# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hongshan He' _publ_contact_author_email HONGSHAN.HE@SDSTATE.EDU _publ_section_title ; Structure and Photophysics of Near-infrared Emissive Ytterbium (?) Monoporphyrinate Acetate Complexes Having Neutral Bidentate Ligands ; loop_ _publ_author_name 'Hongshan He' 'P. Stanley May' 'A Sykes' # Attachment 'CIF.txt' data_08060_4 _database_code_depnum_ccdc_archive 'CCDC 731407' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Yb-TPP-4,7-Me-Phen-Acetate) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H43 N6 O2 Yb' _chemical_formula_weight 1053.04 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2453(6) _cell_length_b 13.4713(7) _cell_length_c 18.5620(10) _cell_angle_alpha 74.6050(10) _cell_angle_beta 89.8300(10) _cell_angle_gamma 68.7340(10) _cell_volume 2289.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple-red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1062 _exptl_absorpt_coefficient_mu 2.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6442 _exptl_absorpt_correction_T_max 0.8021 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23222 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.39 _reflns_number_total 8417 _reflns_number_gt 7089 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII (Bruker, 2006)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2006)' _computing_data_reduction 'Bruker SAINT (Bruker, 2006)' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'Ortep-3(Farrugia, 1997)' _computing_publication_material 'WinGX(Farrugia, 1999)' _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^)+(0.0469P)^2^+2.6104P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8417 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0712(5) 0.2557(4) 0.4238(3) 0.0147(10) Uani 1 1 d . . . C2 C 0.1597(5) 0.1509(4) 0.4190(3) 0.0157(10) Uani 1 1 d . . . C3 C 0.1645(5) 0.0463(4) 0.4680(3) 0.0166(10) Uani 1 1 d . . . H3 H 0.1057 0.0369 0.5053 0.020 Uiso 1 1 calc R . . C4 C 0.2688(5) -0.0346(4) 0.4499(3) 0.0162(10) Uani 1 1 d . . . H4 H 0.2968 -0.1105 0.4726 0.019 Uiso 1 1 calc R . . C5 C 0.3298(5) 0.0183(4) 0.3885(3) 0.0147(10) Uani 1 1 d . . . C6 C 0.4519(5) -0.0376(4) 0.3575(3) 0.0157(10) Uani 1 1 d . . . C7 C 0.5123(5) 0.0137(4) 0.2986(3) 0.0154(10) Uani 1 1 d . . . C8 C 0.6507(5) -0.0389(4) 0.2773(3) 0.0173(10) Uani 1 1 d . . . H8 H 0.7126 -0.1117 0.2986 0.021 Uiso 1 1 calc R . . C9 C 0.6729(5) 0.0373(4) 0.2212(3) 0.0187(11) Uani 1 1 d . . . H9 H 0.7539 0.0271 0.1966 0.022 Uiso 1 1 calc R . . C10 C 0.5500(5) 0.1371(4) 0.2057(3) 0.0156(10) Uani 1 1 d . . . C11 C 0.5348(5) 0.2372(4) 0.1519(3) 0.0161(10) Uani 1 1 d . . . C12 C 0.4319(5) 0.3421(4) 0.1479(3) 0.0160(10) Uani 1 1 d . . . C13 C 0.4209(5) 0.4460(4) 0.0966(3) 0.0184(11) Uani 1 1 d . . . H13 H 0.4706 0.4552 0.0549 0.022 Uiso 1 1 calc R . . C14 C 0.3253(5) 0.5280(4) 0.1195(3) 0.0182(11) Uani 1 1 d . . . H14 H 0.2987 0.6040 0.0976 0.022 Uiso 1 1 calc R . . C15 C 0.2721(5) 0.4752(4) 0.1847(3) 0.0151(10) Uani 1 1 d . . . C16 C 0.1739(5) 0.5321(4) 0.2276(3) 0.0150(10) Uani 1 1 d . . . C17 C 0.1169(5) 0.4814(4) 0.2894(3) 0.0161(10) Uani 1 1 d . . . C18 C 0.0328(5) 0.5391(4) 0.3383(3) 0.0191(11) Uani 1 1 d . . . H18 H 0.0051 0.6144 0.3341 0.023 Uiso 1 1 calc R . . C19 C 0.0015(5) 0.4634(4) 0.3915(3) 0.0186(11) Uani 1 1 d . . . H19 H -0.0529 0.4769 0.4306 0.022 Uiso 1 1 calc R . . C20 C 0.0682(5) 0.3578(4) 0.3766(3) 0.0140(10) Uani 1 1 d . . . C21 C -0.0219(5) 0.2597(4) 0.4864(3) 0.0137(10) Uani 1 1 d . . . C22 C -0.1675(5) 0.3115(4) 0.4711(3) 0.0174(10) Uani 1 1 d . . . H22 H -0.2073 0.3475 0.4217 0.021 Uiso 1 1 calc R . . C23 C -0.2543(5) 0.3101(4) 0.5288(3) 0.0185(11) Uani 1 1 d . . . H23 H -0.3515 0.3444 0.5178 0.022 Uiso 1 1 calc R . . C24 C -0.1965(6) 0.2581(4) 0.6018(3) 0.0246(12) Uani 1 1 d . . . H24 H -0.2546 0.2566 0.6403 0.030 Uiso 1 1 calc R . . C25 C -0.0525(6) 0.2082(4) 0.6181(3) 0.0236(12) Uani 1 1 d . . . H25 H -0.0136 0.1735 0.6678 0.028 Uiso 1 1 calc R . . C26 C 0.0347(5) 0.2095(4) 0.5610(3) 0.0201(11) Uani 1 1 d . . . H26 H 0.1319 0.1766 0.5726 0.024 Uiso 1 1 calc R . . C27 C 0.5265(5) -0.1591(4) 0.3942(3) 0.0189(11) Uani 1 1 d . . . C28 C 0.5803(5) -0.1974(4) 0.4696(3) 0.0201(11) Uani 1 1 d . . . H28 H 0.5703 -0.1468 0.4969 0.024 Uiso 1 1 calc R . . C29 C 0.6487(5) -0.3101(4) 0.5042(3) 0.0261(12) Uani 1 1 d . . . H29 H 0.6830 -0.3347 0.5548 0.031 Uiso 1 1 calc R . . C30 C 0.6660(6) -0.3857(5) 0.4640(3) 0.0320(14) Uani 1 1 d . . . H30 H 0.7119 -0.4612 0.4873 0.038 Uiso 1 1 calc R . . C31 C 0.6154(6) -0.3493(4) 0.3894(4) 0.0318(14) Uani 1 1 d . . . H31 H 0.6275 -0.4003 0.3622 0.038 Uiso 1 1 calc R . . C32 C 0.5461(5) -0.2360(4) 0.3543(3) 0.0238(12) Uani 1 1 d . . . H32 H 0.5128 -0.2120 0.3037 0.029 Uiso 1 1 calc R . . C33 C 0.6477(5) 0.2303(4) 0.0991(3) 0.0167(10) Uani 1 1 d . . . C34 C 0.6771(5) 0.1567(4) 0.0553(3) 0.0215(11) Uani 1 1 d . . . H34 H 0.6210 0.1158 0.0552 0.026 Uiso 1 1 calc R . . C35 C 0.7889(6) 0.1442(4) 0.0122(3) 0.0278(13) Uani 1 1 d . . . H35 H 0.8062 0.0957 -0.0173 0.033 Uiso 1 1 calc R . . C36 C 0.8746(5) 0.2019(4) 0.0123(3) 0.0254(12) Uani 1 1 d . . . H36 H 0.9512 0.1913 -0.0159 0.031 Uiso 1 1 calc R . . C37 C 0.8464(5) 0.2755(5) 0.0542(3) 0.0259(12) Uani 1 1 d . . . H37 H 0.9036 0.3155 0.0544 0.031 Uiso 1 1 calc R . . C38 C 0.7318(5) 0.2905(4) 0.0966(3) 0.0219(11) Uani 1 1 d . . . H38 H 0.7120 0.3422 0.1237 0.026 Uiso 1 1 calc R . . C39 C 0.1278(5) 0.6556(4) 0.2065(3) 0.0167(10) Uani 1 1 d . . . C40 C 0.2206(5) 0.7069(4) 0.2133(3) 0.0199(11) Uani 1 1 d . . . H40 H 0.3144 0.6635 0.2310 0.024 Uiso 1 1 calc R . . C41 C 0.1760(6) 0.8219(4) 0.1941(3) 0.0258(12) Uani 1 1 d . . . H41 H 0.2397 0.8548 0.1994 0.031 Uiso 1 1 calc R . . C42 C 0.0385(6) 0.8868(4) 0.1676(3) 0.0259(12) Uani 1 1 d . . . H42 H 0.0087 0.9638 0.1549 0.031 Uiso 1 1 calc R . . C43 C -0.0553(6) 0.8379(4) 0.1597(3) 0.0237(12) Uani 1 1 d . . . H43 H -0.1483 0.8820 0.1408 0.028 Uiso 1 1 calc R . . C44 C -0.0121(5) 0.7231(4) 0.1799(3) 0.0214(11) Uani 1 1 d . . . H44 H -0.0770 0.6908 0.1756 0.026 Uiso 1 1 calc R . . C45 C 0.0097(5) 0.4788(4) 0.1030(3) 0.0194(11) Uani 1 1 d . . . H45 H 0.0947 0.4686 0.0823 0.023 Uiso 1 1 calc R . . C46 C -0.1065(5) 0.5755(4) 0.0693(3) 0.0232(12) Uani 1 1 d . . . H46 H -0.0985 0.6259 0.0259 0.028 Uiso 1 1 calc R . . C47 C -0.2328(5) 0.5964(4) 0.1001(3) 0.0225(11) Uani 1 1 d . . . C48 C -0.3585(6) 0.7011(5) 0.0642(4) 0.0391(15) Uani 1 1 d . . . H48A H -0.4372 0.7023 0.0926 0.059 Uiso 1 1 calc R . . H48B H -0.3820 0.7029 0.0137 0.059 Uiso 1 1 calc R . . H48C H -0.3361 0.7647 0.0634 0.059 Uiso 1 1 calc R . . C49 C -0.2411(5) 0.5156(4) 0.1642(3) 0.0218(11) Uani 1 1 d . . . C50 C -0.1207(5) 0.4168(4) 0.1920(3) 0.0171(10) Uani 1 1 d . . . C51 C -0.3667(5) 0.5240(4) 0.2004(3) 0.0247(12) Uani 1 1 d . . . H51 H -0.4438 0.5910 0.1865 0.030 Uiso 1 1 calc R . . C52 C -0.3771(5) 0.4374(4) 0.2544(3) 0.0240(12) Uani 1 1 d . . . H52 H -0.4600 0.4468 0.2772 0.029 Uiso 1 1 calc R . . C53 C -0.2629(5) 0.3322(4) 0.2766(3) 0.0213(11) Uani 1 1 d . . . C54 C -0.1325(5) 0.3238(4) 0.2478(3) 0.0180(11) Uani 1 1 d . . . C55 C -0.4076(6) 0.2364(5) 0.3575(3) 0.0293(13) Uani 1 1 d . . . H55A H -0.4745 0.3116 0.3437 0.044 Uiso 1 1 calc R . . H55B H -0.3885 0.2091 0.4112 0.044 Uiso 1 1 calc R . . H55C H -0.4456 0.1909 0.3395 0.044 Uiso 1 1 calc R . . C56 C -0.2740(5) 0.2325(5) 0.3234(3) 0.0214(11) Uani 1 1 d . . . C57 C -0.1610(5) 0.1372(4) 0.3336(3) 0.0233(12) Uani 1 1 d . . . H57 H -0.1673 0.0705 0.3605 0.028 Uiso 1 1 calc R . . C58 C -0.0333(5) 0.1363(4) 0.3044(3) 0.0209(11) Uani 1 1 d . . . H58 H 0.0429 0.0690 0.3138 0.025 Uiso 1 1 calc R . . C59 C 0.2302(5) 0.1274(4) 0.1370(3) 0.0235(12) Uani 1 1 d . . . C60 C 0.2634(7) 0.0618(5) 0.0815(3) 0.0390(15) Uani 1 1 d . . . H60A H 0.2745 0.1073 0.0343 0.059 Uiso 1 1 calc R . . H60B H 0.1879 0.0378 0.0749 0.059 Uiso 1 1 calc R . . H60C H 0.3491 -0.0018 