) 0.034(3) 0.029(3) 0.002(2) -0.003(2) -0.004(2) O10 0.031(3) 0.042(3) 0.028(3) 0.004(2) 0.012(2) -0.003(3) O11 0.034(3) 0.036(3) 0.027(3) -0.011(2) 0.004(2) -0.001(2) O12 0.072(5) 0.040(3) 0.031(3) 0.001(3) 0.020(3) -0.011(3) O13 0.120(7) 0.108(6) 0.026(4) -0.012(4) 0.001(4) -0.053(6) O14 0.088(6) 0.114(6) 0.028(4) 0.008(4) 0.019(4) -0.043(5) O15W 0.048(3) 0.030(3) 0.019(3) -0.001(2) 0.009(2) -0.009(2) O16W 0.023(3) 0.034(3) 0.077(4) -0.002(3) 0.012(3) 0.003(2) O17W 0.027(3) 0.032(3) 0.045(3) -0.001(3) 0.008(2) -0.002(2) O18W 0.039(3) 0.036(3) 0.024(3) 0.002(2) 0.000(2) -0.003(3) O19W 0.048(4) 0.040(3) 0.051(4) -0.007(3) 0.022(3) 0.004(3) O20W 0.028(3) 0.038(3) 0.038(3) 0.004(3) 0.011(2) 0.003(2) O21W 0.098(6) 0.055(4) 0.095(6) 0.003(4) 0.052(5) 0.012(4) O22W 0.101(7) 0.042(4) 0.143(8) -0.001(5) 0.001(6) 0.001(4) Tb1 0.0214(2) 0.0287(2) 0.01726(19) 0.00042(15) 0.00558(14) -0.00088(15) Tb2 0.0210(2) 0.0320(2) 0.01445(18) -0.00021(15) 0.00595(14) 0.00001(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.151(15) 2 ? C1 C1 1.151(15) 2 ? C1 Cu1 1.892(8) . ? C2 N2 0.818(12) . ? C2 Cu2 2.174(13) 2_655 ? C2 Cu2 2.206(12) . ? C3 N3 1.145(10) . ? C3 Cu5 1.941(9) . ? C3 Cu4 2.019(9) . ? C4 N4 1.331(10) . ? C4 C5 1.384(10) . ? C4 H4 0.9300 . ? C5 C6 1.383(10) . ? C5 H5 0.9300 . ? C6 C7 1.376(10) . ? C6 C9 1.516(9) . ? C7 C8 1.376(10) . ? C7 H7 0.9300 . ? C8 N4 1.338(10) . ? C8 H8 0.9300 . ? C9 O2 1.246(8) . ? C9 O1 1.252(8) . ? C10 N5 1.321(9) . ? C10 C11 1.376(10) . ? C10 H10 0.9300 . ? C11 C12 1.370(10) . ? C11 H11 0.9300 . ? C12 C13 1.393(10) . ? C12 C15 1.502(9) . ? C13 C14 1.374(10) . ? C13 H13 0.9300 . ? C14 N5 1.341(10) . ? C14 H14 0.9300 . ? C15 O3 1.245(8) . ? C15 O4 1.253(8) . ? C16 N6 1.338(10) . ? C16 C17 1.376(11) . ? C16 H16 0.9300 . ? C17 C18 1.395(11) . ? C17 H17 0.9300 . ? C18 C19 1.370(11) . ? C18 C21 1.514(10) . ? C19 C20 1.377(11) . ? C19 H19 0.9300 . ? C20 N6 1.335(10) . ? C20 H20 0.9300 . ? C21 O5 1.232(9) . ? C21 O6 1.270(9) . ? C22 N7 1.323(10) . ? C22 C23 1.371(10) . ? C22 H22 0.9300 . ? C23 C24 1.386(10) . ? C23 H23 0.9300 . ? C24 C25 1.394(10) . ? C24 C27 1.504(9) . ? C25 C26 1.368(11) . ? C25 H25 0.9300 . ? C26 N7 1.336(11) . ? C26 H26 0.9300 . ? C27 O8 1.233(8) . ? C27 O7 1.260(8) . ? C28 N8 1.311(11) . ? C28 C29 1.372(11) . ? C28 H28 0.9300 . ? C29 C30 1.386(11) . ? C29 H29 0.9300 . ? C30 C31 1.372(11) . ? C30 C33 1.482(10) . ? C31 C32 1.380(12) . ? C31 H31 0.9300 . ? C32 N8 1.353(12) . ? C32 H32 0.9300 . ? C33 O10 1.249(9) . ? C33 O9 1.262(8) . ? C34 N9 1.329(11) . ? C34 C35 1.382(11) . ? C34 H34 0.9300 . ? C35 C36 1.358(11) . ? C35 H35 0.9300 . ? C36 C37 1.374(11) . ? C36 C39 1.522(10) . ? C37 C38 1.394(11) . ? C37 H37 0.9300 . ? C38 N9 1.327(12) . ? C38 H38 0.9300 . ? C39 O12 1.241(9) . ? C39 O11 1.267(9) . ? C40 N10 1.308(12) . ? C40 C41 1.394(12) . ? C40 H40 0.9300 . ? C41 C42 1.370(11) . ? C41 H41 0.9300 . ? C42 C43 1.358(11) . ? C42 C45 1.529(11) . ? C43 C44 1.368(11) . ? C43 H43 0.9300 . ? C44 N10 1.334(11) . ? C44 H44 0.9300 . ? C45 O14 1.241(11) . ? C45 O13 1.247(11) . ? Cl1 Cu2 2.285(3) . ? Cl1 Cu1 2.332(3) . ? Cl2 Cu6B 2.22(2) 1_455 ? Cl2 Cu4 2.423(3) . ? Cl2 Cu4 2.438(2) 2_765 ? Cl3 Cu6 2.054(3) . ? Cl3 Cu5 2.307(3) . ? Cl3 Cu6B 2.377(14) 2_865 ? Cl3 Cu6B 2.427(12) . ? Cu1 N4 2.046(7) 1_554 ? Cu1 Cu3 2.7859(18) 1_455 ? Cu2 N5 2.041(6) . ? Cu2 C2 2.174(13) 2_655 ? Cu2 Cu2 2.391(2) 2_655 ? Cu3 N3 1.895(9) . ? Cu3 N2 2.042(11) . ? Cu3 N6 2.082(7) 1_655 ? Cu3 Cu1 2.7860(18) 1_655 ? Cu4 N7 2.035(6) . ? Cu4 Cl2 2.438(2) 2_765 ? Cu4 Cu5 2.5040(19) . ? Cu5 N8 2.014(7) 2_765 ? Cu5 Cu6B 3.049(10) 2_865 ? Cu6 Cl3 2.054(3) 2_865 ? Cu7 N9 1.917(7) . ? Cu7 N10 1.923(6) . ? Cu6B Cl2 2.22(2) 1_655 ? Cu6B Cl3 2.377(14) 2_865 ? Cu6B Cu6B 2.49(4) 2_865 ? Cu6B Cu5 3.050(10) 2_865 ? N4 Cu1 2.046(7) 1_556 ? N6 Cu3 2.083(7) 1_455 ? N8 Cu5 2.014(7) 2_765 ? O1 Tb2 2.298(5) 2_556 ? O2 Tb2 2.352(4) . ? O3 Tb2 2.284(5) 2_656 ? O4 Tb2 2.338(5) . ? O6 Tb2 2.431(5) . ? O7 Tb1 2.293(5) . ? O8 Tb1 2.356(5) 2_866 ? O9 Tb1 2.333(5) . ? O10 Tb1 2.301(5) 2_766 ? O11 Tb1 2.429(5) . ? O15W Tb1 2.463(5) . ? O15W H15A 0.8471 . ? O15W H15B 0.8466 . ? O16W Tb1 2.397(4) . ? O16W H16A 0.8499 . ? O16W H16B 0.8500 . ? O17W Tb1 2.537(4) . ? O17W H17A 0.8499 . ? O17W H17B 0.8500 . ? O18W Tb2 2.456(5) . ? O18W H18A 0.8486 . ? O18W H18B 0.8496 . ? O19W Tb2 2.429(5) . ? O19W H19A 0.8461 . ? O19W H19B 0.8474 . ? O20W Tb2 2.493(5) . ? O20W H20A 0.8510 . ? O20W H20B 0.8510 . ? O21W H21A 0.8200 . ? O21W H21B 0.8225 . ? O22W H22A 0.8516 . ? O22W H22B 0.8511 . ? Tb1 O10 2.301(5) 2_766 ? Tb1 O8 2.356(5) 2_866 ? Tb1 H17B 2.4857 . ? Tb2 O3 2.284(5) 2_656 ? Tb2 O1 2.298(5) 2_556 ? Tb2 H19B 2.1831 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C1 0.0(10) 2 2 ? N1 C1 Cu1 166.5(11) 2 . ? C1 C1 Cu1 166.5(11) 2 . ? N2 C2 Cu2 145.9(17) . 2_655 ? N2 C2 Cu2 146.0(18) . . ? Cu2 C2 Cu2 66.2(4) 2_655 . ? N3 C3 Cu5 144.6(8) . . ? N3 C3 Cu4 136.6(7) . . ? Cu5 C3 Cu4 78.4(3) . . ? N4 C4 C5 123.8(8) . . ? N4 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C6 C5 C4 118.9(8) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C7 C6 C5 117.3(7) . . ? C7 C6 C9 120.2(7) . . ? C5 C6 C9 122.5(7) . . ? C6 C7 C8 120.1(7) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? N4 C8 C7 123.0(8) . . ? N4 C8 H8 118.5 . . ? C7 C8 H8 118.5 . . ? O2 C9 O1 125.6(7) . . ? O2 C9 C6 117.2(7) . . ? O1 C9 C6 117.1(7) . . ? N5 C10 C11 123.3(7) . . ? N5 C10 H10 118.3 . . ? C11 C10 H10 118.3 . . ? C12 C11 C10 119.8(7) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 117.3(7) . . ? C11 C12 C15 122.6(7) . . ? C13 C12 C15 120.1(6) . . ? C14 C13 C12 119.5(7) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? N5 C14 C13 122.6(7) . . ? N5 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? O3 C15 O4 126.1(6) . . ? O3 C15 C12 117.7(6) . . ? O4 C15 C12 116.2(6) . . ? N6 C16 C17 125.0(8) . . ? N6 C16 H16 117.5 . . ? C17 C16 H16 117.5 . . ? C16 C17 C18 118.0(8) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C19 C18 C17 117.8(7) . . ? C19 C18 C21 122.2(7) . . ? C17 C18 C21 119.8(8) . . ? C18 C19 C20 119.8(8) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N6 C20 C19 123.8(8) . . ? N6 C20 H20 118.1 . . ? C19 C20 H20 118.1 . . ? O5 C21 O6 125.5(7) . . ? O5 C21 C18 118.0(7) . . ? O6 C21 C18 116.6(7) . . ? N7 C22 C23 123.7(8) . . ? N7 C22 H22 118.2 . . ? C23 C22 H22 118.2 . . ? C22 C23 C24 120.0(7) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 116.4(7) . . ? C23 C24 C27 122.8(7) . . ? C25 C24 C27 120.9(7) . . ? C26 C25 C24 119.4(8) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? N7 C26 C25 123.9(8) . . ? N7 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? O8 C27 O7 126.6(7) . . ? O8 C27 C24 117.6(7) . . ? O7 C27 C24 115.7(7) . . ? N8 C28 C29 123.2(8) . . ? N8 C28 H28 118.4 . . ? C29 C28 H28 118.4 . . ? C28 C29 C30 119.9(8) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 117.2(8) . . ? C31 C30 C33 121.3(7) . . ? C29 C30 C33 121.4(7) . . ? C30 C31 C32 119.9(8) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? N8 C32 C31 122.0(9) . . ? N8 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? O10 C33 O9 123.6(7) . . ? O10 C33 C30 118.5(7) . . ? O9 C33 C30 117.9(7) . . ? N9 C34 C35 122.8(9) . . ? N9 C34 H34 118.6 . . ? C35 C34 H34 118.6 . . ? C36 C35 C34 121.0(9) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 116.3(8) . . ? C35 C36 C39 122.2(7) . . ? C37 C36 C39 121.4(7) . . ? C36 C37 C38 120.4(8) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? N9 C38 C37 122.4(8) . . ? N9 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? O12 C39 O11 125.8(7) . . ? O12 C39 C36 116.8(7) . . ? O11 C39 C36 117.4(7) . . ? N10 C40 C41 123.7(9) . . ? N10 C40 H40 118.1 . . ? C41 C40 H40 118.1 . . ? C42 C41 C40 118.3(9) . . ? C42 C41 H41 120.8 . . ? C40 C41 H41 120.8 . . ? C43 C42 C41 118.0(7) . . ? C43 C42 C45 122.0(8) . . ? C41 C42 C45 119.9(8) . . ? C42 C43 C44 120.0(8) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? N10 C44 C43 122.9(9) . . ? N10 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? O14 C45 O13 128.6(9) . . ? O14 C45 C42 116.3(8) . . ? O13 C45 C42 115.0(8) . . ? Cu2 Cl1 Cu1 101.86(10) . . ? Cu6B Cl2 Cu4 162.0(2) 1_455 . ? Cu6B Cl2 Cu4 101.3(3) 1_455 2_765 ? Cu4 Cl2 Cu4 80.28(8) . 2_765 ? Cu6 Cl3 Cu5 112.59(13) . . ? Cu6 Cl3 Cu6B 31.6(4) . 2_865 ? Cu5 Cl3 Cu6B 81.2(4) . 2_865 ? Cu6 Cl3 Cu6B 30.8(5) . . ? Cu5 Cl3 Cu6B 143.1(5) . . ? Cu6B Cl3 Cu6B 62.4(8) 2_865 . ? C1 Cu1 N4 118.3(3) . 1_554 ? C1 Cu1 Cl1 123.8(3) . . ? N4 Cu1 Cl1 103.6(2) 1_554 . ? C1 Cu1 Cu3 63.8(2) . 1_455 ? N4 Cu1 Cu3 127.2(2) 1_554 1_455 ? Cl1 Cu1 Cu3 117.60(8) . 1_455 ? N5 Cu2 C2 109.5(4) . 2_655 ? N5 Cu2 C2 104.1(4) . . ? C2 Cu2 C2 113.8(4) 2_655 . ? N5 Cu2 Cl1 102.1(2) . . ? C2 Cu2 Cl1 116.9(4) 2_655 . ? C2 Cu2 Cl1 109.1(3) . . ? N5 Cu2 Cu2 121.8(2) . 2_655 ? C2 Cu2 Cu2 57.6(3) 2_655 2_655 ? C2 Cu2 Cu2 56.3(3) . 2_655 ? Cl1 Cu2 Cu2 135.43(9) . 2_655 ? N3 Cu3 N2 142.2(4) . . ? N3 Cu3 N6 107.2(3) . 1_655 ? N2 Cu3 N6 103.0(3) . 1_655 ? N3 Cu3 Cu1 61.1(2) . 1_655 ? N2 Cu3 Cu1 124.3(3) . 1_655 ? N6 Cu3 Cu1 114.2(2) 1_655 1_655 ? C3 Cu4 N7 114.8(3) . . ? C3 Cu4 Cl2 108.7(3) . . ? N7 Cu4 Cl2 104.4(2) . . ? C3 Cu4 Cl2 115.1(2) . 2_765 ? N7 Cu4 Cl2 112.4(2) . 2_765 ? Cl2 Cu4 Cl2 99.72(8) . 2_765 ? C3 Cu4 Cu5 49.4(2) . . ? N7 Cu4 Cu5 115.8(2) . . ? Cl2 Cu4 Cu5 139.33(7) . . ? Cl2 Cu4 Cu5 71.02(7) 2_765 . ? C3 Cu5 N8 121.4(3) . 2_765 ? C3 Cu5 Cl3 129.1(3) . . ? N8 Cu5 Cl3 106.4(2) 2_765 . ? C3 Cu5 Cu4 52.2(3) . . ? N8 Cu5 Cu4 132.0(2) 2_765 . ? Cl3 Cu5 Cu4 107.33(9) . . ? C3 Cu5 Cu6B 131.4(3) . 2_865 ? N8 Cu5 Cu6B 96.4(3) 2_765 2_865 ? Cl3 Cu5 Cu6B 50.4(4) . 2_865 ? Cu4 Cu5 Cu6B 80.2(2) . 2_865 ? Cl3 Cu6 Cl3 179.999(1) . 2_865 ? N9 Cu7 N10 174.6(3) . . ? Cl2 Cu6B Cl3 111.4(4) 1_655 2_865 ? Cl2 Cu6B Cl3 130.8(6) 1_655 . ? Cl3 Cu6B Cl3 117.6(8) 2_865 . ? Cl2 Cu6B Cu6B 170.2(7) 1_655 2_865 ? Cl3 Cu6B Cu6B 59.8(6) 2_865 2_865 ? Cl3 Cu6B Cu6B 57.8(5) . 2_865 ? Cl2 Cu6B Cu5 63.8(3) 1_655 2_865 ? Cl3 Cu6B Cu5 48.39(18) 2_865 2_865 ? Cl3 Cu6B Cu5 165.0(8) . 2_865 ? Cu6B Cu6B Cu5 107.9(6) 2_865 2_865 ? C2 N2 Cu3 170.1(18) . . ? C3 N3 Cu3 164.7(7) . . ? C4 N4 C8 116.7(7) . . ? C4 N4 Cu1 121.3(6) . 1_556 ? C8 N4 Cu1 120.1(6) . 1_556 ? C10 N5 C14 117.5(6) . . ? C10 N5 Cu2 123.7(5) . . ? C14 N5 Cu2 118.7(5) . . ? C20 N6 C16 115.6(7) . . ? C20 N6 Cu3 120.1(6) . 1_455 ? C16 N6 Cu3 124.0(6) . 1_455 ? C22 N7 C26 116.6(7) . . ? C22 N7 Cu4 122.0(6) . . ? C26 N7 Cu4 121.4(6) . . ? C28 N8 C32 117.7(7) . . ? C28 N8 Cu5 119.1(6) . 2_765 ? C32 N8 Cu5 121.0(6) . 2_765 ? C38 N9 C34 117.1(8) . . ? C38 N9 Cu7 120.2(6) . . ? C34 N9 Cu7 122.7(7) . . ? C40 N10 C44 117.0(7) . . ? C40 N10 Cu7 120.8(6) . . ? C44 N10 Cu7 122.1(6) . . ? C9 O1 Tb2 177.6(5) . 2_556 ? C9 O2 Tb2 129.4(5) . . ? C15 O3 Tb2 177.6(5) . 2_656 ? C15 O4 Tb2 131.1(5) . . ? C21 O6 Tb2 129.7(5) . . ? C27 O7 Tb1 171.2(5) . . ? C27 O8 Tb1 130.0(5) . 2_866 ? C33 O9 Tb1 138.7(5) . . ? C33 O10 Tb1 165.5(5) . 2_766 ? C39 O11 Tb1 130.5(5) . . ? Tb1 O15W H15A 120.7 . . ? Tb1 O15W H15B 125.5 . . ? H15A O15W H15B 105.7 . . ? Tb1 O16W H16A 115.6 . . ? Tb1 O16W H16B 129.1 . . ? H16A O16W H16B 107.7 . . ? Tb1 O17W H17A 125.1 . . ? Tb1 O17W H17B 76.8 . . ? H17A O17W H17B 107.7 . . ? Tb2 O18W H18A 118.3 . . ? Tb2 O18W H18B 121.1 . . ? H18A O18W H18B 105.3 . . ? Tb2 O19W H19A 127.8 . . ? Tb2 O19W H19B 63.3 . . ? H19A O19W H19B 106.0 . . ? Tb2 O20W H20A 121.1 . . ? Tb2 O20W H20B 122.0 . . ? H20A O20W H20B 105.0 . . ? H21A O21W H21B 110.6 . . ? H22A O22W H22B 105.0 . . ? O7 Tb1 O10 142.73(19) . 2_766 ? O7 Tb1 O9 90.95(18) . . ? O10 Tb1 O9 99.50(19) 2_766 . ? O7 Tb1 O8 101.50(18) . 2_866 ? O10 Tb1 O8 90.82(18) 2_766 2_866 ? O9 Tb1 O8 143.94(18) . 2_866 ? O7 Tb1 O16W 75.18(16) . . ? O10 Tb1 O16W 74.94(16) 2_766 . ? O9 Tb1 O16W 142.56(15) . . ? O8 Tb1 O16W 73.48(16) 2_866 . ? O7 Tb1 O11 146.08(19) . . ? O10 Tb1 O11 71.14(18) 2_766 . ? O9 Tb1 O11 77.37(17) . . ? O8 Tb1 O11 73.50(17) 2_866 . ? O16W Tb1 O11 131.56(15) . . ? O7 Tb1 O15W 72.06(17) . . ? O10 Tb1 O15W 145.11(17) 2_766 . ? O9 Tb1 O15W 77.22(17) . . ? O8 Tb1 O15W 74.81(18) 2_866 . ? O16W Tb1 O15W 127.96(15) . . ? O11 Tb1 O15W 74.30(17) . . ? O7 Tb1 O17W 74.35(15) . . ? O10 Tb1 O17W 75.34(16) 2_766 . ? O9 Tb1 O17W 71.47(15) . . ? O8 Tb1 O17W 144.44(16) 2_866 . ? O16W Tb1 O17W 71.33(10) . . ? O11 Tb1 O17W 128.97(15) . . ? O15W Tb1 O17W 133.03(14) . . ? O7 Tb1 H17B 66.6 . . ? O10 Tb1 H17B 77.7 2_766 . ? O9 Tb1 H17B 89.8 . . ? O8 Tb1 H17B 126.2 2_866 . ? O16W Tb1 H17B 52.7 . . ? O11 Tb1 H17B 143.5 . . ? O15W Tb1 H17B 136.4 . . ? O17W Tb1 H17B 19.4 . . ? O3 Tb2 O1 142.07(19) 2_656 2_556 ? O3 Tb2 O4 101.46(18) 2_656 . ? O1 Tb2 O4 89.89(18) 2_556 . ? O3 Tb2 O2 88.92(18) 2_656 . ? O1 Tb2 O2 103.09(18) 2_556 . ? O4 Tb2 O2 143.71(18) . . ? O3 Tb2 O19W 75.67(19) 2_656 . ? O1 Tb2 O19W 73.41(19) 2_556 . ? O4 Tb2 O19W 72.82(19) . . ? O2 Tb2 O19W 143.26(18) . . ? O3 Tb2 O6 144.96(19) 2_656 . ? O1 Tb2 O6 72.88(19) 2_556 . ? O4 Tb2 O6 75.01(18) . . ? O2 Tb2 O6 76.75(18) . . ? O19W Tb2 O6 132.76(19) . . ? O3 Tb2 O18W 71.81(18) 2_656 . ? O1 Tb2 O18W 145.65(18) 2_556 . ? O4 Tb2 O18W 73.23(17) . . ? O2 Tb2 O18W 77.39(17) . . ? O19W Tb2 O18W 126.27(18) . . ? O6 Tb2 O18W 73.90(18) . . ? O3 Tb2 O20W 74.48(18) 2_656 . ? O1 Tb2 O20W 75.36(18) 2_556 . ? O4 Tb2 O20W 144.14(17) . . ? O2 Tb2 O20W 72.11(17) . . ? O19W Tb2 O20W 71.68(18) . . ? O6 Tb2 O20W 128.35(17) . . ? O18W Tb2 O20W 134.38(16) . . ? O3 Tb2 H19B 55.5 2_656 . ? O1 Tb2 H19B 91.6 2_556 . ? O4 Tb2 H19B 81.2 . . ? O2 Tb2 H19B 131.1 . . ? O19W Tb2 H19B 20.3 . . ? O6 Tb2 H19B 151.4 . . ? O18W Tb2 H19B 114.3 . . ? O20W Tb2 H19B 67.0 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.698 _refine_diff_density_min -1.245 _refine_diff_density_rms 0.158 _database_code_depnum_ccdc_archive 'CCDC 964396' ####################################################################### # # 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_II-B #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C89 H80 Cl6 Cu13 Dy4 N19 O40, 4(H2 O)' _chemical_formula_sum 'C89 H88 Cl6 Cu13 Dy4 N19 O44' _chemical_formula_weight 3816.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.914(2) _cell_length_b 16.143(3) _cell_length_c 18.407(4) _cell_angle_alpha 92.009(2) _cell_angle_beta 103.583(2) _cell_angle_gamma 91.941(2) _cell_volume 2859.0(10) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10347 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 25.40 _exptl_crystal_description orange _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1850 _exptl_absorpt_coefficient_mu 5.173 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.355 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15074 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.40 _reflns_number_total 10347 _reflns_number_gt 7914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0410P)^2^+9.6109P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10347 _refine_ls_number_parameters 813 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 -0.4806(9) 0.5323(5) -0.0068(5) 0.048(2) Uani 0.50 1 d P . . C2 C 0.1580(11) 0.5612(7) 0.0279(5) 0.045(2) Uani 1 1 d . . . C3 C 0.5587(10) 0.8087(6) -0.0041(5) 0.041(2) Uani 1 1 d U A . C4 C -0.4575(10) 0.3906(6) 0.2008(5) 0.047(2) Uani 1 1 d . . . H4 H -0.3789 0.3964 0.1817 0.056 Uiso 1 1 calc R . . C5 C -0.4439(8) 0.4080(5) 0.2769(5) 0.039(2) Uani 1 1 d . . . H5 H -0.3585 0.4252 0.3079 0.047 Uiso 1 1 calc R . . C6 C -0.5620(8) 0.3989(5) 0.3056(4) 0.0286(17) Uani 1 1 d . . . C7 C -0.6842(8) 0.3686(5) 0.2569(4) 0.036(2) Uani 1 1 d . . . H7 H -0.7635 0.3587 0.2745 0.043 Uiso 1 1 calc R . . C8 C -0.6877(10) 0.3532(5) 0.1827(5) 0.043(2) Uani 1 1 d . . . H8 H -0.7704 0.3327 0.1510 0.051 Uiso 1 1 calc R . . C9 C -0.5607(8) 0.4259(5) 0.3850(4) 0.0261(17) Uani 1 1 d . . . C10 C 0.0616(9) 0.5223(6) 0.1938(5) 0.041(2) Uani 1 1 d . A . H10 H 0.1421 0.5123 0.1778 0.050 Uiso 1 1 calc R . . C11 C 0.0656(8) 0.5188(5) 0.2691(4) 0.0316(18) Uani 1 1 d . . . H11 H 0.1476 0.5072 0.3030 0.038 Uiso 1 1 calc R . . C12 C -0.0534(7) 0.5327(4) 0.2937(4) 0.0237(16) Uani 1 1 d . . . C13 C -0.1720(8) 0.5491(6) 0.2404(4) 0.039(2) Uani 1 1 d . . . H13 H -0.2542 0.5588 0.2547 0.046 Uiso 1 1 calc R . . C14 C -0.1685(9) 0.5511(6) 0.1665(4) 0.048(2) Uani 1 1 d . A . H14 H -0.2499 0.5609 0.1315 0.057 Uiso 1 1 calc R . . C15 C -0.0556(8) 0.5285(4) 0.3745(4) 0.0237(16) Uani 1 1 d . . . C16 C -0.3962(10) 0.7251(6) 0.1942(5) 0.053(3) Uani 1 1 d . . . H16 H -0.3545 0.7580 0.1644 0.063 Uiso 1 1 calc R . . C17 C -0.3520(10) 0.7355(6) 0.2702(5) 0.051(3) Uani 1 1 d . . . H17 H -0.2858 0.7771 0.2914 0.061 Uiso 1 1 calc R . . C18 C -0.4066(8) 0.6839(5) 0.3154(4) 0.0323(18) Uani 1 1 d . . . C19 C -0.5095(8) 0.6258(5) 0.2812(4) 0.037(2) Uani 1 1 d . . . H19 H -0.5507 0.5909 0.3096 0.044 Uiso 1 1 calc R . . C20 C -0.5496(9) 0.6206(6) 0.2050(5) 0.045(2) Uani 1 1 d . . . H20 H -0.6178 0.5805 0.1828 0.054 Uiso 1 1 calc R . . C21 C -0.3523(9) 0.6897(5) 0.3990(5) 0.036(2) Uani 1 1 d . . . C22 C 0.6449(9) 0.9681(5) 0.1991(5) 0.038(2) Uani 1 1 d . A . H22 H 0.5526 0.9827 0.1862 0.046 Uiso 1 1 calc R . . C23 C 0.7139(8) 0.9758(5) 0.2734(4) 0.0331(19) Uani 1 1 d . . . H23 H 0.6689 0.9942 0.3096 0.040 Uiso 1 1 calc R . . C24 C 0.8523(7) 0.9556(5) 0.2930(4) 0.0270(17) Uani 1 1 d . . . C25 C 0.9119(9) 0.9285(6) 0.2369(5) 0.049(3) Uani 1 1 d . . . H25 H 1.0048 0.9151 0.2478 0.059 Uiso 1 1 calc R . . C26 C 0.8331(10) 0.9212(7) 0.1642(5) 0.056(3) Uani 1 1 d . A . H26 H 0.8748 0.9014 0.1271 0.067 Uiso 1 1 calc R . . C27 C 0.9344(8) 0.9644(5) 0.3735(4) 0.0257(17) Uani 1 1 d . . . C28 C 1.5416(11) 0.8348(6) 0.7941(5) 0.053(3) Uani 1 1 d . . . H28 H 1.4801 0.8046 0.8152 0.064 Uiso 1 1 calc R . . C29 C 1.4987(10) 0.8569(6) 0.7221(5) 0.048(2) Uani 1 1 d . . . H29 H 1.4088 0.8429 0.6949 0.058 Uiso 1 1 calc R . . C30 C 1.5912(8) 0.9009(5) 0.6893(4) 0.0285(17) Uani 1 1 d . . . C31 C 1.7259(10) 0.9197(6) 0.7295(5) 0.054(3) Uani 1 1 d . . . H31 H 1.7900 0.9477 0.7085 0.065 Uiso 1 1 calc R . . C32 C 1.7609(12) 0.8947(8) 0.8032(6) 0.069(3) Uani 1 1 d . . . H32 H 1.8510 0.9057 0.8316 0.083 Uiso 1 1 calc R . . C33 C 1.5417(8) 0.9308(4) 0.6110(4) 0.0238(16) Uani 1 1 d . . . C34 C 1.2986(12) 0.8475(7) 0.1872(5) 0.065(3) Uani 1 1 d . . . H34 H 1.3553 0.8827 0.1672 0.078 Uiso 1 1 calc R . . C35 C 1.3134(10) 0.8504(6) 0.2645(5) 0.053(3) Uani 1 1 d . . . H35 H 1.3777 0.8878 0.2948 0.063 Uiso 1 1 calc R . . C36 C 1.2336(8) 0.7985(5) 0.2956(4) 0.0281(17) Uani 1 1 d . . . C37 C 1.1394(10) 0.7458(6) 0.2481(5) 0.048(2) Uani 1 1 d . . . H37 H 1.0828 0.7095 0.2671 0.058 Uiso 1 1 calc R . . C38 C 1.1282(11) 0.7464(6) 0.1710(5) 0.056(3) Uani 1 1 d . . . H38 H 1.0630 0.7104 0.1395 0.067 Uiso 1 1 calc R . . C39 C 1.2428(9) 0.8009(5) 0.3792(4) 0.0337(19) Uani 1 1 d . . . C40 C 1.1005(10) 0.7125(7) -0.1085(5) 0.056(3) Uani 1 1 d . . . H40 H 1.0742 0.6704 -0.0807 0.068 Uiso 1 1 calc R . . C41 C 1.0715(10) 0.7006(6) -0.1849(5) 0.052(3) Uani 1 1 d . . . H41 H 1.0248 0.6522 -0.2079 0.063 Uiso 1 1 calc R . . C42 C 1.1116(9) 0.7602(6) -0.2265(4) 0.042(2) Uani 1 1 d . . . C43 C 1.1792(11) 0.8297(6) -0.1891(5) 0.053(3) Uani 1 1 d . . . H43 H 1.2086 0.8722 -0.2154 0.063 Uiso 1 1 calc R . . C44 C 1.2037(12) 0.8370(7) -0.1124(5) 0.063(3) Uani 1 1 d . . . H44 H 1.2511 0.8847 -0.0882 0.076 Uiso 1 1 calc R . . C45 C 1.0819(12) 0.7506(6) -0.3110(5) 0.060(3) Uani 1 1 d . . . Cl1 Cl -0.1609(3) 0.66975(17) 0.00648(14) 0.0607(7) Uani 1 1 d . . . Cl2 Cl 0.6419(2) 1.02906(14) -0.04374(12) 0.0442(5) Uani 1 1 d . . . Cl3 Cl 0.9390(5) 0.8808(3) -0.0041(2) 0.0575(10) Uani 0.666(5) 1 d PU A 1 Cl3B Cl 0.8694(10) 0.8657(6) -0.0401(5) 0.0575(10) Uani 0.334(5) 1 d P A 2 Cu1 Cu -0.3889(4) 0.6207(3) -0.0397(3) 0.0441(9) Uani 0.666(5) 1 d P . 1 Cu2 Cu -0.05730(12) 0.54754(8) 0.03187(6) 0.0479(3) Uani 1 1 d . . . Cu3 Cu 0.41554(13) 0.66211(9) 0.04563(6) 0.0566(4) Uani 1 1 d . . . Cu4 Cu 0.58875(14) 0.92486(7) 0.03676(6) 0.0567(4) Uani 1 1 d . . . Cu5 Cu 0.70240(18) 0.84875(13) -0.05202(8) 0.0961(6) Uani 1 1 d . . . Cu6 Cu 1.0000 1.0000 0.0000 0.342(10) Uani 0.666(5) 2 d SP . 1 Cu7 Cu 1.18466(16) 0.79685(11) 0.03414(7) 0.0791(5) Uani 1 1 d . . . Cu1B Cu -0.4348(13) 0.6383(7) -0.0460(7) 0.078(3) Uani 0.334(5) 1 d P . 2 Cu6B Cu 0.8575(6) 1.0215(6) -0.0227(5) 0.039(2) Uani 0.167(3) 1 d P . 2 Dy1 Dy 1.24302(3) 0.97304(2) 0.490452(18) 0.02267(11) Uani 1 1 d . . . Dy2 Dy -0.25131(3) 0.52038(2) 0.497138(18) 0.02233(11) Uani 1 1 d . . . N1 N -0.4806(9) 0.5323(5) -0.0068(5) 0.048(2) Uani 0.50 1 d P . . N2 N 0.2414(9) 0.6002(6) 0.0370(4) 0.051(2) Uani 1 1 d . . . N3 N 0.5026(8) 0.7488(5) 0.0018(4) 0.052(2) Uani 1 1 d U . . N4 N -0.5779(8) 0.3662(4) 0.1541(4) 0.0415(18) Uani 1 1 d . . . N5 N -0.0530(7) 0.5394(5) 0.1429(3) 0.0371(17) Uani 1 1 d . . . N6 N -0.4974(7) 0.6692(5) 0.1606(4) 0.0456(19) Uani 1 1 d . . . N7 N 0.7019(7) 0.9409(4) 0.1446(3) 0.0383(17) Uani 1 1 d . . . N8 N 1.6673(10) 0.8545(5) 0.8351(4) 0.057(2) Uani 1 1 d . . . N9 N 1.2072(9) 0.7965(5) 0.1410(4) 0.049(2) Uani 1 1 d . . . N10 N 1.1641(8) 0.7807(5) -0.0720(4) 0.0442(19) Uani 1 1 d . . . O1 O -0.4530(5) 0.4602(4) 0.4241(3) 0.0373(14) Uani 1 1 d . . . O2 O -0.6722(5) 0.4145(3) 0.4058(3) 0.0292(12) Uani 1 1 d . . . O3 O 0.0517(5) 0.5102(3) 0.4200(3) 0.0326(13) Uani 1 1 d . . . O4 O -0.1691(6) 0.5431(4) 0.3912(3) 0.0380(14) Uani 1 1 d . . . O5 O -0.2752(7) 0.7510(4) 0.4271(3) 0.0528(18) Uani 1 1 d . . . O6 O -0.3867(5) 0.6319(3) 0.4362(3) 0.0348(13) Uani 1 1 d . . . O7 O 0.8742(5) 0.9936(3) 0.4204(3) 0.0333(13) Uani 1 1 d . . . O8 O 1.0577(5) 0.9436(4) 0.3865(3) 0.0355(13) Uani 1 1 d . . . O9 O 1.4168(5) 0.9149(3) 0.5786(3) 0.0384(14) Uani 1 1 d . . . O10 O 1.6261(5) 0.9713(3) 0.5838(3) 0.0348(13) Uani 1 1 d . . . O11 O 1.3142(5) 0.8629(3) 0.4174(3) 0.0319(13) Uani 1 1 d . . . O12 O 1.1793(7) 0.7461(4) 0.4036(3) 0.0465(16) Uani 1 1 d . . . O13 O 0.9780(11) 0.7016(6) -0.3398(4) 0.108(4) Uani 1 1 d . . . O14 O 1.1498(9) 0.7947(6) -0.3436(4) 0.092(3) Uani 1 1 d . . . O15W O 1.1255(5) 0.8463(3) 0.5193(3) 0.0339(13) Uani 1 1 d . . . H15A H 1.1225 0.8073 0.4867 0.041 Uiso 1 1 d R . . H15B H 1.1631 0.8282 0.5618 0.041 Uiso 1 1 d R . . O16W O 1.1440(5) 1.1042(3) 0.4542(3) 0.0423(15) Uani 1 1 d . . . H16B H 1.0989 1.0651 0.4291 0.051 Uiso 1 1 d R . . H16A H 1.0928 1.1372 0.4674 0.051 Uiso 1 1 d R . . O17W O 1.3887(5) 1.0881(3) 0.5705(3) 0.0346(13) Uani 1 1 d . . . H17A H 1.3518 1.1339 0.5760 0.042 Uiso 1 1 d R . . H17B H 1.4736 1.1011 0.5727 0.042 Uiso 1 1 d R . . O18W O -0.1006(5) 0.6459(3) 0.5254(3) 0.0364(13) Uani 1 1 d . . . H18A H -0.0692 0.6645 0.5683 0.044 Uiso 1 1 d R . . H18B H -0.1322 0.6829 0.4978 0.044 Uiso 1 1 d R . . O19W O -0.1917(6) 0.3866(4) 0.4539(3) 0.0456(15) Uani 1 1 d . . . H19A H -0.2296 0.3431 0.4291 0.055 Uiso 1 1 d R . . H19B H -0.1214 0.4007 0.4374 0.055 Uiso 1 1 d R . . O20W O -0.3228(5) 0.4114(3) 0.5745(3) 0.0316(12) Uani 1 1 d . . . H20A H -0.4012 0.3911 0.5779 0.038 Uiso 1 1 d R . . H20B H -0.2632 0.3748 0.5877 0.038 Uiso 1 1 d R . . O21W O 0.2997(9) 0.2301(5) 0.4113(5) 0.092(3) Uani 1 1 d . . . H21A H 0.2782 0.1792 0.3994 0.111 Uiso 1 1 d R . . H21B H 0.2551 0.2451 0.4433 0.111 Uiso 1 1 d R . . O22W O 0.5964(10) 0.2663(5) 0.4445(6) 0.132(5) Uani 1 1 d . . . H22A H 0.5088 0.2575 0.4338 0.159 Uiso 1 1 d R . . H22B H 0.6135 0.3164 0.4608 0.159 Uiso 1 1 d R . . 