# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Takashi Kajiwara' _publ_contact_author_email kajiwara@cc.nara-wu.ac.jp _publ_author_name 'Takashi Kajiwara' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 889486' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H65 B N5 O12 Tb Zn2' _chemical_formula_weight 1420.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.335(4) _cell_length_b 9.5267(18) _cell_length_c 34.804(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.830(3) _cell_angle_gamma 90.00 _cell_volume 6048(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 16231 _cell_measurement_theta_min 2.4120 _cell_measurement_theta_max 31.8364 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 2.012 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.6659 _exptl_absorpt_correction_T_max 0.7943 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; Absorption correction was performed using REQAB (Rigaku, 1998) program. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74629 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17502 _reflns_number_gt 14633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear ver. 1.4' _computing_cell_refinement 'CrystalClear ver. 1.4' _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics OrtepIII _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0537P)^2^+0.8771P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17502 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Tb Tb 0.324727(8) 0.115440(16) 0.131491(4) 0.02101(5) Uani 1 1 d . . . Zn1 Zn 0.29198(2) 0.24797(4) 0.218116(11) 0.02155(9) Uani 1 1 d . . . Zn2 Zn 0.37004(2) 0.01221(4) 0.044440(12) 0.02442(9) Uani 1 1 d . . . O1 O 0.31468(13) -0.1508(2) 0.14924(7) 0.0250(5) Uani 1 1 d . . . O2 O 0.30227(13) 0.0575(2) 0.19418(7) 0.0231(5) Uani 1 1 d . . . O3 O 0.25469(13) 0.2876(2) 0.16179(7) 0.0242(5) Uani 1 1 d . . . O4 O 0.23007(14) 0.3108(3) 0.08806(7) 0.0306(6) Uani 1 1 d . . . N1 N 0.28197(17) 0.1519(3) 0.26996(8) 0.0273(6) Uani 1 1 d . . . N2 N 0.20718(16) 0.3626(3) 0.23498(9) 0.0280(6) Uani 1 1 d . . . C1 C 0.3131(2) -0.2687(4) 0.12324(11) 0.0303(8) Uani 1 1 d . . . H1 H 0.3569 -0.3264 0.1295 0.046 Uiso 1 1 calc R . . H2 H 0.3120 -0.2347 0.0966 0.046 Uiso 1 1 calc R . . H3 H 0.2692 -0.3252 0.1259 0.046 Uiso 1 1 calc R . . C2 C 0.31713(18) -0.1852(3) 0.18792(10) 0.0226(7) Uani 1 1 d . . . C3 C 0.32771(19) -0.3167(4) 0.20350(11) 0.0268(7) Uani 1 1 d . . . H4 H 0.3341 -0.3949 0.1872 0.032 Uiso 1 1 calc R . . C4 C 0.3291(2) -0.3354(4) 0.24347(11) 0.0294(8) Uani 1 1 d . . . H5 H 0.3382 -0.4257 0.2545 0.035 Uiso 1 1 calc R . . C5 C 0.3172(2) -0.2236(4) 0.26659(11) 0.0281(7) Uani 1 1 d . . . H6 H 0.3164 -0.2382 0.2935 0.034 Uiso 1 1 calc R . . C6 C 0.30624(19) -0.0878(4) 0.25162(10) 0.0238(7) Uani 1 1 d . . . C7 C 0.30832(18) -0.0649(3) 0.21183(10) 0.0226(7) Uani 1 1 d . . . C8 C 0.2860(2) 0.0214(4) 0.27750(10) 0.0285(7) Uani 1 1 d . . . H7 H 0.2746 -0.0071 0.3024 0.034 Uiso 1 1 calc R . . C9 C 0.2524(2) 0.2526(4) 0.29611(11) 0.0354(9) Uani 1 1 d . . . H8 H 0.2911 0.3197 0.3060 0.042 Uiso 1 1 calc R . . H9 H 0.2350 0.2027 0.3184 0.042 Uiso 1 1 calc R . . C10 C 0.1894(2) 0.3306(5) 0.27423(12) 0.0396(9) Uani 1 1 d . . . H10 H 0.1445 0.2725 0.2730 0.048 Uiso 1 1 calc R . . H11 H 0.1800 0.4189 0.2879 0.048 Uiso 1 1 calc R . . C11 C 0.1671(2) 0.4486(4) 0.21403(12) 0.0329(8) Uani 1 1 d . . . H12 H 0.1325 0.5017 0.2265 0.039 Uiso 1 1 calc R . . C12 C 0.20823(18) 0.3869(3) 0.14931(10) 0.0222(7) Uani 1 1 d . . . C13 C 0.16916(18) 0.4726(4) 0.17331(11) 0.0256(7) Uani 1 1 d . . . C14 C 0.1245(2) 0.5814(4) 0.15618(12) 0.0335(8) Uani 1 1 d . . . H13 H 0.0986 0.6399 0.1722 0.040 Uiso 1 1 calc R . . C15 C 0.1175(2) 0.6051(4) 0.11727(12) 0.0346(9) Uani 1 1 d . . . H14 H 0.0887 0.6814 0.1067 0.042 Uiso 1 1 calc R . . C16 C 0.1527(2) 0.5170(4) 0.09330(12) 0.0310(8) Uani 1 1 d . . . H15 H 0.1475 0.5318 0.0662 0.037 Uiso 1 1 calc R . . C17 C 0.19532(18) 0.4079(3) 0.10894(11) 0.0244(7) Uani 1 1 d . . . C18 C 0.2246(2) 0.3318(4) 0.04729(11) 0.0358(9) Uani 1 1 d . . . H16 H 0.1732 0.3245 0.0366 0.054 Uiso 1 1 calc R . . H17 H 0.2536 0.2602 0.0355 0.054 Uiso 1 1 calc R . . H18 H 0.2434 0.4252 0.0417 0.054 Uiso 1 1 calc R . . O5 O 0.18656(13) 0.0426(3) 0.12299(7) 0.0281(5) Uani 1 1 d . . . O6 O 0.27865(12) 0.0203(3) 0.07276(7) 0.0239(5) Uani 1 1 d . . . O7 O 0.41539(12) -0.0135(2) 0.09971(7) 0.0239(5) Uani 1 1 d . . . O8 O 0.45191(13) -0.0135(3) 0.17261(7) 0.0264(5) Uani 1 1 d . . . N3 N 0.30489(18) -0.0562(4) -0.00303(9) 0.0379(8) Uani 1 1 d . . . N4 N 0.43552(17) -0.1406(3) 0.02593(9) 0.0292(7) Uani 1 1 d . . . C19 C 0.1372(2) 0.0463(5) 0.15278(11) 0.0349(9) Uani 1 1 d . . . H19 H 0.1003 0.1196 0.1467 0.052 Uiso 1 1 calc R . . H20 H 0.1649 0.0668 0.1777 0.052 Uiso 1 1 calc R . . H21 H 0.1128 -0.0449 0.1541 0.052 Uiso 1 1 calc R . . C20 C 0.15698(19) 0.0015(4) 0.08675(10) 0.0269(7) Uani 1 1 d . . . C21 C 0.0839(2) -0.0268(5) 0.07648(12) 0.0378(9) Uani 1 1 d . . . H22 H 0.0489 -0.0147 0.0945 0.045 Uiso 1 1 calc R . . C22 C 0.0622(2) -0.0738(6) 0.03894(14) 0.0504(12) Uani 1 1 d . . . H23 H 0.0121 -0.0945 0.0315 0.061 Uiso 1 1 calc R . . C23 C 0.1122(2) -0.0903(5) 0.01298(13) 0.0457(11) Uani 1 1 d . . . H24 H 0.0965 -0.1228 -0.0123 0.055 Uiso 1 1 calc R . . C24 C 0.1868(2) -0.0599(5) 0.02295(11) 0.0344(8) Uani 1 1 d . . . C25 C 0.20992(19) -0.0120(4) 0.06001(11) 0.0276(7) Uani 1 1 d . . . C26 C 0.2375(2) -0.0870(5) -0.00605(12) 0.0402(10) Uani 1 1 d . . . H25 H 0.2180 -0.1317 -0.0292 0.048 Uiso 1 1 calc R . . C27 C 0.3528(3) -0.0952(6) -0.03281(13) 0.0497(12) Uani 1 1 d . . . H26 H 0.3724 -0.0097 -0.0442 0.060 Uiso 1 1 calc R . . H27 H 0.3246 -0.1489 -0.0537 0.060 Uiso 1 1 calc R . . C28 C 0.4145(2) -0.1828(5) -0.01450(12) 0.0445(11) Uani 1 1 d . . . H28 H 0.3996 -0.2827 -0.0152 0.053 Uiso 1 1 calc R . . H29 H 0.4574 -0.1731 -0.0294 0.053 Uiso 1 1 calc R . . C29 C 0.48310(19) -0.2108(4) 0.04677(11) 0.0291(8) Uani 1 1 d . . . H30 H 0.5093 -0.2798 0.0340 0.035 Uiso 1 1 calc R . . C30 C 0.46731(17) -0.1038(3) 0.11201(11) 0.0231(7) Uani 1 1 d . . . C31 C 0.50166(17) -0.1966(4) 0.08797(10) 0.0240(7) Uani 1 1 d . . . C32 C 0.55474(19) -0.2916(4) 0.10519(11) 0.0294(8) Uani 1 1 d . . . H31 H 0.5773 -0.3560 0.0892 0.035 Uiso 1 1 calc R . . C33 C 0.5743(2) -0.2930(4) 0.14402(12) 0.0311(8) Uani 1 1 d . . . H32 H 0.6109 -0.3564 0.1547 0.037 Uiso 1 1 calc R . . C34 C 0.54059(19) -0.2014(4) 0.16823(11) 0.0283(7) Uani 1 1 d . . . H33 H 0.5538 -0.2029 0.1953 0.034 Uiso 1 1 calc R . . C35 C 0.48818(18) -0.1093(3) 0.15235(10) 0.0229(7) Uani 1 1 d . . . C36 C 0.4782(2) 0.0023(4) 0.21251(11) 0.0341(9) Uani 1 1 d . . . H34 H 0.4713 -0.0860 0.2262 0.051 Uiso 1 1 calc R . . H35 H 0.4508 0.0773 0.2239 0.051 Uiso 1 1 calc R . . H36 H 0.5304 0.0263 0.2148 0.051 Uiso 1 1 calc R . . O9 O 0.40859(13) 0.2608(3) 0.16696(7) 0.0294(5) Uani 1 1 d . . . O10 O 0.38652(13) 0.3513(3) 0.22324(7) 0.0263(5) Uani 1 1 d . . . C37 C 0.42256(19) 0.3444(4) 0.19408(10) 0.0245(7) Uani 1 1 d . . . C38 C 0.4862(2) 0.4427(4) 0.19215(12) 0.0368(9) Uani 1 1 d . . . H37 H 0.5319 0.3942 0.2012 0.055 Uiso 1 1 calc R . . H38 H 0.4800 0.5246 0.2085 0.055 Uiso 1 1 calc R . . H39 H 0.4882 0.4734 0.1654 0.055 Uiso 1 1 calc R . . O11 O 0.37636(14) 0.2693(3) 0.08872(7) 0.0314(6) Uani 1 1 d . . . O12 O 0.40830(16) 0.1987(3) 0.03214(8) 0.0351(6) Uani 1 1 d . . . C39 C 0.4066(2) 0.2886(4) 0.05863(11) 0.0284(7) Uani 1 1 d . . . C40 C 0.4446(3) 0.4268(4) 0.05415(14) 0.0454(11) Uani 1 1 d . . . H40 H 0.4289 0.4942 0.0729 0.068 Uiso 1 1 calc R . . H41 H 0.4319 0.4628 0.0280 0.068 Uiso 1 1 calc R . . H42 H 0.4978 0.4134 0.0587 0.068 Uiso 1 1 calc R . . B1 B -0.1467(2) 0.2252(4) 0.13355(12) 0.0234(7) Uani 1 1 d . . . C41 C -0.12078(19) 0.3134(4) 0.17318(10) 0.0259(7) Uani 1 1 d . . . C42 C -0.0764(2) 0.4324(4) 0.17492(12) 0.0401(10) Uani 1 1 d . . . H43 H -0.0589 0.4655 0.1518 0.048 Uiso 1 1 calc R . . C43 C -0.0567(3) 0.5047(5) 0.20909(13) 0.0479(11) Uani 1 1 d . . . H44 H -0.0266 0.5858 0.2088 0.057 Uiso 1 1 calc R . . C44 C -0.0802(2) 0.4604(5) 0.24330(13) 0.0417(10) Uani 1 1 d . . . H45 H -0.0669 0.5102 0.2666 0.050 Uiso 1 1 calc R . . C45 C -0.1238(2) 0.3415(5) 0.24305(12) 0.0377(9) Uani 1 1 d . . . H46 H -0.1404 0.3082 0.2664 0.045 Uiso 1 1 calc R . . C46 C -0.1429(2) 0.2716(4) 0.20884(11) 0.0310(8) Uani 1 1 d . . . H47 H -0.1729 0.1903 0.2094 0.037 Uiso 1 1 calc R . . C47 C -0.10836(18) 0.0683(4) 0.13495(11) 0.0265(7) Uani 1 1 d . . . C48 C -0.1189(2) -0.0188(4) 0.10227(13) 0.0393(9) Uani 1 1 d . . . H48 H -0.1464 0.0164 0.0797 0.047 Uiso 1 1 calc R . . C49 C -0.0910(2) -0.1536(5) 0.10156(15) 0.0451(11) Uani 1 1 d . . . H49 H -0.0991 -0.2090 0.0788 0.054 Uiso 1 1 calc R . . C50 C -0.0510(2) -0.2070(4) 0.13422(14) 0.0426(11) Uani 1 1 d . . . H50 H -0.0331 -0.3005 0.1343 0.051 Uiso 1 1 calc R . . C51 C -0.0377(2) -0.1246(4) 0.16621(14) 0.0390(10) Uani 1 1 d . . . H51 H -0.0095 -0.1602 0.1885 0.047 Uiso 1 1 calc R . . C52 C -0.0652(2) 0.0117(4) 0.16629(12) 0.0318(8) Uani 1 1 d . . . H52 H -0.0540 0.0681 0.1886 0.038 Uiso 1 1 calc R . . C53 C -0.12271(19) 0.3057(4) 0.09520(10) 0.0273(7) Uani 1 1 d . . . C54 C -0.0486(2) 0.3108(5) 0.08857(12) 0.0383(9) Uani 1 1 d . . . H53 H -0.0134 0.2674 0.1067 0.046 Uiso 1 1 calc R . . C55 C -0.0245(2) 0.3763(6) 0.05665(14) 0.0505(12) Uani 1 1 d . . . H54 H 0.0262 0.3764 0.0532 0.061 Uiso 1 1 calc R . . C56 C -0.0739(3) 0.4416(7) 0.02987(14) 0.0631(16) Uani 1 1 d . . . H55 H -0.0578 0.4878 0.0081 0.076 Uiso 1 1 calc R . . C57 C -0.1464(3) 0.4382(6) 0.03549(14) 0.0580(14) Uani 1 1 d . . . H56 H -0.1811 0.4824 0.0173 0.070 Uiso 1 1 calc R . . C58 C -0.1704(2) 0.3718(4) 0.06710(12) 0.0368(9) Uani 1 1 d . . . H57 H -0.2214 0.3711 0.0698 0.044 Uiso 1 1 calc R . . C59 C -0.23662(18) 0.2087(3) 0.13190(9) 0.0224(6) Uani 1 1 d . . . C60 C -0.2728(2) 0.0809(4) 0.13433(11) 0.0274(7) Uani 1 1 d . . . H58 H -0.2445 -0.0026 0.1367 0.033 Uiso 1 1 calc R . . C61 C -0.3489(2) 0.0703(4) 0.13340(11) 0.0319(8) Uani 1 1 d . . . H59 H -0.3709 -0.0191 0.1358 0.038 Uiso 1 1 calc R . . C62 C -0.3923(2) 0.1877(4) 0.12910(11) 0.0304(8) Uani 1 1 d . . . H60 H -0.4442 0.1804 0.1277 0.036 Uiso 1 1 calc R . . C63 C -0.3587(2) 0.3171(4) 0.12685(11) 0.0309(8) Uani 1 1 d . . . H61 H -0.3876 0.3998 0.1240 0.037 Uiso 1 1 calc R . . C64 C -0.2829(2) 0.3264(4) 0.12869(10) 0.0274(7) Uani 1 1 d . . . H62 H -0.2613 0.4168 0.1277 0.033 Uiso 1 1 calc R . . N5 N -0.3433(3) 0.5348(6) 0.03158(16) 0.0808(15) Uani 1 1 d . . . C65 C -0.3118(3) 0.6271(6) 0.04412(18) 0.0617(15) Uani 1 1 d . . . C66 C -0.2676(4) 0.7303(8) 0.0628(2) 0.095(2) Uani 1 1 d . . . H63 H -0.2979 0.7938 0.0767 0.142 Uiso 1 1 calc R . . H64 H -0.2433 0.7837 0.0437 0.142 Uiso 1 1 calc R . . H65 H -0.2306 0.6861 0.0812 0.142 Uiso 1 1 calc 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 Tb 0.02312(9) 0.02195(9) 0.01859(9) -0.00221(6) 0.00528(6) 0.00034(6) Zn1 0.02396(19) 0.02030(18) 0.0212(2) -0.00159(15) 0.00641(16) 0.00193(14) Zn2 0.0259(2) 0.0272(2) 0.0208(2) -0.00192(16) 0.00540(16) 0.00117(15) O1 0.0323(13) 0.0213(11) 0.0216(13) -0.0040(9) 0.0040(10) 0.0044(9) O2 0.0300(12) 0.0190(11) 0.0209(12) -0.0016(9) 0.0056(10) 0.0019(9) O3 0.0273(12) 0.0253(12) 0.0208(12) 0.0014(9) 0.0061(10) 0.0079(9) O4 0.0379(14) 0.0291(13) 0.0253(13) 0.0032(11) 0.0067(11) 0.0113(11) N1 0.0348(16) 0.0279(15) 0.0197(15) 0.0001(12) 0.0052(12) 0.0049(12) N2 0.0282(15) 0.0303(16) 0.0271(16) -0.0043(12) 0.0104(13) 0.0049(12) C1 0.0378(19) 0.0235(17) 0.0298(19) -0.0066(15) 0.0042(16) -0.0027(14) C2 0.0235(15) 0.0231(16) 0.0215(17) 0.0011(13) 0.0032(13) -0.0009(12) C3 0.0314(18) 0.0212(16) 0.0278(19) -0.0015(14) 0.0025(15) 0.0002(13) C4 0.038(2) 0.0217(16) 0.0276(19) 0.0049(14) -0.0003(16) 0.0018(14) C5 0.0321(18) 0.0262(17) 0.0264(18) 0.0045(14) 0.0047(15) -0.0011(14) C6 0.0248(16) 0.0249(16) 0.0221(17) -0.0005(13) 0.0047(13) -0.0009(13) C7 0.0246(16) 0.0217(15) 0.0214(17) 0.0043(13) 0.0023(13) -0.0040(12) C8 0.0343(19) 0.0322(18) 0.0200(17) 0.0012(14) 0.0077(15) -0.0011(15) C9 0.052(2) 0.033(2) 0.0232(19) -0.0037(15) 0.0134(17) 0.0042(17) C10 0.045(2) 0.044(2) 0.033(2) -0.0013(18) 0.0159(19) 0.0087(19) C11 0.0329(19) 0.0289(19) 0.038(2) -0.0042(16) 0.0105(17) 0.0074(15) C12 0.0196(14) 0.0193(15) 0.0280(18) 0.0001(13) 0.0040(13) 0.0017(12) C13 0.0210(15) 0.0245(16) 0.0315(19) -0.0030(14) 0.0044(14) 0.0039(12) C14 0.0314(19) 0.0306(19) 0.039(2) -0.0010(16) 0.0038(17) 0.0117(15) C15 0.0302(19) 0.0302(19) 0.044(2) 0.0041(17) 0.0040(17) 0.0086(15) C16 0.0283(17) 0.0292(18) 0.035(2) 0.0055(16) 0.0006(16) 0.0007(14) C17 0.0209(15) 0.0241(16) 0.0285(19) 0.0015(14) 0.0046(14) -0.0004(12) C18 0.044(2) 0.038(2) 0.025(2) 0.0053(16) 0.0032(17) 0.0135(18) O5 0.0199(11) 0.0410(15) 0.0239(13) 0.0007(11) 0.0047(10) -0.0009(10) O6 0.0193(11) 0.0305(12) 0.0222(12) -0.0032(10) 0.0028(9) -0.0006(9) O7 0.0229(11) 0.0295(12) 0.0195(12) -0.0014(10) 0.0026(9) 0.0047(9) O8 0.0230(11) 0.0336(13) 0.0227(12) -0.0030(10) 0.0022(10) 0.0037(10) N3 0.0308(17) 0.060(2) 0.0228(17) -0.0083(15) 0.0005(13) 0.0070(15) N4 0.0285(15) 0.0320(16) 0.0278(17) -0.0093(13) 0.0061(13) 0.0000(12) C19 0.0278(18) 0.050(2) 0.028(2) -0.0006(18) 0.0122(16) -0.0047(17) C20 0.0244(16) 0.0313(18) 0.0248(18) 0.0026(14) 0.0009(14) 0.0011(14) C21 0.0237(17) 0.057(3) 0.032(2) 0.0026(19) 0.0021(16) -0.0006(17) C22 0.028(2) 0.078(3) 0.043(3) 0.001(2) -0.0080(19) -0.006(2) C23 0.032(2) 0.069(3) 0.034(2) -0.008(2) -0.0066(18) -0.006(2) C24 0.0273(18) 0.049(2) 0.026(2) -0.0029(17) -0.0028(15) -0.0013(16) C25 0.0231(16) 0.0300(18) 0.0285(19) 0.0034(15) -0.0023(14) 0.0003(13) C26 0.035(2) 0.058(3) 0.027(2) -0.0078(19) -0.0040(17) 0.0032(19) C27 0.048(3) 0.070(3) 0.033(2) -0.013(2) 0.007(2) 0.004(2) C28 0.046(2) 0.061(3) 0.026(2) -0.017(2) 0.0032(18) 0.004(2) C29 0.0260(17) 0.0272(17) 0.036(2) -0.0088(15) 0.0106(15) -0.0011(14) C30 0.0178(14) 0.0199(15) 0.0323(19) -0.0009(13) 0.0064(13) -0.0026(11) C31 0.0200(15) 0.0238(16) 0.0287(18) -0.0015(14) 0.0049(13) -0.0026(12) C32 0.0277(17) 0.0246(17) 0.037(2) -0.0049(15) 0.0084(16) 0.0019(14) C33 0.0261(17) 0.0258(17) 0.041(2) 0.0024(16) 0.0013(16) 0.0036(14) C34 0.0257(17) 0.0261(17) 0.033(2) 0.0069(15) 0.0018(15) -0.0027(13) C35 0.0208(15) 0.0207(15) 0.0280(18) -0.0008(13) 0.0058(14) -0.0016(12) C36 0.0293(18) 0.047(2) 0.0254(19) -0.0072(17) -0.0025(15) 0.0057(16) O9 0.0260(12) 0.0328(13) 0.0301(14) -0.0056(11) 0.0069(11) -0.0029(10) O10 0.0278(12) 0.0269(12) 0.0250(13) -0.0044(10) 0.0067(10) -0.0049(10) C37 0.0251(16) 0.0253(16) 0.0239(18) 0.0013(14) 0.0052(14) -0.0001(13) C38 0.040(2) 0.041(2) 0.031(2) -0.0049(17) 0.0090(17) -0.0157(18) O11 0.0383(14) 0.0280(13) 0.0297(14) 0.0007(11) 0.0113(12) 0.0007(11) O12 0.0478(16) 0.0286(13) 0.0305(15) -0.0007(11) 0.0113(12) -0.0047(12) C39 0.0325(18) 0.0231(16) 0.030(2) 0.0008(14) 0.0067(15) -0.0045(14) C40 0.060(3) 0.031(2) 0.047(3) -0.0006(19) 0.020(2) -0.012(2) B1 0.0223(17) 0.0243(18) 0.0237(19) 0.0044(15) 0.0023(15) -0.0003(14) C41 0.0262(16) 0.0248(17) 0.0263(18) 0.0043(14) 0.0009(14) -0.0009(13) C42 0.053(3) 0.034(2) 0.033(2) 0.0038(17) 0.0054(19) -0.0142(19) C43 0.060(3) 0.041(2) 0.043(3) -0.006(2) 0.002(2) -0.020(2) C44 0.048(2) 0.043(2) 0.033(2) -0.0081(19) -0.0007(19) -0.0032(19) C45 0.041(2) 0.046(2) 0.026(2) -0.0013(18) 0.0028(17) -0.0007(18) C46 0.0325(19) 0.0332(19) 0.0276(19) 0.0053(15) 0.0046(15) -0.0015(15) C47 0.0214(15) 0.0264(17) 0.032(2) 0.0035(15) 0.0050(14) 0.0003(13) C48 0.036(2) 0.038(2) 0.044(2) -0.0011(19) 0.0055(19) 0.0035(17) C49 0.036(2) 0.037(2) 0.063(3) -0.012(2) 0.010(2) -0.0025(18) C50 0.032(2) 0.029(2) 0.070(3) 0.005(2) 0.016(2) 0.0065(16) C51 0.032(2) 0.036(2) 0.050(3) 0.0104(19) 0.0072(19) 0.0066(16) C52 0.0270(17) 0.035(2) 0.034(2) 0.0085(16) 0.0041(16) 0.0011(15) C53 0.0267(17) 0.0295(18) 0.0257(18) 0.0039(14) 0.0031(14) -0.0013(14) C54 0.0274(18) 0.056(3) 0.032(2) 0.0089(19) 0.0019(16) -0.0042(17) C55 0.030(2) 0.081(4) 0.042(3) 0.011(2) 0.0090(19) -0.013(2) C56 0.044(3) 0.104(4) 0.042(3) 0.038(3) 0.009(2) -0.014(3) C57 0.044(3) 0.092(4) 0.038(3) 0.036(3) 0.005(2) 0.005(3) C58 0.0293(19) 0.053(3) 0.028(2) 0.0158(18) 0.0045(16) 0.0000(17) C59 0.0259(16) 0.0236(16) 0.0181(16) 0.0003(13) 0.0034(13) -0.0017(13) C60 0.0296(17) 0.0235(16) 0.0298(19) 0.0048(14) 0.0065(15) 0.0002(13) C61 0.0314(19) 0.0334(19) 0.031(2) 0.0029(16) 0.0050(16) -0.0093(15) C62 0.0231(16) 0.040(2) 0.029(2) -0.0025(16) 0.0057(15) -0.0004(15) C63 0.0308(18) 0.034(2) 0.0283(19) -0.0026(16) 0.0070(15) 0.0058(15) C64 0.0326(18) 0.0247(17) 0.0253(18) 0.0002(14) 0.0051(15) -0.0020(14) N5 0.078(4) 0.090(4) 0.074(4) 0.005(3) 0.006(3) 0.007(3) C65 0.061(3) 0.061(3) 0.069(4) -0.016(3) 0.029(3) -0.017(3) C66 0.086(5) 0.088(5) 0.114(6) -0.028(4) 0.030(4) -0.025(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb O6 2.316(2) . ? Tb O2 2.327(2) . ? Tb O9 2.328(2) . ? Tb O11 2.355(3) . ? Tb O3 2.393(2) . ? Tb O7 2.423(2) . ? Tb O5 2.614(2) . ? Tb O1 2.621(2) . ? Tb O4 2.868(2) . ? Tb O8 2.884(2) . ? Tb Zn2 3.3686(7) . ? Tb Zn1 3.3781(7) . ? Zn1 O10 1.986(2) . ? Zn1 O2 2.014(2) . ? Zn1 N2 2.035(3) . ? Zn1 O3 2.045(2) . ? Zn1 N1 2.048(3) . ? Zn2 O12 1.973(3) . ? Zn2 O6 2.030(2) . ? Zn2 O7 2.031(2) . ? Zn2 N4 2.033(3) . ? Zn2 N3 2.045(3) . ? O1 C2 1.382(4) . ? O1 C1 1.441(4) . ? O2 C7 1.317(4) . ? O3 C12 1.317(4) . ? O4 C17 1.373(4) . ? O4 C18 1.426(4) . ? N1 C8 1.272(5) . ? N1 C9 1.464(5) . ? N2 C11 1.278(5) . ? N2 C10 1.468(5) . ? C2 C3 1.371(5) . ? C2 C7 1.435(5) . ? C3 C4 1.400(5) . ? C4 C5 1.365(5) . ? C5 C6 1.402(5) . ? C6 C7 1.406(5) . ? C6 C8 1.449(5) . ? C9 C10 1.512(6) . ? C11 C13 1.440(5) . ? C12 C13 1.414(5) . ? C12 C17 1.415(5) . ? C13 C14 1.414(5) . ? C14 C15 1.366(6) . ? C15 C16 1.389(5) . ? C16 C17 1.378(5) . ? O5 C20 1.378(4) . ? O5 C19 1.445(4) . ? O6 C25 1.329(4) . ? O7 C30 1.321(4) . ? O8 C35 1.366(4) . ? O8 C36 1.431(4) . ? N3 C26 1.264(5) . ? N3 C27 1.473(5) . ? N4 C29 1.267(5) . ? N4 C28 1.476(5) . ? C20 C21 1.378(5) . ? C20 C25 1.417(5) . ? C21 C22 1.400(6) . ? C22 C23 1.359(6) . ? C23 C24 1.407(5) . ? C24 C25 1.393(5) . ? C24 C26 1.463(6) . ? C27 C28 1.495(6) . ? C29 C31 1.446(5) . ? C30 C31 1.409(5) . ? C30 C35 1.418(5) . ? C31 C32 1.417(5) . ? C32 C33 1.362(5) . ? C33 C34 1.399(5) . ? C34 C35 1.375(5) . ? O9 C37 1.241(4) . ? O10 C37 1.268(4) . ? C37 C38 1.503(5) . ? O11 C39 1.247(4) . ? O12 C39 1.261(4) . ? C39 C40 1.506(5) . ? B1 C53 1.638(5) . ? B1 C41 1.644(5) . ? B1 C47 1.651(5) . ? B1 C59 1.652(5) . ? C41 C42 1.392(5) . ? C41 C46 1.402(5) . ? C42 C43 1.390(6) . ? C43 C44 1.373(6) . ? C44 C45 1.386(6) . ? C45 C46 1.378(5) . ? C47 C52 1.390(5) . ? C47 C48 1.405(5) . ? C48 C49 1.384(6) . ? C49 C50 1.385(6) . ? C50 C51 1.364(6) . ? C51 C52 1.393(5) . ? C53 C58 1.394(5) . ? C53 C54 1.402(5) . ? C54 C55 1.385(6) . ? C55 C56 1.380(7) . ? C56 C57 1.364(6) . ? C57 C58 1.379(6) . ? C59 C60 1.393(5) . ? C59 C64 1.404(5) . ? C60 C61 1.395(5) . ? C61 C62 1.372(5) . ? C62 C63 1.383(5) . ? C63 C64 1.388(5) . ? N5 C65 1.116(7) . ? C65 C66 1.393(8) . ? 