Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'He, Hongshan' _publ_contact_author_email hongshan.he@sdstate.edu _publ_section_title ; Hybridization of Near-infrared Emitting Erbium (\^a\/c) and Ytterbium (\^a\/c) Monoporphyrinate Complexes with Silica Xerogel: Synthesis, Structure and Photophysics ; loop_ _publ_author_name H.He M.Dubey A.Sykes P.May # Attachment '- 09054.cif' data_09054 _database_code_depnum_ccdc_archive 'CCDC 768345' #TrackingRef '- 09054.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ErTPPCl4(acetate).CH2Cl2.MeOH _chemical_melting_point ? _chemical_formula_moiety 'C61 H42 Cl6 Er N6 O3' _chemical_formula_sum 'C61 H42 Cl6 Er N6 O3' _chemical_formula_weight 1286.97 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.381(4) _cell_length_b 22.415(5) _cell_length_c 15.886(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.166(2) _cell_angle_gamma 90.00 _cell_volume 5475(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9968 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.52 _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 1.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3841 _exptl_absorpt_correction_T_max 0.7286 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 51297 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9639 _reflns_number_gt 7413 _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^)+(0.0511P)^2^+64.8606P] 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 9639 _refine_ls_number_parameters 715 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1728 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.20356(2) 0.097929(17) 0.09772(2) 0.02592(14) Uani 1 1 d . . . Cl4 Cl 0.39946(16) 0.16671(13) -0.38962(15) 0.0462(6) Uani 1 1 d . . . Cl2 Cl -0.00995(17) 0.17102(12) 0.58312(15) 0.0438(6) Uani 1 1 d . . . Cl3 Cl -0.37924(18) 0.19152(16) -0.2851(2) 0.0732(11) Uani 1 1 d . . . Cl1 Cl 0.7604(2) 0.2239(2) 0.5122(3) 0.1128(18) Uani 1 1 d . . . Cl5 Cl 0.1070(3) 0.4772(2) 0.1352(3) 0.1008(13) Uani 1 1 d . . . O2 O 0.2459(4) 0.0320(3) 0.0014(4) 0.0342(15) Uani 1 1 d . . . Cl6 Cl 0.2499(6) 0.4730(3) 0.0668(5) 0.186(4) Uani 1 1 d . . . N3 N 0.1429(4) 0.1521(3) -0.0366(4) 0.0232(15) Uani 1 1 d . . . O1 O 0.1095(5) 0.0256(3) -0.0045(4) 0.0466(18) Uani 1 1 d . . . N6 N 0.3287(5) 0.0327(3) 0.1935(5) 0.0328(18) Uani 1 1 d . . . N1 N 0.2575(4) 0.1497(3) 0.2359(4) 0.0241(15) Uani 1 1 d . . . N4 N 0.3200(5) 0.1543(3) 0.0860(4) 0.0264(16) Uani 1 1 d . . . N5 N 0.1655(5) 0.0226(3) 0.1943(5) 0.0316(17) Uani 1 1 d . . . N2 N 0.0811(4) 0.1453(3) 0.1150(4) 0.0242(15) Uani 1 1 d . . . C10 C -0.0094(5) 0.1568(4) -0.0450(5) 0.0232(18) Uani 1 1 d . . . C11 C 0.0039(5) 0.1568(4) 0.0470(5) 0.0248(18) Uani 1 1 d . . . C5 C 0.2727(5) 0.1580(4) -0.0794(5) 0.0255(18) Uani 1 1 d . . . C43 C 0.6522(7) 0.1633(7) 0.3720(9) 0.074(4) Uani 1 1 d . . . H43 H 0.7021 0.1411 0.3735 0.089 Uiso 1 1 calc R . . C21 C 0.3049(6) 0.1613(4) -0.1559(5) 0.0275(19) Uani 1 1 d . . . C12 C -0.0607(5) 0.1725(4) 0.0836(5) 0.029(2) Uani 1 1 d . . . H12 H -0.1195 0.1825 0.0507 0.035 Uiso 1 1 calc R . . C33 C 0.0949(6) 0.1538(4) 0.3557(5) 0.0265(19) Uani 1 1 d . . . C17 C 0.2818(6) 0.1454(4) 0.3865(5) 0.029(2) Uani 1 1 d . . . H17 H 0.2709 0.1413 0.4411 0.035 Uiso 1 1 calc R . . C28 C -0.1248(6) 0.2151(4) -0.1609(5) 0.034(2) Uani 1 1 d . . . H28 H -0.0826 0.2444 -0.1599 0.041 Uiso 1 1 calc R . . C14 C 0.0645(5) 0.1539(4) 0.1928(5) 0.0240(18) Uani 1 1 d . . . C6 C 0.1831(6) 0.1531(4) -0.0980(5) 0.0262(19) Uani 1 1 d . . . C15 C 0.1278(6) 0.1495(4) 0.2800(5) 0.0253(19) Uani 1 1 d . . . C18 C 0.3592(6) 0.1517(4) 0.3778(6) 0.034(2) Uani 1 1 d . . . H18 H 0.4137 0.1529 0.4253 0.040 Uiso 1 1 calc R . . C27 C -0.1005(6) 0.1644(4) -0.1064(5) 0.0278(19) Uani 1 1 d . . . C7 C 0.1186(6) 0.1518(4) -0.1871(5) 0.0279(19) Uani 1 1 d . . . H7 H 0.1293 0.1499 -0.2421 0.034 Uiso 1 1 calc R . . C031 C 0.0550(5) 0.1538(4) -0.0831(5) 0.0237(18) Uani 1 1 d . . . C38 C 0.1239(6) 0.1992(4) 0.4209(5) 0.029(2) Uani 1 1 d . . . H38 H 0.1662 0.2269 0.4169 0.034 Uiso 1 1 calc R . . C31 C -0.2506(6) 0.1325(5) -0.1635(7) 0.046(3) Uani 1 1 d . . . H31 H -0.2943 0.1046 -0.1638 0.056 Uiso 1 1 calc R . . C50 C 0.3171(6) 0.0050(4) 0.2632(6) 0.032(2) Uani 1 1 d . . . C8 C 0.0409(6) 0.1537(4) -0.1768(5) 0.0257(19) Uani 1 1 d . . . H8 H -0.0140 0.1548 -0.2237 0.031 Uiso 1 1 calc R . . C13 C -0.0232(6) 0.1707(4) 0.1746(5) 0.0273(19) Uani 1 1 d . . . H13 H -0.0504 0.1791 0.2173 0.033 Uiso 1 1 calc R . . C1 C 0.3963(5) 0.1684(4) 0.1536(6) 0.029(2) Uani 1 1 d . . . C16 C 0.2183(6) 0.1461(4) 0.2986(5) 0.0247(18) Uani 1 1 d . . . C57 C 0.2312(6) -0.0010(4) 0.2629(6) 0.033(2) Uani 1 1 d . . . C37 C 0.0921(6) 0.2041(4) 0.4898(6) 0.030(2) Uani 