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(5) 0.044(5) 0.051(5) 0.006(4) 0.022(4) 0.002(4) C2 0.046(6) 0.068(7) 0.027(5) 0.016(5) 0.018(4) 0.018(5) C3 0.055(6) 0.041(5) 0.029(5) 0.004(4) 0.011(4) 0.015(4) C4 0.051(6) 0.062(6) 0.032(5) -0.002(4) 0.021(4) 0.003(5) C5 0.028(4) 0.059(6) 0.032(5) -0.005(4) 0.012(4) -0.003(4) C6 0.030(4) 0.033(4) 0.026(4) 0.000(3) 0.012(3) 0.007(3) C7 0.028(4) 0.058(6) 0.023(4) -0.006(4) 0.009(3) 0.001(4) C8 0.049(6) 0.050(6) 0.025(4) -0.004(4) 0.005(4) -0.005(4) C9 0.029(4) 0.030(4) 0.017(4) -0.002(3) 0.001(3) 0.004(3) C10 0.035(5) 0.060(6) 0.034(5) 0.002(4) 0.018(4) 0.003(4) C11 0.029(4) 0.047(5) 0.020(4) 0.001(3) 0.007(3) 0.005(4) C12 0.025(4) 0.030(4) 0.018(4) -0.001(3) 0.009(3) 0.001(3) C13 0.022(4) 0.072(6) 0.025(4) 0.010(4) 0.008(3) 0.013(4) C14 0.037(5) 0.090(8) 0.018(4) 0.009(4) 0.008(4) 0.011(5) C15 0.027(4) 0.026(4) 0.019(4) 0.002(3) 0.007(3) -0.003(3) C16 0.057(6) 0.059(6) 0.040(6) 0.017(5) 0.008(5) -0.016(5) C17 0.057(6) 0.056(6) 0.032(5) 0.006(4) 0.000(4) -0.020(5) C18 0.035(5) 0.037(5) 0.025(4) 0.003(3) 0.006(3) 0.007(4) C19 0.033(5) 0.046(5) 0.032(5) 0.011(4) 0.007(4) -0.005(4) C20 0.034(5) 0.067(6) 0.027(5) 0.008(4) -0.002(4) -0.013(4) C21 0.044(5) 0.037(5) 0.031(5) 0.004(4) 0.012(4) 0.019(4) C22 0.033(5) 0.046(5) 0.032(5) 0.002(4) 0.000(4) 0.008(4) C23 0.027(4) 0.051(5) 0.022(4) 0.005(4) 0.005(3) 0.007(4) C24 0.025(4) 0.029(4) 0.024(4) -0.002(3) 0.001(3) 0.001(3) C25 0.037(5) 0.084(7) 0.024(5) -0.006(4) 0.001(4) 0.022(5) C26 0.051(6) 0.090(8) 0.025(5) -0.010(5) 0.005(4) 0.020(6) C27 0.024(4) 0.029(4) 0.023(4) 0.002(3) 0.004(3) -0.003(3) C28 0.064(7) 0.059(7) 0.039(6) 0.014(5) 0.012(5) 0.011(5) C29 0.055(6) 0.052(6) 0.042(5) 0.014(4) 0.016(5) 0.011(5) C30 0.031(4) 0.032(4) 0.025(4) 0.002(3) 0.011(3) 0.010(3) C31 0.051(6) 0.079(7) 0.028(5) 0.007(5) 0.002(4) -0.005(5) C32 0.059(7) 0.101(9) 0.040(6) -0.002(6) -0.001(5) 0.006(6) C33 0.030(4) 0.024(4) 0.019(4) -0.003(3) 0.009(3) 0.001(3) C34 0.082(8) 0.086(8) 0.024(5) 0.011(5) 0.007(5) -0.022(6) C35 0.060(6) 0.062(6) 0.030(5) -0.004(4) 0.005(4) -0.017(5) C36 0.030(4) 0.030(4) 0.024(4) -0.001(3) 0.006(3) 0.006(3) C37 0.063(6) 0.046(6) 0.032(5) -0.002(4) 0.008(4) -0.012(5) C38 0.079(8) 0.052(6) 0.029(5) -0.018(4) 0.003(5) -0.013(5) C39 0.041(5) 0.034(5) 0.025(4) -0.004(4) 0.008(4) 0.004(4) C40 0.062(7) 0.077(7) 0.030(5) 0.024(5) 0.010(5) -0.015(6) C41 0.058(6) 0.067(7) 0.025(5) 0.002(4) 0.002(4) -0.035(5) C42 0.050(5) 0.053(6) 0.017(4) 0.006(4) 0.001(4) -0.015(4) C43 0.082(7) 0.050(6) 0.023(5) 0.000(4) 0.009(5) -0.024(5) C44 0.089(8) 0.061(7) 0.030(5) -0.005(5) 0.000(5) -0.020(6) C45 0.100(9) 0.059(7) 0.016(4) 0.006(4) 0.004(5) -0.023(6) Cl1 0.0623(17) 0.0650(17) 0.0500(15) 0.0016(12) 0.0037(12) 0.0040(13) Cl2 0.0511(13) 0.0460(13) 0.0341(12) 0.0083(9) 0.0063(10) 0.0037(10) Cl3 0.063(3) 0.069(2) 0.042(2) 0.0071(19) 0.0119(17) 0.020(2) Cl3B 0.063(3) 0.069(2) 0.042(2) 0.0071(19) 0.0119(17) 0.020(2) Cu1 0.0544(15) 0.051(3) 0.0293(12) 0.0017(15) 0.0162(11) -0.0056(14) Cu2 0.0513(7) 0.0708(8) 0.0242(6) -0.0039(5) 0.0165(5) -0.0089(6) Cu3 0.0521(7) 0.0826(9) 0.0318(6) 0.0115(6) 0.0052(5) -0.0201(7) Cu4 0.0800(9) 0.0498(7) 0.0293(6) -0.0023(5) -0.0087(6) 0.0040(6) Cu5 0.0902(12) 0.1560(17) 0.0397(8) 0.0039(9) 0.0156(8) -0.0298(11) Cu6 0.80(3) 0.153(7) 0.121(7) -0.031(5) 0.229(13) -0.127(13) Cu7 0.0902(11) 0.1296(14) 0.0178(6) 0.0004(7) 0.0114(6) 0.0203(10) Cu1B 0.174(11) 0.043(4) 0.034(4) -0.001(3) 0.053(6) 0.006(5) Cu6B 0.016(3) 0.051(5) 0.046(4) -0.006(3) -0.001(3) 0.000(3) Dy1 0.02062(19) 0.0306(2) 0.01704(18) 0.00082(14) 0.00512(14) 0.00040(15) Dy2 0.01992(19) 0.0343(2) 0.01342(18) 0.00069(14) 0.00527(13) 0.00218(15) N1 0.053(5) 0.044(5) 0.051(5) 0.006(4) 0.022(4) 0.002(4) N2 0.047(5) 0.070(6) 0.034(5) 0.002(4) 0.004(4) 0.019(5) N3 0.060(5) 0.044(4) 0.048(5) 0.002(4) 0.004(4) 0.007(4) N4 0.053(5) 0.050(5) 0.023(4) -0.005(3) 0.012(3) -0.004(4) N5 0.036(4) 0.064(5) 0.011(3) -0.002(3) 0.008(3) 0.001(3) N6 0.044(4) 0.066(5) 0.027(4) 0.008(4) 0.008(3) -0.011(4) N7 0.047(5) 0.044(4) 0.018(3) 0.000(3) -0.003(3) 0.002(3) N8 0.091(7) 0.063(6) 0.023(4) 0.008(4) 0.024(4) 0.015(5) N9 0.066(5) 0.066(5) 0.016(4) 0.003(4) 0.006(4) 0.011(4) N10 0.044(4) 0.068(6) 0.022(4) 0.002(4) 0.009(3) 0.013(4) O1 0.031(3) 0.051(4) 0.025(3) -0.007(3) -0.002(2) -0.002(3) O2 0.034(3) 0.034(3) 0.023(3) -0.002(2) 0.015(2) -0.001(2) O3 0.025(3) 0.048(3) 0.022(3) 0.003(2) 0.001(2) 0.003(2) O4 0.033(3) 0.064(4) 0.021(3) 0.009(3) 0.013(2) 0.007(3) O5 0.083(5) 0.035(4) 0.029(3) -0.003(3) -0.009(3) -0.001(3) O6 0.031(3) 0.046(4) 0.029(3) 0.010(3) 0.009(2) 0.008(3) O7 0.032(3) 0.049(4) 0.020(3) -0.006(2) 0.009(2) 0.001(3) O8 0.022(3) 0.052(4) 0.029(3) 0.001(3) 0.001(2) 0.006(3) O9 0.031(3) 0.037(3) 0.040(3) 0.006(3) -0.005(3) -0.004(3) O10 0.033(3) 0.042(3) 0.032(3) 0.007(3) 0.011(2) 0.000(3) O11 0.037(3) 0.037(3) 0.021(3) -0.011(2) 0.008(2) 0.001(3) O12 0.067(4) 0.043(4) 0.031(3) 0.002(3) 0.016(3) -0.009(3) O13 0.155(9) 0.126(8) 0.030(4) -0.015(4) 0.012(5) -0.071(7) O14 0.106(7) 0.141(8) 0.026(4) 0.015(4) 0.014(4) -0.041(6) O15W 0.042(3) 0.036(3) 0.023(3) 0.002(2) 0.007(2) -0.005(3) O16W 0.031(3) 0.036(3) 0.059(4) -0.004(3) 0.008(3) 0.007(3) O17W 0.027(3) 0.031(3) 0.043(3) -0.007(2) 0.005(2) 0.004(2) O18W 0.042(3) 0.041(3) 0.022(3) -0.003(2) 0.001(2) 0.002(3) O19W 0.041(4) 0.050(4) 0.052(4) -0.015(3) 0.025(3) 0.003(3) O20W 0.029(3) 0.038(3) 0.028(3) 0.008(2) 0.006(2) 0.000(2) O21W 0.124(7) 0.054(5) 0.129(8) 0.005(5) 0.088(6) 0.008(5) O22W 0.109(8) 0.053(6) 0.197(12) -0.010(6) -0.040(8) 0.000(5) _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 N1 1.154(15) 2_465 ? C1 C1 1.154(15) 2_465 ? C1 Cu1 1.861(9) . ? C1 Cu1B 1.961(14) . ? C2 N2 1.000(11) . ? C2 Cu2 2.126(12) 2_565 ? C2 Cu2 2.157(10) . ? C3 N3 1.120(10) . ? C3 Cu5 1.948(10) . ? C3 Cu4 1.983(9) . ? C4 N4 1.336(11) . ? C4 C5 1.393(11) . ? C4 H4 0.9300 . ? C5 C6 1.397(11) . ? C5 H5 0.9300 . ? C6 C7 1.389(10) . ? C6 C9 1.507(10) . ? C7 C8 1.371(11) . ? C7 H7 0.9300 . ? C8 N4 1.330(11) . ? C8 H8 0.9300 . ? C9 O1 1.239(8) . ? C9 O2 1.262(9) . ? C10 N5 1.336(10) . ? C10 C11 1.381(10) . ? C10 H10 0.9300 . ? C11 C12 1.382(10) . ? C11 H11 0.9300 . ? C12 C13 1.383(10) . ? C12 C15 1.497(9) . ? C13 C14 1.370(11) . ? C13 H13 0.9300 . ? C14 N5 1.333(11) . ? C14 H14 0.9300 . ? C15 O3 1.241(8) . ? C15 O4 1.261(9) . ? C16 N6 1.347(11) . ? C16 C17 1.367(12) . ? C16 H16 0.9300 . ? C17 C18 1.382(11) . ? C17 H17 0.9300 . ? C18 C19 1.381(11) . ? C18 C21 1.505(11) . ? C19 C20 1.363(11) . ? C19 H19 0.9300 . ? C20 N6 1.330(10) . ? C20 H20 0.9300 . ? C21 O5 1.248(10) . ? C21 O6 1.260(10) . ? C22 N7 1.331(11) . ? C22 C23 1.377(10) . ? C22 H22 0.9300 . ? C23 C24 1.388(10) . ? C23 H23 0.9300 . ? C24 C25 1.370(11) . ? C24 C27 1.513(10) . ? C25 C26 1.381(11) . ? C25 H25 0.9300 . ? C26 N7 1.319(11) . ? C26 H26 0.9300 . ? C27 O7 1.246(9) . ? C27 O8 1.249(9) . ? C28 N8 1.319(12) . ? C28 C29 1.358(12) . ? C28 H28 0.9300 . ? C29 C30 1.399(11) . ? C29 H29 0.9300 . ? C30 C31 1.384(11) . ? C30 C33 1.512(10) . ? C31 C32 1.397(13) . ? C31 H31 0.9300 . ? C32 N8 1.366(13) . ? C32 H32 0.9300 . ? C33 O10 1.248(8) . ? C33 O9 1.255(8) . ? C34 N9 1.326(12) . ? C34 C35 1.394(12) . ? C34 H34 0.9300 . ? C35 C36 1.363(12) . ? C35 H35 0.9300 . ? C36 C37 1.369(11) . ? C36 C39 1.519(10) . ? C37 C38 1.397(12) . ? C37 H37 0.9300 . ? C38 N9 1.328(12) . ? C38 H38 0.9300 . ? C39 O12 1.226(9) . ? C39 O11 1.291(9) . ? C40 N10 1.328(12) . ? C40 C41 1.374(12) . ? C40 H40 0.9300 . ? C41 C42 1.355(11) . ? C41 H41 0.9300 . ? C42 C43 1.364(11) . ? C42 C45 1.515(11) . ? C43 C44 1.374(12) . ? C43 H43 0.9300 . ? C44 N10 1.302(12) . ? C44 H44 0.9300 . ? C45 O14 1.228(11) . ? C45 O13 1.275(12) . ? Cl1 Cu2 2.268(3) . ? Cl1 Cu1 2.321(5) . ? Cl1 Cu1B 2.684(13) . ? Cl2 Cu6B 2.089(6) . ? Cl2 Cu4 2.405(2) . ? Cl2 Cu4 2.459(3) 2_675 ? Cl3 Cu6 1.991(4) . ? Cl3 Cu5 2.337(5) . ? Cl3B Cu5 1.630(10) . ? Cl3B Cu6B 2.534(13) . ? Cu1 N4 2.072(9) 2_465 ? Cu1 Cu3 2.849(5) 1_455 ? Cu2 N5 2.043(6) . ? Cu2 C2 2.126(12) 2_565 ? Cu2 Cu2 2.375(2) 2_565 ? Cu3 N3 1.918(8) . ? Cu3 N2 1.936(10) . ? Cu3 N6 2.086(7) 1_655 ? Cu3 Cu1B 2.522(12) 1_655 ? Cu3 Cu1 2.849(5) 1_655 ? Cu4 N7 2.041(6) . ? Cu4 Cl2 2.459(3) 2_675 ? Cu4 Cu5 2.503(2) . ? Cu5 N8 2.030(7) 1_454 ? Cu6 Cl3 1.991(4) 2_775 ? Cu7 N10 1.923(7) . ? Cu7 N9 1.927(7) . ? Cu7 Cu6B 2.984(9) 2_775 ? Cu1B N4 2.021(14) 2_465 ? Cu1B N3 2.136(13) 1_455 ? Cu1B Cu3 2.522(12) 1_455 ? Cu6B Cu6B 2.869(12) 2_775 ? Cu6B Cu7 2.984(9) 2_775 ? Dy1 O10 2.281(5) 2_876 ? Dy1 O7 2.283(5) 2_776 ? Dy1 O9 2.321(5) . ? Dy1 O8 2.343(5) . ? Dy1 O16W 2.413(5) . ? Dy1 O11 2.415(5) . ? Dy1 O15W 2.456(5) . ? Dy1 O17W 2.517(5) . ? Dy1 H16B 2.2429 . ? Dy2 O3 2.278(5) 2_566 ? Dy2 O1 2.294(5) . ? Dy2 O4 2.318(5) . ? Dy2 O2 2.330(5) 2_466 ? Dy2 O19W 2.415(6) . ? Dy2 O6 2.429(5) . ? Dy2 O18W 2.443(5) . ? Dy2 O20W 2.489(5) . ? N3 Cu1B 2.136(13) 1_655 ? N4 Cu1B 2.021(14) 2_465 ? N4 Cu1 2.072(9) 2_465 ? N6 Cu3 2.086(7) 1_455 ? N8 Cu5 2.030(7) 1_656 ? O2 Dy2 2.330(5) 2_466 ? O3 Dy2 2.278(5) 2_566 ? O7 Dy1 2.283(5) 2_776 ? O10 Dy1 2.281(5) 2_876 ? O15W H15A 0.8499 . ? O15W H15B 0.8499 . ? O16W H16B 0.8208 . ? O16W H16A 0.8180 . ? O17W H17A 0.8503 . ? O17W H17B 0.8512 . ? O18W H18A 0.8188 . ? O18W H18B 0.8194 . ? O19W H19A 0.8500 . ? O19W H19B 0.8500 . ? O20W H20A 0.8500 . ? O20W H20B 0.8500 . ? O21W H21A 0.8499 . ? O21W H21B 0.8500 . ? O22W H22A 0.8501 . ? O22W H22B 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C1 0.0(10) 2_465 2_465 ? N1 C1 Cu1 165.6(12) 2_465 . ? C1 C1 Cu1 165.6(12) 2_465 . ? N1 C1 Cu1B 170.7(12) 2_465 . ? C1 C1 Cu1B 170.7(12) 2_465 . ? Cu1 C1 Cu1B 15.8(4) . . ? N2 C2 Cu2 145.7(10) . 2_565 ? N2 C2 Cu2 145.2(11) . . ? Cu2 C2 Cu2 67.4(3) 2_565 . ? N3 C3 Cu5 138.7(8) . . ? N3 C3 Cu4 141.7(8) . . ? Cu5 C3 Cu4 79.1(4) . . ? N4 C4 C5 123.1(8) . . ? N4 C4 H4 118.4 . . ? C5 C4 H4 118.4 . . ? C4 C5 C6 118.3(8) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C7 C6 C5 117.6(7) . . ? C7 C6 C9 120.5(7) . . ? C5 C6 C9 121.8(7) . . ? C8 C7 C6 119.9(8) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? N4 C8 C7 122.8(8) . . ? N4 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? O1 C9 O2 124.7(7) . . ? O1 C9 C6 118.3(7) . . ? O2 C9 C6 117.0(6) . . ? N5 C10 C11 122.7(8) . . ? N5 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C10 C11 C12 119.4(7) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 117.4(7) . . ? C11 C12 C15 121.6(6) . . ? C13 C12 C15 120.9(7) . . ? C14 C13 C12 120.0(7) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? N5 C14 C13 122.7(8) . . ? N5 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? O3 C15 O4 124.5(7) . . ? O3 C15 C12 118.8(7) . . ? O4 C15 C12 116.7(6) . . ? N6 C16 C17 122.8(8) . . ? N6 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C16 C17 C18 119.5(8) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 117.8(7) . . ? C17 C18 C21 120.6(7) . . ? C19 C18 C21 121.5(7) . . ? C20 C19 C18 118.9(8) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? N6 C20 C19 124.1(8) . . ? N6 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? O5 C21 O6 124.1(8) . . ? O5 C21 C18 118.1(8) . . ? O6 C21 C18 117.8(8) . . ? N7 C22 C23 124.1(8) . . ? N7 C22 H22 118.0 . . ? C23 C22 H22 118.0 . . ? C22 C23 C24 118.4(8) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 C23 117.7(7) . . ? C25 C24 C27 121.5(7) . . ? C23 C24 C27 120.8(7) . . ? C24 C25 C26 119.6(8) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N7 C26 C25 123.4(9) . . ? N7 C26 H26 118.3 . . ? C25 C26 H26 118.3 . . ? O7 C27 O8 126.1(7) . . ? O7 C27 C24 117.2(7) . . ? O8 C27 C24 116.7(7) . . ? N8 C28 C29 122.4(10) . . ? N8 C28 H28 118.8 . . ? C29 C28 H28 118.8 . . ? C28 C29 C30 119.3(9) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 120.0(8) . . ? C31 C30 C33 120.2(7) . . ? C29 C30 C33 119.7(7) . . ? C30 C31 C32 116.8(9) . . ? C30 C31 H31 121.6 . . ? C32 C31 H31 121.6 . . ? N8 C32 C31 122.2(10) . . ? N8 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? O10 C33 O9 124.7(7) . . ? O10 C33 C30 118.1(6) . . ? O9 C33 C30 117.2(7) . . ? N9 C34 C35 122.7(9) . . ? N9 C34 H34 118.6 . . ? C35 C34 H34 118.6 . . ? C36 C35 C34 120.0(9) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 117.2(8) . . ? C35 C36 C39 122.1(7) . . ? C37 C36 C39 120.6(7) . . ? C36 C37 C38 120.1(9) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? N9 C38 C37 122.4(8) . . ? N9 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? O12 C39 O11 126.4(7) . . ? O12 C39 C36 117.7(7) . . ? O11 C39 C36 115.9(7) . . ? N10 C40 C41 123.6(8) . . ? N10 C40 H40 118.2 . . ? C41 C40 H40 118.2 . . ? C42 C41 C40 119.3(8) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 C43 117.2(8) . . ? C41 C42 C45 121.6(8) . . ? C43 C42 C45 121.2(8) . . ? C42 C43 C44 119.9(8) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? N10 C44 C43 123.5(9) . . ? N10 C44 H44 118.3 . . ? C43 C44 H44 118.3 . . ? O14 C45 O13 127.8(9) . . ? O14 C45 C42 118.1(9) . . ? O13 C45 C42 113.7(9) . . ? Cu2 Cl1 Cu1 99.55(16) . . ? Cu2 Cl1 Cu1B 108.5(3) . . ? Cu1 Cl1 Cu1B 9.1(3) . . ? Cu6B Cl2 Cu4 100.2(3) . . ? Cu6B Cl2 Cu4 161.0(3) . 2_675 ? Cu4 Cl2 Cu4 82.14(8) . 2_675 ? Cu6 Cl3 Cu5 116.69(19) . . ? Cu5 Cl3B Cu6B 93.9(4) . . ? C1 Cu1 N4 117.8(4) . 2_465 ? C1 Cu1 Cl1 127.8(4) . . ? N4 Cu1 Cl1 103.7(3) 2_465 . ? C1 Cu1 Cu3 63.5(3) . 1_455 ? N4 Cu1 Cu3 124.0(3) 2_465 1_455 ? Cl1 Cu1 Cu3 117.2(2) . 1_455 ? N5 Cu2 C2 109.5(3) . 2_565 ? N5 Cu2 C2 104.7(3) . . ? C2 Cu2 C2 112.6(3) 2_565 . ? N5 Cu2 Cl1 101.3(2) . . ? C2 Cu2 Cl1 117.8(3) 2_565 . ? C2 Cu2 Cl1 109.5(3) . . ? N5 Cu2 Cu2 122.0(2) . 2_565 ? C2 Cu2 Cu2 56.9(3) 2_565 2_565 ? C2 Cu2 Cu2 55.7(3) . 2_565 ? Cl1 Cu2 Cu2 136.07(10) . 2_565 ? N3 Cu3 N2 143.0(3) . . ? N3 Cu3 N6 107.7(3) . 1_655 ? N2 Cu3 N6 103.4(3) . 1_655 ? N3 Cu3 Cu1B 55.5(4) . 1_655 ? N2 Cu3 Cu1B 121.8(4) . 1_655 ? N6 Cu3 Cu1B 120.7(3) 1_655 1_655 ? N3 Cu3 Cu1 60.7(3) . 1_655 ? N2 Cu3 Cu1 123.3(3) . 1_655 ? N6 Cu3 Cu1 112.8(2) 1_655 1_655 ? Cu1B Cu3 Cu1 9.1(3) 1_655 1_655 ? C3 Cu4 N7 115.9(3) . . ? C3 Cu4 Cl2 117.6(3) . . ? N7 Cu4 Cl2 113.3(2) . . ? C3 Cu4 Cl2 105.7(3) . 2_675 ? N7 Cu4 Cl2 103.2(2) . 2_675 ? Cl2 Cu4 Cl2 97.86(8) . 2_675 ? C3 Cu4 Cu5 49.8(3) . . ? N7 Cu4 Cu5 116.2(2) . . ? Cl2 Cu4 Cu5 75.24(8) . . ? Cl2 Cu4 Cu5 139.60(8) 2_675 . ? Cl3B Cu5 C3 143.9(4) . . ? Cl3B Cu5 N8 92.8(4) . 1_454 ? C3 Cu5 N8 121.6(4) . 1_454 ? Cl3B Cu5 Cl3 14.3(3) . . ? C3 Cu5 Cl3 131.4(3) . . ? N8 Cu5 Cl3 106.5(3) 1_454 . ? Cl3B Cu5 Cu4 116.6(3) . . ? C3 Cu5 Cu4 51.1(3) . . ? N8 Cu5 Cu4 129.1(3) 1_454 . ? Cl3 Cu5 Cu4 103.62(12) . . ? Cl3 Cu6 Cl3 180.000(1) . 2_775 ? N10 Cu7 N9 172.0(4) . . ? N10 Cu7 Cu6B 92.5(3) . 2_775 ? N9 Cu7 Cu6B 95.4(3) . 2_775 ? C1 Cu1B N4 115.6(7) . 2_465 ? C1 Cu1B N3 117.6(7) . 1_455 ? N4 Cu1B N3 119.9(6) 2_465 1_455 ? C1 Cu1B Cu3 70.2(5) . 1_455 ? N4 Cu1B Cu3 147.2(6) 2_465 1_455 ? N3 Cu1B Cu3 47.8(3) 1_455 1_455 ? C1 Cu1B Cl1 107.2(5) . . ? N4 Cu1B Cl1 93.5(5) 2_465 . ? N3 Cu1B Cl1 95.8(5) 1_455 . ? Cu3 Cu1B Cl1 116.3(5) 1_455 . ? Cl2 Cu6B Cl3B 98.7(4) . . ? Cl2 Cu6B Cu6B 167.3(6) . 2_775 ? Cl3B Cu6B Cu6B 71.5(4) . 2_775 ? Cl2 Cu6B Cu7 76.6(2) . 2_775 ? Cl3B Cu6B Cu7 168.7(4) . 2_775 ? Cu6B Cu6B Cu7 114.5(4) 2_775 2_775 ? O10 Dy1 O7 143.0(2) 2_876 2_776 ? O10 Dy1 O9 99.5(2) 2_876 . ? O7 Dy1 O9 91.2(2) 2_776 . ? O10 Dy1 O8 90.95(19) 2_876 . ? O7 Dy1 O8 100.75(19) 2_776 . ? O9 Dy1 O8 144.3(2) . . ? O10 Dy1 O16W 74.3(2) 2_876 . ? O7 Dy1 O16W 75.5(2) 2_776 . ? O9 Dy1 O16W 142.02(19) . . ? O8 Dy1 O16W 73.65(19) . . ? O10 Dy1 O11 70.84(19) 2_876 . ? O7 Dy1 O11 146.18(19) 2_776 . ? O9 Dy1 O11 78.03(19) . . ? O8 Dy1 O11 73.40(18) . . ? O16W Dy1 O11 130.86(19) . . ? O10 Dy1 O15W 145.27(19) 2_876 . ? O7 Dy1 O15W 71.62(19) 2_776 . ? O9 Dy1 O15W 77.64(18) . . ? O8 Dy1 O15W 74.60(18) . . ? O16W Dy1 O15W 128.29(18) . . ? O11 Dy1 O15W 74.76(18) . . ? O10 Dy1 O17W 75.27(19) 2_876 . ? O7 Dy1 O17W 74.87(18) 2_776 . ? O9 Dy1 O17W 71.31(18) . . ? O8 Dy1 O17W 144.24(18) . . ? O16W Dy1 O17W 70.90(18) . . ? O11 Dy1 O17W 129.06(18) . . ? O15W Dy1 O17W 133.19(17) . . ? O10 Dy1 H16B 78.8 2_876 . ? O7 Dy1 H16B 80.2 2_776 . ? O9 Dy1 H16B 161.7 . . ? O8 Dy1 H16B 53.9 . . ? O16W Dy1 H16B 19.9 . . ? O11 Dy1 H16B 117.7 . . ? O15W Dy1 H16B 114.2 . . ? O17W Dy1 H16B 90.8 . . ? O3 Dy2 O1 142.1(2) 2_566 . ? O3 Dy2 O4 100.83(19) 2_566 . ? O1 Dy2 O4 90.24(19) . . ? O3 Dy2 O2 89.58(18) 2_566 2_466 ? O1 Dy2 O2 102.42(19) . 2_466 ? O4 Dy2 O2 144.1(2) . 2_466 ? O3 Dy2 O19W 74.9(2) 2_566 . ? O1 Dy2 O19W 73.8(2) . . ? O4 Dy2 O19W 73.6(2) . . ? O2 Dy2 O19W 142.11(19) 2_466 . ? O3 Dy2 O6 144.67(19) 2_566 . ? O1 Dy2 O6 73.16(19) . . ? O4 Dy2 O6 75.00(19) . . ? O2 Dy2 O6 76.81(18) 2_466 . ? O19W Dy2 O6 133.68(19) . . ? O3 Dy2 O18W 71.54(18) 2_566 . ? O1 Dy2 O18W 145.92(19) . . ? O4 Dy2 O18W 73.72(19) . . ? O2 Dy2 O18W 77.36(18) 2_466 . ? O19W Dy2 O18W 126.83(19) . . ? O6 Dy2 O18W 73.69(18) . . ? O3 Dy2 O20W 75.11(18) 2_566 . ? O1 Dy2 O20W 74.95(18) . . ? O4 Dy2 O20W 144.17(19) . . ? O2 Dy2 O20W 71.68(17) 2_466 . ? O19W Dy2 O20W 70.99(19) . . ? O6 Dy2 O20W 128.33(18) . . ? O18W Dy2 O20W 134.07(17) . . ? C2 N2 Cu3 170.6(10) . . ? C3 N3 Cu3 160.5(8) . . ? C3 N3 Cu1B 117.8(9) . 1_655 ? Cu3 N3 Cu1B 76.7(4) . 1_655 ? C8 N4 C4 118.0(7) . . ? C8 N4 Cu1B 129.5(7) . 2_465 ? C4 N4 Cu1B 112.4(7) . 2_465 ? C8 N4 Cu1 118.3(6) . 2_465 ? C4 N4 Cu1 121.5(6) . 2_465 ? Cu1B N4 Cu1 15.0(3) 2_465 2_465 ? C14 N5 C10 117.7(7) . . ? C14 N5 Cu2 119.6(5) . . ? C10 N5 Cu2 122.7(6) . . ? C20 N6 C16 116.7(7) . . ? C20 N6 Cu3 119.5(6) . 1_455 ? C16 N6 Cu3 123.6(6) . 1_455 ? C26 N7 C22 116.8(7) . . ? C26 N7 Cu4 121.6(6) . . ? C22 N7 Cu4 121.5(6) . . ? C28 N8 C32 119.2(8) . . ? C28 N8 Cu5 118.6(7) . 1_656 ? C32 N8 Cu5 120.7(7) . 1_656 ? C38 N9 C34 117.5(8) . . ? C38 N9 Cu7 120.8(6) . . ? C34 N9 Cu7 121.7(7) . . ? C44 N10 C40 116.4(8) . . ? C44 N10 Cu7 122.6(7) . . ? C40 N10 Cu7 120.9(6) . . ? C9 O1 Dy2 178.6(5) . . ? C9 O2 Dy2 130.1(5) . 2_466 ? C15 O3 Dy2 178.6(5) . 2_566 ? C15 O4 Dy2 132.8(5) . . ? C21 O6 Dy2 129.9(5) . . ? C27 O7 Dy1 171.4(5) . 2_776 ? C27 O8 Dy1 130.8(5) . . ? C33 O9 Dy1 138.3(5) . . ? C33 O10 Dy1 166.6(5) . 2_876 ? C39 O11 Dy1 130.1(5) . . ? Dy1 O15W H15A 112.1 . . ? Dy1 O15W H15B 113.2 . . ? H15A O15W H15B 107.7 . . ? Dy1 O16W H16B 68.3 . . ? Dy1 O16W H16A 139.1 . . ? H16B O16W H16A 110.9 . . ? Dy1 O17W H17A 118.8 . . ? Dy1 O17W H17B 126.9 . . ? H17A O17W H17B 104.7 . . ? Dy2 O18W H18A 122.3 . . ? Dy2 O18W H18B 110.8 . . ? H18A O18W H18B 110.9 . . ? Dy2 O19W H19A 140.5 . . ? Dy2 O19W H19B 100.3 . . ? H19A O19W H19B 107.7 . . ? Dy2 O20W H20A 133.4 . . ? Dy2 O20W H20B 114.4 . . ? H20A O20W H20B 107.7 . . ? H21A O21W H21B 107.7 . . ? H22A O22W H22B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.133 _refine_diff_density_min -1.833 _refine_diff_density_rms 0.162 _database_code_depnum_ccdc_archive 'CCDC 964397' ####################################################################### # # 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_III-A #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H26 Cu5 F5 N10 O17 S Tb4' _chemical_formula_sum 'C40 H26 Cu5 F5 N10 O17 S Tb4' _chemical_formula_weight 1999.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.632(4) _cell_length_b 7.7785(7) _cell_length_c 17.7721(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.2120(10) _cell_angle_gamma 90.00 _cell_volume 5161.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4749 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.39 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3752 _exptl_absorpt_coefficient_mu 7.