0.0996 0.059 Uiso 1 1 calc R . . N1 N 0.3344(4) 0.3614(3) 0.1996(2) 0.0126(8) Uani 1 1 d . . . N2 N 0.1378(4) 0.3702(3) 0.3130(2) 0.0128(8) Uani 1 1 d . . . N3 N 0.2576(4) 0.1308(3) 0.3688(2) 0.0140(8) Uani 1 1 d . . . N4 N 0.4533(4) 0.1212(3) 0.2543(2) 0.0152(9) Uani 1 1 d . . . N5 N 0.0052(4) 0.4004(3) 0.1634(2) 0.0156(9) Uani 1 1 d . . . N6 N -0.0185(4) 0.2274(3) 0.2642(2) 0.0178(9) Uani 1 1 d . . . O1 O 0.2277(3) 0.2256(3) 0.11752(19) 0.0213(8) Uani 1 1 d . . . O2 O 0.2116(4) 0.0834(3) 0.20312(19) 0.0231(8) Uani 1 1 d . . . Yb1 Yb 0.21517(2) 0.240216(17) 0.241941(12) 0.01366(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.011(2) 0.022(3) 0.013(2) -0.007(2) 0.0033(19) -0.007(2) C2 0.015(2) 0.017(3) 0.013(2) -0.001(2) 0.0024(19) -0.006(2) C3 0.018(2) 0.021(3) 0.009(2) 0.000(2) 0.0012(19) -0.007(2) C4 0.017(2) 0.012(2) 0.015(2) 0.0022(19) -0.0006(19) -0.004(2) C5 0.015(2) 0.012(2) 0.014(2) -0.0002(19) 0.0005(19) -0.0040(19) C6 0.015(2) 0.012(2) 0.018(3) -0.002(2) 0.0024(19) -0.004(2) C7 0.017(2) 0.013(2) 0.015(2) -0.005(2) 0.0019(19) -0.004(2) C8 0.017(3) 0.012(2) 0.020(3) -0.007(2) 0.004(2) 0.000(2) C9 0.016(2) 0.018(3) 0.020(3) -0.007(2) 0.007(2) -0.003(2) C10 0.016(2) 0.016(2) 0.016(2) -0.008(2) 0.0061(19) -0.004(2) C11 0.013(2) 0.018(3) 0.017(3) -0.007(2) 0.0057(19) -0.004(2) C12 0.013(2) 0.018(3) 0.015(3) -0.003(2) 0.0023(19) -0.004(2) C13 0.017(3) 0.022(3) 0.014(2) -0.001(2) 0.007(2) -0.007(2) C14 0.019(3) 0.016(2) 0.013(2) 0.001(2) 0.006(2) -0.003(2) C15 0.014(2) 0.017(2) 0.012(2) -0.0027(19) 0.0024(19) -0.003(2) C16 0.011(2) 0.014(2) 0.018(3) -0.004(2) 0.0038(19) -0.0029(19) C17 0.012(2) 0.015(2) 0.016(3) -0.001(2) 0.0027(19) -0.0012(19) C18 0.019(3) 0.016(3) 0.019(3) -0.004(2) 0.009(2) -0.005(2) C19 0.018(3) 0.022(3) 0.014(2) -0.007(2) 0.008(2) -0.003(2) C20 0.010(2) 0.017(2) 0.011(2) -0.0014(19) 0.0016(18) -0.0021(19) C21 0.018(2) 0.011(2) 0.014(2) -0.0042(19) 0.0074(19) -0.0067(19) C22 0.020(3) 0.017(3) 0.018(3) -0.006(2) 0.004(2) -0.009(2) C23 0.013(2) 0.019(3) 0.028(3) -0.013(2) 0.010(2) -0.007(2) C24 0.028(3) 0.033(3) 0.025(3) -0.016(2) 0.018(2) -0.020(3) C25 0.036(3) 0.025(3) 0.012(3) -0.002(2) 0.007(2) -0.016(2) C26 0.021(3) 0.023(3) 0.016(3) -0.005(2) 0.004(2) -0.009(2) C27 0.010(2) 0.015(3) 0.029(3) -0.003(2) 0.006(2) -0.003(2) C28 0.014(2) 0.021(3) 0.024(3) -0.003(2) 0.005(2) -0.007(2) C29 0.012(3) 0.026(3) 0.029(3) 0.004(2) 0.005(2) -0.003(2) C30 0.018(3) 0.018(3) 0.047(4) 0.002(3) 0.013(3) -0.001(2) C31 0.028(3) 0.019(3) 0.050(4) -0.014(3) 0.017(3) -0.008(2) C32 0.022(3) 0.019(3) 0.029(3) -0.007(2) 0.007(2) -0.006(2) C33 0.017(2) 0.016(2) 0.013(2) -0.002(2) 0.0030(19) -0.002(2) C34 0.021(3) 0.022(3) 0.018(3) -0.004(2) 0.005(2) -0.006(2) C35 0.032(3) 0.025(3) 0.019(3) -0.008(2) 0.009(2) -0.001(2) C36 0.017(3) 0.035(3) 0.016(3) -0.002(2) 0.008(2) -0.004(2) C37 0.021(3) 0.036(3) 0.023(3) -0.009(2) 0.008(2) -0.012(2) C38 0.019(3) 0.025(3) 0.021(3) -0.008(2) 0.007(2) -0.007(2) C39 0.021(3) 0.015(2) 0.012(2) -0.0010(19) 0.0068(19) -0.005(2) C40 0.020(3) 0.017(3) 0.020(3) -0.004(2) 0.010(2) -0.005(2) C41 0.032(3) 0.024(3) 0.027(3) -0.008(2) 0.018(2) -0.015(2) C42 0.036(3) 0.014(3) 0.024(3) -0.006(2) 0.019(2) -0.006(2) C43 0.028(3) 0.016(3) 0.015(3) -0.004(2) 0.006(2) 0.003(2) C44 0.024(3) 0.021(3) 0.019(3) -0.007(2) 0.007(2) -0.007(2) C45 0.023(3) 0.023(3) 0.014(3) -0.004(2) 0.003(2) -0.011(2) C46 0.029(3) 0.021(3) 0.018(3) -0.001(2) 0.001(2) -0.011(2) C47 0.019(3) 0.020(3) 0.021(3) 0.000(2) -0.004(2) -0.003(2) C48 0.029(3) 0.032(3) 0.039(4) 0.006(3) -0.001(3) -0.004(3) C49 0.018(3) 0.025(3) 0.021(3) -0.007(2) -0.002(2) -0.006(2) C50 0.016(2) 0.021(3) 0.013(2) -0.002(2) -0.0010(19) -0.007(2) C51 0.014(3) 0.027(3) 0.025(3) -0.008(2) 0.002(2) 0.001(2) C52 0.011(2) 0.032(3) 0.027(3) -0.008(2) 0.003(2) -0.006(2) C53 0.018(3) 0.032(3) 0.015(3) -0.007(2) 0.000(2) -0.010(2) C54 0.017(3) 0.024(3) 0.014(3) -0.006(2) 0.004(2) -0.009(2) C55 0.025(3) 0.043(3) 0.021(3) -0.003(3) 0.004(2) -0.017(3) C56 0.022(3) 0.040(3) 0.012(2) -0.010(2) 0.007(2) -0.021(3) C57 0.028(3) 0.025(3) 0.019(3) 0.004(2) -0.004(2) -0.020(2) C58 0.020(3) 0.022(3) 0.018(3) -0.002(2) -0.002(2) -0.007(2) C59 0.020(3) 0.027(3) 0.026(3) -0.007(2) 0.004(2) -0.012(2) C60 0.066(5) 0.033(3) 0.032(3) -0.015(3) 0.016(3) -0.030(3) N1 0.013(2) 0.013(2) 0.012(2) -0.0045(16) 0.0047(16) -0.0043(16) N2 0.0108(19) 0.012(2) 0.013(2) -0.0011(16) 0.0047(16) -0.0033(16) N3 0.015(2) 0.013(2) 0.013(2) -0.0027(16) 0.0041(16) -0.0043(16) N4 0.017(2) 0.014(2) 0.014(2) -0.0037(17) 0.0065(16) -0.0049(17) N5 0.017(2) 0.015(2) 0.015(2) -0.0027(17) 0.0023(16) -0.0065(17) N6 0.019(2) 0.018(2) 0.013(2) 0.0007(17) 0.0025(17) -0.0070(18) O1 0.0223(19) 0.0185(19) 0.0199(19) -0.0038(15) 0.0005(15) -0.0051(15) O2 0.027(2) 0.0219(19) 0.021(2) -0.0037(15) 0.0050(15) -0.0115(16) Yb1 0.01274(11) 0.01271(11) 0.01291(11) -0.00194(8) 0.00369(7) -0.00300(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.400(6) . ? C1 C20 1.411(6) . ? C1 C21 1.501(6) . ? C2 N3 1.371(6) . ? C2 C3 1.444(7) . ? C3 C4 1.338(7) . ? C3 H3 0.9300 . ? C4 C5 1.444(6) . ? C4 H4 0.9300 . ? C5 N3 1.368(6) . ? C5 C6 1.416(6) . ? C6 C7 1.400(6) . ? C6 C27 1.494(6) . ? C7 N4 1.369(6) . ? C7 C8 1.444(6) . ? C8 C9 1.337(7) . ? C8 H8 0.9300 . ? C9 C10 1.430(6) . ? C9 H9 0.9300 . ? C10 N4 1.373(6) . ? C10 C11 1.405(7) . ? C11 C12 1.406(6) . ? C11 C33 1.508(6) . ? C12 N1 1.388(6) . ? C12 C13 1.433(7) . ? C13 C14 1.351(7) . ? C13 H13 0.9300 . ? C14 C15 1.444(6) . ? C14 H14 0.9300 . ? C15 N1 1.379(6) . ? C15 C16 1.411(6) . ? C16 C17 1.412(6) . ? C16 C39 1.494(6) . ? C17 N2 1.379(6) . ? C17 C18 1.433(6) . ? C18 C19 1.350(7) . ? C18 H18 0.9300 . ? C19 C20 1.438(6) . ? C19 H19 0.9300 . ? C20 N2 1.382(6) . ? C21 C26 1.391(7) . ? C21 C22 1.391(7) . ? C22 C23 1.390(6) . ? C22 H22 0.9300 . ? C23 C24 1.370(7) . ? C23 H23 0.9300 . ? C24 C25 1.377(7) . ? C24 H24 0.9300 . ? C25 C26 1.386(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.385(7) . ? C27 C28 1.393(7) . ? C28 C29 1.386(7) . ? C28 H28 0.9300 . ? C29 C30 1.377(8) . ? C29 H29 0.9300 . ? C30 C31 1.373(8) . ? C30 H30 0.9300 . ? C31 C32 1.395(7) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.374(7) . ? C33 C34 1.394(7) . ? C34 C35 1.381(7) . ? C34 H34 0.9300 . ? C35 C36 1.369(8) . ? C35 H35 0.9300 . ? C36 C37 1.368(8) . ? C36 H36 0.9300 . ? C37 C38 1.395(7) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.386(7) . ? C39 C44 1.394(7) . ? C40 C41 1.390(7) . ? C40 H40 0.9300 . ? C41 C42 1.368(8) . ? C41 H41 0.9300 . ? C42 C43 1.375(8) . ? C42 H42 0.9300 . ? C43 C44 1.388(7) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 N5 1.334(6) . ? C45 C46 1.397(7) . ? C45 H45 0.9300 . ? C46 C47 1.378(7) . ? C46 H46 0.9300 . ? C47 C49 1.409(7) . ? C47 C48 1.510(7) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.417(7) . ? C49 C51 1.432(7) . ? C50 N5 1.359(6) . ? C50 C54 1.441(7) . ? C51 C52 1.358(7) . ? C51 H51 0.9300 . ? C52 C53 1.427(7) . ? C52 H52 0.9300 . ? C53 C54 1.415(7) . ? C53 C56 1.435(7) . ? C54 N6 1.355(6) . ? C55 C56 1.496(7) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.349(7) . ? C57 C58 1.412(7) . ? C57 H57 0.9300 . ? C58 N6 1.317(6) . ? C58 H58 0.9300 . ? C59 O2 1.260(6) . ? C59 O1 1.266(6) . ? C59 C60 1.491(7) . ? C59 Yb1 2.743(5) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? N1 Yb1 2.352(4) . ? N2 Yb1 2.376(4) . ? N3 Yb1 2.367(4) . ? N4 Yb1 2.355(4) . ? N5 Yb1 2.528(4) . ? N6 Yb1 2.488(4) . ? O1 Yb1 2.369(3) . ? O2 Yb1 2.418(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C20 124.9(4) . . ? C2 C1 C21 117.6(4) . . ? C20 C1 C21 117.4(4) . . ? N3 C2 C1 125.9(4) . . ? N3 C2 C3 109.1(4) . . ? C1 C2 C3 124.9(4) . . ? C4 C3 C2 107.5(4) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? C3 C4 C5 107.0(4) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? N3 C5 C6 125.5(4) . . ? N3 C5 C4 109.6(4) . . ? C6 C5 C4 124.8(4) . . ? C7 C6 