1 1 d . . . H37 H 0.1122 0.2348 0.5332 0.036 Uiso 1 1 calc R . . C4 C 0.3350(5) 0.1627(4) 0.0077(5) 0.0258(19) Uani 1 1 d . . . C23 C 0.3977(6) 0.1219(5) -0.2345(6) 0.039(2) Uani 1 1 d . . . H23 H 0.4397 0.0940 -0.2388 0.047 Uiso 1 1 calc R . . C42 C 0.6585(8) 0.2103(7) 0.4325(8) 0.068(4) Uani 1 1 d . . . C22 C 0.3679(6) 0.1212(4) -0.1618(6) 0.031(2) Uani 1 1 d . . . H22 H 0.3911 0.0927 -0.1154 0.038 Uiso 1 1 calc R . . C3 C 0.4231(6) 0.1819(4) 0.0266(6) 0.032(2) Uani 1 1 d . . . H3 H 0.4502 0.1900 -0.0162 0.038 Uiso 1 1 calc R . . C34 C 0.0337(6) 0.1144(4) 0.3656(6) 0.033(2) Uani 1 1 d . . . H34 H 0.0139 0.0827 0.3238 0.039 Uiso 1 1 calc R . . C56 C 0.0853(7) 0.0101(4) 0.1839(8) 0.046(3) Uani 1 1 d . . . H56 H 0.0401 0.0243 0.1323 0.055 Uiso 1 1 calc R . . C19 C 0.3452(5) 0.1562(4) 0.2828(5) 0.0276(19) Uani 1 1 d . . . C20 C 0.4092(6) 0.1671(4) 0.2455(6) 0.030(2) Uani 1 1 d . . . C39 C 0.4982(6) 0.1826(5) 0.3090(6) 0.037(2) Uani 1 1 d . . . C32 C -0.1643(6) 0.1233(4) -0.1083(6) 0.034(2) Uani 1 1 d . . . H32 H -0.1494 0.0886 -0.0718 0.041 Uiso 1 1 calc R . . C29 C -0.2108(6) 0.2224(5) -0.2166(6) 0.042(3) Uani 1 1 d . . . H29 H -0.2269 0.2563 -0.2547 0.050 Uiso 1 1 calc R . . C30 C -0.2716(6) 0.1816(5) -0.2170(7) 0.046(3) Uani 1 1 d . . . C26 C 0.2744(5) 0.2036(4) -0.2234(5) 0.0270(19) Uani 1 1 d . . . H26 H 0.2332 0.2322 -0.2194 0.032 Uiso 1 1 calc R . . C24 C 0.3641(6) 0.1644(5) -0.2993(6) 0.035(2) Uani 1 1 d . . . C46 C 0.4076(7) 0.0337(5) 0.1879(8) 0.049(3) Uani 1 1 d . . . H46 H 0.4147 0.0521 0.1370 0.059 Uiso 1 1 calc R . . C35 C 0.0009(7) 0.1194(5) 0.4335(7) 0.042(2) Uani 1 1 d . . . H35 H -0.0423 0.0924 0.4374 0.050 Uiso 1 1 calc R . . C36 C 0.0307(6) 0.1639(4) 0.4958(6) 0.035(2) Uani 1 1 d . . . C51 C 0.3693(8) -0.0527(5) 0.4039(7) 0.049(3) Uani 1 1 d . . . C2 C 0.4602(6) 0.1864(4) 0.1167(6) 0.038(2) Uani 1 1 d . . . H2 H 0.5178 0.1991 0.1491 0.046 Uiso 1 1 calc R . . C25 C 0.3019(6) 0.2051(4) -0.2951(6) 0.032(2) Uani 1 1 d . . . H25 H 0.2788 0.2337 -0.3415 0.038 Uiso 1 1 calc R . . C60 C 0.1532(9) -0.0297(6) -0.1089(8) 0.066(4) Uani 1 1 d . . . H60A H 0.0919 -0.0414 -0.1287 0.098 Uiso 1 1 calc R . . H60B H 0.1899 -0.0652 -0.0900 0.098 Uiso 1 1 calc R . . H60C H 0.1655 -0.0102 -0.1584 0.098 Uiso 1 1 calc R . . C53 C 0.2162(7) -0.0350(4) 0.3303(7) 0.042(2) Uani 1 1 d . . . C40 C 0.5085(7) 0.2289(5) 0.3661(6) 0.045(3) Uani 1 1 d . . . H40 H 0.4595 0.2524 0.3636 0.053 Uiso 1 1 calc R . . C48 C 0.4691(7) -0.0181(5) 0.3245(7) 0.047(3) Uani 1 1 d . . . H48 H 0.5178 -0.0347 0.3703 0.057 Uiso 1 1 calc R . . C49 C 0.3885(7) -0.0221(4) 0.3320(6) 0.038(2) Uani 1 1 d . . . C55 C 0.0645(8) -0.0237(5) 0.2471(9) 0.055(3) Uani 1 1 d . . . H55 H 0.0054 -0.0322 0.2388 0.066 Uiso 1 1 calc R . . C44 C 0.5708(7) 0.1502(6) 0.3102(7) 0.053(3) Uani 1 1 d . . . H44 H 0.5647 0.1189 0.2682 0.064 Uiso 1 1 calc R . . C54 C 0.1290(8) -0.0446(5) 0.3209(8) 0.055(3) Uani 1 1 d . . . H54 H 0.1148 -0.0656 0.3659 0.066 Uiso 1 1 calc R . . C59 C 0.1711(7) 0.0105(4) -0.0357(7) 0.040(2) Uani 1 1 d . . . C47 C 0.4809(7) 0.0091(5) 0.2527(9) 0.060(3) Uani 1 1 d . . . H47 H 0.5367 0.0112 0.2470 0.072 Uiso 1 1 calc R . . C58 C 0.4453(9) -0.0825(6) 0.4754(8) 0.073(4) Uani 1 1 d . . . H58A H 0.4996 -0.0722 0.4658 0.110 Uiso 1 1 calc R . . H58B H 0.4374 -0.1259 0.4716 0.110 Uiso 1 1 calc R . . H58C H 0.4480 -0.0687 0.5348 0.110 Uiso 1 1 calc R . . C41 C 0.5903(8) 0.2430(6) 0.4290(8) 0.062(4) Uani 1 1 d . . . H41 H 0.5965 0.2758 0.4687 0.074 Uiso 1 1 calc R . . C52 C 0.2882(9) -0.0591(5) 0.4012(7) 0.054(3) Uani 1 1 d . . . H52 H 0.2775 -0.0805 0.4480 0.065 Uiso 1 1 calc R . . C61 C 0.2016(13) 0.4484(10) 0.1403(16) 0.132(8) Uani 1 1 d . . . H61A H 0.1938 0.4047 0.1324 0.159 Uiso 1 1 calc R . . H61B H 0.2431 0.4552 0.2018 0.159 Uiso 1 1 calc R . . O3 O 0.3762(7) -0.0119(5) -0.0441(7) 0.039(3) Uani 0.590(12) 1 d P . . C62 C 0.4127(13) -0.0609(12) 0.0102(14) 0.083(9) Uani 0.590(12) 1 d P . . H62A H 0.4515 -0.0469 0.0688 0.125 Uiso 0.590(12) 1 calc PR . . H62B H 0.4458 -0.0849 -0.0184 0.125 Uiso 0.590(12) 1 calc PR . . H62C H 0.3663 -0.0853 0.0182 0.125 Uiso 0.590(12) 1 calc PR . . O3' O 0.6717(12) 0.0539(9) 0.2120(13) 0.057(6) Uani 0.410(12) 1 d PD . . C62' C 0.710(2) 0.1116(13) 0.201(3) 0.12(2) Uani 0.410(12) 1 d PD . . H62D H 0.6780 0.1441 0.2165 0.181 Uiso 0.410(12) 1 calc PR . . H62E H 0.7069 0.1160 0.1384 0.181 Uiso 0.410(12) 1 calc PR . . H62F H 0.7711 0.1129 0.2404 0.181 Uiso 0.410(12) 1 calc PR . . 