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 O6 Tb O2 130.63(8) . . ? O6 Tb O9 149.65(8) . . ? O2 Tb O9 79.30(9) . . ? O6 Tb O11 79.62(9) . . ? O2 Tb O11 149.41(9) . . ? O9 Tb O11 71.26(9) . . ? O6 Tb O3 119.56(8) . . ? O2 Tb O3 66.14(8) . . ? O9 Tb O3 73.36(8) . . ? O11 Tb O3 96.90(9) . . ? O6 Tb O7 66.68(8) . . ? O2 Tb O7 120.17(8) . . ? O9 Tb O7 95.57(8) . . ? O11 Tb O7 71.86(8) . . ? O3 Tb O7 166.55(8) . . ? O6 Tb O5 62.21(8) . . ? O2 Tb O5 77.37(8) . . ? O9 Tb O5 142.95(8) . . ? O11 Tb O5 122.74(9) . . ? O3 Tb O5 71.01(8) . . ? O7 Tb O5 121.03(8) . . ? O6 Tb O1 78.54(8) . . ? O2 Tb O1 61.72(8) . . ? O9 Tb O1 120.60(8) . . ? O11 Tb O1 142.52(8) . . ? O3 Tb O1 120.37(8) . . ? O7 Tb O1 71.63(8) . . ? O5 Tb O1 71.29(8) . . ? O6 Tb O4 69.01(8) . . ? O2 Tb O4 119.52(8) . . ? O9 Tb O4 103.01(9) . . ? O11 Tb O4 61.55(8) . . ? O3 Tb O4 57.63(8) . . ? O7 Tb O4 119.66(7) . . ? O5 Tb O4 65.49(8) . . ? O1 Tb O4 134.32(8) . . ? O6 Tb O8 118.38(7) . . ? O2 Tb O8 69.20(7) . . ? O9 Tb O8 62.17(8) . . ? O11 Tb O8 102.84(8) . . ? O3 Tb O8 121.09(7) . . ? O7 Tb O8 56.83(7) . . ? O5 Tb O8 131.94(8) . . ? O1 Tb O8 62.84(7) . . ? O4 Tb O8 162.43(7) . . ? O6 Tb Zn2 36.20(6) . . ? O2 Tb Zn2 148.99(6) . . ? O9 Tb Zn2 116.14(6) . . ? O11 Tb Zn2 57.42(6) . . ? O3 Tb Zn2 142.08(6) . . ? O7 Tb Zn2 36.68(5) . . ? O5 Tb Zn2 98.36(5) . . ? O1 Tb Zn2 87.66(5) . . ? O4 Tb Zn2 84.64(5) . . ? O8 Tb Zn2 93.50(5) . . ? O6 Tb Zn1 148.44(6) . . ? O2 Tb Zn1 35.67(6) . . ? O9 Tb Zn1 58.14(6) . . ? O11 Tb Zn1 116.79(6) . . ? O3 Tb Zn1 36.73(6) . . ? O7 Tb Zn1 142.13(5) . . ? O5 Tb Zn1 86.69(5) . . ? O1 Tb Zn1 97.36(5) . . ? O4 Tb Zn1 94.30(5) . . ? O8 Tb Zn1 85.67(5) . . ? Zn2 Tb Zn1 173.831(11) . . ? O10 Zn1 O2 111.50(10) . . ? O10 Zn1 N2 113.17(11) . . ? O2 Zn1 N2 135.20(11) . . ? O10 Zn1 O3 101.45(10) . . ? O2 Zn1 O3 78.81(9) . . ? N2 Zn1 O3 89.22(11) . . ? O10 Zn1 N1 107.33(12) . . ? O2 Zn1 N1 89.00(11) . . ? N2 Zn1 N1 81.15(12) . . ? O3 Zn1 N1 151.17(11) . . ? O10 Zn1 Tb 91.88(7) . . ? O2 Zn1 Tb 42.38(7) . . ? N2 Zn1 Tb 131.94(9) . . ? O3 Zn1 Tb 44.42(6) . . ? N1 Zn1 Tb 131.25(9) . . ? O12 Zn2 O6 113.61(11) . . ? O12 Zn2 O7 101.18(11) . . ? O6 Zn2 O7 79.83(9) . . ? O12 Zn2 N4 109.98(12) . . ? O6 Zn2 N4 136.40(11) . . ? O7 Zn2 N4 90.89(11) . . ? O12 Zn2 N3 107.63(14) . . ? O6 Zn2 N3 87.78(12) . . ? O7 Zn2 N3 151.18(13) . . ? N4 Zn2 N3 80.28(13) . . ? O12 Zn2 Tb 93.32(8) . . ? O6 Zn2 Tb 42.36(7) . . ? O7 Zn2 Tb 45.43(6) . . ? N4 Zn2 Tb 134.55(9) . . ? N3 Zn2 Tb 129.99(9) . . ? C2 O1 C1 115.0(3) . . ? C2 O1 Tb 117.60(19) . . ? C1 O1 Tb 127.1(2) . . ? C7 O2 Zn1 127.7(2) . . ? C7 O2 Tb 129.2(2) . . ? Zn1 O2 Tb 101.95(10) . . ? C12 O3 Zn1 126.2(2) . . ? C12 O3 Tb 134.8(2) . . ? Zn1 O3 Tb 98.85(9) . . ? C17 O4 C18 116.3(3) . . ? C17 O4 Tb 116.5(2) . . ? C18 O4 Tb 126.4(2) . . ? C8 N1 C9 122.0(3) . . ? C8 N1 Zn1 127.6(3) . . ? C9 N1 Zn1 109.1(2) . . ? C11 N2 C10 119.6(3) . . ? C11 N2 Zn1 126.3(3) . . ? C10 N2 Zn1 113.9(2) . . ? C3 C2 O1 126.3(3) . . ? C3 C2 C7 121.4(3) . . ? O1 C2 C7 112.4(3) . . ? C2 C3 C4 119.8(3) . . ? C5 C4 C3 119.9(3) . . ? C4 C5 C6 121.8(3) . . ? C5 C6 C7 119.5(3) . . ? C5 C6 C8 117.9(3) . . ? C7 C6 C8 122.4(3) . . ? O2 C7 C6 126.0(3) . . ? O2 C7 C2 116.5(3) . . ? C6 C7 C2 117.6(3) . . ? N1 C8 C6 125.9(3) . . ? N1 C9 C10 108.7(3) . . ? N2 C10 C9 109.9(3) . . ? N2 C11 C13 126.3(3) . . ? O3 C12 C13 124.7(3) . . ? O3 C12 C17 117.8(3) . . ? C13 C12 C17 117.5(3) . . ? C12 C13 C14 118.7(3) . . ? C12 C13 C11 123.7(3) . . ? C14 C13 C11 117.3(3) . . ? C15 C14 C13 122.1(4) . . ? C14 C15 C16 119.5(4) . . ? C17 C16 C15 119.9(4) . . ? O4 C17 C16 125.0(3) . . ? O4 C17 C12 113.0(3) . . ? C16 C17 C12 122.0(3) . . ? C20 O5 C19 116.5(3) . . ? C20 O5 Tb 117.75(19) . . ? C19 O5 Tb 125.7(2) . . ? C25 O6 Zn2 129.1(2) . . ? C25 O6 Tb 129.3(2) . . ? Zn2 O6 Tb 101.44(9) . . ? C30 O7 Zn2 126.7(2) . . ? C30 O7 Tb 133.4(2) . . ? Zn2 O7 Tb 97.89(9) . . ? C35 O8 C36 116.0(3) . . ? C35 O8 Tb 116.1(2) . . ? C36 O8 Tb 127.7(2) . . ? C26 N3 C27 122.1(4) . . ? C26 N3 Zn2 128.8(3) . . ? C27 N3 Zn2 107.9(3) . . ? C29 N4 C28 120.0(3) . . ? C29 N4 Zn2 126.2(3) . . ? C28 N4 Zn2 113.0(2) . . ? C21 C20 O5 125.1(3) . . ? C21 C20 C25 121.7(3) . . ? O5 C20 C25 113.2(3) . . ? C20 C21 C22 118.7(4) . . ? C23 C22 C21 120.7(4) . . ? C22 C23 C24 121.1(4) . . ? C25 C24 C23 119.5(4) . . ? C25 C24 C26 122.8(3) . . ? C23 C24 C26 117.6(4) . . ? O6 C25 C24 125.0(3) . . ? O6 C25 C20 116.7(3) . . ? C24 C25 C20 118.3(3) . . ? N3 C26 C24 125.9(4) . . ? N3 C27 C28 108.7(4) . . ? N4 C28 C27 111.6(3) . . ? N4 C29 C31 126.7(3) . . ? O7 C30 C31 124.5(3) . . ? O7 C30 C35 117.3(3) . . ? C31 C30 C35 118.2(3) . . ? C30 C31 C32 118.6(3) . . ? C30 C31 C29 125.0(3) . . ? C32 C31 C29 116.2(3) . . ? C33 C32 C31 121.7(3) . . ? C32 C33 C34 120.3(3) . . ? C35 C34 C33 119.3(4) . . ? O8 C35 C34 125.1(3) . . ? O8 C35 C30 112.9(3) . . ? C34 C35 C30 121.9(3) . . ? C37 O9 Tb 149.2(2) . . ? C37 O10 Zn1 115.1(2) . . ? O9 C37 O10 123.9(3) . . ? O9 C37 C38 117.8(3) . . ? O10 C37 C38 118.3(3) . . ? C39 O11 Tb 149.7(2) . . ? C39 O12 Zn2 114.6(2) . . ? O11 C39 O12 124.1(3) . . ? O11 C39 C40 117.8(3) . . ? O12 C39 C40 118.2(3) . . ? C53 B1 C41 111.4(3) . . ? C53 B1 C47 107.4(3) . . ? C41 B1 C47 110.6(3) . . ? C53 B1 C59 111.5(3) . . ? C41 B1 C59 106.3(3) . . ? C47 B1 C59 109.6(3) . . ? C42 C41 C46 114.4(3) . . ? C42 C41 B1 124.8(3) . . ? C46 C41 B1 120.8(3) . . ? C43 C42 C41 122.7(4) . . ? C44 C43 C42 120.8(4) . . ? C43 C44 C45 118.5(4) . . ? C46 C45 C44 119.8(4) . . ? C45 C46 C41 123.8(4) . . ? C52 C47 C48 115.3(3) . . ? C52 C47 B1 125.5(3) . . ? C48 C47 B1 119.2(3) . . ? C49 C48 C47 122.8(4) . . ? C48 C49 C50 119.5(4) . . ? C51 C50 C49 119.7(4) . . ? C50 C51 C52 120.2(4) . . ? C47 C52 C51 122.5(4) . . ? C58 C53 C54 114.7(3) . . ? C58 C53 B1 125.6(3) . . ? C54 C53 B1 119.7(3) . . ? C55 C54 C53 122.7(4) . . ? C56 C55 C54 120.3(4) . . ? C57 C56 C55 118.3(4) . . ? C56 C57 C58 121.3(4) . . ? C57 C58 C53 122.6(4) . . ? C60 C59 C64 114.5(3) . . ? C60 C59 B1 124.1(3) . . ? C64 C59 B1 121.3(3) . . ? C59 C60 C61 122.9(3) . . ? C62 C61 C60 120.7(4) . . ? C61 C62 C63 118.4(3) . . ? C62 C63 C64 120.3(3) . . ? C63 C64 C59 123.1(3) . . ? N5 C65 C66 172.9(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.997 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.129 # Attachment '- 2.cif' data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 889487' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H65 B Dy N5 O12 Zn2' _chemical_formula_weight 1424.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.372(2) _cell_length_b 9.5395(12) _cell_length_c 34.846(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.9606(18) _cell_angle_gamma 90.00 _cell_volume 6073.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15826 _cell_measurement_theta_min 2.4085 _cell_measurement_theta_max 31.7784 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2892 _exptl_absorpt_coefficient_mu 2.069 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.6258 _exptl_absorpt_correction_T_max 0.9405 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; Absorption correction was performed using REQAB (Rigaku, 1998) program. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72340 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17498 _reflns_number_gt 15052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear ver. 1.4' _computing_cell_refinement 'CrystalClear ver. 1.4' _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics OrtepIII _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0518P)^2^+2.0436P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17498 _refine_ls_number_parameters 790 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Dy Dy 0.324391(7) 0.112425(15) 0.131562(4) 0.02185(5) Uani 1 1 d . . . Zn1 Zn 0.291524(18) 0.24524(4) 0.217785(9) 0.02137(8) Uani 1 1 d . . . Zn2 Zn 0.370507(19) 0.01014(4) 0.044951(10) 0.02537(8) Uani 1 1 d . . . O1 O 0.31480(12) -0.1542(2) 0.14893(6) 0.0245(4) Uani 1 1 d . . . O2 O 0.30178(11) 0.0543(2) 0.19396(6) 0.0226(4) Uani 1 1 d . . . O3 O 0.25474(11) 0.2856(2) 0.16147(6) 0.0240(4) Uani 1 1 d . . . O4 O 0.22917(13) 0.3078(2) 0.08763(6) 0.0318(5) Uani 1 1 d . . . N1 N 0.28109(15) 0.1496(3) 0.26956(7) 0.0283(6) Uani 1 1 d . . . N2 N 0.20674(15) 0.3611(3) 0.23455(8) 0.0292(6) Uani 1 1 d . . . C1 C 0.31360(19) -0.2718(4) 0.12302(9) 0.0320(7) Uani 1 1 d . . . H1 H 0.3586 -0.3266 0.1286 0.048 Uiso 1 1 calc R . . H2 H 0.3102 -0.2380 0.0963 0.048 Uiso 1 1 calc R . . H3 H 0.2712 -0.3310 0.1265 0.048 Uiso 1 1 calc R . . C2 C 0.31719(16) -0.1875(3) 0.18776(8) 0.0228(6) Uani 1 1 d . . . C3 C 0.32770(18) -0.3197(3) 0.20328(9) 0.0290(7) Uani 1 1 d . . . H4 H 0.3342 -0.3977 0.1870 0.035 Uiso 1 1 calc R . . C4 C 0.32869(19) -0.3380(3) 0.24325(9) 0.0312(7) Uani 1 1 d . . . H5 H 0.3379 -0.4282 0.2543 0.037 Uiso 1 1 calc R . . C5 C 0.31650(18) -0.2269(3) 0.26633(9) 0.0298(7) Uani 1 1 d . . . H6 H 0.3152 -0.2418 0.2932 0.036 Uiso 1 1 calc R . . C6 C 0.30571(17) -0.0904(3) 0.25126(9) 0.0248(6) Uani 1 1 d . . . C7 C 0.30799(15) -0.0685(3) 0.21142(8) 0.0219(6) Uani 1 1 d . . . C8 C 0.28518(18) 0.0193(3) 0.27735(9) 0.0281(6) Uani 1 1 d . . . H7 H 0.2739 -0.0090 0.3022 0.034 Uiso 1 1 calc R . . C9 C 0.2515(2) 0.2500(4) 0.29585(9) 0.0369(8) Uani 1 1 d . . . H8 H 0.2901 0.3170 0.3058 0.044 Uiso 1 1 calc R . . H9 H 0.2341 0.1998 0.3180 0.044 Uiso 1 1 calc R . . C10 C 0.1891(2) 0.3274(4) 0.27400(10) 0.0393(8) Uani 1 1 d . . . H10 H 0.1444 0.2690 0.2725 0.047 Uiso 1 1 calc R . . H11 H 0.1794 0.4151 0.2878 0.047 Uiso 1 1 calc R . . C11 C 0.16703(18) 0.4474(4) 0.21359(10) 0.0323(7) Uani 1 1 d . . . H12 H 0.1326 0.5008 0.2260 0.039 Uiso 1 1 calc R . . C12 C 0.20827(16) 0.3850(3) 0.14882(9) 0.0225(6) Uani 1 1 d . . . C13 C 0.16955(17) 0.4712(3) 0.17285(9) 0.0271(6) Uani 1 1 d . . . C14 C 0.12464(19) 0.5801(4) 0.15580(11) 0.0353(8) Uani 1 1 d . . . H13 H 0.0986 0.6381 0.1718 0.042 Uiso 1 1 calc R . . C15 C 0.11782(19) 0.6037(4) 0.11687(11) 0.0359(8) Uani 1 1 d . . . H14 H 0.0894 0.6803 0.1063 0.043 Uiso 1 1 calc R . . C16 C 0.15264(17) 0.5148(3) 0.09279(10) 0.0304(7) Uani 1 1 d . . . H15 H 0.1472 0.5297 0.0657 0.036 Uiso 1 1 calc R . . C17 C 0.19516(16) 0.4051(3) 0.10831(9) 0.0248(6) Uani 1 1 d . . . C18 C 0.2245(2) 0.3288(4) 0.04688(9) 0.0384(8) Uani 1 1 d . . . H16 H 0.1733 0.3232 0.0360 0.058 Uiso 1 1 calc R . . H17 H 0.2530 0.2562 0.0352 0.058 Uiso 1 1 calc R . . H18 H 0.2442 0.4213 0.0414 0.058 Uiso 1 1 calc R . . O5 O 0.18696(11) 0.0399(2) 0.12327(6) 0.0281(5) Uani 1 1 d . . . O6 O 0.27888(11) 0.0176(2) 0.07317(6) 0.0249(4) Uani 1 1 d . . . O7 O 0.41578(11) -0.0154(2) 0.10038(6) 0.0240(4) Uani 1 1 d . . . O8 O 0.45211(12) -0.0174(2) 0.17315(6) 0.0286(5) Uani 1 1 d . . . N3 N 0.30544(16) -0.0578(4) -0.00279(8) 0.0385(7) Uani 1 1 d . . . N4 N 0.43626(15) -0.1425(3) 0.02647(8) 0.0309(6) Uani 1 1 d . . . C19 C 0.13740(19) 0.0437(4) 0.15261(10) 0.0385(8) Uani 1 1 d . . . H19 H 0.1004 0.1164 0.1463 0.058 Uiso 1 1 calc R . . H20 H 0.1647 0.0650 0.1776 0.058 Uiso 1 1 calc R . . H21 H 0.1133 -0.0476 0.1540 0.058 Uiso 1 1 calc R . . C20 C 0.15736(17) -0.0009(4) 0.08713(9) 0.0287(7) Uani 1 1 d . . . C21 C 0.08435(18) -0.0284(4) 0.07638(10) 0.0382(8) Uani 1 1 d . . . H22 H 0.0493 -0.0160 0.0943 0.046 Uiso 1 1 calc R . . C22 C 0.0625(2) -0.0747(5) 0.03885(12) 0.0499(11) Uani 1 1 d . . . H23 H 0.0124 -0.0941 0.0313 0.060 Uiso 1 1 calc R . . C23 C 0.1125(2) -0.0922(5) 0.01302(11) 0.0472(10) Uani 1 1 d . . . H24 H 0.0967 -0.1254 -0.0122 0.057 Uiso 1 1 calc R . . C24 C 0.18776(18) -0.0619(4) 0.02299(9) 0.0351(8) Uani 1 1 d . . . C25 C 0.21020(17) -0.0141(3) 0.06046(9) 0.0269(6) Uani 1 1 d . . . C26 C 0.2379(2) -0.0889(4) -0.00609(10) 0.0397(9) Uani 1 1 d . . . H25 H 0.2184 -0.1333 -0.0293 0.048 Uiso 1 1 calc R . . C27 C 0.3534(2) -0.0977(5) -0.03230(11) 0.0508(11) Uani 1 1 d . . . H26 H 0.3728 -0.0125 -0.0439 0.061 Uiso 1 1 calc R . . H27 H 0.3253 -0.1519 -0.0531 0.061 Uiso 1 1 calc R . . C28 C 0.4152(2) -0.1844(5) -0.01401(10) 0.0461(10) Uani 1 1 d . . . H28 H 0.4007 -0.2844 -0.0148 0.055 Uiso 1 1 calc R . . H29 H 0.4580 -0.1741 -0.0289 0.055 Uiso 1 1 calc R . . C29 C 0.48376(17) -0.2139(4) 0.04721(10) 0.0302(7) Uani 1 1 d . . . H30 H 0.5096 -0.2833 0.0345 0.036 Uiso 1 1 calc R . . C30 C 0.46752(16) -0.1064(3) 0.11248(9) 0.0234(6) Uani 1 1 d . . . C31 C 0.50209(16) -0.1988(3) 0.08869(9) 0.0256(6) Uani 1 1 d . . . C32 C 0.55589(18) -0.2932(3) 0.10578(10) 0.0322(7) Uani 1 1 d . . . H31 H 0.5793 -0.3556 0.0897 0.039 Uiso 1 1 calc R . . C33 C 0.57471(18) -0.2964(3) 0.14461(10) 0.0318(7) Uani 1 1 d . . . H32 H 0.6107 -0.3608 0.1553 0.038 Uiso 1 1 calc R . . C34 C 0.54101(17) -0.2046(3) 0.16876(10) 0.0291(7) Uani 1 1 d . . . H33 H 0.5542 -0.2063 0.1958 0.035 Uiso 1 1 calc R . . C35 C 0.48882(16) -0.1124(3) 0.15301(9) 0.0238(6) Uani 1 1 d . . . C36 C 0.47750(19) -0.0021(4) 0.21304(9) 0.0358(8) Uani 1 1 d . . . H34 H 0.4729 -0.0919 0.2263 0.054 Uiso 1 1 calc R . . H35 H 0.4481 0.0690 0.2246 0.054 Uiso 1 1 calc R . . H36 H 0.5289 0.0270 0.2156 0.054 Uiso 1 1 calc R . . O9 O 0.40857(12) 0.2556(2) 0.16675(6) 0.0305(5) Uani 1 1 d . . . O10 O 0.38631(12) 0.3480(2) 0.22272(6) 0.0272(5) Uani 1 1 d . . . C37 C 0.42271(16) 0.3399(3) 0.19350(9) 0.0246(6) Uani 1 1 d . . . C38 C 0.4863(2) 0.4377(4) 0.19125(11) 0.0392(8) Uani 1 1 d . . . H37 H 0.5316 0.3909 0.2016 0.059 Uiso 1 1 calc R . . H38 H 0.4791 0.5222 0.2064 0.059 Uiso 1 1 calc R . . H39 H 0.4896 0.4637 0.1643 0.059 Uiso 1 1 calc R . . O11 O 0.37543(13) 0.2672(2) 0.08909(6) 0.0328(5) Uani 1 1 d . . . O12 O 0.40819(14) 0.1971(3) 0.03263(7) 0.0354(5) Uani 1 1 d . . . C39 C 0.40646(18) 0.2869(4) 0.05948(9) 0.0307(7) Uani 1 1 d . . . C40 C 0.4440(3) 0.4257(4) 0.05496(13) 0.0483(10) Uani 1 1 d . . . H40 H 0.4245 0.4954 0.0718 0.072 Uiso 1 1 calc R . . H41 H 0.4351 0.4569 0.0281 0.072 Uiso 1 1 calc R . . H42 H 0.4967 0.4151 0.0620 0.072 Uiso 1 1 calc R . . B1 B -0.14632(18) 0.2231(4) 0.13341(10) 0.0240(7) Uani 1 1 d . . . C41 C -0.12018(16) 0.3108(3) 0.17325(8) 0.0254(6) Uani 1 1 d . . . C42 C -0.0752(2) 0.4295(4) 0.17519(11) 0.0408(9) Uani 1 1 d . . . H43 H -0.0575 0.4623 0.1521 0.049 Uiso 1 1 calc R . . C43 C -0.0555(2) 0.5012(4) 0.20913(12) 0.0472(10) Uani 1 1 d . . . H44 H -0.0253 0.5819 0.2088 0.057 Uiso 1 1 calc R . . C44 C -0.0792(2) 0.4568(4) 0.24349(11) 0.0433(9) Uani 1 1 d . . . H45 H -0.0657 0.5062 0.2668 0.052 Uiso 1 1 calc R . . C45 C -0.1232(2) 0.3388(4) 0.24307(10) 0.0389(8) Uani 1 1 d . . . H46 H -0.1400 0.3058 0.2663 0.047 Uiso 1 1 calc R . . C46 C -0.14263(18) 0.2686(4) 0.20869(9) 0.0317(7) Uani 1 1 d . . . H47 H -0.1727 0.1878 0.2092 0.038 Uiso 1 1 calc R . . C47 C -0.10832(17) 0.0668(3) 0.13429(9) 0.0279(6) Uani 1 1 d . . . C48 C -0.1185(2) -0.0202(4) 0.10150(11) 0.0386(8) Uani 1 1 d . . . H48 H -0.1455 0.0155 0.0789 0.046 Uiso 1 1 calc R . . C49 C -0.0910(2) -0.1558(4) 0.10067(13) 0.0460(9) Uani 1 1 d . . . H49 H -0.0993 -0.2108 0.0779 0.055 Uiso 1 1 calc R . . C50 C -0.0511(2) -0.2104(4) 0.13342(13) 0.0439(9) Uani 1 1 d . . . H50 H -0.0330 -0.3037 0.1334 0.053 Uiso 1 1 calc R . . C51 C -0.0384(2) -0.1282(4) 0.16558(12) 0.0417(9) Uani 1 1 d . . . H51 H -0.0106 -0.1643 0.1879 0.050 Uiso 1 1 calc R . . C52 C -0.06578(17) 0.0082(4) 0.16596(10) 0.0324(7) Uani 1 1 d . . . H52 H -0.0552 0.0634 0.1885 0.039 Uiso 1 1 calc R . . C53 C -0.12238(17) 0.3046(3) 0.09508(9) 0.0274(6) Uani 1 1 d . . . C54 C -0.04844(19) 0.3082(4) 0.08824(10) 0.0384(8) Uani 1 1 d . . . H53 H -0.0134 0.2627 0.1060 0.046 Uiso 1 1 calc R . . C55 C -0.0245(2) 0.3756(5) 0.05652(12) 0.0535(12) Uani 1 1 d . . . H54 H 0.0261 0.3752 0.0529 0.064 Uiso 1 1 calc R . . C56 C -0.0736(2) 0.4430(6) 0.03030(12) 0.0634(14) Uani 1 1 d . . . H55 H -0.0573 0.4911 0.0089 0.076 Uiso 1 1 calc R . . C57 C -0.1467(2) 0.4394(6) 0.03555(12) 0.0620(14) Uani 1 1 d . . . H56 H -0.1815 0.4830 0.0173 0.074 Uiso 1 1 calc R . . C58 C -0.16972(19) 0.3722(4) 0.06746(10) 0.0368(8) Uani 1 1 d . . . H57 H -0.2205 0.3726 0.0706 0.044 Uiso 1 1 calc R . . C59 C -0.23615(16) 0.2071(3) 0.13162(8) 0.0228(6) Uani 1 1 d . . . C60 C -0.27273(18) 0.0784(3) 0.13406(9) 0.0282(6) Uani 1 1 d . . . H58 H -0.2444 -0.0051 0.1364 0.034 Uiso 1 1 calc R . . C61 C -0.34823(18) 0.0673(4) 0.13327(10) 0.0326(7) Uani 1 1 d . . . H59 H -0.3700 -0.0222 0.1356 0.039 Uiso 1 1 calc R . . C62 C -0.39206(18) 0.1856(4) 0.12917(9) 0.0315(7) Uani 1 1 d . . . H60 H -0.4438 0.1782 0.1279 0.038 Uiso 1 1 calc R . . C63 C -0.35831(18) 0.3158(4) 0.12702(9) 0.0308(7) Uani 1 1 d . . . H61 H -0.3871 0.3987 0.1244 0.037 Uiso 1 1 calc R . . C64 C -0.28248(17) 0.3245(3) 0.12875(8) 0.0255(6) Uani 1 1 d . . . H62 H -0.2609 0.4147 0.1279 0.031 Uiso 1 1 calc R . . N5 N -0.3435(3) 0.5372(6) 0.03109(14) 0.0817(14) Uani 1 1 d . . . C65 C -0.3125(3) 0.6281(5) 0.04434(16) 0.0608(13) Uani 1 1 d . . . C66 C -0.2684(4) 0.7311(7) 0.0636(2) 0.098(2) Uani 1 1 d . . . H63 H -0.2994 0.8026 0.0738 0.147 Uiso 1 1 d . . . H64 H -0.2376 0.7746 0.0455 0.147 Uiso 1 1 d . . . H65 H -0.2371 0.6880 0.0849 0.147 Uiso 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 Dy 0.02436(8) 0.02357(8) 0.01825(7) -0.00216(5) 0.00518(5) 0.00034(5) Zn1 0.02381(17) 0.02092(17) 0.02011(16) -0.00112(12) 0.00577(12) 0.00222(13) Zn2 0.02637(18) 0.0298(2) 0.02054(16) -0.00232(14) 0.00524(13) 0.00123(14) O1 0.0309(11) 0.0219(10) 0.0205(10) -0.0041(8) 0.0025(8) 0.0014(9) O2 0.0290(11) 0.0179(10) 0.0216(10) -0.0007(8) 0.0061(8) 0.0021(8) O3 0.0254(10) 0.0246(11) 0.0225(10) 0.0020(8) 0.0049(8) 0.0059(9) O4 0.0404(13) 0.0322(13) 0.0235(11) 0.0048(9) 0.0070(9) 0.0108(10) N1 0.0367(15) 0.0250(13) 0.0237(12) -0.0021(10) 0.0068(11) 0.0023(11) N2 0.0304(14) 0.0335(15) 0.0254(13) -0.0016(11) 0.0104(11) 0.0055(12) C1 0.0409(18) 0.0299(18) 0.0258(15) -0.0133(13) 0.0063(13) -0.0059(14) C2 0.0234(14) 0.0223(15) 0.0227(13) -0.0016(11) 0.0017(11) 0.0009(11) C3 0.0324(16) 0.0236(16) 0.0308(16) -0.0024(12) 0.0026(13) -0.0005(13) C4 0.0382(18) 0.0227(16) 0.0320(17) 0.0038(13) 0.0012(13) 0.0017(14) C5 0.0343(17) 0.0299(17) 0.0245(15) 0.0038(13) 0.0000(12) -0.0019(14) C6 0.0261(15) 0.0238(15) 0.0248(14) -0.0008(12) 0.0037(11) 0.0003(12) C7 0.0204(13) 0.0211(14) 0.0234(13) 0.0044(11) -0.0006(10) -0.0035(11) C8 0.0335(16) 0.0302(17) 0.0212(14) 0.0014(12) 0.0048(12) 0.0002(13) C9 0.051(2) 0.037(2) 0.0241(15) -0.0041(14) 0.0105(14) 0.0048(16) C10 0.043(2) 0.045(2) 0.0320(17) -0.0008(16) 0.0161(15) 0.0100(17) C11 0.0301(16) 0.0321(18) 0.0358(17) -0.0049(14) 0.0075(13) 