C5 124.9(4) . . ? C7 C6 C27 118.0(4) . . ? C5 C6 C27 117.0(4) . . ? N4 C7 C6 126.1(4) . . ? N4 C7 C8 109.4(4) . . ? C6 C7 C8 124.5(4) . . ? C9 C8 C7 106.9(4) . . ? C9 C8 H8 126.6 . . ? C7 C8 H8 126.6 . . ? C8 C9 C10 107.9(4) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? N4 C10 C11 125.7(4) . . ? N4 C10 C9 109.3(4) . . ? C11 C10 C9 124.9(4) . . ? C10 C11 C12 125.6(4) . . ? C10 C11 C33 115.6(4) . . ? C12 C11 C33 118.5(4) . . ? N1 C12 C11 123.9(4) . . ? N1 C12 C13 109.5(4) . . ? C11 C12 C13 126.3(4) . . ? C14 C13 C12 107.7(4) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? C13 C14 C15 106.9(4) . . ? C13 C14 H14 126.5 . . ? C15 C14 H14 126.5 . . ? N1 C15 C16 125.3(4) . . ? N1 C15 C14 109.8(4) . . ? C16 C15 C14 124.9(4) . . ? C15 C16 C17 125.2(4) . . ? C15 C16 C39 117.5(4) . . ? C17 C16 C39 117.3(4) . . ? N2 C17 C16 125.4(4) . . ? N2 C17 C18 110.6(4) . . ? C16 C17 C18 123.9(4) . . ? C19 C18 C17 106.9(4) . . ? C19 C18 H18 126.5 . . ? C17 C18 H18 126.5 . . ? C18 C19 C20 107.2(4) . . ? C18 C19 H19 126.4 . . ? C20 C19 H19 126.4 . . ? N2 C20 C1 125.2(4) . . ? N2 C20 C19 110.1(4) . . ? C1 C20 C19 124.5(4) . . ? C26 C21 C22 118.3(4) . . ? C26 C21 C1 120.9(4) . . ? C22 C21 C1 120.8(4) . . ? C23 C22 C21 120.8(5) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 120.0(5) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.0(5) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 120.3(5) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 120.5(5) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C32 C27 C28 118.4(5) . . ? C32 C27 C6 121.2(5) . . ? C28 C27 C6 120.4(5) . . ? C29 C28 C27 120.8(5) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C30 C29 C28 120.1(5) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 119.9(5) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.2(5) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C27 C32 C31 120.6(5) . . ? C27 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C38 C33 C34 117.8(4) . . ? C38 C33 C11 121.0(4) . . ? C34 C33 C11 121.1(4) . . ? C35 C34 C33 120.4(5) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C36 C35 C34 121.1(5) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C37 C36 C35 119.2(5) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C37 C38 120.0(5) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C33 C38 C37 121.3(5) . . ? C33 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C40 C39 C44 117.9(4) . . ? C40 C39 C16 121.7(4) . . ? C44 C39 C16 120.3(4) . . ? C39 C40 C41 121.1(5) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 120.1(5) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 119.8(5) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C42 C43 C44 120.4(5) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 120.6(5) . . ? C43 C44 H44 119.7 . . ? C39 C44 H44 119.7 . . ? N5 C45 C46 123.5(5) . . ? N5 C45 H45 118.2 . . ? C46 C45 H45 118.2 . . ? C47 C46 C45 120.1(5) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C49 117.8(5) . . ? C46 C47 C48 120.4(5) . . ? C49 C47 C48 121.8(5) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 C50 118.3(5) . . ? C47 C49 C51 124.0(5) . . ? C50 C49 C51 117.6(5) . . ? N5 C50 C49 123.0(4) . . ? N5 C50 C54 116.9(4) . . ? C49 C50 C54 119.8(4) . . ? C52 C51 C49 122.2(5) . . ? C52 C51 H51 118.9 . . ? C49 C51 H51 118.9 . . ? C51 C52 C53 121.1(5) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C54 C53 C52 118.3(5) . . ? C54 C53 C56 117.6(5) . . ? C52 C53 C56 124.0(5) . . ? N6 C54 C53 122.9(5) . . ? N6 C54 C50 116.6(4) . . ? C53 C54 C50 120.2(4) . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C53 117.2(4) . . ? C57 C56 C55 122.5(5) . . ? C53 C56 C55 120.3(5) . . ? C56 C57 C58 121.5(5) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? N6 C58 C57 122.2(5) . . ? N6 C58 H58 118.9 . . ? C57 C58 H58 118.9 . . ? O2 C59 O1 121.0(5) . . ? O2 C59 C60 120.1(5) . . ? O1 C59 C60 118.8(5) . . ? O2 C59 Yb1 61.8(3) . . ? O1 C59 Yb1 59.6(3) . . ? C60 C59 Yb1 170.7(4) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C15 N1 C12 105.9(4) . . ? C15 N1 Yb1 123.8(3) . . ? C12 N1 Yb1 120.6(3) . . ? C17 N2 C20 105.2(4) . . ? C17 N2 Yb1 127.0(3) . . ? C20 N2 Yb1 125.6(3) . . ? C5 N3 C2 106.5(4) . . ? C5 N3 Yb1 121.6(3) . . ? C2 N3 Yb1 122.4(3) . . ? C7 N4 C10 106.4(4) . . ? C7 N4 Yb1 126.6(3) . . ? C10 N4 Yb1 125.3(3) . . ? C45 N5 C50 117.0(4) . . ? C45 N5 Yb1 126.0(3) . . ? C50 N5 Yb1 116.2(3) . . ? C58 N6 C54 118.2(4) . . ? C58 N6 Yb1 123.0(3) . . ? C54 N6 Yb1 117.3(3) . . ? C59 O1 Yb1 93.0(3) . . ? C59 O2 Yb1 90.8(3) . . ? N1 Yb1 N4 75.95(13) . . ? N1 Yb1 N3 120.01(13) . . ? N4 Yb1 N3 76.17(13) . . ? N1 Yb1 O1 83.08(12) . . ? N4 Yb1 O1 81.71(12) . . ? N3 Yb1 O1 141.91(12) . . ? N1 Yb1 N2 75.77(12) . . ? N4 Yb1 N2 120.91(13) . . ? N3 Yb1 N2 75.03(13) . . ? O1 Yb1 N2 142.91(12) . . ? N1 Yb1 O2 131.36(12) . . ? N4 Yb1 O2 75.17(13) . . ? N3 Yb1 O2 89.52(12) . . ? O1 Yb1 O2 54.68(11) . . ? N2 Yb1 O2 152.77(12) . . ? N1 Yb1 N6 145.15(13) . . ? N4 Yb1 N6 138.90(13) . . ? N3 Yb1 N6 78.70(13) . . ? O1 Yb1 N6 99.43(12) . . ? N2 Yb1 N6 82.30(13) . . ? O2 Yb1 N6 72.62(12) . . ? N1 Yb1 N5 83.82(12) . . ? N4 Yb1 N5 149.74(13) . . ? N3 Yb1 N5 134.00(12) . . ? O1 Yb1 N5 73.61(12) . . ? N2 Yb1 N5 74.09(13) . . ? O2 Yb1 N5 103.23(12) . . ? N6 Yb1 N5 64.10(12) . . ? N1 Yb1 C59 106.93(14) . . ? N4 Yb1 C59 75.16(14) . . ? N3 Yb1 C59 115.44(14) . . ? O1 Yb1 C59 27.46(13) . . ? N2 Yb1 C59 163.45(14) . . ? O2 Yb1 C59 27.33(13) . . ? N6 Yb1 C59 87.20(14) . . ? N5 Yb1 C59 89.83(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.073 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.128 #===END data_08061tw4_6 _database_code_depnum_ccdc_archive 'CCDC 731408' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Yb-TPP-EPO-Phen-Acetate).MeOH _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H41 N6 O4 Yb' _chemical_formula_weight 1071.02 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.766(2) _cell_length_b 13.559(3) _cell_length_c 17.444(3) _cell_angle_alpha 82.934(3) _cell_angle_beta 89.885(3) _cell_angle_gamma 88.619(3) _cell_volume 2291.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8487 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 25.70 _exptl_crystal_description plate _exptl_crystal_colour purple-red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1078 _exptl_absorpt_coefficient_mu 2.099 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5801 _exptl_absorpt_correction_T_max 0.8102 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8487 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.70 _reflns_number_total 8487 _reflns_number_gt 7553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII (Bruker, 2006)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2006)' _computing_data_reduction 'Bruker SAINT (Bruker, 2006)' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'Ortep-3(Farrugia, 1997)' _computing_publication_material 'WinGX(Farrugia, 1999)' _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^)+(0.0445P)^2^+1.4663P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8487 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.015 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1 C 0.3360(4) 0.1532(3) 0.5770(3) 0.0135(9) Uani 1 d . . . C2 C 0.4109(5) 0.2359(3) 0.5935(3) 0.0142(9) Uani 1 d . . . C3 C 0.4779(5) 0.3041(3) 0.5379(3) 0.0163(10) Uani 1 d . . . H3 H 0.4776 0.3042 0.4846 0.02 Uiso 1 calc R . . C4 C 0.5418(5) 0.3686(3) 0.5779(3) 0.0161(10) Uani 1 d . . . H4 H 0.5937 0.4218 0.5568 0.019 Uiso 1 calc R . . C5 C 0.5156(5) 0.3407(3) 0.6588(3) 0.0148(9) Uani 1 d . . . C6 C 0.5776(4) 0.3821(3) 0.7188(3) 0.0147(9) Uani 1 d . . . C7 C 0.5625(5) 0.3492(3) 0.7984(3) 0.0166(10) Uani 1 d . . . C8 C 0.6402(5) 0.3816(4) 0.8595(3) 0.0198(10) Uani 1 d . . . H8 H 0.7073 0.4295 0.8541 0.024 Uiso 1 calc R . . C9 C 0.5991(5) 0.3307(4) 0.9261(3) 0.0221(11) Uani 1 d . . . H9 H 0.6343 0.335 