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 Er1 0.0266(2) 0.0255(2) 0.01670(19) 0.00334(17) -0.00388(14) 0.00482(18) Cl4 0.0357(13) 0.0790(19) 0.0234(11) -0.0101(12) 0.0098(10) -0.0055(12) Cl2 0.0485(15) 0.0592(16) 0.0262(12) 0.0042(11) 0.0159(11) 0.0035(12) Cl3 0.0327(15) 0.095(2) 0.0608(19) -0.0299(17) -0.0241(13) 0.0205(15) Cl1 0.048(2) 0.167(4) 0.080(3) 0.035(3) -0.0324(18) -0.048(2) Cl5 0.110(3) 0.087(3) 0.106(3) 0.003(2) 0.038(3) 0.020(3) O2 0.036(4) 0.032(3) 0.025(3) 0.001(3) -0.002(3) 0.005(3) Cl6 0.259(9) 0.189(7) 0.178(6) 0.080(5) 0.164(7) 0.091(6) N3 0.019(3) 0.028(4) 0.016(3) 0.004(3) -0.003(3) 0.004(3) O1 0.053(5) 0.036(4) 0.033(4) -0.002(3) -0.008(3) -0.005(3) N6 0.032(4) 0.028(4) 0.031(4) 0.008(3) 0.001(3) 0.011(3) N1 0.027(4) 0.024(4) 0.015(3) -0.001(3) -0.001(3) -0.002(3) N4 0.029(4) 0.031(4) 0.011(3) 0.002(3) -0.004(3) 0.005(3) N5 0.023(4) 0.033(4) 0.033(4) 0.005(3) 0.001(3) -0.002(3) N2 0.028(4) 0.022(4) 0.015(3) 0.003(3) -0.003(3) 0.001(3) C10 0.018(4) 0.026(4) 0.019(4) 0.007(3) -0.002(3) 0.004(3) C11 0.026(4) 0.027(4) 0.015(4) 0.003(3) -0.003(3) 0.002(3) C5 0.028(5) 0.027(5) 0.015(4) 0.002(3) -0.001(3) 0.003(4) C43 0.021(6) 0.123(13) 0.066(9) 0.034(9) -0.001(6) 0.007(7) C21 0.026(5) 0.031(5) 0.019(4) -0.002(3) 0.000(4) 0.004(4) C12 0.019(4) 0.042(5) 0.019(4) 0.002(4) -0.004(3) 0.008(4) C33 0.031(5) 0.027(5) 0.016(4) 0.002(3) 0.002(4) 0.000(4) C17 0.030(5) 0.037(5) 0.010(4) 0.005(3) -0.006(3) 0.000(4) C28 0.029(5) 0.044(6) 0.018(4) 0.005(4) -0.005(4) 0.009(4) C14 0.028(5) 0.027(5) 0.014(4) 0.002(3) 0.002(3) -0.008(4) C6 0.031(5) 0.023(4) 0.019(4) 0.000(3) 0.001(4) 0.005(4) C15 0.031(5) 0.021(4) 0.018(4) 0.000(3) 0.001(4) -0.004(3) C18 0.027(5) 0.044(6) 0.019(4) 0.007(4) -0.007(4) 0.004(4) C27 0.026(5) 0.033(5) 0.016(4) -0.001(3) -0.003(3) 0.005(4) C7 0.035(5) 0.026(5) 0.018(4) -0.001(3) 0.001(4) 0.001(4) C031 0.023(4) 0.026(4) 0.014(4) 0.002(3) -0.004(3) 0.003(3) C38 0.031(5) 0.027(5) 0.017(4) 0.004(3) -0.005(4) -0.004(4) C31 0.031(5) 0.053(7) 0.046(6) -0.017(5) 0.002(5) -0.006(5) C50 0.033(5) 0.028(5) 0.023(4) -0.001(4) -0.008(4) 0.009(4) C8 0.030(5) 0.029(5) 0.009(4) -0.001(3) -0.005(3) 0.004(4) C13 0.028(5) 0.034(5) 0.018(4) 0.001(4) 0.006(4) -0.004(4) C1 0.020(4) 0.033(5) 0.023(4) -0.002(4) -0.005(4) 0.004(4) C16 0.032(5) 0.023(4) 0.013(4) 0.002(3) -0.001(3) 0.001(4) C57 0.045(6) 0.026(5) 0.024(5) 0.002(4) 0.007(4) 0.005(4) C37 0.037(5) 0.029(5) 0.021(4) 0.002(4) 0.005(4) 0.004(4) C4 0.024(4) 0.031(5) 0.018(4) -0.001(3) 0.002(3) 0.004(4) C23 0.031(5) 0.054(6) 0.026(5) 0.000(4) 0.004(4) 0.015(5) C42 0.030(6) 0.113(12) 0.042(7) 0.006(7) -0.013(5) -0.031(7) C22 0.029(5) 0.042(5) 0.019(4) 0.003(4) 0.002(4) 0.008(4) C3 0.030(5) 0.042(5) 0.023(4) -0.002(4) 0.009(4) 0.002(4) C34 0.043(5) 0.035(5) 0.016(4) 0.000(4) 0.004(4) -0.013(4) C56 0.049(7) 0.033(6) 0.058(7) -0.001(5) 0.022(5) -0.002(5) C19 0.025(5) 0.029(5) 0.019(4) 0.001(3) -0.004(4) 0.007(4) C20 0.025(5) 0.039(5) 0.019(4) -0.002(4) -0.002(4) 0.004(4) C39 0.022(5) 0.059(7) 0.018(4) 0.006(4) -0.008(4) -0.007(4) C32 0.030(5) 0.041(5) 0.022(4) -0.004(4) -0.004(4) 0.005(4) C29 0.029(5) 0.054(6) 0.029(5) -0.001(5) -0.007(4) 0.016(5) C30 0.026(5) 0.070(8) 0.029(5) -0.015(5) -0.008(4) 0.008(5) C26 0.024(4) 0.031(5) 0.024(4) 0.002(4) 0.006(4) -0.001(4) C24 0.032(5) 0.056(6) 0.016(4) -0.011(4) 0.006(4) -0.005(4) C46 0.038(6) 0.048(6) 0.054(7) 0.016(5) 0.007(5) 0.014(5) C35 0.040(6) 0.040(6) 0.040(6) 0.009(5) 0.006(5) -0.007(5) C36 0.044(6) 0.040(5) 0.019(4) 0.006(4) 0.006(4) 0.008(5) C51 0.063(8) 0.042(6) 0.031(5) 0.006(5) 0.001(5) -0.002(5) C2 0.034(5) 0.050(6) 0.021(5) 0.001(4) -0.002(4) -0.001(4) C25 0.028(5) 0.042(5) 0.018(4) 0.003(4) -0.003(4) -0.008(4) C60 0.086(9) 0.065(8) 0.039(6) -0.012(6) 0.014(6) -0.032(7) C53 0.060(7) 0.035(5) 0.035(5) 0.000(4) 0.019(5) 0.003(5) C40 0.031(5) 0.072(8) 0.021(5) -0.001(5) -0.004(4) -0.012(5) C48 0.034(6) 0.044(6) 0.049(6) 0.013(5) -0.005(5) 0.006(5) C49 0.048(6) 0.035(5) 0.022(5) 0.009(4) -0.001(4) 0.006(4) C55 0.053(7) 0.042(6) 0.076(8) -0.002(6) 0.030(7) -0.006(5) C44 0.035(6) 0.075(8) 0.038(6) 0.005(6) -0.001(5) 0.003(6) C54 0.077(9) 0.043(7) 0.056(7) 0.010(5) 0.037(7) 0.000(6) C59 0.049(6) 0.035(6) 0.035(5) 0.011(4) 0.013(5) 0.005(5) C47 0.028(6) 0.042(6) 0.092(10) 0.017(6) 0.000(6) 0.010(5) C58 0.087(10) 0.085(10) 0.036(6) 0.017(6) 0.007(6) 0.008(8) C41 0.039(7) 0.094(10) 0.038(6) -0.006(6) -0.004(5) -0.030(7) C52 0.087(10) 0.045(6) 0.028(5) 0.010(5) 0.016(6) -0.011(6) C61 0.113(16) 0.136(18) 0.17(2) 0.057(16) 0.079(15) 0.058(14) O3 0.037(7) 0.042(7) 0.036(6) 0.003(5) 0.011(5) 0.017(5) C62 0.046(12) 0.13(2) 0.063(14) -0.043(14) 0.001(10) 0.058(13) O3' 0.044(11) 0.072(14) 0.065(13) -0.031(11) 0.034(10) 0.004(10) C62' 0.06(2) 0.17(4) 0.16(4) -0.12(4) 0.06(3) -0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N4 2.348(7) . ? Er1 N3 2.357(6) . ? Er1 N2 2.368(7) . ? Er1 N1 2.368(6) . ? Er1 O2 2.396(6) . ? Er1 O1 2.432(6) . ? Er1 N5 