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.178 _exptl_absorpt_correction_T_max 0.221 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13036 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.39 _reflns_number_total 4749 _reflns_number_gt 4122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0248P)^2^+27.3524P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000175(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4749 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.25263(19) 0.4784(11) 0.3212(4) 0.0437(18) Uani 1 1 d . . . C2 C 0.25117(17) 0.4102(9) 0.0694(4) 0.0378(17) Uani 1 1 d . . . C5 C 0.12553(6) 0.2675(3) 0.50284(17) 0.0248(13) Uani 1 1 d G . . C6 C 0.14823(8) 0.3071(3) 0.56840(13) 0.0379(17) Uani 1 1 d G . . H6 H 0.1388 0.3435 0.6116 0.045 Uiso 1 1 calc R . . C7 C 0.18510(7) 0.2922(3) 0.56943(15) 0.0442(18) Uani 1 1 d G . . H7 H 0.2003 0.3187 0.6133 0.053 Uiso 1 1 calc R . . N3 N 0.19927(6) 0.2378(3) 0.50490(18) 0.0371(14) Uani 1 1 d G . . C3 C 0.17657(8) 0.1982(3) 0.43935(16) 0.0390(17) Uani 1 1 d G . . H3 H 0.1860 0.1618 0.3962 0.047 Uiso 1 1 calc R . . C4 C 0.13970(7) 0.2131(3) 0.43832(16) 0.0348(16) Uani 1 1 d G . . H4 H 0.1245 0.1866 0.3945 0.042 Uiso 1 1 calc R . . C13 C 0.16251(7) 0.7719(3) 0.50751(16) 0.0431(18) Uani 1 1 d G . . H13 H 0.1772 0.8139 0.5494 0.052 Uiso 1 1 calc R . . C12 C 0.12575(8) 0.7994(3) 0.50095(17) 0.0322(15) Uani 1 1 d G . . H12 H 0.1159 0.8599 0.5384 0.039 Uiso 1 1 calc R . . C11 C 0.10373(6) 0.7365(3) 0.43836(18) 0.0202(12) Uani 1 1 d G . . C10 C 0.11846(7) 0.6460(3) 0.38234(14) 0.0283(14) Uani 1 1 d G . . H10 H 0.1037 0.6039 0.3405 0.034 Uiso 1 1 calc R . . C9 C 0.15522(7) 0.6185(3) 0.38890(12) 0.0376(17) Uani 1 1 d G . . H9 H 0.1651 0.5580 0.3514 0.045 Uiso 1 1 calc R . . N4 N 0.17724(6) 0.6814(3) 0.45148(16) 0.0346(13) Uani 1 1 d G . . C8 C 0.08544(15) 0.3049(7) 0.4986(4) 0.0257(14) Uani 1 1 d . . . C14 C 0.06409(14) 0.7739(7) 0.4303(3) 0.0181(12) Uani 1 1 d . . . C15 C -0.14526(19) -0.0167(10) 0.2551(5) 0.049(2) Uani 1 1 d . . . H15 H -0.1489 -0.1311 0.2408 0.058 Uiso 1 1 calc R . . C16 C -0.11078(19) 0.0365(8) 0.2775(4) 0.0397(17) Uani 1 1 d . . . H16 H -0.0919 -0.0416 0.2805 0.048 Uiso 1 1 calc R . . C17 C -0.10442(15) 0.2068(7) 0.2954(3) 0.0218(12) Uani 1 1 d . . . C18 C -0.13372(17) 0.3160(9) 0.2891(4) 0.0377(16) Uani 1 1 d . . . H18 H -0.1307 0.4331 0.2983 0.045 Uiso 1 1 calc R . . C19 C -0.16767(18) 0.2473(10) 0.2687(4) 0.0448(19) Uani 1 1 d . . . H19 H -0.1872 0.3211 0.2663 0.054 Uiso 1 1 calc R . . C20 C -0.06744(15) 0.2694(7) 0.3268(3) 0.0214(12) Uani 1 1 d . . . Cu1 Cu 0.27442(2) 0.48801(13) 0.23389(5) 0.0444(2) Uani 1 1 d . . . Cu2 Cu 0.23067(2) 0.61610(13) 0.46768(5) 0.0445(3) Uani 1 1 d . . . Cu3 Cu 0.2500 0.2500 0.5000 0.0639(5) Uani 1 2 d S . . F1 F 0.01169(10) 0.3797(5) 0.3257(2) 0.0326(9) Uani 0.50 1 d P . . F2 F -0.01988(9) -0.1144(4) 0.44711(19) 0.0262(8) Uani 1 1 d . . . F3 F -0.00865(9) 0.3625(4) 0.47028(17) 0.0209(7) Uani 1 1 d . . . N1 N 0.24068(18) 0.5007(10) 0.3758(4) 0.0559(18) Uani 1 1 d . . . N2 N 0.26129(16) 0.4434(8) 0.1308(3) 0.0445(15) Uani 1 1 d . . . N5 N -0.17374(15) 0.0843(8) 0.2525(3) 0.0392(14) Uani 1 1 d . . . O1W O 0.01169(10) 0.3797(5) 0.3257(2) 0.0326(9) Uani 0.50 1 d P . . H1A H 0.0154 0.3897 0.2822 0.039 Uiso 0.50 1 d PR . . H1B H 0.0298 0.4097 0.3535 0.039 Uiso 0.50 1 d PR . . O2 O 0.06667(10) 0.2705(5) 0.4374(2) 0.0281(10) Uani 1 1 d . . . O3 O 0.07442(11) 0.3595(5) 0.5573(3) 0.0339(11) Uani 1 1 d . . . O4 O 0.04314(10) 0.6652(5) 0.3975(2) 0.0233(9) Uani 1 1 d . . . O5 O 0.05580(11) 0.9147(5) 0.4573(2) 0.0256(9) Uani 1 1 d . . . O6 O -0.04637(10) 0.1567(5) 0.3535(2) 0.0257(9) Uani 1 1 d . . . O7 O -0.06216(10) 0.4280(5) 0.3254(2) 0.0259(9) Uani 1 1 d . . . O8 O 0.02435(10) -0.2376(5) 0.2119(2) 0.0214(9) Uani 1 1 d . . . O9 O 0.02169(10) -0.0190(5) 0.3054(2) 0.0205(8) Uani 1 1 d . . . S1 S 0.0000 -0.1277(2) 0.2500 0.0162(4) Uani 1 2 d S . . Tb1 Tb 0.012232(7) 0.12644(3) 0.414694(14) 0.01369(9) Uani 1 1 d . . . Tb2 Tb -0.017770(7) 0.60296(3) 0.398231(14) 0.01365(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(4) 0.077(6) 0.023(4) -0.005(4) 0.002(3) -0.007(4) C2 0.020(4) 0.057(5) 0.038(4) -0.002(3) 0.006(3) -0.007(3) C5 0.014(3) 0.030(3) 0.031(3) -0.005(3) 0.003(2) 0.000(2) C6 0.019(3) 0.058(5) 0.037(4) -0.013(3) 0.003(3) 0.000(3) C7 0.025(4) 0.068(5) 0.039(4) -0.009(4) 0.000(3) 0.000(3) N3 0.014(3) 0.054(4) 0.043(3) 0.005(3) 0.005(2) 0.012(2) C3 0.025(4) 0.056(5) 0.036(4) 0.002(3) 0.006(3) 0.007(3) C4 0.024(3) 0.046(4) 0.034(4) -0.005(3) 0.002(3) 0.001(3) C13 0.026(4) 0.068(5) 0.034(4) -0.003(4) -0.001(3) 0.001(3) C12 0.018(3) 0.040(4) 0.038(4) -0.006(3) 0.002(3) 0.003(3) C11 0.016(3) 0.021(3) 0.024(3) 0.004(2) 0.002(2) 0.002(2) C10 0.016(3) 0.035(3) 0.033(4) -0.005(3) -0.001(3) 0.002(3) C9 0.027(4) 0.044(4) 0.042(4) -0.005(3) 0.005(3) 0.010(3) N4 0.018(3) 0.052(4) 0.033(3) 0.003(3) 0.002(2) 0.007(3) C8 0.014(3) 0.014(3) 0.049(4) 0.000(3) 0.005(3) -0.001(2) C14 0.015(3) 0.017(3) 0.022(3) 0.005(2) 0.002(2) -0.001(2) C15 0.035(4) 0.038(4) 0.070(6) -0.019(4) -0.006(4) -0.017(3) C16 0.032(4) 0.030(4) 0.054(5) -0.008(3) -0.005(3) -0.006(3) C17 0.023(3) 0.026(3) 0.015(3) 0.000(2) -0.002(2) -0.001(2) C18 0.027(4) 0.034(4) 0.049(4) -0.010(3) -0.005(3) 0.002(3) C19 0.022(4) 0.059(5) 0.051(5) -0.006(4) -0.004(3) 0.006(3) C20 0.022(3) 0.026(3) 0.016(3) -0.002(2) -0.002(2) -0.001(2) Cu1 0.0314(5) 0.0709(7) 0.0303(5) -0.0069(4) 0.0013(4) -0.0122(4) Cu2 0.0209(5) 0.0817(7) 0.0301(5) 0.0045(4) 0.0004(4) 0.0104(4) Cu3 0.0121(6) 0.1188(14) 0.0616(10) -0.0095(9) 0.0073(6) 0.0054(7) F1 0.029(2) 0.029(2) 0.038(2) -0.0039(17) -0.0008(18) -0.0002(17) F2 0.029(2) 0.0243(18) 0.0250(19) -0.0002(13) 0.0024(15) -0.0039(14) F3 0.032(2) 0.0131(16) 0.0162(17) -0.0005(12) -0.0014(13) 0.0048(13) N1 0.041(4) 0.077(5) 0.048(4) 0.005(4) -0.001(3) 0.007(3) N2 0.033(3) 0.063(4) 0.035(4) -0.007(3) -0.003(3) -0.010(3) N5 0.026(3) 0.057(4) 0.034(3) -0.007(3) -0.001(2) -0.007(3) O1W 0.029(2) 0.029(2) 0.038(2) -0.0039(17) -0.0008(18) -0.0002(17) O2 0.017(2) 0.027(2) 0.039(3) 0.0036(19) -0.0013(19) -0.0047(17) O3 0.021(2) 0.036(3) 0.047(3) -0.017(2) 0.011(2) -0.0026(19) O4 0.018(2) 0.017(2) 0.035(2) -0.0014(17) 0.0005(17) 0.0024(16) O5 0.023(2) 0.021(2) 0.031(2) -0.0069(17) -0.0054(18) 0.0061(17) O6 0.022(2) 0.022(2) 0.030(2) 0.0001(17) -0.0091(18) -0.0008(17) O7 0.019(2) 0.023(2) 0.034(2) -0.0009(18) -0.0054(18) -0.0015(17) O8 0.028(2) 0.021(2) 0.015(2) -0.0050(16) 0.0042(16) 0.0043(17) O9 0.027(2) 0.018(2) 0.015(2) -0.0029(15) 0.0005(16) -0.0037(16) S1 0.0238(11) 0.0142(9) 0.0106(9) 0.000 0.0019(8) 0.000 Tb1 0.01335(15) 0.01444(15) 0.01280(15) -0.00113(9) -0.00028(10) 0.00025(10) Tb2 0.01353(15) 0.01428(14) 0.01248(15) 0.00154(9) -0.00090(10) -0.00157(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.134(9) . ? C1 Cu1 1.845(7) . ? C2 N2 1.139(9) . ? C2 Cu2 1.885(7) 6_565 ? C2 Cu2 2.499(7) 4_545 ? C5 C6 1.3900 . ? C5 C4 1.3900 . ? C5 C8 1.529(6) . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 N3 1.3900 . ? C7 H7 0.9300 . ? N3 C3 1.3900 . ? N3 Cu3 1.924(2) . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C13 N4 1.3901 . ? C13 C12 1.3902 . ? C13 H13 0.9300 . ? C12 C11 1.3900 . ? C12 H12 0.9300 . ? C11 C10 1.3899 . ? C11 C14 1.509(6) . ? C10 C9 1.3902 . ? C10 H10 0.9300 . ? C9 N4 1.3899 . ? C9 H9 0.9300 . ? N4 Cu2 2.059(2) . ? C8 O3 1.244(7) . ? C8 O2 1.249(7) . ? C14 O4 1.249(6) . ? C14 O5 1.251(6) . ? C15 N5 1.325(9) . ? C15 C16 1.373(9) . ? C15 H15 0.9300 . ? C16 C17 1.376(9) . ? C16 H16 0.9300 . ? C17 C18 1.385(8) . ? C17 C20 1.513(8) . ? C18 C19 1.391(9) . ? C18 H18 0.9300 . ? C19 N5 1.313(9) . ? C19 H19 0.9300 . ? C20 O6 1.236(7) . ? C20 O7 1.250(7) . ? Cu1 N2 1.870(6) . ? Cu1 N5 2.077(6) 3 ? Cu2 C2 1.885(7) 6_566 ? Cu2 N1 1.941(7) . ? Cu2 C2 2.499(7) 4 ? Cu2 Cu2 2.712(2) 7_566 ? Cu2 Cu3 2.9772(10) . ? Cu3 N3 1.925(2) 7_556 ? Cu3 Cu2 2.9772(10) 7_556 ? F1 Tb2 2.503(4) . ? F1 Tb1 2.525(4) . ? F1 H1A 0.8060 . ? F1 H1B 0.8241 . ? F2 Tb1 2.340(3) . ? F2 Tb2 2.369(3) 1_545 ? F2 Tb1 2.438(3) 5_556 ? F3 Tb2 2.268(3) . ? F3 Tb1 2.272(3) . ? F3 Tb2 2.437(3) 5_566 ? N5 Cu1 2.077(6) 3_445 ? O2 Tb1 2.326(4) . ? O3 Tb2 2.383(4) 5_566 ? O4 Tb2 2.344(4) . ? O5 Tb1 2.379(4) 1_565 ? O6 Tb1 2.345(4) . ? O7 Tb2 2.403(4) . ? O8 S1 1.478(4) . ? O8 Tb2 2.304(3) 2_545 ? O9 S1 1.466(4) . ? O9 Tb1 2.313(4) . ? S1 O9 1.466(4) 2 ? S1 O8 1.478(4) 2 ? Tb1 O5 2.379(4) 1_545 ? Tb1 F2 2.438(3) 5_556 ? Tb1 Tb1 3.8224(5) 5_556 ? Tb1 Tb2 3.9184(4) 5_566 ? Tb1 H1B 2.5798 . ? Tb2 O8 2.304(3) 2_565 ? Tb2 F2 2.369(3) 1_565 ? Tb2 O3 2.383(4) 5_566 ? Tb2 F3 2.437(3) 5_566 ? Tb2 Tb1 3.9184(4) 5_566 ? Tb2 H1B 2.5405 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cu1 168.6(8) . . ? N2 C2 Cu2 171.9(7) . 6_565 ? N2 C2 Cu2 113.0(6) . 4_545 ? Cu2 C2 Cu2 75.0(2) 6_565 4_545 ? C6 C5 C4 120.0 . . ? C6 C5 C8 119.8(3) . . ? C4 C5 C8 119.7(3) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 N3 120.0 . . ? C6 C7 H7 120.0 . . ? N3 C7 H7 120.0 . . ? C3 N3 C7 120.0 . . ? C3 N3 Cu3 118.80(16) . . ? C7 N3 Cu3 120.51(16) . . ? N3 C3 C4 120.0 . . ? N3 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N4 C13 C12 120.0 . . ? N4 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 C14 120.5(3) . . ? C12 C11 C14 119.4(3) . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? N4 C9 C10 120.0 . . ? N4 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 N4 C13 120.0 . . ? C9 N4 Cu2 119.92(13) . . ? C13 N4 Cu2 119.67(14) . . ? O3 C8 O2 126.3(5) . . ? O3 C8 C5 117.0(5) . . ? O2 C8 C5 116.6(5) . . ? O4 C14 O5 126.7(5) . . ? O4 C14 C11 118.2(4) . . ? O5 C14 C11 115.1(4) . . ? N5 C15 C16 124.2(7) . . ? N5 C15 H15 117.9 . . ? C16 C15 H15 117.9 . . ? C15 C16 C17 119.2(7) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 117.2(6) . . ? C16 C17 C20 121.3(5) . . ? C18 C17 C20 121.2(5) . . ? C17 C18 C19 118.8(6) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? N5 C19 C18 123.8(7) . . ? N5 C19 H19 118.1 . . ? C18 C19 H19 118.1 . . ? O6 C20 O7 127.7(5) . . ? O6 C20 C17 115.4(5) . . ? O7 C20 C17 116.8(5) . . ? C1 Cu1 N2 136.6(3) . . ? C1 Cu1 N5 112.9(3) . 3 ? N2 Cu1 N5 110.5(2) . 3 ? C2 Cu2 N1 131.1(3) 6_566 . ? C2 Cu2 N4 115.8(2) 6_566 . ? N1 Cu2 N4 106.6(2) . . ? C2 Cu2 C2 105.0(2) 6_566 4 ? N1 Cu2 C2 96.5(3) . 4 ? N4 Cu2 C2 91.82(16) . 4 ? C2 Cu2 Cu2 62.9(2) 6_566 7_566 ? N1 Cu2 Cu2 124.1(2) . 7_566 ? N4 Cu2 Cu2 109.40(9) . 7_566 ? C2 Cu2 Cu2 42.17(17) 4 7_566 ? C2 Cu2 Cu3 69.6(2) 6_566 . ? N1 Cu2 Cu3 69.6(2) . . ? N4 Cu2 Cu3 118.28(7) . . ? C2 Cu2 Cu3 149.10(15) 4 . ? Cu2 Cu2 Cu3 123.22(5) 7_566 . ? N3 Cu3 N3 180.00(16) . 7_556 ? N3 Cu3 Cu2 80.57(7) . . ? N3 Cu3 Cu2 99.43(15) 7_556 . ? N3 Cu3 Cu2 99.43(7) . 7_556 ? N3 Cu3 Cu2 80.57(15) 7_556 7_556 ? Cu2 Cu3 Cu2 180.0 . 7_556 ? Tb2 F1 Tb1 100.81(14) . . ? Tb2 F1 H1A 124.6 . . ? Tb1 F1 H1A 133.4 . . ? Tb2 F1 H1B 83.2 . . ? Tb1 F1 H1B 84.5 . . ? H1A F1 H1B 108.6 . . ? Tb1 F2 Tb2 127.63(15) . 1_545 ? Tb1 F2 Tb1 106.22(12) . 5_556 ? Tb2 F2 Tb1 109.19(12) 1_545 5_556 ? Tb2 F3 Tb1 117.20(13) . . ? Tb2 F3 Tb2 117.72(12) . 5_566 ? Tb1 F3 Tb2 112.60(12) . 5_566 ? C1 N1 Cu2 158.6(7) . . ? C2 N2 Cu1 175.0(6) . . ? C19 N5 C15 116.6(6) . . ? C19 N5 Cu1 121.1(5) . 3_445 ? C15 N5 Cu1 122.1(5) . 3_445 ? C8 O2 Tb1 130.1(4) . . ? C8 O3 Tb2 136.6(4) . 5_566 ? C14 O4 Tb2 134.2(4) . . ? C14 O5 Tb1 132.8(4) . 1_565 ? C20 O6 Tb1 140.3(4) . . ? C20 O7 Tb2 130.5(4) . . ? S1 O8 Tb2 133.9(2) . 2_545 ? S1 O9 Tb1 135.6(2) . . ? O9 S1 O9 109.5(3) 2 . ? O9 S1 O8 108.5(2) 2 2 ? O9 S1 O8 110.5(2) . 2 ? O9 S1 O8 110.5(2) 2 . ? O9 S1 O8 108.4(2) . . ? O8 S1 O8 109.4(3) 2 . ? F3 Tb1 O9 149.13(12) . . ? F3 Tb1 O2 83.12(13) . . ? O9 Tb1 O2 99.00(14) . . ? F3 Tb1 F2 108.82(12) . . ? O9 Tb1 F2 87.35(12) . . ? O2 Tb1 F2 144.47(13) . . ? F3 Tb1 O6 76.37(12) . . ? O9 Tb1 O6 83.92(14) . . ? O2 Tb1 O6 142.08(14) . . ? F2 Tb1 O6 73.14(13) . . ? F3 Tb1 O5 133.10(12) . 1_545 ? O9 Tb1 O5 75.90(13) . 1_545 ? O2 Tb1 O5 73.82(14) . 1_545 ? F2 Tb1 O5 73.99(13) . 1_545 ? O6 Tb1 O5 141.93(13) . 1_545 ? F3 Tb1 F2 66.21(10) . 5_556 ? O9 Tb1 F2 144.66(12) . 5_556 ? O2 Tb1 F2 81.57(13) . 5_556 ? F2 Tb1 F2 73.78(12) . 5_556 ? O6 Tb1 F2 117.16(13) . 5_556 ? O5 Tb1 F2 70.33(12) 1_545 5_556 ? F3 Tb1 F1 70.47(12) . . ? O9 Tb1 F1 81.11(12) . . ? O2 Tb1 F1 70.77(13) . . ? F2 Tb1 F1 144.58(12) . . ? O6 Tb1 F1 72.42(13) . . ? O5 Tb1 F1 133.65(14) 1_545 . ? F2 Tb1 F1 130.66(11) 5_556 . ? F3 Tb1 Tb1 86.57(8) . 5_556 ? O9 Tb1 Tb1 119.48(9) . 5_556 ? O2 Tb1 Tb1 113.88(10) . 5_556 ? F2 Tb1 Tb1 37.77(8) . 5_556 ? O6 Tb1 Tb1 96.53(10) . 5_556 ? O5 Tb1 Tb1 67.44(10) 1_545 5_556 ? F2 Tb1 Tb1 36.01(7) 5_556 5_556 ? F1 Tb1 Tb1 156.16(9) . 5_556 ? F3 Tb1 Tb2 35.04(7) . 5_566 ? O9 Tb1 Tb2 167.85(9) . 5_566 ? O2 Tb1 Tb2 69.02(11) . 5_566 ? F2 Tb1 Tb2 101.26(8) . 5_566 ? O6 Tb1 Tb2 106.66(10) . 5_566 ? O5 Tb1 Tb2 98.08(9) 1_545 5_566 ? F2 Tb1 Tb2 34.82(7) 5_556 5_566 ? F1 Tb1 Tb2 96.20(9) . 5_566 ? Tb1 Tb1 Tb2 66.160(10) 5_556 5_566 ? F3 Tb1 H1B 67.3 . . ? O9 Tb1 H1B 89.4 . . ? O2 Tb1 H1B 52.8 . . ? F2 Tb1 H1B 162.8 . . ? O6 Tb1 H1B 89.7 . . ? O5 Tb1 H1B 121.5 1_545 . ? F2 Tb1 H1B 116.9 5_556 . ? F1 Tb1 H1B 18.5 . . ? Tb1 Tb1 H1B 150.9 5_556 . ? Tb2 Tb1 H1B 84.8 5_566 . ? F3 Tb2 O8 156.33(12) . 2_565 ? F3 Tb2 O4 95.42(12) . . ? O8 Tb2 O4 83.42(13) 2_565 . ? F3 Tb2 F2 124.60(11) . 1_565 ? O8 Tb2 F2 78.87(12) 2_565 1_565 ? O4 Tb2 F2 83.58(12) . 1_565 ? F3 Tb2 O3 89.54(14) . 5_566 ? O8 Tb2 O3 102.16(15) 2_565 5_566 ? O4 Tb2 O3 153.19(14) . 5_566 ? F2 Tb2 O3 72.06(13) 1_565 5_566 ? F3 Tb2 O7 83.26(12) . . ? O8 Tb2 O7 81.61(13) 2_565 . ? O4 Tb2 O7 136.75(14) . . ? F2 Tb2 O7 132.06(12) 1_565 . ? O3 Tb2 O7 69.97(14) 5_566 . ? F3 Tb2 F3 62.28(12) . 5_566 ? O8 Tb2 F3 137.97(12) 2_565 5_566 ? O4 Tb2 F3 72.59(12) . 5_566 ? F2 Tb2 F3 64.82(10) 1_565 5_566 ? O3 Tb2 F3 86.71(13) 5_566 5_566 ? O7 Tb2 F3 138.68(12) . 5_566 ? F3 Tb2 F1 70.95(12) . . ? O8 Tb2 F1 86.73(13) 2_565 . ? O4 Tb2 F1 69.14(13) . . ? F2 Tb2 F1 150.47(12) 1_565 . ? O3 Tb2 F1 136.76(13) 5_566 . ? O7 Tb2 F1 69.69(13) . . ? F3 Tb2 F1 114.63(11) 5_566 . ? F3 Tb2 Tb1 88.61(7) . 5_566 ? O8 Tb2 Tb1 114.85(9) 2_565 5_566 ? O4 Tb2 Tb1 86.88(10) . 5_566 ? F2 Tb2 Tb1 36.00(8) 1_565 5_566 ? O3 Tb2 Tb1 66.87(10) 5_566 5_566 ? O7 Tb2 Tb1 136.08(10) . 5_566 ? F3 Tb2 Tb1 32.36(7) 5_566 5_566 ? F1 Tb2 Tb1 146.09(9) . 5_566 ? F3 Tb2 H1B 68.0 . . ? O8 Tb2 H1B 93.3 2_565 . ? O4 Tb2 H1B 52.6 . . ? F2 Tb2 H1B 136.2 1_565 . ? O3 Tb2 H1B 150.6 5_566 . ? O7 Tb2 H1B 88.1 . . ? F3 Tb2 H1B 98.4 5_566 . ? F1 Tb2 H1B 18.8 . . ? Tb1 Tb2 H1B 128.2 5_566 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.267 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.165 _database_code_depnum_ccdc_archive 'CCDC 964398' ####################################################################### # # 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_III-B #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H26 Cu5 Dy4 F5 N10 O17 S' _chemical_formula_sum 'C40 H26 Cu5 Dy4 F5 N10 O17 S' _chemical_formula_weight 2013.53 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.632(4) _cell_length_b 7.7785(7) _cell_length_c 17.7721(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.2120(10) _cell_angle_gamma 90.00 _cell_volume 5161.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4729 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.39 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3768 _exptl_absorpt_coefficient_mu 7.868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.165 _exptl_absorpt_correction_T_max 0.207 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12836 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.39 _reflns_number_total 4729 _reflns_number_gt 4120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0435P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000101(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4729 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.2521(2) 0.4780(12) 0.3214(4) 0.044(2) Uani 1 1 d . . . C2 C 0.2515(2) 0.4106(11) 0.0691(4) 0.040(2) Uani 1 1 d . . . C5 C 0.12542(7) 0.2673(3) 0.50285(18) 0.0269(15) Uani 1 1 d G . . C6 C 0.14807(9) 0.3070(4) 0.56848(14) 0.0369(18) Uani 1 1 d G . . H6 H 0.1385 0.3433 0.6116 0.044 Uiso 1 1 calc R . . C7 C 0.18494(9) 0.2922(4) 0.56964(16) 0.046(2) Uani 1 1 d G . . H7 H 0.2001 0.3187 0.6136 0.055 Uiso 1 1 calc R . . N3 N 0.19917(7) 0.2379(4) 0.5052(2) 0.0387(15) Uani 1 1 d G . . C3 C 0.17652(9) 0.1983(3) 0.43955(18) 0.0393(19) Uani 1 1 d G . . H3 H 0.1860 0.1619 0.3964 0.047 Uiso 1 1 calc R . . C4 C 0.13965(8) 0.2130(3) 0.43839(17) 0.0345(17) Uani 1 1 d G . . H4 H 0.1245 0.1865 0.3945 0.041 Uiso 1 1 calc R . . C13 C 0.16233(9) 0.7718(3) 0.50769(18) 0.043(2) Uani 1 1 d G . . H13 H 0.1770 0.8139 0.5496 0.051 Uiso 1 1 calc R . . C12 C 0.12557(9) 0.7992(3) 0.50100(19) 0.0318(16) Uani 1 1 d G . . H12 H 0.1157 0.8597 0.5384 0.038 Uiso 1 1 calc R . . C11 C 0.10360(8) 0.7363(4) 0.43834(19) 0.0228(14) Uani 1 1 d G . . C10 C 0.11839(8) 0.6459(4) 0.38238(15) 0.0290(16) Uani 1 1 d G . . H10 H 0.1037 0.6038 0.3405 0.035 Uiso 1 1 calc R . . C9 C 0.15516(8) 0.6185(4) 0.38907(14) 0.0363(18) Uani 1 1 d G . . H9 H 0.1651 0.5581 0.3516 0.044 Uiso 1 1 calc R . . N4 N 0.17713(7) 0.6815(3) 0.45172(18) 0.0342(14) Uani 1 1 d G . . C8 C 0.08508(17) 0.3044(8) 0.4992(4) 0.0271(15) Uani 1 1 d . . . C14 C 0.06390(16) 0.7736(8) 0.4304(3) 0.0190(13) Uani 1 1 d . . . C15 C -0.1448(2) -0.0191(12) 0.2562(5) 0.052(2) Uani 1 1 d . . . H15 H -0.1486 -0.1341 0.2433 0.062 Uiso 1 1 calc R . . C16 C -0.1102(2) 0.0354(10) 0.2780(4) 0.0397(19) Uani 1 1 d . . . H16 H -0.0912 -0.0419 0.2806 0.048 Uiso 1 1 calc R . . C17 C -0.10419(17) 0.2064(9) 0.2958(3) 0.0231(14) Uani 1 1 d . . . C18 C -0.1334(2) 0.3175(10) 0.2891(4) 0.0407(19) Uani 1 1 d . . . H18 H -0.1302 0.4346 0.2978 0.049 Uiso 1 1 calc R . . C19 C -0.1677(2) 0.2500(12) 0.2690(5) 0.048(2) Uani 1 1 d . . . H19 H -0.1873 0.3234 0.2671 0.058 Uiso 1 1 calc R . . C20 C -0.06707(17) 0.2700(8) 0.3271(3) 0.0203(13) Uani 1 1 d . . . Cu1 Cu 0.27470(3) 0.48801(15) 0.23436(5) 0.0455(3) Uani 1 1 d . . . Cu2 Cu 0.23047(3) 0.61662(15) 0.46768(5) 0.0455(3) Uani 1 1 d . . . Cu3 Cu 0.2500 0.2500 0.5000 0.0646(5) Uani 1 2 d S . . Dy1 Dy 0.012208(7) 0.12650(3) 0.414851(15) 0.01439(11) Uani 1 1 d . . . Dy2 Dy -0.017621(7) 0.60317(3) 0.398442(15) 0.01430(11) Uani 1 1 d . . . F1 F 0.01190(12) 0.3800(5) 0.3261(2) 0.0325(11) Uani 0.50 1 d P . . F2 F -0.01986(10) -0.1145(4) 0.4471(2) 0.0274(9) Uani 1 1 d . . . F3 F -0.00855(10) 0.3634(4) 0.47000(18) 0.0206(8) Uani 1 1 d . . . N1 N 0.2405(2) 0.4995(12) 0.3769(5) 0.065(2) Uani 1 1 d . . . N2 N 0.26120(18) 0.4448(10) 0.1312(4) 0.0449(17) Uani 1 1 d . . . N5 N -0.17333(17) 0.0856(9) 0.2525(3) 0.0394(16) Uani 1 1 d . . . O1W O 0.01190(12) 0.3800(5) 0.3261(2) 0.0325(11) Uani 0.50 1 d P . . H1A H 0.0164 0.3906 0.2823 0.039 Uiso 0.50 1 d PR . . H1B H 0.0308 0.4107 0.3537 0.039 Uiso 0.50 1 d PR . . O2 O 0.06643(12) 0.2698(6) 0.4372(3) 0.0287(11) Uani 1 1 d . . . O3 O 0.07415(12) 0.3601(6) 0.5572(3) 0.0346(12) Uani 1 1 d . . . O4 O 0.04326(11) 0.6641(6) 0.3977(2) 0.0236(10) Uani 1 1 d . . . O5 O 0.05589(12) 0.9151(6) 0.4569(3) 0.0272(11) Uani 1 1 d . . . O6 O -0.04579(12) 0.1555(6) 0.3540(2) 0.0264(10) Uani 1 1 d . . . O7 O -0.06173(12) 0.4287(6) 0.3257(3) 0.0279(11) Uani 1 1 d . . . O8 O 0.02451(11) -0.2370(5) 0.2117(2) 0.0195(9) Uani 1 1 d . . . O9 O 0.02157(11) -0.0182(5) 0.3056(2) 0.0210(10) Uani 1 1 d . . . S1 S 0.0000 -0.1276(3) 0.2500 0.0165(5) 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 0.028(4) 0.073(6) 0.032(4) -0.012(4) 0.005(3) -0.011(4) C2 0.029(4) 0.061(6) 0.031(4) -0.002(4) 0.006(3) -0.016(4) C5 0.014(3) 0.034(4) 0.033(4) -0.002(3) 0.006(3) -0.004(3) C6 0.023(4) 0.049(5) 0.040(4) -0.011(4) 0.007(3) 0.001(3) C7 0.024(4) 0.066(6) 0.047(5) -0.008(4) -0.001(4) 0.001(4) N3 0.016(3) 0.050(4) 0.050(4) 0.006(3) 0.005(3) 0.003(3) C3 0.020(4) 0.059(5) 0.041(4) 0.001(4) 0.011(3) 0.010(4) C4 0.028(4) 0.046(5) 0.029(4) -0.006(3) 0.003(3) 0.003(3) C13 0.033(5) 0.056(6) 0.040(4) -0.002(4) 0.005(4) 0.004(4) C12 0.023(4) 0.038(4) 0.033(4) -0.007(3) 0.000(3) 0.003(3) C11 0.026(4) 0.017(3) 0.025(3) 0.002(2) 0.002(3) 0.002(3) C10 0.019(4) 0.038(4) 0.030(4) -0.004(3) 0.005(3) 0.004(3) C9 0.025(4) 0.049(5) 0.037(4) 0.001(3) 0.009(3) 0.005(3) N4 0.021(3) 0.046(4) 0.036(3) 0.003(3) 0.004(3) 0.003(3) C8 0.021(4) 0.015(3) 0.046(4) -0.002(3) 0.009(3) 0.000(3) C14 0.019(3) 0.018(3) 0.021(3) 0.002(2) 0.005(3) 0.003(3) C15 0.038(5) 0.041(5) 0.073(6) -0.016(4) -0.007(4) -0.014(4) C16 0.029(4) 0.029(4) 0.060(5) -0.011(4) 0.000(4) -0.006(3) C17 0.020(3) 0.027(4) 0.023(3) 0.004(3) 0.002(3) 0.001(3) C18 0.031(4) 0.032(4) 0.057(5) -0.007(4) -0.002(4) 0.005(3) C19 0.028(4) 0.056(6) 0.057(5) -0.005(4) -0.004(4) -0.001(4) C20 0.019(3) 0.021(4) 0.021(3) -0.007(3) 0.003(3) -0.001(3) Cu1 0.0329(6) 0.0714(8) 0.0319(5) -0.0072(5) 0.0031(4) -0.0122(5) Cu2 0.0233(5) 0.0818(9) 0.0313(5) 0.0047(5) 0.0028(4) 0.0105(5) Cu3 0.0139(7) 0.1196(17) 0.0614(10) -0.0118(10) 0.0095(7) 0.0040(8) Dy1 0.01530(19) 0.01388(18) 0.01400(17) -0.00126(10) 0.00183(12) -0.00006(10) Dy2 0.01575(19) 0.01355(18) 0.01349(17) 0.00176(10) 0.00138(12) -0.00152(10) F1 0.034(3) 0.024(3) 0.039(3) -0.0069(18) 0.001(2) 0.0001(18) F2 0.031(2) 0.023(2) 0.028(2) 0.0014(14) 0.0021(17) -0.0019(16) F3 0.031(2) 0.0110(18) 0.0184(17) 0.0012(13) -0.0013(15) 0.0027(14) N1 0.043(5) 0.089(7) 0.061(5) -0.001(5) 0.006(4) 0.014(4) N2 0.036(4) 0.059(5) 0.039(4) -0.007(3) 0.000(3) -0.016(3) N5 0.028(4) 0.055(5) 0.035(3) -0.004(3) 0.003(3) -0.012(3) O1W 0.034(3) 0.024(3) 0.039(3) -0.0069(18) 0.001(2) 0.0001(18) O2 0.022(3) 0.026(3) 0.037(3) 0.003(2) -0.001(2) -0.007(2) O3 0.020(3) 0.037(3) 0.050(3) -0.014(2) 0.015(2) -0.007(2) O4 0.018(2) 0.019(2) 0.033(2) -0.0046(19) 0.0022(19) -0.0006(18) O5 0.025(3) 0.024(3) 0.032(3) -0.005(2) -0.002(2) 0.0020(19) O6 0.023(3) 0.022(2) 0.032(2) -0.0007(19) -0.006(2) -0.0006(19) O7 0.030(3) 0.016(2) 0.037(3) -0.003(2) 0.000(2) -0.001(2) O8 0.028(3) 0.015(2) 0.017(2) -0.0044(16) 0.0066(18) 0.0025(17) O9 0.027(3) 0.018(2) 0.017(2) -0.0062(17) 0.0007(18) -0.0011(18) S1 0.0252(12) 0.0121(11) 0.0126(10) 0.000 0.0036(9) 0.000 _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 N1 1.141(10) . ? C1 Cu1 1.857(8) . ? C2 N2 1.149(10) . ? C2 Cu2 1.887(8) 6_565 ? C2 Cu2 2.496(9) 4_545 ? C5 C6 1.3900 . ? C5 C4 1.3900 . ? C5 C8 1.539(7) . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 N3 1.3900 . ? C7 H7 0.9300 . ? N3 C3 1.3900 . ? N3 Cu3 1.929(3) . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C13 N4 1.3901 . ? C13 C12 1.3903 . ? C13 H13 0.9300 . ? C12 C11 1.3900 . ? C12 H12 0.9300 . ? C11 C10 1.3899 . ? C11 C14 1.511(7) . ? C10 C9 1.3902 . ? C10 H10 0.9300 . ? C9 N4 1.3899 . ? C9 H9 0.9300 . ? N4 Cu2 2.055(3) . ? C8 O3 1.236(8) . ? C8 O2 1.258(8) . ? C14 O4 1.246(7) . ? C14 O5 1.248(7) . ? C15 N5 1.342(11) . ? C15 C16 1.377(10) . ? C15 H15 0.9300 . ? C16 C17 1.380(10) . ? C16 H16 0.9300 . ? C17 C18 1.391(10) . ? C17 C20 1.520(8) . ? C18 C19 1.398(11) . ? C18 H18 0.9300 . ? C19 N5 1.323(10) . ? C19 H19 0.9300 . ? C20 O6 1.252(7) . ? C20 O7 1.252(7) . ? Cu1 N2 1.871(7) . ? Cu1 N5 2.085(6) 3 ? Cu2 C2 1.887(8) 6_566 ? Cu2 N1 1.931(9) . ? Cu2 C2 2.496(9) 4 ? Cu2 Cu2 2.713(2) 7_566 ? Cu2 Cu3 2.9827(11) . ? Cu3 N3 1.929(3) 7_556 ? Cu3 Cu2 2.9827(11) 7_556 ? Dy1 F3 2.271(3) . ? Dy1 O9 2.309(4) . ? Dy1 O2 2.315(4) . ? Dy1 O6 2.322(4) . ? Dy1 F2 2.340(4) . ? Dy1 O5 2.378(4) 1_545 ? Dy1 F2 2.436(4) 5_556 ? Dy1 F1 2.524(4) . ? Dy1 Dy1 3.8177(6) 5_556 ? Dy1 Dy2 3.9120(5) 5_566 ? Dy2 F3 2.259(3) . ? Dy2 O8 2.306(4) 2_565 ? Dy2 O4 2.341(4) . ? Dy2 F2 2.365(4) 1_565 ? Dy2 O3 2.377(5) 5_566 ? Dy2 O7 2.393(4) . ? Dy2 F3 2.434(3) 5_566 ? Dy2 F1 2.502(4) . ? Dy2 Dy1 3.9119(5) 5_566 ? Dy2 H1B 2.5609 . ? F1 H1A 0.8206 . ? F1 H1B 0.8454 . ? F2 Dy2 2.366(4) 1_545 ? F2 Dy1 2.436(4) 5_556 ? F3 Dy2 2.434(3) 5_566 ? N5 Cu1 2.085(6) 3_445 ? O3 Dy2 2.377(5) 5_566 ? O5 Dy1 2.379(4) 1_565 ? O8 S1 1.482(4) . ? O8 Dy2 2.306(4) 2_545 ? O9 S1 1.469(4) . ? S1 O9 1.469(4) 2 ? S1 O8 1.482(4) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cu1 168.4(9) . . ? N2 C2 Cu2 171.0(8) . 6_565 ? N2 C2 Cu2 113.5(7) . 4_545 ? Cu2 C2 Cu2 75.1(3) 6_565 4_545 ? C6 C5 C4 120.0 . . ? C6 C5 C8 119.5(3) . . ? C4 C5 C8 120.1(3) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 N3 120.0 . . ? C6 C7 H7 120.0 . . ? N3 C7 H7 120.0 . . ? C7 N3 C3 120.0 . . ? C7 N3 Cu3 120.76(17) . . ? C3 N3 Cu3 118.56(17) . . ? C4 C3 N3 120.0 . . ? C4 C3 H3 120.0 . . ? N3 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N4 C13 C12 120.0 . . ? N4 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 C14 120.7(3) . . ? C12 C11 C14 119.2(3) . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? N4 C9 C10 120.0 . . ? N4 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 N4 C13 120.0 . . ? C9 N4 Cu2 119.78(15) . . ? C13 N4 Cu2 119.83(15) . . ? O3 C8 O2 126.7(6) . . ? O3 C8 C5 117.4(6) . . ? O2 C8 C5 115.9(5) . . ? O4 C14 O5 127.7(6) . . ? O4 C14 C11 117.6(5) . . ? O5 C14 C11 114.7(5) . . ? N5 C15 C16 123.3(8) . . ? N5 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C15 C16 C17 118.9(7) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 118.3(6) . . ? C16 C17 C20 121.0(6) . . ? C18 C17 C20 120.6(6) . . ? C17 C18 C19 118.9(8) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? N5 C19 C18 122.4(8) . . ? N5 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? O6 C20 O7 127.8(6) . . ? O6 C20 C17 115.0(6) . . ? O7 C20 C17 117.1(6) . . ? C1 Cu1 N2 135.4(3) . . ? C1 Cu1 N5 113.8(3) . 3 ? N2 Cu1 N5 110.6(3) . 3 ? C2 Cu2 N1 130.0(3) 6_566 . ? C2 Cu2 N4 116.4(3) 6_566 . ? N1 Cu2 N4 106.9(3) . . ? C2 Cu2 C2 104.9(3) 6_566 4 ? N1 Cu2 C2 97.2(3) . 4 ? N4 Cu2 C2 91.84(19) . 4 ? C2 Cu2 Cu2 62.7(3) 6_566 7_566 ? N1 Cu2 Cu2 124.2(3) . 7_566 ? N4 Cu2 Cu2 109.79(10) . 7_566 ? C2 Cu2 Cu2 42.22(18) 4 7_566 ? C2 Cu2 Cu3 69.2(3) 6_566 . ? N1 Cu2 Cu3 68.9(3) . . ? N4 Cu2 Cu3 118.30(8) . . ? C2 Cu2 Cu3 149.09(17) 4 . ? Cu2 Cu2 Cu3 122.84(5) 7_566 . ? N3 Cu3 N3 180.0(3) 7_556 . ? N3 Cu3 Cu2 99.55(17) 7_556 . ? N3 Cu3 Cu2 80.45(8) . . ? N3 Cu3 Cu2 80.45(17) 7_556 7_556 ? N3 Cu3 Cu2 99.55(8) . 7_556 ? Cu2 Cu3 Cu2 180.0 . 7_556 ? F3 Dy1 O9 148.79(13) . . ? F3 Dy1 O2 83.04(15) . . ? O9 Dy1 O2 98.91(16) . . ? F3 Dy1 O6 76.59(14) . . ? O9 Dy1 O6 83.64(15) . . ? O2 Dy1 O6 142.18(16) . . ? F3 Dy1 F2 109.17(13) . . ? O9 Dy1 F2 87.33(14) . . ? O2 Dy1 F2 144.51(14) . . ? O6 Dy1 F2 73.05(15) . . ? F3 Dy1 O5 133.39(13) . 1_545 ? O9 Dy1 O5 75.81(15) . 1_545 ? O2 Dy1 O5 73.71(16) . 1_545 ? O6 Dy1 O5 141.78(15) . 1_545 ? F2 Dy1 O5 74.11(15) . 1_545 ? F3 Dy1 F2 66.42(11) . 5_556 ? O9 Dy1 F2 144.79(13) . 5_556 ? O2 Dy1 F2 81.67(14) . 5_556 ? O6 Dy1 F2 117.28(15) . 5_556 ? F2 Dy1 F2 73.85(14) . 5_556 ? O5 Dy1 F2 70.58(14) 1_545 5_556 ? F3 Dy1 F1 70.18(13) . . ? O9 Dy1 F1 81.06(14) . . ? O2 Dy1 F1 70.50(15) . . ? O6 Dy1 F1 72.70(15) . . ? F2 Dy1 F1 144.80(13) . . ? O5 Dy1 F1 133.26(15) 1_545 . ? F2 Dy1 F1 130.53(12) 5_556 . ? F3 Dy1 Dy1 86.91(9) . 5_556 ? O9 Dy1 Dy1 119.52(11) . 5_556 ? O2 Dy1 Dy1 113.99(11) . 5_556 ? O6 Dy1 Dy1 96.53(12) . 5_556 ? F2 Dy1 Dy1 37.79(9) . 5_556 ? O5 Dy1 Dy1 67.67(12) 1_545 5_556 ? F2 Dy1 Dy1 36.06(8) 5_556 5_556 ? F1 Dy1 Dy1 156.25(10) . 5_556 ? F3 Dy1 Dy2 35.11(8) . 5_566 ? O9 Dy1 Dy2 167.95(10) . 5_566 ? O2 Dy1 Dy2 69.18(12) . 5_566 ? O6 Dy1 Dy2 106.79(11) . 5_566 ? F2 Dy1 Dy2 101.33(9) . 5_566 ? O5 Dy1 Dy2 98.33(10) 1_545 5_566 ? F2 Dy1 Dy2 34.84(8) 5_556 5_566 ? F1 Dy1 Dy2 96.06(9) . 5_566 ? Dy1 Dy1 Dy2 66.220(10) 5_556 5_566 ? F3 Dy2 O8 156.35(13) . 2_565 ? F3 Dy2 O4 95.24(14) . . ? O8 Dy2 O4 83.80(15) 2_565 . ? F3 Dy2 F2 124.78(12) . 1_565 ? O8 Dy2 F2 78.72(13) 2_565 1_565 ? O4 Dy2 F2 83.90(14) . 1_565 ? F3 Dy2 O3 89.48(16) . 5_566 ? O8 Dy2 O3 101.93(17) 2_565 5_566 ? O4 Dy2 O3 153.46(15) . 5_566 ? F2 Dy2 O3 72.11(15) 1_565 5_566 ? F3 Dy2 O7 83.19(14) . . ? O8 Dy2 O7 81.43(15) 2_565 . ? O4 Dy2 O7 136.46(15) . . ? F2 Dy2 O7 132.04(14) 1_565 . ? O3 Dy2 O7 70.01(16) 5_566 . ? F3 Dy2 F3 62.18(13) . 5_566 ? O8 Dy2 F3 138.27(13) 2_565 5_566 ? O4 Dy2 F3 72.85(13) . 5_566 ? F2 Dy2 F3 65.05(12) 1_565 5_566 ? O3 Dy2 F3 86.55(15) 5_566 5_566 ? O7 Dy2 F3 138.49(14) . 5_566 ? F3 Dy2 F1 70.78(13) . . ? O8 Dy2 F1 87.02(14) 2_565 . ? O4 Dy2 F1 68.89(14) . . ? F2 Dy2 F1 150.52(13) 1_565 . ? O3 Dy2 F1 136.67(15) 5_566 . ? O7 Dy2 F1 69.62(15) . . ? F3 Dy2 F1 114.55(13) 5_566 . ? F3 Dy2 Dy1 88.75(8) . 5_566 ? O8 Dy2 Dy1 114.73(10) 2_565 5_566 ? O4 Dy2 Dy1 87.06(10) . 5_566 ? F2 Dy2 Dy1 36.03(9) 1_565 5_566 ? O3 Dy2 Dy1 66.90(11) 5_566 5_566 ? O7 Dy2 Dy1 136.18(12) . 5_566 ? F3 Dy2 Dy1 32.45(8) 5_566 5_566 ? F1 Dy2 Dy1 146.06(10) . 5_566 ? F3 Dy2 H1B 68.2 . . ? O8 Dy2 H1B 93.5 2_565 . ? O4 Dy2 H1B 51.8 . . ? F2 Dy2 H1B 135.7 1_565 . ? O3 Dy2 H1B 151.0 5_566 . ? O7 Dy2 H1B 88.5 . . ? F3 Dy2 H1B 98.2 5_566 . ? F1 Dy2 H1B 19.2 . . ? Dy1 Dy2 H1B 127.9 5_566 . ? Dy2 F1 Dy1 100.87(16) . . ? Dy2 F1 H1A 125.1 . . ? Dy1 F1 H1A 133.3 . . ? Dy2 F1 H1B 84.4 . . ? Dy1 F1 H1B 85.5 . . ? H1A F1 H1B 105.3 . . ? Dy1 F2 Dy2 127.67(17) . 1_545 ? Dy1 F2 Dy1 106.15(14) . 5_556 ? Dy2 F2 Dy1 109.13(13) 1_545 5_556 ? Dy2 F3 Dy1 117.56(15) . . ? Dy2 F3 Dy2 117.82(13) . 5_566 ? Dy1 F3 Dy2 112.43(13) . 5_566 ? C1 N1 Cu2 158.2(9) . . ? C2 N2 Cu1 175.8(7) . . ? C19 N5 C15 118.1(7) . . ? C19 N5 Cu1 120.4(6) . 3_445 ? C15 N5 Cu1 121.0(6) . 3_445 ? C8 O2 Dy1 129.5(4) . . ? C8 O3 Dy2 136.4(4) . 5_566 ? C14 O4 Dy2 133.6(4) . . ? C14 O5 Dy1 132.9(4) . 1_565 ? C20 O6 Dy1 140.0(4) . . ? C20 O7 Dy2 130.6(4) . . ? S1 O8 Dy2 133.6(2) . 2_545 ? S1 O9 Dy1 135.9(3) . . ? O9 S1 O9 109.2(4) . 2 ? O9 S1 O8 110.3(2) . 2 ? O9 S1 O8 108.6(2) 2 2 ? O9 S1 O8 108.6(2) . . ? O9 S1 O8 110.3(2) 2 . ? O8 S1 O8 109.9(3) 2 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.484 _refine_diff_density_min -1.731 _refine_diff_density_rms 0.246 _database_code_depnum_ccdc_archive 'CCDC 964399' ####################################################################### # # 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_IV-A #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C87 H64 Cu9 N19 O36 Tb6, 2(H2 O)' _chemical_formula_sum 'C87 H68 Cu9 N19 O38 Tb6' _chemical_formula_weight 3513.14 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7096(9) _cell_length_b 12.7197(10) _cell_length_c 18.5102(15) _cell_angle_alpha 108.9560(10) _cell_angle_beta 95.6490(10) _cell_angle_gamma 97.9160(10) _cell_volume 2552.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9216 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 25.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1678 _exptl_absorpt_coefficient_mu 6.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.245 _exptl_absorpt_correction_T_max 0.300 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13438 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.40 _reflns_number_total 9216 _reflns_number_gt 7656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0292P)^2^+3.6165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00041(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9216 _refine_ls_number_parameters 721 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.017 _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 0.1914(5) -0.2007(5) 1.0101(3) 0.0298(13) Uani 1 1 d U . . C2 C -0.1151(5) 0.6009(6) 0.0334(3) 0.0320(14) Uani 1 1 d U . . C3 C -0.0089(6) -0.0400(5) 0.0097(3) 0.0412(16) Uani 0.50 1 d P . . C4 C 0.4818(9) 0.7504(8) 0.9753(4) 0.073(3) Uani 1 1 d U . . C5 C 0.2926(6) 0.1755(5) 0.1357(3) 0.0355(16) Uani 1 1 d . . . H5 H 0.2519 0.2070 0.1046 0.043 Uiso 1 1 calc R . . C6 C 0.3481(6) 0.2457(5) 0.2080(3) 0.0301(14) Uani 1 1 d . . . H6 H 0.3450 0.3224 0.2250 0.036 Uiso 1 1 calc R . . C7 C 0.4088(5) 0.1995(5) 0.2553(3) 0.0239(13) Uani 1 1 d . . . C8 C 0.4146(6) 0.0871(5) 0.2265(3) 0.0320(15) Uani 1 1 d . . . H8 H 0.4579 0.0545 0.2554 0.038 Uiso 1 1 calc R . . C9 C 0.3553(6) 0.0231(5) 0.1541(4) 0.0366(16) Uani 1 1 d . . . H9 H 0.3576 -0.0537 0.1360 0.044 Uiso 1 1 calc R . . C10 C 0.4622(5) 0.2689(5) 0.3375(3) 0.0216(12) Uani 1 1 d . . . C11 C 0.2535(6) 0.0392(5) 0.8786(3) 0.0348(16) Uani 1 1 d . . . H11 H 0.2504 0.1091 0.9146 0.042 Uiso 1 1 calc R . . C12 C 0.2719(6) 0.0332(5) 0.8051(3) 0.0327(15) Uani 1 1 d . . . H12 H 0.2832 0.0988 0.7928 0.039 Uiso 1 1 calc R . . C13 C 0.2735(5) -0.0691(5) 0.7500(3) 0.0253(13) Uani 1 1 d . . . C14 C 0.2598(6) -0.1619(5) 0.7721(3) 0.0345(15) Uani 1 1 d . . . H14 H 0.2618 -0.2326 0.7367 0.041 Uiso 1 1 calc R . . C15 C 0.2429(6) -0.1511(5) 0.8472(3) 0.0369(16) Uani 1 1 d . . . H15 H 0.2334 -0.2155 0.8610 0.044 Uiso 1 1 calc R . . C16 C 0.2935(5) -0.0794(5) 0.6691(3) 0.0247(13) Uani 1 1 d . . . C17 C -0.0069(6) 0.5794(6) 0.2092(4) 0.0437(18) Uani 1 1 d . . . H17 H -0.0377 0.6398 0.2025 0.052 Uiso 1 1 calc R . . C18 C 0.0571(6) 0.5947(5) 0.2799(4) 0.0373(16) Uani 1 1 d . . . H18 H 0.0669 0.6638 0.3198 0.045 Uiso 1 1 calc R . . C19 C 0.1057(5) 0.5090(5) 0.2914(3) 0.0223(12) Uani 1 1 d . . . C20 C 0.0861(6) 0.4085(5) 0.2314(3) 0.0351(15) Uani 1 1 d . . . H20 H 0.1170 0.3476 0.2372 0.042 Uiso 1 1 calc R . . C21 C 0.0203(6) 0.3973(6) 0.1622(4) 0.0418(18) Uani 1 1 d . . . H21 H 0.0078 0.3281 0.1222 0.050 Uiso 1 1 calc R . . C22 C 0.1778(5) 0.5243(5) 0.3674(3) 0.0216(13) Uani 1 1 d . . . C23 C 0.1109(7) -0.1147(5) 0.2112(4) 0.0438(19) Uani 1 1 d . . . H23 H 0.1124 -0.1915 0.1900 0.053 Uiso 1 1 calc R . . C24 C 0.1709(6) -0.0562(5) 0.2846(3) 0.0375(16) Uani 1 1 d . . . H24 H 0.2115 -0.0928 0.3119 0.045 Uiso 1 1 calc R . . C25 C 0.1695(5) 0.0580(5) 0.3169(3) 0.0247(13) Uani 1 1 d . . . C26 C 0.1069(5) 0.1078(5) 0.2744(3) 0.0304(14) Uani 1 1 d . . . H26 H 0.1034 0.1842 0.2944 0.036 Uiso 1 1 calc R . . C27 C 0.0496(6) 0.0420(5) 0.2017(4) 0.0389(17) Uani 1 1 d . . . H27 H 0.0073 0.0764 0.1736 0.047 Uiso 1 1 calc R . . C28 C 0.2411(5) 0.1267(5) 0.3944(3) 0.0238(13) Uani 1 1 d . . . C29 C 0.3230(7) 0.4002(6) 0.8457(4) 0.0465(19) Uani 1 1 d . . . H29 H 0.3091 0.3628 0.8804 0.056 Uiso 1 1 calc R . . C30 C 0.3127(6) 0.3361(5) 0.7688(3) 0.0373(16) Uani 1 1 d . . . H30 H 0.2908 0.2579 0.7524 0.045 Uiso 1 1 calc R . . C31 C 0.3351(5) 0.3891(5) 0.7169(3) 0.0249(13) Uani 1 1 d . . . C32 C 0.3635(7) 0.5054(5) 0.7437(3) 0.0443(19) Uani 1 1 d . . . H32 H 0.3764 0.5444 0.7097 0.053 Uiso 1 1 calc R . . C33 C 0.3724(8) 0.5626(6) 0.8219(4) 0.056(2) Uani 1 1 d . . . H33 H 0.3941 0.6409 0.8398 0.067 Uiso 1 1 calc R . . C34 C 0.3370(5) 0.3228(5) 0.6325(3) 0.0208(12) Uani 1 1 d . . . C35 C 0.5575(7) 0.2565(6) 0.8627(4) 0.0455(19) Uani 1 1 d . . . H35 H 0.5245 0.2094 0.8874 0.055 Uiso 1 1 calc R . . C36 C 0.5527(7) 0.2136(6) 0.7840(3) 0.0431(19) Uani 1 1 d . . . H36 H 0.5182 0.1388 0.7568 0.052 Uiso 1 1 calc R . . C37 C 0.5990(5) 0.2815(5) 0.7452(3) 0.0237(13) Uani 1 1 d . . . C38 C 0.6463(6) 0.3909(6) 0.7883(3) 0.0431(18) Uani 1 1 d . . . H38 H 0.6763 0.4404 0.7645 0.052 Uiso 1 1 calc R . . C39 C 0.6496(7) 0.4282(6) 0.8681(4) 0.050(2) Uani 1 1 d . . . H39 H 0.6832 0.5028 0.8968 0.060 Uiso 1 1 calc R . . C40 C 0.5886(5) 0.2332(5) 0.6579(3) 0.0215(12) Uani 1 1 d . . . C41 C 0.1493(5) -0.0966(5) 0.5042(3) 0.0291(14) Uani 1 1 d . . . C42 C 0.0358(6) -0.1745(6) 0.4904(5) 0.055(2) Uani 1 1 d . . . H42A H 0.0172 -0.1795 0.5387 0.082 Uiso 1 1 calc R . . H42B H 0.0414 -0.2481 0.4563 0.082 Uiso 1 1 calc R . . H42C H -0.0245 -0.1460 0.4674 0.082 Uiso 1 1 calc R . . C43 C 0.1789(5) 0.5274(5) 0.5545(3) 0.0273(14) Uani 1 1 d . . . C44 C 0.0935(6) 0.5847(6) 0.6015(4) 0.050(2) Uani 1 1 d . . . H44A H 0.0160 0.5560 0.5733 0.074 Uiso 1 1 calc R . . H44B H 0.1120 0.6647 0.6121 0.074 Uiso 1 1 calc R . . H44C H 0.0978 0.5701 0.6494 0.074 Uiso 1 1 calc R . . Cu1 Cu 0.21699(9) -0.04834(8) 1.00682(4) 0.0484(3) Uani 1 1 d . . . Cu2 Cu -0.12699(8) 0.45612(7) 0.04080(5) 0.0440(2) Uani 1 1 d . . . Cu3 Cu -0.02280(9) -0.15509(7) 0.05335(5) 0.0476(2) Uani 1 1 d . . . Cu4 Cu 0.37834(10) 0.60202(10) 0.98288(5) 0.0642(3) Uani 1 1 d . . . Cu5 Cu 0.5000 1.0000 1.0000 0.0750(5) Uani 1 2 d SU . . Tb1 Tb 0.34621(2) -0.26771(2) 0.509451(14) 0.01592(8) Uani 1 1 d . . . Tb2 Tb 0.37023(2) 0.04845(2) 0.542128(14) 0.01835(8) Uani 1 1 d . . . Tb3 Tb 0.34547(2) 0.41763(2) 0.474164(14) 0.01724(8) Uani 1 1 d . . . N1 N 0.1780(5) -0.2978(5) 0.9971(3) 0.0479(15) Uani 1 1 d U . . N2 N -0.0931(6) 0.6935(5) 0.0378(3) 0.0485(16) Uani 1 1 d U . . N3 N -0.0089(6) -0.0400(5) 0.0097(3) 0.0412(16) Uani 0.50 1 d P . . N4 N 0.4911(7) 0.8368(8) 0.9827(4) 0.082(3) Uani 1 1 d U . . N5 N 0.2943(5) 0.0653(4) 0.1079(3) 0.0304(12) Uani 1 1 d . . . N6 N 0.2400(5) -0.0515(4) 0.9001(3) 0.0309(12) Uani 1 1 d . . . N7 N -0.0261(5) 0.4821(5) 0.1504(3) 0.0391(14) Uani 1 1 d . . . N8 N 0.0510(5) -0.0676(4) 0.1692(3) 0.0353(13) Uani 1 1 d . . . N9 N 0.3515(5) 0.5117(5) 0.8734(3) 0.0430(15) Uani 1 1 d . . . N10 N 0.6063(5) 0.3608(5) 0.9050(3) 0.0392(14) Uani 1 1 d . . . O1 O 0.4443(4) 0.3675(3) 0.3635(2) 0.0266(9) Uani 1 1 d . . . O2 O 0.5163(4) 0.2194(3) 0.3743(2) 0.0297(10) Uani 1 1 d . . . O3 O 0.3436(4) 0.0061(3) 0.6584(2) 0.0322(10) Uani 1 1 d . . . O4 O 0.2598(4) -0.1755(3) 0.6184(2) 0.0296(10) Uani 1 1 d . . . O5 O 0.1819(3) 0.6156(3) 0.4218(2) 0.0285(9) Uani 1 1 d . . . O6 O 0.2301(4) 0.4468(3) 0.3707(2) 0.0323(10) Uani 1 1 d . . . O7 O 0.2825(4) 0.0749(3) 0.4337(2) 0.0322(10) Uani 1 1 d . . . O8 O 0.2570(4) 0.2322(3) 0.4117(2) 0.0309(10) Uani 1 1 d . . . O9 O 0.3320(4) 0.2203(3) 0.6153(2) 0.0332(10) Uani 1 1 d . . . O10 O 0.3475(4) 0.3782(3) 0.5886(2) 0.0291(10) Uani 1 1 d . . . O11 O 0.5500(4) 0.1291(3) 0.6282(2) 0.0270(9) Uani 1 1 d . . . O12 O 0.6171(4) 0.2988(3) 0.6228(2) 0.0271(9) Uani 1 1 d . . . O13 O 0.2401(3) -0.1349(3) 0.4786(2) 0.0239(9) Uani 1 1 d . . . O14 O 0.1600(4) 0.0054(3) 0.5420(2) 0.0346(10) Uani 1 1 d . . . O15 O 0.1530(3) 0.4260(3) 0.5133(2) 0.0355(11) Uani 1 1 d . . . O16 O 0.2808(3) 0.5836(3) 0.5581(2) 0.0215(8) Uani 1 1 d . . . O17 O 0.4796(3) -0.0977(3) 0.52820(19) 0.0178(8) Uani 1 1 d D . . H17A H 0.5054 -0.0803 0.5742 0.021 Uiso 1 1 d RD . . O18 O 0.4584(3) 0.5880(3) 0.47453(19) 0.0169(8) Uani 1 1 d D . . H18A H 0.4607 0.5810 0.4292 0.020 Uiso 1 1 d RD . . O19W O 0.0931(10) 0.1348(11) 0.6833(6) 0.224(6) Uani 1 1 d . . . H19A H 0.0252 0.1405 0.6949 0.269 Uiso 1 1 d R . . H19B H 0.0854 0.0940 0.6360 0.269 Uiso 1 1 d R . . 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 0.034(4) 0.039(2) 0.017(3) 0.012(3) 0.002(3) 0.008(3) C2 0.026(3) 0.043(3) 0.023(3) 0.010(3) -0.004(3) 0.003(3) C3 0.048(4) 0.041(4) 0.027(3) 0.004(3) -0.005(3) 0.011(3) C4 0.101(8) 0.068(6) 0.022(4) 0.008(4) 0.002(4) -0.051(6) C5 0.042(4) 0.041(4) 0.026(3) 0.018(3) -0.004(3) 0.009(3) C6 0.045(4) 0.025(3) 0.022(3) 0.012(3) 0.000(3) 0.006(3) C7 0.027(3) 0.023(3) 0.020(3) 0.005(2) 0.005(2) 0.004(2) C8 0.041(4) 0.026(3) 0.025(3) 0.003(3) -0.003(3) 0.011(3) C9 0.051(4) 0.021(3) 0.033(4) 0.002(3) 0.003(3) 0.010(3) C10 0.027(3) 0.021(3) 0.019(3) 0.008(2) 0.006(2) 0.006(2) C11 0.050(4) 0.025(3) 0.027(3) 0.004(3) 0.011(3) 0.004(3) C12 0.048(4) 0.026(3) 0.029(3) 0.013(3) 0.012(3) 0.008(3) C13 0.030(3) 0.032(3) 0.015(3) 0.006(2) 0.008(2) 0.009(3) C14 0.054(4) 0.026(3) 0.024(3) 0.007(3) 0.010(3) 0.008(3) C15 0.055(5) 0.031(4) 0.026(3) 0.012(3) 0.010(3) 0.004(3) C16 0.027(3) 0.029(3) 0.022(3) 0.011(3) 0.006(3) 0.015(3) C17 0.055(5) 0.035(4) 0.037(4) 0.013(3) -0.015(3) 0.010(3) C18 0.044(4) 0.032(4) 0.029(3) 0.008(3) -0.012(3) 0.004(3) C19 0.024(3) 0.022(3) 0.021(3) 0.008(2) -0.001(2) 0.003(2) C20 0.048(4) 0.026(3) 0.031(3) 0.010(3) 0.000(3) 0.009(3) C21 0.059(5) 0.033(4) 0.023(3) 0.001(3) -0.008(3) 0.003(3) C22 0.021(3) 0.023(3) 0.022(3) 0.014(3) 0.000(2) -0.003(2) C23 0.072(5) 0.019(3) 0.028(4) -0.001(3) -0.004(4) -0.001(3) C24 0.053(4) 0.022(3) 0.031(3) 0.005(3) -0.007(3) 0.003(3) C25 0.031(3) 0.020(3) 0.020(3) 0.008(2) -0.001(3) -0.004(2) C26 0.040(4) 0.019(3) 0.029(3) 0.008(3) -0.007(3) 0.006(3) C27 0.043(4) 0.036(4) 0.034(4) 0.013(3) -0.012(3) 0.005(3) C28 0.023(3) 0.023(3) 0.022(3) 0.005(3) 0.003(2) 0.001(2) C29 0.066(5) 0.054(5) 0.021(3) 0.016(3) 0.007(3) 0.008(4) C30 0.056(5) 0.031(4) 0.029(3) 0.012(3) 0.016(3) 0.010(3) C31 0.033(3) 0.024(3) 0.019(3) 0.007(2) 0.006(3) 0.009(3) C32 0.080(6) 0.026(4) 0.023(3) 0.003(3) 0.013(4) 0.006(3) C33 0.099(7) 0.039(4) 0.027(4) 0.003(3) 0.009(4) 0.020(4) C34 0.022(3) 0.021(3) 0.019(3) 0.006(2) 0.003(2) 0.005(2) C35 0.075(6) 0.044(4) 0.021(3) 0.014(3) 0.010(3) 0.014(4) C36 0.084(6) 0.028(4) 0.021(3) 0.011(3) 0.014(3) 0.014(4) C37 0.030(3) 0.024(3) 0.014(3) 0.002(2) -0.001(2) 0.005(2) C38 0.053(5) 0.043(4) 0.023(3) 0.003(3) 0.005(3) -0.005(3) C39 0.052(5) 0.049(5) 0.033(4) -0.001(3) 0.000(4) -0.008(4) C40 0.025(3) 0.021(3) 0.018(3) 0.006(2) 0.001(2) 0.007(2) C41 0.031(4) 0.023(3) 0.037(4) 0.013(3) 0.003(3) 0.008(3) C42 0.034(4) 0.041(4) 0.078(6) 0.008(4) 0.009(4) 0.005(3) C43 0.026(3) 0.029(3) 0.034(3) 0.018(3) 0.011(3) 0.008(3) C44 0.033(4) 0.050(5) 0.059(5) 0.004(4) 0.029(4) 0.005(3) Cu1 0.0761(7) 0.0444(5) 0.0162(4) 0.0036(4) 0.0009(4) 0.0036(5) Cu2 0.0521(6) 0.0404(5) 0.0374(5) 0.0147(4) -0.0056(4) 0.0065(4) Cu3 0.0614(6) 0.0362(5) 0.0332(5) 0.0040(4) -0.0078(4) -0.0006(4) Cu4 0.0738(7) 0.0845(8) 0.0174(4) -0.0007(5) 0.0062(4) 0.0042(6) Cu5 0.0737(11) 0.0913(12) 0.0495(9) 0.0245(8) 0.0045(8) -0.0168(9) Tb1 0.02152(15) 0.01225(13) 0.01322(13) 0.00356(10) 0.00149(10) 0.00334(10) Tb2 0.02602(16) 0.01352(14) 0.01558(14) 0.00440(11) 0.00387(11) 0.00475(11) Tb3 0.02066(15) 0.01328(14) 0.01626(14) 0.00419(10) 0.00025(11) 0.00210(10) N1 0.057(4) 0.042(3) 0.045(3) 0.016(3) 0.001(3) 0.011(3) N2 0.058(4) 0.043(3) 0.038(3) 0.009(3) 0.001(3) 0.003(3) N3 0.048(4) 0.041(4) 0.027(3) 0.004(3) -0.005(3) 0.011(3) N4 0.070(6) 0.126(6) 0.040(4) 0.027(5) 0.009(4) -0.021(6) N5 0.040(3) 0.027(3) 0.022(3) 0.006(2) 0.003(2) 0.003(2) N6 0.043(3) 0.034(3) 0.013(2) 0.006(2) 0.002(2) 0.005(2) N7 0.050(4) 0.033(3) 0.030(3) 0.012(3) -0.016(3) 0.007(3) N8 0.049(4) 0.028(3) 0.022(3) 0.006(2) -0.002(2) -0.003(3) N9 0.058(4) 0.043(4) 0.024(3) 0.002(3) 0.012(3) 0.018(3) N10 0.042(3) 0.050(4) 0.020(3) 0.006(3) 0.002(2) 0.011(3) O1 0.038(2) 0.021(2) 0.021(2) 0.0047(17) 0.0074(18) 0.0083(18) O2 0.040(3) 0.023(2) 0.021(2) 0.0060(18) -0.0093(19) 0.0025(19) O3 0.047(3) 0.029(2) 0.024(2) 0.0119(19) 0.014(2) 0.003(2) O4 0.041(3) 0.026(2) 0.022(2) 0.0033(18) 0.0152(19) 0.0112(19) O5 0.030(2) 0.026(2) 0.024(2) 0.0049(18) -0.0017(18) 0.0011(18) O6 0.036(3) 0.035(2) 0.028(2) 0.011(2) -0.0048(19) 0.014(2) O7 0.046(3) 0.032(2) 0.020(2) 0.0099(19) -0.0040(19) 0.013(2) O8 0.042(3) 0.014(2) 0.028(2) 0.0006(17) -0.002(2) -0.0017(18) O9 0.054(3) 0.018(2) 0.028(2) 0.0038(18) 0.010(2) 0.0157(19) O10 0.041(3) 0.032(2) 0.017(2) 0.0132(18) 0.0017(18) 0.0037(19) O11 0.039(3) 0.021(2) 0.018(2) 0.0057(17) 0.0018(18) 0.0040(18) O12 0.040(3) 0.023(2) 0.019(2) 0.0085(17) 0.0070(18) 0.0053(18) O13 0.026(2) 0.020(2) 0.028(2) 0.0102(17) 0.0049(18) 0.0061(17) O14 0.032(2) 0.023(2) 0.047(3) 0.006(2) 0.011(2) 0.0106(18) O15 0.025(2) 0.024(2) 0.053(3) 0.010(2) 0.006(2) -0.0006(18) O16 0.019(2) 0.023(2) 0.022(2) 0.0071(17) 0.0064(16) 0.0025(16) O17 0.025(2) 0.0153(18) 0.0127(18) 0.0037(15) 0.0035(16) 0.0050(15) O18 0.026(2) 0.0150(18) 0.0107(17) 0.0052(15) 0.0015(15) 0.0049(15) O19W 0.185(12) 0.286(16) 0.163(10) 0.027(10) 0.077(9) 0.002(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.163(8) . ? C1 Cu1 1.941(6) . ? C2 N2 1.144(8) . ? C2 Cu2 1.878(7) . ? C3 N3 1.185(12) 2 ? C3 C3 1.185(12) 2 ? C3 Cu3 1.884(6) . ? C4 N4 1.051(12) . ? C4 Cu4 2.151(8) . ? C5 N5 1.331(8) . ? C5 C6 1.380(8) . ? C5 H5 0.9300 . ? C6 C7 1.394(8) . ? C6 H6 0.9300 . ? C7 C8 1.367(8) . ? C7 C10 1.509(7) . ? C8 C9 1.375(8) . ? C8 H8 0.9300 . ? C9 N5 1.347(8) . ? C9 H9 0.9300 . ? C10 O1 1.244(6) . ? C10 O2 1.250(7) . ? C11 N6 1.331(8) . ? C11 C12 1.378(8) . ? C11 H11 0.9300 . ? C12 C13 1.372(8) . ? C12 H12 0.9300 . ? C13 C14 1.363(8) . ? C13 C16 1.506(7) . ? C14 C15 1.388(8) . ? C14 H14 0.9300 . ? C15 N6 1.334(8) . ? C15 H15 0.9300 . ? C16 O3 1.246(7) . ? C16 O4 1.257(7) . ? C17 N7 1.329(8) . ? C17 C18 1.383(8) . ? C17 H17 0.9300 . ? C18 C19 1.361(9) . ? C18 H18 0.9300 . ? C19 C20 1.366(8) . ? C19 C22 1.509(7) . ? C20 C21 1.383(8) . ? C20 H20 0.9300 . ? C21 N7 1.342(9) . ? C21 H21 0.9300 . ? C22 O6 1.244(7) . ? C22 O5 1.256(7) . ? C23 N8 1.329(9) . ? C23 C24 1.380(8) . ? C23 H23 0.9300 . ? C24 C25 1.382(8) . ? C24 H24 0.9300 . ? C25 C26 1.375(8) . ? C25 C28 1.508(7) . ? C26 C27 1.378(8) . ? C26 H26 0.9300 . ? C27 N8 1.330(8) . ? C27 H27 0.9300 . ? C28 O7 1.237(7) . ? C28 O8 1.256(7) . ? C29 N9 1.322(9) . ? C29 C30 1.375(9) . ? C29 H29 0.9300 . ? C30 C31 1.367(8) . ? C30 H30 0.9300 . ? C31 C32 1.379(8) . ? C31 C34 1.519(7) . ? C32 C33 1.379(9) . ? C32 H32 0.9300 . ? C33 N9 1.339(9) . ? C33 H33 0.9300 . ? C34 O9 1.229(6) . ? C34 O10 1.242(6) . ? C35 N10 1.314(8) . ? C35 C36 1.372(8) . ? C35 H35 0.9300 . ? C36 C37 1.380(8) . ? C36 H36 0.9300 . ? C37 C38 1.363(8) . ? C37 C40 1.517(7) . ? C38 C39 1.391(9) . ? C38 H38 0.9300 . ? C39 N10 1.337(9) . ? C39 H39 0.9300 . ? C40 O12 1.244(6) . ? C40 O11 1.254(6) . ? C41 O14 1.239(7) . ? C41 O13 1.298(7) . ? C41 C42 1.490(8) . ? C41 Tb2 2.842(6) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 O15 1.243(7) . ? C43 O16 