0.975 0.026 Uiso 1 calc R . . C10 C 0.4911(5) 0.2684(3) 0.9074(3) 0.0163(10) Uani 1 d . . . C11 C 0.4182(5) 0.2052(3) 0.9621(3) 0.0169(10) Uani 1 d . . . C12 C 0.3229(4) 0.1366(3) 0.9439(3) 0.0140(9) Uani 1 d . . . C13 C 0.2466(5) 0.0743(3) 0.9999(3) 0.0170(10) Uani 1 d . . . H13 H 0.2454 0.0764 1.053 0.02 Uiso 1 calc R . . C14 C 0.1763(5) 0.0117(3) 0.9606(3) 0.0166(10) Uani 1 d . . . H14 H 0.1182 -0.0378 0.9817 0.02 Uiso 1 calc R . . C15 C 0.2080(5) 0.0359(3) 0.8801(3) 0.0158(10) Uani 1 d . . . C16 C 0.1628(4) -0.0153(3) 0.8206(3) 0.0139(9) Uani 1 d . . . C17 C 0.1916(5) 0.0093(3) 0.7419(3) 0.0152(9) Uani 1 d . . . C18 C 0.1669(5) -0.0531(3) 0.6824(3) 0.0169(10) Uani 1 d . . . H18 H 0.1261 -0.1148 0.6892 0.02 Uiso 1 calc R . . C19 C 0.2138(5) -0.0056(3) 0.6144(3) 0.0176(10) Uani 1 d . . . H19 H 0.2105 -0.0281 0.5662 0.021 Uiso 1 calc R . . C20 C 0.2697(4) 0.0865(3) 0.6320(3) 0.0119(9) Uani 1 d . . . C21 C 0.3292(5) 0.1330(3) 0.4956(3) 0.0142(9) Uani 1 d . . . C22 C 0.2035(5) 0.1299(3) 0.4593(3) 0.0170(10) Uani 1 d . . . H22 H 0.124 0.1442 0.4856 0.02 Uiso 1 calc R . . C23 C 0.1943(5) 0.1057(3) 0.3845(3) 0.0206(10) Uani 1 d . . . H23 H 0.1091 0.1039 0.3611 0.025 Uiso 1 calc R . . C24 C 0.3126(5) 0.0841(3) 0.3445(3) 0.0200(10) Uani 1 d . . . H24 H 0.3067 0.0677 0.2944 0.024 Uiso 1 calc R . . C25 C 0.4387(5) 0.0871(3) 0.3797(3) 0.0182(10) Uani 1 d . . . H25 H 0.518 0.0728 0.3532 0.022 Uiso 1 calc R . . C26 C 0.4476(5) 0.1116(3) 0.4546(3) 0.0164(10) Uani 1 d . . . H26 H 0.533 0.1137 0.4778 0.02 Uiso 1 calc R . . C27 C 0.6702(5) 0.4667(3) 0.6994(3) 0.0147(9) Uani 1 d . . . C28 C 0.8110(5) 0.4537(4) 0.7107(3) 0.0199(10) Uani 1 d . . . H28 H 0.8474 0.3909 0.728 0.024 Uiso 1 calc R . . C29 C 0.8969(5) 0.5332(4) 0.6966(3) 0.0221(11) Uani 1 d . . . H29 H 0.9908 0.5244 0.7043 0.027 Uiso 1 calc R . . C30 C 0.8411(5) 0.6272(4) 0.6706(3) 0.0213(11) Uani 1 d . . . H30 H 0.8983 0.6813 0.6623 0.026 Uiso 1 calc R . . C31 C 0.7010(5) 0.6408(3) 0.6571(3) 0.0196(10) Uani 1 d . . . H31 H 0.665 0.7035 0.639 0.024 Uiso 1 calc R . . C32 C 0.6165(5) 0.5614(3) 0.6705(3) 0.0170(10) Uani 1 d . . . H32 H 0.5232 0.57 0.6604 0.02 Uiso 1 calc R . . C33 C 0.4463(5) 0.2114(4) 1.0452(3) 0.0208(10) Uani 1 d . . . C34 C 0.4289(5) 0.3016(4) 1.0753(3) 0.0273(12) Uani 1 d . . . H34 H 0.3984 0.3577 1.0432 0.033 Uiso 1 calc R . . C35 C 0.4565(6) 0.3088(5) 1.1524(3) 0.0336(14) Uani 1 d . . . H35 H 0.4465 0.3695 1.1717 0.04 Uiso 1 calc R . . C36 C 0.4992(6) 0.2243(5) 1.2007(3) 0.0353(14) Uani 1 d . . . H36 H 0.5156 0.2284 1.2527 0.042 Uiso 1 calc R . . C37 C 0.5175(5) 0.1339(5) 1.1718(3) 0.0292(13) Uani 1 d . . . H37 H 0.547 0.0779 1.2043 0.035 Uiso 1 calc R . . C38 C 0.4920(5) 0.1269(4) 1.0947(3) 0.0221(11) Uani 1 d . . . H38 H 0.505 0.0664 1.0755 0.026 Uiso 1 calc R . . C39 C 0.0823(5) -0.1060(3) 0.8427(3) 0.0160(10) Uani 1 d . . . C40 C -0.0464(5) -0.1139(4) 0.8104(3) 0.0186(10) Uani 1 d . . . H40 H -0.0815 -0.0627 0.775 0.022 Uiso 1 calc R . . C41 C -0.1220(5) -0.1976(4) 0.8309(3) 0.0239(11) Uani 1 d . . . H41 H -0.2073 -0.2036 0.8086 0.029 Uiso 1 calc R . . C42 C -0.0702(6) -0.2726(4) 0.8850(3) 0.0310(13) Uani 1 d . . . H42 H -0.1219 -0.3286 0.8992 0.037 Uiso 1 calc R . . C43 C 0.0572(6) -0.2654(4) 0.9180(3) 0.0309(13) Uani 1 d . . . H43 H 0.0904 -0.3159 0.9546 0.037 Uiso 1 calc R . . C44 C 0.1344(5) -0.1831(4) 0.8963(3) 0.0237(11) Uani 1 d . . . H44 H 0.2212 -0.1786 0.9172 0.028 Uiso 1 calc R . . C45 C 0.1701(5) 0.3747(3) 0.5932(3) 0.0189(10) Uani 1 d . . . H45 H 0.2501 0.4076 0.6017 0.023 Uiso 1 calc R . . C46 C 0.1041(5) 0.3989(4) 0.5222(3) 0.0206(10) Uani 1 d . . . H46 H 0.1388 0.4468 0.485 0.025 Uiso 1 calc R . . C47 C -0.0138(5) 0.3499(4) 0.5088(3) 0.0221(11) Uani 1 d . . . H47 H -0.0605 0.3637 0.4621 0.027 Uiso 1 calc R . . C48 C -0.0609(5) 0.2800(4) 0.5662(3) 0.0199(10) Uani 1 d . . . C49 C 0.0096(5) 0.2621(3) 0.6359(3) 0.0180(10) Uani 1 d . . . C50 C -0.1838(5) 0.2219(4) 0.5538(3) 0.0241(11) Uani 1 d . . . C51 C -0.2438(5) 0.1631(4) 0.6219(3) 0.0261(12) Uani 1 d . . . C52 C -0.1816(5) 0.1660(3) 0.6985(3) 0.0208(11) Uani 1 d . . . C53 C -0.2514(5) 0.1371(4) 0.7676(3) 0.0229(11) Uani 1 d . . . H53 H -0.3401 0.1139 0.7665 0.027 Uiso 1 calc R . . C54 C -0.1878(5) 0.1432(4) 0.8370(3) 0.0229(11) Uani 1 d . . . H54 H -0.2338 0.1254 0.8832 0.027 Uiso 1 calc R . . C55 C -0.0542(5) 0.1762(4) 0.8376(3) 0.0221(11) Uani 1 d . . . H55 H -0.0104 0.1772 0.8847 0.027 Uiso 1 calc R . . C56 C -0.0518(5) 0.2052(3) 0.7039(3) 0.0171(10) Uani 1 d . . . C57 C 0.2003(6) 0.4144(4) 0.8284(3) 0.0282(12) Uani 1 d . . . C58 C 0.1779(9) 0.5035(5) 0.8717(4) 0.058(2) Uani 1 d . . . H58A H 0.2012 0.5629 0.8389 0.086 Uiso 1 calc R . . H58B H 0.2348 0.4964 0.9169 0.086 Uiso 1 calc R . . H58C H 0.0835 0.5077 0.8867 0.086 Uiso 1 calc R . . C59 C 0.2358(6) 0.6783(4) 0.6788(4) 0.0434(16) Uani 1 d . . . H59A H 0.3081 0.682 0.7154 0.065 Uiso 1 calc R . . H59B H 0.1489 0.683 0.704 0.065 Uiso 1 calc R . . H59C H 0.243 0.732 0.6378 0.065 Uiso 1 calc R . . N1 N 0.2544(4) 0.0947(3) 0.7102(2) 0.0142(8) Uani 1 d . . . N2 N 0.4320(4) 0.2602(3) 0.6677(2) 0.0135(8) Uani 1 d . . . N3 N 0.4718(4) 0.2798(3) 0.8287(2) 0.0168(8) Uani 1 d . . . N4 N 0.2936(4) 0.1150(3) 0.8705(2) 0.0148(8) Uani 1 d . . . N5 N 0.0136(4) 0.2065(3) 0.7726(2) 0.0184(9) Uani 1 d . . . N6 N 0.1264(4) 0.3077(3) 0.6497(2) 0.0185(9) Uani 1 d . . . O1 O 0.1745(4) 0.3295(3) 0.8634(2) 0.0260(8) Uani 1 d . . . O2 O 0.2473(4) 0.4229(2) 0.7606(2) 0.0230(8) Uani 1 d . . . O3 O 0.2467(4) 0.5879(3) 0.6483(3) 0.0357(10) Uani 1 d . . . 04 O -0.1597(4) 0.1146(3) 0.5672(2) 0.0282(8) Uiso 1 d . . . Yb1 Yb 0.268761(18) 0.242687(13) 0.766385(11) 0.01307(8) Uani 1 d . . . H99 H 0.324(12) 0.565(8) 0.682(7) 0.14(4) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.008(2) 0.015(2) 0.018(2) -0.0032(18) -0.0032(17) 0.0005(17) C2 0.018(2) 0.014(2) 0.011(2) -0.0012(18) -0.0005(17) -0.0058(18) C3 0.020(2) 0.022(2) 0.007(2) 0.0006(18) -0.0002(17) -0.0043(19) C4 0.016(2) 0.019(2) 0.013(2) 0.0024(19) 0.0004(18) -0.0080(18) C5 0.019(2) 0.010(2) 0.015(2) 0.0023(18) -0.0025(18) -0.0020(17) C6 0.013(2) 0.014(2) 0.016(2) 0.0033(18) -0.0029(18) -0.0019(17) C7 0.015(2) 0.018(2) 0.018(2) -0.0047(19) -0.0041(18) -0.0015(18) C8 0.021(3) 0.021(3) 0.019(3) -0.005(2) -0.0033(19) -0.008(2) C9 0.022(3) 0.028(3) 0.017(3) -0.007(2) -0.005(2) -0.004(2) C10 0.020(2) 0.019(2) 0.011(2) -0.0028(19) -0.0012(18) -0.0041(19) C11 0.017(2) 0.018(2) 0.017(2) -0.0025(19) -0.0023(18) -0.0008(18) C12 0.012(2) 0.015(2) 0.015(2) 0.0007(18) -0.0026(17) -0.0016(17) C13 0.019(2) 0.020(2) 0.011(2) -0.0026(19) -0.0011(18) -0.0015(19) C14 0.012(2) 0.019(2) 0.018(2) 0.0026(19) 0.0008(18) -0.0026(18) C15 0.014(2) 0.014(2) 0.019(2) 0.0007(19) 0.0004(18) 0.0004(17) C16 0.011(2) 0.014(2) 0.016(2) 0.0021(18) -0.0048(17) -0.0004(17) C17 0.017(2) 0.012(2) 0.017(2) -0.0012(18) -0.0040(18) -0.0001(17) C18 0.014(2) 0.013(2) 0.024(3) -0.0039(19) -0.0049(19) -0.0010(17) C19 0.018(2) 0.019(2) 0.016(2) -0.0056(19) -0.0048(19) 0.0002(19) C20 0.009(2) 0.014(2) 0.012(2) 0.0014(17) 0.0017(16) -0.0023(16) C21 0.022(2) 0.008(2) 0.013(2) 0.0007(17) -0.0016(18) 0.0002(17) C22 0.016(2) 0.016(2) 0.019(2) -0.0012(19) -0.0011(18) -0.0027(18) C23 0.023(3) 0.021(3) 0.018(3) -0.002(2) -0.007(2) -0.008(2) C24 0.029(3) 0.018(2) 0.014(2) -0.0038(19) -0.003(2) -0.005(2) C25 0.022(3) 0.016(2) 0.016(2) 0.0003(19) 0.0000(19) 0.0009(19) C26 0.020(2) 0.012(2) 0.016(2) 0.0001(18) -0.0036(19) -0.0013(18) C27 0.016(2) 0.015(2) 0.013(2) -0.0027(18) -0.0011(18) -0.0068(18) C28 0.021(3) 0.015(2) 0.022(3) 0.003(2) -0.005(2) 0.0007(19) C29 0.011(2) 0.027(3) 0.028(3) -0.002(2) -0.004(2) -0.0046(19) C30 0.023(3) 0.021(3) 0.019(3) 0.000(2) -0.001(2) -0.012(2) C31 0.026(3) 0.013(2) 0.019(3) -0.0011(19) -0.004(2) -0.0009(19) C32 0.013(2) 0.018(2) 0.020(3) -0.0023(19) -0.0033(18) 0.0008(18) C33 0.018(2) 0.027(3) 0.017(3) -0.001(2) 0.0013(19) -0.007(2) C34 