2.501(7) . ? Er1 N6 2.551(7) . ? Er1 C59 2.800(11) . ? Cl4 C24 1.723(9) . ? Cl2 C36 1.741(9) . ? Cl3 C30 1.736(9) . ? Cl1 C42 1.739(11) . ? Cl5 C61 1.655(17) . ? O2 C59 1.259(12) . ? Cl6 C61 1.711(19) . ? N3 C6 1.351(11) . ? N3 C031 1.374(10) . ? O1 C59 1.313(12) . ? N6 C46 1.325(13) . ? N6 C50 1.340(12) . ? N1 C16 1.362(11) . ? N1 C19 1.379(10) . ? N4 C4 1.362(11) . ? N4 C1 1.374(10) . ? N5 C56 1.297(12) . ? N5 C57 1.348(11) . ? N2 C14 1.367(10) . ? N2 C11 1.375(10) . ? C10 C031 1.388(12) . ? C10 C11 1.401(11) . ? C10 C27 1.485(11) . ? C11 C12 1.418(12) . ? C5 C6 1.399(12) . ? C5 C4 1.411(11) . ? C5 C21 1.484(12) . ? C43 C44 1.388(15) . ? C43 C42 1.41(2) . ? C43 H43 0.9500 . ? C21 C26 1.388(12) . ? C21 C22 1.398(12) . ? C12 C13 1.363(11) . ? C12 H12 0.9500 . ? C33 C34 1.386(12) . ? C33 C38 1.414(12) . ? C33 C15 1.481(12) . ? C17 C18 1.328(13) . ? C17 C16 1.425(10) . ? C17 H17 0.9500 . ? C28 C29 1.392(12) . ? C28 C27 1.401(12) . ? C28 H28 0.9500 . ? C14 C13 1.416(12) . ? C14 C15 1.418(11) . ? C6 C7 1.445(11) . ? C15 C16 1.409(12) . ? C18 C19 1.450(12) . ? C18 H18 0.9500 . ? C27 C32 1.386(13) . ? C7 C8 1.339(12) . ? C7 H7 0.9500 . ? C031 C8 1.424(11) . ? C38 C37 1.368(12) . ? C38 H38 0.9500 . ? C31 C30 1.360(16) . ? C31 C32 1.398(13) . ? C31 H31 0.9500 . ? C50 C57 1.412(13) . ? C50 C49 1.432(12) . ? C8 H8 0.9500 . ? C13 H13 0.9500 . ? C1 C20 1.402(12) . ? C1 C2 1.423(13) . ? C57 C53 1.403(13) . ? C37 C36 1.377(13) . ? C37 H37 0.9500 . ? C4 C3 1.435(12) . ? C23 C24 1.372(13) . ? C23 C22 1.400(13) . ? C23 H23 0.9500 . ? C42 C41 1.323(19) . ? C22 H22 0.9500 . ? C3 C2 1.352(12) . ? C3 H3 0.9500 . ? C34 C35 1.365(14) . ? C34 H34 0.9500 . ? C56 C55 1.391(15) . ? C56 H56 0.9500 . ? C19 C20 1.392(13) . ? C20 C39 1.500(11) . ? C39 C40 1.350(14) . ? C39 C44 1.388(15) . ? C32 H32 0.9500 . ? C29 C30 1.350(15) . ? C29 H29 0.9500 . ? C26 C25 1.362(12) . ? C26 H26 0.9500 . ? C24 C25 1.387(13) . ? C46 C47 1.397(14) . ? C46 H46 0.9500 . ? C35 C36 1.371(14) . ? C35 H35 0.9500 . ? C51 C52 1.324(16) . ? C51 C49 1.455(14) . ? C51 C58 1.520(15) . ? C2 H2 0.9500 . ? C25 H25 0.9500 . ? C60 C59 1.419(15) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C53 C54 1.401(16) . ? C53 C52 1.425(15) . ? C40 C41 1.403(14) . ? C40 H40 0.9500 . ? C48 C47 1.366(17) . ? C48 C49 1.369(15) . ? C48 H48 0.9500 . ? C55 C54 1.362(17) . ? C55 H55 0.9500 . ? C44 H44 0.9500 . ? C54 H54 0.9500 . ? C47 H47 0.9500 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C41 H41 0.9500 . ? C52 H52 0.9500 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? O3 C62 1.40(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O3' C62' 1.475(19) . ? C62' H62D 0.9800 . ? C62' H62E 0.9800 . ? C62' H62F 0.9800 . ? 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 N4 Er1 N3 75.6(2) . . ? N4 Er1 N2 120.8(2) . . ? N3 Er1 N2 76.4(2) . . ? N4 Er1 N1 75.9(2) . . ? N3 Er1 N1 119.5(2) . . ? N2 Er1 N1 74.5(2) . . ? N4 Er1 O2 81.9(2) . . ? N3 Er1 O2 82.2(2) . . ? N2 Er1 O2 142.6(2) . . ? N1 Er1 O2 142.8(2) . . ? N4 Er1 O1 130.6(2) . . ? N3 Er1 O1 76.5(2) . . ? N2 Er1 O1 90.5(2) . . ? N1 Er1 O1 153.3(3) . . ? O2 Er1 O1 54.5(2) . . ? N4 Er1 N5 142.4(2) . . ? N3 Er1 N5 141.9(2) . . ? N2 Er1 N5 80.3(2) . . ? N1 Er1 N5 81.6(2) . . ? O2 Er1 N5 99.4(2) . . ? O1 Er1 N5 74.0(2) . . ? N4 Er1 N6 81.2(2) . . ? N3 Er1 N6 146.8(2) . . ? N2 Er1 N6 136.6(2) . . ? N1 Er1 N6 76.2(2) . . ? O2 Er1 N6 71.1(2) . . ? O1 Er1 N6 102.1(2) . . ? N5 Er1 N6 64.3(2) . . ? N4 Er1 C59 105.3(3) . . ? N3 Er1 C59 76.4(3) . . ? N2 Er1 C59 117.0(3) . . ? N1 Er1 C59 163.2(3) . . ? O2 Er1 C59 26.6(3) . . ? O1 Er1 C59 27.9(3) . . ? N5 Er1 C59 88.2(3) . . ? N6 Er1 C59 87.4(3) . . ? C59 O2 Er1 94.9(6) . . ? C6 N3 C031 107.0(7) . . ? C6 N3 Er1 120.2(5) . . ? C031 N3 Er1 122.5(5) . . ? C59 O1 Er1 91.8(6) . . ? C46 N6 C50 118.9(8) . . ? C46 N6 Er1 123.6(6) . . ? C50 N6 Er1 116.4(6) . . ? C16 N1 C19 106.1(7) . . ? C16 N1 Er1 122.0(5) . . ? C19 N1 Er1 122.6(5) . . ? C4 N4 C1 106.2(7) . . ? C4 N4 Er1 123.7(5) . . ? C1 N4 Er1 127.4(6) . . ? C56 N5 C57 120.7(9) . . ? C56 N5 Er1 121.5(7) . . ? C57 N5 Er1 117.6(6) . . ? C14 N2 C11 105.6(7) . . ? C14 N2 Er1 127.4(5) . . ? C11 N2 Er1 125.4(5) . . ? C031 C10 C11 125.9(7) . . ? C031 C10 C27 117.5(7) . . ? C11 C10 C27 116.5(7) . . ? N2 C11 C10 126.2(8) . . ? N2 C11 C12 109.8(7) . . ? C10 C11 C12 123.9(7) . . ? C6 C5 C4 124.3(8) . . ? C6 C5 C21 118.3(7) . . ? C4 C5 C21 117.3(8) . . ? C44 C43 C42 117.9(12) . . ? C44 C43 H43 121.1 . . ? C42 C43 H43 121.1 . . ? C26 C21 C22 117.7(8) . . ? C26 C21 C5 122.2(8) . . ? C22 C21 C5 120.2(8) . . ? C13 C12 C11 107.4(7) . . ? C13 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? C34 C33 C38 116.7(8) . . ? C34 C33 C15 122.1(8) . . ? C38 C33 C15 