0.0088(14) C12 0.0207(13) 0.0190(14) 0.0278(15) 0.0023(11) 0.0025(11) 0.0007(11) C13 0.0240(14) 0.0268(16) 0.0306(16) -0.0008(13) 0.0036(12) 0.0036(12) C14 0.0310(17) 0.0342(19) 0.0410(19) 0.0008(15) 0.0049(14) 0.0107(14) C15 0.0288(17) 0.0323(19) 0.045(2) 0.0068(15) -0.0013(14) 0.0082(14) C16 0.0246(15) 0.0305(17) 0.0352(17) 0.0051(14) -0.0015(12) -0.0010(13) C17 0.0215(14) 0.0248(16) 0.0283(15) 0.0018(12) 0.0034(11) 0.0003(11) C18 0.048(2) 0.043(2) 0.0249(16) 0.0064(15) 0.0055(14) 0.0128(17) O5 0.0234(10) 0.0369(13) 0.0247(11) -0.0005(9) 0.0057(8) -0.0010(9) O6 0.0199(10) 0.0322(12) 0.0224(10) -0.0023(9) 0.0012(8) -0.0008(9) O7 0.0224(10) 0.0295(11) 0.0202(10) -0.0015(8) 0.0019(8) 0.0046(9) O8 0.0264(11) 0.0363(13) 0.0230(10) -0.0034(9) 0.0023(8) 0.0052(9) N3 0.0308(15) 0.060(2) 0.0242(14) -0.0068(14) 0.0011(11) 0.0066(14) N4 0.0297(14) 0.0368(16) 0.0266(13) -0.0095(12) 0.0049(11) 0.0014(12) C19 0.0283(17) 0.057(2) 0.0320(17) 0.0007(17) 0.0114(13) -0.0054(16) C20 0.0240(15) 0.0357(18) 0.0262(15) 0.0027(13) 0.0018(11) 0.0004(13) C21 0.0225(15) 0.057(2) 0.0351(18) 0.0072(17) 0.0005(13) 0.0004(16) C22 0.0234(17) 0.082(3) 0.043(2) 0.002(2) -0.0064(15) -0.0076(19) C23 0.0309(19) 0.075(3) 0.0326(19) -0.0047(19) -0.0093(15) -0.0058(19) C24 0.0279(16) 0.051(2) 0.0250(16) -0.0006(15) -0.0050(12) 0.0002(15) C25 0.0232(14) 0.0329(17) 0.0241(14) 0.0028(12) 0.0004(11) 0.0017(13) C26 0.0372(19) 0.058(2) 0.0225(15) -0.0067(15) -0.0050(13) 0.0057(17) C27 0.041(2) 0.084(3) 0.0268(18) -0.0126(19) 0.0046(15) 0.003(2) C28 0.046(2) 0.064(3) 0.0286(17) -0.0180(18) 0.0056(15) 0.010(2) C29 0.0260(15) 0.0302(17) 0.0356(17) -0.0078(14) 0.0082(13) 0.0010(13) C30 0.0195(13) 0.0240(15) 0.0270(14) -0.0026(11) 0.0042(11) -0.0018(11) C31 0.0199(13) 0.0262(15) 0.0316(15) -0.0026(13) 0.0064(11) -0.0030(12) C32 0.0279(16) 0.0238(16) 0.0456(19) -0.0036(14) 0.0076(14) 0.0018(13) C33 0.0252(15) 0.0253(16) 0.0443(19) 0.0036(14) -0.0001(13) 0.0033(13) C34 0.0241(15) 0.0286(17) 0.0344(16) 0.0068(13) 0.0022(12) -0.0022(13) C35 0.0184(13) 0.0258(15) 0.0277(15) -0.0002(12) 0.0052(11) -0.0009(11) C36 0.0344(18) 0.047(2) 0.0251(16) -0.0035(15) -0.0021(13) 0.0046(16) O9 0.0273(11) 0.0345(13) 0.0305(12) -0.0072(10) 0.0072(9) -0.0032(10) O10 0.0262(11) 0.0285(11) 0.0275(11) -0.0033(9) 0.0059(8) -0.0034(9) C37 0.0234(14) 0.0240(15) 0.0268(14) 0.0001(12) 0.0046(11) 0.0020(12) C38 0.041(2) 0.042(2) 0.0355(18) -0.0067(16) 0.0105(15) -0.0160(17) O11 0.0387(13) 0.0331(13) 0.0282(11) 0.0025(10) 0.0110(10) 0.0007(10) O12 0.0484(15) 0.0321(13) 0.0278(12) -0.0016(10) 0.0131(10) -0.0055(11) C39 0.0328(17) 0.0334(18) 0.0266(15) 0.0019(13) 0.0062(12) 0.0016(14) C40 0.059(3) 0.039(2) 0.050(2) -0.0035(18) 0.020(2) -0.0144(19) B1 0.0224(15) 0.0278(18) 0.0220(15) 0.0025(13) 0.0023(12) -0.0027(13) C41 0.0228(14) 0.0294(16) 0.0233(14) 0.0040(12) -0.0006(11) -0.0001(12) C42 0.052(2) 0.041(2) 0.0307(18) 0.0005(15) 0.0082(16) -0.0157(18) C43 0.058(3) 0.043(2) 0.041(2) -0.0062(17) 0.0052(18) -0.0207(19) C44 0.044(2) 0.050(2) 0.0340(19) -0.0104(17) -0.0053(16) -0.0033(18) C45 0.042(2) 0.047(2) 0.0279(17) 0.0016(15) 0.0032(14) 0.0027(17) C46 0.0330(17) 0.0332(18) 0.0293(16) 0.0034(13) 0.0049(13) -0.0047(14) C47 0.0234(14) 0.0284(16) 0.0327(16) 0.0056(13) 0.0067(12) -0.0020(12) C48 0.0336(18) 0.038(2) 0.045(2) -0.0013(16) 0.0043(15) 0.0062(15) C49 0.037(2) 0.040(2) 0.061(3) -0.0110(19) 0.0098(18) -0.0003(17) C50 0.0332(19) 0.0303(19) 0.070(3) 0.0082(19) 0.0155(18) 0.0083(15) C51 0.0314(18) 0.040(2) 0.054(2) 0.0178(18) 0.0071(16) 0.0079(15) C52 0.0242(15) 0.0353(19) 0.0378(18) 0.0091(14) 0.0039(13) 0.0006(13) C53 0.0265(15) 0.0310(17) 0.0246(14) 0.0019(12) 0.0024(11) -0.0039(13) C54 0.0269(16) 0.056(2) 0.0316(17) 0.0115(16) 0.0013(13) -0.0038(16) C55 0.0303(19) 0.088(4) 0.042(2) 0.016(2) 0.0051(16) -0.015(2) C56 0.047(2) 0.103(4) 0.042(2) 0.036(3) 0.0110(18) -0.015(3) C57 0.045(2) 0.101(4) 0.040(2) 0.041(2) 0.0089(18) 0.008(2) C58 0.0287(17) 0.057(2) 0.0248(16) 0.0128(15) 0.0030(13) -0.0021(16) C59 0.0266(14) 0.0249(15) 0.0172(12) 0.0016(11) 0.0027(10) 0.0013(12) C60 0.0286(16) 0.0247(16) 0.0320(16) 0.0048(13) 0.0059(12) 0.0012(13) C61 0.0322(17) 0.0329(18) 0.0334(17) 0.0013(14) 0.0061(13) -0.0079(14) C62 0.0254(15) 0.041(2) 0.0294(16) -0.0020(14) 0.0060(12) -0.0020(14) C63 0.0312(16) 0.0344(18) 0.0276(15) -0.0006(13) 0.0072(12) 0.0059(14) C64 0.0302(15) 0.0231(15) 0.0234(14) 0.0003(12) 0.0036(11) -0.0026(12) N5 0.082(3) 0.087(4) 0.074(3) 0.000(3) 0.003(3) 0.008(3) C65 0.059(3) 0.062(3) 0.066(3) -0.019(2) 0.028(2) -0.016(2) C66 0.082(4) 0.091(5) 0.124(6) -0.023(4) 0.027(4) -0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy O6 2.303(2) . ? Dy O9 2.317(2) . ? Dy O2 2.323(2) . ? Dy O11 2.354(2) . ? Dy O3 2.393(2) . ? Dy O7 2.422(2) . ? Dy O5 2.605(2) . ? Dy O1 2.624(2) . ? Dy O4 2.885(2) . ? Dy O8 2.904(2) . ? Dy Zn2 3.3629(5) . ? Dy Zn1 3.3725(5) . ? Zn1 O10 1.990(2) . ? Zn1 O2 2.018(2) . ? Zn1 N2 2.044(3) . ? Zn1 O3 2.045(2) . ? Zn1 N1 2.048(3) . ? Zn2 O12 1.976(2) . ? Zn2 O7 2.037(2) . ? Zn2 O6 2.037(2) . ? Zn2 N4 2.038(3) . ? Zn2 N3 2.050(3) . ? O1 C2 1.386(3) . ? O1 C1 1.439(4) . ? O2 C7 1.320(3) . ? O3 C12 1.321(3) . ? O4 C17 1.366(4) . ? O4 C18 1.428(4) . ? N1 C8 1.273(4) . ? N1 C9 1.468(4) . ? N2 C11 1.278(4) . ? N2 C10 1.480(4) . ? C2 C3 1.378(4) . ? C2 C7 1.423(4) . ? C3 C4 1.402(4) . ? C4 C5 1.363(5) . ? C5 C6 1.410(4) . ? C6 C7 1.409(4) . ? C6 C8 1.461(4) . ? C9 C10 1.503(5) . ? C11 C13 1.443(5) . ? C12 C13 1.417(4) . ? C12 C17 1.420(4) . ? C13 C14 1.418(5) . ? C14 C15 1.368(5) . ? C15 C16 1.394(5) . ? C16 C17 1.382(4) . ? O5 C20 1.375(4) . ? O5 C19 1.439(4) . ? O6 C25 1.328(4) . ? O7 C30 1.323(4) . ? O8 C35 1.366(4) . ? O8 C36 1.427(4) . ? N3 C26 1.270(5) . ? N3 C27 1.472(5) . ? N4 C29 1.272(4) . ? N4 C28 1.478(4) . ? C20 C21 1.380(4) . ? C20 C25 1.417(4) . ? C21 C22 1.399(5) . ? C22 C23 1.361(6) . ? C23 C24 1.420(5) . ? C24 C25 1.404(4) . ? C24 C26 1.461(5) . ? C27 C28 1.493(6) . ? C29 C31 1.457(4) . ? C30 C31 1.406(4) . ? C30 C35 1.427(4) . ? C31 C32 1.422(4) . ? C32 C33 1.361(5) . ? C33 C34 1.402(5) . ? C34 C35 1.373(4) . ? O9 C37 1.238(4) . ? O10 C37 1.277(4) . ? C37 C38 1.504(5) . ? O11 C39 1.244(4) . ? O12 C39 1.272(4) . ? C39 C40 1.508(5) . ? B1 C53 1.644(5) . ? B1 C47 1.646(5) . ? B1 C41 1.649(5) . ? B1 C59 1.652(4) . ? C41 C42 1.399(5) . ? C41 C46 1.401(4) . ? C42 C43 1.382(5) . ? C43 C44 1.383(6) . ? C44 C45 1.385(6) . ? C45 C46 1.386(5) . ? C47 C52 1.401(4) . ? C47 C48 1.409(5) . ? C48 C49 1.390(5) . ? C49 C50 1.392(6) . ? C50 C51 1.368(6) . ? C51 C52 1.395(5) . ? C53 C58 1.388(4) . ? C53 C54 1.404(5) . ? C54 C55 1.389(5) . ? C55 C56 1.375(6) . ? C56 C57 1.373(6) . ? C57 C58 1.387(5) . ? C59 C64 1.404(4) . ? C59 C60 1.407(4) . ? C60 C61 1.388(4) . ? C61 C62 1.386(5) . ? C62 C63 1.394(5) . ? C63 C64 1.390(4) . ? N5 C65 1.112(6) . ? C65 C66 1.399(8) . ? 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 O6 Dy O9 149.35(8) . . ? O6 Dy O2 130.51(7) . . ? O9 Dy O2 79.62(8) . . ? O6 Dy O11 79.78(8) . . ? O9 Dy O11 71.04(8) . . ? O2 Dy O11 149.32(8) . . ? O6 Dy O3 119.62(7) . . ? O9 Dy O3 73.76(7) . . ? O2 Dy O3 66.50(7) . . ? O11 Dy O3 96.12(8) . . ? O6 Dy O7 67.10(7) . . ? O9 Dy O7 94.50(7) . . ? O2 Dy O7 119.97(7) . . ? O11 Dy O7 72.17(8) . . ? O3 Dy O7 165.86(7) . . ? O6 Dy O5 62.54(7) . . ? O9 Dy O5 143.26(7) . . ? O2 Dy O5 77.00(7) . . ? O11 Dy O5 122.80(8) . . ? O3 Dy O5 71.07(7) . . ? O7 Dy O5 121.72(7) . . ? O6 Dy O1 78.24(7) . . ? O9 Dy O1 120.43(7) . . ? O2 Dy O1 61.98(7) . . ? O11 Dy O1 142.54(7) . . ? O3 Dy O1 121.11(7) . . ? O7 Dy O1 71.44(7) . . ? O5 Dy O1 71.38(7) . . ? O6 Dy O4 68.92(7) . . ? O9 Dy O4 103.57(8) . . ? O2 Dy O4 119.56(7) . . ? O11 Dy O4 61.32(7) . . ? O3 Dy O4 57.53(7) . . ? O7 Dy O4 119.85(6) . . ? O5 Dy O4 65.49(7) . . ? O1 Dy O4 134.18(7) . . ? O6 Dy O8 118.28(7) . . ? O9 Dy O8 61.77(7) . . ? O2 Dy O8 69.20(7) . . ? O11 Dy O8 103.15(7) . . ? O3 Dy O8 121.19(6) . . ? O7 Dy O8 56.44(6) . . ? O5 Dy O8 131.74(7) . . ? O1 Dy O8 62.72(7) . . ? O4 Dy O8 162.64(7) . . ? O6 Dy Zn2 36.42(5) . . ? O9 Dy Zn2 115.43(5) . . ? O2 Dy Zn2 148.99(5) . . ? O11 Dy Zn2 57.57(6) . . ? O3 Dy Zn2 141.90(5) . . ? O7 Dy Zn2 36.90(5) . . ? O5 Dy Zn2 98.92(5) . . ? O1 Dy Zn2 87.42(4) . . ? O4 Dy Zn2 84.64(4) . . ? O8 Dy Zn2 93.34(4) . . ? O6 Dy Zn1 148.48(5) . . ? O9 Dy Zn1 58.57(5) . . ? O2 Dy Zn1 35.87(5) . . ? O11 Dy Zn1 116.38(6) . . ? O3 Dy Zn1 36.83(5) . . ? O7 Dy Zn1 141.76(5) . . ? O5 Dy Zn1 86.41(5) . . ? O1 Dy Zn1 97.82(4) . . ? O4 Dy Zn1 94.32(5) . . ? O8 Dy Zn1 85.74(4) . . ? Zn2 Dy Zn1 173.522(10) . . ? O10 Zn1 O2 111.21(9) . . ? O10 Zn1 N2 113.26(10) . . ? O2 Zn1 N2 135.39(10) . . ? O10 Zn1 O3 100.91(9) . . ? O2 Zn1 O3 79.08(8) . . ? N2 Zn1 O3 89.24(10) . . ? O10 Zn1 N1 107.72(10) . . ? O2 Zn1 N1 88.95(9) . . ? N2 Zn1 N1 81.10(11) . . ? O3 Zn1 N1 151.33(10) . . ? O10 Zn1 Dy 91.49(6) . . ? O2 Zn1 Dy 42.40(6) . . ? N2 Zn1 Dy 132.07(8) . . ? O3 Zn1 Dy 44.56(6) . . ? N1 Zn1 Dy 131.23(8) . . ? O12 Zn2 O7 101.32(9) . . ? O12 Zn2 O6 113.51(10) . . ? O7 Zn2 O6 79.80(8) . . ? O12 Zn2 N4 110.08(11) . . ? O7 Zn2 N4 90.99(10) . . ? O6 Zn2 N4 136.39(10) . . ? O12 Zn2 N3 107.28(12) . . ? O7 Zn2 N3 151.39(12) . . ? O6 Zn2 N3 87.79(10) . . ? N4 Zn2 N3 80.35(12) . . ? O12 Zn2 Dy 93.42(7) . . ? O7 Zn2 Dy 45.55(6) . . ? O6 Zn2 Dy 42.16(6) . . ? N4 Zn2 Dy 134.72(8) . . ? N3 Zn2 Dy 129.79(8) . . ? C2 O1 C1 115.5(2) . . ? C2 O1 Dy 116.80(17) . . ? C1 O1 Dy 127.46(19) . . ? C7 O2 Zn1 128.21(18) . . ? C7 O2 Dy 128.91(18) . . ? Zn1 O2 Dy 101.73(8) . . ? C12 O3 Zn1 126.37(19) . . ? C12 O3 Dy 134.96(18) . . ? Zn1 O3 Dy 98.61(8) . . ? C17 O4 C18 116.5(2) . . ? C17 O4 Dy 116.39(18) . . ? C18 O4 Dy 126.05(19) . . ? C8 N1 C9 121.4(3) . . ? C8 N1 Zn1 127.9(2) . . ? C9 N1 Zn1 109.5(2) . . ? C11 N2 C10 120.3(3) . . ? C11 N2 Zn1 126.3(2) . . ? C10 N2 Zn1 113.3(2) . . ? C3 C2 O1 125.6(3) . . ? C3 C2 C7 121.5(3) . . ? O1 C2 C7 112.9(3) . . ? C2 C3 C4 119.4(3) . . ? C5 C4 C3 120.2(3) . . ? C4 C5 C6 121.6(3) . . ? C7 C6 C5 119.1(3) . . ? C7 C6 C8 122.9(3) . . ? C5 C6 C8 117.7(3) . . ? O2 C7 C6 125.2(3) . . ? O2 C7 C2 116.8(3) . . ? C6 C7 C2 118.0(3) . . ? N1 C8 C6 125.4(3) . . ? N1 C9 C10 108.5(3) . . ? N2 C10 C9 110.4(3) . . ? N2 C11 C13 126.1(3) . . ? O3 C12 C13 124.5(3) . . ? O3 C12 C17 117.7(3) . . ? C13 C12 C17 117.8(3) . . ? C12 C13 C14 118.9(3) . . ? C12 C13 C11 124.0(3) . . ? C14 C13 C11 116.8(3) . . ? C15 C14 C13 121.7(3) . . ? C14 C15 C16 119.8(3) . . ? C17 C16 C15 120.1(3) . . ? O4 C17 C16 125.4(3) . . ? O4 C17 C12 113.2(3) . . ? C16 C17 C12 121.4(3) . . ? C20 O5 C19 116.0(2) . . ? C20 O5 Dy 117.60(18) . . ? C19 O5 Dy 126.32(19) . . ? C25 O6 Zn2 129.42(19) . . ? C25 O6 Dy 129.01(19) . . ? Zn2 O6 Dy 101.41(8) . . ? C30 O7 Zn2 126.13(18) . . ? C30 O7 Dy 134.10(18) . . ? Zn2 O7 Dy 97.55(8) . . ? C35 O8 C36 116.1(2) . . ? C35 O8 Dy 116.28(17) . . ? C36 O8 Dy 127.44(19) . . ? C26 N3 C27 121.8(3) . . ? C26 N3 Zn2 129.0(2) . . ? C27 N3 Zn2 107.9(2) . . ? C29 N4 C28 119.6(3) . . ? C29 N4 Zn2 126.7(2) . . ? C28 N4 Zn2 113.0(2) . . ? O5 C20 C21 125.7(3) . . ? O5 C20 C25 113.1(3) . . ? C21 C20 C25 121.2(3) . . ? C20 C21 C22 119.3(3) . . ? C23 C22 C21 120.6(3) . . ? C22 C23 C24 121.3(3) . . ? C25 C24 C23 118.6(3) . . ? C25 C24 C26 123.8(3) . . ? C23 C24 C26 117.5(3) . . ? O6 C25 C24 124.2(3) . . ? O6 C25 C20 116.9(3) . . ? C24 C25 C20 118.9(3) . . ? N3 C26 C24 125.2(3) . . ? N3 C27 C28 109.2(3) . . ? N4 C28 C27 111.7(3) . . ? N4 C29 C31 125.8(3) . . ? O7 C30 C31 125.2(3) . . ? O7 C30 C35 117.1(3) . . ? C31 C30 C35 117.7(3) . . ? C30 C31 C32 119.2(3) . . ? C30 C31 C29 125.1(3) . . ? C32 C31 C29 115.6(3) . . ? C33 C32 C31 121.6(3) . . ? C32 C33 C34 120.0(3) . . ? C35 C34 C33 119.6(3) . . ? O8 C35 C34 125.5(3) . . ? O8 C35 C30 112.5(3) . . ? C34 C35 C30 122.0(3) . . ? C37 O9 Dy 149.1(2) . . ? C37 O10 Zn1 115.3(2) . . ? O9 C37 O10 123.6(3) . . ? O9 C37 C38 117.8(3) . . ? O10 C37 C38 118.5(3) . . ? C39 O11 Dy 149.7(2) . . ? C39 O12 Zn2 114.4(2) . . ? O11 C39 O12 123.9(3) . . ? O11 C39 C40 118.2(3) . . ? O12 C39 C40 117.9(3) . . ? C53 B1 C47 107.1(3) . . ? C53 B1 C41 111.4(3) . . ? C47 B1 C41 111.0(2) . . ? C53 B1 C59 111.3(2) . . ? C47 B1 C59 109.7(2) . . ? C41 B1 C59 106.3(2) . . ? C42 C41 C46 114.6(3) . . ? C42 C41 B1 124.7(3) . . ? C46 C41 B1 120.7(3) . . ? C43 C42 C41 122.9(3) . . ? C42 C43 C44 120.8(4) . . ? C43 C44 C45 118.4(3) . . ? C44 C45 C46 120.0(3) . . ? C45 C46 C41 123.4(3) . . ? C52 C47 C48 114.8(3) . . ? C52 C47 B1 125.2(3) . . ? C48 C47 B1 119.9(3) . . ? C49 C48 C47 123.2(4) . . ? C48 C49 C50 119.5(4) . . ? C51 C50 C49 119.2(4) . . ? C50 C51 C52 120.7(4) . . ? C51 C52 C47 122.5(4) . . ? C58 C53 C54 114.8(3) . . ? C58 C53 B1 125.6(3) . . ? C54 C53 B1 119.6(3) . . ? C55 C54 C53 122.6(3) . . ? C56 C55 C54 120.3(4) . . ? C57 C56 C55 118.9(4) . . ? C56 C57 C58 120.2(4) . . ? C57 C58 C53 123.3(3) . . ? C64 C59 C60 114.2(3) . . ? C64 C59 B1 121.7(3) . . ? C60 C59 B1 124.1(3) . . ? C61 C60 C59 123.2(3) . . ? C62 C61 C60 120.6(3) . . ? C61 C62 C63 118.3(3) . . ? C64 C63 C62 120.0(3) . . ? C63 C64 C59 123.6(3) . . ? N5 C65 C66 173.3(7) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.076 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.118 # Attachment '- 3.cif' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 889488' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H65 B Ho N5 O12 Zn2' _chemical_formula_weight 1426.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.367(2) _cell_length_b 9.5447(11) _cell_length_c 34.800(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.8459(12) _cell_angle_gamma 90.00 _cell_volume 6069.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15113 _cell_measurement_theta_min 1.1765 _cell_measurement_theta_max 31.8205 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 2.143 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.6164 _exptl_absorpt_correction_T_max 0.8645 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; Absorption correction was performed using REQAB (Rigaku, 1998) program. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45730 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17182 _reflns_number_gt 13870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear ver. 1.4' _computing_cell_refinement 'CrystalClear ver. 1.4' _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics OrtepIII _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0514P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17182 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Ho Ho 0.324558(8) 0.111575(15) 0.131618(4) 0.02126(5) Uani 1 1 d . . . Zn1 Zn 0.29182(2) 0.24458(4) 0.217561(10) 0.02122(8) Uani 1 1 d . . . Zn2 Zn 0.37080(2) 0.01075(4) 0.045190(10) 0.02449(9) Uani 1 1 d . . . O1 O 0.31510(12) -0.1544(2) 0.14867(6) 0.0233(4) Uani 1 1 d . . . O2 O 0.30190(12) 0.0536(2) 0.19384(6) 0.0224(4) Uani 1 1 d . . . O3 O 0.25514(12) 0.2850(2) 0.16098(6) 0.0243(5) Uani 1 1 d . . . O4 O 0.22884(14) 0.3058(3) 0.08713(7) 0.0314(5) Uani 1 1 d . . . N1 N 0.28115(16) 0.1485(3) 0.26959(8) 0.0268(6) Uani 1 1 d . . . N2 N 0.20708(16) 0.3602(3) 0.23447(8) 0.0280(6) Uani 1 1 d . . . C1 C 0.3140(2) -0.2727(4) 0.12287(10) 0.0330(8) Uani 1 1 d . . . H1 H 0.3598 -0.3252 0.1279 0.050 Uiso 1 1 calc R . . H2 H 0.3088 -0.2395 0.0961 0.050 Uiso 1 1 calc R . . H3 H 0.2727 -0.3337 0.1271 0.050 Uiso 1 1 calc R . . C2 C 0.31680(17) -0.1870(3) 0.18772(9) 0.0223(6) Uani 1 1 d . . . C3 C 0.32775(19) -0.3194(4) 0.20306(10) 0.0288(7) Uani 1 1 d . . . H4 H 0.3347 -0.3968 0.1866 0.035 Uiso 1 1 calc R . . C4 C 0.3286(2) -0.3394(4) 0.24305(10) 0.0311(7) Uani 1 1 d . . . H5 H 0.3375 -0.4299 0.2539 0.037 Uiso 1 1 calc R . . C5 C 0.31641(19) -0.2276(4) 0.26637(9) 0.0281(7) Uani 1 1 d . . . H6 H 0.3150 -0.2423 0.2933 0.034 Uiso 1 1 calc R . . C6 C 0.30590(18) -0.0912(3) 0.25117(9) 0.0237(6) Uani 1 1 d . . . C7 C 0.30820(16) -0.0689(3) 0.21130(9) 0.0213(6) Uani 1 1 d . . . C8 C 0.28519(19) 0.0187(4) 0.27723(9) 0.0299(7) Uani 1 1 d . . . H7 H 0.2737 -0.0096 0.3021 0.036 Uiso 1 1 calc R . . C9 C 0.2519(2) 0.2488(4) 0.29566(10) 0.0363(8) Uani 1 1 d . . . H8 H 0.2906 0.3155 0.3056 0.044 Uiso 1 1 calc R . . H9 H 0.2345 0.1990 0.3179 0.044 Uiso 1 1 calc R . . C10 C 0.1889(2) 0.3273(5) 0.27368(10) 0.0384(9) Uani 1 1 d . . . H10 H 0.1441 0.2692 0.2722 0.046 Uiso 1 1 calc R . . H11 H 0.1794 0.4150 0.2875 0.046 Uiso 1 1 calc R . . C11 C 0.16757(19) 0.4469(4) 0.21330(10) 0.0316(7) Uani 1 1 d . . . H12 H 0.1333 0.5007 0.2257 0.038 Uiso 1 1 calc R . . C12 C 0.20865(17) 0.3843(3) 0.14859(9) 0.0206(6) Uani 1 1 d . . . C13 C 0.17006(18) 0.4707(3) 0.17238(10) 0.0261(7) Uani 1 1 d . . . C14 C 0.1256(2) 0.5786(4) 0.15557(11) 0.0341(8) Uani 1 1 d . . . H13 H 0.0998 0.6366 0.1717 0.041 Uiso 1 1 calc R . . C15 C 0.1184(2) 0.6026(4) 0.11658(11) 0.0338(8) Uani 1 1 d . . . H14 H 0.0900 0.6794 0.1061 0.041 Uiso 1 1 calc R . . C16 C 0.15283(19) 0.5139(4) 0.09247(10) 0.0304(7) Uani 1 1 d . . . H15 H 0.1472 0.5286 0.0653 0.036 Uiso 1 1 calc R . . C17 C 0.19540(17) 0.4039(3) 0.10803(9) 0.0238(6) Uani 1 1 d . . . C18 C 0.2249(2) 0.3275(4) 0.04657(10) 0.0360(8) Uani 1 1 d . . . H16 H 0.1735 0.3294 0.0358 0.054 Uiso 1 1 calc R . . H17 H 0.2503 0.2512 0.0347 0.054 Uiso 1 1 calc R . . H18 H 0.2481 0.4170 0.0413 0.054 Uiso 1 1 calc R . . O5 O 0.18742(12) 0.0394(3) 0.12359(6) 0.0267(5) Uani 1 1 d . . . O6 O 0.27918(12) 0.0174(2) 0.07351(6) 0.0247(5) Uani 1 1 d . . . O7 O 0.41610(12) -0.0152(2) 0.10070(6) 0.0249(5) Uani 1 1 d . . . O8 O 0.45200(12) -0.0185(3) 0.17360(6) 0.0268(5) Uani 1 1 d . . . N3 N 0.30607(17) -0.0556(4) -0.00274(8) 0.0361(7) Uani 1 1 d . . . N4 N 0.43595(16) -0.1424(3) 0.02658(8) 0.0300(6) Uani 1 1 d . . . C19 C 0.13768(19) 0.0434(5) 0.15303(10) 0.0365(8) Uani 1 1 d . . . H19 H 0.1012 0.1172 0.1469 0.055 Uiso 1 1 calc R . . H20 H 0.1651 0.0630 0.1781 0.055 Uiso 1 1 calc R . . H21 H 0.1129 -0.0472 0.1541 0.055 Uiso 1 1 calc R . . C20 C 0.15779(18) -0.0006(4) 0.08735(9) 0.0270(7) Uani 1 1 d . . . C21 C 0.08450(19) -0.0266(4) 0.07673(11) 0.0367(9) Uani 1 1 d . . . H22 H 0.0494 -0.0131 0.0946 0.044 Uiso 1 1 calc R . . C22 C 0.0630(2) -0.0731(5) 0.03921(13) 0.0504(11) Uani 1 1 d . . . H23 H 0.0129 -0.0933 0.0318 0.060 Uiso 1 1 calc R . . C23 C 0.1129(2) -0.0902(5) 0.01290(12) 0.0447(10) Uani 1 1 d . . . H24 H 0.0970 -0.1223 -0.0124 0.054 Uiso 1 1 calc R . . C24 C 0.18786(19) -0.0605(4) 0.02305(10) 0.0321(8) Uani 1 1 d . . . C25 C 0.21062(17) -0.0133(4) 0.06073(9) 0.0257(7) Uani 1 1 d . . . C26 C 0.2381(2) -0.0870(4) -0.00607(10) 0.0389(9) Uani 1 1 d . . . H25 H 0.2187 -0.1311 -0.0294 0.047 Uiso 1 1 calc R . . C27 C 0.3543(2) -0.0954(5) -0.03221(11) 0.0465(11) Uani 1 1 d . . . H26 H 0.3748 -0.0104 -0.0433 0.056 Uiso 1 1 calc R . . H27 H 0.3261 -0.1476 -0.0533 