0.032(3) 0.031(3) 0.020(3) -0.006(2) 0.004(2) -0.012(2) C35 0.041(3) 0.041(3) 0.022(3) -0.013(3) 0.005(2) -0.022(3) C36 0.029(3) 0.064(4) 0.015(3) -0.009(3) -0.001(2) -0.024(3) C37 0.014(3) 0.053(4) 0.018(3) 0.006(3) -0.005(2) -0.005(2) C38 0.014(2) 0.036(3) 0.016(3) 0.001(2) 0.0002(19) -0.002(2) C39 0.019(2) 0.014(2) 0.016(2) -0.0040(18) 0.0008(18) -0.0007(18) C40 0.020(2) 0.020(2) 0.016(2) -0.0047(19) -0.0018(19) -0.0027(19) C41 0.019(3) 0.024(3) 0.030(3) -0.006(2) -0.003(2) -0.006(2) C42 0.034(3) 0.017(3) 0.042(4) -0.002(2) 0.003(3) -0.010(2) C43 0.031(3) 0.019(3) 0.042(3) 0.003(2) -0.004(2) -0.005(2) C44 0.021(3) 0.021(3) 0.030(3) -0.004(2) -0.002(2) -0.003(2) C45 0.018(2) 0.017(2) 0.021(3) -0.001(2) 0.0005(19) 0.0015(19) C46 0.022(3) 0.018(2) 0.021(3) -0.002(2) 0.000(2) 0.005(2) C47 0.022(3) 0.023(3) 0.020(3) -0.002(2) -0.006(2) 0.006(2) C48 0.016(2) 0.019(2) 0.025(3) -0.007(2) -0.004(2) 0.0041(19) C49 0.016(2) 0.014(2) 0.025(3) -0.006(2) -0.0012(19) 0.0033(18) C50 0.019(3) 0.025(3) 0.030(3) -0.009(2) -0.005(2) -0.001(2) C51 0.018(3) 0.025(3) 0.036(3) -0.006(2) -0.006(2) 0.001(2) C52 0.016(2) 0.014(2) 0.032(3) -0.002(2) -0.002(2) 0.0033(18) C53 0.015(2) 0.020(3) 0.033(3) 0.000(2) 0.005(2) 0.0005(19) C54 0.021(3) 0.023(3) 0.023(3) 0.003(2) 0.006(2) 0.001(2) C55 0.023(3) 0.021(3) 0.021(3) 0.001(2) 0.001(2) 0.006(2) C56 0.015(2) 0.014(2) 0.021(3) 0.0010(19) -0.0010(19) 0.0029(18) C57 0.027(3) 0.026(3) 0.033(3) -0.011(2) -0.011(2) 0.010(2) C58 0.095(6) 0.029(4) 0.050(5) -0.015(3) 0.004(4) 0.009(4) C59 0.041(4) 0.021(3) 0.070(5) -0.012(3) -0.013(3) -0.008(3) N1 0.0100(19) 0.016(2) 0.017(2) -0.0034(16) -0.0002(15) -0.0018(15) N2 0.018(2) 0.0118(18) 0.0109(19) -0.0012(15) -0.0064(15) -0.0013(15) N3 0.017(2) 0.017(2) 0.016(2) 0.0017(16) -0.0023(16) -0.0046(16) N4 0.017(2) 0.0139(19) 0.013(2) -0.0013(15) -0.0019(15) -0.0003(15) N5 0.017(2) 0.013(2) 0.024(2) 0.0015(17) 0.0003(17) 0.0025(15) N6 0.017(2) 0.015(2) 0.023(2) -0.0034(17) -0.0010(17) 0.0006(16) O1 0.0255(19) 0.024(2) 0.029(2) -0.0071(16) -0.0005(15) 0.0014(15) O2 0.0268(19) 0.0196(18) 0.023(2) -0.0060(15) -0.0057(15) 0.0016(14) O3 0.041(2) 0.023(2) 0.043(3) -0.0043(18) -0.007(2) 0.0003(17) Yb1 0.01392(12) 0.01297(12) 0.01226(12) -0.00100(8) -0.00172(8) -0.00200(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C20 1.404(6) . ? C1 C2 1.411(6) . ? C1 C21 1.481(6) . ? C2 N2 1.392(6) . ? C2 C3 1.425(6) . ? C3 C4 1.348(6) . ? C3 H3 0.93 . ? C4 C5 1.440(6) . ? C4 H4 0.93 . ? C5 N2 1.372(6) . ? C5 C6 1.394(6) . ? C6 C7 1.413(7) . ? C6 C27 1.484(6) . ? C7 N3 1.367(6) . ? C7 C8 1.428(6) . ? C8 C9 1.342(7) . ? C8 H8 0.93 . ? C9 C10 1.430(6) . ? C9 H9 0.93 . ? C10 N3 1.374(6) . ? C10 C11 1.406(6) . ? C11 C12 1.396(6) . ? C11 C33 1.489(7) . ? C12 N4 1.379(6) . ? C12 C13 1.431(6) . ? C13 C14 1.356(6) . ? C13 H13 0.93 . ? C14 C15 1.438(6) . ? C14 H14 0.93 . ? C15 N4 1.370(6) . ? C15 C16 1.396(6) . ? C16 C17 1.402(6) . ? C16 C39 1.485(6) . ? C17 N1 1.377(6) . ? C17 C18 1.442(6) . ? C18 C19 1.362(7) . ? C18 H18 0.93 . ? C19 C20 1.442(6) . ? C19 H19 0.93 . ? C20 N1 1.390(6) . ? C21 C22 1.385(6) . ? C21 C26 1.401(6) . ? C22 C23 1.388(7) . ? C22 H22 0.93 . ? C23 C24 1.392(7) . ? C23 H23 0.93 . ? C24 C25 1.381(7) . ? C24 H24 0.93 . ? C25 C26 1.391(6) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C27 C28 1.393(7) . ? C27 C32 1.410(6) . ? C28 C29 1.381(6) . ? C28 H28 0.93 . ? C29 C30 1.396(7) . ? C29 H29 0.93 . ? C30 C31 1.394(7) . ? C30 H30 0.93 . ? C31 C32 1.369(6) . ? C31 H31 0.93 . ? C32 H32 0.93 . ? C33 C34 1.395(7) . ? C33 C38 1.411(7) . ? C34 C35 1.388(7) . ? C34 H34 0.93 . ? C35 C36 1.391(9) . ? C35 H35 0.93 . ? C36 C37 1.390(8) . ? C36 H36 0.93 . ? C37 C38 1.383(7) . ? C37 H37 0.93 . ? C38 H38 0.93 . ? C39 C40 1.390(7) . ? C39 C44 1.400(7) . ? C40 C41 1.378(7) . ? C40 H40 0.93 . ? C41 C42 1.386(8) . ? C41 H41 0.93 . ? C42 C43 1.382(8) . ? C42 H42 0.93 . ? C43 C44 1.377(7) . ? C43 H43 0.93 . ? C44 H44 0.93 . ? C45 N6 1.331(6) . ? C45 C46 1.396(7) . ? C45 H45 0.93 . ? C46 C47 1.378(7) . ? C46 H46 0.93 . ? C47 C48 1.378(7) . ? C47 H47 0.93 . ? C48 C49 1.392(7) . ? C48 C50 1.481(7) . ? C49 N6 1.346(6) . ? C49 C56 1.468(7) . ? C50 04 1.459(6) . ? C50 C51 1.475(8) . ? C51 04 1.463(6) . ? C51 C52 1.475(7) . ? C52 C56 1.394(7) . ? C52 C53 1.402(7) . ? C53 C54 1.373(7) . ? C53 H53 0.93 . ? C54 C55 1.391(7) . ? C54 H54 0.93 . ? C55 N5 1.337(6) . ? C55 H55 0.93 . ? C56 N5 1.361(6) . ? C57 O2 1.260(7) . ? C57 O1 1.266(7) . ? C57 C58 1.513(8) . ? C57 Yb1 2.753(5) . ? C58 H58A 0.96 . ? C58 H58B 0.96 . ? C58 H58C 0.96 . ? C59 O3 1.396(7) . ? C59 H59A 0.96 . ? C59 H59B 0.96 . ? C59 H59C 0.96 . ? N1 Yb1 2.346(4) . ? N2 Yb1 2.338(4) . ? N3 Yb1 2.358(4) . ? N4 Yb1 2.359(4) . ? N5 Yb1 2.551(4) . ? N6 Yb1 2.523(4) . ? O1 Yb1 2.351(3) . ? O2 Yb1 2.437(3) . ? O3 H99 0.98(12) . ? 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 C20 C1 C2 125.2(4) . . ? C20 C1 C21 116.9(4) . . ? C2 C1 C21 117.9(4) . . ? N2 C2 C1 123.9(4) . . ? N2 C2 C3 110.5(4) . . ? C1 C2 C3 125.5(4) . . ? C4 C3 C2 106.5(4) . . ? C4 C3 H3 126.8 . . ? C2 C3 H3 126.8 . . ? C3 C4 C5 108.1(4) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? N2 C5 C6 125.2(4) . . ? N2 C5 C4 109.4(4) . . ? C6 C5 C4 125.1(4) . . ? C5 C6 C7 125.6(4) . . ? C5 C6 C27 118.6(4) . . ? C7 C6 C27 115.8(4) . . ? N3 C7 C6 125.0(4) . . ? N3 C7 C8 109.2(4) . . ? C6 C7 C8 125.8(4) . . ? C9 C8 C7 107.8(4) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? C8 C9 C10 106.9(4) . . ? C8 C9 H9 126.5 . . ? C10 C9 H9 126.5 . . ? N3 C10 C11 126.2(4) . . ? N3 C10 C9 109.4(4) . . ? C11 C10 C9 124.3(4) . . ? C12 C11 C10 124.6(4) . . ? C12 C11 C33 118.0(4) . . ? C10 C11 C33 117.4(4) . . ? N4 C12 C11 125.5(4) . . ? N4 C12 C13 110.2(4) . . ? C11 C12 C13 124.2(4) . . ? C14 C13 C12 106.6(4) . . ? C14 C13 H13 126.7 . . ? C12 C13 H13 126.7 . . ? C13 C14 C15 107.3(4) . . ? C13 C14 H14 126.3 . . ? C15 C14 H14 126.3 . . ? N4 C15 C16 124.9(4) . . ? N4 C15 C14 109.8(4) . . ? C16 C15 C14 125.3(4) . . ? C15 C16 C17 125.4(4) . . ? C15 C16 C39 117.4(4) . . ? C17 C16 C39 117.1(4) . . ? N1 C17 C16 125.2(4) . . ? N1 C17 C18 109.5(4) . . ? C16 C17 C18 125.3(4) . . ? C19 C18 C17 107.9(4) . . ? C19 C18 H18 126.1 . . ? C17 C18 H18 126.1 . . ? C18 C19 C20 106.4(4) . . ? C18 C19 H19 126.8 . . ? C20 C19 H19 126.8 . . ? N1 C20 C1 126.8(4) . . ? N1 C20 C19 110.0(4) . . ? C1 C20 C19 123.1(4) . . ? C22 C21 C26 118.3(4) . . ? C22 C21 C1 120.2(4) . . ? C26 C21 C1 121.4(4) . . ? C21 C22 C23 121.2(4) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120 . . ? C24 C23 H23 120 . . ? C25 C24 C23 119.6(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.2(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.6(4) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 119.3(4) . . ? C28 C27 C6 120.3(4) . . ? C32 C27 C6 120.3(4) . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 119.2(4) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 120.9(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 119.6(4) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C27 120.3(4) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C34 C33 C38 118.8(5) . . ? C34 C33 C11 120.3(5) . . ? C38 C33 C11 120.8(4) . . ? C35 C34 C33 120.9(5) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 119.5(5) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 120.5(5) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 120.1(5) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C33 120.1(5) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? C40 C39 C44 119.7(4) . . ? C40 C39 C16 119.7(4) . . ? C44 C39 C16 120.6(4) . . ? C41 C40 C39 120.0(5) . . ? C41 C40 H40 120 . . ? C39 C40 H40 120 . . ? C40 C41 C42 119.7(5) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 120.9(5) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C44 C43 C42 119.6(5) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C39 120.0(5) . . ? C43 C44 H44 120 . . ? C39 C44 H44 120 . . ? N6 C45 C46 124.5(4) . . ? N6 C45 H45 117.7 . . ? C46 C45 H45 117.7 . . ? C47 C46 C45 118.2(5) . . ? C47 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? C46 C47 C48 118.4(5) . . ? C46 C47 H47 120.8 . . ? C48 C47 H47 120.8 . . ? C47 C48 C49 119.6(4) . . ? C47 C48 C50 120.8(5) . . ? C49 C48 C50 119.6(4) . . ? N6 C49 C48 123.0(4) . . ? N6 C49 C56 115.1(4) . . ? C48 C49 C56 121.1(4) . . ? 