121.2(8) . . ? C18 C17 C16 107.4(8) . . ? C18 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? C29 C28 C27 119.8(10) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? N2 C14 C13 110.9(7) . . ? N2 C14 C15 124.5(8) . . ? C13 C14 C15 124.5(8) . . ? N3 C6 C5 125.9(7) . . ? N3 C6 C7 109.5(7) . . ? C5 C6 C7 124.6(8) . . ? C16 C15 C14 124.8(8) . . ? C16 C15 C33 118.9(7) . . ? C14 C15 C33 116.1(8) . . ? C17 C18 C19 107.5(7) . . ? C17 C18 H18 126.2 . . ? C19 C18 H18 126.2 . . ? C32 C27 C28 118.4(8) . . ? C32 C27 C10 121.1(8) . . ? C28 C27 C10 120.4(8) . . ? C8 C7 C6 106.5(8) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? N3 C031 C10 125.5(7) . . ? N3 C031 C8 108.9(7) . . ? C10 C031 C8 125.6(7) . . ? C37 C38 C33 121.3(8) . . ? C37 C38 H38 119.4 . . ? C33 C38 H38 119.4 . . ? C30 C31 C32 119.7(10) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? N6 C50 C57 117.9(7) . . ? N6 C50 C49 121.1(9) . . ? C57 C50 C49 120.8(9) . . ? C7 C8 C031 108.0(7) . . ? C7 C8 H8 126.0 . . ? C031 C8 H8 126.0 . . ? C12 C13 C14 106.2(8) . . ? C12 C13 H13 126.9 . . ? C14 C13 H13 126.9 . . ? N4 C1 C20 125.4(8) . . ? N4 C1 C2 110.1(8) . . ? C20 C1 C2 124.5(8) . . ? N1 C16 C15 124.8(7) . . ? N1 C16 C17 110.3(8) . . ? C15 C16 C17 124.6(8) . . ? N5 C57 C53 122.0(9) . . ? N5 C57 C50 118.8(8) . . ? C53 C57 C50 119.1(9) . . ? C38 C37 C36 119.4(8) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? N4 C4 C5 126.0(8) . . ? N4 C4 C3 109.6(7) . . ? C5 C4 C3 124.2(8) . . ? C24 C23 C22 117.6(9) . . ? C24 C23 H23 121.2 . . ? C22 C23 H23 121.2 . . ? C41 C42 C43 121.7(10) . . ? C41 C42 Cl1 121.2(12) . . ? C43 C42 Cl1 117.1(11) . . ? C21 C22 C23 121.5(8) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C2 C3 C4 107.3(8) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? C35 C34 C33 122.3(9) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? N5 C56 C55 121.0(11) . . ? N5 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? N1 C19 C20 125.8(7) . . ? N1 C19 C18 108.4(8) . . ? C20 C19 C18 125.7(8) . . ? C19 C20 C1 125.6(8) . . ? C19 C20 C39 117.0(8) . . ? C1 C20 C39 117.3(8) . . ? C40 C39 C44 119.0(9) . . ? C40 C39 C20 119.8(9) . . ? C44 C39 C20 121.1(9) . . ? C27 C32 C31 120.4(9) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C30 C29 C28 120.5(10) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 121.2(9) . . ? C29 C30 Cl3 120.3(9) . . ? C31 C30 Cl3 118.5(9) . . ? C25 C26 C21 122.0(9) . . ? C25 C26 H26 119.0 . . ? C21 C26 H26 119.0 . . ? C23 C24 C25 122.2(8) . . ? C23 C24 Cl4 118.8(8) . . ? C25 C24 Cl4 119.0(7) . . ? N6 C46 C47 123.7(11) . . ? N6 C46 H46 118.2 . . ? C47 C46 H46 118.2 . . ? C34 C35 C36 119.4(9) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C35 C36 C37 120.9(9) . . ? C35 C36 Cl2 120.2(8) . . ? C37 C36 Cl2 118.9(7) . . ? C52 C51 C49 120.8(10) . . ? C52 C51 C58 122.1(11) . . ? C49 C51 C58 116.8(11) . . ? C3 C2 C1 106.8(8) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? C26 C25 C24 118.9(8) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? 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 . . ? C54 C53 C57 116.2(10) . . ? C54 C53 C52 124.2(10) . . ? C57 C53 C52 119.6(10) . . ? C39 C40 C41 121.3(11) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C47 C48 C49 121.4(9) . . ? C47 C48 H48 119.3 . . ? C49 C48 H48 119.3 . . ? C48 C49 C50 117.7(9) . . ? C48 C49 C51 125.0(9) . . ? C50 C49 C51 117.3(10) . . ? C54 C55 C56 119.9(11) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C39 C44 C43 120.6(12) . . ? C39 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C55 C54 C53 119.9(10) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? O2 C59 O1 118.4(9) . . ? O2 C59 C60 121.3(10) . . ? O1 C59 C60 120.3(10) . . ? O2 C59 Er1 58.5(5) . . ? O1 C59 Er1 60.2(5) . . ? C60 C59 Er1 175.0(8) . . ? C48 C47 C46 117.3(11) . . ? C48 C47 H47 121.4 . . ? C46 C47 H47 121.4 . . ? C51 C58 H58A 109.5 . . ? C51 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C51 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C42 C41 C40 119.3(13) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C51 C52 C53 122.1(10) . . ? C51 C52 H52 118.9 . . ? C53 C52 H52 118.9 . . ? Cl5 C61 Cl6 119.1(12) . . ? Cl5 C61 H61A 107.5 . . ? Cl6 C61 H61A 107.5 . . ? Cl5 C61 H61B 107.5 . . ? Cl6 C61 H61B 107.5 . . ? H61A C61 H61B 107.0 . . ? O3 C62 H62A 109.5 . . ? O3 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O3 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O3' C62' H62D 109.5 . . ? O3' C62' H62E 109.5 . . ? H62D C62' H62E 109.5 . . ? O3' C62' H62F 109.5 . . ? H62D C62' H62F 109.5 . . ? H62E C62' H62F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.304 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.155 # Attachment '- 08059.cif' data_08059 _database_code_depnum_ccdc_archive 'CCDC 768346' #TrackingRef '- 08059.