0.056 Uiso 1 1 calc R . . C28 C 0.4148(2) -0.1852(5) -0.01371(11) 0.0432(10) Uani 1 1 d . . . H28 H 0.3988 -0.2842 -0.0143 0.052 Uiso 1 1 calc R . . H29 H 0.4578 -0.1779 -0.0286 0.052 Uiso 1 1 calc R . . C29 C 0.48357(19) -0.2134(4) 0.04732(10) 0.0299(7) Uani 1 1 d . . . H30 H 0.5094 -0.2826 0.0345 0.036 Uiso 1 1 calc R . . C30 C 0.46753(17) -0.1059(3) 0.11266(9) 0.0218(6) Uani 1 1 d . . . C31 C 0.50244(17) -0.1989(4) 0.08886(10) 0.0259(7) Uani 1 1 d . . . C32 C 0.55560(19) -0.2933(4) 0.10572(11) 0.0304(7) Uani 1 1 d . . . H31 H 0.5788 -0.3561 0.0896 0.036 Uiso 1 1 calc R . . C33 C 0.57439(19) -0.2962(4) 0.14465(11) 0.0312(7) Uani 1 1 d . . . H32 H 0.6104 -0.3605 0.1554 0.037 Uiso 1 1 calc R . . C34 C 0.54080(18) -0.2047(4) 0.16889(10) 0.0277(7) Uani 1 1 d . . . H33 H 0.5540 -0.2063 0.1960 0.033 Uiso 1 1 calc R . . C35 C 0.48862(17) -0.1126(3) 0.15314(9) 0.0227(6) Uani 1 1 d . . . C36 C 0.4779(2) -0.0035(4) 0.21345(10) 0.0355(8) Uani 1 1 d . . . H34 H 0.4717 -0.0922 0.2269 0.053 Uiso 1 1 calc R . . H35 H 0.4500 0.0702 0.2250 0.053 Uiso 1 1 calc R . . H36 H 0.5299 0.0219 0.2158 0.053 Uiso 1 1 calc R . . O9 O 0.40859(12) 0.2539(3) 0.16660(7) 0.0287(5) Uani 1 1 d . . . O10 O 0.38606(12) 0.3482(2) 0.22244(7) 0.0268(5) Uani 1 1 d . . . C37 C 0.42222(18) 0.3387(3) 0.19322(9) 0.0242(6) Uani 1 1 d . . . C38 C 0.4862(2) 0.4355(4) 0.19073(11) 0.0373(8) Uani 1 1 d . . . H37 H 0.5315 0.3873 0.2004 0.056 Uiso 1 1 calc R . . H38 H 0.4800 0.5191 0.2064 0.056 Uiso 1 1 calc R . . H39 H 0.4886 0.4631 0.1638 0.056 Uiso 1 1 calc R . . O11 O 0.37496(14) 0.2668(2) 0.08955(7) 0.0311(5) Uani 1 1 d . . . O12 O 0.40932(15) 0.1976(3) 0.03323(7) 0.0356(6) Uani 1 1 d . . . C39 C 0.40620(19) 0.2863(4) 0.06008(10) 0.0296(7) Uani 1 1 d . . . C40 C 0.4428(3) 0.4260(4) 0.05543(13) 0.0474(11) Uani 1 1 d . . . H40 H 0.4280 0.4917 0.0748 0.071 Uiso 1 1 calc R . . H41 H 0.4281 0.4630 0.0295 0.071 Uiso 1 1 calc R . . H42 H 0.4961 0.4140 0.0589 0.071 Uiso 1 1 calc R . . B1 B -0.1459(2) 0.2214(4) 0.13337(10) 0.0242(7) Uani 1 1 d . . . C41 C -0.11980(18) 0.3102(4) 0.17321(9) 0.0257(7) Uani 1 1 d . . . C42 C -0.0757(2) 0.4291(4) 0.17466(11) 0.0407(9) Uani 1 1 d . . . H43 H -0.0586 0.4620 0.1514 0.049 Uiso 1 1 calc R . . C43 C -0.0558(3) 0.5015(5) 0.20863(12) 0.0484(11) Uani 1 1 d . . . H44 H -0.0258 0.5825 0.2082 0.058 Uiso 1 1 calc R . . C44 C -0.0794(2) 0.4566(5) 0.24323(11) 0.0427(10) Uani 1 1 d . . . H45 H -0.0658 0.5061 0.2665 0.051 Uiso 1 1 calc R . . C45 C -0.1230(2) 0.3389(4) 0.24318(10) 0.0374(8) Uani 1 1 d . . . H46 H -0.1395 0.3060 0.2665 0.045 Uiso 1 1 calc R . . C46 C -0.1425(2) 0.2689(4) 0.20870(10) 0.0305(7) Uani 1 1 d . . . H47 H -0.1729 0.1886 0.2092 0.037 Uiso 1 1 calc R . . C47 C -0.10800(17) 0.0659(4) 0.13434(10) 0.0261(7) Uani 1 1 d . . . C48 C -0.1184(2) -0.0213(4) 0.10167(12) 0.0386(9) Uani 1 1 d . . . H48 H -0.1458 0.0136 0.0791 0.046 Uiso 1 1 calc R . . C49 C -0.0902(2) -0.1568(5) 0.10104(13) 0.0439(10) Uani 1 1 d . . . H49 H -0.0983 -0.2119 0.0783 0.053 Uiso 1 1 calc R . . C50 C -0.0506(2) -0.2110(4) 0.13360(13) 0.0425(10) Uani 1 1 d . . . H50 H -0.0326 -0.3043 0.1337 0.051 Uiso 1 1 calc R . . C51 C -0.0377(2) -0.1281(4) 0.16573(13) 0.0398(9) Uani 1 1 d . . . H51 H -0.0092 -0.1633 0.1880 0.048 Uiso 1 1 calc R . . C52 C -0.06613(19) 0.0076(4) 0.16613(10) 0.0307(7) Uani 1 1 d . . . H52 H -0.0566 0.0624 0.1889 0.037 Uiso 1 1 calc R . . C53 C -0.12237(18) 0.3026(4) 0.09482(9) 0.0268(7) Uani 1 1 d . . . C54 C -0.0484(2) 0.3074(5) 0.08785(11) 0.0378(9) Uani 1 1 d . . . H53 H -0.0131 0.2635 0.1058 0.045 Uiso 1 1 calc R . . C55 C -0.0248(2) 0.3731(5) 0.05609(13) 0.0534(13) Uani 1 1 d . . . H54 H 0.0258 0.3732 0.0526 0.064 Uiso 1 1 calc R . . C56 C -0.0734(3) 0.4379(6) 0.02965(13) 0.0622(15) Uani 1 1 d . . . H55 H -0.0571 0.4837 0.0079 0.075 Uiso 1 1 calc R . . C57 C -0.1465(3) 0.4356(6) 0.03505(13) 0.0617(15) Uani 1 1 d . . . H56 H -0.1812 0.4801 0.0169 0.074 Uiso 1 1 calc R . . C58 C -0.1697(2) 0.3685(4) 0.06698(10) 0.0357(9) Uani 1 1 d . . . H57 H -0.2206 0.3677 0.0699 0.043 Uiso 1 1 calc R . . C59 C -0.23607(17) 0.2059(3) 0.13180(8) 0.0227(6) Uani 1 1 d . . . C60 C -0.27248(19) 0.0778(4) 0.13438(10) 0.0286(7) Uani 1 1 d . . . H58 H -0.2441 -0.0055 0.1367 0.034 Uiso 1 1 calc R . . C61 C -0.34830(19) 0.0662(4) 0.13367(10) 0.0307(7) Uani 1 1 d . . . H59 H -0.3700 -0.0232 0.1361 0.037 Uiso 1 1 calc R . . C62 C -0.39216(19) 0.1848(4) 0.12938(10) 0.0323(8) Uani 1 1 d . . . H60 H -0.4439 0.1779 0.1281 0.039 Uiso 1 1 calc R . . C63 C -0.35785(19) 0.3145(4) 0.12704(10) 0.0304(7) Uani 1 1 d . . . H61 H -0.3865 0.3974 0.1243 0.036 Uiso 1 1 calc R . . C64 C -0.28240(18) 0.3231(4) 0.12869(9) 0.0253(6) Uani 1 1 d . . . H62 H -0.2608 0.4133 0.1277 0.030 Uiso 1 1 calc R . . N5 N -0.3436(3) 0.5361(6) 0.03080(14) 0.0774(14) Uani 1 1 d . . . C65 C -0.3113(3) 0.6248(6) 0.04486(16) 0.0567(13) Uani 1 1 d . . . C66 C -0.2665(4) 0.7283(7) 0.0638(2) 0.094(2) Uani 1 1 d . . . H63 H -0.2951 0.7829 0.0808 0.142 Uiso 1 1 calc R . . H64 H -0.2481 0.7906 0.0446 0.142 Uiso 1 1 calc R . . H65 H -0.2252 0.6837 0.0791 0.142 Uiso 1 1 calc 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 Ho 0.02315(8) 0.02262(9) 0.01873(7) -0.00225(5) 0.00562(5) 0.00034(6) Zn1 0.02365(18) 0.02019(19) 0.02070(17) -0.00157(13) 0.00656(13) 0.00222(14) Zn2 0.02489(19) 0.0286(2) 0.02070(17) -0.00260(14) 0.00555(14) 0.00095(16) O1 0.0295(12) 0.0197(11) 0.0208(10) -0.0044(8) 0.0033(8) 0.0005(9) O2 0.0268(11) 0.0191(11) 0.0221(10) -0.0007(8) 0.0072(8) 0.0011(9) O3 0.0266(11) 0.0248(12) 0.0221(10) 0.0012(9) 0.0055(8) 0.0082(9) O4 0.0403(14) 0.0303(13) 0.0244(11) 0.0041(10) 0.0070(10) 0.0059(11) N1 0.0347(16) 0.0257(15) 0.0207(12) -0.0019(11) 0.0066(11) 0.0027(12) N2 0.0286(15) 0.0307(16) 0.0261(13) -0.0038(11) 0.0099(11) 0.0061(12) C1 0.041(2) 0.0280(19) 0.0302(17) -0.0159(14) 0.0054(14) -0.0068(16) C2 0.0242(15) 0.0199(15) 0.0232(14) -0.0005(11) 0.0050(11) -0.0004(12) C3 0.0333(18) 0.0254(17) 0.0273(16) -0.0028(13) 0.0014(13) 0.0023(15) C4 0.039(2) 0.0208(17) 0.0335(18) 0.0044(13) 0.0031(14) 0.0027(15) C5 0.0342(18) 0.0259(17) 0.0241(15) 0.0061(13) 0.0021(13) -0.0008(14) C6 0.0241(16) 0.0228(16) 0.0245(15) -0.0013(12) 0.0041(12) 0.0016(13) C7 0.0182(14) 0.0220(15) 0.0238(14) 0.0023(12) 0.0019(11) -0.0016(12) C8 0.0367(19) 0.0332(19) 0.0206(15) 0.0007(13) 0.0074(13) -0.0005(15) C9 0.050(2) 0.037(2) 0.0240(16) -0.0029(14) 0.0119(15) 0.0061(18) C10 0.039(2) 0.048(2) 0.0308(18) -0.0023(17) 0.0156(15) 0.0091(18) C11 0.0282(17) 0.0307(19) 0.0371(19) -0.0057(15) 0.0099(14) 0.0045(15) C12 0.0183(14) 0.0162(14) 0.0271(15) 0.0005(11) 0.0015(11) 0.0036(11) C13 0.0236(16) 0.0226(16) 0.0324(17) 0.0000(13) 0.0040(13) 0.0024(13) C14 0.0267(18) 0.0301(19) 0.045(2) -0.0006(16) 0.0036(15) 0.0091(15) C15 0.0265(18) 0.031(2) 0.042(2) 0.0056(15) -0.0035(15) 0.0098(15) C16 0.0281(17) 0.0303(19) 0.0320(17) 0.0060(14) -0.0008(13) 0.0027(14) C17 0.0203(15) 0.0219(16) 0.0294(16) 0.0001(12) 0.0030(12) 0.0000(12) C18 0.043(2) 0.041(2) 0.0248(16) 0.0060(15) 0.0036(14) 0.0099(18) O5 0.0212(11) 0.0368(14) 0.0230(11) -0.0002(10) 0.0059(8) -0.0009(10) O6 0.0197(10) 0.0331(13) 0.0213(10) -0.0026(9) 0.0024(8) -0.0008(9) O7 0.0215(11) 0.0285(12) 0.0250(11) -0.0018(9) 0.0040(8) 0.0048(9) O8 0.0237(11) 0.0338(13) 0.0227(11) -0.0039(9) 0.0014(8) 0.0037(10) N3 0.0301(16) 0.056(2) 0.0226(14) -0.0070(13) 0.0028(11) 0.0050(15) N4 0.0279(15) 0.0367(17) 0.0262(14) -0.0096(12) 0.0065(11) -0.0006(13) C19 0.0263(17) 0.055(2) 0.0295(17) -0.0030(17) 0.0102(14) -0.0083(17) C20 0.0234(16) 0.0324(19) 0.0248(15) 0.0027(13) 0.0008(12) 0.0005(14) C21 0.0221(17) 0.053(2) 0.0352(19) 0.0026(17) 0.0018(14) -0.0019(17) C22 0.0245(19) 0.080(3) 0.044(2) -0.005(2) -0.0052(16) -0.007(2) C23 0.0288(19) 0.072(3) 0.0307(19) -0.0040(19) -0.0081(15) -0.0021(19) C24 0.0261(17) 0.044(2) 0.0251(16) 0.0000(15) -0.0026(13) 0.0014(16) C25 0.0212(15) 0.0316(18) 0.0239(15) 0.0012(13) 0.0002(12) 0.0004(13) C26 0.039(2) 0.055(3) 0.0212(16) -0.0092(16) -0.0047(14) 0.0038(18) C27 0.040(2) 0.077(3) 0.0239(17) -0.0093(18) 0.0080(15) 0.004(2) C28 0.040(2) 0.058(3) 0.0320(19) -0.0156(18) 0.0063(16) 0.005(2) C29 0.0294(17) 0.0297(19) 0.0316(17) -0.0061(14) 0.0087(13) 0.0025(15) C30 0.0157(14) 0.0225(16) 0.0277(15) -0.0008(12) 0.0046(11) 0.0012(12) C31 0.0204(15) 0.0257(17) 0.0323(17) -0.0017(13) 0.0060(12) -0.0033(13) C32 0.0283(17) 0.0224(17) 0.0412(19) -0.0023(14) 0.0072(14) 0.0021(14) C33 0.0274(17) 0.0205(17) 0.045(2) 0.0041(14) 0.0025(14) 0.0032(14) C34 0.0219(15) 0.0254(17) 0.0356(17) 0.0039(13) 0.0020(13) -0.0020(13) C35 0.0180(14) 0.0231(16) 0.0276(15) -0.0031(12) 0.0054(11) -0.0011(12) C36 0.0338(19) 0.048(2) 0.0239(16) -0.0039(15) -0.0026(13) 0.0069(17) O9 0.0252(12) 0.0306(13) 0.0307(12) -0.0068(10) 0.0051(9) -0.0024(10) O10 0.0248(12) 0.0285(12) 0.0279(11) -0.0031(9) 0.0069(9) -0.0036(10) C37 0.0251(16) 0.0221(16) 0.0255(15) 0.0012(12) 0.0029(12) 0.0003(13) C38 0.038(2) 0.044(2) 0.0314(18) -0.0047(16) 0.0081(15) -0.0134(18) O11 0.0382(14) 0.0281(13) 0.0284(12) 0.0013(10) 0.0106(10) -0.0009(11) O12 0.0486(16) 0.0311(14) 0.0289(12) 0.0007(10) 0.0122(11) -0.0042(12) C39 0.0312(18) 0.0276(18) 0.0301(17) 0.0029(13) 0.0035(13) -0.0003(15) C40 0.061(3) 0.035(2) 0.049(2) -0.0049(18) 0.020(2) -0.013(2) B1 0.0222(17) 0.0281(19) 0.0224(16) 0.0024(14) 0.0025(13) 0.0001(15) C41 0.0248(16) 0.0248(17) 0.0270(15) 0.0036(13) 0.0002(12) 0.0003(13) C42 0.050(2) 0.039(2) 0.0338(19) 0.0001(16) 0.0086(17) -0.0149(19) C43 0.059(3) 0.045(3) 0.041(2) -0.0035(18) 0.0025(19) -0.020(2) C44 0.048(2) 0.044(2) 0.034(2) -0.0113(17) -0.0057(17) -0.004(2) C45 0.038(2) 0.047(2) 0.0266(17) 0.0028(16) 0.0027(14) 0.0003(18) C46 0.0323(18) 0.0313(19) 0.0281(16) 0.0032(14) 0.0034(13) -0.0049(15) C47 0.0190(15) 0.0301(18) 0.0297(16) 0.0040(13) 0.0047(12) -0.0010(13) C48 0.037(2) 0.037(2) 0.042(2) -0.0032(17) 0.0048(16) 0.0049(17) C49 0.039(2) 0.039(2) 0.055(3) -0.0123(19) 0.0113(18) 0.0011(19) C50 0.0300(19) 0.031(2) 0.069(3) 0.0060(19) 0.0164(19) 0.0032(16) C51 0.0303(19) 0.038(2) 0.052(2) 0.0164(18) 0.0095(17) 0.0089(16) C52 0.0255(16) 0.0331(19) 0.0342(18) 0.0080(14) 0.0054(13) -0.0007(15) C53 0.0289(17) 0.0277(17) 0.0240(15) 0.0011(13) 0.0040(12) -0.0069(14) C54 0.0260(17) 0.056(3) 0.0311(18) 0.0097(17) -0.0002(14) -0.0060(17) C55 0.029(2) 0.090(4) 0.042(2) 0.017(2) 0.0080(17) -0.018(2) C56 0.046(3) 0.097(4) 0.046(3) 0.037(3) 0.013(2) -0.016(3) C57 0.042(2) 0.105(4) 0.039(2) 0.040(3) 0.0071(19) 0.003(3) C58 0.0268(17) 0.054(2) 0.0266(16) 0.0127(16) 0.0038(13) -0.0040(17) C59 0.0278(16) 0.0231(16) 0.0175(13) 0.0018(11) 0.0046(11) -0.0012(13) C60 0.0294(17) 0.0279(18) 0.0286(16) 0.0064(13) 0.0043(13) 0.0005(14) C61 0.0308(18) 0.0291(18) 0.0331(18) 0.0007(14) 0.0079(14) -0.0092(15) C62 0.0264(17) 0.040(2) 0.0316(17) -0.0040(15) 0.0073(13) -0.0021(16) C63 0.0299(18) 0.034(2) 0.0278(16) 0.0015(14) 0.0070(13) 0.0094(15) C64 0.0305(17) 0.0228(16) 0.0233(14) -0.0009(12) 0.0068(12) -0.0004(13) N5 0.077(3) 0.087(4) 0.067(3) 0.002(3) 0.000(3) 0.007(3) C65 0.056(3) 0.058(3) 0.060(3) -0.011(2) 0.024(2) -0.011(2) C66 0.078(4) 0.092(5) 0.117(6) -0.020(4) 0.031(4) -0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho O6 2.291(2) . ? Ho O9 2.308(2) . ? Ho O2 2.313(2) . ? Ho O11 2.339(2) . ? Ho O3 2.382(2) . ? Ho O7 2.412(2) . ? Ho O5 2.599(2) . ? Ho O1 2.617(2) . ? Ho O4 2.893(2) . ? Ho Zn2 3.3488(5) . ? Ho Zn1 3.3592(5) . ? Zn1 O10 1.986(2) . ? Zn1 O2 2.017(2) . ? Zn1 N2 2.043(3) . ? Zn1 O3 2.052(2) . ? Zn1 N1 2.057(3) . ? Zn2 O12 1.979(3) . ? Zn2 O6 2.036(2) . ? Zn2 N4 2.036(3) . ? Zn2 O7 2.039(2) . ? Zn2 N3 2.047(3) . ? O1 C2 1.391(4) . ? O1 C1 1.441(4) . ? O2 C7 1.318(4) . ? O3 C12 1.319(4) . ? O4 C17 1.369(4) . ? O4 C18 1.421(4) . ? N1 C8 1.267(4) . ? N1 C9 1.458(4) . ? N2 C11 1.283(5) . ? N2 C10 1.471(4) . ? C2 C3 1.379(5) . ? C2 C7 1.412(4) . ? C3 C4 1.403(5) . ? C4 C5 1.373(5) . ? C5 C6 1.411(4) . ? C6 C7 1.408(4) . ? C6 C8 1.462(5) . ? C9 C10 1.518(5) . ? C11 C13 1.447(5) . ? C12 C13 1.409(4) . ? C12 C17 1.420(4) . ? C13 C14 1.405(5) . ? C14 C15 1.369(5) . ? C15 C16 1.389(5) . ? C16 C17 1.386(5) . ? O5 C20 1.375(4) . ? O5 C19 1.441(4) . ? O6 C25 1.325(4) . ? O7 C30 1.318(4) . ? O8 C35 1.365(4) . ? O8 C36 1.427(4) . ? N3 C26 1.277(5) . ? N3 C27 1.472(5) . ? N4 C29 1.271(5) . ? N4 C28 1.474(4) . ? C20 C21 1.382(5) . ? C20 C25 1.414(5) . ? C21 C22 1.397(6) . ? C22 C23 1.369(6) . ? C23 C24 1.416(5) . ? C24 C25 1.409(5) . ? C24 C26 1.461(5) . ? C27 C28 1.497(6) . ? C29 C31 1.458(5) . ? C30 C31 1.412(4) . ? C30 C35 1.424(4) . ? C31 C32 1.412(5) . ? C32 C33 1.364(5) . ? C33 C34 1.400(5) . ? C34 C35 1.373(5) . ? O9 C37 1.237(4) . ? O10 C37 1.273(4) . ? C37 C38 1.504(5) . ? O11 C39 1.239(4) . ? O12 C39 1.266(4) . ? C39 C40 1.509(5) . ? B1 C47 1.638(5) . ? B1 C53 1.645(5) . ? B1 C41 1.654(5) . ? B1 C59 1.659(5) . ? C41 C42 1.392(5) . ? C41 C46 1.399(5) . ? C42 C43 1.386(6) . ? C43 C44 1.388(6) . ? C44 C45 1.379(6) . ? C45 C46 1.388(5) . ? C47 C52 1.397(5) . ? C47 C48 1.406(5) . ? C48 C49 1.394(6) . ? C49 C50 1.383(6) . ? C50 C51 1.371(6) . ? C51 C52 1.397(5) . ? C53 C58 1.385(5) . ? C53 C54 1.406(5) . ? C54 C55 1.379(5) . ? C55 C56 1.364(6) . ? C56 C57 1.375(6) . ? C57 C58 1.387(5) . ? C59 C60 1.401(5) . ? C59 C64 1.403(5) . ? C60 C61 1.395(5) . ? C61 C62 1.389(5) . ? C62 C63 1.395(5) . ? C63 C64 1.384(5) . ? N5 C65 1.118(7) . ? C65 C66 1.405(8) . ? 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 O6 Ho O9 149.32(8) . . ? O6 Ho O2 130.43(8) . . ? O9 Ho O2 79.71(8) . . ? O6 Ho O11 80.07(8) . . ? O9 Ho O11 70.81(8) . . ? O2 Ho O11 149.06(8) . . ? O6 Ho O3 119.25(8) . . ? O9 Ho O3 73.93(8) . . ? O2 Ho O3 67.02(7) . . ? O11 Ho O3 95.25(8) . . ? O6 Ho O7 67.48(8) . . ? O9 Ho O7 94.09(8) . . ? O2 Ho O7 119.85(8) . . ? O11 Ho O7 72.56(8) . . ? O3 Ho O7 165.42(8) . . ? O6 Ho O5 62.59(7) . . ? O9 Ho O5 143.28(8) . . ? O2 Ho O5 76.85(7) . . ? O11 Ho O5 122.79(8) . . ? O3 Ho O5 71.04(8) . . ? O7 Ho O5 122.08(7) . . ? O6 Ho O1 78.06(7) . . ? O9 Ho O1 120.50(8) . . ? O2 Ho O1 62.19(7) . . ? O11 Ho O1 142.75(8) . . ? O3 Ho O1 121.74(7) . . ? O7 Ho O1 71.33(7) . . ? O5 Ho O1 71.41(7) . . ? O6 Ho O4 68.42(7) . . ? O9 Ho O4 104.04(8) . . ? O2 Ho O4 119.78(7) . . ? O11 Ho O4 61.11(8) . . ? O3 Ho O4 57.43(7) . . ? O7 Ho O4 119.73(7) . . ? O5 Ho O4 65.34(7) . . ? O1 Ho O4 133.80(7) . . ? O6 Ho Zn2 36.60(5) . . ? O9 Ho Zn2 115.19(6) . . ? O2 Ho Zn2 149.12(5) . . ? O11 Ho Zn2 57.80(6) . . ? O3 Ho Zn2 141.32(5) . . ? O7 Ho Zn2 37.16(5) . . ? O5 Ho Zn2 99.15(5) . . ? O1 Ho Zn2 87.34(5) . . ? O4 Ho Zn2 84.22(5) . . ? O6 Ho Zn1 148.44(5) . . ? O9 Ho Zn1 58.58(6) . . ? O2 Ho Zn1 36.04(5) . . ? O11 Ho Zn1 115.85(6) . . ? O3 Ho Zn1 37.20(5) . . ? O7 Ho Zn1 141.52(5) . . ? O5 Ho Zn1 86.36(5) . . ? O1 Ho Zn1 98.20(5) . . ? O4 Ho Zn1 94.60(5) . . ? Zn2 Ho Zn1 173.230(10) . . ? O10 Zn1 O2 111.68(9) . . ? O10 Zn1 N2 112.93(11) . . ? O2 Zn1 N2 135.26(11) . . ? O10 Zn1 O3 100.75(9) . . ? O2 Zn1 O3 79.17(9) . . ? N2 Zn1 O3 89.39(10) . . ? O10 Zn1 N1 107.88(11) . . ? O2 Zn1 N1 88.77(10) . . ? N2 Zn1 N1 81.00(11) . . ? O3 Zn1 N1 151.33(11) . . ? O10 Zn1 Ho 91.77(7) . . ? O2 Zn1 Ho 42.43(6) . . ? N2 Zn1 Ho 132.17(8) . . ? O3 Zn1 Ho 44.58(6) . . ? N1 Zn1 Ho 131.08(8) . . ? O12 Zn2 O6 113.85(10) . . ? O12 Zn2 N4 110.25(12) . . ? O6 Zn2 N4 135.88(11) . . ? O12 Zn2 O7 100.87(10) . . ? O6 Zn2 O7 79.79(9) . . ? N4 Zn2 O7 91.02(10) . . ? O12 Zn2 N3 107.32(13) . . ? O6 Zn2 N3 87.94(11) . . ? N4 Zn2 N3 80.23(12) . . ? O7 Zn2 N3 151.79(12) . . ? O12 Zn2 Ho 93.37(7) . . ? O6 Zn2 Ho 42.14(6) . . ? N4 Zn2 Ho 134.66(9) . . ? O7 Zn2 Ho 45.60(6) . . ? N3 Zn2 Ho 129.88(9) . . ? C2 O1 C1 115.5(3) . . ? C2 O1 Ho 116.29(17) . . ? C1 O1 Ho 128.0(2) . . ? C7 O2 Zn1 128.37(19) . . ? C7 O2 Ho 128.91(19) . . ? Zn1 O2 Ho 101.53(9) . . ? C12 O3 Zn1 125.97(19) . . ? C12 O3 Ho 135.77(19) . . ? Zn1 O3 Ho 98.22(8) . . ? C17 O4 C18 116.6(3) . . ? C17 O4 Ho 115.79(19) . . ? C18 O4 Ho 126.3(2) . . ? C8 N1 C9 121.9(3) . . ? C8 N1 Zn1 127.7(2) . . ? C9 N1 Zn1 109.2(2) . . ? C11 N2 C10 120.1(3) . . ? C11 N2 Zn1 125.9(2) . . ? C10 N2 Zn1 113.8(2) . . ? C3 C2 O1 124.8(3) . . ? C3 C2 C7 121.8(3) . . ? O1 C2 C7 113.4(3) . . ? C2 C3 C4 119.7(3) . . ? C5 C4 C3 119.6(3) . . ? C4 C5 C6 121.3(3) . . ? C7 C6 C5 119.5(3) . . ? C7 C6 C8 122.6(3) . . ? C5 C6 C8 117.6(3) . . ? O2 C7 C6 125.3(3) . . ? O2 C7 C2 116.8(3) . . ? C6 C7 C2 117.9(3) . . ? N1 C8 C6 125.8(3) . . ? N1 C9 C10 108.7(3) . . ? N2 C10 C9 109.9(3) . . ? N2 C11 C13 126.4(3) . . ? O3 C12 C13 125.2(3) . . ? O3 C12 C17 117.3(3) . . ? C13 C12 C17 117.5(3) . . ? C14 C13 C12 119.3(3) . . ? C14 C13 C11 116.7(3) . . ? C12 C13 C11 123.7(3) . . ? C15 C14 C13 122.0(3) . . ? C14 C15 C16 119.5(3) . . ? C17 C16 C15 120.0(3) . . ? O4 C17 C16 125.2(3) . . ? O4 C17 C12 113.4(3) . . ? C16 C17 C12 121.4(3) . . ? C20 O5 C19 116.0(3) . . ? C20 O5 Ho 117.44(18) . . ? C19 O5 Ho 126.46(19) . . ? C25 O6 Zn2 129.4(2) . . ? C25 O6 Ho 129.13(19) . . ? Zn2 O6 Ho 101.26(9) . . ? C30 O7 Zn2 126.1(2) . . ? C30 O7 Ho 134.34(19) . . ? Zn2 O7 Ho 97.23(8) . . ? C35 O8 C36 116.1(3) . . ? C26 N3 C27 121.9(3) . . ? C26 N3 Zn2 128.9(2) . . ? C27 N3 Zn2 107.9(2) . . ? C29 N4 C28 119.5(3) . . ? C29 N4 Zn2 126.5(2) . . ? C28 N4 Zn2 113.3(2) . . ? O5 C20 C21 125.4(3) . . ? O5 C20 C25 113.0(3) . . ? C21 C20 C25 121.6(3) . . ? C20 C21 C22 118.8(4) . . ? C23 C22 C21 121.2(4) . . ? C22 C23 C24 120.6(4) . . ? C25 C24 C23 119.0(3) . . ? C25 C24 C26 123.5(3) . . ? C23 C24 C26 117.4(3) . . ? O6 C25 C24 124.4(3) . . ? O6 C25 C20 117.0(3) . . ? C24 C25 C20 118.6(3) . . ? N3 C26 C24 125.3(3) . . ? N3 C27 C28 108.7(3) . . ? N4 C28 C27 111.3(3) . . ? N4 C29 C31 126.3(3) . . ? O7 C30 C31 125.6(3) . . ? O7 C30 C35 117.1(3) . . ? C31 C30 C35 117.3(3) . . ? C30 C31 C32 119.6(3) . . ? C30 C31 C29 124.4(3) . . ? C32 C31 C29 115.8(3) . . ? C33 C32 C31 121.4(3) . . ? C32 C33 C34 120.2(3) . . ? C35 C34 C33 119.5(3) . . ? O8 C35 C34 125.0(3) . . ? O8 C35 C30 112.8(3) . . ? C34 C35 C30 122.1(3) . . ? C37 O9 Ho 148.6(2) . . ? C37 O10 Zn1 114.7(2) . . ? O9 C37 O10 124.3(3) . . ? O9 C37 C38 117.3(3) . . ? O10 C37 C38 118.4(3) . . ? C39 O11 Ho 149.2(2) . . ? C39 O12 Zn2 113.8(2) . . ? O11 C39 O12 124.7(3) . . ? O11 C39 C40 118.1(3) . . ? O12 C39 C40 117.2(3) . . ? C47 B1 C53 107.3(3) . . ? C47 B1 C41 111.2(3) . . ? C53 B1 C41 111.4(3) . . ? C47 B1 C59 109.9(3) . . ? C53 B1 C59 111.0(3) . . ? C41 B1 C59 106.0(3) . . ? C42 C41 C46 114.9(3) . . ? C42 C41 B1 124.5(3) . . ? C46 C41 B1 120.6(3) . . ? C43 C42 C41 122.7(4) . . ? C42 C43 C44 120.5(4) . . ? C45 C44 C43 118.8(4) . . ? C44 C45 C46 119.5(3) . . ? C45 C46 C41 123.6(3) . . ? C52 C47 C48 115.1(3) . . ? C52 C47 B1 125.1(3) . . ? C48 C47 B1 119.8(3) . . ? C49 C48 C47 122.8(4) . . ? C50 C49 C48 119.9(4) . . ? C51 C50 C49 119.0(4) . . ? C50 C51 C52 120.7(4) . . ? C51 C52 C47 122.5(4) . . ? C58 C53 C54 114.5(3) . . ? C58 C53 B1 125.9(3) . . ? C54 C53 B1 119.6(3) . . ? C55 C54 C53 122.8(4) . . ? C56 C55 C54 120.6(4) . . ? C55 C56 C57 118.9(4) . . ? C56 C57 C58 120.1(4) . . ? C53 C58 C57 123.2(4) . . ? C60 C59 C64 114.3(3) . . ? C60 C59 B1 123.9(3) . . ? C64 C59 B1 121.8(3) . . ? C61 C60 C59 123.4(3) . . ? C62 C61 C60 120.3(3) . . ? C61 C62 C63 118.0(3) . . ? C64 C63 C62 120.5(3) . . ? C63 C64 C59 123.5(3) . . ? N5 C65 C66 175.4(7) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.158 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.126 # Attachment '- 4.cif' data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 889489' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H65 B Er N5 O12 Zn2' _chemical_formula_weight 1429.