1.287(6) . ? C43 C44 1.500(8) . ? C43 Tb3 2.818(6) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? Cu1 N5 1.990(5) 1_556 ? Cu1 N6 2.008(5) . ? Cu2 N1 1.891(6) 2_556 ? Cu2 N7 2.145(5) . ? Cu2 Cu4 2.8874(15) 2_566 ? Cu3 N2 1.904(6) 1_545 ? Cu3 N8 2.098(5) . ? Cu4 N9 1.946(5) . ? Cu4 N10 1.957(5) 2_667 ? Cu4 Cu2 2.8874(15) 2_566 ? Cu5 N4 1.981(10) 2_677 ? Cu5 N4 1.981(10) . ? Tb1 O5 2.361(4) 1_545 ? Tb1 O18 2.360(4) 1_545 ? Tb1 O4 2.378(4) . ? Tb1 O17 2.390(3) . ? Tb1 O2 2.406(4) 2_656 ? Tb1 O13 2.406(4) . ? Tb1 O16 2.413(3) 1_545 ? Tb1 O12 2.441(4) 2_656 ? Tb1 Tb2 3.8330(5) . ? Tb1 Tb3 3.8388(5) 1_545 ? Tb2 O9 2.298(4) . ? Tb2 O7 2.308(4) . ? Tb2 O17 2.361(4) . ? Tb2 O11 2.388(4) . ? Tb2 O17 2.420(3) 2_656 ? Tb2 O3 2.420(4) . ? Tb2 O14 2.446(4) . ? Tb2 O13 2.456(4) . ? Tb2 Tb2 3.7287(6) 2_656 ? Tb3 O8 2.300(4) . ? Tb3 O10 2.328(4) . ? Tb3 O18 2.376(3) . ? Tb3 O6 2.392(4) . ? Tb3 O1 2.400(4) . ? Tb3 O18 2.417(4) 2_666 ? Tb3 O15 2.440(4) . ? Tb3 O16 2.446(4) . ? Tb3 Tb3 3.7855(6) 2_666 ? Tb3 Tb1 3.8388(5) 1_565 ? N1 Cu2 1.891(6) 2_556 ? N2 Cu3 1.904(6) 1_565 ? N5 Cu1 1.990(5) 1_554 ? N10 Cu4 1.957(5) 2_667 ? O2 Tb1 2.406(4) 2_656 ? O5 Tb1 2.361(4) 1_565 ? O12 Tb1 2.441(4) 2_656 ? O16 Tb1 2.413(3) 1_565 ? O17 Tb2 2.420(3) 2_656 ? O17 H17A 0.8203 . ? O18 Tb1 2.360(4) 1_565 ? O18 Tb3 2.417(4) 2_666 ? O18 H18A 0.8172 . ? O19W H19A 0.8500 . ? O19W H19B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cu1 166.8(5) . . ? N2 C2 Cu2 169.3(6) . . ? N3 C3 C3 0.0(8) 2 2 ? N3 C3 Cu3 171.9(8) 2 . ? C3 C3 Cu3 171.9(8) 2 . ? N4 C4 Cu4 148.5(11) . . ? N5 C5 C6 123.5(6) . . ? N5 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C5 C6 C7 118.8(6) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C8 C7 C6 118.3(5) . . ? C8 C7 C10 120.1(5) . . ? C6 C7 C10 121.6(5) . . ? C7 C8 C9 119.0(6) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? N5 C9 C8 123.8(6) . . ? N5 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? O1 C10 O2 126.1(5) . . ? O1 C10 C7 117.7(5) . . ? O2 C10 C7 116.1(5) . . ? N6 C11 C12 122.5(6) . . ? N6 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 120.3(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 117.2(5) . . ? C14 C13 C16 120.8(5) . . ? C12 C13 C16 122.0(5) . . ? C13 C14 C15 120.3(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? N6 C15 C14 122.1(6) . . ? N6 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? O3 C16 O4 125.9(5) . . ? O3 C16 C13 117.9(5) . . ? O4 C16 C13 116.2(5) . . ? N7 C17 C18 122.8(6) . . ? N7 C17 H17 118.6 . . ? C18 C17 H17 118.6 . . ? C19 C18 C17 120.3(6) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 117.4(6) . . ? C18 C19 C22 121.3(5) . . ? C20 C19 C22 121.3(5) . . ? C19 C20 C21 119.9(6) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? N7 C21 C20 122.8(6) . . ? N7 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? O6 C22 O5 125.4(5) . . ? O6 C22 C19 117.5(5) . . ? O5 C22 C19 117.0(5) . . ? N8 C23 C24 123.7(6) . . ? N8 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C25 118.8(6) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 118.3(5) . . ? C26 C25 C28 121.3(5) . . ? C24 C25 C28 120.4(5) . . ? C25 C26 C27 118.6(6) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? N8 C27 C26 124.1(6) . . ? N8 C27 H27 117.9 . . ? C26 C27 H27 117.9 . . ? O7 C28 O8 125.9(5) . . ? O7 C28 C25 117.6(5) . . ? O8 C28 C25 116.4(5) . . ? N9 C29 C30 124.3(6) . . ? N9 C29 H29 117.9 . . ? C30 C29 H29 117.9 . . ? C31 C30 C29 118.9(6) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 118.4(5) . . ? C30 C31 C34 121.6(5) . . ? C32 C31 C34 119.9(5) . . ? C33 C32 C31 118.6(6) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? N9 C33 C32 123.6(7) . . ? N9 C33 H33 118.2 . . ? C32 C33 H33 118.2 . . ? O9 C34 O10 126.6(5) . . ? O9 C34 C31 116.6(5) . . ? O10 C34 C31 116.7(5) . . ? N10 C35 C36 123.3(6) . . ? N10 C35 H35 118.4 . . ? C36 C35 H35 118.4 . . ? C35 C36 C37 120.0(6) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 117.1(5) . . ? C38 C37 C40 124.0(5) . . ? C36 C37 C40 118.9(5) . . ? C37 C38 C39 119.8(6) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? N10 C39 C38 122.4(6) . . ? N10 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? O12 C40 O11 126.5(5) . . ? O12 C40 C37 118.2(5) . . ? O11 C40 C37 115.3(5) . . ? O14 C41 O13 118.5(5) . . ? O14 C41 C42 120.9(6) . . ? O13 C41 C42 120.5(6) . . ? O14 C41 Tb2 59.0(3) . . ? O13 C41 Tb2 59.6(3) . . ? C42 C41 Tb2 175.2(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O15 C43 O16 119.8(5) . . ? O15 C43 C44 120.7(5) . . ? O16 C43 C44 119.5(5) . . ? O15 C43 Tb3 59.7(3) . . ? O16 C43 Tb3 60.1(3) . . ? C44 C43 Tb3 176.5(5) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C1 Cu1 N5 112.2(2) . 1_556 ? C1 Cu1 N6 110.3(2) . . ? N5 Cu1 N6 128.4(2) 1_556 . ? C2 Cu2 N1 153.4(3) . 2_556 ? C2 Cu2 N7 104.6(2) . . ? N1 Cu2 N7 101.9(2) 2_556 . ? C2 Cu2 Cu4 98.01(19) . 2_566 ? N1 Cu2 Cu4 68.6(2) 2_556 2_566 ? N7 Cu2 Cu4 120.92(16) . 2_566 ? C3 Cu3 N2 145.0(3) . 1_545 ? C3 Cu3 N8 102.5(2) . . ? N2 Cu3 N8 111.6(2) 1_545 . ? N9 Cu4 N10 159.6(3) . 2_667 ? N9 Cu4 C4 97.8(3) . . ? N10 Cu4 C4 101.0(3) 2_667 . ? N9 Cu4 Cu2 80.62(18) . 2_566 ? N10 Cu4 Cu2 94.08(17) 2_667 2_566 ? C4 Cu4 Cu2 127.3(3) . 2_566 ? N4 Cu5 N4 179.998(2) 2_677 . ? O5 Tb1 O18 91.69(13) 1_545 1_545 ? O5 Tb1 O4 101.83(14) 1_545 . ? O18 Tb1 O4 137.37(13) 1_545 . ? O5 Tb1 O17 139.09(13) 1_545 . ? O18 Tb1 O17 104.58(12) 1_545 . ? O4 Tb1 O17 91.22(12) . . ? O5 Tb1 O2 151.35(13) 1_545 2_656 ? O18 Tb1 O2 78.53(13) 1_545 2_656 ? O4 Tb1 O2 70.31(14) . 2_656 ? O17 Tb1 O2 69.52(12) . 2_656 ? O5 Tb1 O13 76.64(13) 1_545 . ? O18 Tb1 O13 151.12(12) 1_545 . ? O4 Tb1 O13 71.42(13) . . ? O17 Tb1 O13 71.12(12) . . ? O2 Tb1 O13 123.28(13) 2_656 . ? O5 Tb1 O16 73.20(13) 1_545 1_545 ? O18 Tb1 O16 69.37(12) 1_545 1_545 ? O4 Tb1 O16 76.18(13) . 1_545 ? O17 Tb1 O16 147.64(12) . 1_545 ? O2 Tb1 O16 78.15(12) 2_656 1_545 ? O13 Tb1 O16 129.38(13) . 1_545 ? O5 Tb1 O12 70.40(13) 1_545 2_656 ? O18 Tb1 O12 71.24(12) 1_545 2_656 ? O4 Tb1 O12 151.36(14) . 2_656 ? O17 Tb1 O12 79.63(12) . 2_656 ? O2 Tb1 O12 129.15(14) 2_656 2_656 ? O13 Tb1 O12 79.94(13) . 2_656 ? O16 Tb1 O12 124.41(12) 1_545 2_656 ? O5 Tb1 Tb2 114.83(10) 1_545 . ? O18 Tb1 Tb2 139.81(8) 1_545 . ? O4 Tb1 Tb2 68.74(9) . . ? O17 Tb1 Tb2 35.95(9) . . ? O2 Tb1 Tb2 88.62(9) 2_656 . ? O13 Tb1 Tb2 38.43(9) . . ? O16 Tb1 Tb2 144.89(9) 1_545 . ? O12 Tb1 Tb2 89.10(9) 2_656 . ? O5 Tb1 Tb3 67.92(10) 1_545 1_545 ? O18 Tb1 Tb3 36.00(8) 1_545 1_545 ? O4 Tb1 Tb3 114.26(9) . 1_545 ? O17 Tb1 Tb3 139.92(9) . 1_545 ? O2 Tb1 Tb3 89.72(9) 2_656 1_545 ? O13 Tb1 Tb3 144.55(9) . 1_545 ? O16 Tb1 Tb3 38.11(9) 1_545 1_545 ? O12 Tb1 Tb3 88.95(9) 2_656 1_545 ? Tb2 Tb1 Tb3 175.808(9) . 1_545 ? O9 Tb2 O7 88.54(15) . . ? O9 Tb2 O17 149.40(14) . . ? O7 Tb2 O17 119.77(13) . . ? O9 Tb2 O11 78.49(15) . . ? O7 Tb2 O11 134.98(14) . . ? O17 Tb2 O11 73.13(13) . . ? O9 Tb2 O17 103.68(13) . 2_656 ? O7 Tb2 O17 71.30(14) . 2_656 ? O17 Tb2 O17 77.48(13) . 2_656 ? O11 Tb2 O17 70.37(12) . 2_656 ? O9 Tb2 O3 81.91(14) . . ? O7 Tb2 O3 146.78(15) . . ? O17 Tb2 O3 79.54(13) . . ? O11 Tb2 O3 74.08(13) . . ? O17 Tb2 O3 141.89(14) 2_656 . ? O9 Tb2 O14 77.88(14) . . ? O7 Tb2 O14 74.13(15) . . ? O17 Tb2 O14 118.75(13) . . ? O11 Tb2 O14 141.44(13) . . ? O17 Tb2 O14 145.32(13) 2_656 . ? O3 Tb2 O14 72.77(15) . . ? O9 Tb2 O13 130.72(14) . . ? O7 Tb2 O13 79.12(13) . . ? O17 Tb2 O13 70.75(12) . . ? O11 Tb2 O13 140.13(13) . . ? O17 Tb2 O13 116.49(12) 2_656 . ? O3 Tb2 O13 83.26(13) . . ? O14 Tb2 O13 52.84(13) . . ? O9 Tb2 C41 103.59(17) . . ? O7 Tb2 C41 75.91(16) . . ? O17 Tb2 C41 95.11(15) . . ? O11 Tb2 C41 148.97(15) . . ? O17 Tb2 C41 136.26(15) 2_656 . ? O3 Tb2 C41 75.59(16) . . ? O14 Tb2 C41 25.73(15) . . ? O13 Tb2 C41 27.14(15) . . ? O9 Tb2 Tb2 134.30(11) . 2_656 ? O7 Tb2 Tb2 96.10(11) . 2_656 ? O17 Tb2 Tb2 39.31(8) . 2_656 ? O11 Tb2 Tb2 66.32(9) . 2_656 ? O17 Tb2 Tb2 38.17(8) 2_656 2_656 ? O3 Tb2 Tb2 113.30(11) . 2_656 ? O14 Tb2 Tb2 146.94(9) . 2_656 ? O13 Tb2 Tb2 94.63(9) . 2_656 ? C41 Tb2 Tb2 121.68(13) . 2_656 ? O9 Tb2 Tb1 147.63(10) . . ? O7 Tb2 Tb1 110.38(10) . . ? O17 Tb2 Tb1 36.48(8) . . ? O11 Tb2 Tb1 102.78(9) . . ? O17 Tb2 Tb1 107.16(8) 2_656 . ? O3 Tb2 Tb1 67.80(10) . . ? O14 Tb2 Tb1 82.31(10) . . ? O13 Tb2 Tb1 37.51(9) . . ? C41 Tb2 Tb1 58.98(12) . . ? Tb2 Tb2 Tb1 71.485(9) 2_656 . ? O8 Tb3 O10 86.81(14) . . ? O8 Tb3 O18 150.98(13) . . ? O10 Tb3 O18 119.48(13) . . ? O8 Tb3 O6 82.96(14) . . ? O10 Tb3 O6 146.61(15) . . ? O18 Tb3 O6 80.49(13) . . ? O8 Tb3 O1 78.79(14) . . ? O10 Tb3 O1 136.28(14) . . ? O18 Tb3 O1 73.56(12) . . ? O6 Tb3 O1 72.37(14) . . ? O8 Tb3 O18 105.78(13) . 2_666 ? O10 Tb3 O18 69.36(13) . 2_666 ? O18 Tb3 O18 75.67(13) . 2_666 ? O6 Tb3 O18 144.03(13) . 2_666 ? O1 Tb3 O18 75.26(13) . 2_666 ? O8 Tb3 O15 80.36(14) . . ? O10 Tb3 O15 71.69(15) . . ? O18 Tb3 O15 117.69(13) . . ? O6 Tb3 O15 75.29(15) . . ? O1 Tb3 O15 143.23(14) . . ? O18 Tb3 O15 140.04(13) 2_666 . ? O8 Tb3 O16 133.60(14) . . ? O10 Tb3 O16 78.74(13) . . ? O18 Tb3 O16 68.56(12) . . ? O6 Tb3 O16 85.58(13) . . ? O1 Tb3 O16 138.72(12) . . ? O18 Tb3 O16 109.61(12) 2_666 . ? O15 Tb3 O16 53.24(12) . . ? O8 Tb3 C43 106.44(16) . . ? O10 Tb3 C43 72.72(16) . . ? O18 Tb3 C43 93.92(14) . . ? O6 Tb3 C43 79.88(16) . . ? O1 Tb3 C43 150.97(15) . . ? O18 Tb3 C43 127.85(15) 2_666 . ? O15 Tb3 C43 26.10(14) . . ? O16 Tb3 C43 27.16(14) . . ? O8 Tb3 Tb3 136.27(11) . 2_666 ? O10 Tb3 Tb3 94.81(10) . 2_666 ? O18 Tb3 Tb3 38.21(9) . 2_666 ? O6 Tb3 Tb3 114.39(10) . 2_666 ? O1 Tb3 Tb3 70.12(9) . 2_666 ? O18 Tb3 Tb3 37.46(8) 2_666 2_666 ? O15 Tb3 Tb3 141.36(9) . 2_666 ? O16 Tb3 Tb3 89.13(8) . 2_666 ? C43 Tb3 Tb3 115.76(12) . 2_666 ? O8 Tb3 Tb1 148.86(11) . 1_565 ? O10 Tb3 Tb1 111.57(10) . 1_565 ? O18 Tb3 Tb1 35.73(9) . 1_565 ? O6 Tb3 Tb1 67.81(10) . 1_565 ? O1 Tb3 Tb1 101.22(9) . 1_565 ? O18 Tb3 Tb1 104.24(8) 2_666 1_565 ? O15 Tb3 Tb1 82.00(9) . 1_565 ? O16 Tb3 Tb1 37.50(8) . 1_565 ? C43 Tb3 Tb1 59.36(11) . 1_565 ? Tb3 Tb3 Tb1 69.355(9) 2_666 1_565 ? C1 N1 Cu2 166.8(6) . 2_556 ? C2 N2 Cu3 167.4(6) . 1_565 ? C4 N4 Cu5 176.4(9) . . ? C5 N5 C9 116.5(5) . . ? C5 N5 Cu1 128.9(4) . 1_554 ? C9 N5 Cu1 114.5(4) . 1_554 ? C11 N6 C15 117.6(5) . . ? C11 N6 Cu1 124.6(4) . . ? C15 N6 Cu1 117.8(4) . . ? C17 N7 C21 116.7(5) . . ? C17 N7 Cu2 123.4(5) . . ? C21 N7 Cu2 119.9(4) . . ? C23 N8 C27 116.5(5) . . ? C23 N8 Cu3 122.3(4) . . ? C27 N8 Cu3 120.8(4) . . ? C29 N9 C33 116.2(6) . . ? C29 N9 Cu4 124.4(5) . . ? C33 N9 Cu4 119.1(5) . . ? C35 N10 C39 117.4(6) . . ? C35 N10 Cu4 116.3(4) . 2_667 ? C39 N10 Cu4 126.0(5) . 2_667 ? C10 O1 Tb3 118.2(3) . . ? C10 O2 Tb1 138.3(4) . 2_656 ? C16 O3 Tb2 132.3(4) . . ? C16 O4 Tb1 129.2(4) . . ? C22 O5 Tb1 128.2(4) . 1_565 ? C22 O6 Tb3 132.8(4) . . ? C28 O7 Tb2 157.5(4) . . ? C28 O8 Tb3 157.7(4) . . ? C34 O9 Tb2 153.4(4) . . ? C34 O10 Tb3 159.5(4) . . ? C40 O11 Tb2 124.2(4) . . ? C40 O12 Tb1 132.7(4) . 2_656 ? C41 O13 Tb1 130.6(3) . . ? C41 O13 Tb2 93.2(3) . . ? Tb1 O13 Tb2 104.05(14) . . ? C41 O14 Tb2 95.3(4) . . ? C43 O15 Tb3 94.2(3) . . ? C43 O16 Tb1 132.2(4) . 1_565 ? C43 O16 Tb3 92.7(3) . . ? Tb1 O16 Tb3 104.38(13) 1_565 . ? Tb2 O17 Tb1 107.56(14) . . ? Tb2 O17 Tb2 102.52(12) . 2_656 ? Tb1 O17 Tb2 133.41(15) . 2_656 ? Tb2 O17 H17A 96.8 . . ? Tb1 O17 H17A 100.1 . . ? Tb2 O17 H17A 110.9 2_656 . ? Tb1 O18 Tb3 108.27(14) 1_565 . ? Tb1 O18 Tb3 130.48(14) 1_565 2_666 ? Tb3 O18 Tb3 104.33(13) . 2_666 ? Tb1 O18 H18A 100.6 1_565 . ? Tb3 O18 H18A 106.2 . . ? Tb3 O18 H18A 104.9 2_666 . ? H19A O19W H19B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.611 _refine_diff_density_min -1.179 _refine_diff_density_rms 0.139 _database_code_depnum_ccdc_archive 'CCDC 964400' ####################################################################### # # 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_IV-B #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C87 H64 Cu9 Dy6 N19 O36, 2(H2 O)' _chemical_formula_sum 'C87 H68 Cu9 Dy6 N19 O38' _chemical_formula_weight 3534.56 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7096(9) _cell_length_b 12.7197(10) _cell_length_c 18.5102(15) _cell_angle_alpha 108.9560(10) _cell_angle_beta 95.6490(10) _cell_angle_gamma 97.9160(10) _cell_volume 2552.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9193 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 25.40 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1684 _exptl_absorpt_coefficient_mu 6.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.243 _exptl_absorpt_correction_T_max 0.286 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13417 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.40 _reflns_number_total 9193 _reflns_number_gt 7453 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0303P)^2^+8.0632P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00022(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9193 _refine_ls_number_parameters 721 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.027 _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 0.1919(6) -0.1994(7) 1.0097(4) 0.0329(16) Uani 1 1 d U . . C2 C -0.1157(6) 0.5996(7) 0.0338(4) 0.0354(17) Uani 1 1 d U . . C3 C -0.0097(7) -0.0395(6) 0.0098(4) 0.0437(18) Uani 0.50 1 d P . . C4 C 0.4861(10) 0.7492(10) 0.9768(5) 0.073(4) Uani 1 1 d U . . C5 C 0.2937(7) 0.1783(6) 0.1363(4) 0.0364(18) Uani 1 1 d . . . H5 H 0.2548 0.2109 0.1053 0.044 Uiso 1 1 calc R . . C6 C 0.3481(6) 0.2454(6) 0.2086(4) 0.0331(17) Uani 1 1 d . . . H6 H 0.3438 0.3219 0.2262 0.040 Uiso 1 1 calc R . . C7 C 0.4096(5) 0.2008(6) 0.2559(4) 0.0237(14) Uani 1 1 d . . . C8 C 0.4127(6) 0.0873(6) 0.2253(4) 0.0330(17) Uani 1 1 d . . . H8 H 0.4547 0.0536 0.2541 0.040 Uiso 1 1 calc R . . C9 C 0.3549(6) 0.0233(6) 0.1533(4) 0.0354(18) Uani 1 1 d . . . H9 H 0.3578 -0.0534 0.1348 0.042 Uiso 1 1 calc R . . C10 C 0.4630(5) 0.2693(5) 0.3381(4) 0.0211(14) Uani 1 1 d . . . C11 C 0.2544(7) 0.0409(6) 0.8791(4) 0.0362(18) Uani 1 1 d . . . H11 H 0.2526 0.1110 0.9155 0.043 Uiso 1 1 calc R . . C12 C 0.2724(7) 0.0348(6) 0.8045(4) 0.0354(18) Uani 1 1 d . . . H12 H 0.2836 0.1001 0.7919 0.043 Uiso 1 1 calc R . . C13 C 0.2734(6) -0.0683(6) 0.7498(4) 0.0263(15) Uani 1 1 d . . . C14 C 0.2599(6) -0.1624(6) 0.7721(4) 0.0335(17) Uani 1 1 d . . . H14 H 0.2616 -0.2334 0.7370 0.040 Uiso 1 1 calc R . . C15 C 0.2440(7) -0.1498(6) 0.8469(4) 0.0392(19) Uani 1 1 d . . . H15 H 0.2358 -0.2137 0.8613 0.047 Uiso 1 1 calc R . . C16 C 0.2941(6) -0.0807(6) 0.6675(4) 0.0273(15) Uani 1 1 d . . . C17 C -0.0076(7) 0.5783(7) 0.2094(5) 0.047(2) Uani 1 1 d . . . H17 H -0.0402 0.6377 0.2024 0.057 Uiso 1 1 calc R . . C18 C 0.0582(7) 0.5962(6) 0.2809(5) 0.042(2) Uani 1 1 d . . . H18 H 0.0690 0.6660 0.3202 0.050 Uiso 1 1 calc R . . C19 C 0.1064(6) 0.5099(6) 0.2927(4) 0.0272(15) Uani 1 1 d . . . C20 C 0.0860(7) 0.4079(7) 0.2326(4) 0.0378(18) Uani 1 1 d . . . H20 H 0.1156 0.3467 0.2391 0.045 Uiso 1 1 calc R . . C21 C 0.0215(7) 0.3962(7) 0.1625(5) 0.043(2) Uani 1 1 d . . . H21 H 0.0108 0.3273 0.1224 0.052 Uiso 1 1 calc R . . C22 C 0.1799(5) 0.5247(6) 0.3686(4) 0.0242(15) Uani 1 1 d . . . C23 C 0.1121(7) -0.1135(6) 0.2111(5) 0.044(2) Uani 1 1 d . . . H23 H 0.1155 -0.1897 0.1890 0.052 Uiso 1 1 calc R . . C24 C 0.1705(7) -0.0559(6) 0.2845(4) 0.0367(19) Uani 1 1 d . . . H24 H 0.2095 -0.0936 0.3118 0.044 Uiso 1 1 calc R . . C25 C 0.1710(6) 0.0594(5) 0.3181(4) 0.0247(15) Uani 1 1 d . . . C26 C 0.1076(6) 0.1088(6) 0.2748(4) 0.0337(17) Uani 1 1 d . . . H26 H 0.1042 0.1853 0.2947 0.040 Uiso 1 1 calc R . . C27 C 0.0501(7) 0.0437(7) 0.2026(5) 0.041(2) Uani 1 1 d . . . H27 H 0.0079 0.0783 0.1745 0.049 Uiso 1 1 calc R . . C28 C 0.2435(5) 0.1281(5) 0.3946(4) 0.0229(14) Uani 1 1 d . . . C29 C 0.3229(8) 0.3991(8) 0.8451(5) 0.050(2) Uani 1 1 d . . . H29 H 0.3069 0.3612 0.8793 0.060 Uiso 1 1 calc R . . C30 C 0.3147(7) 0.3356(6) 0.7685(4) 0.0366(18) Uani 1 1 d . . . H30 H 0.2949 0.2572 0.7520 0.044 Uiso 1 1 calc R . . C31 C 0.3363(6) 0.3899(5) 0.7160(4) 0.0236(14) Uani 1 1 d . . . C32 C 0.3631(8) 0.5062(6) 0.7442(4) 0.044(2) Uani 1 1 d . . . H32 H 0.3755 0.5462 0.7108 0.053 Uiso 1 1 calc R . . C33 C 0.3714(9) 0.5619(7) 0.8217(5) 0.054(2) Uani 1 1 d . . . H33 H 0.3917 0.6403 0.8396 0.065 Uiso 1 1 calc R . . C34 C 0.3380(5) 0.3253(5) 0.6331(4) 0.0240(15) Uani 1 1 d . . . C35 C 0.5594(8) 0.2584(8) 0.8631(5) 0.052(2) Uani 1 1 d . . . H35 H 0.5269 0.2116 0.8881 0.062 Uiso 1 1 calc R . . C36 C 0.5556(8) 0.2140(7) 0.7838(4) 0.046(2) Uani 1 1 d . . . H36 H 0.5232 0.1386 0.7569 0.055 Uiso 1 1 calc R . . C37 C 0.5999(6) 0.2822(6) 0.7449(4) 0.0264(15) Uani 1 1 d . . . C38 C 0.6457(7) 0.3914(7) 0.7878(5) 0.046(2) Uani 1 1 d . . . H38 H 0.6747 0.4406 0.7635 0.055 Uiso 1 1 calc R . . C39 C 0.6499(8) 0.4303(8) 0.8671(5) 0.056(2) Uani 1 1 d . . . H39 H 0.6834 0.5051 0.8952 0.067 Uiso 1 1 calc R . . C40 C 0.5888(5) 0.2337(6) 0.6579(4) 0.0234(14) Uani 1 1 d . . . C41 C 0.1514(6) -0.0957(6) 0.5049(4) 0.0301(16) Uani 1 1 d . . . C42 C 0.0373(6) -0.1748(7) 0.4893(6) 0.056(3) Uani 1 1 d . . . H42A H 0.0239 -0.1913 0.5351 0.084 Uiso 1 1 calc R . . H42B H 0.0394 -0.2435 0.4482 0.084 Uiso 1 1 calc R . . H42C H -0.0245 -0.1400 0.4745 0.084 Uiso 1 1 calc R . . C43 C 0.1796(6) 0.5270(6) 0.5534(4) 0.0277(16) Uani 1 1 d . . . C44 C 0.0943(7) 0.5846(7) 0.6012(5) 0.049(2) Uani 1 1 d . . . H44A H 0.0161 0.5474 0.5773 0.073 Uiso 1 1 calc R . . H44B H 0.1042 0.6623 0.6044 0.073 Uiso 1 1 calc R . . H44C H 0.1081 0.5808 0.6522 0.073 Uiso 1 1 calc R . . Cu1 Cu 0.21751(10) -0.04620(9) 1.00644(6) 0.0496(3) Uani 1 1 d . . . Cu2 Cu -0.12678(9) 0.45525(9) 0.04123(6) 0.0457(3) Uani 1 1 d . . . Cu3 Cu -0.02299(10) -0.15476(9) 0.05402(6) 0.0498(3) Uani 1 1 d . . . Cu4 Cu 0.37779(11) 0.60054(12) 0.98304(6) 0.0674(4) Uani 1 1 d . . . Cu5 Cu 0.5000 1.0000 1.0000 0.0816(6) Uani 1 2 d SU . . Dy1 Dy 0.34692(2) -0.26737(2) 0.509479(17) 0.01705(8) Uani 1 1 d . . . Dy2 Dy 0.37096(3) 0.04855(2) 0.542051(17) 0.01934(9) Uani 1 1 d . . . Dy3 Dy 0.34615(3) 0.41845(2) 0.474503(17) 0.01820(9) Uani 1 1 d . . . N1 N 0.1778(6) -0.2971(6) 0.9965(4) 0.0500(18) Uani 1 1 d U . . N2 N -0.0919(6) 0.6938(6) 0.0383(4) 0.0506(18) Uani 1 1 d U . . N3 N -0.0097(7) -0.0395(6) 0.0098(4) 0.0437(18) Uani 0.50 1 d P . . N4 N 0.4909(8) 0.8397(10) 0.9833(5) 0.084(3) Uani 1 1 d U . . N5 N 0.2944(5) 0.0665(5) 0.1083(3) 0.0340(14) Uani 1 1 d . . . N6 N 0.2397(5) -0.0504(5) 0.9000(3) 0.0325(14) Uani 1 1 d . . . N7 N -0.0260(6) 0.4804(5) 0.1505(4) 0.0416(17) Uani 1 1 d . . . N8 N 0.0513(6) -0.0666(5) 0.1700(4) 0.0377(15) Uani 1 1 d . . . N9 N 0.3522(6) 0.5109(6) 0.8739(4) 0.0460(17) Uani 1 1 d . . . N10 N 0.6067(6) 0.3631(6) 0.9048(3) 0.0412(16) Uani 1 1 d . . . O1 O 0.4444(4) 0.3680(4) 0.3642(3) 0.0271(11) Uani 1 1 d . . . O2 O 0.5169(4) 0.2199(4) 0.3750(3) 0.0278(11) Uani 1 1 d . . . O3 O 0.3440(4) 0.0066(4) 0.6577(3) 0.0316(11) Uani 1 1 d . . . O4 O 0.2602(4) -0.1757(4) 0.6176(3) 0.0282(11) Uani 1 1 d . . . O5 O 0.1831(4) 0.6159(4) 0.4226(3) 0.0282(11) Uani 1 1 d . . . O6 O 0.2312(4) 0.4468(4) 0.3716(3) 0.0327(12) Uani 1 1 d . . . O7 O 0.2835(4) 0.0748(4) 0.4341(3) 0.0337(12) Uani 1 1 d . . . O8 O 0.2589(4) 0.2335(4) 0.4127(3) 0.0318(11) Uani 1 1 d . . . O9 O 0.3341(4) 0.2208(4) 0.6144(3) 0.0347(12) Uani 1 1 d . . . O10 O 0.3475(4) 0.3793(4) 0.5883(3) 0.0304(11) Uani 1 1 d . . . O11 O 0.5495(4) 0.1287(4) 0.6279(3) 0.0304(11) Uani 1 1 d . . . O12 O 0.6163(4) 0.2995(4) 0.6225(3) 0.0284(11) Uani 1 1 d . . . O13 O 0.2419(4) -0.1338(4) 0.4787(3) 0.0246(10) Uani 1 1 d . . . O14 O 0.1605(4) 0.0062(4) 0.5420(3) 0.0379(13) Uani 1 1 d . . . O15 O 0.1535(4) 0.4252(4) 0.5120(3) 0.0370(13) Uani 1 1 d . . . O16 O 0.2815(4) 0.5845(4) 0.5574(3) 0.0239(10) Uani 1 1 d . . . O17 O 0.4796(3) -0.0989(3) 0.5275(2) 0.0184(9) Uani 1 1 d D . . H17A H 0.5054 -0.0816 0.5735 0.022 Uiso 1 1 d RD . . O18 O 0.4585(3) 0.5877(3) 0.4745(2) 0.0190(9) Uani 1 1 d D . . H18A H 0.4607 0.5806 0.4292 0.023 Uiso 1 1 d RD . . O19W O 0.0928(12) 0.1366(13) 0.6832(8) 0.223(7) Uani 1 1 d . . . H19A H 0.0249 0.1423 0.6947 0.268 Uiso 1 1 d R . . H19B H 0.0851 0.0957 0.6358 0.268 Uiso 1 1 d R . . 