04 C50 C51 59.8(3) . . ? 04 C50 C48 113.6(4) . . ? C51 C50 C48 117.6(4) . . ? 04 C51 C50 59.6(3) . . ? 04 C51 C52 115.3(4) . . ? C50 C51 C52 119.2(4) . . ? C56 C52 C53 117.5(5) . . ? C56 C52 C51 119.6(5) . . ? C53 C52 C51 122.7(4) . . ? C54 C53 C52 119.6(5) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C55 119.4(5) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? N5 C55 C54 122.2(5) . . ? N5 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? N5 C56 C52 122.6(4) . . ? N5 C56 C49 116.8(4) . . ? C52 C56 C49 119.9(4) . . ? O2 C57 O1 120.3(5) . . ? O2 C57 C58 121.9(5) . . ? O1 C57 C58 117.8(5) . . ? O2 C57 Yb1 62.3(3) . . ? O1 C57 Yb1 58.4(3) . . ? C58 C57 Yb1 171.5(4) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O3 C59 H59A 109.5 . . ? O3 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O3 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C17 N1 C20 106.2(4) . . ? C17 N1 Yb1 126.1(3) . . ? C20 N1 Yb1 125.2(3) . . ? C5 N2 C2 105.4(4) . . ? C5 N2 Yb1 120.7(3) . . ? C2 N2 Yb1 124.4(3) . . ? C7 N3 C10 106.5(4) . . ? C7 N3 Yb1 124.0(3) . . ? C10 N3 Yb1 124.9(3) . . ? C15 N4 C12 105.9(4) . . ? C15 N4 Yb1 121.9(3) . . ? C12 N4 Yb1 121.0(3) . . ? C55 N5 C56 118.3(4) . . ? C55 N5 Yb1 124.4(3) . . ? C56 N5 Yb1 116.7(3) . . ? C45 N6 C49 116.3(4) . . ? C45 N6 Yb1 123.6(3) . . ? C49 N6 Yb1 119.2(3) . . ? C57 O1 Yb1 94.3(3) . . ? C57 O2 Yb1 90.5(3) . . ? C59 O3 H99 93(7) . . ? C50 04 C51 60.6(3) . . ? N2 Yb1 N1 76.29(13) . . ? N2 Yb1 O1 140.66(12) . . ? N1 Yb1 O1 143.04(13) . . ? N2 Yb1 N3 75.72(13) . . ? N1 Yb1 N3 120.24(13) . . ? O1 Yb1 N3 80.43(13) . . ? N2 Yb1 N4 120.42(13) . . ? N1 Yb1 N4 75.21(13) . . ? O1 Yb1 N4 82.12(13) . . ? N3 Yb1 N4 75.47(13) . . ? N2 Yb1 O2 90.08(12) . . ? N1 Yb1 O2 151.88(12) . . ? O1 Yb1 O2 54.45(12) . . ? N3 Yb1 O2 78.57(12) . . ? N4 Yb1 O2 132.36(12) . . ? N2 Yb1 N6 77.51(13) . . ? N1 Yb1 N6 81.41(13) . . ? O1 Yb1 N6 102.66(12) . . ? N3 Yb1 N6 139.47(13) . . ? N4 Yb1 N6 145.00(13) . . ? O2 Yb1 N6 71.58(12) . . ? N2 Yb1 N5 134.65(13) . . ? N1 Yb1 N5 76.57(13) . . ? O1 Yb1 N5 73.11(13) . . ? N3 Yb1 N5 149.61(14) . . ? N4 Yb1 N5 86.18(13) . . ? O2 Yb1 N5 97.33(12) . . ? N6 Yb1 N5 63.02(13) . . ? N2 Yb1 C57 115.22(15) . . ? N1 Yb1 C57 162.50(15) . . ? O1 Yb1 C57 27.30(15) . . ? N3 Yb1 C57 76.56(15) . . ? N4 Yb1 C57 106.99(15) . . ? O2 Yb1 C57 27.23(14) . . ? N6 Yb1 C57 88.17(14) . . ? N5 Yb1 C57 86.19(15) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.550 _refine_diff_density_min -1.253 _refine_diff_density_rms 0.136 #===END data_08058_7 _database_code_depnum_ccdc_archive 'CCDC 731409' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Yb-TPP-DPA-Acetate).2MeOH _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H48 N7 O4 Yb' _chemical_formula_weight 1080.07 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0590(12) _cell_length_b 13.2450(15) _cell_length_c 19.689(3) _cell_angle_alpha 102.797(2) _cell_angle_beta 92.282(2) _cell_angle_gamma 111.7990(10) _cell_volume 2353.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour Purple-red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1094 _exptl_absorpt_coefficient_mu 2.045 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5471 _exptl_absorpt_correction_T_max 0.7812 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23790 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.52 _reflns_number_total 8637 _reflns_number_gt 7760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII (Bruker, 2006)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2006)' _computing_data_reduction 'Bruker SAINT (Bruker, 2006)' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'Ortep-3(Farrugia, 1997)' _computing_publication_material 'WinGX(Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+16.9428P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8637 _refine_ls_number_parameters 645 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.013 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1 C 1.0089(6) 0.2972(5) 0.1663(3) 0.0162(11) Uani 1 d . . . C2 C 1.0267(6) 0.3931(4) 0.2196(3) 0.0146(11) Uani 1 d . . . C3 C 1.1434(6) 0.5023(5) 0.2303(3) 0.0168(11) Uani 1 d . . . H3 H 1.2151 0.5224 0.2016 0.02 Uiso 1 calc R . . C4 C 1.1290(6) 0.5694(5) 0.2895(3) 0.0156(11) Uani 1 d . . . H4 H 1.1904 0.6437 0.3098 0.019 Uiso 1 calc R . . C5 C 1.0012(6) 0.5049(4) 0.3156(3) 0.0138(11) Uani 1 d . . . C6 C 0.9486(5) 0.5450(4) 0.3763(3) 0.0140(11) Uani 1 d . . . C7 C 0.8280(6) 0.4800(4) 0.4044(3) 0.0142(11) Uani 1 d . . . C8 C 0.7733(6) 0.5222(5) 0.4660(3) 0.0179(12) Uani 1 d . . . H8 H 0.8084 0.5961 0.4932 0.021 Uiso 1 calc R . . C9 C 0.6612(6) 0.4343(5) 0.4771(3) 0.0170(11) Uani 1 d . . . H9 H 0.6045 0.4363 0.5131 0.02 Uiso 1 calc R . . C10 C 0.6467(6) 0.3376(5) 0.4228(3) 0.0150(11) Uani 1 d . . . C11 C 0.5461(6) 0.2271(4) 0.4175(3) 0.0138(11) Uani 1 d . . . C12 C 0.5278(6) 0.1320(4) 0.3638(3) 0.0156(11) Uani 1 d . . . C13 C 0.4359(6) 0.0179(5) 0.3636(3) 0.0178(11) Uani 1 d . . . H13 H 0.3789 -0.0045 0.3978 0.021 Uiso 1 calc R . . C14 C 0.4487(6) -0.0497(5) 0.3043(3) 0.0179(12) Uani 1 d . . . H14 H 0.4006 -0.1274 0.2895 0.022 Uiso 1 calc R . . C15 C 0.5506(6) 0.0207(4) 0.2679(3) 0.0149(11) Uani 1 d . . . C16 C 0.6030(6) -0.0200(4) 0.2071(3) 0.0160(11) Uani 1 d . . . C17 C 0.7198(6) 0.0462(4) 0.1774(3) 0.0147(11) Uani 1 d . . . C18 C 0.7912(6) 0.0000(5) 0.1247(3) 0.0175(11) Uani 1 d . . . H18 H 0.7641 -0.0756 0.102 0.021 Uiso 1 calc R . . C19 C 0.9054(6) 0.0874(5) 0.1141(3) 0.0182(12) Uani 1 d . . . H19 H 0.9723 0.083 0.0835 0.022 Uiso 1 calc R . . C20 C 1.1149(6) 0.3063(4) 0.1143(3) 0.0161(11) Uani 1 d . . . C59 C 0.9034(6) 0.1891(4) 0.1595(3) 0.0147(11) Uani 1 d . . . C21 C 1.0680(7) 0.2787(5) 0.0424(3) 0.0216(12) Uani 1 d . . . H21 H 0.9715 0.261 0.0271 0.026 Uiso 1 calc R . . C23 C 1.1630(7) 0.2774(5) -0.0064(3) 0.0258(13) Uani 1 d . . . H23 H 1.1298 0.2582 -0.0541 0.031 Uiso 1 calc R . . C24 C 1.3075(7) 0.3045(5) 0.0156(3) 0.0262(14) Uani 1 d . . . H24 H 1.3709 0.3029 -0.0173 0.031 Uiso 1 calc R . . C25 C 1.3570(7) 0.3339(5) 0.0864(3) 0.0240(13) Uani 1 d . . . H25 H 1.454 0.3528 0.1013 0.029 Uiso 1 calc R . . C26 C 1.0250(5) 0.6665(4) 0.4148(3) 0.0140(11) Uani 1 d . . . C27 C 1.0377(6) 0.7514(5) 0.3811(3) 0.0168(11) Uani 1 d . . . H27 H 0.998 0.7324 0.3343 0.02 Uiso 1 calc R . . C28 C 1.1084(6) 0.8631(5) 0.4163(3) 0.0199(12) Uani 1 d . . . H28 H 1.1156 0.9185 0.3931 0.024 Uiso 1 calc R . . C29 C 1.1688(6) 0.8935(5) 0.4860(3) 0.0243(13) Uani 1 d . . . H29 H 1.2167 0.9689 0.5096 0.029 Uiso 1 calc R . . C30 C 1.1569(6) 0.8104(5) 0.5203(3) 0.0217(12) Uani 1 d . . . H30 H 1.1969 0.8301 0.5671 0.026 Uiso 1 calc R . . C31 C 1.0851(6) 0.6969(5) 0.4848(3) 0.0172(11) Uani 1 d . . . H31 H 1.0775 0.6416 0.5081 0.021 Uiso 1 calc R . . C32 C 0.4558(6) 0.2129(4) 0.4762(3) 0.0158(11) Uani 1 d . . . C33 C 0.5140(6) 0.2198(5) 0.5428(3) 0.0215(12) Uani 1 d . . . H33 H 0.6099 0.2286 0.5508 0.026 Uiso 1 calc R . . C34 C 0.4319(7) 0.2139(5) 0.5979(3) 0.0252(13) Uani 1 d . . . H34 H 0.4722 0.2175 0.6421 0.03 Uiso 1 calc R . . C35 C 0.2898(7) 0.2025(5) 0.5868(3) 0.0224(13) Uani 1 d . . . H35 H 0.2358 0.2018 0.6241 0.027 Uiso 1 calc R . . C36 C 0.2283(6) 0.1924(5) 0.5204(3) 0.0237(13) Uani 1 d . . . H36 H 0.1321 0.1829 0.5127 0.028 Uiso 1 calc R . . C37 C 0.3101(6) 0.1962(5) 0.4652(3) 0.0211(12) Uani 1 d . . . H37 H 0.2675 0.1877 0.4204 0.025 Uiso 1 calc R . . C38 C 0.5346(6) -0.1431(4) 0.1728(3) 0.0173(11) Uani 1 d . . . C39 C 