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Yb.TPP.(Methylphen).acetate).2MeOH _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53.14 H35.14 N5.14 O4.29 Yb0.86' _chemical_formula_weight 962.61 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 45.5728(14) _cell_length_b 45.5728(14) _cell_length_c 13.5061(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 24292.5(19) _cell_formula_units_Z 21 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10170 _exptl_absorpt_coefficient_mu 1.787 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 75306 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.38 _reflns_number_total 9858 _reflns_number_gt 6944 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+188.7288P] 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 9858 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.008 _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 C22 C 0.55588(19) 0.06343(19) -0.3910(6) 0.046(2) Uani 1 1 d . . . H22 H 0.5491 0.0775 -0.3615 0.056 Uiso 1 1 calc R . . C51 C 0.7766(3) 0.2025(3) -0.4133(10) 0.102(4) Uani 1 1 d . . . H51A H 0.7857 0.2245 -0.3836 0.153 Uiso 1 1 calc R . . H51B H 0.7664 0.2023 -0.4758 0.153 Uiso 1 1 calc R . . H51C H 0.7944 0.1975 -0.4236 0.153 Uiso 1 1 calc R . . C58 C 0.6869(3) 0.1108(3) 0.1026(8) 0.068(3) Uani 1 1 d . . . C59 C 0.7037(4) 0.1022(4) 0.1850(9) 0.114(5) Uani 1 1 d . . . H59A H 0.7183 0.1224 0.2217 0.170 Uiso 1 1 calc R . . H59B H 0.7167 0.0929 0.1575 0.170 Uiso 1 1 calc R . . H59C H 0.6866 0.0859 0.2284 0.170 Uiso 1 1 calc R . . C60 C 0.7860(4) 0.1660(4) 0.3689(13) 0.127(6) Uani 1 1 d . . . H60A H 0.7969 0.1869 0.3327 0.191 Uiso 1 1 calc R . . H60B H 0.7897 0.1494 0.3359 0.191 Uiso 1 1 calc R . . H60C H 0.7951 0.1696 0.4347 0.191 Uiso 1 1 calc R . . C61 C 0.7501(4) 0.2191(4) 0.2057(11) 0.112(5) Uani 1 1 d . . . H61A H 0.7602 0.2309 0.2662 0.168 Uiso 1 1 calc R . . H61B H 0.7316 0.2224 0.1881 0.168 Uiso 1 1 calc R . . H61C H 0.7668 0.2277 0.1539 0.168 Uiso 1 1 calc R . . O1 O 0.69369(13) 0.14153(16) 0.0915(4) 0.0544(15) Uani 1 1 d . . . O2 O 0.66622(17) 0.08741(17) 0.0459(5) 0.0568(16) Uani 1 1 d . . . O3 O 0.7379(3) 0.1835(3) 0.2190(10) 0.153(5) Uani 1 1 d . . . O4 O 0.7499(3) 0.1538(4) 0.3742(11) 0.189(6) Uani 1 1 d . . . O6 O 0.6976(4) 0.0963(4) 0.4300(12) 0.092(5) Uiso 0.50 1 d P . . O5 O 0.6667 0.3333 -0.566(3) 0.142(13) Uiso 0.50 3 d SP . . C1 C 0.59846(17) 0.07946(16) -0.2553(5) 0.0319(15) Uani 1 1 d . . . C2 C 0.59021(17) 0.06112(16) -0.1666(5) 0.0322(15) Uani 1 1 d . . . C3 C 0.56793(19) 0.02533(18) -0.1588(6) 0.0425(18) Uani 1 1 d . . . H3 H 0.5575 0.0105 -0.2114 0.051 Uiso 1 1 calc R . . C4 C 0.56472(19) 0.01679(17) -0.0631(5) 0.0383(17) Uani 1 1 d . . . H4 H 0.5519 -0.0049 -0.0370 0.046 Uiso 1 1 calc R . . C5 C 0.58478(17) 0.04748(16) -0.0082(5) 0.0319(15) Uani 1 1 d . . . C6 C 0.58549(17) 0.05029(17) 0.0947(6) 0.0344(16) Uani 1 1 d . . . C7 C 0.60031(16) 0.08026(16) 0.1494(5) 0.0317(15) Uani 1 1 d . . . C8 C 0.59613(18) 0.08260(18) 0.2539(6) 0.0383(17) Uani 1 1 d . . . H8 H 0.5849 0.0645 0.2972 0.046 Uiso 1 1 calc R . . C9 C 0.61136(18) 0.11575(18) 0.2784(6) 0.0374(17) Uani 1 1 d . . . H9 H 0.6122 0.1248 0.3408 0.045 Uiso 1 1 calc R . . C10 C 0.62627(17) 0.13454(17) 0.1871(5) 0.0324(15) Uani 1 1 d . . . C11 C 0.64415(18) 0.17025(17) 0.1802(5) 0.0346(16) Uani 1 1 d . . . C12 C 0.65604(17) 0.18848(17) 0.0924(5) 0.0314(15) Uani 1 1 d . . . C13 C 0.67436(17) 0.22481(16) 0.0851(5) 0.0306(15) Uani 1 1 d . . . H13 H 0.6823 0.2399 0.1379 0.037 Uiso 1 1 calc R . . C14 C 0.67809(16) 0.23314(16) -0.0118(5) 0.0295(15) Uani 1 1 d . . . H14 H 0.6884 0.2549 -0.0381 0.035 Uiso 1 1 calc R . . C15 C 0.66306(15) 0.20203(16) -0.0665(5) 0.0265(14) Uani 1 1 d . . . C16 C 0.66068(15) 0.19934(15) -0.1703(5) 0.0262(14) Uani 1 1 d . . . C17 C 0.64632(15) 0.16894(15) -0.2242(5) 0.0256(14) Uani 1 1 d . . . C18 C 0.64114(16) 0.16656(16) -0.3296(5) 0.0322(15) Uani 1 1 d . . . H18 H 0.6482 0.1846 -0.3732 0.039 Uiso 1 1 calc R . . C19 C 0.62423(17) 0.13332(16) -0.3539(5) 0.0323(15) Uani 1 1 d . . . H19 H 0.6177 0.1243 -0.4171 0.039 Uiso 1 1 calc R . . C20 C 0.61837(15) 0.11464(16) -0.2636(5) 0.0288(15) Uani 1 1 d . . . C21 C 0.58218(19) 0.06044(17) -0.3485(5) 0.0369(17) Uani 1 1 d . . . C23 C 0.5397(2) 0.0459(2) -0.4765(7) 0.055(2) Uani 1 1 d . . . H23 H 0.5218 0.0478 -0.5025 0.066 Uiso 1 1 calc R . . C24 C 0.5498(2) 0.0257(2) -0.5225(6) 0.054(2) Uani 1 1 d . . . H24 H 0.5394 0.0144 -0.5807 0.065 Uiso 1 1 calc R . . C25 C 0.5757(3) 0.0225(2) -0.4812(7) 0.063(3) Uani 1 1 d . . . H25 H 0.5825 0.0086 -0.5116 0.076 Uiso 1 1 calc R . . C26 C 