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 0.036(4) 0.044(3) 0.019(4) 0.012(3) 0.003(3) 0.005(3) C2 0.033(4) 0.047(4) 0.024(4) 0.016(4) -0.010(3) 0.002(3) C3 0.050(4) 0.045(5) 0.034(5) 0.010(4) 0.002(3) 0.015(4) C4 0.114(9) 0.065(6) 0.015(5) 0.007(5) 0.001(5) -0.044(6) C5 0.046(5) 0.039(5) 0.025(4) 0.013(4) -0.003(3) 0.008(4) C6 0.044(4) 0.027(4) 0.027(4) 0.009(3) -0.003(3) 0.008(3) C7 0.022(3) 0.025(4) 0.020(4) 0.004(3) -0.001(3) 0.001(3) C8 0.044(4) 0.028(4) 0.026(4) 0.006(3) -0.002(3) 0.014(3) C9 0.049(5) 0.025(4) 0.026(4) 0.001(3) -0.001(3) 0.008(3) C10 0.027(3) 0.019(3) 0.018(4) 0.007(3) 0.004(3) 0.005(3) C11 0.054(5) 0.030(4) 0.021(4) 0.001(3) 0.011(3) 0.009(3) C12 0.063(5) 0.023(4) 0.028(4) 0.013(3) 0.016(4) 0.017(4) C13 0.029(4) 0.029(4) 0.022(4) 0.011(3) 0.004(3) 0.005(3) C14 0.049(5) 0.030(4) 0.018(4) 0.002(3) 0.009(3) 0.007(3) C15 0.062(5) 0.031(4) 0.024(4) 0.012(4) 0.004(4) 0.003(4) C16 0.029(4) 0.032(4) 0.025(4) 0.010(3) 0.007(3) 0.013(3) C17 0.065(6) 0.031(5) 0.041(5) 0.009(4) -0.015(4) 0.014(4) C18 0.058(5) 0.030(4) 0.029(5) 0.000(4) -0.009(4) 0.017(4) C19 0.026(4) 0.024(4) 0.026(4) 0.006(3) -0.003(3) 0.000(3) C20 0.047(5) 0.041(5) 0.025(4) 0.011(4) -0.002(3) 0.016(4) C21 0.060(5) 0.033(4) 0.026(4) 0.000(4) -0.011(4) 0.008(4) C22 0.023(3) 0.026(4) 0.022(4) 0.009(3) 0.002(3) -0.003(3) C23 0.066(6) 0.018(4) 0.032(5) -0.004(3) -0.012(4) 0.002(4) C24 0.066(5) 0.016(4) 0.023(4) 0.000(3) -0.005(4) 0.012(3) C25 0.031(4) 0.017(3) 0.021(4) 0.003(3) 0.000(3) 0.000(3) C26 0.043(4) 0.022(4) 0.034(5) 0.011(3) -0.006(3) 0.005(3) C27 0.044(5) 0.040(5) 0.038(5) 0.015(4) -0.010(4) 0.008(4) C28 0.027(4) 0.025(4) 0.020(4) 0.009(3) 0.009(3) 0.002(3) C29 0.076(6) 0.057(6) 0.025(5) 0.024(4) 0.012(4) 0.009(5) C30 0.057(5) 0.025(4) 0.028(4) 0.006(3) 0.014(4) 0.009(3) C31 0.036(4) 0.020(3) 0.017(4) 0.005(3) 0.007(3) 0.014(3) C32 0.078(6) 0.025(4) 0.023(4) 0.002(3) 0.003(4) 0.009(4) C33 0.101(8) 0.030(5) 0.018(4) -0.006(4) 0.000(4) 0.014(5) C34 0.022(3) 0.022(4) 0.029(4) 0.009(3) 0.006(3) 0.008(3) C35 0.086(7) 0.048(6) 0.029(5) 0.020(4) 0.013(4) 0.017(5) C36 0.083(6) 0.035(5) 0.017(4) 0.005(4) 0.008(4) 0.013(4) C37 0.033(4) 0.028(4) 0.014(4) 0.002(3) -0.001(3) 0.010(3) C38 0.057(5) 0.041(5) 0.028(5) 0.002(4) 0.011(4) -0.007(4) C39 0.059(6) 0.054(6) 0.033(5) -0.004(4) 0.008(4) -0.014(4) C40 0.025(3) 0.026(4) 0.016(4) 0.003(3) 0.001(3) 0.008(3) C41 0.025(4) 0.030(4) 0.038(5) 0.015(4) 0.001(3) 0.009(3) C42 0.022(4) 0.047(5) 0.095(8) 0.017(5) 0.009(4) 0.012(4) C43 0.030(4) 0.037(4) 0.025(4) 0.020(4) 0.005(3) 0.011(3) C44 0.032(4) 0.051(5) 0.058(6) 0.008(5) 0.020(4) 0.007(4) Cu1 0.0790(8) 0.0450(6) 0.0156(5) 0.0023(5) 0.0013(5) 0.0046(5) Cu2 0.0546(6) 0.0409(6) 0.0375(6) 0.0132(5) -0.0070(5) 0.0062(5) Cu3 0.0651(7) 0.0381(6) 0.0338(6) 0.0039(5) -0.0088(5) 0.0005(5) Cu4 0.0752(8) 0.0908(10) 0.0179(6) -0.0016(6) 0.0066(5) 0.0047(7) Cu5 0.0787(13) 0.1030(16) 0.0500(12) 0.0245(11) 0.0062(9) -0.0201(11) Dy1 0.02367(17) 0.01292(15) 0.01291(16) 0.00225(12) 0.00164(12) 0.00404(11) Dy2 0.02817(17) 0.01407(16) 0.01501(17) 0.00310(13) 0.00398(12) 0.00545(12) Dy3 0.02281(16) 0.01380(15) 0.01562(17) 0.00298(12) 0.00021(12) 0.00250(11) N1 0.059(5) 0.045(3) 0.040(4) 0.013(4) -0.004(3) 0.003(4) N2 0.065(5) 0.045(3) 0.034(4) 0.011(4) 0.000(3) 0.000(4) N3 0.050(4) 0.045(5) 0.034(5) 0.010(4) 0.002(3) 0.015(4) N4 0.075(6) 0.124(7) 0.043(6) 0.025(6) 0.011(5) -0.009(6) N5 0.044(4) 0.036(4) 0.017(3) 0.005(3) 0.001(3) 0.002(3) N6 0.048(4) 0.026(3) 0.020(3) 0.005(3) 0.004(3) 0.001(3) N7 0.055(4) 0.036(4) 0.032(4) 0.014(3) -0.014(3) 0.006(3) N8 0.054(4) 0.027(3) 0.022(3) 0.003(3) -0.007(3) -0.001(3) N9 0.061(5) 0.051(5) 0.020(4) 0.001(3) 0.011(3) 0.015(4) N10 0.049(4) 0.053(4) 0.017(3) 0.001(3) 0.006(3) 0.015(3) O1 0.037(3) 0.028(3) 0.019(3) 0.008(2) 0.006(2) 0.012(2) O2 0.038(3) 0.024(3) 0.018(3) 0.006(2) -0.003(2) 0.004(2) O3 0.047(3) 0.030(3) 0.017(3) 0.009(2) 0.010(2) 0.001(2) O4 0.041(3) 0.020(3) 0.022(3) 0.003(2) 0.012(2) 0.010(2) O5 0.026(3) 0.028(3) 0.024(3) 0.004(2) -0.004(2) 0.001(2) O6 0.039(3) 0.034(3) 0.025(3) 0.009(2) -0.003(2) 0.015(2) O7 0.048(3) 0.034(3) 0.021(3) 0.012(2) -0.001(2) 0.013(2) O8 0.043(3) 0.018(3) 0.025(3) 0.001(2) -0.005(2) -0.003(2) O9 0.053(3) 0.019(3) 0.028(3) -0.002(2) 0.009(2) 0.014(2) O10 0.042(3) 0.032(3) 0.021(3) 0.016(2) 0.005(2) 0.001(2) O11 0.042(3) 0.024(3) 0.018(3) 0.003(2) 0.000(2) 0.000(2) O12 0.044(3) 0.023(3) 0.017(3) 0.004(2) 0.007(2) 0.007(2) O13 0.020(2) 0.025(3) 0.029(3) 0.009(2) 0.0013(19) 0.0090(19) O14 0.038(3) 0.022(3) 0.052(4) 0.005(3) 0.012(2) 0.011(2) O15 0.033(3) 0.024(3) 0.049(4) 0.008(3) 0.006(2) 0.001(2) O16 0.021(2) 0.020(2) 0.029(3) 0.007(2) 0.0061(19) 0.0009(18) O17 0.025(2) 0.016(2) 0.016(2) 0.0072(19) 0.0013(18) 0.0055(17) O18 0.027(2) 0.018(2) 0.013(2) 0.0046(19) 0.0051(18) 0.0078(18) O19W 0.202(15) 0.264(18) 0.158(14) 0.009(13) 0.060(11) 0.020(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.170(10) . ? C1 Cu1 1.953(8) . ? C2 N2 1.167(10) . ? C2 Cu2 1.873(8) . ? C3 N3 1.177(14) 2 ? C3 C3 1.177(14) 2 ? C3 Cu3 1.893(7) . ? C4 N4 1.111(13) . ? C4 Cu4 2.170(9) . ? C5 N5 1.348(9) . ? C5 C6 1.365(10) . ? C5 H5 0.9300 . ? C6 C7 1.386(9) . ? C6 H6 0.9300 . ? C7 C8 1.376(9) . ? C7 C10 1.505(9) . ? C8 C9 1.365(10) . ? C8 H8 0.9300 . ? C9 N5 1.335(9) . ? C9 H9 0.9300 . ? C10 O1 1.250(7) . ? C10 O2 1.250(7) . ? C11 N6 1.333(9) . ? C11 C12 1.396(10) . ? C11 H11 0.9300 . ? C12 C13 1.375(10) . ? C12 H12 0.9300 . ? C13 C14 1.382(9) . ? C13 C16 1.528(9) . ? C14 C15 1.376(10) . ? C14 H14 0.9300 . ? C15 N6 1.336(9) . ? C15 H15 0.9300 . ? C16 O4 1.241(8) . ? C16 O3 1.257(8) . ? C17 N7 1.336(10) . ? C17 C18 1.398(10) . ? C17 H17 0.9300 . ? C18 C19 1.368(10) . ? C18 H18 0.9300 . ? C19 C20 1.379(10) . ? C19 C22 1.515(9) . ? C20 C21 1.388(10) . ? C20 H20 0.9300 . ? C21 N7 1.343(9) . ? C21 H21 0.9300 . ? C22 O6 1.241(8) . ? C22 O5 1.254(8) . ? C23 N8 1.322(9) . ? C23 C24 1.374(10) . ? C23 H23 0.9300 . ? C24 C25 1.394(9) . ? C24 H24 0.9300 . ? C25 C26 1.387(9) . ? C25 C28 1.498(9) . ? C26 C27 1.370(10) . ? C26 H26 0.9300 . ? C27 N8 1.338(10) . ? C27 H27 0.9300 . ? C28 O8 1.253(8) . ? C28 O7 1.247(7) . ? C29 N9 1.328(11) . ? C29 C30 1.371(11) . ? C29 H29 0.9300 . ? C30 C31 1.387(9) . ? C30 H30 0.9300 . ? C31 C32 1.377(10) . ? C31 C34 1.491(9) . ? C32 C33 1.365(10) . ? C32 H32 0.9300 . ? C33 N9 1.347(10) . ? C33 H33 0.9300 . ? C34 O10 1.240(7) . ? C34 O9 1.253(8) . ? C35 N10 1.312(11) . ? C35 C36 1.385(11) . ? C35 H35 0.9300 . ? C36 C37 1.377(10) . ? C36 H36 0.9300 . ? C37 C38 1.357(10) . ? C37 C40 1.510(9) . ? C38 C39 1.382(11) . ? C38 H38 0.9300 . ? C39 N10 1.346(11) . ? C39 H39 0.9300 . ? C40 O12 1.248(8) . ? C40 O11 1.266(8) . ? C41 O14 1.237(8) . ? C41 O13 1.298(8) . ? C41 C42 1.498(10) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 O15 1.249(8) . ? C43 O16 1.292(8) . ? C43 C44 1.507(10) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? Cu1 N5 1.994(6) 1_556 ? Cu1 N6 1.997(6) . ? Cu2 N1 1.888(7) 2_556 ? Cu2 N7 2.142(6) . ? Cu2 Cu4 2.8815(17) 2_566 ? Cu3 N2 1.899(7) 1_545 ? Cu3 N8 2.102(6) . ? Cu4 N9 1.940(7) . ? Cu4 N10 1.959(6) 2_667 ? Cu4 Cu2 2.8814(17) 2_566 ? Cu5 N4 1.946(12) . ? Cu5 N4 1.946(12) 2_677 ? Dy1 O5 2.351(4) 1_545 ? Dy1 O18 2.362(4) 1_545 ? Dy1 O4 2.368(4) . ? Dy1 O17 2.373(4) . ? Dy1 O2 2.388(4) 2_656 ? Dy1 O16 2.397(4) 1_545 ? Dy1 O13 2.406(4) . ? Dy1 O12 2.435(4) 2_656 ? Dy1 Dy3 3.8338(5) 1_545 ? Dy2 O9 2.290(5) . ? Dy2 O7 2.298(4) . ? Dy2 O17 2.368(4) . ? Dy2 O11 2.375(5) . ? Dy2 O17 2.409(4) 2_656 ? Dy2 O3 2.408(4) . ? Dy2 O13 2.441(4) . ? Dy2 O14 2.449(5) . ? Dy2 Dy2 3.7129(6) 2_656 ? Dy3 O8 2.291(4) . ? Dy3 O10 2.316(4) . ? Dy3 O18 2.363(4) . ? Dy3 O6 2.376(4) . ? Dy3 O1 2.391(4) . ? Dy3 O18 2.408(4) 2_666 ? Dy3 O15 2.429(5) . ? Dy3 O16 2.440(4) . ? Dy3 Dy3 3.7651(6) 2_666 ? Dy3 Dy1 3.8337(5) 1_565 ? N1 Cu2 1.888(7) 2_556 ? N2 Cu3 1.899(7) 1_565 ? N5 Cu1 1.994(6) 1_554 ? N10 Cu4 1.959(6) 2_667 ? O2 Dy1 2.388(4) 2_656 ? O5 Dy1 2.351(4) 1_565 ? O12 Dy1 2.435(4) 2_656 ? O16 Dy1 2.397(4) 1_565 ? O17 Dy2 2.409(4) 2_656 ? O17 H17A 0.8203 . ? O18 Dy1 2.362(4) 1_565 ? O18 Dy3 2.408(4) 2_666 ? O18 H18A 0.8172 . ? O19W H19A 0.8500 . ? O19W H19B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cu1 166.8(7) . . ? N2 C2 Cu2 168.4(7) . . ? N3 C3 C3 0.0(9) 2 2 ? N3 C3 Cu3 171.4(10) 2 . ? C3 C3 Cu3 171.4(10) 2 . ? N4 C4 Cu4 145.0(12) . . ? N5 C5 C6 122.4(7) . . ? N5 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C7 120.7(7) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 116.1(6) . . ? C8 C7 C10 121.2(6) . . ? C6 C7 C10 122.5(6) . . ? C9 C8 C7 121.0(7) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? N5 C9 C8 122.7(7) . . ? N5 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? O1 C10 O2 126.1(6) . . ? O1 C10 C7 117.1(6) . . ? O2 C10 C7 116.7(6) . . ? N6 C11 C12 122.1(7) . . ? N6 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 119.7(6) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 117.9(6) . . ? C12 C13 C16 122.3(6) . . ? C14 C13 C16 119.8(6) . . ? C15 C14 C13 119.2(7) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N6 C15 C14 123.4(7) . . ? N6 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? O4 C16 O3 127.1(6) . . ? O4 C16 C13 116.6(6) . . ? O3 C16 C13 116.3(6) . . ? N7 C17 C18 123.4(7) . . ? N7 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C19 C18 C17 119.4(7) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 117.6(7) . . ? C18 C19 C22 121.8(6) . . ? C20 C19 C22 120.6(6) . . ? C19 C20 C21 120.1(7) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? N7 C21 C20 122.6(7) . . ? N7 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? O6 C22 O5 126.3(6) . . ? O6 C22 C19 117.6(6) . . ? O5 C22 C19 116.1(6) . . ? N8 C23 C24 123.6(7) . . ? N8 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C25 119.7(7) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 116.7(6) . . ? C26 C25 C28 121.7(6) . . ? C24 C25 C28 121.5(6) . . ? C27 C26 C25 119.4(7) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? N8 C27 C26 123.9(7) . . ? N8 C27 H27 118.1 . . ? C26 C27 H27 118.1 . . ? O8 C28 O7 126.2(6) . . ? O8 C28 C25 117.1(6) . . ? O7 C28 C25 116.7(6) . . ? N9 C29 C30 124.5(7) . . ? N9 C29 H29 117.7 . . ? C30 C29 H29 117.7 . . ? C29 C30 C31 119.0(7) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C32 C31 C30 117.5(7) . . ? C32 C31 C34 120.9(6) . . ? C30 C31 C34 121.5(6) . . ? C33 C32 C31 119.2(7) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? N9 C33 C32 124.4(8) . . ? N9 C33 H33 117.8 . . ? C32 C33 H33 117.8 . . ? O10 C34 O9 124.9(7) . . ? O10 C34 C31 117.7(6) . . ? O9 C34 C31 117.4(6) . . ? N10 C35 C36 123.3(8) . . ? N10 C35 H35 118.4 . . ? C36 C35 H35 118.4 . . ? C35 C36 C37 119.7(8) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 117.0(7) . . ? C38 C37 C40 124.3(7) . . ? C36 C37 C40 118.7(6) . . ? C37 C38 C39 120.9(8) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? N10 C39 C38 121.8(8) . . ? N10 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? O12 C40 O11 126.3(6) . . ? O12 C40 C37 118.1(6) . . ? O11 C40 C37 115.5(6) . . ? O14 C41 O13 119.3(6) . . ? O14 C41 C42 120.9(7) . . ? O13 C41 C42 119.9(7) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O15 C43 O16 120.5(6) . . ? O15 C43 C44 120.8(6) . . ? O16 C43 C44 118.7(7) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C1 Cu1 N5 111.6(3) . 1_556 ? C1 Cu1 N6 110.0(3) . . ? N5 Cu1 N6 129.4(2) 1_556 . ? C2 Cu2 N1 153.3(3) . 2_556 ? C2 Cu2 N7 105.1(3) . . ? N1 Cu2 N7 101.6(3) 2_556 . ? C2 Cu2 Cu4 97.1(2) . 2_566 ? N1 Cu2 Cu4 69.1(2) 2_556 2_566 ? N7 Cu2 Cu4 121.3(2) . 2_566 ? C3 Cu3 N2 144.9(3) . 1_545 ? C3 Cu3 N8 102.5(3) . . ? N2 Cu3 N8 111.9(3) 1_545 . ? N9 Cu4 N10 159.5(3) . 2_667 ? N9 Cu4 C4 97.9(3) . . ? N10 Cu4 C4 100.6(3) 2_667 . ? N9 Cu4 Cu2 81.0(2) . 2_566 ? N10 Cu4 Cu2 94.4(2) 2_667 2_566 ? C4 Cu4 Cu2 128.1(4) . 2_566 ? N4 Cu5 N4 179.999(3) . 2_677 ? O5 Dy1 O18 91.43(15) 1_545 1_545 ? O5 Dy1 O4 101.52(16) 1_545 . ? O18 Dy1 O4 137.39(15) 1_545 . ? O5 Dy1 O17 139.23(15) 1_545 . ? O18 Dy1 O17 104.69(14) 1_545 . ? O4 Dy1 O17 91.55(15) . . ? O5 Dy1 O2 150.89(15) 1_545 2_656 ? O18 Dy1 O2 78.59(15) 1_545 2_656 ? O4 Dy1 O2 70.46(16) . 2_656 ? O17 Dy1 O2 69.84(14) . 2_656 ? O5 Dy1 O16 72.70(15) 1_545 1_545 ? O18 Dy1 O16 69.15(14) 1_545 1_545 ? O4 Dy1 O16 76.30(15) . 1_545 ? O17 Dy1 O16 148.02(14) . 1_545 ? O2 Dy1 O16 78.20(15) 2_656 1_545 ? O5 Dy1 O13 77.12(15) 1_545 . ? O18 Dy1 O13 151.14(15) 1_545 . ? O4 Dy1 O13 71.37(16) . . ? O17 Dy1 O13 70.79(14) . . ? O2 Dy1 O13 123.16(15) 2_656 . ? O16 Dy1 O13 129.62(14) 1_545 . ? O5 Dy1 O12 70.55(16) 1_545 2_656 ? O18 Dy1 O12 71.00(14) 1_545 2_656 ? O4 Dy1 O12 151.54(15) . 2_656 ? O17 Dy1 O12 79.62(15) . 2_656 ? O2 Dy1 O12 129.20(16) 2_656 2_656 ? O16 Dy1 O12 123.92(15) 1_545 2_656 ? O13 Dy1 O12 80.19(15) . 2_656 ? O5 Dy1 Dy3 67.77(11) 1_545 1_545 ? O18 Dy1 Dy3 35.78(10) 1_545 1_545 ? O4 Dy1 Dy3 114.22(11) . 1_545 ? O17 Dy1 Dy3 139.82(9) . 1_545 ? O2 Dy1 Dy3 89.55(11) 2_656 1_545 ? O16 Dy1 Dy3 37.96(11) 1_545 1_545 ? O13 Dy1 Dy3 144.88(10) . 1_545 ? O12 Dy1 Dy3 88.67(10) 2_656 1_545 ? O9 Dy2 O7 88.35(17) . . ? O9 Dy2 O17 149.75(16) . . ? O7 Dy2 O17 119.51(16) . . ? O9 Dy2 O11 78.25(17) . . ? O7 Dy2 O11 135.15(17) . . ? O17 Dy2 O11 73.53(15) . . ? O9 Dy2 O17 102.71(16) . 2_656 ? O7 Dy2 O17 71.29(16) . 2_656 ? O17 Dy2 O17 77.98(14) . 2_656 ? O11 Dy2 O17 70.39(15) . 2_656 ? O9 Dy2 O3 82.29(17) . . ? O7 Dy2 O3 146.62(17) . . ? O17 Dy2 O3 79.72(15) . . ? O11 Dy2 O3 74.02(16) . . ? O17 Dy2 O3 142.04(15) 2_656 . ? O9 Dy2 O13 131.28(16) . . ? O7 Dy2 O13 79.04(16) . . ? O17 Dy2 O13 70.28(14) . . ? O11 Dy2 O13 140.04(15) . . ? O17 Dy2 O13 116.72(15) 2_656 . ? O3 Dy2 O13 83.32(15) . . ? O9 Dy2 O14 78.14(17) . . ? O7 Dy2 O14 74.00(18) . . ? O17 Dy2 O14 118.64(15) . . ? O11 Dy2 O14 141.27(17) . . ? O17 Dy2 O14 145.22(16) 2_656 . ? O3 Dy2 O14 72.73(17) . . ? O13 Dy2 O14 53.14(15) . . ? O9 Dy2 Dy2 133.92(13) . 2_656 ? O7 Dy2 Dy2 96.09(13) . 2_656 ? O17 Dy2 Dy2 39.39(10) . 2_656 ? O11 Dy2 Dy2 66.52(12) . 2_656 ? O17 Dy2 Dy2 38.59(9) 2_656 2_656 ? O3 Dy2 Dy2 113.43(12) . 2_656 ? O13 Dy2 Dy2 94.39(10) . 2_656 ? O14 Dy2 Dy2 146.99(12) . 2_656 ? O8 Dy3 O10 86.56(17) . . ? O8 Dy3 O18 150.94(16) . . ? O10 Dy3 O18 119.68(15) . . ? O8 Dy3 O6 83.08(16) . . ? O10 Dy3 O6 146.35(17) . . ? O18 Dy3 O6 80.61(15) . . ? O8 Dy3 O1 78.65(17) . . ? O10 Dy3 O1 136.38(16) . . ? O18 Dy3 O1 73.56(15) . . ? O6 Dy3 O1 72.37(16) . . ? O8 Dy3 O18 105.32(15) . 2_666 ? O10 Dy3 O18 69.54(15) . 2_666 ? O18 Dy3 O18 75.79(15) . 2_666 ? O6 Dy3 O18 144.11(15) . 2_666 ? O1 Dy3 O18 75.22(14) . 2_666 ? O8 Dy3 O15 79.99(17) . . ? O10 Dy3 O15 71.89(17) . . ? O18 Dy3 O15 118.12(15) . . ? O6 Dy3 O15 74.81(17) . . ? O1 Dy3 O15 142.55(16) . . ? O18 Dy3 O15 140.57(16) 2_666 . ? O8 Dy3 O16 133.87(16) . . ? O10 Dy3 O16 79.08(16) . . ? O18 Dy3 O16 68.42(14) . . ? O6 Dy3 O16 85.31(16) . . ? O1 Dy3 O16 138.44(14) . . ? O18 Dy3 O16 109.97(14) 2_666 . ? O15 Dy3 O16 53.89(15) . . ? O8 Dy3 Dy3 135.85(13) . 2_666 ? O10 Dy3 Dy3 95.00(12) . 2_666 ? O18 Dy3 Dy3 38.32(10) . 2_666 ? O6 Dy3 Dy3 114.57(12) . 2_666 ? O1 Dy3 Dy3 70.08(11) . 2_666 ? O18 Dy3 Dy3 37.47(9) 2_666 2_666 ? O15 Dy3 Dy3 142.17(12) . 2_666 ? O16 Dy3 Dy3 89.29(10) . 2_666 ? O8 Dy3 Dy1 149.18(12) . 1_565 ? O10 Dy3 Dy1 111.59(12) . 1_565 ? O18 Dy3 Dy1 35.77(10) . 1_565 ? O6 Dy3 Dy1 67.95(12) . 1_565 ? O1 Dy3 Dy1 101.28(11) . 1_565 ? O18 Dy3 Dy1 104.38(9) 2_666 1_565 ? O15 Dy3 Dy1 82.37(11) . 1_565 ? O16 Dy3 Dy1 37.19(10) . 1_565 ? Dy3 Dy3 Dy1 69.492(10) 2_666 1_565 ? C1 N1 Cu2 167.1(7) . 2_556 ? C2 N2 Cu3 168.6(7) . 1_565 ? C4 N4 Cu5 177.3(9) . . ? C9 N5 C5 117.2(6) . . ? C9 N5 Cu1 114.2(5) . 1_554 ? C5 N5 Cu1 128.6(5) . 1_554 ? C15 N6 C11 117.7(6) . . ? C15 N6 Cu1 118.4(5) . . ? C11 N6 Cu1 123.9(5) . . ? C17 N7 C21 116.8(6) . . ? C17 N7 Cu2 122.7(5) . . ? C21 N7 Cu2 120.5(5) . . ? C27 N8 C23 116.8(6) . . ? C27 N8 Cu3 120.9(5) . . ? C23 N8 Cu3 121.9(5) . . ? C29 N9 C33 115.4(7) . . ? C29 N9 Cu4 124.9(6) . . ? C33 N9 Cu4 119.6(6) . . ? C35 N10 C39 117.3(7) . . ? C35 N10 Cu4 115.5(6) . 2_667 ? C39 N10 Cu4 126.8(6) . 2_667 ? C10 O1 Dy3 118.5(4) . . ? C10 O2 Dy1 138.5(4) . 2_656 ? C16 O3 Dy2 131.5(4) . . ? C16 O4 Dy1 128.7(4) . . ? C22 O5 Dy1 127.8(4) . 1_565 ? C22 O6 Dy3 132.3(4) . . ? C28 O7 Dy2 156.9(5) . . ? C28 O8 Dy3 158.2(4) . . ? C34 O9 Dy2 155.1(5) . . ? C34 O10 Dy3 160.4(5) . . ? C40 O11 Dy2 124.4(4) . . ? C40 O12 Dy1 132.4(4) . 2_656 ? C41 O13 Dy1 129.9(4) . . ? C41 O13 Dy2 93.1(4) . . ? Dy1 O13 Dy2 104.42(15) . . ? C41 O14 Dy2 94.3(4) . . ? C43 O15 Dy3 93.6(4) . . ? C43 O16 Dy1 132.8(4) . 1_565 ? C43 O16 Dy3 91.9(4) . . ? Dy1 O16 Dy3 104.85(16) 1_565 . ? Dy2 O17 Dy1 107.79(15) . . ? Dy2 O17 Dy2 102.03(14) . 2_656 ? Dy1 O17 Dy2 134.04(19) . 2_656 ? Dy2 O17 H17A 96.5 . . ? Dy1 O17 H17A 99.9 . . ? Dy2 O17 H17A 110.7 2_656 . ? Dy1 O18 Dy3 108.46(16) 1_565 . ? Dy1 O18 Dy3 130.44(18) 1_565 2_666 ? Dy3 O18 Dy3 104.21(15) . 2_666 ? Dy1 O18 H18A 100.5 1_565 . ? Dy3 O18 H18A 106.4 . . ? Dy3 O18 H18A 104.8 2_666 . ? H19A O19W H19B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.811 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.157 _database_code_depnum_ccdc_archive 'CCDC 964401' ####################################################################### # # 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_V-A #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H31 Cu5 N10 O16 Tb2 ' _chemical_formula_sum 'C42 H31 Cu5 N10 O16 Tb2' _chemical_formula_weight 1567.38 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.8782(10) _cell_length_b 30.7430(18) _cell_length_c 9.0004(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.0690(10) _cell_angle_gamma 90.00 _cell_volume 4798.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8824 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 25.40 _exptl_crystal_description platelike _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 5.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.356 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46988 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.40 _reflns_number_total 8824 _reflns_number_gt 7228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0216P)^2^+3.1128P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00040(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8824 _refine_ls_number_parameters 706 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.006 _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 Cu2 Cu 0.97369(5) 0.45168(3) 1.46382(10) 0.0393(3) Uani 0.6633(16) 1 d P . 1 Cu2B Cu 0.95711(11) 0.54286(6) 1.4748(2) 0.0450(7) Uani 0.3367(16) 1 d P . 2 C11 C 0.8040(4) 0.4372(2) 1.4276(9) 0.0423(17) Uani 0.6633(16) 1 d P . 1 H11 H 0.8220 0.4093 1.4563 0.051 Uiso 0.6633(16) 1 calc PR . 1 C12 C 0.7285(5) 0.4451(2) 1.4140(9) 0.0367(17) Uani 0.6633(16) 1 d P . 1 H12 H 0.6959 0.4230 1.4302 0.044 Uiso 0.6633(16) 1 calc PR . 1 C13 C 0.6998(8) 0.4870(3) 1.3754(15) 0.022(2) Uani 0.6633(16) 1 d P . 1 C14 C 0.7490(4) 0.5178(2) 1.3458(8) 0.0334(15) Uani 0.6633(16) 1 d P . 1 H14 H 0.7319 0.5459 1.3170 0.040 Uiso 0.6633(16) 1 calc PR . 1 C15 C 0.8260(6) 0.5061(3) 1.3602(13) 0.041(2) Uani 0.6633(16) 1 d P . 1 H15 H 0.8591 0.5272 1.3386 0.049 Uiso 0.6633(16) 1 calc PR . 1 N6 N 0.8553(3) 0.4670(2) 1.4025(7) 0.0353(15) Uani 0.6633(16) 1 d P . 1 C11B C 0.8228(10) 0.4775(6) 1.416(2) 0.0423(17) Uani 0.3367(16) 1 d P . 2 H11B H 0.8599 0.4564 1.4526 0.051 Uiso 0.3367(16) 1 calc PR . 2 C12B C 0.7412(11) 0.4684(5) 1.401(2) 0.0367(17) Uani 0.3367(16) 1 d P . 2 H12B H 0.7247 0.4406 1.4186 0.044 Uiso 0.3367(16) 1 calc PR . 2 C13B C 0.6899(19) 0.5013(7) 1.360(3) 0.022(2) Uani 0.3367(16) 1 d P . 2 C14B C 0.7133(8) 0.5404(4) 1.3065(16) 0.0334(15) Uani 0.3367(16) 1 d P . 2 H14B H 0.6773 0.5616 1.2639 0.040 Uiso 0.3367(16) 1 calc PR . 2 C15B C 0.7919(8) 0.5469(5) 1.3178(16) 0.041(2) Uani 0.3367(16) 1 d P . 2 H15B H 0.8076 0.5730 1.2826 0.049 Uiso 0.3367(16) 1 calc PR . 2 N6B N 0.8439(10) 0.5181(5) 1.376(2) 0.0353(15) Uani 0.3367(16) 1 d P . 2 C1 C 1.0106(3) 0.49804(15) 1.1993(6) 0.0372(11) Uani 1 1 d . . . C2 C 0.9925(3) 0.59502(17) 1.3937(6) 0.0472(13) Uani 1 1 d . . . C3 C 0.9672(3) 0.73100(15) 1.2218(5) 0.0366(11) Uani 1 1 d . . . C4 C 0.9668(2) 0.63223(14) 0.9637(5) 0.0291(10) Uani 1 1 d . . . C5 C 0.8155(3) 0.48741(16) 0.9404(8) 0.0684(19) Uani 1 1 d . . . H5 H 0.8470 0.4630 0.9610 0.082 Uiso 1 1 calc R . . C6 C 0.7392(3) 0.48173(16) 0.8721(7) 0.0605(17) Uani 1 1 d . . . H6 H 0.7198 0.4539 0.8484 0.073 Uiso 1 1 calc R . . C7 C 0.6914(2) 0.51693(14) 0.8384(5) 0.0281(10) Uani 1 1 d . . . C8 C 0.7217(3) 0.55676(14) 0.8903(5) 0.0368(11) Uani 1 1 d . . . H8 H 0.6904 0.5813 0.8796 0.044 Uiso 1 1 calc R . . C9 C 0.7999(3) 0.55976(15) 0.9588(6) 0.0407(12) Uani 1 1 d . . . H9 H 0.8199 0.5870 0.9922 0.049 Uiso 1 1 calc R . . C10 C 0.6116(3) 0.51264(15) 0.7350(5) 0.0309(10) Uani 1 1 d . . . C17 C 0.1524(3) 0.63183(14) 0.2440(6) 0.0394(12) Uani 1 1 d . . . H17 H 0.1215 0.6076 0.2455 0.047 Uiso 1 1 calc R . . C18 C 0.2307(2) 0.62667(14) 0.2848(5) 0.0368(11) Uani 1 1 d . . . H18 H 0.2520 0.5996 0.3165 0.044 Uiso 1 1 calc R . . C19 C 0.2781(2) 0.66169(13) 0.2789(5) 0.0272(10) Uani 1 1 d . . . C20 C 0.2439(3) 0.70085(15) 0.2317(6) 0.0417(12) Uani 1 1 d . . . H20 H 0.2737 0.7251 0.2232 0.050 Uiso 1 1 calc R . . C21 C 0.1644(3) 0.70374(15) 0.1971(6) 0.0481(14) Uani 1 1 d . . . H21 H 0.1418 0.7307 0.1687 0.058 Uiso 1 1 calc R . . C22 C 0.3639(2) 0.65512(14) 0.3226(4) 0.0259(9) Uani 1 1 d . . . C23 C 0.7746(3) 0.68107(14) 0.9717(5) 0.0329(11) Uani 1 1 d . . . H23 H 0.8029 0.6644 1.0522 0.039 Uiso 1 1 calc R . . C24 C 0.6979(3) 0.68771(13) 0.9633(5) 0.0325(11) Uani 1 1 d . . . H24 H 0.6752 0.6753 1.0358 0.039 Uiso 1 1 calc R . . C25 C 0.6544(2) 0.71297(12) 0.8468(5) 0.0251(9) Uani 1 1 d . . . C26 C 0.6907(2) 0.72818(14) 0.7380(5) 0.0311(10) Uani 1 1 d . . . H26 H 0.6630 0.7438 0.6540 0.037 Uiso 1 1 calc R . . C27 C 0.7685(3) 0.72005(14) 0.7545(5) 0.0352(11) Uani 1 1 d . . . H27 H 0.7921 0.7311 0.6810 0.042 Uiso 1 1 calc R . . C28 C 0.5726(2) 0.72603(13) 0.8441(5) 0.0249(9) Uani 1 1 d . . . C29 C 0.8453(3) 0.66654(17) 0.4659(6) 0.0445(13) Uani 1 1 d . . . H29 H 0.8777 0.6852 0.4292 0.053 Uiso 1 1 calc R . . C30 C 0.7670(2) 0.66935(15) 0.4058(5) 0.0365(11) Uani 1 1 d . . . H30 H 0.7473 0.6894 0.3287 0.044 Uiso 1 1 calc R . . C31 C 0.7177(2) 0.64248(13) 0.4599(4) 0.0259(9) Uani 1 1 d . . . C32 C 0.7504(3) 0.61253(15) 0.5701(5) 0.0377(11) Uani 1 1 d . . . H32 H 0.7194 0.5932 0.6076 0.045 Uiso 1 1 calc R . . C33 C 0.8290(3) 0.61128(17) 0.6244(5) 0.0442(12) Uani 1 1 d . . . H33 H 0.8500 0.5908 0.6990 0.053 Uiso 1 1 calc R . . C34 C 0.6315(2) 0.64602(13) 0.3998(5) 0.0272(10) Uani 1 1 d . . . C35 C 0.1420(3) 0.62990(18) -0.1667(6) 0.0509(14) Uani 1 1 d . . . H35 H 0.1208 0.6123 -0.1034 0.061 Uiso 1 1 calc R . . C36 C 0.2202(3) 0.63629(17) -0.1288(5) 0.0474(13) Uani 1 1 d . . . H36 H 0.2506 0.6237 -0.0407 0.057 Uiso 1 1 calc R . . C37 C 0.2537(2) 0.66151(14) -0.2222(5) 0.0305(10) Uani 1 1 d . . . C38 C 0.2056(3) 0.67973(15) -0.3496(5) 0.0370(11) Uani 1 1 d . . . H38 H 0.2259 0.6969 -0.4155 0.044 Uiso 1 1 calc R . . C39 C 0.1276(3) 0.67255(16) -0.3793(6) 0.0430(12) Uani 1 1 d . . . H39 H 0.0961 0.6856 -0.4654 0.052 Uiso 1 1 calc R . . C40 C 0.3406(3) 0.66867(14) -0.1844(6) 0.0359(11) Uani 1 1 d . . . C41 C 0.5046(3) 0.59641(14) 0.0700(5) 0.0375(11) Uani 1 1 d . . . C42 C 0.4960(5) 0.55079(17) 0.0116(7) 0.104(3) Uani 1 1 d . . . H42A H 0.4480 0.5479 -0.0637 0.155 Uiso 1 1 calc R . . H42B H 0.4966 0.5312 0.0950 0.155 Uiso 1 1 calc R . . H42C H 0.5378 0.5439 -0.0340 0.155 Uiso 1 1 calc R . . Cu1 Cu 0.96780(3) 0.534681(18) 1.02255(7) 0.03930(15) Uani 1 1 d . . . Cu3 Cu 0.99942(3) 0.674670(18) 1.18396(7) 0.03607(14) Uani 1 1 d . . . Cu4 Cu 0.92980(3) 0.688006(17) 0.88873(7) 0.03573(14) Uani 1 1 d . . . Cu5 Cu 0.98601(4) 0.63716(3) 0.65180(8) 0.0631(2) Uani 1 1 d . . . Tb1 Tb 0.486261(11) 0.685581(6) 0.12188(2) 0.02082(6) Uani 1 1 d . . . Tb2 Tb 0.494537(11) 0.573844(6) 