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.369(2) _cell_length_b 9.5339(11) _cell_length_c 34.787(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.8602(14) _cell_angle_gamma 90.00 _cell_volume 6060.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15015 _cell_measurement_theta_min 2.3542 _cell_measurement_theta_max 31.8893 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2900 _exptl_absorpt_coefficient_mu 2.225 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7761 _exptl_absorpt_correction_T_max 0.8598 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; Absorption correction was performed using REQAB (Rigaku, 1998) program. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74916 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17628 _reflns_number_gt 14571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear ver. 1.4' _computing_cell_refinement 'CrystalClear ver. 1.4' _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics OrtepIII _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0590P)^2^+0.3346P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17628 _refine_ls_number_parameters 790 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Er Er 0.324231(8) 0.108813(15) 0.131567(4) 0.02299(5) Uani 1 1 d . . . Zn1 Zn 0.291617(19) 0.24210(4) 0.217190(10) 0.02232(8) Uani 1 1 d . . . Zn2 Zn 0.37106(2) 0.00896(4) 0.045491(11) 0.02685(9) Uani 1 1 d . . . O1 O 0.31528(12) -0.1568(2) 0.14834(6) 0.0244(4) Uani 1 1 d . . . O2 O 0.30170(12) 0.0513(2) 0.19330(6) 0.0230(4) Uani 1 1 d . . . O3 O 0.25527(12) 0.2820(2) 0.16041(6) 0.0255(5) Uani 1 1 d . . . O4 O 0.22822(14) 0.3025(3) 0.08652(7) 0.0328(5) Uani 1 1 d . . . N1 N 0.28104(16) 0.1464(3) 0.26930(8) 0.0296(6) Uani 1 1 d . . . N2 N 0.20731(16) 0.3578(3) 0.23390(8) 0.0305(6) Uani 1 1 d . . . C1 C 0.3148(2) -0.2756(4) 0.12261(10) 0.0345(8) Uani 1 1 d . . . H1 H 0.3599 -0.3298 0.1285 0.052 Uiso 1 1 calc R . . H2 H 0.3116 -0.2426 0.0958 0.052 Uiso 1 1 calc R . . H3 H 0.2725 -0.3352 0.1261 0.052 Uiso 1 1 calc R . . C2 C 0.31731(17) -0.1904(3) 0.18720(9) 0.0243(6) Uani 1 1 d . . . C3 C 0.32812(18) -0.3227(3) 0.20288(10) 0.0297(7) Uani 1 1 d . . . H4 H 0.3353 -0.4007 0.1867 0.036 Uiso 1 1 calc R . . C4 C 0.3285(2) -0.3411(4) 0.24282(10) 0.0332(7) Uani 1 1 d . . . H5 H 0.3372 -0.4316 0.2538 0.040 Uiso 1 1 calc R . . C5 C 0.31633(19) -0.2303(4) 0.26603(10) 0.0299(7) Uani 1 1 d . . . H6 H 0.3153 -0.2452 0.2930 0.036 Uiso 1 1 calc R . . C6 C 0.30531(18) -0.0940(3) 0.25086(10) 0.0261(6) Uani 1 1 d . . . C7 C 0.30777(17) -0.0707(3) 0.21098(9) 0.0241(6) Uani 1 1 d . . . C8 C 0.28508(19) 0.0152(4) 0.27696(9) 0.0297(7) Uani 1 1 d . . . H7 H 0.2739 -0.0134 0.3018 0.036 Uiso 1 1 calc R . . C9 C 0.2515(2) 0.2467(4) 0.29531(10) 0.0372(8) Uani 1 1 d . . . H8 H 0.2901 0.3135 0.3053 0.045 Uiso 1 1 calc R . . H9 H 0.2339 0.1967 0.3175 0.045 Uiso 1 1 calc R . . C10 C 0.1890(2) 0.3251(4) 0.27343(11) 0.0404(9) Uani 1 1 d . . . H10 H 0.1440 0.2672 0.2720 0.048 Uiso 1 1 calc R . . H11 H 0.1796 0.4131 0.2872 0.048 Uiso 1 1 calc R . . C11 C 0.16739(19) 0.4445(4) 0.21297(10) 0.0331(7) Uani 1 1 d . . . H12 H 0.1329 0.4978 0.2254 0.040 Uiso 1 1 calc R . . C12 C 0.20835(16) 0.3818(3) 0.14807(9) 0.0232(6) Uani 1 1 d . . . C13 C 0.17036(18) 0.4683(4) 0.17200(10) 0.0283(7) Uani 1 1 d . . . C14 C 0.1259(2) 0.5774(4) 0.15509(12) 0.0365(8) Uani 1 1 d . . . H13 H 0.1003 0.6359 0.1713 0.044 Uiso 1 1 calc R . . C15 C 0.1187(2) 0.6013(4) 0.11605(12) 0.0355(8) Uani 1 1 d . . . H14 H 0.0906 0.6784 0.1055 0.043 Uiso 1 1 calc R . . C16 C 0.15304(19) 0.5108(4) 0.09179(11) 0.0320(7) Uani 1 1 d . . . H15 H 0.1474 0.5248 0.0646 0.038 Uiso 1 1 calc R . . C17 C 0.19521(17) 0.4012(3) 0.10756(10) 0.0252(6) Uani 1 1 d . . . C18 C 0.2243(2) 0.3237(4) 0.04572(10) 0.0381(8) Uani 1 1 d . . . H16 H 0.1732 0.3169 0.0346 0.057 Uiso 1 1 calc R . . H17 H 0.2534 0.2519 0.0342 0.057 Uiso 1 1 calc R . . H18 H 0.2434 0.4168 0.0404 0.057 Uiso 1 1 calc R . . O5 O 0.18739(12) 0.0373(3) 0.12386(6) 0.0280(5) Uani 1 1 d . . . O6 O 0.27947(12) 0.0146(2) 0.07368(6) 0.0260(5) Uani 1 1 d . . . O7 O 0.41583(12) -0.0163(2) 0.10120(6) 0.0261(5) Uani 1 1 d . . . O8 O 0.45203(12) -0.0207(3) 0.17419(6) 0.0282(5) Uani 1 1 d . . . N3 N 0.30630(17) -0.0568(4) -0.00257(8) 0.0387(7) Uani 1 1 d . . . N4 N 0.43595(16) -0.1437(3) 0.02684(8) 0.0330(6) Uani 1 1 d . . . C19 C 0.13734(19) 0.0412(5) 0.15314(10) 0.0381(8) Uani 1 1 d . . . H19 H 0.1015 0.1163 0.1472 0.057 Uiso 1 1 calc R . . H20 H 0.1646 0.0591 0.1784 0.057 Uiso 1 1 calc R . . H21 H 0.1119 -0.0489 0.1538 0.057 Uiso 1 1 calc R . . C20 C 0.15761(18) -0.0030(4) 0.08743(9) 0.0285(7) Uani 1 1 d . . . C21 C 0.08473(19) -0.0283(4) 0.07692(11) 0.0384(8) Uani 1 1 d . . . H22 H 0.0496 -0.0147 0.0948 0.046 Uiso 1 1 calc R . . C22 C 0.0633(2) -0.0746(5) 0.03932(13) 0.0523(11) Uani 1 1 d . . . H23 H 0.0132 -0.0943 0.0319 0.063 Uiso 1 1 calc R . . C23 C 0.1129(2) -0.0920(5) 0.01315(12) 0.0473(11) Uani 1 1 d . . . H24 H 0.0970 -0.1245 -0.0121 0.057 Uiso 1 1 calc R . . C24 C 0.1880(2) -0.0621(4) 0.02319(10) 0.0368(8) Uani 1 1 d . . . C25 C 0.21069(17) -0.0160(4) 0.06090(9) 0.0267(6) Uani 1 1 d . . . C26 C 0.2385(2) -0.0884(4) -0.00590(11) 0.0398(9) Uani 1 1 d . . . H25 H 0.2192 -0.1328 -0.0292 0.048 Uiso 1 1 calc R . . C27 C 0.3545(2) -0.0969(5) -0.03190(12) 0.0506(11) Uani 1 1 d . . . H26 H 0.3750 -0.0118 -0.0431 0.061 Uiso 1 1 calc R . . H27 H 0.3262 -0.1492 -0.0530 0.061 Uiso 1 1 calc R . . C28 C 0.4152(2) -0.1866(5) -0.01362(11) 0.0470(10) Uani 1 1 d . . . H28 H 0.3994 -0.2860 -0.0143 0.056 Uiso 1 1 calc R . . H29 H 0.4582 -0.1786 -0.0285 0.056 Uiso 1 1 calc R . . C29 C 0.48389(19) -0.2155(4) 0.04756(10) 0.0320(7) Uani 1 1 d . . . H30 H 0.5099 -0.2845 0.0347 0.038 Uiso 1 1 calc R . . C30 C 0.46774(17) -0.1083(3) 0.11322(10) 0.0243(6) Uani 1 1 d . . . C31 C 0.50214(17) -0.2008(3) 0.08911(10) 0.0275(7) Uani 1 1 d . . . C32 C 0.55567(19) -0.2955(4) 0.10599(11) 0.0329(7) Uani 1 1 d . . . H31 H 0.5788 -0.3582 0.0898 0.039 Uiso 1 1 calc R . . C33 C 0.57466(19) -0.2986(4) 0.14500(11) 0.0332(8) Uani 1 1 d . . . H32 H 0.6110 -0.3625 0.1556 0.040 Uiso 1 1 calc R . . C34 C 0.54066(18) -0.2078(3) 0.16938(10) 0.0301(7) Uani 1 1 d . . . H33 H 0.5534 -0.2105 0.1965 0.036 Uiso 1 1 calc R . . C35 C 0.48865(17) -0.1149(3) 0.15364(10) 0.0264(7) Uani 1 1 d . . . C36 C 0.4777(2) -0.0065(4) 0.21404(10) 0.0374(8) Uani 1 1 d . . . H34 H 0.4716 -0.0958 0.2273 0.056 Uiso 1 1 calc R . . H35 H 0.4496 0.0667 0.2257 0.056 Uiso 1 1 calc R . . H36 H 0.5296 0.0193 0.2166 0.056 Uiso 1 1 calc R . . O9 O 0.40877(12) 0.2491(3) 0.16619(7) 0.0306(5) Uani 1 1 d . . . O10 O 0.38616(12) 0.3453(2) 0.22200(7) 0.0287(5) Uani 1 1 d . . . C37 C 0.42267(18) 0.3351(3) 0.19298(10) 0.0267(6) Uani 1 1 d . . . C38 C 0.4862(2) 0.4326(4) 0.19019(11) 0.0392(9) Uani 1 1 d . . . H37 H 0.5317 0.3853 0.2000 0.059 Uiso 1 1 calc R . . H38 H 0.4797 0.5169 0.2056 0.059 Uiso 1 1 calc R . . H39 H 0.4886 0.4591 0.1631 0.059 Uiso 1 1 calc R . . O11 O 0.37395(14) 0.2645(3) 0.08982(7) 0.0341(5) Uani 1 1 d . . . O12 O 0.40929(15) 0.1960(3) 0.03365(7) 0.0370(6) Uani 1 1 d . . . C39 C 0.40591(19) 0.2855(4) 0.06047(10) 0.0309(7) Uani 1 1 d . . . C40 C 0.4427(3) 0.4241(4) 0.05642(13) 0.0498(11) Uani 1 1 d . . . H40 H 0.4268 0.4900 0.0755 0.075 Uiso 1 1 calc R . . H41 H 0.4294 0.4612 0.0304 0.075 Uiso 1 1 calc R . . H42 H 0.4958 0.4120 0.0607 0.075 Uiso 1 1 calc R . . B1 B -0.1461(2) 0.2197(4) 0.13343(10) 0.0251(7) Uani 1 1 d . . . C41 C -0.11958(17) 0.3072(3) 0.17313(9) 0.0257(6) Uani 1 1 d . . . C42 C -0.0746(2) 0.4256(4) 0.17492(12) 0.0425(9) Uani 1 1 d . . . H43 H -0.0571 0.4587 0.1518 0.051 Uiso 1 1 calc R . . C43 C -0.0545(3) 0.4972(5) 0.20916(13) 0.0510(11) Uani 1 1 d . . . H44 H -0.0235 0.5769 0.2090 0.061 Uiso 1 1 calc R . . C44 C -0.0790(2) 0.4535(5) 0.24341(12) 0.0438(9) Uani 1 1 d . . . H45 H -0.0659 0.5036 0.2667 0.053 Uiso 1 1 calc R . . C45 C -0.1229(2) 0.3353(4) 0.24330(11) 0.0392(8) Uani 1 1 d . . . H46 H -0.1395 0.3019 0.2666 0.047 Uiso 1 1 calc R . . C46 C -0.1424(2) 0.2664(4) 0.20870(10) 0.0330(7) Uani 1 1 d . . . H47 H -0.1731 0.1864 0.2091 0.040 Uiso 1 1 calc R . . C47 C -0.10806(17) 0.0625(4) 0.13408(10) 0.0279(7) Uani 1 1 d . . . C48 C -0.1183(2) -0.0231(4) 0.10135(12) 0.0403(9) Uani 1 1 d . . . H48 H -0.1454 0.0129 0.0788 0.048 Uiso 1 1 calc R . . C49 C -0.0903(2) -0.1591(4) 0.10032(13) 0.0465(10) Uani 1 1 d . . . H49 H -0.0982 -0.2137 0.0774 0.056 Uiso 1 1 calc R . . C50 C -0.0510(2) -0.2137(4) 0.13304(14) 0.0455(10) Uani 1 1 d . . . H50 H -0.0328 -0.3071 0.1331 0.055 Uiso 1 1 calc R . . C51 C -0.0387(2) -0.1319(4) 0.16513(13) 0.0427(9) Uani 1 1 d . . . H51 H -0.0107 -0.1681 0.1874 0.051 Uiso 1 1 calc R . . C52 C -0.06618(19) 0.0036(4) 0.16590(11) 0.0335(8) Uani 1 1 d . . . H52 H -0.0563 0.0580 0.1887 0.040 Uiso 1 1 calc R . . C53 C -0.12219(18) 0.3018(4) 0.09498(9) 0.0286(7) Uani 1 1 d . . . C54 C -0.0483(2) 0.3043(5) 0.08792(11) 0.0400(9) Uani 1 1 d . . . H53 H -0.0134 0.2578 0.1055 0.048 Uiso 1 1 calc R . . C55 C -0.0241(2) 0.3721(6) 0.05624(13) 0.0539(12) Uani 1 1 d . . . H54 H 0.0265 0.3719 0.0527 0.065 Uiso 1 1 calc R . . C56 C -0.0738(3) 0.4400(6) 0.02983(14) 0.0640(15) Uani 1 1 d . . . H55 H -0.0577 0.4872 0.0082 0.077 Uiso 1 1 calc R . . C57 C -0.1462(3) 0.4378(6) 0.03553(12) 0.0584(13) Uani 1 1 d . . . H56 H -0.1807 0.4835 0.0176 0.070 Uiso 1 1 calc R . . C58 C -0.1700(2) 0.3697(4) 0.06714(10) 0.0357(8) Uani 1 1 d . . . H57 H -0.2209 0.3692 0.0700 0.043 Uiso 1 1 calc R . . C59 C -0.23577(17) 0.2043(3) 0.13197(8) 0.0235(6) Uani 1 1 d . . . C60 C -0.27234(19) 0.0752(4) 0.13423(10) 0.0290(7) Uani 1 1 d . . . H58 H -0.2440 -0.0083 0.1364 0.035 Uiso 1 1 calc R . . C61 C -0.34804(19) 0.0643(4) 0.13343(10) 0.0329(7) Uani 1 1 d . . . H59 H -0.3699 -0.0253 0.1356 0.039 Uiso 1 1 calc R . . C62 C -0.39197(19) 0.1832(4) 0.12954(10) 0.0319(7) Uani 1 1 d . . . H60 H -0.4437 0.1761 0.1285 0.038 Uiso 1 1 calc R . . C63 C -0.35793(19) 0.3127(4) 0.12721(10) 0.0311(7) Uani 1 1 d . . . H61 H -0.3867 0.3956 0.1244 0.037 Uiso 1 1 calc R . . C64 C -0.28205(18) 0.3218(4) 0.12899(9) 0.0275(7) Uani 1 1 d . . . H62 H -0.2605 0.4122 0.1281 0.033 Uiso 1 1 calc R . . N5 N -0.3436(3) 0.5355(6) 0.03087(15) 0.0791(14) Uani 1 1 d . . . C65 C -0.3119(3) 0.6251(6) 0.04494(16) 0.0606(13) Uani 1 1 d . . . C66 C -0.2677(4) 0.7304(8) 0.0640(2) 0.097(2) Uani 1 1 d . . . H63 H -0.2963 0.7824 0.0815 0.145 Uiso 1 1 d . . . H64 H -0.2508 0.7948 0.0449 0.145 Uiso 1 1 d . . . H65 H -0.2254 0.6868 0.0788 0.145 Uiso 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 Er 0.02535(8) 0.02476(8) 0.01945(8) -0.00208(5) 0.00519(5) 0.00034(5) Zn1 0.02426(17) 0.02221(17) 0.02116(17) -0.00140(13) 0.00556(14) 0.00233(13) Zn2 0.02730(19) 0.0316(2) 0.02211(18) -0.00241(15) 0.00481(14) 0.00071(15) O1 0.0310(11) 0.0218(10) 0.0207(11) -0.0050(8) 0.0034(9) 0.0008(9) O2 0.0292(11) 0.0185(10) 0.0218(11) -0.0003(8) 0.0047(9) 0.0018(8) O3 0.0290(11) 0.0245(11) 0.0231(11) 0.0022(9) 0.0032(9) 0.0077(9) O4 0.0414(14) 0.0347(13) 0.0229(12) 0.0035(10) 0.0060(10) 0.0094(11) N1 0.0367(16) 0.0297(14) 0.0233(14) -0.0004(11) 0.0077(12) 0.0045(12) N2 0.0301(14) 0.0349(15) 0.0274(14) -0.0031(12) 0.0078(12) 0.0070(12) C1 0.0369(18) 0.0380(19) 0.0300(17) -0.0208(15) 0.0098(14) -0.0110(15) C2 0.0226(14) 0.0243(15) 0.0259(16) -0.0018(12) 0.0021(12) 0.0004(12) C3 0.0323(17) 0.0218(15) 0.0346(18) -0.0009(13) 0.0011(14) 0.0013(13) C4 0.0401(19) 0.0234(15) 0.0359(19) 0.0058(14) 0.0020(15) 0.0015(14) C5 0.0350(17) 0.0292(16) 0.0252(16) 0.0041(13) 0.0015(13) -0.0024(14) C6 0.0263(15) 0.0256(15) 0.0263(16) -0.0001(12) 0.0019(12) -0.0009(12) C7 0.0232(14) 0.0255(15) 0.0235(15) 0.0046(12) 0.0022(12) -0.0049(12) C8 0.0366(18) 0.0314(17) 0.0216(16) -0.0008(13) 0.0057(13) -0.0018(14) C9 0.052(2) 0.0375(19) 0.0231(17) -0.0049(14) 0.0115(15) 0.0039(17) C10 0.042(2) 0.047(2) 0.034(2) -0.0021(17) 0.0157(16) 0.0104(18) C11 0.0311(17) 0.0331(18) 0.0361(19) -0.0061(15) 0.0083(14) 0.0091(14) C12 0.0194(13) 0.0215(14) 0.0283(16) -0.0010(12) 0.0001(12) 0.0023(11) C13 0.0265(16) 0.0281(16) 0.0302(17) -0.0006(13) 0.0019(13) 0.0066(13) C14 0.0319(18) 0.0342(19) 0.044(2) -0.0016(16) 0.0041(16) 0.0105(15) C15 0.0304(18) 0.0300(18) 0.045(2) 0.0040(15) -0.0012(16) 0.0093(14) C16 0.0290(16) 0.0316(17) 0.0341(18) 0.0076(14) -0.0031(14) 0.0020(13) C17 0.0211(14) 0.0246(15) 0.0300(17) -0.0003(12) 0.0025(12) 0.0013(12) C18 0.048(2) 0.043(2) 0.0234(17) 0.0052(15) 0.0025(15) 0.0072(17) O5 0.0235(11) 0.0379(13) 0.0232(11) 0.0019(10) 0.0055(9) -0.0001(10) O6 0.0202(10) 0.0347(12) 0.0228(11) -0.0018(9) 0.0012(8) -0.0013(9) O7 0.0228(11) 0.0305(12) 0.0247(11) -0.0024(9) 0.0013(9) 0.0032(9) O8 0.0254(11) 0.0362(13) 0.0224(11) -0.0042(9) 0.0000(9) 0.0043(10) N3 0.0334(16) 0.059(2) 0.0233(15) -0.0068(14) 0.0012(12) 0.0063(15) N4 0.0319(15) 0.0407(16) 0.0267(15) -0.0103(12) 0.0044(12) -0.0002(13) C19 0.0274(17) 0.058(2) 0.0305(19) 0.0002(17) 0.0086(14) -0.0041(17) C20 0.0263(16) 0.0341(17) 0.0245(16) 0.0018(13) -0.0005(12) 0.0003(13) C21 0.0249(16) 0.055(2) 0.034(2) 0.0057(17) -0.0012(14) 0.0002(16) C22 0.0255(18) 0.083(3) 0.046(2) 0.000(2) -0.0077(17) -0.008(2) C23 0.035(2) 0.077(3) 0.0277(19) -0.0070(19) -0.0093(16) 0.000(2) C24 0.0306(18) 0.051(2) 0.0274(18) -0.0002(16) -0.0028(14) 0.0037(16) C25 0.0245(15) 0.0314(16) 0.0235(16) 0.0035(13) -0.0008(12) 0.0028(13) C26 0.038(2) 0.057(2) 0.0226(17) -0.0077(16) -0.0029(15) 0.0049(18) C27 0.048(2) 0.078(3) 0.026(2) -0.0129(19) 0.0081(18) 0.006(2) C28 0.046(2) 0.064(3) 0.032(2) -0.0197(19) 0.0069(17) 0.005(2) C29 0.0319(17) 0.0317(17) 0.0342(18) -0.0081(14) 0.0126(14) -0.0008(14) C30 0.0187(14) 0.0234(14) 0.0308(17) 0.0000(12) 0.0019(12) -0.0020(11) C31 0.0210(14) 0.0280(16) 0.0340(17) -0.0038(13) 0.0054(13) -0.0022(12) C32 0.0302(17) 0.0240(15) 0.046(2) -0.0030(14) 0.0099(15) 0.0020(13) C33 0.0296(17) 0.0254(16) 0.044(2) 0.0039(14) 0.0009(15) 0.0051(13) C34 0.0263(16) 0.0286(16) 0.0350(18) 0.0059(14) 0.0017(13) -0.0015(13) C35 0.0208(14) 0.0258(15) 0.0325(17) -0.0020(12) 0.0031(13) -0.0038(12) C36 0.0377(19) 0.045(2) 0.0275(18) -0.0019(15) -0.0036(15) 0.0029(16) O9 0.0260(11) 0.0340(13) 0.0323(13) -0.0043(10) 0.0052(10) -0.0002(10) O10 0.0282(12) 0.0287(12) 0.0299(12) -0.0027(10) 0.0066(10) -0.0043(9) C37 0.0266(15) 0.0248(15) 0.0285(16) 0.0010(13) 0.0019(13) -0.0005(12) C38 0.042(2) 0.043(2) 0.034(2) -0.0053(16) 0.0079(16) -0.0168(17) O11 0.0392(14) 0.0335(13) 0.0310(13) 0.0036(10) 0.0102(11) 0.0004(11) O12 0.0494(15) 0.0323(13) 0.0310(13) -0.0010(10) 0.0118(11) -0.0043(12) C39 0.0347(18) 0.0285(16) 0.0300(17) 0.0026(13) 0.0068(14) -0.0006(14) C40 0.062(3) 0.041(2) 0.048(3) -0.0065(19) 0.017(2) -0.016(2) B1 0.0240(16) 0.0283(17) 0.0225(17) 0.0025(14) 0.0004(13) -0.0010(14) C41 0.0255(15) 0.0271(15) 0.0240(15) 0.0043(12) -0.0002(12) -0.0005(12) C42 0.053(2) 0.041(2) 0.035(2) 0.0026(16) 0.0074(18) -0.0158(18) C43 0.059(3) 0.046(2) 0.047(2) -0.0058(19) 0.002(2) -0.024(2) C44 0.044(2) 0.049(2) 0.036(2) -0.0123(18) -0.0072(17) -0.0028(18) C45 0.041(2) 0.050(2) 0.0265(18) 0.0024(16) 0.0052(15) -0.0016(18) C46 0.0341(18) 0.0358(18) 0.0291(17) 0.0029(14) 0.0033(14) -0.0056(15) C47 0.0231(15) 0.0285(16) 0.0325(17) 0.0062(13) 0.0045(13) -0.0025(12) C48 0.0351(19) 0.042(2) 0.044(2) -0.0043(17) 0.0017(16) 0.0052(16) C49 0.041(2) 0.040(2) 0.059(3) -0.010(2) 0.010(2) 0.0006(18) C50 0.036(2) 0.0318(19) 0.071(3) 0.0076(19) 0.015(2) 0.0075(16) C51 0.0329(19) 0.039(2) 0.057(3) 0.0151(19) 0.0059(18) 0.0088(16) C52 0.0269(16) 0.0395(19) 0.0343(19) 0.0108(15) 0.0040(14) 0.0036(14) C53 0.0303(16) 0.0324(17) 0.0228(16) 0.0029(13) 0.0014(13) -0.0056(13) C54 0.0265(17) 0.057(2) 0.036(2) 0.0095(18) 0.0005(15) -0.0055(17) C55 0.030(2) 0.091(4) 0.040(2) 0.015(2) 0.0041(17) -0.016(2) C56 0.046(3) 0.102(4) 0.046(3) 0.035(3) 0.012(2) -0.012(3) C57 0.045(2) 0.094(4) 0.037(2) 0.035(2) 0.0057(19) 0.005(2) C58 0.0303(17) 0.050(2) 0.0273(18) 0.0139(16) 0.0051(14) -0.0002(16) C59 0.0276(15) 0.0263(15) 0.0169(14) 0.0019(11) 0.0033(11) 0.0001(12) C60 0.0306(17) 0.0267(16) 0.0297(17) 0.0052(13) 0.0030(13) 0.0005(13) C61 0.0321(17) 0.0349(18) 0.0324(18) 0.0015(15) 0.0067(14) -0.0066(14) C62 0.0263(16) 0.042(2) 0.0278(17) -0.0014(14) 0.0053(13) -0.0006(14) C63 0.0339(17) 0.0322(17) 0.0279(17) -0.0014(14) 0.0064(14) 0.0048(14) C64 0.0322(16) 0.0272(16) 0.0234(16) -0.0003(12) 0.0042(13) -0.0010(13) N5 0.085(4) 0.080(4) 0.072(3) 0.004(3) 0.005(3) 0.007(3) C65 0.058(3) 0.062(3) 0.066(3) -0.014(3) 0.025(3) -0.007(2) C66 0.085(5) 0.094(5) 0.117(6) -0.029(4) 0.038(4) -0.034(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er O6 2.280(2) . ? Er O2 2.295(2) . ? Er O9 2.296(2) . ? Er O11 2.328(2) . ? Er O3 2.366(2) . ? Er O7 2.394(2) . ? Er O5 2.592(2) . ? Er O1 2.607(2) . ? Er Zn2 3.3374(5) . ? Er Zn1 3.3481(5) . ? Zn1 O10 1.988(2) . ? Zn1 O2 2.016(2) . ? Zn1 N2 2.034(3) . ? Zn1 O3 2.055(2) . ? Zn1 N1 2.056(3) . ? Zn2 O12 1.975(3) . ? Zn2 N4 2.029(3) . ? Zn2 O6 2.033(2) . ? Zn2 O7 2.041(2) . ? Zn2 N3 2.049(3) . ? O1 C2 1.386(4) . ? O1 C1 1.443(4) . ? O2 C7 1.315(4) . ? O3 C12 1.325(3) . ? O4 C17 1.371(4) . ? O4 C18 1.428(4) . ? N1 C8 1.280(4) . ? N1 C9 1.459(4) . ? N2 C11 1.281(5) . ? N2 C10 1.482(5) . ? C2 C3 1.381(4) . ? C2 C7 1.431(4) . ? C3 C4 1.400(5) . ? C4 C5 1.362(5) . ? C5 C6 1.410(4) . ? C6 C7 1.410(4) . ? C6 C8 1.454(5) . ? C9 C10 1.509(5) . ? C11 C13 1.450(5) . ? C12 C13 1.407(4) . ? C12 C17 1.417(5) . ? C13 C14 1.413(5) . ? C14 C15 1.370(5) . ? C15 C16 1.401(5) . ? C16 C17 1.381(4) . ? O5 C20 1.383(4) . ? O5 C19 1.441(4) . ? O6 C25 1.328(4) . ? O7 C30 1.331(4) . ? O8 C35 1.367(4) . ? O8 C36 1.424(4) . ? N3 C26 1.275(5) . ? N3 C27 1.468(5) . ? N4 C29 1.278(5) . ? N4 C28 1.478(5) . ? C20 C21 1.373(5) . ? C20 C25 1.415(5) . ? C21 C22 1.398(6) . ? C22 C23 1.362(6) . ? C23 C24 1.417(5) . ? C24 C25 1.406(5) . ? C24 C26 1.463(5) . ? C27 C28 1.494(6) . ? C29 C31 1.457(5) . ? C30 C31 1.410(4) . ? C30 C35 1.420(5) . ? C31 C32 1.417(5) . ? C32 C33 1.367(5) . ? C33 C34 1.402(5) . ? C34 C35 1.375(5) . ? O9 C37 1.248(4) . ? O10 C37 1.271(4) . ? C37 C38 1.502(5) . ? O11 C39 1.245(4) . ? O12 C39 1.271(4) . ? C39 C40 1.497(5) . ? B1 C41 1.644(5) . ? B1 C53 1.648(5) . ? B1 C59 1.648(5) . ? B1 C47 1.653(5) . ? C41 C42 1.397(5) . ? C41 C46 1.401(5) . ? C42 C43 1.390(6) . ? C43 C44 1.380(6) . ? C44 C45 1.386(6) . ? C45 C46 1.385(5) . ? C47 C48 1.397(5) . ? C47 C52 1.400(5) . ? C48 C49 1.397(6) . ? C49 C50 1.386(6) . ? C50 C51 1.362(6) . ? C51 C52 1.388(5) . ? C53 C58 1.398(5) . ? C53 C54 1.404(5) . ? C54 C55 1.389(5) . ? C55 C56 1.388(7) . ? C56 C57 1.364(6) . ? C57 C58 1.386(5) . ? C59 C64 1.404(4) . ? C59 C60 1.408(4) . ? C60 C61 1.392(5) . ? C61 C62 1.390(5) . ? C62 C63 1.391(5) . ? C63 C64 1.392(5) . ? N5 C65 1.118(7) . ? C65 C66 1.413(8) . ? 