0.5920(2) 0.0398(2) -0.3947(7) 0.054(2) Uani 1 1 d . . . H26 H 0.6095 0.0373 -0.3682 0.065 Uiso 1 1 calc R . . C27 C 0.56578(18) 0.01765(17) 0.1538(5) 0.0351(16) Uani 1 1 d . . . C28 C 0.53102(19) 0.00022(18) 0.1542(6) 0.0396(17) Uani 1 1 d . . . H28 H 0.5193 0.0080 0.1158 0.048 Uiso 1 1 calc R . . C29 C 0.5131(2) -0.02871(18) 0.2109(6) 0.0444(19) Uani 1 1 d . . . H29 H 0.4895 -0.0402 0.2106 0.053 Uiso 1 1 calc R . . C30 C 0.5299(2) -0.04048(18) 0.2674(6) 0.0430(19) Uani 1 1 d . . . H30 H 0.5179 -0.0597 0.3065 0.052 Uiso 1 1 calc R . . C31 C 0.5646(2) -0.02359(18) 0.2656(6) 0.046(2) Uani 1 1 d . . . H31 H 0.5761 -0.0318 0.3028 0.056 Uiso 1 1 calc R . . C32 C 0.5828(2) 0.00536(18) 0.2097(6) 0.0407(18) Uani 1 1 d . . . H32 H 0.6063 0.0166 0.2096 0.049 Uiso 1 1 calc R . . C33 C 0.64834(19) 0.18969(17) 0.2728(5) 0.0365(17) Uani 1 1 d . . . C34 C 0.6716(2) 0.1939(2) 0.3448(5) 0.0458(19) Uani 1 1 d . . . H34 H 0.6855 0.1847 0.3349 0.055 Uiso 1 1 calc R . . C35 C 0.6748(2) 0.2114(2) 0.4307(6) 0.058(2) Uani 1 1 d . . . H35 H 0.6904 0.2136 0.4787 0.069 Uiso 1 1 calc R . . C36 C 0.6544(3) 0.2257(2) 0.4450(7) 0.063(3) Uani 1 1 d . . . H36 H 0.6564 0.2379 0.5023 0.075 Uiso 1 1 calc R . . C37 C 0.6313(3) 0.2216(2) 0.3731(7) 0.065(3) Uani 1 1 d . . . H37 H 0.6173 0.2308 0.3824 0.078 Uiso 1 1 calc R . . C38 C 0.6286(3) 0.2041(2) 0.2880(6) 0.057(2) Uani 1 1 d . . . H38 H 0.6131 0.2019 0.2397 0.068 Uiso 1 1 calc R . . C39 C 0.67211(16) 0.23115(16) -0.2280(5) 0.0280(14) Uani 1 1 d . . . C40 C 0.65563(15) 0.24961(16) -0.2198(5) 0.0268(14) Uani 1 1 d . . . H40 H 0.6379 0.2429 -0.1751 0.032 Uiso 1 1 calc R . . C41 C 0.66557(17) 0.27817(16) -0.2783(5) 0.0314(15) Uani 1 1 d . . . H41 H 0.6542 0.2903 -0.2734 0.038 Uiso 1 1 calc R . . C42 C 0.69220(18) 0.28858(17) -0.3437(5) 0.0347(16) Uani 1 1 d . . . H42 H 0.6988 0.3078 -0.3822 0.042 Uiso 1 1 calc R . . C43 C 0.70892(18) 0.27076(16) -0.3519(5) 0.0356(16) Uani 1 1 d . . . H43 H 0.7268 0.2778 -0.3963 0.043 Uiso 1 1 calc R . . C44 C 0.69923(16) 0.24225(16) -0.2942(5) 0.0298(15) Uani 1 1 d . . . H44 H 0.7108 0.2304 -0.2996 0.036 Uiso 1 1 calc R . . C45 C 0.72629(18) 0.19813(18) -0.0706(7) 0.045(2) Uani 1 1 d . . . H45 H 0.7212 0.2026 -0.0077 0.054 Uiso 1 1 calc R . . C46 C 0.75320(19) 0.2240(2) -0.1206(8) 0.053(2) Uani 1 1 d . . . H46 H 0.7656 0.2455 -0.0924 0.064 Uiso 1 1 calc R . . C47 C 0.7612(2) 0.2177(2) -0.2107(9) 0.067(3) Uani 1 1 d . . . H47 H 0.7790 0.2350 -0.2458 0.081 Uiso 1 1 calc R . . C48 C 0.74260(18) 0.1847(2) -0.2532(7) 0.051(2) Uani 1 1 d . . . C49 C 0.71642(18) 0.16020(18) -0.1965(6) 0.0411(19) Uani 1 1 d . . . C50 C 0.7504(2) 0.1764(3) -0.3465(8) 0.061(3) Uani 1 1 d . . . C52 C 0.7345(2) 0.1438(3) -0.3749(7) 0.065(3) Uani 1 1 d . . . H52 H 0.7399 0.1384 -0.4360 0.078 Uiso 1 1 calc R . . C53 C 0.7087(2) 0.1162(2) -0.3127(7) 0.051(2) Uani 1 1 d . . . C54 C 0.69886(17) 0.12532(18) -0.2256(6) 0.0362(17) Uani 1 1 d . . . C55 C 0.6947(2) 0.0816(2) -0.3333(8) 0.061(2) Uani 1 1 d . . . H55 H 0.7010 0.0746 -0.3902 0.073 Uiso 1 1 calc R . . C56 C 0.6720(2) 0.0585(2) -0.2700(8) 0.061(3) Uani 1 1 d . . . H56 H 0.6628 0.0355 -0.2822 0.074 Uiso 1 1 calc R . . C57 C 0.66241(19) 0.06985(19) -0.1843(7) 0.046(2) Uani 1 1 d . . . H57 H 0.6467 0.0538 -0.1411 0.056 Uiso 1 1 calc R . . N1 N 0.63328(12) 0.13714(12) -0.1846(4) 0.0254(12) Uani 1 1 d . . . N2 N 0.60108(14) 0.07414(13) -0.0730(4) 0.0296(12) Uani 1 1 d . . . N3 N 0.61948(13) 0.11230(13) 0.1109(4) 0.0297(12) Uani 1 1 d . . . N4 N 0.65079(13) 0.17477(13) -0.0015(4) 0.0281(12) Uani 1 1 d . . . N5 N 0.70747(14) 0.16744(14) -0.1071(5) 0.0387(15) Uani 1 1 d . . . N6 N 0.67502(14) 0.10245(13) -0.1635(5) 0.0350(14) Uani 1 1 d . . . Yb1 Yb 0.651277(7) 0.124342(7) -0.03546(2) 0.02955(12) 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 C22 0.041(4) 0.033(4) 0.051(5) -0.003(4) 0.004(4) 0.008(4) C51 0.055(6) 0.119(10) 0.117(10) 0.066(8) 0.037(7) 0.032(7) C58 0.060(6) 0.109(9) 0.067(7) 0.048(7) 0.029(5) 0.067(7) C59 0.128(11) 0.208(16) 0.069(8) 0.032(9) 0.003(7) 0.132(12) C60 0.087(10) 0.110(11) 0.181(16) 0.038(11) 0.000(10) 0.045(9) C61 0.101(10) 0.121(12) 0.108(11) -0.019(9) -0.036(8) 0.051(9) O1 0.037(3) 0.072(4) 0.056(4) 0.012(3) -0.006(3) 0.028(3) O2 0.059(4) 0.067(4) 0.066(4) 0.023(3) 0.021(3) 0.048(4) O3 0.143(9) 0.122(9) 0.203(12) -0.027(8) -0.089(9) 0.073(8) O4 0.101(9) 0.238(16) 0.187(13) -0.024(11) -0.009(8) 0.055(9) C1 0.029(4) 0.028(3) 0.034(4) -0.004(3) 0.006(3) 0.010(3) C2 0.032(4) 0.024(3) 0.040(4) 0.003(3) 0.007(3) 0.014(3) C3 0.048(5) 0.026(4) 0.051(5) -0.003(3) 0.002(4) 0.016(3) C4 0.046(4) 0.027(4) 0.038(4) 0.008(3) 0.009(3) 0.015(3) C5 0.031(4) 0.023(3) 0.038(4) 0.005(3) 0.006(3) 0.011(3) C6 0.033(4) 0.028(4) 0.046(5) 