0.45374(2) 0.02312(6) Uani 1 1 d . . . N1 N 1.0133(2) 0.48368(14) 1.3156(5) 0.0451(10) Uani 1 1 d . . . N2 N 0.9865(2) 0.62503(13) 1.3172(4) 0.0392(10) Uani 1 1 d . . . N3 N 0.9538(2) 0.76343(13) 1.2746(5) 0.0445(10) Uani 1 1 d . . . N4 N 0.9770(2) 0.59574(12) 0.9766(4) 0.0318(9) Uani 1 1 d . . . N5 N 0.8472(2) 0.52655(12) 0.9794(4) 0.0403(10) Uani 1 1 d . . . N7 N 0.1183(2) 0.66987(12) 0.2022(4) 0.0346(9) Uani 1 1 d . . . N8 N 0.8113(2) 0.69726(11) 0.8702(4) 0.0316(9) Uani 1 1 d . . . N9 N 0.8766(2) 0.63780(13) 0.5758(4) 0.0372(9) Uani 1 1 d . . . N10 N 0.0943(2) 0.64772(14) -0.2905(5) 0.0436(10) Uani 1 1 d . . . O1 O 0.5842(2) 0.47506(11) 0.7151(4) 0.0534(10) Uani 1 1 d . . . O2 O 0.58195(17) 0.54674(11) 0.6733(3) 0.0410(8) Uani 1 1 d . . . O3 O 0.58257(19) 0.46441(12) 1.4143(4) 0.0553(10) Uani 1 1 d . . . O4 O 0.5886(2) 0.53445(11) 1.3623(4) 0.0602(11) Uani 1 1 d . . . O5 O 0.40688(16) 0.68524(9) 0.2938(3) 0.0280(7) Uani 1 1 d . . . O6 O 0.38714(16) 0.61991(10) 0.3849(3) 0.0362(8) Uani 1 1 d . . . O7 O 0.54682(17) 0.71327(10) 0.9511(3) 0.0400(8) Uani 1 1 d . . . O8 O 0.53838(18) 0.74975(10) 0.7380(4) 0.0439(9) Uani 1 1 d . . . O9 O 0.60723(17) 0.67028(10) 0.2874(4) 0.0448(9) Uani 1 1 d . . . O10 O 0.59145(17) 0.62507(10) 0.4702(3) 0.0351(7) Uani 1 1 d . . . O11 O 0.37635(17) 0.65872(10) -0.0510(4) 0.0412(8) Uani 1 1 d . . . O12 O 0.36798(19) 0.68344(12) -0.2884(4) 0.0553(10) Uani 1 1 d . . . O13 O 0.48370(17) 0.60616(9) 0.1916(3) 0.0296(7) Uani 1 1 d . . . O14 O 0.53119(19) 0.62432(10) -0.0029(3) 0.0399(8) Uani 1 1 d . . . O15W O 0.39819(17) 0.74753(9) 0.0242(3) 0.0370(8) Uani 1 1 d . . . H15A H 0.3598 0.7585 -0.0397 0.044 Uiso 1 1 d R . . H15W H 0.4160 0.7668 0.0911 0.044 Uiso 1 1 d R . . O16W O 0.48908(18) 0.62167(10) 0.6700(3) 0.0424(8) Uani 1 1 d . . . H16A H 0.4513 0.6391 0.6608 0.051 Uiso 1 1 d R . . H16B H 0.5128 0.6210 0.7641 0.051 Uiso 1 1 d R . . C16 C 0.6151(3) 0.49705(14) 1.3811(5) 0.0298(10) 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 Cu2 0.0295(6) 0.0451(6) 0.0433(6) 0.0122(4) 0.0089(4) 0.0042(4) Cu2B 0.0302(13) 0.0568(13) 0.0477(12) 0.0162(9) 0.0087(9) -0.0015(9) C11 0.027(4) 0.029(3) 0.071(5) 0.011(3) 0.013(3) 0.008(3) C12 0.035(4) 0.020(4) 0.059(4) 0.007(4) 0.019(3) 0.003(4) C13 0.020(5) 0.014(7) 0.034(4) -0.003(5) 0.010(3) 0.011(5) C14 0.024(4) 0.027(4) 0.051(4) 0.004(3) 0.012(3) -0.001(3) C15 0.034(5) 0.034(5) 0.055(5) 0.002(4) 0.013(4) -0.003(3) N6 0.022(3) 0.039(4) 0.047(4) 0.008(3) 0.013(3) 0.004(3) C11B 0.027(4) 0.029(3) 0.071(5) 0.011(3) 0.013(3) 0.008(3) C12B 0.035(4) 0.020(4) 0.059(4) 0.007(4) 0.019(3) 0.003(4) C13B 0.020(5) 0.014(7) 0.034(4) -0.003(5) 0.010(3) 0.011(5) C14B 0.024(4) 0.027(4) 0.051(4) 0.004(3) 0.012(3) -0.001(3) C15B 0.034(5) 0.034(5) 0.055(5) 0.002(4) 0.013(4) -0.003(3) N6B 0.022(3) 0.039(4) 0.047(4) 0.008(3) 0.013(3) 0.004(3) C1 0.034(3) 0.041(3) 0.037(3) 0.003(2) 0.010(2) 0.001(2) C2 0.064(4) 0.040(3) 0.047(3) 0.001(3) 0.032(3) 0.007(3) C3 0.032(3) 0.033(3) 0.045(3) -0.001(2) 0.011(2) 0.003(2) C4 0.021(2) 0.029(3) 0.037(3) 0.001(2) 0.005(2) -0.0005(19) C5 0.039(3) 0.024(3) 0.127(6) 0.011(3) -0.009(3) 0.005(3) C6 0.037(3) 0.026(3) 0.106(5) -0.002(3) -0.008(3) -0.002(2) C7 0.027(3) 0.029(2) 0.028(2) 0.0037(18) 0.0050(19) 0.000(2) C8 0.026(3) 0.027(2) 0.052(3) -0.002(2) -0.001(2) 0.006(2) C9 0.028(3) 0.033(3) 0.057(3) -0.007(2) 0.002(2) 0.000(2) C10 0.025(3) 0.043(3) 0.024(2) 0.001(2) 0.0039(19) -0.006(2) C17 0.027(3) 0.026(2) 0.068(3) 0.003(2) 0.016(2) -0.001(2) C18 0.021(3) 0.026(2) 0.064(3) 0.006(2) 0.010(2) 0.008(2) C19 0.022(2) 0.028(2) 0.032(2) 0.0002(19) 0.0076(19) 0.0028(19) C20 0.022(3) 0.027(3) 0.073(4) 0.014(2) 0.007(2) -0.005(2) C21 0.024(3) 0.028(3) 0.086(4) 0.016(3) 0.000(3) 0.005(2) C22 0.025(2) 0.031(2) 0.023(2) -0.0018(18) 0.0077(19) 0.002(2) C23 0.032(3) 0.030(2) 0.035(3) 0.011(2) 0.004(2) 0.009(2) C24 0.029(3) 0.033(3) 0.038(3) 0.010(2) 0.013(2) 0.002(2) C25 0.025(2) 0.020(2) 0.029(2) -0.0010(17) 0.0035(19) 0.0013(18) C26 0.027(3) 0.034(3) 0.033(2) 0.014(2) 0.009(2) 0.008(2) C27 0.036(3) 0.038(3) 0.037(3) 0.006(2) 0.018(2) 0.002(2) C28 0.021(2) 0.023(2) 0.030(2) -0.0022(18) 0.0063(19) -0.0002(18) C29 0.023(3) 0.067(4) 0.045(3) 0.008(3) 0.011(2) -0.008(2) C30 0.022(3) 0.045(3) 0.040(3) 0.015(2) 0.003(2) -0.003(2) C31 0.018(2) 0.032(2) 0.024(2) 0.0026(18) -0.0025(18) -0.0004(18) C32 0.025(3) 0.037(3) 0.045(3) 0.015(2) -0.001(2) -0.003(2) C33 0.029(3) 0.055(3) 0.042(3) 0.009(2) -0.006(2) 0.007(2) C34 0.019(2) 0.024(2) 0.034(2) 0.0017(19) -0.0019(19) -0.0042(19) C35 0.030(3) 0.087(4) 0.036(3) 0.007(3) 0.008(2) -0.008(3) C36 0.026(3) 0.077(4) 0.033(3) 0.007(3) -0.005(2) -0.003(3) C37 0.024(2) 0.035(3) 0.031(2) -0.008(2) 0.006(2) -0.001(2) C38 0.030(3) 0.039(3) 0.038(3) 0.000(2) 0.001(2) -0.002(2) C39 0.030(3) 0.053(3) 0.040(3) -0.005(2) -0.004(2) 0.009(2) C40 0.029(3) 0.028(2) 0.048(3) -0.011(2) 0.003(2) -0.002(2) C41 0.048(3) 0.027(3) 0.034(3) -0.003(2) 0.005(2) 0.008(2) C42 0.240(10) 0.027(3) 0.060(4) -0.010(3) 0.067(5) -0.006(4) Cu1 0.0314(3) 0.0292(3) 0.0526(4) 0.0087(3) 0.0011(3) 0.0045(3) Cu3 0.0271(3) 0.0304(3) 0.0500(4) -0.0003(3) 0.0081(3) 0.0057(2) Cu4 0.0295(3) 0.0284(3) 0.0487(4) 0.0097(3) 0.0082(3) 0.0041(2) Cu5 0.0168(3) 0.0985(6) 0.0681(5) 0.0042(4) -0.0010(3) 0.0015(4) Tb1 0.01409(11) 0.02428(11) 0.02359(11) 0.00003(8) 0.00357(8) -0.00073(8) Tb2 0.01678(11) 0.02229(11) 0.02859(12) 0.00408(8) 0.00221(8) -0.00093(8) N1 0.038(3) 0.050(3) 0.049(3) 0.005(2) 0.012(2) 0.007(2) N2 0.039(3) 0.043(2) 0.037(2) -0.001(2) 0.0130(19) -0.001(2) N3 0.036(3) 0.038(2) 0.061(3) -0.010(2) 0.015(2) -0.003(2) N4 0.032(2) 0.027(2) 0.033(2) 0.0011(16) 0.0011(17) 0.0007(17) N5 0.025(2) 0.038(2) 0.052(3) 0.0052(19) -0.0034(19) 0.0016(18) N7 0.016(2) 0.033(2) 0.050(2) 0.0007(18) -0.0003(17) -0.0007(17) N8 0.027(2) 0.029(2) 0.040(2) 0.0031(17) 0.0086(18) 0.0037(16) N9 0.020(2) 0.059(3) 0.031(2) -0.0041(19) 0.0031(17) -0.0011(19) N10 0.018(2) 0.071(3) 0.040(2) -0.006(2) 0.0041(19) 0.003(2) O1 0.055(2) 0.044(2) 0.051(2) -0.0014(17) -0.0063(18) -0.0234(18) O2 0.0269(18) 0.052(2) 0.0377(18) 0.0117(16) -0.0042(15) 0.0022(16) O3 0.036(2) 0.068(3) 0.062(2) 0.019(2) 0.0112(18) -0.0178(19) O4 0.080(3) 0.048(2) 0.054(2) 0.0037(18) 0.018(2) 0.037(2) O5 0.0200(16) 0.0327(17) 0.0334(16) -0.0022(13) 0.0104(13) -0.0029(13) O6 0.0203(17) 0.0402(19) 0.0482(19) 0.0149(15) 0.0084(14) 0.0077(14) O7 0.0303(19) 0.055(2) 0.0396(19) 0.0138(16) 0.0186(15) 0.0030(16) O8 0.0296(19) 0.045(2) 0.058(2) 0.0226(17) 0.0117(17) 0.0115(16) O9 0.0235(18) 0.048(2) 0.055(2) 0.0233(17) -0.0066(16) -0.0064(15) O10 0.0260(18) 0.0417(19) 0.0355(17) 0.0038(14) 0.0036(14) -0.0114(14) O11 0.0228(18) 0.046(2) 0.046(2) -0.0040(16) -0.0082(15) -0.0047(15) O12 0.032(2) 0.073(3) 0.063(2) 0.012(2) 0.0149(19) -0.0073(18) O13 0.0390(19) 0.0256(16) 0.0246(16) 0.0002(13) 0.0087(14) 0.0023(14) O14 0.053(2) 0.0363(19) 0.0354(18) -0.0002(15) 0.0203(17) 0.0071(16) O15W 0.0316(19) 0.0349(18) 0.0400(18) 0.0064(14) -0.0001(15) 0.0075(14) O16W 0.048(2) 0.047(2) 0.0324(17) -0.0035(15) 0.0095(16) 0.0126(16) C16 0.026(3) 0.035(3) 0.030(2) 0.0011(19) 0.010(2) 0.002(2) _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 Cu2 C2 1.922(5) 3_768 ? Cu2 N1 1.925(4) . ? Cu2 N6 2.106(6) . ? Cu2B C2 1.931(6) . ? Cu2B N1 2.005(5) 3_768 ? Cu2B N6B 2.144(16) . ? Cu2B Cu2B 3.027(4) 3_768 ? C11 C12 1.347(10) . ? C11 N6 1.355(9) . ? C11 H11 0.9300 . ? C12 C13 1.397(9) . ? C12 H12 0.9300 . ? C13 C14 1.364(15) . ? C13 C16 1.559(13) . ? C14 C15 1.398(12) . ? C14 H14 0.9300 . ? C15 N6 1.329(12) . ? C15 H15 0.9300 . ? C11B N6B 1.38(2) . ? C11B C12B 1.46(2) . ? C11B H11B 0.9300 . ? C12B C13B 1.35(2) . ? C12B H12B 0.9300 . ? C13B C14B 1.40(3) . ? C13B C16 1.40(3) . ? C14B C15B 1.400(18) . ? C14B H14B 0.9300 . ? C15B N6B 1.30(2) . ? C15B H15B 0.9300 . ? C1 N1 1.127(5) . ? C1 Cu1 1.947(5) . ? C1 Cu1 2.350(5) 3_767 ? C2 N2 1.141(6) . ? C2 Cu2 1.922(5) 3_768 ? C3 N3 1.154(5) . ? C3 Cu3 1.882(5) . ? C4 N4 1.138(5) . ? C4 Cu4 1.902(4) . ? C4 Cu3 2.326(4) . ? C5 N5 1.340(6) . ? C5 C6 1.363(7) . ? C5 H5 0.9300 . ? C6 C7 1.367(6) . ? C6 H6 0.9300 . ? C7 C8 1.374(6) . ? C7 C10 1.507(6) . ? C8 C9 1.386(6) . ? C8 H8 0.9300 . ? C9 N5 1.310(6) . ? C9 H9 0.9300 . ? C10 O2 1.243(5) . ? C10 O1 1.251(5) . ? C17 N7 1.330(5) . ? C17 C18 1.367(6) . ? C17 H17 0.9300 . ? C18 C19 1.379(6) . ? C18 H18 0.9300 . ? C19 C20 1.370(6) . ? C19 C22 1.502(6) . ? C20 C21 1.382(6) . ? C20 H20 0.9300 . ? C21 N7 1.335(6) . ? C21 H21 0.9300 . ? C22 O6 1.243(5) . ? C22 O5 1.269(5) . ? C23 N8 1.342(5) . ? C23 C24 1.370(6) . ? C23 H23 0.9300 . ? C24 C25 1.383(5) . ? C24 H24 0.9300 . ? C25 C26 1.381(6) . ? C25 C28 1.511(6) . ? C26 C27 1.385(6) . ? C26 H26 0.9300 . ? C27 N8 1.332(5) . ? C27 H27 0.9300 . ? C28 O7 1.228(5) . ? C28 O8 1.239(5) . ? C29 N9 1.343(6) . ? C29 C30 1.376(6) . ? C29 H29 0.9300 . ? C30 C31 1.381(6) . ? C30 H30 0.9300 . ? C31 C32 1.375(5) . ? C31 C34 1.508(5) . ? C32 C33 1.372(6) . ? C32 H32 0.9300 . ? C33 N9 1.327(6) . ? C33 H33 0.9300 . ? C34 O10 1.245(5) . ? C34 O9 1.247(5) . ? C35 N10 1.344(6) . ? C35 C36 1.371(6) . ? C35 H35 0.9300 . ? C36 C37 1.382(6) . ? C36 H36 0.9300 . ? C37 C38 1.374(6) . ? C37 C40 1.524(6) . ? C38 C39 1.372(6) . ? C38 H38 0.9300 . ? C39 N10 1.344(6) . ? C39 H39 0.9300 . ? C40 O12 1.242(5) . ? C40 O11 1.253(5) . ? C41 O14 1.243(5) . ? C41 O13 1.274(5) . ? C41 C42 1.493(7) . ? C41 Tb1 2.813(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Cu1 N4 1.938(4) . ? Cu1 N5 2.111(4) . ? Cu1 C1 2.350(5) 3_767 ? Cu1 Cu1 2.5029(11) 3_767 ? Cu3 N2 1.988(4) . ? Cu3 N7 2.098(4) 1_656 ? Cu3 Cu4 2.6777(8) . ? Cu4 N3 1.919(4) 4_575 ? Cu4 N8 2.104(4) . ? Cu4 Cu5 3.0071(10) . ? Cu5 N10 1.907(4) 1_656 ? Cu5 N9 1.909(4) . ? Tb1 O7 2.251(3) 1_554 ? Tb1 O8 2.332(3) 4_575 ? Tb1 O5 2.340(3) . ? Tb1 O11 2.340(3) . ? Tb1 O9 2.356(3) . ? Tb1 O14 2.427(3) . ? Tb1 O15W 2.491(3) . ? Tb1 O13 2.524(3) . ? Tb2 O10 2.319(3) . ? Tb2 O3 2.343(3) 3_667 ? Tb2 O6 2.345(3) . ? Tb2 O1 2.348(3) 3_666 ? Tb2 O2 2.354(3) . ? Tb2 O4 2.377(3) 1_554 ? Tb2 O16W 2.460(3) . ? Tb2 O13 2.524(3) . ? N1 Cu2B 2.005(5) 3_768 ? N3 Cu4 1.919(4) 4_576 ? N7 Cu3 2.098(3) 1_454 ? N10 Cu5 1.907(4) 1_454 ? O1 Tb2 2.348(3) 3_666 ? O3 C16 1.232(5) . ? O3 Tb2 2.343(3) 3_667 ? O4 C16 1.239(5) . ? O4 Tb2 2.377(3) 1_556 ? O7 Tb1 2.251(3) 1_556 ? O8 Tb1 2.333(3) 4_576 ? O15W H15A 0.8508 . ? O15W H15W 0.8509 . ? O16W H16A 0.8511 . ? O16W H16B 0.8505 . ? 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 Cu2 N1 137.3(2) 3_768 . ? C2 Cu2 N6 118.3(2) 3_768 . ? N1 Cu2 N6 102.7(2) . . ? C2 Cu2B N1 131.1(2) . 3_768 ? C2 Cu2B N6B 120.0(5) . . ? N1 Cu2B N6B 104.7(5) 3_768 . ? C2 Cu2B Cu2B 125.36(19) . 3_768 ? N1 Cu2B Cu2B 59.74(13) 3_768 3_768 ? N6B Cu2B Cu2B 98.4(5) . 3_768 ? C12 C11 N6 124.5(7) . . ? C12 C11 H11 117.8 . . ? N6 C11 H11 117.8 . . ? C11 C12 C13 119.3(8) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 118.3(9) . . ? C14 C13 C16 123.1(5) . . ? C12 C13 C16 118.4(9) . . ? C13 C14 C15 118.0(7) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? N6 C15 C14 124.9(8) . . ? N6 C15 H15 117.6 . . ? C14 C15 H15 117.6 . . ? C15 N6 C11 115.0(7) . . ? C15 N6 Cu2 125.4(6) . . ? C11 N6 Cu2 118.9(5) . . ? N6B C11B C12B 118.7(16) . . ? N6B C11B H11B 120.7 . . ? C12B C11B H11B 120.7 . . ? C13B C12B C11B 119(2) . . ? C13B C12B H12B 120.7 . . ? C11B C12B H12B 120.7 . . ? C12B C13B C14B 120(3) . . ? C12B C13B C16 120(2) . . ? C14B C13B C16 120.2(16) . . ? C13B C14B C15B 118.6(17) . . ? C13B C14B H14B 120.7 . . ? C15B C14B H14B 120.7 . . ? N6B C15B C14B 122.6(14) . . ? N6B C15B H15B 118.7 . . ? C14B C15B H15B 118.7 . . ? C15B N6B C11B 120.7(16) . . ? C15B N6B Cu2B 115.8(11) . . ? C11B N6B Cu2B 120.1(14) . . ? N1 C1 Cu1 154.9(4) . . ? N1 C1 Cu1 130.0(4) . 3_767 ? Cu1 C1 Cu1 70.54(15) . 3_767 ? N2 C2 Cu2 167.2(5) . 3_768 ? N2 C2 Cu2B 155.3(5) . . ? Cu2 C2 Cu2B 37.47(12) 3_768 . ? N3 C3 Cu3 166.5(4) . . ? N4 C4 Cu4 163.5(4) . . ? N4 C4 Cu3 117.7(3) . . ? Cu4 C4 Cu3 77.88(15) . . ? N5 C5 C6 123.1(5) . . ? N5 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C5 C6 C7 120.1(5) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C8 117.1(4) . . ? C6 C7 C10 121.0(4) . . ? C8 C7 C10 121.6(4) . . ? C7 C8 C9 118.8(4) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? N5 C9 C8 123.9(4) . . ? N5 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? O2 C10 O1 127.3(4) . . ? O2 C10 C7 116.0(4) . . ? O1 C10 C7 116.6(4) . . ? N7 C17 C18 123.1(4) . . ? N7 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C17 C18 C19 119.8(4) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 117.8(4) . . ? C20 C19 C22 123.3(4) . . ? C18 C19 C22 118.9(4) . . ? C19 C20 C21 118.9(4) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? N7 C21 C20 123.5(4) . . ? N7 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? O6 C22 O5 125.1(4) . . ? O6 C22 C19 116.3(4) . . ? O5 C22 C19 118.6(4) . . ? N8 C23 C24 123.7(4) . . ? N8 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C23 C24 C25 119.8(4) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 117.0(4) . . ? C26 C25 C28 121.2(4) . . ? C24 C25 C28 121.7(4) . . ? C25 C26 C27 119.7(4) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? N8 C27 C26 123.4(4) . . ? N8 C27 H27 118.3 . . ? C26 C27 H27 118.3 . . ? O7 C28 O8 125.6(4) . . ? O7 C28 C25 116.7(4) . . ? O8 C28 C25 117.6(4) . . ? N9 C29 C30 122.2(4) . . ? N9 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 117.3(4) . . ? C32 C31 C34 121.7(4) . . ? C30 C31 C34 121.0(4) . . ? C33 C32 C31 119.7(4) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? N9 C33 C32 123.3(4) . . ? N9 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? O10 C34 O9 126.4(4) . . ? O10 C34 C31 116.3(4) . . ? O9 C34 C31 117.3(4) . . ? N10 C35 C36 123.4(5) . . ? N10 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C35 C36 C37 119.7(5) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 117.4(4) . . ? C38 C37 C40 121.7(4) . . ? C36 C37 C40 120.9(4) . . ? C39 C38 C37 119.8(5) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? N10 C39 C38 123.5(4) . . ? N10 C39 H39 118.3 . . ? C38 C39 H39 118.3 . . ? O12 C40 O11 127.5(5) . . ? O12 C40 C37 116.8(4) . . ? O11 C40 C37 115.7(4) . . ? O14 C41 O13 121.4(4) . . ? O14 C41 C42 118.9(4) . . ? O13 C41 C42 119.8(5) . . ? O14 C41 Tb1 59.3(2) . . ? O13 C41 Tb1 63.8(2) . . ? C42 C41 Tb1 165.4(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 Cu1 C1 134.24(18) . . ? N4 Cu1 N5 102.23(15) . . ? C1 Cu1 N5 105.23(18) . . ? N4 Cu1 C1 101.14(16) . 3_767 ? C1 Cu1 C1 109.46(15) . 3_767 ? N5 Cu1 C1 99.47(16) . 3_767 ? N4 Cu1 Cu1 136.40(12) . 3_767 ? C1 Cu1 Cu1 62.28(14) . 3_767 ? N5 Cu1 Cu1 111.03(11) . 3_767 ? C1 Cu1 Cu1 47.18(12) 3_767 3_767 ? C3 Cu3 N2 120.79(18) . . ? C3 Cu3 N7 113.54(17) . 1_656 ? N2 Cu3 N7 99.36(15) . 1_656 ? C3 Cu3 C4 130.23(18) . . ? N2 Cu3 C4 92.38(15) . . ? N7 Cu3 C4 93.83(15) 1_656 . ? C3 Cu3 Cu4 87.11(15) . . ? N2 Cu3 Cu4 128.45(11) . . ? N7 Cu3 Cu4 107.84(11) 1_656 . ? C4 Cu3 Cu4 43.97(11) . . ? C4 Cu4 N3 141.97(18) . 4_575 ? C4 Cu4 N8 114.00(16) . . ? N3 Cu4 N8 101.79(15) 4_575 . ? C4 Cu4 Cu3 58.14(13) . . ? N3 Cu4 Cu3 122.68(13) 4_575 . ? N8 Cu4 Cu3 108.40(10) . . ? C4 Cu4 Cu5 68.62(13) . . ? N3 Cu4 Cu5 82.41(12) 4_575 . ? N8 Cu4 Cu5 121.19(10) . . ? Cu3 Cu4 Cu5 117.99(3) . . ? N10 Cu5 N9 168.56(19) 1_656 . ? N10 Cu5 Cu4 102.17(12) 1_656 . ? N9 Cu5 Cu4 76.05(11) . . ? O7 Tb1 O8 77.15(12) 1_554 4_575 ? O7 Tb1 O5 157.33(11) 1_554 . ? O8 Tb1 O5 87.01(10) 4_575 . ? O7 Tb1 O11 98.33(11) 1_554 . ? O8 Tb1 O11 141.08(11) 4_575 . ? O5 Tb1 O11 83.80(10) . . ? O7 Tb1 O9 89.27(11) 1_554 . ? O8 Tb1 O9 71.43(11) 4_575 . ? O5 Tb1 O9 101.07(11) . . ? O11 Tb1 O9 147.48(11) . . ? O7 Tb1 O14 73.11(11) 1_554 . ? O8 Tb1 O14 136.69(11) 4_575 . ? O5 Tb1 O14 128.65(10) . . ? O11 Tb1 O14 74.78(11) . . ? O9 Tb1 O14 77.37(12) . . ? O7 Tb1 O15W 80.64(10) 1_554 . ? O8 Tb1 O15W 69.87(11) 4_575 . ? O5 Tb1 O15W 78.70(10) . . ? O11 Tb1 O15W 71.25(10) . . ? O9 Tb1 O15W 141.27(11) . . ? O14 Tb1 O15W 132.98(10) . . ? O7 Tb1 O13 125.19(10) 1_554 . ? O8 Tb1 O13 137.95(11) 4_575 . ? O5 Tb1 O13 77.34(9) . . ? O11 Tb1 O13 76.17(10) . . ? O9 Tb1 O13 73.68(10) . . ? O14 Tb1 O13 52.59(9) . . ? O15W Tb1 O13 141.18(10) . . ? O7 Tb1 C41 99.24(13) 1_554 . ? O8 Tb1 C41 148.76(13) 4_575 . ? O5 Tb1 C41 102.65(12) . . ? O11 Tb1 C41 70.05(12) . . ? O9 Tb1 C41 77.54(13) . . ? O14 Tb1 C41 26.13(11) . . ? O15W Tb1 C41 140.85(12) . . ? O13 Tb1 C41 26.93(11) . . ? O10 Tb2 O3 146.18(11) . 3_667 ? O10 Tb2 O6 99.09(10) . . ? O3 Tb2 O6 83.81(11) 3_667 . ? O10 Tb2 O1 142.87(11) . 3_666 ? O3 Tb2 O1 70.90(13) 3_667 3_666 ? O6 Tb2 O1 83.81(12) . 3_666 ? O10 Tb2 O2 81.57(10) . . ? O3 Tb2 O2 75.47(11) 3_667 . ? O6 Tb2 O2 140.31(11) . . ? O1 Tb2 O2 119.22(11) 3_666 . ? O10 Tb2 O4 77.73(12) . 1_554 ? O3 Tb2 O4 118.23(13) 3_667 1_554 ? O6 Tb2 O4 145.03(11) . 1_554 ? O1 Tb2 O4 79.22(14) 3_666 1_554 ? O2 Tb2 O4 74.28(12) . 1_554 ? O10 Tb2 O16W 73.52(10) . . ? O3 Tb2 O16W 75.97(12) 3_667 . ? O6 Tb2 O16W 70.15(10) . . ? O1 Tb2 O16W 139.65(12) 3_666 . ? O2 Tb2 O16W 72.14(11) . . ? O4 Tb2 O16W 138.27(12) 1_554 . ? O10 Tb2 O13 71.27(10) . . ? O3 Tb2 O13 138.65(11) 3_667 . ? O6 Tb2 O13 69.12(10) . . ? O1 Tb2 O13 75.48(10) 3_666 . ? O2 Tb2 O13 143.97(10) . . ? O4 Tb2 O13 77.09(10) 1_554 . ? O16W Tb2 O13 119.70(9) . . ? C1 N1 Cu2 154.7(4) . . ? C1 N1 Cu2B 167.4(4) . 3_768 ? Cu2 N1 Cu2B 36.64(10) . 3_768 ? C2 N2 Cu3 167.7(4) . . ? C3 N3 Cu4 171.1(4) . 4_576 ? C4 N4 Cu1 163.1(4) . . ? C9 N5 C5 116.4(4) . . ? C9 N5 Cu1 122.0(3) . . ? C5 N5 Cu1 120.2(3) . . ? C17 N7 C21 116.8(4) . . ? C17 N7 Cu3 118.0(3) . 1_454 ? C21 N7 Cu3 124.4(3) . 1_454 ? C27 N8 C23 116.4(4) . . ? C27 N8 Cu4 120.6(3) . . ? C23 N8 Cu4 123.0(3) . . ? C33 N9 C29 117.5(4) . . ? C33 N9 Cu5 124.0(3) . . ? C29 N9 Cu5 118.6(3) . . ? C39 N10 C35 116.2(4) . . ? C39 N10 Cu5 120.1(3) . 1_454 ? C35 N10 Cu5 123.6(4) . 1_454 ? C10 O1 Tb2 146.8(3) . 3_666 ? C10 O2 Tb2 142.9(3) . . ? C16 O3 Tb2 154.4(3) . 3_667 ? C16 O4 Tb2 134.7(3) . 1_556 ? C22 O5 Tb1 129.2(2) . . ? C22 O6 Tb2 143.8(3) . . ? C28 O7 Tb1 172.0(3) . 1_556 ? C28 O8 Tb1 156.3(3) . 4_576 ? C34 O9 Tb1 135.8(3) . . ? C34 O10 Tb2 146.3(3) . . ? C40 O11 Tb1 134.5(3) . . ? C41 O13 Tb2 137.6(3) . . ? C41 O13 Tb1 89.3(2) . . ? Tb2 O13 Tb1 127.68(11) . . ? C41 O14 Tb1 94.5(3) . . ? Tb1 O15W H15A 151.5 . . ? Tb1 O15W H15W 100.8 . . ? H15A O15W H15W 107.7 . . ? Tb2 O16W H16A 118.9 . . ? Tb2 O16W H16B 131.9 . . ? H16A O16W H16B 107.7 . . ? O3 C16 O4 127.0(5) . . ? O3 C16 C13B 129.1(8) . . ? O4 C16 C13B 103.9(8) . . ? O3 C16 C13 111.4(5) . . ? O4 C16 C13 121.4(5) . . ? C13B C16 C13 17.7(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.563 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 964402' ####################################################################### # # 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_V-B #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H31 Cu5 Dy2 N10 O16' _chemical_formula_sum 'C42 H31 Cu5 Dy2 N10 O16' _chemical_formula_weight 1574.52 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.857(4) _cell_length_b 30.693(7) _cell_length_c 8.995(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.064(3) _cell_angle_gamma 90.00 _cell_volume 4782.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8790 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 25.40 _exptl_crystal_description platelike _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 5.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.288 _exptl_absorpt_correction_T_max 0.343 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25041 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.40 _reflns_number_total 8790 _reflns_number_gt 6951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0000P)^2^+15.2750P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00076(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8790 _refine_ls_number_parameters 706 _refine_ls_number_restraints 936 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu2 Cu 0.97373(8) 0.45186(4) 1.46372(16) 0.0385(5) Uani 0.645(2) 1 d P . 1 Cu2B Cu 0.95735(15) 0.54263(8) 1.4742(3) 0.0443(9) Uani 0.355(2) 1 d P . 2 C11 C 0.8041(6) 0.4375(3) 1.4265(13) 0.0340(13) Uani 0.645(2) 1 d PU . 1 H11 H 0.8222 0.4096 1.4553 0.041 Uiso 0.645(2) 1 calc PR . 1 C12 C 0.7275(6) 0.4449(3) 1.4097(13) 0.0340(14) Uani 0.645(2) 1 d PU . 1 H12 H 0.6948 0.4222 1.4204 0.041 Uiso 0.645(2) 1 calc PR . 1 C13 C 0.6979(9) 0.4874(3) 1.3759(17) 0.0310(14) Uani 0.645(2) 1 d PU . 1 C14 C 0.7485(6) 0.5179(3) 1.3447(13) 0.0338(13) Uani 0.645(2) 1 d PU . 1 H14 H 0.7312 0.5459 1.3147 0.041 Uiso 0.645(2) 1 calc PR . 1 C15 C 0.8271(8) 0.5067(4) 1.3583(16) 0.0356(13) Uani 0.645(2) 1 d PU . 1 H15 H 0.8600 0.5275 1.3338 0.043 Uiso 0.645(2) 1 calc PR . 1 N6 N 0.8557(5) 0.4673(3) 1.4050(12) 0.036(2) Uani 0.645(2) 1 d P . 1 C11B C 0.8235(13) 0.4778(7) 1.405(3) 0.0340(13) Uani 0.355(2) 1 d PU . 2 H11B H 0.8590 0.4550 1.4213 0.041 Uiso 0.355(2) 1 calc PR . 2 C12B C 0.7421(12) 0.4692(7) 1.406(2) 0.0340(14) Uani 0.355(2) 1 d PU . 2 H12B H 0.7270 0.4426 1.4389 0.041 Uiso 0.355(2) 1 calc PR . 2 C13B C 0.6926(16) 0.5002(6) 1.359(3) 0.0310(14) Uani 0.355(2) 1 d PU . 2 C14B C 0.7142(11) 0.5396(6) 1.305(2) 0.0338(13) Uani 0.355(2) 1 d PU . 2 H14B H 0.6775 0.5604 1.2615 0.041 Uiso 0.355(2) 1 calc PR . 2 C15B C 0.7929(11) 0.5471(6) 1.319(2) 0.0356(13) Uani 0.355(2) 1 d PU . 2 H15B H 0.8081 0.5731 1.2816 0.043 Uiso 0.355(2) 1 calc PR . 2 N6B N 0.8462(11) 0.5183(6) 1.382(2) 0.036(2) Uani 0.355(2) 1 d P . 