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 O6 Er O2 130.48(8) . . ? O6 Er O9 148.92(8) . . ? O2 Er O9 79.93(8) . . ? O6 Er O11 80.17(8) . . ? O2 Er O11 148.88(8) . . ? O9 Er O11 70.62(9) . . ? O6 Er O3 119.27(8) . . ? O2 Er O3 67.32(7) . . ? O9 Er O3 74.55(8) . . ? O11 Er O3 94.62(8) . . ? O6 Er O7 67.69(8) . . ? O2 Er O7 119.73(7) . . ? O9 Er O7 93.07(8) . . ? O11 Er O7 72.80(8) . . ? O3 Er O7 164.93(8) . . ? O6 Er O5 63.04(7) . . ? O2 Er O5 76.60(7) . . ? O9 Er O5 143.56(8) . . ? O11 Er O5 122.77(8) . . ? O3 Er O5 70.84(8) . . ? O7 Er O5 122.77(7) . . ? O6 Er O1 77.87(7) . . ? O2 Er O1 62.42(7) . . ? O9 Er O1 120.22(8) . . ? O11 Er O1 142.82(8) . . ? O3 Er O1 122.29(7) . . ? O7 Er O1 71.23(7) . . ? O5 Er O1 71.65(7) . . ? O6 Er Zn2 36.68(5) . . ? O2 Er Zn2 149.23(5) . . ? O9 Er Zn2 114.48(6) . . ? O11 Er Zn2 57.90(6) . . ? O3 Er Zn2 141.05(5) . . ? O7 Er Zn2 37.34(5) . . ? O5 Er Zn2 99.69(5) . . ? O1 Er Zn2 87.23(5) . . ? O6 Er Zn1 148.65(5) . . ? O2 Er Zn1 36.13(5) . . ? O9 Er Zn1 59.00(6) . . ? O11 Er Zn1 115.49(6) . . ? O3 Er Zn1 37.41(5) . . ? O7 Er Zn1 141.19(5) . . ? O5 Er Zn1 86.10(5) . . ? O1 Er Zn1 98.54(5) . . ? Zn2 Er Zn1 172.913(10) . . ? O10 Zn1 O2 111.40(9) . . ? O10 Zn1 N2 113.05(11) . . ? O2 Zn1 N2 135.39(11) . . ? O10 Zn1 O3 100.63(9) . . ? O2 Zn1 O3 78.78(9) . . ? N2 Zn1 O3 89.55(10) . . ? O10 Zn1 N1 107.80(11) . . ? O2 Zn1 N1 89.08(10) . . ? N2 Zn1 N1 81.11(12) . . ? O3 Zn1 N1 151.51(11) . . ? O10 Zn1 Er 91.63(7) . . ? O2 Zn1 Er 42.15(6) . . ? N2 Zn1 Er 132.13(8) . . ? O3 Zn1 Er 44.38(6) . . ? N1 Zn1 Er 131.11(8) . . ? O12 Zn2 N4 110.35(12) . . ? O12 Zn2 O6 113.95(10) . . ? N4 Zn2 O6 135.68(11) . . ? O12 Zn2 O7 100.78(10) . . ? N4 Zn2 O7 91.49(11) . . ? O6 Zn2 O7 79.52(9) . . ? O12 Zn2 N3 107.17(13) . . ? N4 Zn2 N3 80.25(12) . . ? O6 Zn2 N3 87.80(11) . . ? O7 Zn2 N3 152.01(12) . . ? O12 Zn2 Er 93.40(7) . . ? N4 Zn2 Er 134.83(9) . . ? O6 Zn2 Er 42.08(6) . . ? O7 Zn2 Er 45.36(6) . . ? N3 Zn2 Er 129.65(9) . . ? C2 O1 C1 114.9(3) . . ? C2 O1 Er 116.52(17) . . ? C1 O1 Er 128.3(2) . . ? C7 O2 Zn1 127.7(2) . . ? C7 O2 Er 129.36(19) . . ? Zn1 O2 Er 101.72(9) . . ? C12 O3 Zn1 125.5(2) . . ? C12 O3 Er 136.2(2) . . ? Zn1 O3 Er 98.21(8) . . ? C17 O4 C18 116.9(3) . . ? C8 N1 C9 122.0(3) . . ? C8 N1 Zn1 127.5(2) . . ? C9 N1 Zn1 109.3(2) . . ? C11 N2 C10 119.5(3) . . ? C11 N2 Zn1 126.6(2) . . ? C10 N2 Zn1 113.8(2) . . ? C3 C2 O1 125.8(3) . . ? C3 C2 C7 121.4(3) . . ? O1 C2 C7 112.8(3) . . ? C2 C3 C4 119.5(3) . . ? C5 C4 C3 120.4(3) . . ? C4 C5 C6 121.3(3) . . ? C5 C6 C7 119.7(3) . . ? C5 C6 C8 117.5(3) . . ? C7 C6 C8 122.5(3) . . ? O2 C7 C6 126.2(3) . . ? O2 C7 C2 116.4(3) . . ? C6 C7 C2 117.5(3) . . ? N1 C8 C6 125.7(3) . . ? N1 C9 C10 108.9(3) . . ? N2 C10 C9 109.8(3) . . ? N2 C11 C13 125.7(3) . . ? O3 C12 C13 125.1(3) . . ? O3 C12 C17 117.0(3) . . ? C13 C12 C17 117.9(3) . . ? C12 C13 C14 119.1(3) . . ? C12 C13 C11 124.1(3) . . ? C14 C13 C11 116.5(3) . . ? C15 C14 C13 121.9(3) . . ? C14 C15 C16 119.4(3) . . ? C17 C16 C15 119.7(3) . . ? O4 C17 C16 124.6(3) . . ? O4 C17 C12 113.7(3) . . ? C16 C17 C12 121.7(3) . . ? C20 O5 C19 115.7(3) . . ? C20 O5 Er 117.18(18) . . ? C19 O5 Er 127.0(2) . . ? C25 O6 Zn2 129.7(2) . . ? C25 O6 Er 128.8(2) . . ? Zn2 O6 Er 101.24(9) . . ? C30 O7 Zn2 125.6(2) . . ? C30 O7 Er 134.6(2) . . ? Zn2 O7 Er 97.30(8) . . ? C35 O8 C36 116.1(3) . . ? C26 N3 C27 121.9(3) . . ? C26 N3 Zn2 128.8(3) . . ? C27 N3 Zn2 107.8(2) . . ? C29 N4 C28 119.0(3) . . ? C29 N4 Zn2 126.7(2) . . ? C28 N4 Zn2 113.6(2) . . ? C21 C20 O5 125.2(3) . . ? C21 C20 C25 122.0(3) . . ? O5 C20 C25 112.8(3) . . ? C20 C21 C22 118.6(4) . . ? C23 C22 C21 121.3(4) . . ? C22 C23 C24 120.8(4) . . ? C25 C24 C23 118.8(3) . . ? C25 C24 C26 123.4(3) . . ? C23 C24 C26 117.7(3) . . ? O6 C25 C24 124.2(3) . . ? O6 C25 C20 117.2(3) . . ? C24 C25 C20 118.5(3) . . ? N3 C26 C24 125.4(3) . . ? N3 C27 C28 109.3(3) . . ? N4 C28 C27 110.8(3) . . ? N4 C29 C31 125.7(3) . . ? O7 C30 C31 125.1(3) . . ? O7 C30 C35 116.9(3) . . ? C31 C30 C35 117.9(3) . . ? C30 C31 C32 119.1(3) . . ? C30 C31 C29 125.3(3) . . ? C32 C31 C29 115.4(3) . . ? C33 C32 C31 121.4(3) . . ? C32 C33 C34 120.2(3) . . ? C35 C34 C33 119.4(3) . . ? O8 C35 C34 125.0(3) . . ? O8 C35 C30 113.0(3) . . ? C34 C35 C30 122.0(3) . . ? C37 O9 Er 148.3(2) . . ? C37 O10 Zn1 115.0(2) . . ? O9 C37 O10 124.0(3) . . ? O9 C37 C38 117.3(3) . . ? O10 C37 C38 118.7(3) . . ? C39 O11 Er 149.6(2) . . ? C39 O12 Zn2 114.1(2) . . ? O11 C39 O12 123.8(3) . . ? O11 C39 C40 118.3(3) . . ? O12 C39 C40 117.9(3) . . ? C41 B1 C53 111.1(3) . . ? C41 B1 C59 106.3(3) . . ? C53 B1 C59 111.5(3) . . ? C41 B1 C47 111.1(3) . . ? C53 B1 C47 107.1(3) . . ? C59 B1 C47 109.9(3) . . ? C42 C41 C46 114.4(3) . . ? C42 C41 B1 124.8(3) . . ? C46 C41 B1 120.7(3) . . ? C43 C42 C41 122.7(4) . . ? C44 C43 C42 120.7(4) . . ? C43 C44 C45 119.0(4) . . ? C46 C45 C44 119.1(3) . . ? C45 C46 C41 124.2(3) . . ? C48 C47 C52 115.3(3) . . ? C48 C47 B1 119.8(3) . . ? C52 C47 B1 124.9(3) . . ? C49 C48 C47 122.9(4) . . ? C50 C49 C48 119.3(4) . . ? C51 C50 C49 119.1(4) . . ? C50 C51 C52 121.3(4) . . ? C51 C52 C47 122.0(4) . . ? C58 C53 C54 114.9(3) . . ? C58 C53 B1 125.5(3) . . ? C54 C53 B1 119.6(3) . . ? C55 C54 C53 122.7(4) . . ? C56 C55 C54 120.0(4) . . ? C57 C56 C55 118.8(4) . . ? C56 C57 C58 120.9(4) . . ? C57 C58 C53 122.7(4) . . ? C64 C59 C60 114.4(3) . . ? C64 C59 B1 121.8(3) . . ? C60 C59 B1 123.8(3) . . ? C61 C60 C59 123.1(3) . . ? C62 C61 C60 120.6(3) . . ? C61 C62 C63 118.0(3) . . ? C62 C63 C64 120.5(3) . . ? C63 C64 C59 123.4(3) . . ? N5 C65 C66 175.4(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.343 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.126 # Attachment '- 5.cif' data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 889490' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H65 B N5 O12 Tm Zn2' _chemical_formula_weight 1430.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.3746(18) _cell_length_b 9.5525(9) _cell_length_c 34.799(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.795(2) _cell_angle_gamma 90.00 _cell_volume 6076.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 27962 _cell_measurement_theta_min 12.4982 _cell_measurement_theta_max 47.2653 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 2.298 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7243 _exptl_absorpt_correction_T_max 0.8557 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; Absorption correction was performed using REQAB (Rigaku, 1998) program. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 124815 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17599 _reflns_number_gt 16741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear ver. 1.4' _computing_cell_refinement 'CrystalClear ver. 1.4' _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics OrtepIII _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0415P)^2^+6.6851P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17599 _refine_ls_number_parameters 790 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm Tm 0.324397(4) 0.108780(9) 0.131729(2) 0.01978(3) Uani 1 1 d . . . Zn1 Zn 0.291700(12) 0.24240(2) 0.217031(6) 0.01988(5) Uani 1 1 d . . . Zn2 Zn 0.371406(12) 0.01018(3) 0.045755(6) 0.02206(5) Uani 1 1 d . . . O1 O 0.31514(8) -0.15667(15) 0.14836(4) 0.0229(3) Uani 1 1 d . . . O2 O 0.30175(8) 0.05188(15) 0.19318(4) 0.0207(3) Uani 1 1 d . . . O3 O 0.25561(8) 0.28191(16) 0.16027(4) 0.0230(3) Uani 1 1 d . . . O4 O 0.22735(9) 0.30217(18) 0.08613(4) 0.0299(3) Uani 1 1 d . . . N1 N 0.28146(10) 0.1470(2) 0.26921(5) 0.0264(3) Uani 1 1 d . . . N2 N 0.20722(10) 0.3574(2) 0.23380(5) 0.0275(4) Uani 1 1 d . . . C1 C 0.31441(13) -0.2744(3) 0.12244(7) 0.0305(4) Uani 1 1 d . . . H1 H 0.3594 -0.3289 0.1282 0.046 Uiso 1 1 calc R . . H2 H 0.3114 -0.2406 0.0957 0.046 Uiso 1 1 calc R . . H3 H 0.2720 -0.3336 0.1258 0.046 Uiso 1 1 calc R . . C2 C 0.31724(10) -0.1896(2) 0.18711(6) 0.0216(3) Uani 1 1 d . . . C3 C 0.32807(12) -0.3219(2) 0.20279(6) 0.0268(4) Uani 1 1 d . . . H4 H 0.3351 -0.3996 0.1866 0.032 Uiso 1 1 calc R . . C4 C 0.32859(13) -0.3407(2) 0.24272(7) 0.0294(4) Uani 1 1 d . . . H5 H 0.3375 -0.4309 0.2537 0.035 Uiso 1 1 calc R . . C5 C 0.31623(12) -0.2294(2) 0.26607(6) 0.0273(4) Uani 1 1 d . . . H6 H 0.3150 -0.2442 0.2930 0.033 Uiso 1 1 calc R . . C6 C 0.30527(11) -0.0932(2) 0.25084(6) 0.0230(4) Uani 1 1 d . . . C7 C 0.30793(10) -0.0712(2) 0.21085(6) 0.0209(3) Uani 1 1 d . . . C8 C 0.28493(12) 0.0162(2) 0.27704(6) 0.0259(4) Uani 1 1 d . . . H7 H 0.2733 -0.0120 0.3019 0.031 Uiso 1 1 calc R . . C9 C 0.25220(14) 0.2481(3) 0.29539(6) 0.0331(5) Uani 1 1 d . . . H8 H 0.2909 0.3152 0.3051 0.040 Uiso 1 1 calc R . . H9 H 0.2351 0.1987 0.3178 0.040 Uiso 1 1 calc R . . C10 C 0.18888(14) 0.3257(3) 0.27336(7) 0.0356(5) Uani 1 1 d . . . H10 H 0.1442 0.2674 0.2720 0.043 Uiso 1 1 calc R . . H11 H 0.1793 0.4138 0.2869 0.043 Uiso 1 1 calc R . . C11 C 0.16804(12) 0.4446(3) 0.21287(7) 0.0301(4) Uani 1 1 d . . . H12 H 0.1340 0.4988 0.2253 0.036 Uiso 1 1 calc R . . C12 C 0.20901(10) 0.3816(2) 0.14780(6) 0.0210(3) Uani 1 1 d . . . C13 C 0.17074(11) 0.4685(2) 0.17194(6) 0.0257(4) Uani 1 1 d . . . C14 C 0.12619(13) 0.5780(3) 0.15522(7) 0.0323(5) Uani 1 1 d . . . H13 H 0.1007 0.6364 0.1714 0.039 Uiso 1 1 calc R . . C15 C 0.11906(13) 0.6019(2) 0.11610(8) 0.0333(5) Uani 1 1 d . . . H14 H 0.0913 0.6794 0.1056 0.040 Uiso 1 1 calc R . . C16 C 0.15293(12) 0.5113(2) 0.09167(7) 0.0281(4) Uani 1 1 d . . . H15 H 0.1470 0.5256 0.0645 0.034 Uiso 1 1 calc R . . C17 C 0.19489(11) 0.4014(2) 0.10717(6) 0.0234(4) Uani 1 1 d . . . C18 C 0.22402(15) 0.3248(3) 0.04536(7) 0.0362(5) Uani 1 1 d . . . H16 H 0.1730 0.3211 0.0341 0.054 Uiso 1 1 calc R . . H17 H 0.2522 0.2520 0.0337 0.054 Uiso 1 1 calc R . . H18 H 0.2446 0.4169 0.0404 0.054 Uiso 1 1 calc R . . O5 O 0.18808(8) 0.03744(17) 0.12426(4) 0.0255(3) Uani 1 1 d . . . O6 O 0.27997(7) 0.01552(16) 0.07418(4) 0.0228(3) Uani 1 1 d . . . O7 O 0.41612(7) -0.01576(16) 0.10145(4) 0.0221(3) Uani 1 1 d . . . O8 O 0.45221(8) -0.02125(17) 0.17454(4) 0.0260(3) Uani 1 1 d . . . N3 N 0.30668(11) -0.0532(2) -0.00250(5) 0.0327(4) Uani 1 1 d . . . N4 N 0.43596(10) -0.1431(2) 0.02685(5) 0.0278(4) Uani 1 1 d . . . C19 C 0.13797(12) 0.0429(3) 0.15350(7) 0.0345(5) Uani 1 1 d . . . H19 H 0.1012 0.1156 0.1469 0.052 Uiso 1 1 calc R . . H20 H 0.1649 0.0647 0.1785 0.052 Uiso 1 1 calc R . . H21 H 0.1137 -0.0480 0.1550 0.052 Uiso 1 1 calc R . . C20 C 0.15830(11) -0.0016(2) 0.08778(6) 0.0256(4) Uani 1 1 d . . . C21 C 0.08519(12) -0.0270(3) 0.07721(7) 0.0353(5) Uani 1 1 d . . . H22 H 0.0502 -0.0146 0.0953 0.042 Uiso 1 1 calc R . . C22 C 0.06314(13) -0.0717(4) 0.03934(8) 0.0463(7) Uani 1 1 d . . . H23 H 0.0130 -0.0904 0.0318 0.056 Uiso 1 1 calc R . . C23 C 0.11386(14) -0.0886(4) 0.01309(8) 0.0433(6) Uani 1 1 d . . . H24 H 0.0982 -0.1203 -0.0123 0.052 Uiso 1 1 calc R . . C24 C 0.18853(12) -0.0596(3) 0.02332(6) 0.0314(5) Uani 1 1 d . . . C25 C 0.21129(11) -0.0142(2) 0.06116(6) 0.0240(4) Uani 1 1 d . . . C26 C 0.23886(13) -0.0849(3) -0.00599(7) 0.0345(5) Uani 1 1 d . . . H25 H 0.2195 -0.1282 -0.0294 0.041 Uiso 1 1 calc R . . C27 C 0.35491(15) -0.0923(3) -0.03205(7) 0.0393(6) Uani 1 1 d . . . H26 H 0.3765 -0.0072 -0.0426 0.047 Uiso 1 1 calc R . . H27 H 0.3266 -0.1421 -0.0536 0.047 Uiso 1 1 calc R . . C28 C 0.41499(14) -0.1864(3) -0.01345(7) 0.0385(6) Uani 1 1 d . . . H28 H 0.3977 -0.2845 -0.0140 0.046 Uiso 1 1 calc R . . H29 H 0.4582 -0.1812 -0.0283 0.046 Uiso 1 1 calc R . . C29 C 0.48377(11) -0.2146(2) 0.04762(6) 0.0271(4) Uani 1 1 d . . . H30 H 0.5096 -0.2838 0.0348 0.033 Uiso 1 1 calc R . . C30 C 0.46752(10) -0.1071(2) 0.11340(6) 0.0206(3) Uani 1 1 d . . . C31 C 0.50224(10) -0.1998(2) 0.08911(6) 0.0241(4) Uani 1 1 d . . . C32 C 0.55557(11) -0.2950(2) 0.10603(7) 0.0287(4) Uani 1 1 d . . . H31 H 0.5784 -0.3578 0.0898 0.034 Uiso 1 1 calc R . . C33 C 0.57496(12) -0.2990(2) 0.14511(7) 0.0299(4) Uani 1 1 d . . . H32 H 0.6112 -0.3631 0.1556 0.036 Uiso 1 1 calc R . . C34 C 0.54110(11) -0.2079(2) 0.16948(6) 0.0264(4) Uani 1 1 d . . . H33 H 0.5542 -0.2104 0.1966 0.032 Uiso 1 1 calc R . . C35 C 0.48875(10) -0.1147(2) 0.15392(6) 0.0219(4) Uani 1 1 d . . . C36 C 0.47778(13) -0.0070(3) 0.21450(6) 0.0328(5) Uani 1 1 d . . . H34 H 0.4732 -0.0970 0.2276 0.049 Uiso 1 1 calc R . . H35 H 0.4485 0.0637 0.2263 0.049 Uiso 1 1 calc R . . H36 H 0.5292 0.0220 0.2170 0.049 Uiso 1 1 calc R . . O9 O 0.40851(8) 0.24779(17) 0.16623(5) 0.0277(3) Uani 1 1 d . . . O10 O 0.38575(8) 0.34626(17) 0.22176(4) 0.0256(3) Uani 1 1 d . . . C37 C 0.42224(11) 0.3346(2) 0.19259(6) 0.0229(4) Uani 1 1 d . . . C38 C 0.48627(14) 0.4312(3) 0.18967(7) 0.0355(5) Uani 1 1 d . . . H37 H 0.5317 0.3827 0.1989 0.053 Uiso 1 1 calc R . . H38 H 0.4808 0.5145 0.2056 0.053 Uiso 1 1 calc R . . H39 H 0.4880 0.4593 0.1627 0.053 Uiso 1 1 calc R . . O11 O 0.37308(9) 0.26452(17) 0.09014(5) 0.0298(3) Uani 1 1 d . . . O12 O 0.41024(10) 0.19701(18) 0.03400(5) 0.0320(3) Uani 1 1 d . . . C39 C 0.40560(12) 0.2856(2) 0.06099(6) 0.0271(4) Uani 1 1 d . . . C40 C 0.44237(18) 0.4259(3) 0.05699(9) 0.0434(6) Uani 1 1 d . . . H40 H 0.4242 0.4928 0.0752 0.065 Uiso 1 1 calc R . . H41 H 0.4313 0.4606 0.0305 0.065 Uiso 1 1 calc R . . H42 H 0.4954 0.4153 0.0627 0.065 Uiso 1 1 calc R . . B1 B -0.14608(12) 0.2195(3) 0.13341(6) 0.0227(4) Uani 1 1 d . . . C41 C -0.11967(11) 0.3077(2) 0.17304(6) 0.0251(4) Uani 1 1 d . . . C42 C -0.07504(16) 0.4263(3) 0.17449(7) 0.0396(6) Uani 1 1 d . . . H43 H -0.0574 0.4587 0.1513 0.048 Uiso 1 1 calc R . . C43 C -0.05533(18) 0.4992(3) 0.20893(9) 0.0479(7) Uani 1 1 d . . . H44 H -0.0252 0.5799 0.2086 0.057 Uiso 1 1 calc R . . C44 C -0.07902(16) 0.4553(3) 0.24320(8) 0.0412(6) Uani 1 1 d . . . H45 H -0.0657 0.5052 0.2665 0.049 Uiso 1 1 calc R . . C45 C -0.12275(14) 0.3369(3) 0.24319(7) 0.0362(5) Uani 1 1 d . . . H46 H -0.1391 0.3041 0.2666 0.043 Uiso 1 1 calc R . . C46 C -0.14267(13) 0.2663(3) 0.20873(6) 0.0298(4) Uani 1 1 d . . . H47 H -0.1733 0.1863 0.2093 0.036 Uiso 1 1 calc R . . C47 C -0.10789(11) 0.0630(2) 0.13439(6) 0.0262(4) Uani 1 1 d . . . C48 C -0.11766(13) -0.0236(3) 0.10165(7) 0.0357(5) Uani 1 1 d . . . H48 H -0.1447 0.0119 0.0790 0.043 Uiso 1 1 calc R . . C49 C -0.08963(14) -0.1592(3) 0.10070(9) 0.0409(6) Uani 1 1 d . . . H49 H -0.0976 -0.2137 0.0778 0.049 Uiso 1 1 calc R . . C50 C -0.05004(14) -0.2138(3) 0.13343(9) 0.0414(6) Uani 1 1 d . . . H50 H -0.0317 -0.3068 0.1334 0.050 Uiso 1 1 calc R . . C51 C -0.03770(14) -0.1307(3) 0.16592(9) 0.0385(5) Uani 1 1 d . . . H51 H -0.0100 -0.1664 0.1883 0.046 Uiso 1 1 calc R . . C52 C -0.06559(12) 0.0052(3) 0.16616(7) 0.0295(4) Uani 1 1 d . . . H52 H -0.0554 0.0606 0.1887 0.035 Uiso 1 1 calc R . . C53 C -0.12220(11) 0.3000(2) 0.09476(6) 0.0253(4) Uani 1 1 d . . . C54 C -0.04796(13) 0.3043(3) 0.08762(7) 0.0375(5) Uani 1 1 d . . . H53 H -0.0128 0.2603 0.1056 0.045 Uiso 1 1 calc R . . C55 C -0.02395(15) 0.3697(4) 0.05574(9) 0.0508(8) Uani 1 1 d . . . H54 H 0.0266 0.3698 0.0522 0.061 Uiso 1 1 calc R . . C56 C -0.07365(18) 0.4350(5) 0.02897(9) 0.0620(10) Uani 1 1 d . . . H55 H -0.0576 0.4811 0.0072 0.074 Uiso 1 1 calc R . . C57 C -0.14670(16) 0.4318(4) 0.03453(9) 0.0557(9) Uani 1 1 d . . . H56 H -0.1815 0.4752 0.0162 0.067 Uiso 1 1 calc R . . C58 C -0.16999(13) 0.3657(3) 0.06668(7) 0.0347(5) Uani 1 1 d . . . H57 H -0.2208 0.3652 0.0697 0.042 Uiso 1 1 calc R . . C59 C -0.23583(11) 0.2034(2) 0.13189(5) 0.0218(3) Uani 1 1 d . . . C60 C -0.27207(12) 0.0748(2) 0.13458(6) 0.0264(4) Uani 1 1 d . . . H58 H -0.2437 -0.0084 0.1371 0.032 Uiso 1 1 calc R . . C61 C -0.34781(12) 0.0638(3) 0.13374(7) 0.0299(4) Uani 1 1 d . . . H59 H -0.3697 -0.0256 0.1360 0.036 Uiso 1 1 calc R . . C62 C -0.39175(12) 0.1826(3) 0.12966(6) 0.0297(4) Uani 1 1 d . . . H60 H -0.4435 0.1754 0.1286 0.036 Uiso 1 1 calc R . . C63 C -0.35811(12) 0.3122(2) 0.12715(6) 0.0289(4) Uani 1 1 d . . . H61 H -0.3870 0.3947 0.1243 0.035 Uiso 1 1 calc R . . C64 C -0.28195(11) 0.3212(2) 0.12879(6) 0.0247(4) Uani 1 1 d . . . H62 H -0.2603 0.4113 0.1278 0.030 Uiso 1 1 calc R . . N5 N -0.34412(19) 0.5354(4) 0.03088(10) 0.0680(8) Uani 1 1 d . . . C65 C -0.3104(2) 0.6222(4) 0.04509(11) 0.0553(8) Uani 1 1 d . . . C66 C -0.2660(3) 0.7262(6) 0.06470(17) 0.0891(15) Uani 1 1 d . . . H63 H -0.2963 0.7824 0.0815 0.134 Uiso 1 1 d . . . H64 H -0.2508 0.7948 0.0449 0.134 Uiso 1 1 d . . . H65 H -0.2254 0.6868 0.0788 0.134 Uiso 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 Tm 0.02160(5) 0.02131(5) 0.01677(4) -0.00256(3) 0.00357(3) -0.00016(3) Zn1 0.02173(10) 0.01916(10) 0.01919(10) -0.00164(8) 0.00427(8) 0.00193(8) Zn2 0.02268(10) 0.02522(12) 0.01855(10) -0.00281(8) 0.00348(8) 0.00047(8) O1 0.0298(7) 0.0194(7) 0.0194(6) -0.0037(5) 0.0019(5) 0.0006(5) O2 0.0257(6) 0.0179(6) 0.0190(6) 0.0003(5) 0.0036(5) 0.0020(5) O3 0.0249(6) 0.0224(7) 0.0219(6) 0.0013(5) 0.0034(5) 0.0071(5) O4 0.0395(8) 0.0294(8) 0.0213(7) 0.0029(6) 0.0048(6) 0.0103(7) N1 0.0332(9) 0.0264(9) 0.0202(8) -0.0025(7) 0.0061(6) 0.0020(7) N2 0.0272(8) 0.0307(9) 0.0256(8) -0.0017(7) 0.0077(7) 0.0050(7) C1 0.0357(11) 0.0296(11) 0.0267(10) -0.0148(9) 0.0065(8) -0.0069(9) C2 0.0219(8) 0.0218(9) 0.0210(8) -0.0007(7) 0.0017(6) 0.0001(7) C3 0.0307(10) 0.0208(9) 0.0285(10) -0.0016(7) 0.0012(8) 0.0021(8) C4 0.0361(11) 0.0209(10) 0.0306(10) 0.0046(8) 0.0007(8) 0.0024(8) C5 0.0336(10) 0.0260(10) 0.0222(9) 0.0046(8) 0.0017(7) 0.0011(8) C6 0.0262(9) 0.0225(9) 0.0204(9) 0.0002(7) 0.0023(7) 0.0002(7) C7 0.0211(8) 0.0209(9) 0.0203(8) 0.0035(7) 0.0004(6) -0.0016(7) C8 0.0327(10) 0.0276(10) 0.0177(8) -0.0001(7) 0.0043(7) 0.0002(8) C9 0.0479(13) 0.0317(11) 0.0208(9) -0.0041(8) 0.0086(9) 0.0057(10) C10 0.0389(12) 0.0403(13) 0.0297(11) -0.0029(9) 0.0133(9) 0.0078(10) C11 0.0267(9) 0.0310(11) 0.0334(11) -0.0037(9) 0.0070(8) 0.0087(8) C12 0.0181(8) 0.0191(8) 0.0256(9) 0.0003(7) 0.0011(7) 0.0014(6) C13 0.0228(9) 0.0242(10) 0.0298(10) -0.0002(8) 