0.5797(7) -0.2209(5) 0.1914(4) 0.0296(14) Uani 1 d . . . H39 H 0.6575 -0.197 0.2264 0.035 Uiso 1 calc R . . C40 C 0.5099(8) -0.3351(5) 0.1582(4) 0.0317(15) Uani 1 d . . . H40 H 0.541 -0.3865 0.1719 0.038 Uiso 1 calc R . . C41 C 0.3965(7) -0.3726(5) 0.1059(3) 0.0294(15) Uani 1 d . . . H41 H 0.3522 -0.4487 0.0832 0.035 Uiso 1 calc R . . C42 C 0.3490(8) -0.2965(5) 0.0874(4) 0.0354(16) Uani 1 d . . . H42 H 0.2703 -0.3215 0.0527 0.042 Uiso 1 calc R . . C43 C 0.4176(7) -0.1824(5) 0.1201(4) 0.0300(15) Uani 1 d . . . H43 H 0.385 -0.1317 0.1066 0.036 Uiso 1 calc R . . C44 C 0.5011(7) 0.1383(5) 0.0992(3) 0.0219(12) Uani 1 d . . . H44 H 0.5937 0.1731 0.0885 0.026 Uiso 1 calc R . . C45 C 0.3957(7) 0.0639(5) 0.0454(3) 0.0268(14) Uani 1 d . . . H45 H 0.4156 0.0508 -0.0007 0.032 Uiso 1 calc R . . C46 C 0.2584(7) 0.0087(5) 0.0617(3) 0.0271(14) Uani 1 d . . . H46 H 0.1859 -0.0445 0.0268 0.033 Uiso 1 calc R . . C47 C 0.2310(7) 0.0332(5) 0.1292(3) 0.0245(13) Uani 1 d . . . H47 H 0.1401 -0.0038 0.141 0.029 Uiso 1 calc R . . C48 C 0.3414(6) 0.1147(5) 0.1807(3) 0.0196(12) Uani 1 d . . . C49 C 0.3473(6) 0.2591(5) 0.2834(3) 0.0188(12) Uani 1 d . . . C50 C 0.2421(7) 0.2925(5) 0.3153(3) 0.0216(12) Uani 1 d . . . H50 H 0.1498 0.2397 0.3148 0.026 Uiso 1 calc R . . C51 C 0.2780(7) 0.4039(5) 0.3472(3) 0.0241(13) Uani 1 d . . . H51 H 0.2114 0.4274 0.37 0.029 Uiso 1 calc R . . C52 C 0.4151(7) 0.4813(5) 0.3450(3) 0.0254(13) Uani 1 d . . . H52 H 0.4405 0.5577 0.3644 0.03 Uiso 1 calc R . . C53 C 0.5125(6) 0.4426(5) 0.3134(3) 0.0206(12) Uani 1 d . . . H53 H 0.6042 0.4947 0.3121 0.025 Uiso 1 calc R . . C54 C 0.8037(16) 0.4973(8) 0.0998(5) 0.121(6) Uani 1 d . . . H54A H 0.845 0.5747 0.0985 0.181 Uiso 1 calc R . . H54B H 0.7203 0.4574 0.0648 0.181 Uiso 1 calc R . . H54C H 0.8738 0.4645 0.0905 0.181 Uiso 1 calc R . . C55 C 0.7583(7) 0.4895(6) 0.1740(4) 0.0297(15) Uani 1 d . . . O2 O 0.7849(5) 0.5786(4) 0.2213(3) 0.0402(12) Uani 1 d . . . C57 C -0.0628(7) 0.0325(6) 0.3249(4) 0.0345(16) Uani 1 d . . . H57A H -0.0146 0.0638 0.3723 0.052 Uiso 1 calc R . . H57B H -0.1472 -0.0337 0.3228 0.052 Uiso 1 calc R . . H57C H -0.0906 0.0868 0.3098 0.052 Uiso 1 calc R . . C58 C 1.0789(8) 0.7768(6) 0.1910(4) 0.0399(17) Uani 1 d . . . H58A H 1.1572 0.8462 0.2144 0.06 Uiso 1 calc R . . H58B H 1.0825 0.7621 0.1413 0.06 Uiso 1 calc R . . H58C H 1.0873 0.7165 0.208 0.06 Uiso 1 calc R . . C60 C 1.2614(6) 0.3352(5) 0.1355(3) 0.0178(11) Uani 1 d . . . H60 H 1.2956 0.3556 0.1831 0.021 Uiso 1 calc R . . N1 N 0.7906(5) 0.1607(4) 0.1979(2) 0.0186(10) Uani 1 d . . . N2 N 0.9421(5) 0.3976(4) 0.2722(2) 0.0138(9) Uani 1 d . . . N3 N 0.7468(5) 0.3660(4) 0.3771(2) 0.0144(9) Uani 1 d . . . N4 N 0.5970(5) 0.1319(4) 0.3049(2) 0.0143(9) Uani 1 d . . . N5 N 0.4820(5) 0.3325(4) 0.2842(2) 0.0198(10) Uani 1 d . . . N7 N 0.3072(5) 0.1472(4) 0.2474(3) 0.0204(10) Uani 1 d D . . N6 N 0.4774(5) 0.1636(4) 0.1667(2) 0.0187(10) Uani 1 d . . . O1 O 0.7025(5) 0.3927(4) 0.1836(2) 0.0322(11) Uani 1 d . . . O4 O 0.9455(6) 0.7852(4) 0.2050(3) 0.0414(12) Uani 1 d D . . O3 O 0.0317(6) 0.0042(4) 0.2805(3) 0.0421(13) Uani 1 d D . . Yb1 Yb 0.69343(3) 0.286265(19) 0.256624(12) 0.01357(8) Uani 1 d . . . H98 H 0.225(3) 0.115(6) 0.253(4) 0.04(2) Uiso 1 d D . . H99 H -0.005(8) -0.060(3) 0.258(4) 0.05(3) Uiso 1 d D . . H100 H 0.894(11) 0.722(4) 0.206(6) 0.11(5) Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.015(3) 0.022(3) 0.013(3) 0.005(2) 0.003(2) 0.007(2) C2 0.014(3) 0.016(3) 0.015(3) 0.006(2) 0.003(2) 0.006(2) C3 0.014(3) 0.019(3) 0.018(3) 0.008(2) 0.007(2) 0.005(2) C4 0.009(3) 0.015(3) 0.021(3) 0.006(2) 0.001(2) 0.001(2) C5 0.013(3) 0.011(2) 0.017(3) 0.005(2) -0.001(2) 0.004(2) C6 0.009(2) 0.013(3) 0.019(3) 0.006(2) 0.002(2) 0.003(2) C7 0.015(3) 0.013(3) 0.014(3) 0.003(2) 0.002(2) 0.005(2) C8 0.018(3) 0.014(3) 0.017(3) 0.001(2) 0.004(2) 0.003(2) C9 0.017(3) 0.018(3) 0.016(3) 0.005(2) 0.006(2) 0.007(2) C10 0.013(3) 0.019(3) 0.013(3) 0.003(2) 0.002(2) 0.008(2) C11 0.010(3) 0.018(3) 0.014(3) 0.007(2) 0.004(2) 0.005(2) C12 0.013(3) 0.016(3) 0.016(3) 0.006(2) 0.002(2) 0.003(2) C13 0.014(3) 0.019(3) 0.021(3) 0.007(2) 0.005(2) 0.005(2) C14 0.016(3) 0.013(3) 0.023(3) 0.005(2) 0.002(2) 0.003(2) C15 0.012(3) 0.014(3) 0.017(3) 0.004(2) 0.001(2) 0.003(2) C16 0.014(3) 0.013(3) 0.020(3) 0.004(2) 0.001(2) 0.004(2) C17 0.013(3) 0.013(3) 0.016(3) 0.003(2) 0.001(2) 0.004(2) C18 0.018(3) 0.012(3) 0.021(3) 0.002(2) 0.002(2) 0.005(2) C19 0.017(3) 0.023(3) 0.016(3) 0.003(2) 0.008(2) 0.009(2) C20 0.018(3) 0.010(3) 0.020(3) 0.006(2) 0.007(2) 0.004(2) C59 0.015(3) 0.012(3) 0.017(3) 0.005(2) 0.004(2) 0.003(2) C21 0.024(3) 0.019(3) 0.020(3) 0.004(2) 0.006(2) 0.007(2) C23 0.039(4) 0.023(3) 0.015(3) 0.004(2) 0.007(3) 0.011(3) C24 0.033(4) 0.018(3) 0.030(3) 0.009(3) 0.022(3) 0.011(3) C25 0.024(3) 0.017(3) 0.035(4) 0.009(3) 0.012(3) 0.009(2) C26 0.008(2) 0.013(3) 0.018(3) 0.002(2) 0.006(2) 0.001(2) C27 0.013(3) 0.019(3) 0.018(3) 0.004(2) 0.008(2) 0.006(2) C28 0.017(3) 0.013(3) 0.031(3) 0.008(2) 0.011(2) 0.005(2) C29 0.015(3) 0.014(3) 0.037(4) -0.001(2) 0.008(3) 0.002(2) C30 0.014(3) 0.024(3) 0.020(3) -0.004(2) 0.000(2) 0.006(2) C31 0.013(3) 0.017(3) 0.019(3) 0.002(2) 0.003(2) 0.005(2) C32 0.017(3) 0.012(3) 0.018(3) 0.004(2) 0.007(2) 0.004(2) C33 0.017(3) 0.028(3) 0.021(3) 0.009(2) 0.006(2) 0.009(3) C34 0.029(3) 0.030(3) 0.020(3) 0.010(3) 0.008(3) 0.012(3) C35 0.028(3) 0.017(3) 0.025(3) 0.008(2) 0.013(3) 0.009(3) C36 0.016(3) 0.025(3) 0.032(3) 0.009(3) 0.011(2) 0.008(2) C37 0.017(3) 0.024(3) 0.024(3) 0.011(2) 0.005(2) 0.007(2) C38 0.017(3) 0.013(3) 0.019(3) 0.003(2) 0.010(2) 0.002(2) C39 0.027(3) 0.026(3) 0.036(4) 0.009(3) 0.000(3) 0.010(3) C40 0.039(4) 0.021(3) 0.040(4) 0.010(3) 0.014(3) 0.015(3) C41 0.033(4) 0.016(3) 0.030(4) 0.002(3) 0.018(3) 0.000(3) C42 0.030(4) 0.024(3) 0.041(4) -0.003(3) -0.004(3) 0.006(3) C43 0.029(4) 0.019(3) 0.038(4) 0.002(3) -0.002(3) 0.009(3) C44 0.027(3) 0.023(3) 0.021(3) 0.006(2) 0.008(2) 0.014(3) C45 0.035(4) 0.029(3) 0.018(3) 0.002(3) 0.000(3) 0.017(3) C46 0.027(3) 0.020(3) 0.027(3) 0.000(3) -0.009(3) 0.007(3) C47 0.021(3) 0.020(3) 0.031(3) 0.007(3) 0.001(3) 0.006(2) C48 0.021(3) 0.017(3) 0.024(3) 0.008(2) 0.003(2) 0.010(2) C49 0.019(3) 0.021(3) 0.018(3) 0.007(2) 0.002(2) 0.009(2) C50 0.022(3) 0.025(3) 0.021(3) 0.009(2) 0.004(2) 0.012(3) C51 0.028(3) 0.034(3) 0.021(3) 0.010(3) 0.009(3) 0.023(3) C52 0.033(4) 0.023(3) 0.024(3) 0.003(2) 0.002(3) 0.017(3) C53 0.020(3) 0.020(3) 0.020(3) 0.001(2) -0.001(2) 0.009(2) C54 0.200(14) 0.035(5) 0.048(6) 0.027(4) -0.060(7) -0.044(7) C55 0.021(3) 0.029(4) 0.038(4) 0.014(3) 0.000(3) 0.006(3) O2 0.033(3) 0.031(3) 0.051(3) 0.010(2) 0.004(2) 0.008(2) C57 0.027(4) 0.036(4) 0.041(4) 0.013(3) 0.010(3) 0.010(3) C58 0.031(4) 0.042(4) 0.049(5) 0.018(4) 0.001(3) 0.014(3) C60 0.018(3) 0.018(3) 0.019(3) 0.006(2) 0.006(2) 0.008(2) N1 0.022(3) 0.022(2) 0.007(2) 0.0011(18) 0.0038(18) 0.005(2) N2 0.015(2) 0.010(2) 0.013(2) 0.0016(17) 0.0023(18) 0.0012(18) N3 0.009(2) 0.018(2) 0.018(2) 0.0080(19) 0.0056(18) 0.0057(19) N4 0.013(2) 0.015(2) 0.014(2) 0.0033(18) 0.0021(17) 0.0037(18) N5 0.025(3) 0.015(2) 0.017(2) 0.0040(19) 0.001(2) 0.005(2) N7 0.016(3) 0.020(3) 0.025(3) 0.007(2) 0.006(2) 0.006(2) N6 0.021(3) 0.017(2) 0.021(3) 0.0059(19) 0.003(2) 0.011(2) O1 0.022(2) 0.031(3) 0.044(3) 0.019(2) 0.000(2) 0.005(2) O4 0.035(3) 0.030(3) 0.054(3) 0.010(2) 0.002(2) 0.007(2) O3 0.036(3) 0.030(3) 0.045(3) 0.002(2) 0.019(2) -0.001(2) Yb1 0.01199(12) 0.01194(12) 0.01509(13) 0.00296(9) 0.00373(8) 0.00285(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C59 1.403(7) . ? C1 C2 1.404(8) . ? C1 C20 1.499(7) . ? C2 N2 1.371(7) . ? C2 C3 1.448(7) . ? C3 C4 1.350(8) . ? C3 H3 0.93 . ? C4 C5 1.441(7) . ? C4 H4 0.93 . ? C5 N2 1.377(7) . ? C5 C6 1.403(8) . ? C6 C7 1.416(7) . ? C6 C26 1.500(7) . ? C7 N3 1.387(7) . ? C7 C8 1.439(7) . ? C8 C9 1.353(8) . ? C8 H8 0.93 . ? C9 C10 1.430(7) . ? C9 H9 0.93 . ? C10 N3 1.380(7) . ? C10 C11 