2 C1 C 1.0111(4) 0.4980(2) 1.1992(9) 0.0410(17) Uani 1 1 d U . . C2 C 0.9918(5) 0.5950(2) 1.3932(9) 0.0457(17) Uani 1 1 d U . . C3 C 0.9673(4) 0.7315(2) 1.2230(8) 0.0347(16) Uani 1 1 d . . . C4 C 0.9669(4) 0.6323(2) 0.9639(8) 0.0317(14) Uani 1 1 d U . . C5 C 0.8156(4) 0.4875(2) 0.9418(9) 0.0504(16) Uani 1 1 d U . . H5 H 0.8470 0.4631 0.9642 0.061 Uiso 1 1 calc R . . C6 C 0.7390(4) 0.4815(2) 0.8707(9) 0.0481(17) Uani 1 1 d U . . H6 H 0.7199 0.4536 0.8454 0.058 Uiso 1 1 calc R . . C7 C 0.6910(4) 0.51685(19) 0.8374(8) 0.0302(13) Uani 1 1 d U . . C8 C 0.7214(4) 0.5567(2) 0.8906(8) 0.0381(14) Uani 1 1 d U . . H8 H 0.6899 0.5812 0.8805 0.046 Uiso 1 1 calc R . . C9 C 0.7993(4) 0.5599(2) 0.9590(8) 0.0387(13) Uani 1 1 d U . . H9 H 0.8192 0.5872 0.9921 0.046 Uiso 1 1 calc R . . C10 C 0.6118(4) 0.5123(2) 0.7337(8) 0.0319(14) Uani 1 1 d U . . C17 C 0.1524(4) 0.6316(2) 0.2438(8) 0.0381(14) Uani 1 1 d U . . H17 H 0.1215 0.6073 0.2449 0.046 Uiso 1 1 calc R . . C18 C 0.2309(4) 0.6267(2) 0.2843(8) 0.0353(14) Uani 1 1 d U . . H18 H 0.2521 0.5995 0.3149 0.042 Uiso 1 1 calc R . . C19 C 0.2785(4) 0.66143(19) 0.2801(7) 0.0267(13) Uani 1 1 d U . . C20 C 0.2447(4) 0.7010(2) 0.2327(9) 0.0393(15) Uani 1 1 d U . . H20 H 0.2746 0.7254 0.2258 0.047 Uiso 1 1 calc R . . C21 C 0.1656(4) 0.7034(2) 0.1960(9) 0.0421(15) Uani 1 1 d U . . H21 H 0.1431 0.7302 0.1640 0.050 Uiso 1 1 calc R . . C22 C 0.3651(4) 0.65507(19) 0.3242(7) 0.0274(13) Uani 1 1 d U . . C23 C 0.7749(4) 0.6810(2) 0.9719(8) 0.0335(14) Uani 1 1 d U . . H23 H 0.8036 0.6643 1.0520 0.040 Uiso 1 1 calc R . . C24 C 0.6976(4) 0.68768(19) 0.9655(8) 0.0301(13) Uani 1 1 d U . . H24 H 0.6751 0.6755 1.0388 0.036 Uiso 1 1 calc R . . C25 C 0.6540(3) 0.71313(18) 0.8464(7) 0.0239(12) Uani 1 1 d U . . C26 C 0.6897(4) 0.7282(2) 0.7382(8) 0.0306(13) Uani 1 1 d U . . H26 H 0.6618 0.7438 0.6543 0.037 Uiso 1 1 calc R . . C27 C 0.7676(4) 0.7201(2) 0.7541(8) 0.0327(12) Uani 1 1 d U . . H27 H 0.7911 0.7313 0.6805 0.039 Uiso 1 1 calc R . . C28 C 0.5725(4) 0.72655(18) 0.8446(7) 0.0252(13) Uani 1 1 d U . . C29 C 0.8447(4) 0.6664(2) 0.4670(8) 0.0384(14) Uani 1 1 d U . . H29 H 0.8771 0.6852 0.4311 0.046 Uiso 1 1 calc R . . C30 C 0.7670(4) 0.6694(2) 0.4052(8) 0.0361(14) Uani 1 1 d U . . H30 H 0.7476 0.6893 0.3275 0.043 Uiso 1 1 calc R . . C31 C 0.7175(4) 0.6423(2) 0.4601(7) 0.0275(13) Uani 1 1 d U . . C32 C 0.7501(4) 0.6121(2) 0.5705(8) 0.0370(14) Uani 1 1 d U . . H32 H 0.7190 0.5927 0.6074 0.044 Uiso 1 1 calc R . . C33 C 0.8288(4) 0.6111(2) 0.6254(8) 0.0406(14) Uani 1 1 d U . . H33 H 0.8498 0.5908 0.7005 0.049 Uiso 1 1 calc R . . C34 C 0.6310(4) 0.6456(2) 0.4007(8) 0.0303(13) Uani 1 1 d U . . C35 C 0.1420(4) 0.6297(2) -0.1675(9) 0.0454(16) Uani 1 1 d U . . H35 H 0.1207 0.6119 -0.1047 0.054 Uiso 1 1 calc R . . C36 C 0.2208(4) 0.6358(2) -0.1287(9) 0.0415(14) Uani 1 1 d U . . H36 H 0.2513 0.6228 -0.0414 0.050 Uiso 1 1 calc R . . C37 C 0.2539(4) 0.6616(2) -0.2216(8) 0.0328(14) Uani 1 1 d U . . C38 C 0.2056(4) 0.6796(2) -0.3491(8) 0.0384(15) Uani 1 1 d U . . H38 H 0.2257 0.6967 -0.4156 0.046 Uiso 1 1 calc R . . C39 C 0.1276(4) 0.6723(2) -0.3780(9) 0.0431(16) Uani 1 1 d U . . H39 H 0.0959 0.6852 -0.4641 0.052 Uiso 1 1 calc R . . C40 C 0.3407(4) 0.6690(2) -0.1837(9) 0.0354(15) Uani 1 1 d U . . C41 C 0.5044(4) 0.5964(2) 0.0713(8) 0.0380(17) Uani 1 1 d U . . C42 C 0.4955(6) 0.5513(2) 0.0108(10) 0.081(3) Uani 1 1 d U . . H42A H 0.4605 0.5513 -0.0890 0.122 Uiso 1 1 calc R . . H42B H 0.4753 0.5331 0.0786 0.122 Uiso 1 1 calc R . . H42C H 0.5448 0.5404 0.0034 0.122 Uiso 1 1 calc R . . Cu1 Cu 0.96769(5) 0.53463(3) 1.02263(11) 0.0389(2) Uani 1 1 d . . . Cu3 Cu 0.99967(5) 0.67466(3) 1.18351(11) 0.0355(2) Uani 1 1 d . . . Cu4 Cu 0.92937(5) 0.68809(2) 0.88896(10) 0.0352(2) Uani 1 1 d . . . Cu5 Cu 0.98608(5) 0.63727(4) 0.65207(13) 0.0628(3) Uani 1 1 d . . . Dy1 Dy 0.486308(16) 0.685462(9) 0.12318(3) 0.02046(9) Uani 1 1 d . . . Dy2 Dy 0.494568(16) 0.573798(8) 0.45449(3) 0.02293(9) Uani 1 1 d . . . N1 N 1.0137(4) 0.48390(19) 1.3153(8) 0.0448(16) Uani 1 1 d . . . N2 N 0.9864(3) 0.62515(18) 1.3161(7) 0.0390(14) Uani 1 1 d . . . N3 N 0.9534(3) 0.76334(18) 1.2739(7) 0.0419(15) Uani 1 1 d . . . N4 N 0.9771(3) 0.59548(17) 0.9761(6) 0.0335(14) Uani 1 1 d . . . N5 N 0.8472(3) 0.52636(17) 0.9803(7) 0.0412(16) Uani 1 1 d . . . N7 N 0.1184(3) 0.66998(16) 0.2029(7) 0.0317(13) Uani 1 1 d . . . N8 N 0.8107(3) 0.69710(16) 0.8699(7) 0.0322(13) Uani 1 1 d . . . N9 N 0.8767(3) 0.63784(19) 0.5764(7) 0.0370(14) Uani 1 1 d . . . N10 N 0.0944(3) 0.6475(2) -0.2890(7) 0.0418(15) Uani 1 1 d . . . O1 O 0.5845(3) 0.47469(16) 0.7143(6) 0.0513(14) Uani 1 1 d . . . O2 O 0.5815(3) 0.54627(15) 0.6718(6) 0.0419(12) Uani 1 1 d . . . O3 O 0.5823(3) 0.46427(17) 1.4126(6) 0.0535(15) Uani 1 1 d . . . O4 O 0.5870(4) 0.53399(17) 1.3624(6) 0.0646(17) Uani 1 1 d . . . O5 O 0.4077(2) 0.68516(13) 0.2945(5) 0.0268(10) Uani 1 1 d . . . O6 O 0.3882(2) 0.61975(14) 0.3861(5) 0.0345(11) Uani 1 1 d . . . O7 O 0.5470(3) 0.71342(15) 0.9529(6) 0.0394(12) Uani 1 1 d . . . O8 O 0.5381(3) 0.75024(14) 0.7407(6) 0.0419(13) Uani 1 1 d . . . O9 O 0.6068(3) 0.66995(15) 0.2881(6) 0.0436(13) Uani 1 1 d . . . O10 O 0.5906(2) 0.62447(14) 0.4709(5) 0.0327(11) Uani 1 1 d . . . O11 O 0.3768(3) 0.65857(14) -0.0496(6) 0.0382(12) Uani 1 1 d . . . O12 O 0.3686(3) 0.68353(17) -0.2872(7) 0.0562(15) Uani 1 1 d . . . O13 O 0.4838(3) 0.60608(12) 0.1925(5) 0.0297(10) Uani 1 1 d . . . O14 O 0.5310(3) 0.62438(14) -0.0019(5) 0.0394(12) Uani 1 1 d . . . O15W O 0.3987(3) 0.74739(13) 0.0255(5) 0.0362(12) Uani 1 1 d . . . H15A H 0.3603 0.7583 -0.0383 0.043 Uiso 1 1 d R . . H15W H 0.4165 0.7667 0.0925 0.043 Uiso 1 1 d R . . O16W O 0.4896(3) 0.62147(14) 0.6697(5) 0.0417(12) Uani 1 1 d . . . H16A H 0.4518 0.6389 0.6605 0.050 Uiso 1 1 d R . . H16B H 0.5133 0.6208 0.7638 0.050 Uiso 1 1 d R . . C16 C 0.6149(4) 0.4969(2) 1.3803(8) 0.0307(13) Uani 1 1 d U . . 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 Cu2 0.0303(9) 0.0442(8) 0.0408(9) 0.0118(6) 0.0082(7) 0.0028(6) Cu2B 0.0347(18) 0.0539(16) 0.0450(17) 0.0161(12) 0.0113(14) -0.0008(12) C11 0.030(3) 0.030(3) 0.043(3) 0.006(2) 0.012(2) 0.001(2) C12 0.030(3) 0.030(3) 0.044(3) 0.006(3) 0.013(2) 0.001(2) C13 0.029(2) 0.029(3) 0.037(3) 0.003(3) 0.012(2) 0.001(3) C14 0.031(3) 0.029(3) 0.042(3) 0.007(2) 0.010(2) 0.001(2) C15 0.032(2) 0.031(2) 0.044(2) 0.006(2) 0.010(2) -0.001(2) N6 0.030(5) 0.032(5) 0.047(5) 0.007(4) 0.014(4) 0.006(4) C11B 0.030(3) 0.030(3) 0.043(3) 0.006(2) 0.012(2) 0.001(2) C12B 0.030(3) 0.030(3) 0.044(3) 0.006(3) 0.013(2) 0.001(2) C13B 0.029(2) 0.029(3) 0.037(3) 0.003(3) 0.012(2) 0.001(3) C14B 0.031(3) 0.029(3) 0.042(3) 0.007(2) 0.010(2) 0.001(2) C15B 0.032(2) 0.031(2) 0.044(2) 0.006(2) 0.010(2) -0.001(2) N6B 0.030(5) 0.032(5) 0.047(5) 0.007(4) 0.014(4) 0.006(4) C1 0.045(4) 0.038(3) 0.039(4) 0.001(3) 0.009(3) 0.001(3) C2 0.061(4) 0.042(4) 0.041(4) 0.001(3) 0.026(4) 0.002(3) C3 0.025(4) 0.037(4) 0.044(4) -0.001(3) 0.011(3) 0.007(3) C4 0.032(3) 0.030(3) 0.031(3) -0.002(3) 0.004(3) 0.000(3) C5 0.041(3) 0.034(3) 0.068(3) 0.003(3) -0.002(3) 0.005(3) C6 0.039(3) 0.030(3) 0.068(4) 0.000(3) -0.001(3) -0.003(3) C7 0.029(3) 0.023(3) 0.036(3) 0.003(2) 0.004(3) -0.002(2) C8 0.034(3) 0.031(2) 0.045(3) -0.002(2) 0.002(2) 0.005(2) C9 0.033(3) 0.035(2) 0.046(3) -0.005(2) 0.004(2) -0.003(2) C10 0.028(3) 0.032(3) 0.034(3) -0.003(2) 0.004(3) -0.002(2) C17 0.030(3) 0.030(3) 0.054(3) 0.003(3) 0.010(3) 0.001(2) C18 0.029(3) 0.028(3) 0.050(3) 0.006(2) 0.011(3) 0.007(2) C19 0.024(3) 0.025(3) 0.034(3) 0.003(2) 0.013(2) 0.003(2) C20 0.026(3) 0.035(3) 0.055(3) 0.010(3) 0.006(3) -0.001(2) C21 0.029(3) 0.034(3) 0.059(3) 0.011(3) 0.003(3) 0.004(3) C22 0.027(3) 0.026(3) 0.030(3) 0.002(2) 0.009(3) 0.005(2) C23 0.033(3) 0.031(3) 0.036(3) 0.007(2) 0.006(3) 0.005(2) C24 0.028(3) 0.028(3) 0.036(3) 0.009(2) 0.010(3) 0.002(2) C25 0.022(3) 0.023(2) 0.028(3) 0.002(2) 0.007(2) -0.001(2) C26 0.026(3) 0.034(3) 0.033(3) 0.010(2) 0.009(3) 0.003(2) C27 0.029(3) 0.037(2) 0.034(3) 0.006(2) 0.010(2) 0.002(2) C28 0.027(3) 0.022(3) 0.028(3) 0.002(2) 0.011(3) -0.002(2) C29 0.028(3) 0.049(3) 0.037(3) 0.007(3) 0.004(3) -0.008(3) C30 0.027(3) 0.044(3) 0.034(3) 0.011(3) 0.002(3) -0.003(2) C31 0.023(3) 0.033(3) 0.025(3) 0.002(2) 0.003(2) -0.002(2) C32 0.028(3) 0.041(3) 0.039(3) 0.009(2) 0.003(2) -0.006(2) C33 0.034(3) 0.044(3) 0.038(3) 0.005(2) -0.002(2) -0.001(2) C34 0.029(3) 0.031(3) 0.030(3) 0.002(2) 0.004(3) -0.003(2) C35 0.032(3) 0.058(3) 0.044(3) 0.005(3) 0.006(3) -0.002(3) C36 0.032(3) 0.051(3) 0.038(3) 0.008(3) 0.001(3) -0.001(2) C37 0.024(3) 0.040(3) 0.032(3) -0.005(3) 0.002(3) 0.000(2) C38 0.030(3) 0.043(3) 0.037(3) 0.002(3) -0.001(3) 0.003(3) C39 0.033(3) 0.048(3) 0.042(3) 0.000(3) -0.003(3) 0.005(3) C40 0.027(3) 0.034(3) 0.042(3) -0.003(3) 0.001(3) 0.001(2) C41 0.053(4) 0.025(3) 0.038(4) -0.005(3) 0.012(3) 0.002(3) C42 0.164(10) 0.033(4) 0.052(5) -0.005(4) 0.036(6) 0.001(5) Cu1 0.0336(5) 0.0285(4) 0.0507(6) 0.0086(4) 0.0023(4) 0.0040(3) Cu3 0.0288(5) 0.0298(4) 0.0481(6) -0.0006(4) 0.0098(4) 0.0052(3) Cu4 0.0309(5) 0.0273(4) 0.0473(6) 0.0093(4) 0.0092(4) 0.0041(3) Cu5 0.0182(5) 0.0990(9) 0.0653(7) 0.0059(6) -0.0009(5) 0.0014(5) Dy1 0.01539(16) 0.02354(15) 0.02226(17) 0.00002(11) 0.00419(12) -0.00068(11) Dy2 0.01798(17) 0.02175(15) 0.02783(18) 0.00429(12) 0.00320(13) -0.00099(11) N1 0.048(4) 0.045(4) 0.041(4) 0.001(3) 0.011(3) 0.007(3) N2 0.047(4) 0.039(3) 0.034(3) -0.001(3) 0.016(3) -0.001(3) N3 0.040(4) 0.034(3) 0.054(4) -0.009(3) 0.017(3) 0.000(3) N4 0.034(3) 0.031(3) 0.033(3) -0.004(2) 0.003(3) -0.003(2) N5 0.027(3) 0.035(3) 0.055(4) 0.004(3) -0.003(3) 0.005(2) N7 0.019(3) 0.026(3) 0.048(4) 0.002(2) 0.004(3) 0.000(2) N8 0.024(3) 0.030(3) 0.042(4) 0.007(3) 0.007(3) 0.002(2) N9 0.022(3) 0.055(4) 0.031(3) -0.004(3) 0.002(3) 0.000(3) N10 0.020(3) 0.066(4) 0.038(4) -0.005(3) 0.003(3) 0.002(3) O1 0.050(3) 0.045(3) 0.050(3) 0.001(2) -0.005(3) -0.021(2) O2 0.030(3) 0.048(3) 0.043(3) 0.006(2) 0.000(2) 0.000(2) O3 0.036(3) 0.068(4) 0.059(4) 0.024(3) 0.016(3) -0.017(3) O4 0.092(5) 0.048(3) 0.055(4) -0.003(3) 0.019(3) 0.036(3) O5 0.021(2) 0.031(2) 0.030(3) -0.0048(19) 0.012(2) -0.0022(18) O6 0.023(2) 0.037(3) 0.043(3) 0.016(2) 0.009(2) 0.0104(19) O7 0.030(3) 0.052(3) 0.040(3) 0.013(2) 0.015(2) 0.005(2) O8 0.031(3) 0.039(3) 0.055(3) 0.019(2) 0.009(3) 0.013(2) O9 0.030(3) 0.044(3) 0.050(3) 0.020(2) -0.005(2) -0.007(2) O10 0.025(3) 0.039(3) 0.034(3) 0.003(2) 0.007(2) -0.009(2) O11 0.025(3) 0.039(3) 0.043(3) -0.002(2) -0.006(2) -0.002(2) O12 0.033(3) 0.069(4) 0.067(4) 0.016(3) 0.013(3) -0.009(3) O13 0.042(3) 0.022(2) 0.027(3) -0.0038(18) 0.011(2) -0.0021(19) O14 0.048(3) 0.037(3) 0.038(3) 0.000(2) 0.021(3) 0.004(2) O15W 0.035(3) 0.028(2) 0.045(3) 0.005(2) 0.007(2) 0.0090(19) O16W 0.047(3) 0.048(3) 0.030(3) -0.004(2) 0.008(2) 0.014(2) C16 0.028(3) 0.035(3) 0.034(3) 0.003(2) 0.017(2) 0.004(2) _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 Cu2 C2 1.928(8) 3_768 ? Cu2 N1 1.929(7) . ? Cu2 N6 2.098(9) . ? Cu2B C2 1.926(8) . ? Cu2B N1 2.010(7) 3_768 ? Cu2B N6B 2.093(18) . ? Cu2B Cu2B 3.006(5) 3_768 ? C11 N6 1.346(13) . ? C11 C12 1.357(14) . ? C11 H11 0.9300 . ? C12 C13 1.411(14) . ? C12 H12 0.9300 . ? C13 C14 1.377(17) . ? C13 C16 1.520(16) . ? C14 C15 1.421(17) . ? C14 H14 0.9300 . ? C15 N6 1.340(15) . ? C15 H15 0.9300 . ? C11B N6B 1.34(3) . ? C11B C12B 1.48(3) . ? C11B H11B 0.9300 . ? C12B C13B 1.30(3) . ? C12B H12B 0.9300 . ? C13B C14B 1.39(3) . ? C13B C16 1.45(3) . ? C14B C15B 1.40(3) . ? C14B H14B 0.9300 . ? C15B N6B 1.32(3) . ? C15B H15B 0.9300 . ? C1 N1 1.121(9) . ? C1 Cu1 1.946(8) . ? C1 Cu1 2.344(8) 3_767 ? C2 N2 1.147(9) . ? C2 Cu2 1.928(8) 3_768 ? C3 N3 1.132(8) . ? C3 Cu3 1.898(7) . ? C4 N4 1.144(7) . ? C4 Cu4 1.903(6) . ? C4 Cu3 2.319(6) . ? C5 N5 1.328(9) . ? C5 C6 1.374(10) . ? C5 H5 0.9300 . ? C6 C7 1.370(9) . ? C6 H6 0.9300 . ? C7 C8 1.377(8) . ? C7 C10 1.500(9) . ? C8 C9 1.380(9) . ? C8 H8 0.9300 . ? C9 N5 1.323(8) . ? C9 H9 0.9300 . ? C10 O2 1.242(7) . ? C10 O1 1.249(7) . ? C17 N7 1.334(8) . ? C17 C18 1.369(9) . ? C17 H17 0.9300 . ? C18 C19 1.370(9) . ? C18 H18 0.9300 . ? C19 C20 1.378(8) . ? C19 C22 1.513(8) . ? C20 C21 1.372(9) . ? C20 H20 0.9300 . ? C21 N7 1.338(8) . ? C21 H21 0.9300 . ? C22 O6 1.243(7) . ? C22 O5 1.265(7) . ? C23 N8 1.334(8) . ? C23 C24 1.382(9) . ? C23 H23 0.9300 . ? C24 C25 1.400(8) . ? C24 H24 0.9300 . ? C25 C26 1.366(9) . ? C25 C28 1.509(8) . ? C26 C27 1.386(9) . ? C26 H26 0.9300 . ? C27 N8 1.337(8) . ? C27 H27 0.9300 . ? C28 O8 1.225(7) . ? C28 O7 1.239(7) . ? C29 N9 1.337(8) . ? C29 C30 1.366(9) . ? C29 H29 0.9300 . ? C30 C31 1.390(9) . ? C30 H30 0.9300 . ? C31 C32 1.379(8) . ? C31 C34 1.509(9) . ? C32 C33 1.372(9) . ? C32 H32 0.9300 . ? C33 N9 1.334(9) . ? C33 H33 0.9300 . ? C34 O9 1.248(7) . ? C34 O10 1.250(7) . ? C35 N10 1.328(9) . ? C35 C36 1.379(9) . ? C35 H35 0.9300 . ? C36 C37 1.384(10) . ? C36 H36 0.9300 . ? C37 C38 1.372(9) . ? C37 C40 1.521(9) . ? C38 C39 1.373(9) . ? C38 H38 0.9300 . ? C39 N10 1.340(9) . ? C39 H39 0.9300 . ? C40 O12 1.241(9) . ? C40 O11 1.263(8) . ? C41 O14 1.245(8) . ? C41 O13 1.268(8) . ? C41 C42 1.480(10) . ? C41 Dy1 2.806(6) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Cu1 N4 1.930(5) . ? Cu1 N5 2.107(6) . ? Cu1 C1 2.344(8) 3_767 ? Cu1 Cu1 2.4989(17) 3_767 ? Cu3 N2 1.981(6) . ? Cu3 N7 2.090(5) 1_656 ? Cu3 Cu4 2.6737(14) . ? Cu4 N3 1.922(6) 4_575 ? Cu4 N8 2.102(5) . ? Cu4 Cu5 3.0079(16) . ? Cu5 N10 1.904(6) 1_656 ? Cu5 N9 1.906(5) . ? Dy1 O7 2.250(5) 1_554 ? Dy1 O8 2.322(4) 4_575 ? Dy1 O5 2.323(4) . ? Dy1 O11 2.332(4) . ? Dy1 O9 2.346(4) . ? Dy1 O14 2.419(4) . ? Dy1 O15W 2.482(4) . ? Dy1 O13 2.518(4) . ? Dy2 O10 2.293(4) . ? Dy2 O6 2.325(4) . ? Dy2 O2 2.339(5) . ? Dy2 O1 2.339(5) 3_666 ? Dy2 O3 2.340(5) 3_667 ? Dy2 O4 2.360(5) 1_554 ? Dy2 O16W 2.445(4) . ? Dy2 O13 2.520(4) . ? N1 Cu2B 2.010(7) 3_768 ? N3 Cu4 1.922(6) 4_576 ? N7 Cu3 2.090(5) 1_454 ? N10 Cu5 1.904(6) 1_454 ? O1 Dy2 2.339(5) 3_666 ? O3 C16 1.228(8) . ? O3 Dy2 2.340(5) 3_667 ? O4 C16 1.238(7) . ? O4 Dy2 2.360(5) 1_556 ? O7 Dy1 2.250(5) 1_556 ? O8 Dy1 2.322(4) 4_576 ? O15W H15A 0.8500 . ? O15W H15W 0.8499 . ? O16W H16A 0.8499 . ? O16W H16B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Cu2 N1 136.9(3) 3_768 . ? C2 Cu2 N6 118.3(4) 3_768 . ? N1 Cu2 N6 103.2(3) . . ? C2 Cu2B N1 131.4(3) . 3_768 ? C2 Cu2B N6B 120.5(6) . . ? N1 Cu2B N6B 103.3(6) 3_768 . ? C2 Cu2B Cu2B 126.0(3) . 3_768 ? N1 Cu2B Cu2B 59.80(19) 3_768 3_768 ? N6B Cu2B Cu2B 98.5(5) . 3_768 ? N6 C11 C12 125.2(10) . . ? N6 C11 H11 117.4 . . ? C12 C11 H11 117.4 . . ? C11 C12 C13 119.6(11) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 116.3(13) . . ? C14 C13 C16 124.5(9) . . ? C12 C13 C16 119.2(10) . . ? C13 C14 C15 120.1(10) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N6 C15 C14 122.6(11) . . ? N6 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C15 N6 C11 115.9(10) . . ? C15 N6 Cu2 124.4(9) . . ? C11 N6 Cu2 119.5(7) . . ? N6B C11B C12B 120.0(19) . . ? N6B C11B H11B 120.0 . . ? C12B C11B H11B 120.0 . . ? C13B C12B C11B 118(2) . . ? C13B C12B H12B 121.2 . . ? C11B C12B H12B 121.2 . . ? C12B C13B C14B 122(2) . . ? C12B C13B C16 120.3(19) . . ? C14B C13B C16 117.6(17) . . ? C13B C14B C15B 118.0(19) . . ? C13B C14B H14B 121.0 . . ? C15B C14B H14B 121.0 . . ? N6B C15B C14B 122.1(18) . . ? N6B C15B H15B 118.9 . . ? C14B C15B H15B 118.9 . . ? C15B N6B C11B 118.2(19) . . ? C15B N6B Cu2B 116.6(13) . . ? C11B N6B Cu2B 124.2(16) . . ? N1 C1 Cu1 154.4(7) . . ? N1 C1 Cu1 130.5(6) . 3_767 ? Cu1 C1 Cu1 70.5(3) . 3_767 ? N2 C2 Cu2B 156.1(7) . . ? N2 C2 Cu2 166.5(7) . 3_768 ? Cu2B C2 Cu2 37.33(17) . 3_768 ? N3 C3 Cu3 167.4(7) . . ? N4 C4 Cu4 163.0(6) . . ? N4 C4 Cu3 118.1(5) . . ? Cu4 C4 Cu3 77.9(2) . . ? N5 C5 C6 123.7(7) . . ? N5 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C7 C6 C5 119.6(7) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 117.1(6) . . ? C6 C7 C10 120.5(6) . . ? C8 C7 C10 122.1(6) . . ? C7 C8 C9 119.2(6) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? N5 C9 C8 123.7(6) . . ? N5 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? O2 C10 O1 126.9(6) . . ? O2 C10 C7 116.3(6) . . ? O1 C10 C7 116.8(6) . . ? N7 C17 C18 122.6(6) . . ? N7 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C17 C18 C19 120.6(6) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 117.9(6) . . ? C18 C19 C22 119.6(5) . . ? C20 C19 C22 122.5(6) . . ? C21 C20 C19 118.0(6) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? N7 C21 C20 124.8(6) . . ? N7 C21 H21 117.6 . . ? C20 C21 H21 117.6 . . ? O6 C22 O5 125.5(6) . . ? O6 C22 C19 115.9(5) . . ? O5 C22 C19 118.6(5) . . ? N8 C23 C24 123.8(6) . . ? N8 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C23 C24 C25 118.6(6) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? C26 C25 C24 117.7(6) . . ? C26 C25 C28 121.1(5) . . ? C24 C25 C28 121.1(6) . . ? C25 C26 C27 119.8(6) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? N8 C27 C26 123.2(6) . . ? N8 C27 H27 118.4 . . ? C26 C27 H27 118.4 . . ? O8 C28 O7 125.5(6) . . ? O8 C28 C25 118.3(6) . . ? O7 C28 C25 116.2(5) . . ? N9 C29 C30 123.7(7) . . ? N9 C29 H29 118.1 . . ? C30 C29 H29 118.1 . . ? C29 C30 C31 119.0(6) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C32 C31 C30 117.6(6) . . ? C32 C31 C34 121.1(6) . . ? C30 C31 C34 121.2(6) . . ? C33 C32 C31 119.4(6) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? N9 C33 C32 123.4(6) . . ? N9 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? O9 C34 O10 126.3(6) . . ? O9 C34 C31 116.8(6) . . ? O10 C34 C31 116.9(6) . . ? N10 C35 C36 124.1(7) . . ? N10 C35 H35 117.9 . . ? C36 C35 H35 117.9 . . ? C35 C36 C37 119.0(7) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C38 C37 C36 117.6(6) . . ? C38 C37 C40 121.7(7) . . ? C36 C37 C40 120.7(6) . . ? C37 C38 C39 119.6(7) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? N10 C39 C38 123.8(7) . . ? N10 C39 H39 118.1 . . ? C38 C39 H39 118.1 . . ? O12 C40 O11 126.9(7) . . ? O12 C40 C37 117.3(6) . . ? O11 C40 C37 115.7(7) . . ? O14 C41 O13 121.3(6) . . ? O14 C41 C42 118.1(7) . . ? O13 C41 C42 120.5(7) . . ? O14 C41 Dy1 59.3(3) . . ? O13 C41 Dy1 63.8(3) . . ? C42 C41 Dy1 164.8(6) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 Cu1 C1 134.2(3) . . ? N4 Cu1 N5 102.5(2) . . ? C1 Cu1 N5 105.3(3) . . ? N4 Cu1 C1 100.9(2) . 3_767 ? C1 Cu1 C1 109.5(3) . 3_767 ? N5 Cu1 C1 99.4(3) . 3_767 ? N4 Cu1 Cu1 136.06(18) . 3_767 ? C1 Cu1 Cu1 62.2(2) . 3_767 ? N5 Cu1 Cu1 111.08(16) . 3_767 ? C1 Cu1 Cu1 47.26(18) 3_767 3_767 ? C3 Cu3 N2 120.4(3) . . ? C3 Cu3 N7 113.3(2) . 1_656 ? N2 Cu3 N7 99.5(2) . 1_656 ? C3 Cu3 C4 130.6(3) . . ? N2 Cu3 C4 92.3(2) . . ? N7 Cu3 C4 94.2(2) 1_656 . ? C3 Cu3 Cu4 87.3(2) . . ? N2 Cu3 Cu4 128.20(17) . . ? N7 Cu3 Cu4 108.42(17) 1_656 . ? C4 Cu3 Cu4 44.10(16) . . ? C4 Cu4 N3 141.6(3) . 4_575 ? C4 Cu4 N8 114.1(3) . . ? N3 Cu4 N8 101.9(2) 4_575 . ? C4 Cu4 Cu3 58.0(2) . . ? N3 Cu4 Cu3 122.73(19) 4_575 . ? N8 Cu4 Cu3 108.80(16) . . ? C4 Cu4 Cu5 68.5(2) . . ? N3 Cu4 Cu5 82.12(19) 4_575 . ? N8 Cu4 Cu5 121.11(16) . . ? Cu3 Cu4 Cu5 117.66(4) . . ? N10 Cu5 N9 169.1(3) 1_656 . ? N10 Cu5 Cu4 102.21(19) 1_656 . ? N9 Cu5 Cu4 75.87(18) . . ? O7 Dy1 O8 77.38(18) 1_554 4_575 ? O7 Dy1 O5 157.17(15) 1_554 . ? O8 Dy1 O5 86.53(16) 4_575 . ? O7 Dy1 O11 98.37(17) 1_554 . ? O8 Dy1 O11 141.31(16) 4_575 . ? O5 Dy1 O11 84.08(16) . . ? O7 Dy1 O9 89.34(17) 1_554 . ? O8 Dy1 O9 71.47(17) 4_575 . ? O5 Dy1 O9 100.88(17) . . ? O11 Dy1 O9 147.20(16) . . ? O7 Dy1 O14 73.21(17) 1_554 . ? O8 Dy1 O14 136.93(17) 4_575 . ? O5 Dy1 O14 128.76(15) . . ? O11 Dy1 O14 74.55(16) . . ? O9 Dy1 O14 77.38(17) . . ? O7 Dy1 O15W 80.40(16) 1_554 . ? O8 Dy1 O15W 69.95(16) 4_575 . ? O5 Dy1 O15W 78.91(15) . . ? O11 Dy1 O15W 71.42(15) . . ? O9 Dy1 O15W 141.37(15) . . ? O14 Dy1 O15W 132.79(16) . . ? O7 Dy1 O13 125.32(16) 1_554 . ? O8 Dy1 O13 137.63(16) 4_575 . ? O5 Dy1 O13 77.39(14) . . ? O11 Dy1 O13 76.11(15) . . ? O9 Dy1 O13 73.50(14) . . ? O14 Dy1 O13 52.64(15) . . ? O15W Dy1 O13 141.33(14) . . ? O7 Dy1 C41 99.5(2) 1_554 . ? O8 Dy1 C41 148.74(19) 4_575 . ? O5 Dy1 C41 102.64(19) . . ? O11 Dy1 C41 69.88(18) . . ? O9 Dy1 C41 77.43(19) . . ? O14 Dy1 C41 26.26(18) . . ? O15W Dy1 C41 140.85(18) . . ? O13 Dy1 C41 26.86(17) . . ? O10 Dy2 O6 98.95(15) . . ? O10 Dy2 O2 81.78(16) . . ? O6 Dy2 O2 140.70(17) . . ? O10 Dy2 O1 142.86(18) . 3_666 ? O6 Dy2 O1 83.63(18) . 3_666 ? O2 Dy2 O1 119.07(17) . 3_666 ? O10 Dy2 O3 145.89(18) . 3_667 ? O6 Dy2 O3 84.00(17) . 3_667 ? O2 Dy2 O3 75.23(17) . 3_667 ? O1 Dy2 O3 71.20(19) 3_666 3_667 ? O10 Dy2 O4 78.33(19) . 1_554 ? O6 Dy2 O4 144.80(18) . 1_554 ? O2 Dy2 O4 74.19(19) . 1_554 ? O1 Dy2 O4 78.8(2) 3_666 1_554 ? O3 Dy2 O4 117.9(2) 3_667 1_554 ? O10 Dy2 O16W 73.37(16) . . ? O6 Dy2 O16W 70.25(16) . . ? O2 Dy2 O16W 72.48(16) . . ? O1 Dy2 O16W 139.67(18) 3_666 . ? O3 Dy2 O16W 75.85(18) 3_667 . ? O4 Dy2 O16W 138.67(18) 1_554 . ? O10 Dy2 O13 71.32(14) . . ? O6 Dy2 O13 69.03(15) . . ? O2 Dy2 O13 143.90(16) . . ? O1 Dy2 O13 75.30(16) 3_666 . ? O3 Dy2 O13 138.85(16) 3_667 . ? O4 Dy2 O13 77.08(17) 1_554 . ? O16W Dy2 O13 119.71(14) . . ? C1 N1 Cu2 154.5(7) . . ? C1 N1 Cu2B 167.7(7) . 3_768 ? Cu2 N1 Cu2B 36.42(15) . 3_768 ? C2 N2 Cu3 168.1(6) . . ? C3 N3 Cu4 170.7(6) . 4_576 ? C4 N4 Cu1 162.8(6) . . ? C9 N5 C5 116.2(6) . . ? C9 N5 Cu1 121.9(5) . . ? C5 N5 Cu1 120.4(5) . . ? C17 N7 C21 116.1(6) . . ? C17 N7 Cu3 117.9(4) . 1_454 ? C21 N7 Cu3 125.5(4) . 1_454 ? C23 N8 C27 116.8(6) . . ? C23 N8 Cu4 122.5(4) . . ? C27 N8 Cu4 120.7(5) . . ? C33 N9 C29 116.8(6) . . ? C33 N9 Cu5 124.1(5) . . ? C29 N9 Cu5 119.1(5) . . ? C35 N10 C39 116.0(6) . . ? C35 N10 Cu5 124.3(6) . 1_454 ? C39 N10 Cu5 119.6(5) . 1_454 ? C10 O1 Dy2 146.4(5) . 3_666 ? C10 O2 Dy2 143.7(4) . . ? C16 O3 Dy2 154.0(5) . 3_667 ? C16 O4 Dy2 136.4(5) . 1_556 ? C22 O5 Dy1 129.3(4) . . ? C22 O6 Dy2 144.0(4) . . ? C28 O7 Dy1 171.6(5) . 1_556 ? C28 O8 Dy1 157.2(5) . 4_576 ? C34 O9 Dy1 135.9(4) . . ? C34 O10 Dy2 146.5(4) . . ? C40 O11 Dy1 134.3(4) . . ? C41 O13 Dy1 89.3(4) . . ? C41 O13 Dy2 137.7(4) . . ? Dy1 O13 Dy2 127.59(17) . . ? C41 O14 Dy1 94.5(4) . . ? Dy1 O15W H15A 151.4 . . ? Dy1 O15W H15W 100.9 . . ? H15A O15W H15W 107.7 . . ? Dy2 O16W H16A 118.7 . . ? Dy2 O16W H16B 132.0 . . ? H16A O16W H16B 107.7 . . ? O3 C16 O4 125.5(7) . . ? O3 C16 C13B 127.8(9) . . ? O4 C16 C13B 106.7(9) . . ? O3 C16 C13 111.8(6) . . ? O4 C16 C13 122.5(7) . . ? C13B C16 C13 16.2(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.440 _refine_diff_density_min -1.818 _refine_diff_density_rms 0.191 _database_code_depnum_ccdc_archive 'CCDC 964403'