0.0022(7) 0.0049(7) C14 0.0281(10) 0.0299(11) 0.0388(12) -0.0007(9) 0.0031(9) 0.0115(9) C15 0.0281(10) 0.0296(11) 0.0412(13) 0.0042(9) -0.0016(9) 0.0108(8) C16 0.0255(9) 0.0260(10) 0.0315(10) 0.0053(8) -0.0030(8) 0.0035(8) C17 0.0217(8) 0.0227(9) 0.0257(9) 0.0014(7) 0.0023(7) 0.0010(7) C18 0.0463(13) 0.0387(13) 0.0236(10) 0.0056(9) 0.0043(9) 0.0102(11) O5 0.0197(6) 0.0356(8) 0.0214(7) -0.0003(6) 0.0032(5) -0.0014(6) O6 0.0185(6) 0.0290(7) 0.0206(6) -0.0022(5) 0.0008(5) -0.0007(5) O7 0.0196(6) 0.0250(7) 0.0216(6) -0.0029(5) 0.0013(5) 0.0042(5) O8 0.0238(7) 0.0326(8) 0.0208(7) -0.0035(6) -0.0008(5) 0.0049(6) N3 0.0293(9) 0.0477(12) 0.0207(8) -0.0051(8) 0.0008(7) 0.0030(8) N4 0.0271(8) 0.0325(9) 0.0241(8) -0.0098(7) 0.0043(6) -0.0003(7) C19 0.0246(10) 0.0533(15) 0.0269(10) -0.0013(10) 0.0088(8) -0.0045(10) C20 0.0208(8) 0.0313(11) 0.0239(9) 0.0029(8) -0.0011(7) 0.0002(7) C21 0.0203(9) 0.0533(15) 0.0317(11) 0.0025(10) 0.0000(8) -0.0007(9) C22 0.0208(10) 0.076(2) 0.0400(14) -0.0011(13) -0.0079(9) -0.0061(12) C23 0.0263(11) 0.072(2) 0.0291(12) -0.0064(12) -0.0082(9) -0.0029(11) C24 0.0236(9) 0.0442(13) 0.0253(10) -0.0024(9) -0.0039(7) 0.0010(9) C25 0.0197(8) 0.0287(10) 0.0228(9) 0.0007(7) -0.0019(7) 0.0004(7) C26 0.0313(11) 0.0493(14) 0.0216(10) -0.0068(9) -0.0041(8) 0.0023(10) C27 0.0371(12) 0.0589(17) 0.0223(10) -0.0080(10) 0.0052(9) 0.0004(11) C28 0.0371(12) 0.0510(15) 0.0276(11) -0.0149(10) 0.0038(9) 0.0042(11) C29 0.0243(9) 0.0259(10) 0.0321(10) -0.0078(8) 0.0071(8) 0.0003(7) C30 0.0167(8) 0.0200(9) 0.0251(9) -0.0009(7) 0.0024(6) -0.0016(6) C31 0.0200(8) 0.0226(9) 0.0301(10) -0.0038(7) 0.0042(7) -0.0010(7) C32 0.0239(9) 0.0221(10) 0.0406(12) -0.0038(8) 0.0063(8) 0.0029(7) C33 0.0244(9) 0.0212(10) 0.0435(12) 0.0033(8) -0.0004(8) 0.0032(7) C34 0.0232(9) 0.0247(10) 0.0310(10) 0.0049(8) 0.0006(7) -0.0002(7) C35 0.0179(8) 0.0227(9) 0.0250(9) -0.0011(7) 0.0023(7) -0.0011(6) C36 0.0301(10) 0.0449(13) 0.0221(10) -0.0039(9) -0.0041(8) 0.0049(9) O9 0.0249(7) 0.0296(8) 0.0289(7) -0.0075(6) 0.0040(6) -0.0029(6) O10 0.0253(7) 0.0260(7) 0.0260(7) -0.0038(6) 0.0051(5) -0.0035(6) C37 0.0231(8) 0.0230(9) 0.0225(9) 0.0004(7) 0.0014(7) -0.0003(7) C38 0.0367(12) 0.0398(13) 0.0308(11) -0.0055(10) 0.0078(9) -0.0157(10) O11 0.0359(8) 0.0264(8) 0.0283(8) 0.0020(6) 0.0093(6) -0.0004(6) O12 0.0416(9) 0.0285(8) 0.0275(8) -0.0025(6) 0.0106(6) -0.0032(7) C39 0.0304(10) 0.0258(10) 0.0254(9) 0.0007(8) 0.0040(7) -0.0033(8) C40 0.0591(17) 0.0303(12) 0.0432(14) -0.0037(11) 0.0169(12) -0.0147(12) B1 0.0218(9) 0.0250(10) 0.0209(9) 0.0032(8) -0.0001(7) -0.0013(8) C41 0.0255(9) 0.0258(10) 0.0231(9) 0.0035(7) -0.0010(7) -0.0014(7) C42 0.0517(15) 0.0384(13) 0.0290(11) -0.0002(10) 0.0049(10) -0.0163(11) C43 0.0597(17) 0.0425(15) 0.0404(14) -0.0063(12) -0.0001(12) -0.0214(13) C44 0.0469(14) 0.0432(15) 0.0312(12) -0.0088(10) -0.0069(10) -0.0016(11) C45 0.0403(12) 0.0444(14) 0.0236(10) -0.0001(9) 0.0019(9) 0.0003(11) C46 0.0323(10) 0.0323(11) 0.0247(10) 0.0014(8) 0.0019(8) -0.0044(9) C47 0.0214(8) 0.0273(10) 0.0300(10) 0.0041(8) 0.0035(7) -0.0003(7) C48 0.0329(11) 0.0372(13) 0.0363(12) -0.0030(10) 0.0003(9) 0.0048(9) C49 0.0338(12) 0.0347(13) 0.0543(16) -0.0099(11) 0.0055(11) 0.0008(10) C50 0.0308(11) 0.0297(12) 0.0651(18) 0.0053(12) 0.0116(11) 0.0047(9) C51 0.0303(11) 0.0371(13) 0.0485(15) 0.0135(11) 0.0057(10) 0.0068(9) C52 0.0256(9) 0.0315(11) 0.0313(11) 0.0079(8) 0.0026(8) 0.0013(8) C53 0.0243(9) 0.0294(10) 0.0217(9) 0.0025(7) 0.0008(7) -0.0048(8) C54 0.0259(10) 0.0552(16) 0.0310(11) 0.0111(11) 0.0013(8) -0.0060(10) C55 0.0281(12) 0.084(2) 0.0412(14) 0.0168(14) 0.0063(10) -0.0151(13) C56 0.0460(16) 0.101(3) 0.0398(15) 0.0351(18) 0.0073(12) -0.0155(17) C57 0.0389(14) 0.089(2) 0.0394(15) 0.0347(16) 0.0025(11) 0.0005(15) C58 0.0273(10) 0.0495(14) 0.0271(10) 0.0147(10) 0.0021(8) -0.0013(9) C59 0.0241(8) 0.0229(9) 0.0182(8) 0.0012(7) 0.0016(6) -0.0013(7) C60 0.0269(9) 0.0233(9) 0.0290(10) 0.0036(8) 0.0031(7) -0.0012(8) C61 0.0285(10) 0.0297(11) 0.0322(11) 0.0018(9) 0.0053(8) -0.0067(8) C62 0.0233(9) 0.0384(12) 0.0282(10) -0.0029(9) 0.0061(7) -0.0016(8) C63 0.0284(10) 0.0310(11) 0.0276(10) -0.0009(8) 0.0045(8) 0.0057(8) C64 0.0281(9) 0.0235(9) 0.0230(9) 0.0006(7) 0.0045(7) -0.0016(7) N5 0.068(2) 0.070(2) 0.065(2) -0.0049(17) 0.0011(15) 0.0027(17) C65 0.0549(18) 0.058(2) 0.0564(19) -0.0068(15) 0.0211(15) -0.0078(15) C66 0.080(3) 0.080(3) 0.111(4) -0.022(3) 0.030(3) -0.032(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 Tm O6 2.2671(14) . ? Tm O9 2.2845(15) . ? Tm O2 2.2849(14) . ? Tm O11 2.3171(16) . ? Tm O3 2.3607(14) . ? Tm O7 2.3926(14) . ? Tm O5 2.5836(14) . ? Tm O1 2.6103(15) . ? Tm Zn2 3.3326(4) . ? Tm Zn1 3.3410(4) . ? Zn1 O10 1.9851(15) . ? Zn1 O2 2.0165(14) . ? Zn1 N2 2.0348(18) . ? Zn1 O3 2.0540(14) . ? Zn1 N1 2.0569(18) . ? Zn2 O12 1.9801(17) . ? Zn2 O6 2.0347(14) . ? Zn2 N4 2.0348(19) . ? Zn2 O7 2.0424(14) . ? Zn2 N3 2.0488(19) . ? O1 C2 1.381(2) . ? O1 C1 1.441(2) . ? O2 C7 1.326(2) . ? O3 C12 1.324(2) . ? O4 C17 1.371(3) . ? O4 C18 1.430(3) . ? N1 C8 1.279(3) . ? N1 C9 1.466(3) . ? N2 C11 1.279(3) . ? N2 C10 1.481(3) . ? C2 C3 1.383(3) . ? C2 C7 1.421(3) . ? C3 C4 1.400(3) . ? C4 C5 1.371(3) . ? C5 C6 1.412(3) . ? C6 C7 1.413(3) . ? C6 C8 1.460(3) . ? C9 C10 1.520(4) . ? C11 C13 1.448(3) . ? C12 C13 1.417(3) . ? C12 C17 1.424(3) . ? C13 C14 1.417(3) . ? C14 C15 1.374(4) . ? C15 C16 1.402(3) . ? C16 C17 1.380(3) . ? O5 C20 1.382(2) . ? O5 C19 1.440(3) . ? O6 C25 1.328(2) . ? O7 C30 1.322(2) . ? O8 C35 1.364(2) . ? O8 C36 1.429(2) . ? N3 C26 1.276(3) . ? N3 C27 1.472(3) . ? N4 C29 1.278(3) . ? N4 C28 1.475(3) . ? C20 C21 1.378(3) . ? C20 C25 1.415(3) . ? C21 C22 1.405(4) . ? C22 C23 1.379(4) . ? C23 C24 1.410(3) . ? C24 C25 1.409(3) . ? C24 C26 1.464(3) . ? C27 C28 1.517(4) . ? C29 C31 1.456(3) . ? C30 C31 1.419(3) . ? C30 C35 1.426(3) . ? C31 C32 1.420(3) . ? C32 C33 1.371(3) . ? C33 C34 1.404(3) . ? C34 C35 1.381(3) . ? O9 C37 1.243(3) . ? O10 C37 1.277(2) . ? C37 C38 1.507(3) . ? O11 C39 1.245(3) . ? O12 C39 1.274(3) . ? C39 C40 1.514(3) . ? B1 C41 1.647(3) . ? B1 C53 1.647(3) . ? B1 C47 1.650(3) . ? B1 C59 1.652(3) . ? C41 C42 1.397(3) . ? C41 C46 1.408(3) . ? C42 C43 1.402(4) . ? C43 C44 1.375(4) . ? C44 C45 1.387(4) . ? C45 C46 1.392(3) . ? C47 C52 1.399(3) . ? C47 C48 1.404(3) . ? C48 C49 1.395(4) . ? C49 C50 1.390(4) . ? C50 C51 1.381(4) . ? C51 C52 1.397(3) . ? C53 C58 1.395(3) . ? C53 C54 1.411(3) . ? C54 C55 1.383(4) . ? C55 C56 1.385(4) . ? C56 C57 1.376(4) . ? C57 C58 1.389(3) . ? C59 C60 1.405(3) . ? C59 C64 1.407(3) . ? C60 C61 1.393(3) . ? C61 C62 1.392(3) . ? C62 C63 1.390(3) . ? C63 C64 1.397(3) . ? N5 C65 1.120(5) . ? C65 C66 1.416(6) . ? 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 O6 Tm O9 148.96(5) . . ? O6 Tm O2 130.52(5) . . ? O9 Tm O2 79.86(5) . . ? O6 Tm O11 80.09(6) . . ? O9 Tm O11 70.84(6) . . ? O2 Tm O11 148.81(5) . . ? O6 Tm O3 119.12(5) . . ? O9 Tm O3 74.58(5) . . ? O2 Tm O3 67.48(5) . . ? O11 Tm O3 94.01(6) . . ? O6 Tm O7 67.82(5) . . ? O9 Tm O7 92.94(5) . . ? O2 Tm O7 119.79(5) . . ? O11 Tm O7 73.18(5) . . ? O3 Tm O7 164.69(5) . . ? O6 Tm O5 63.16(5) . . ? O9 Tm O5 143.49(5) . . ? O2 Tm O5 76.41(5) . . ? O11 Tm O5 122.55(5) . . ? O3 Tm O5 70.87(5) . . ? O7 Tm O5 122.92(5) . . ? O6 Tm O1 77.79(5) . . ? O9 Tm O1 120.26(5) . . ? O2 Tm O1 62.57(5) . . ? O11 Tm O1 143.14(5) . . ? O3 Tm O1 122.52(5) . . ? O7 Tm O1 71.29(5) . . ? O5 Tm O1 71.45(5) . . ? O6 Tm Zn2 36.76(4) . . ? O9 Tm Zn2 114.41(4) . . ? O2 Tm Zn2 149.44(4) . . ? O11 Tm Zn2 57.95(4) . . ? O3 Tm Zn2 140.72(3) . . ? O7 Tm Zn2 37.45(3) . . ? O5 Tm Zn2 99.89(3) . . ? O1 Tm Zn2 87.31(3) . . ? O6 Tm Zn1 148.64(4) . . ? O9 Tm Zn1 58.92(4) . . ? O2 Tm Zn1 36.22(4) . . ? O11 Tm Zn1 115.15(4) . . ? O3 Tm Zn1 37.49(3) . . ? O7 Tm Zn1 141.18(3) . . ? O5 Tm Zn1 86.02(3) . . ? O1 Tm Zn1 98.77(3) . . ? Zn2 Tm Zn1 172.654(6) . . ? O10 Zn1 O2 111.72(6) . . ? O10 Zn1 N2 112.91(7) . . ? O2 Zn1 N2 135.21(7) . . ? O10 Zn1 O3 100.46(6) . . ? O2 Zn1 O3 78.70(6) . . ? N2 Zn1 O3 89.72(7) . . ? O10 Zn1 N1 107.74(7) . . ? O2 Zn1 N1 89.08(7) . . ? N2 Zn1 N1 81.12(8) . . ? O3 Zn1 N1 151.74(7) . . ? O10 Zn1 Tm 91.80(4) . . ? O2 Zn1 Tm 42.04(4) . . ? N2 Zn1 Tm 132.22(5) . . ? O3 Zn1 Tm 44.39(4) . . ? N1 Zn1 Tm 130.98(5) . . ? O12 Zn2 O6 114.23(7) . . ? O12 Zn2 N4 110.34(8) . . ? O6 Zn2 N4 135.42(7) . . ? O12 Zn2 O7 100.75(7) . . ? O6 Zn2 O7 79.30(6) . . ? N4 Zn2 O7 91.60(7) . . ? O12 Zn2 N3 106.76(8) . . ? O6 Zn2 N3 88.08(7) . . ? N4 Zn2 N3 80.30(8) . . ? O7 Zn2 N3 152.45(8) . . ? O12 Zn2 Tm 93.57(5) . . ? O6 Zn2 Tm 41.82(4) . . ? N4 Zn2 Tm 134.91(6) . . ? O7 Zn2 Tm 45.43(4) . . ? N3 Zn2 Tm 129.62(6) . . ? C2 O1 C1 115.56(17) . . ? C2 O1 Tm 116.19(11) . . ? C1 O1 Tm 128.02(13) . . ? C7 O2 Zn1 128.03(12) . . ? C7 O2 Tm 129.03(12) . . ? Zn1 O2 Tm 101.74(6) . . ? C12 O3 Zn1 125.64(13) . . ? C12 O3 Tm 136.20(13) . . ? Zn1 O3 Tm 98.12(6) . . ? C17 O4 C18 116.60(17) . . ? C8 N1 C9 121.60(19) . . ? C8 N1 Zn1 127.87(15) . . ? C9 N1 Zn1 109.21(14) . . ? C11 N2 C10 119.64(19) . . ? C11 N2 Zn1 126.15(16) . . ? C10 N2 Zn1 114.07(15) . . ? O1 C2 C3 125.57(18) . . ? O1 C2 C7 113.18(17) . . ? C3 C2 C7 121.24(18) . . ? C2 C3 C4 119.7(2) . . ? C5 C4 C3 120.2(2) . . ? C4 C5 C6 121.2(2) . . ? C5 C6 C7 119.26(19) . . ? C5 C6 C8 117.45(19) . . ? C7 C6 C8 123.04(19) . . ? O2 C7 C6 125.36(18) . . ? O2 C7 C2 116.44(17) . . ? C6 C7 C2 118.20(18) . . ? N1 C8 C6 125.19(19) . . ? N1 C9 C10 108.51(19) . . ? N2 C10 C9 109.53(18) . . ? N2 C11 C13 126.1(2) . . ? O3 C12 C13 124.74(19) . . ? O3 C12 C17 117.91(18) . . ? C13 C12 C17 117.34(18) . . ? C14 C13 C12 119.3(2) . . ? C14 C13 C11 116.4(2) . . ? C12 C13 C11 124.00(19) . . ? C15 C14 C13 121.5(2) . . ? C14 C15 C16 119.7(2) . . ? C17 C16 C15 119.8(2) . . ? O4 C17 C16 125.0(2) . . ? O4 C17 C12 113.14(17) . . ? C16 C17 C12 121.9(2) . . ? C20 O5 C19 115.89(16) . . ? C20 O5 Tm 116.96(12) . . ? C19 O5 Tm 127.01(13) . . ? C25 O6 Zn2 129.18(13) . . ? C25 O6 Tm 129.09(13) . . ? Zn2 O6 Tm 101.42(6) . . ? C30 O7 Zn2 125.79(13) . . ? C30 O7 Tm 134.63(13) . . ? Zn2 O7 Tm 97.11(5) . . ? C35 O8 C36 116.32(17) . . ? C26 N3 C27 121.6(2) . . ? C26 N3 Zn2 128.95(16) . . ? C27 N3 Zn2 107.87(15) . . ? C29 N4 C28 119.1(2) . . ? C29 N4 Zn2 126.29(15) . . ? C28 N4 Zn2 113.84(15) . . ? C21 C20 O5 125.3(2) . . ? C21 C20 C25 121.8(2) . . ? O5 C20 C25 112.92(17) . . ? C20 C21 C22 119.0(2) . . ? C23 C22 C21 120.4(2) . . ? C22 C23 C24 121.0(2) . . ? C25 C24 C23 119.1(2) . . ? C25 C24 C26 123.57(19) . . ? C23 C24 C26 117.3(2) . . ? O6 C25 C24 124.53(19) . . ? O6 C25 C20 116.84(18) . . ? C24 C25 C20 118.61(18) . . ? N3 C26 C24 125.0(2) . . ? N3 C27 C28 108.4(2) . . ? N4 C28 C27 110.4(2) . . ? N4 C29 C31 125.92(19) . . ? O7 C30 C31 125.07(19) . . ? O7 C30 C35 117.39(17) . . ? C31 C30 C35 117.54(18) . . ? C30 C31 C32 119.0(2) . . ? C30 C31 C29 125.26(19) . . ? C32 C31 C29 115.50(19) . . ? C33 C32 C31 121.9(2) . . ? C32 C33 C34 119.7(2) . . ? C35 C34 C33 119.8(2) . . ? O8 C35 C34 125.18(19) . . ? O8 C35 C30 112.75(17) . . ? C34 C35 C30 122.07(19) . . ? C37 O9 Tm 148.39(14) . . ? C37 O10 Zn1 114.41(13) . . ? O9 C37 O10 124.12(19) . . ? O9 C37 C38 117.42(19) . . ? O10 C37 C38 118.46(19) . . ? C39 O11 Tm 149.36(15) . . ? C39 O12 Zn2 113.23(14) . . ? O11 C39 O12 124.5(2) . . ? O11 C39 C40 118.3(2) . . ? O12 C39 C40 117.2(2) . . ? C41 B1 C53 111.39(17) . . ? C41 B1 C47 110.94(16) . . ? C53 B1 C47 106.99(17) . . ? C41 B1 C59 106.46(16) . . ? C53 B1 C59 111.40(16) . . ? C47 B1 C59 109.71(16) . . ? C42 C41 C46 115.0(2) . . ? C42 C41 B1 124.58(19) . . ? C46 C41 B1 120.39(19) . . ? C41 C42 C43 122.3(2) . . ? C44 C43 C42 120.8(3) . . ? C43 C44 C45 118.8(2) . . ? C44 C45 C46 119.8(2) . . ? C45 C46 C41 123.2(2) . . ? C52 C47 C48 115.1(2) . . ? C52 C47 B1 125.1(2) . . ? C48 C47 B1 119.84(19) . . ? C49 C48 C47 123.3(2) . . ? C50 C49 C48 119.5(3) . . ? C51 C50 C49 119.0(2) . . ? C50 C51 C52 120.6(2) . . ? C51 C52 C47 122.5(2) . . ? C58 C53 C54 114.5(2) . . ? C58 C53 B1 125.54(18) . . ? C54 C53 B1 119.94(19) . . ? C55 C54 C53 123.1(2) . . ? C54 C55 C56 120.0(3) . . ? C57 C56 C55 118.8(3) . . ? C56 C57 C58 120.5(3) . . ? C57 C58 C53 123.0(2) . . ? C60 C59 C64 114.77(18) . . ? C60 C59 B1 123.91(18) . . ? C64 C59 B1 121.30(18) . . ? C61 C60 C59 123.0(2) . . ? C62 C61 C60 120.6(2) . . ? C63 C62 C61 118.4(2) . . ? C62 C63 C64 120.2(2) . . ? C63 C64 C59 123.1(2) . . ? N5 C65 C66 176.7(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.978 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.096 # Attachment '- 6.cif' data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 889491' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H65 B N5 O12 Yb Zn2' _chemical_formula_weight 1434.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.360(3) _cell_length_b 9.5339(14) _cell_length_c 34.750(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.7600(16) _cell_angle_gamma 90.00 _cell_volume 6052.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15086 _cell_measurement_theta_min 2.3563 _cell_measurement_theta_max 31.8628 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2908 _exptl_absorpt_coefficient_mu 2.387 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7160 _exptl_absorpt_correction_T_max 0.7963 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; Absorption correction was performed using REQAB (Rigaku, 1998) program. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50844 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17309 _reflns_number_gt 13640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear ver. 1.4' _computing_cell_refinement 'CrystalClear ver. 1.4' _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics OrtepIII _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17309 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Yb Yb 0.323959(9) 0.105117(17) 0.131873(4) 0.02294(5) Uani 1 1 d . . . Zn1 Zn 0.29088(2) 0.23954(4) 0.216723(12) 0.02259(10) Uani 1 1 d . . . Zn2 Zn 0.37168(2) 0.00735(5) 0.046299(12) 0.02516(10) Uani 1 1 d . . . O1 O 0.31485(14) -0.1596(3) 0.14836(7) 0.0249(5) Uani 1 1 d . . . O2 O 0.30125(13) 0.0490(2) 0.19297(7) 0.0217(5) Uani 1 1 d . . . O3 O 0.25495(14) 0.2792(3) 0.15972(7) 0.0252(5) Uani 1 1 d . . . O4 O 0.22584(16) 0.2989(3) 0.08562(8) 0.0322(6) Uani 1 1 d . . . N1 N 0.27999(19) 0.1447(3) 0.26892(9) 0.0290(7) Uani 1 1 d . . . N2 N 0.20677(18) 0.3559(4) 0.23366(10) 0.0300(7) Uani 1 1 d . . . C1 C 0.3152(2) -0.2796(4) 0.12325(11) 0.0300(9) Uani 1 1 d . . . H1 H 0.3597 -0.3347 0.1301 0.045 Uiso 1 1 calc R . . H2 H 0.3140 -0.2480 0.0964 0.045 Uiso 1 1 calc R . . H3 H 0.2721 -0.3377 0.1262 0.045 Uiso 1 1 calc R . . C2 C 0.3167(2) -0.1926(4) 0.18715(10) 0.0234(7) Uani 1 1 d . . . C3 C 0.3281(2) -0.3253(4) 0.20283(11) 0.0278(8) Uani 1 1 d . . . H4 H 0.3357 -0.4031 0.1866 0.033 Uiso 1 1 calc R . . C4 C 0.3283(2) -0.3435(4) 0.24257(12) 0.0304(9) Uani 1 1 d . . . H5 H 0.3371 -0.4340 0.2535 0.036 Uiso 1 1 calc R . . C5 C 0.3158(2) -0.2320(4) 0.26617(12) 0.0307(9) Uani 1 1 d . . . H6 H 0.3144 -0.2468 0.2931 0.037 Uiso 1 1 calc R . . C6 C 0.3051(2) -0.0961(4) 0.25075(11) 0.0249(8) Uani 1 1 d . . . C7 C 0.3073(2) -0.0739(4) 0.21089(11) 0.0227(7) Uani 1 1 d . . . C8 C 0.2843(2) 0.0133(4) 0.27676(11) 0.0295(8) Uani 1 1 d . . . H7 H 0.2730 -0.0151 0.3017 0.035 Uiso 1 1 calc R . . C9 C 0.2508(3) 0.2452(5) 0.29515(12) 0.0363(10) Uani 1 1 d . . . H8 H 0.2896 0.3116 0.3052 0.044 Uiso 1 1 calc R . . H9 H 0.2329 0.1953 0.3174 0.044 Uiso 1 1 calc R . . C10 C 0.1886(3) 0.3240(5) 0.27305(12) 0.0395(10) Uani 1 1 d . . . H10 H 0.1435 0.2666 0.2717 0.047 Uiso 1 1 calc R . . H11 H 0.1794 0.4124 0.2867 0.047 Uiso 1 1 calc R . . C11 C 0.1679(2) 0.4432(4) 0.21247(13) 0.0323(9) Uani 1 1 d . . . H12 H 0.1342 0.4987 0.2249 0.039 Uiso 1 1 calc R . . C12 C 0.2086(2) 0.3790(4) 0.14720(11) 0.0248(8) Uani 1 1 d . . . C13 C 0.1701(2) 0.4656(4) 0.17146(12) 0.0282(8) Uani 1 1 d . . . C14 C 0.1261(2) 0.5770(4) 0.15466(14) 0.0351(10) Uani 1 1 d . . . H13 H 0.1012 0.6365 0.1709 0.042 Uiso 1 1 calc R . . C15 C 0.1189(2) 0.6003(4) 0.11566(14) 0.0367(10) Uani 1 1 d . . . H14 H 0.0911 0.6780 0.1052 0.044 Uiso 1 1 calc R . . C16 C 0.1524(2) 0.5098(4) 0.09112(12) 0.0311(9) Uani 1 1 d . . . H15 H 0.1465 0.5241 0.0639 0.037 Uiso 1 1 calc R . . C17 C 0.1943(2) 0.3990(4) 0.10686(12) 0.0261(8) Uani 1 1 d . . . C18 C 0.2228(3) 0.3214(5) 0.04510(12) 0.0393(10) Uani 1 1 d . . . H16 H 0.1718 0.3184 0.0338 0.059 Uiso 1 1 calc R . . H17 H 0.2508 0.2480 0.0334 0.059 Uiso 1 1 calc R . . H18 H 0.2438 0.4133 0.0401 0.059 Uiso 1 1 calc R . . O5 O 0.18736(14) 0.0338(3) 0.12437(7) 0.0269(6) Uani 1 1 d . . . O6 O 0.28005(13) 0.0127(3) 0.07466(7) 0.0248(5) Uani 1 1 d . . . O7 O 0.41652(13) -0.0187(3) 0.10186(7) 0.0241(5) Uani 1 1 d . . . O8 O 0.45224(14) -0.0261(3) 0.17515(7) 0.0278(6) Uani 1 1 d . . . N3 N 0.30707(19) -0.0574(4) -0.00206(9) 0.0353(8) Uani 1 1 d . . . N4 N 0.43669(18) -0.1452(4) 0.02739(10) 0.0299(7) Uani 1 1 d . . . C19 C 0.1376(2) 0.0399(5) 0.15342(12) 0.0377(10) Uani 1 1 d . . . H19 H 0.1016 0.1143 0.1470 0.056 Uiso 1 1 calc R . . H20 H 0.1647 0.0597 0.1786 0.056 Uiso 1 1 calc R . . H21 H 0.1123 -0.0503 0.1546 0.056 Uiso 1 1 calc R . . C20 C 0.1579(2) -0.0050(4) 0.08782(11) 0.0278(8) Uani 1 1 d . . . C21 C 0.0851(2) -0.0291(5) 0.07702(12) 0.0362(10) Uani 1 1 d . . . H22 H 0.0499 -0.0154 0.0949 0.043 Uiso 1 1 calc R . . C22 C 0.0633(3) -0.0744(6) 0.03909(14) 0.0495(13) Uani 1 1 d . . . H23 H 0.0131 -0.0938 0.0315 0.059 Uiso 1 1 calc R . . C23 C 0.1138(2) -0.0904(5) 0.01332(13) 0.0442(12) Uani 1 1 d . . . H24 H 0.0982 -0.1213 -0.0122 0.053 Uiso 1 1 calc R . . C24 C 0.1887(2) -0.0623(5) 0.02350(12) 0.0323(9) Uani 1 1 d . . . C25 C 0.2112(2) -0.0174(4) 0.06158(11) 0.0251(8) Uani 1 1 d . . . C26 C 0.2388(2) -0.0880(5) -0.00552(12) 0.0386(10) Uani 1 1 d . . . H25 H 0.2194 -0.1310 -0.0290 0.046 Uiso 1 1 calc R . . C27 C 0.3550(3) -0.0953(6) -0.03175(13) 0.0449(12) Uani 1 1 d . . . H26 H 0.3759 -0.0097 -0.0425 0.054 Uiso 1 1 calc R . . H27 H 0.3268 -0.1464 -0.0531 0.054 Uiso 1 1 calc R . . C28 C 0.4155(3) -0.1871(5) -0.01309(12) 0.0420(11) Uani 1 1 d . . . H28 H 0.3990 -0.2860 -0.0138 0.050 Uiso 1 1 calc R . . H29 H 0.4586 -0.1804 -0.0280 0.050 Uiso 1 1 calc R . . C29 C 0.4844(2) -0.2171(4) 0.04812(12) 0.0308(9) Uani 1 1 d . . . H30 H 0.5104 -0.2861 0.0353 0.037 Uiso 1 1 calc R . . C30 C 0.46799(19) -0.1108(4) 0.11381(11) 0.0225(7) Uani 1 1 d . . . C31 C 0.5024(2) -0.2025(4) 0.08974(12) 0.0262(8) Uani 1 1 d . . . C32 C 0.5563(2) -0.2978(4) 0.10697(13) 0.0317(9) Uani 1 1 d . . . H31 H 0.5796 -0.3600 0.0907 0.038 Uiso 1 1 calc R . . C33 C 0.5753(2) -0.3028(4) 0.14534(13) 0.0334(9) Uani 1 1 d . . . H32 H 0.6114 -0.3676 0.1557 0.040 Uiso 1 1 calc R . . C34 C 