1.415(7) . ? C11 C12 1.400(8) . ? C11 C32 1.499(7) . ? C12 N4 1.376(7) . ? C12 C13 1.448(7) . ? C13 C14 1.347(8) . ? C13 H13 0.93 . ? C14 C15 1.442(7) . ? C14 H14 0.93 . ? C15 N4 1.381(7) . ? C15 C16 1.405(8) . ? C16 C17 1.417(7) . ? C16 C38 1.494(7) . ? C17 N1 1.369(7) . ? C17 C18 1.440(8) . ? C18 C19 1.357(8) . ? C18 H18 0.93 . ? C19 C59 1.450(7) . ? C19 H19 0.93 . ? C20 C21 1.397(8) . ? C20 C60 1.397(8) . ? C59 N1 1.370(7) . ? C21 C23 1.384(8) . ? C21 H21 0.93 . ? C23 C24 1.386(9) . ? C23 H23 0.93 . ? C24 C25 1.380(9) . ? C24 H24 0.93 . ? C25 C60 1.391(8) . ? C25 H25 0.93 . ? C26 C31 1.391(8) . ? C26 C27 1.397(8) . ? C27 C28 1.378(8) . ? C27 H27 0.93 . ? C28 C29 1.387(9) . ? C28 H28 0.93 . ? C29 C30 1.384(9) . ? C29 H29 0.93 . ? C30 C31 1.399(8) . ? C30 H30 0.93 . ? C31 H31 0.93 . ? C32 C33 1.385(8) . ? C32 C37 1.399(8) . ? C33 C34 1.388(8) . ? C33 H33 0.93 . ? C34 C35 1.383(9) . ? C34 H34 0.93 . ? C35 C36 1.380(9) . ? C35 H35 0.93 . ? C36 C37 1.388(8) . ? C36 H36 0.93 . ? C37 H37 0.93 . ? C38 C39 1.379(9) . ? C38 C43 1.394(9) . ? C39 C40 1.394(9) . ? C39 H39 0.93 . ? C40 C41 1.366(10) . ? C40 H40 0.93 . ? C41 C42 1.372(10) . ? C41 H41 0.93 . ? C42 C43 1.391(9) . ? C42 H42 0.93 . ? C43 H43 0.93 . ? C44 N6 1.350(7) . ? C44 C45 1.375(9) . ? C44 H44 0.93 . ? C45 C46 1.391(9) . ? C45 H45 0.93 . ? C46 C47 1.361(9) . ? C46 H46 0.93 . ? C47 C48 1.400(8) . ? C47 H47 0.93 . ? C48 N6 1.348(7) . ? C48 N7 1.388(8) . ? C49 N5 1.340(7) . ? C49 N7 1.389(7) . ? C49 C50 1.409(8) . ? C50 C51 1.370(8) . ? C50 H50 0.93 . ? C51 C52 1.389(9) . ? C51 H51 0.93 . ? C52 C53 1.375(8) . ? C52 H52 0.93 . ? C53 N5 1.353(7) . ? C53 H53 0.93 . ? C54 C55 1.560(13) . ? C54 H54A 0.96 . ? C54 H54B 0.96 . ? C54 H54C 0.96 . ? C55 O1 1.256(8) . ? C55 O2 1.261(8) . ? C57 O3 1.413(8) . ? C57 H57A 0.96 . ? C57 H57B 0.96 . ? C57 H57C 0.96 . ? C58 O4 1.420(9) . ? C58 H58A 0.96 . ? C58 H58B 0.96 . ? C58 H58C 0.96 . ? C60 H60 0.93 . ? N1 Yb1 2.346(5) . ? N2 Yb1 2.351(4) . ? N3 Yb1 2.324(4) . ? N4 Yb1 2.342(4) . ? N5 Yb1 2.471(5) . ? N7 H98 0.80(2) . ? N6 Yb1 2.508(5) . ? O1 Yb1 2.207(4) . ? O4 H100 0.81(2) . ? O3 H99 0.80(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C59 C1 C2 125.3(5) . . ? C59 C1 C20 115.6(5) . . ? C2 C1 C20 119.0(5) . . ? N2 C2 C1 125.9(5) . . ? N2 C2 C3 108.8(5) . . ? C1 C2 C3 125.1(5) . . ? C4 C3 C2 107.3(5) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? C3 C4 C5 107.5(5) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? N2 C5 C6 126.0(5) . . ? N2 C5 C4 108.8(5) . . ? C6 C5 C4 125.2(5) . . ? C5 C6 C7 125.3(5) . . ? C5 C6 C26 117.8(5) . . ? C7 C6 C26 116.9(5) . . ? N3 C7 C6 125.0(5) . . ? N3 C7 C8 110.0(5) . . ? C6 C7 C8 124.9(5) . . ? C9 C8 C7 107.2(5) . . ? C9 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? C8 C9 C10 106.9(5) . . ? C8 C9 H9 126.5 . . ? C10 C9 H9 126.5 . . ? N3 C10 C11 124.4(5) . . ? N3 C10 C9 110.9(5) . . ? C11 C10 C9 124.7(5) . . ? C12 C11 C10 125.5(5) . . ? C12 C11 C32 118.6(5) . . ? C10 C11 C32 115.9(5) . . ? N4 C12 C11 125.6(5) . . ? N4 C12 C13 109.8(5) . . ? C11 C12 C13 124.5(5) . . ? C14 C13 C12 107.0(5) . . ? C14 C13 H13 126.5 . . ? C12 C13 H13 126.5 . . ? C13 C14 C15 107.4(5) . . ? C13 C14 H14 126.3 . . ? C15 C14 H14 126.3 . . ? N4 C15 C16 125.6(5) . . ? N4 C15 C14 109.8(5) . . ? C16 C15 C14 124.4(5) . . ? C15 C16 C17 125.0(5) . . ? C15 C16 C38 117.6(5) . . ? C17 C16 C38 117.4(5) . . ? N1 C17 C16 126.5(5) . . ? N1 C17 C18 109.4(5) . . ? C16 C17 C18 123.8(5) . . ? C19 C18 C17 107.2(5) . . ? C19 C18 H18 126.4 . . ? C17 C18 H18 126.4 . . ? C18 C19 C59 107.0(5) . . ? C18 C19 H19 126.5 . . ? C59 C19 H19 126.5 . . ? C21 C20 C60 117.9(5) . . ? C21 C20 C1 120.6(5) . . ? C60 C20 C1 121.4(5) . . ? N1 C59 C1 126.5(5) . . ? N1 C59 C19 109.0(4) . . ? C1 C59 C19 124.3(5) . . ? C23 C21 C20 121.0(6) . . ? C23 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C23 C24 120.2(6) . . ? C21 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.9(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C60 119.9(6) . . ? C24 C25 H25 120.1 . . ? C60 C25 H25 120.1 . . ? C31 C26 C27 118.6(5) . . ? C31 C26 C6 120.6(5) . . ? C27 C26 C6 120.8(5) . . ? C28 C27 C26 120.9(5) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.6(5) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 119.4(5) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 120.3(5) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C26 C31 C30 120.3(5) . . ? C26 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C37 118.2(5) . . ? C33 C32 C11 121.6(5) . . ? C37 C32 C11 120.2(5) . . ? C32 C33 C34 121.2(6) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 119.8(6) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 C34 120.0(5) . . ? C36 C35 H35 120 . . ? C34 C35 H35 120 . . ? C35 C36 C37 119.9(6) . . ? C35 C36 H36 120 . . ? C37 C36 H36 120 . . ? C36 C37 C32 120.8(6) . . ? C36 C37 H37 119.6 . . ? C32 C37 H37 119.6 . . ? C39 C38 C43 117.9(5) . . ? C39 C38 C16 123.4(5) . . ? C43 C38 C16 118.7(5) . . ? C38 C39 C40 120.8(6) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C41 C40 C39 120.9(6) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C42 119.1(6) . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? C41 C42 C43 120.6(6) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C38 120.8(6) . . ? C42 C43 H43 119.6 . . ? C38 C43 H43 119.6 . . ? N6 C44 C45 123.6(6) . . ? N6 C44 H44 118.2 . . ? C45 C44 H44 118.2 . . ? C44 C45 C46 118.2(6) . . ? C44 C45 H45 120.9 . . ? C46 C45 H45 120.9 . . ? C47 C46 C45 119.5(6) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 C48 119.2(6) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? N6 C48 N7 119.6(5) . . ? N6 C48 C47 122.1(5) . . ? N7 C48 C47 118.3(5) . . ? N5 C49 N7 119.3(5) . . ? N5 C49 C50 122.1(5) . . ? N7 C49 C50 118.5(5) . . ? C51 C50 C49 119.0(6) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C50 C51 C52 119.2(6) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? C53 C52 C51 118.6(6) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? N5 C53 C52 123.5(6) . . ? N5 C53 H53 118.3 . . ? C52 C53 H53 118.3 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O1 C55 O2 123.7(6) . . ? O1 C55 C54 116.7(6) . . ? O2 C55 C54 119.5(6) . . ? O3 C57 H57A 109.5 . . ? O3 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O3 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O4 C58 H58A 109.5 . . ? O4 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O4 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C25 C60 C20 121.1(5) . . ? C25 C60 H60 119.4 . . ? C20 C60 H60 119.4 . . ? C17 N1 C59 107.3(4) . . ? C17 N1 Yb1 125.1(4) . . ? C59 N1 Yb1 124.5(4) . . ? C2 N2 C5 107.4(4) . . ? C2 N2 Yb1 122.8(3) . . ? C5 N2 Yb1 122.3(3) . . ? C10 N3 C7 105.0(4) . . ? C10 N3 Yb1 122.6(3) . . ? C7 N3 Yb1 121.3(3) . . ? C12 N4 C15 106.0(4) . . ? C12 N4 Yb1 124.9(3) . . ? C15 N4 Yb1 125.0(3) . . ? C49 N5 C53 117.5(5) . . ? C49 N5 Yb1 126.4(4) . . ? C53 N5 Yb1 115.2(4) . . ? C48 N7 C49 122.8(5) . . ? C48 N7 H98 116(5) . . ? C49 N7 H98 106(6) . . ? C48 N6 C44 117.2(5) . . ? C48 N6 Yb1 125.5(4) . . ? C44 N6 Yb1 117.1(4) . . ? C55 O1 Yb1 145.9(4) . . ? C58 O4 H100 104(9) . . ? C57 O3 H99 111(6) . . ? O1 Yb1 N3 120.08(17) . . ? O1 Yb1 N4 157.20(16) . . ? N3 Yb1 N4 76.32(15) . . ? O1 Yb1 N1 102.90(17) . . ? N3 Yb1 N1 122.75(16) . . ? N4 Yb1 N1 76.96(16) . . ? O1 Yb1 N2 78.62(16) . . ? N3 Yb1 N2 76.63(15) . . ? N4 Yb1 N2 122.70(15) . . ? N1 Yb1 N2 76.98(16) . . ? O1 Yb1 N5 80.69(16) . . ? N3 Yb1 N5 77.46(15) . . ? N4 Yb1 N5 88.50(15) . . ? N1 Yb1 N5 150.08(16) . . ? N2 Yb1 N5 132.19(15) . . ? O1 Yb1 N6 77.85(16) . . ? N3 Yb1 N6 138.93(15) . . ? N4 Yb1 N6 79.56(15) . . ? N1 Yb1 N6 82.47(16) . . ? N2 Yb1 N6 144.23(15) . . ? N5 Yb1 N6 69.12(15) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.52 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.453 _refine_diff_density_min -1.209 _refine_diff_density_rms 0.142 #===END