0.5418(2) -0.2122(4) 0.16996(12) 0.0297(8) Uani 1 1 d . . . H33 H 0.5551 -0.2150 0.1971 0.036 Uiso 1 1 calc R . . C35 C 0.4893(2) -0.1184(4) 0.15441(11) 0.0246(8) Uani 1 1 d . . . C36 C 0.4779(2) -0.0130(5) 0.21511(11) 0.0364(10) Uani 1 1 d . . . H34 H 0.4718 -0.1027 0.2282 0.055 Uiso 1 1 calc R . . H35 H 0.4498 0.0598 0.2269 0.055 Uiso 1 1 calc R . . H36 H 0.5299 0.0128 0.2177 0.055 Uiso 1 1 calc R . . O9 O 0.40799(14) 0.2414(3) 0.16618(8) 0.0287(6) Uani 1 1 d . . . O10 O 0.38523(14) 0.3426(3) 0.22131(8) 0.0273(6) Uani 1 1 d . . . C37 C 0.4221(2) 0.3293(4) 0.19226(11) 0.0256(8) Uani 1 1 d . . . C38 C 0.4861(2) 0.4254(5) 0.18911(13) 0.0377(10) Uani 1 1 d . . . H37 H 0.5313 0.3778 0.1991 0.057 Uiso 1 1 calc R . . H38 H 0.4799 0.5106 0.2042 0.057 Uiso 1 1 calc R . . H39 H 0.4887 0.4505 0.1619 0.057 Uiso 1 1 calc R . . O11 O 0.37194(15) 0.2620(3) 0.09071(8) 0.0332(6) Uani 1 1 d . . . O12 O 0.40934(16) 0.1948(3) 0.03473(8) 0.0353(7) Uani 1 1 d . . . C39 C 0.4041(2) 0.2838(4) 0.06140(12) 0.0302(9) Uani 1 1 d . . . C40 C 0.4398(3) 0.4247(5) 0.05729(15) 0.0499(13) Uani 1 1 d . . . H40 H 0.4107 0.4973 0.0686 0.075 Uiso 1 1 calc R . . H41 H 0.4425 0.4450 0.0298 0.075 Uiso 1 1 calc R . . H42 H 0.4892 0.4233 0.0708 0.075 Uiso 1 1 calc R . . B1 B -0.1460(2) 0.2170(5) 0.13314(12) 0.0236(8) Uani 1 1 d . . . C41 C -0.1198(2) 0.3049(4) 0.17296(11) 0.0256(8) Uani 1 1 d . . . C42 C -0.0748(3) 0.4231(5) 0.17484(14) 0.0429(11) Uani 1 1 d . . . H43 H -0.0574 0.4561 0.1516 0.051 Uiso 1 1 calc R . . C43 C -0.0542(3) 0.4945(5) 0.20886(14) 0.0487(13) Uani 1 1 d . . . H44 H -0.0234 0.5744 0.2084 0.058 Uiso 1 1 calc R . . C44 C -0.0781(3) 0.4510(5) 0.24356(14) 0.0431(11) Uani 1 1 d . . . H45 H -0.0649 0.5008 0.2669 0.052 Uiso 1 1 calc R . . C45 C -0.1216(2) 0.3332(5) 0.24306(12) 0.0383(10) Uani 1 1 d . . . H46 H -0.1378 0.2993 0.2665 0.046 Uiso 1 1 calc R . . C46 C -0.1419(2) 0.2636(4) 0.20843(12) 0.0327(9) Uani 1 1 d . . . H47 H -0.1725 0.1835 0.2090 0.039 Uiso 1 1 calc R . . C47 C -0.1078(2) 0.0610(4) 0.13394(12) 0.0269(8) Uani 1 1 d . . . C48 C -0.1181(2) -0.0263(5) 0.10110(14) 0.0382(10) Uani 1 1 d . . . H48 H -0.1452 0.0094 0.0785 0.046 Uiso 1 1 calc R . . C49 C -0.0907(2) -0.1616(5) 0.10008(15) 0.0440(11) Uani 1 1 d . . . H49 H -0.0990 -0.2165 0.0773 0.053 Uiso 1 1 calc R . . C50 C -0.0510(2) -0.2158(5) 0.13278(16) 0.0445(12) Uani 1 1 d . . . H50 H -0.0327 -0.3091 0.1327 0.053 Uiso 1 1 calc R . . C51 C -0.0384(2) -0.1341(5) 0.16513(15) 0.0403(11) Uani 1 1 d . . . H51 H -0.0104 -0.1702 0.1874 0.048 Uiso 1 1 calc R . . C52 C -0.0662(2) 0.0017(4) 0.16555(12) 0.0316(9) Uani 1 1 d . . . H52 H -0.0563 0.0563 0.1884 0.038 Uiso 1 1 calc R . . C53 C -0.1221(2) 0.2986(4) 0.09475(11) 0.0272(8) Uani 1 1 d . . . C54 C -0.0483(2) 0.3024(5) 0.08754(12) 0.0378(10) Uani 1 1 d . . . H53 H -0.0130 0.2579 0.1054 0.045 Uiso 1 1 calc R . . C55 C -0.0248(3) 0.3680(6) 0.05577(15) 0.0519(14) Uani 1 1 d . . . H54 H 0.0257 0.3661 0.0519 0.062 Uiso 1 1 calc R . . C56 C -0.0740(3) 0.4369(7) 0.02932(16) 0.0652(18) Uani 1 1 d . . . H55 H -0.0576 0.4847 0.0078 0.078 Uiso 1 1 calc R . . C57 C -0.1463(3) 0.4344(6) 0.03496(15) 0.0585(16) Uani 1 1 d . . . H56 H -0.1811 0.4790 0.0169 0.070 Uiso 1 1 calc R . . C58 C -0.1694(2) 0.3670(5) 0.06689(12) 0.0376(10) Uani 1 1 d . . . H57 H -0.2202 0.3674 0.0700 0.045 Uiso 1 1 calc R . . C59 C -0.2360(2) 0.2013(4) 0.13191(10) 0.0245(8) Uani 1 1 d . . . C60 C -0.2723(2) 0.0730(4) 0.13427(12) 0.0288(8) Uani 1 1 d . . . H58 H -0.2438 -0.0104 0.1365 0.035 Uiso 1 1 calc R . . C61 C -0.3481(2) 0.0614(4) 0.13343(12) 0.0317(9) Uani 1 1 d . . . H59 H -0.3700 -0.0282 0.1356 0.038 Uiso 1 1 calc R . . C62 C -0.3916(2) 0.1797(5) 0.12948(12) 0.0320(9) Uani 1 1 d . . . H60 H -0.4434 0.1726 0.1285 0.038 Uiso 1 1 calc R . . C63 C -0.3581(2) 0.3086(4) 0.12702(11) 0.0310(9) Uani 1 1 d . . . H61 H -0.3871 0.3911 0.1240 0.037 Uiso 1 1 calc R . . C64 C -0.2822(2) 0.3189(4) 0.12889(10) 0.0276(8) Uani 1 1 d . . . H62 H -0.2608 0.4094 0.1281 0.033 Uiso 1 1 calc R . . N5 N -0.3441(3) 0.5386(7) 0.03068(17) 0.0804(16) Uani 1 1 d . . . C65 C -0.3125(4) 0.6268(7) 0.0441(2) 0.0658(17) Uani 1 1 d . . . C66 C -0.2682(4) 0.7288(8) 0.0639(2) 0.095(3) Uani 1 1 d . . . H63 H -0.2991 0.8023 0.0734 0.142 Uiso 1 1 calc R . . H64 H -0.2357 0.7702 0.0463 0.142 Uiso 1 1 calc R . . H65 H -0.2388 0.6853 0.0858 0.142 Uiso 1 1 calc 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 Yb 0.02458(10) 0.02424(9) 0.02043(8) -0.00276(6) 0.00438(6) -0.00020(6) Zn1 0.0243(2) 0.0214(2) 0.0227(2) -0.00172(16) 0.00516(17) 0.00239(17) Zn2 0.0253(2) 0.0282(2) 0.0223(2) -0.00268(17) 0.00431(17) 0.00110(18) O1 0.0314(15) 0.0218(12) 0.0214(12) -0.0039(10) 0.0028(11) -0.0010(11) O2 0.0262(14) 0.0161(12) 0.0229(12) -0.0026(10) 0.0022(10) 0.0021(10) O3 0.0257(14) 0.0252(13) 0.0246(13) 0.0024(11) 0.0022(11) 0.0066(11) O4 0.0426(17) 0.0306(15) 0.0243(13) 0.0021(12) 0.0074(12) 0.0107(13) N1 0.0366(19) 0.0271(17) 0.0239(16) -0.0024(13) 0.0058(14) 0.0029(14) N2 0.0308(18) 0.0317(18) 0.0290(17) -0.0037(14) 0.0109(14) 0.0073(14) C1 0.028(2) 0.036(2) 0.0280(19) -0.0216(17) 0.0131(16) -0.0104(16) C2 0.0208(18) 0.0251(18) 0.0238(17) -0.0057(14) -0.0010(14) -0.0007(14) C3 0.032(2) 0.0218(18) 0.0288(19) -0.0042(15) 0.0009(16) 0.0022(16) C4 0.034(2) 0.0220(18) 0.034(2) 0.0037(16) 0.0015(17) 0.0028(16) C5 0.035(2) 0.029(2) 0.0277(19) 0.0051(16) 0.0005(17) -0.0016(17) C6 0.0251(19) 0.0263(19) 0.0230(17) 0.0008(15) 0.0011(15) -0.0003(15) C7 0.0201(18) 0.0223(17) 0.0251(18) 0.0042(14) -0.0014(14) -0.0040(14) C8 0.031(2) 0.035(2) 0.0223(18) 0.0019(16) 0.0002(16) -0.0017(17) C9 0.050(3) 0.035(2) 0.026(2) -0.0034(17) 0.0126(19) 0.007(2) C10 0.045(3) 0.045(3) 0.031(2) 0.001(2) 0.016(2) 0.010(2) C11 0.030(2) 0.029(2) 0.040(2) -0.0036(18) 0.0120(18) 0.0061(17) C12 0.0226(19) 0.0220(18) 0.0296(19) 0.0004(15) 0.0009(15) 0.0021(14) C13 0.023(2) 0.0255(19) 0.036(2) 0.0017(17) 0.0047(16) 0.0040(15) C14 0.028(2) 0.032(2) 0.045(3) -0.0022(19) 0.0051(19) 0.0114(17) C15 0.028(2) 0.032(2) 0.051(3) 0.008(2) 0.0037(19) 0.0116(17) C16 0.026(2) 0.031(2) 0.035(2) 0.0067(17) -0.0007(17) 0.0028(16) C17 0.0232(19) 0.0238(18) 0.031(2) 0.0007(15) 0.0024(16) -0.0007(15) C18 0.046(3) 0.044(3) 0.029(2) 0.0083(19) 0.0063(19) 0.009(2) O5 0.0213(13) 0.0339(15) 0.0257(13) 0.0006(11) 0.0030(11) -0.0010(11) O6 0.0191(13) 0.0334(15) 0.0219(12) -0.0023(11) 0.0023(10) 0.0000(11) O7 0.0198(13) 0.0269(13) 0.0255(13) -0.0007(11) 0.0009(10) 0.0051(10) O8 0.0246(14) 0.0344(15) 0.0240(13) -0.0036(11) -0.0002(11) 0.0036(11) N3 0.0303(19) 0.055(2) 0.0206(16) -0.0096(15) 0.0009(14) 0.0048(17) N4 0.0238(17) 0.0358(19) 0.0305(17) -0.0092(15) 0.0041(14) 0.0006(14) C19 0.026(2) 0.055(3) 0.034(2) 0.000(2) 0.0107(18) -0.001(2) C20 0.025(2) 0.031(2) 0.0259(19) 0.0015(16) -0.0046(15) -0.0003(16) C21 0.021(2) 0.054(3) 0.034(2) 0.003(2) 0.0022(17) 0.0016(19) C22 0.023(2) 0.081(4) 0.043(3) -0.001(3) -0.008(2) -0.004(2) C23 0.032(2) 0.068(3) 0.030(2) -0.008(2) -0.0092(19) -0.001(2) C24 0.027(2) 0.044(2) 0.0253(19) -0.0021(17) -0.0008(16) 0.0009(18) C25 0.0203(19) 0.030(2) 0.0251(18) 0.0010(15) 0.0017(15) 0.0007(15) C26 0.037(3) 0.055(3) 0.0219(19) -0.0063(19) -0.0065(18) 0.003(2) C27 0.039(3) 0.071(4) 0.026(2) -0.013(2) 0.0062(19) -0.003(2) C28 0.043(3) 0.054(3) 0.030(2) -0.015(2) 0.0040(19) 0.006(2) C29 0.028(2) 0.031(2) 0.035(2) -0.0093(17) 0.0102(17) 0.0005(17) C30 0.0146(17) 0.0206(17) 0.0322(19) 0.0014(15) 0.0014(14) -0.0035(13) C31 0.0226(19) 0.0225(18) 0.035(2) -0.0053(16) 0.0083(16) -0.0040(14) C32 0.024(2) 0.0239(19) 0.047(2) -0.0009(18) 0.0049(18) 0.0028(15) C33 0.031(2) 0.0229(19) 0.045(2) 0.0061(18) 0.0015(19) 0.0044(16) C34 0.024(2) 0.0263(19) 0.039(2) 0.0057(17) 0.0015(17) -0.0024(15) C35 0.0192(18) 0.0234(18) 0.0315(19) -0.0025(15) 0.0034(15) -0.0032(14) C36 0.034(2) 0.048(3) 0.027(2) -0.0038(19) -0.0015(17) 0.004(2) O9 0.0261(14) 0.0305(14) 0.0301(14) -0.0090(12) 0.0060(11) -0.0028(11) O10 0.0277(14) 0.0294(14) 0.0257(13) -0.0030(11) 0.0068(11) -0.0005(11) C37 0.0242(19) 0.0243(18) 0.0277(19) 0.0028(15) -0.0003(15) 0.0016(15) C38 0.040(3) 0.044(3) 0.031(2) -0.0051(19) 0.0110(19) -0.013(2) O11 0.0344(16) 0.0312(15) 0.0355(16) 0.0027(12) 0.0111(13) -0.0001(12) O12 0.0479(18) 0.0279(15) 0.0315(15) 0.0003(12) 0.0103(13) -0.0062(13) C39 0.037(2) 0.0223(19) 0.032(2) 0.0012(16) 0.0074(18) 0.0010(16) C40 0.067(4) 0.037(3) 0.048(3) -0.008(2) 0.019(3) -0.016(2) B1 0.024(2) 0.025(2) 0.0210(19) 0.0014(16) 0.0009(16) -0.0005(16) C41 0.0248(19) 0.0252(19) 0.0267(18) 0.0037(15) 0.0014(15) 0.0004(15) C42 0.051(3) 0.042(3) 0.036(2) 0.003(2) 0.006(2) -0.019(2) C43 0.061(3) 0.040(3) 0.044(3) -0.006(2) -0.001(2) -0.023(2) C44 0.043(3) 0.048(3) 0.036(2) -0.012(2) -0.006(2) -0.004(2) C45 0.041(3) 0.047(3) 0.026(2) 0.0034(19) 0.0009(18) 0.000(2) C46 0.033(2) 0.033(2) 0.032(2) 0.0031(17) 0.0025(17) -0.0023(18) C47 0.0198(19) 0.030(2) 0.032(2) 0.0029(16) 0.0047(16) -0.0042(15) C48 0.034(2) 0.035(2) 0.044(3) -0.004(2) -0.001(2) 0.0062(19) C49 0.037(3) 0.034(2) 0.061(3) -0.012(2) 0.008(2) 0.002(2) C50 0.032(2) 0.028(2) 0.075(4) 0.006(2) 0.013(2) 0.0059(18) C51 0.031(2) 0.036(2) 0.054(3) 0.015(2) 0.004(2) 0.0073(18) C52 0.026(2) 0.034(2) 0.035(2) 0.0066(17) 0.0055(17) 0.0010(17) C53 0.028(2) 0.0276(19) 0.0255(18) 0.0019(15) 0.0013(16) -0.0023(16) C54 0.027(2) 0.058(3) 0.028(2) 0.010(2) -0.0002(17) -0.002(2) C55 0.027(2) 0.084(4) 0.044(3) 0.015(3) 0.004(2) -0.016(2) C56 0.046(3) 0.105(5) 0.045(3) 0.037(3) 0.009(2) -0.016(3) C57 0.041(3) 0.090(4) 0.044(3) 0.040(3) 0.003(2) 0.004(3) C58 0.029(2) 0.055(3) 0.028(2) 0.016(2) 0.0025(17) 0.001(2) C59 0.029(2) 0.0269(19) 0.0178(16) 0.0017(14) 0.0026(15) -0.0018(15) C60 0.027(2) 0.028(2) 0.032(2) 0.0051(16) 0.0060(17) 0.0013(16) C61 0.032(2) 0.031(2) 0.032(2) 0.0022(17) 0.0039(17) -0.0087(17) C62 0.027(2) 0.039(2) 0.030(2) -0.0024(18) 0.0043(17) -0.0006(18) C63 0.033(2) 0.034(2) 0.0267(19) -0.0011(17) 0.0069(17) 0.0078(17) C64 0.034(2) 0.0263(19) 0.0225(18) 0.0026(15) 0.0043(16) 0.0000(16) N5 0.079(4) 0.085(4) 0.075(4) -0.002(3) 0.000(3) 0.008(3) C65 0.066(4) 0.064(4) 0.072(4) -0.021(3) 0.030(3) -0.021(3) C66 0.084(5) 0.090(5) 0.116(7) -0.029(5) 0.038(5) -0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb O6 2.249(2) . ? Yb O9 2.263(3) . ? Yb O2 2.268(2) . ? Yb O11 2.305(3) . ? Yb O3 2.354(2) . ? Yb O7 2.393(2) . ? Yb O5 2.586(3) . ? Yb O1 2.597(3) . ? Yb O8 2.943(3) . ? Yb O4 2.943(3) . ? Yb Zn2 3.3170(6) . ? Yb Zn1 3.3264(6) . ? Zn1 O10 1.984(3) . ? Zn1 O2 2.012(2) . ? Zn1 N2 2.036(3) . ? Zn1 N1 2.054(3) . ? Zn1 O3 2.059(3) . ? Zn2 O12 1.973(3) . ? Zn2 N4 2.032(3) . ? Zn2 O6 2.034(2) . ? Zn2 O7 2.037(3) . ? Zn2 N3 2.053(3) . ? O1 C2 1.381(4) . ? O1 C1 1.440(4) . ? O2 C7 1.326(4) . ? O3 C12 1.320(4) . ? O4 C17 1.369(5) . ? O4 C18 1.420(5) . ? N1 C8 1.283(5) . ? N1 C9 1.461(5) . ? N2 C11 1.281(5) . ? N2 C10 1.473(5) . ? C2 C3 1.385(5) . ? C2 C7 1.422(5) . ? C3 C4 1.392(5) . ? C4 C5 1.376(6) . ? C5 C6 1.409(5) . ? C6 C7 1.406(5) . ? C6 C8 1.455(5) . ? C9 C10 1.511(6) . ? C11 C13 1.446(6) . ? C12 C17 1.413(5) . ? C12 C13 1.419(5) . ? C13 C14 1.424(5) . ? C14 C15 1.366(6) . ? C15 C16 1.399(6) . ? C16 C17 1.387(5) . ? O5 C20 1.380(4) . ? O5 C19 1.429(5) . ? O6 C25 1.332(4) . ? O7 C30 1.326(4) . ? O8 C35 1.362(4) . ? O8 C36 1.427(4) . ? N3 C26 1.280(6) . ? N3 C27 1.467(5) . ? N4 C29 1.276(5) . ? N4 C28 1.477(5) . ? C20 C21 1.370(5) . ? C20 C25 1.408(5) . ? C21 C22 1.407(6) . ? C22 C23 1.361(7) . ? C23 C24 1.412(6) . ? C24 C25 1.412(5) . ? C24 C26 1.452(6) . ? C27 C28 1.509(7) . ? C29 C31 1.458(6) . ? C30 C31 1.403(5) . ? C30 C35 1.428(5) . ? C31 C32 1.429(5) . ? C32 C33 1.345(6) . ? C33 C34 1.400(6) . ? C34 C35 1.384(5) . ? O9 C37 1.242(4) . ? O10 C37 1.277(4) . ? C37 C38 1.502(5) . ? O11 C39 1.246(5) . ? O12 C39 1.267(5) . ? C39 C40 1.506(6) . ? B1 C53 1.642(6) . ? B1 C47 1.643(6) . ? B1 C41 1.648(6) . ? B1 C59 1.655(6) . ? C41 C46 1.392(5) . ? C41 C42 1.396(6) . ? C42 C43 1.384(6) . ? C43 C44 1.387(7) . ? C44 C45 1.377(7) . ? C45 C46 1.392(6) . ? C47 C52 1.394(6) . ? C47 C48 1.410(6) . ? C48 C49 1.386(6) . ? C49 C50 1.387(7) . ? C50 C51 1.368(7) . ? C51 C52 1.393(6) . ? C53 C58 1.396(5) . ? C53 C54 1.403(6) . ? C54 C55 1.375(6) . ? C55 C56 1.388(7) . ? C56 C57 1.361(7) . ? C57 C58 1.385(6) . ? C59 C60 1.399(5) . ? C59 C64 1.403(5) . ? C60 C61 1.395(5) . ? C61 C62 1.381(6) . ? C62 C63 1.381(6) . ? C63 C64 1.392(5) . ? N5 C65 1.098(7) . ? C65 C66 1.403(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Yb O9 148.83(9) . . ? O6 Yb O2 130.69(9) . . ? O9 Yb O2 79.74(9) . . ? O6 Yb O11 80.27(10) . . ? O9 Yb O11 70.82(10) . . ? O2 Yb O11 148.37(9) . . ? O6 Yb O3 118.65(9) . . ? O9 Yb O3 75.24(9) . . ? O2 Yb O3 67.94(9) . . ? O11 Yb O3 93.01(9) . . ? O6 Yb O7 68.21(9) . . ? O9 Yb O7 92.09(9) . . ? O2 Yb O7 119.80(9) . . ? O11 Yb O7 73.57(9) . . ? O3 Yb O7 164.16(9) . . ? O6 Yb O5 63.25(8) . . ? O9 Yb O5 143.81(9) . . ? O2 Yb O5 76.40(8) . . ? O11 Yb O5 122.37(9) . . ? O3 Yb O5 70.76(9) . . ? O7 Yb O5 123.39(9) . . ? O6 Yb O1 77.83(9) . . ? O9 Yb O1 119.83(9) . . ? O2 Yb O1 62.77(8) . . ? O11 Yb O1 143.58(9) . . ? O3 Yb O1 123.03(8) . . ? O7 Yb O1 71.40(8) . . ? O5 Yb O1 71.54(8) . . ? O6 Yb O8 118.87(8) . . ? O9 Yb O8 60.43(9) . . ? O2 Yb O8 68.56(8) . . ? O11 Yb O8 104.88(9) . . ? O3 Yb O8 121.72(8) . . ? O7 Yb O8 56.36(8) . . ? O5 Yb O8 131.14(8) . . ? O1 Yb O8 62.63(8) . . ? O6 Yb O4 67.52(9) . . ? O9 Yb O4 105.94(9) . . ? O2 Yb O4 119.95(8) . . ? O11 Yb O4 60.32(9) . . ? O3 Yb O4 57.09(8) . . ? O7 Yb O4 119.62(8) . . ? O5 Yb O4 64.91(8) . . ? O1 Yb O4 132.93(8) . . ? O8 Yb O4 163.83(8) . . ? O6 Yb Zn2 36.95(6) . . ? O9 Yb Zn2 113.97(7) . . ? O2 Yb Zn2 149.63(6) . . ? O11 Yb Zn2 58.28(7) . . ? O3 Yb Zn2 140.18(6) . . ? O7 Yb Zn2 37.58(6) . . ? O5 Yb Zn2 100.16(6) . . ? O1 Yb Zn2 87.33(6) . . ? O8 Yb Zn2 93.95(5) . . ? O4 Yb Zn2 83.63(5) . . ? O6 Yb Zn1 148.59(6) . . ? O9 Yb Zn1 59.15(7) . . ? O2 Yb Zn1 36.30(6) . . ? O11 Yb Zn1 114.53(7) . . ? O3 Yb Zn1 37.85(6) . . ? O7 Yb Zn1 141.01(6) . . ? O5 Yb Zn1 85.94(6) . . ? O1 Yb Zn1 99.05(6) . . ? O8 Yb Zn1 85.34(5) . . ? O4 Yb Zn1 94.93(5) . . ? Zn2 Yb Zn1 172.352(12) . . ? O10 Zn1 O2 111.23(10) . . ? O10 Zn1 N2 112.87(13) . . ? O2 Zn1 N2 135.74(12) . . ? O10 Zn1 N1 107.97(12) . . ? O2 Zn1 N1 89.23(12) . . ? N2 Zn1 N1 80.83(13) . . ? O10 Zn1 O3 100.32(11) . . ? O2 Zn1 O3 78.78(10) . . ? N2 Zn1 O3 89.94(12) . . ? N1 Zn1 O3 151.65(12) . . ? O10 Zn1 Yb 91.51(8) . . ? O2 Zn1 Yb 41.87(7) . . ? N2 Zn1 Yb 132.65(10) . . ? N1 Zn1 Yb 130.97(9) . . ? O3 Zn1 Yb 44.55(7) . . ? O12 Zn2 N4 110.69(13) . . ? O12 Zn2 O6 113.56(12) . . ? N4 Zn2 O6 135.73(13) . . ? O12 Zn2 O7 100.78(11) . . ? N4 Zn2 O7 91.41(12) . . ? O6 Zn2 O7 79.58(10) . . ? O12 Zn2 N3 106.94(14) . . ? N4 Zn2 N3 80.21(14) . . ? O6 Zn2 N3 88.06(12) . . ? O7 Zn2 N3 152.24(13) . . ? O12 Zn2 Yb 93.30(8) . . ? N4 Zn2 Yb 135.04(10) . . ? O6 Zn2 Yb 41.65(7) . . ? O7 Zn2 Yb 45.76(7) . . ? N3 Zn2 Yb 129.47(10) . . ? C2 O1 C1 114.2(3) . . ? C2 O1 Yb 116.2(2) . . ? C1 O1 Yb 129.4(2) . . ? C7 O2 Zn1 127.7(2) . . ? C7 O2 Yb 129.3(2) . . ? Zn1 O2 Yb 101.83(10) . . ? C12 O3 Zn1 125.7(2) . . ? C12 O3 Yb 136.7(2) . . ? Zn1 O3 Yb 97.60(10) . . ? C17 O4 C18 117.0(3) . . ? C17 O4 Yb 114.3(2) . . ? C18 O4 Yb 126.6(2) . . ? C8 N1 C9 121.8(3) . . ? C8 N1 Zn1 127.4(3) . . ? C9 N1 Zn1 109.7(3) . . ? C11 N2 C10 120.2(3) . . ? C11 N2 Zn1 125.7(3) . . ? C10 N2 Zn1 113.9(3) . . ? O1 C2 C3 125.5(3) . . ? O1 C2 C7 113.1(3) . . ? C3 C2 C7 121.4(3) . . ? C2 C3 C4 119.3(3) . . ? C5 C4 C3 120.7(4) . . ? C4 C5 C6 120.6(4) . . ? C7 C6 C5 119.8(3) . . ? C7 C6 C8 122.6(3) . . ? C5 C6 C8 117.3(3) . . ? O2 C7 C6 125.9(3) . . ? O2 C7 C2 116.1(3) . . ? C6 C7 C2 118.0(3) . . ? N1 C8 C6 125.6(4) . . ? N1 C9 C10 108.4(3) . . ? N2 C10 C9 110.2(3) . . ? N2 C11 C13 126.4(4) . . ? O3 C12 C17 118.3(3) . . ? O3 C12 C13 124.5(3) . . ? C17 C12 C13 117.2(3) . . ? C12 C13 C14 119.1(4) . . ? C12 C13 C11 124.4(4) . . ? C14 C13 C11 116.3(4) . . ? C15 C14 C13 121.5(4) . . ? C14 C15 C16 119.9(4) . . ? C17 C16 C15 119.4(4) . . ? O4 C17 C16 124.4(4) . . ? O4 C17 C12 113.2(3) . . ? C16 C17 C12 122.3(4) . . ? C20 O5 C19 116.2(3) . . ? C20 O5 Yb 116.8(2) . . ? C19 O5 Yb 126.9(2) . . ? C25 O6 Zn2 129.2(2) . . ? C25 O6 Yb 129.1(2) . . ? Zn2 O6 Yb 101.40(10) . . ? C30 O7 Zn2 125.8(2) . . ? C30 O7 Yb 134.9(2) . . ? Zn2 O7 Yb 96.65(9) . . ? C35 O8 C36 115.9(3) . . ? C35 O8 Yb 114.9(2) . . ? C36 O8 Yb 129.0(2) . . ? C26 N3 C27 121.9(4) . . ? C26 N3 Zn2 128.7(3) . . ? C27 N3 Zn2 108.2(3) . . ? C29 N4 C28 119.5(3) . . ? C29 N4 Zn2 126.4(3) . . ? C28 N4 Zn2 113.3(3) . . ? C21 C20 O5 125.3(4) . . ? C21 C20 C25 122.0(4) . . ? O5 C20 C25 112.6(3) . . ? C20 C21 C22 119.1(4) . . ? C23 C22 C21 120.1(4) . . ? C22 C23 C24 121.7(4) . . ? C25 C24 C23 118.5(4) . . ? C25 C24 C26 123.8(4) . . ? C23 C24 C26 117.6(4) . . ? O6 C25 C20 117.3(3) . . ? O6 C25 C24 124.2(3) . . ? C20 C25 C24 118.4(3) . . ? N3 C26 C24 125.3(4) . . ? N3 C27 C28 108.0(4) . . ? N4 C28 C27 111.4(4) . . ? N4 C29 C31 125.7(4) . . ? O7 C30 C31 125.1(3) . . ? O7 C30 C35 117.3(3) . . ? C31 C30 C35 117.5(3) . . ? C30 C31 C32 118.7(4) . . ? C30 C31 C29 125.4(4) . . ? C32 C31 C29 115.7(4) . . ? C33 C32 C31 122.5(4) . . ? C32 C33 C34 119.9(4) . . ? C35 C34 C33 119.4(4) . . ? O8 C35 C34 125.2(4) . . ? O8 C35 C30 112.9(3) . . ? C34 C35 C30 122.0(4) . . ? C37 O9 Yb 148.5(3) . . ? C37 O10 Zn1 114.6(2) . . ? O9 C37 O10 123.7(3) . . ? O9 C37 C38 117.8(3) . . ? O10 C37 C38 118.6(3) . . ? C39 O11 Yb 149.1(3) . . ? C39 O12 Zn2 113.8(3) . . ? O11 C39 O12 124.3(4) . . ? O11 C39 C40 118.2(4) . . ? O12 C39 C40 117.5(4) . . ? C53 B1 C47 107.1(3) . . ? C53 B1 C41 111.2(3) . . ? C47 B1 C41 111.0(3) . . ? C53 B1 C59 111.7(3) . . ? C47 B1 C59 110.0(3) . . ? C41 B1 C59 105.9(3) . . ? C46 C41 C42 114.2(4) . . ? C46 C41 B1 120.9(3) . . ? C42 C41 B1 124.9(4) . . ? C43 C42 C41 123.2(4) . . ? C42 C43 C44 120.8(4) . . ? C45 C44 C43 117.8(4) . . ? C44 C45 C46 120.3(4) . . ? C45 C46 C41 123.7(4) . . ? C52 C47 C48 114.6(4) . . ? C52 C47 B1 125.5(4) . . ? C48 C47 B1 119.9(3) . . ? C49 C48 C47 123.4(4) . . ? C48 C49 C50 119.2(5) . . ? C51 C50 C49 119.5(4) . . ? C50 C51 C52 120.4(4) . . ? C51 C52 C47 122.8(4) . . ? C58 C53 C54 114.1(4) . . ? C58 C53 B1 125.9(4) . . ? C54 C53 B1 120.0(3) . . ? C55 C54 C53 122.8(4) . . ? C54 C55 C56 120.7(4) . . ? C57 C56 C55 118.4(4) . . ? C56 C57 C58 120.3(5) . . ? C57 C58 C53 123.6(4) . . ? C60 C59 C64 114.5(4) . . ? C60 C59 B1 123.8(3) . . ? C64 C59 B1 121.6(3) . . ? C61 C60 C59 123.2(4) . . ? C62 C61 C60 120.3(4) . . ? C63 C62 C61 118.4(4) . . ? C62 C63 C64 120.7(4) . . ? C63 C64 C59 122.8(4) . . ? N5 C65 C66 173.9(9) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.128 _refine_diff_density_min -1.137 _refine_diff_density_rms 0.134