0.006(3) 0.005(3) 0.018(3) C7 0.027(3) 0.027(3) 0.040(4) 0.005(3) 0.003(3) 0.013(3) C8 0.036(4) 0.036(4) 0.041(4) 0.010(3) 0.003(3) 0.016(3) C9 0.038(4) 0.037(4) 0.034(4) 0.004(3) -0.001(3) 0.016(3) C10 0.033(4) 0.035(4) 0.031(4) 0.002(3) -0.004(3) 0.019(3) C11 0.039(4) 0.034(4) 0.033(4) 0.001(3) -0.006(3) 0.020(3) C12 0.035(4) 0.031(4) 0.034(4) -0.003(3) -0.008(3) 0.021(3) C13 0.034(4) 0.025(3) 0.033(4) -0.006(3) -0.011(3) 0.015(3) C14 0.028(3) 0.024(3) 0.037(4) -0.001(3) -0.003(3) 0.013(3) C15 0.021(3) 0.026(3) 0.032(4) 0.000(3) -0.002(3) 0.012(3) C16 0.017(3) 0.024(3) 0.037(4) 0.005(3) 0.005(3) 0.010(3) C17 0.017(3) 0.025(3) 0.031(4) -0.003(3) -0.002(3) 0.007(3) C18 0.030(4) 0.026(3) 0.034(4) 0.002(3) 0.007(3) 0.009(3) C19 0.036(4) 0.028(4) 0.027(4) 0.002(3) 0.007(3) 0.011(3) C20 0.023(3) 0.027(3) 0.034(4) -0.004(3) 0.007(3) 0.011(3) C21 0.042(4) 0.025(4) 0.033(4) -0.001(3) 0.012(3) 0.009(3) C23 0.049(5) 0.047(5) 0.052(5) -0.014(4) -0.004(4) 0.012(4) C24 0.064(6) 0.035(4) 0.037(5) -0.003(4) -0.002(4) 0.005(4) C25 0.076(7) 0.034(5) 0.070(7) -0.013(4) 0.010(5) 0.021(5) C26 0.068(6) 0.041(5) 0.056(6) -0.012(4) -0.002(4) 0.029(4) C27 0.039(4) 0.029(4) 0.037(4) -0.001(3) 0.002(3) 0.017(3) C28 0.041(4) 0.033(4) 0.045(5) 0.004(3) 0.003(3) 0.018(3) C29 0.044(4) 0.033(4) 0.045(5) 0.003(3) 0.006(4) 0.012(4) C30 0.061(5) 0.024(4) 0.039(5) 0.005(3) 0.013(4) 0.018(4) C31 0.069(6) 0.033(4) 0.045(5) 0.008(3) 0.002(4) 0.031(4) C32 0.044(4) 0.033(4) 0.047(5) 0.001(3) -0.003(4) 0.020(3) C33 0.044(4) 0.026(4) 0.033(4) 0.004(3) 0.000(3) 0.013(3) C34 0.045(5) 0.054(5) 0.026(4) -0.001(3) -0.001(3) 0.016(4) C35 0.051(5) 0.061(6) 0.031(5) 0.000(4) 0.000(4) 0.005(4) C36 0.091(7) 0.045(5) 0.036(5) -0.004(4) 0.003(5) 0.021(5) C37 0.094(8) 0.067(6) 0.045(6) -0.006(5) 0.004(5) 0.050(6) C38 0.080(6) 0.064(6) 0.037(5) -0.006(4) -0.006(4) 0.045(5) C39 0.026(3) 0.027(3) 0.026(4) -0.003(3) -0.006(3) 0.009(3) C40 0.019(3) 0.029(3) 0.031(4) -0.003(3) -0.002(3) 0.010(3) C41 0.032(4) 0.026(3) 0.036(4) -0.002(3) -0.007(3) 0.014(3) C42 0.049(4) 0.023(3) 0.033(4) 0.001(3) -0.006(3) 0.018(3) C43 0.035(4) 0.025(3) 0.034(4) -0.004(3) 0.007(3) 0.005(3) C44 0.027(3) 0.024(3) 0.036(4) -0.003(3) 0.005(3) 0.012(3) C45 0.030(4) 0.035(4) 0.072(6) 0.000(4) -0.013(4) 0.017(3) C46 0.024(4) 0.033(4) 0.101(8) 0.006(5) -0.002(4) 0.013(3) C47 0.021(4) 0.042(5) 0.129(10) 0.032(6) -0.004(5) 0.008(4) C48 0.026(4) 0.050(5) 0.078(6) 0.021(4) 0.010(4) 0.021(4) C49 0.028(4) 0.035(4) 0.063(5) 0.013(4) 0.003(4) 0.018(3) C50 0.037(5) 0.061(6) 0.083(7) 0.029(5) 0.012(5) 0.024(4) C52 0.043(5) 0.103(8) 0.062(6) 0.017(6) 0.020(4) 0.047(6) C53 0.039(4) 0.062(5) 0.065(6) 0.010(4) 0.012(4) 0.035(4) C54 0.026(3) 0.039(4) 0.051(5) 0.006(3) 0.006(3) 0.021(3) C55 0.046(5) 0.065(6) 0.079(7) -0.005(5) 0.013(5) 0.034(5) C56 0.050(5) 0.052(5) 0.094(8) -0.018(5) 0.002(5) 0.034(5) C57 0.037(4) 0.034(4) 0.073(6) 0.000(4) 0.004(4) 0.022(4) N1 0.024(3) 0.019(3) 0.034(3) 0.003(2) 0.004(2) 0.011(2) N2 0.032(3) 0.027(3) 0.033(3) 0.002(2) 0.005(2) 0.016(2) N3 0.031(3) 0.026(3) 0.032(3) 0.003(2) -0.005(2) 0.014(2) N4 0.030(3) 0.032(3) 0.025(3) 0.004(2) -0.001(2) 0.017(2) N5 0.026(3) 0.027(3) 0.063(4) 0.006(3) -0.003(3) 0.012(3) N6 0.033(3) 0.024(3) 0.052(4) 0.001(3) 0.003(3) 0.017(3) Yb1 0.02594(17) 0.02407(17) 0.0389(2) 0.00308(12) 0.00111(12) 0.01270(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C22 C23 1.388(11) . ? C22 C21 1.395(11) . ? C51 C50 1.494(12) . ? C58 O2 1.268(13) . ? C58 O1 1.283(12) . ? C58 C59 1.508(13) . ? C58 Yb1 2.738(9) . ? C60 O4 1.449(16) . ? C61 O3 1.442(16) . ? O1 Yb1 2.403(5) . ? O2 Yb1 2.377(5) . ? C1 C20 1.397(9) . ? C1 C2 1.401(10) . ? C1 C21 1.498(10) . ? C2 N2 1.378(9) . ? C2 C3 1.431(9) . ? C3 C4 1.337(10) . ? C4 C5 1.436(10) . ? C5 N2 1.376(8) . ? C5 C6 1.395(10) . ? C6 C7 1.395(10) . ? C6 C27 1.523(10) . ? C7 N3 1.375(8) . ? C7 C8 1.434(10) . ? C8 C9 1.351(10) . ? C9 C10 1.461(10) . ? C10 N3 1.367(9) . ? C10 C11 1.412(10) . ? C11 C12 1.393(10) . ? C11 C33 1.489(10) . ? C12 N4 1.381(8) . ? C12 C13 1.437(9) . ? C13 C14 1.349(9) . ? C14 C15 1.433(9) . ? C15 N4 1.390(8) . ? C15 C16 1.406(9) . ? C16 C17 1.404(9) . ? C16 C39 1.492(9) . ? C17 N1 1.370(8) . ? C17 C18 1.437(9) . ? C18 C19 1.353(9) . ? C19 C20 1.433(9) . ? C20 N1 1.398(8) . ? C21 C26 1.377(10) . ? C23 C24 1.365(12) . ? C24 C25 1.378(13) . ? C25 C26 1.397(12) . ? C27 C28 1.372(10) . ? C27 C32 1.384(10) . ? C28 C29 1.384(10) . ? C29 C30 1.364(11) . ? C30 C31 1.371(11) . ? C31 C32 1.380(10) . ? C33 C38 1.369(11) . ? C33 C34 1.379(10) . ? C34 C35 1.373(11) . ? C35 C36 1.388(14) . ? C36 C37 1.376(14) . ? C37 C38 1.369(12) . ? C39 C40 1.384(9) . ? C39 C44 1.400(9) . ? C40 C41 1.391(9) . ? C41 C42 1.379(10) . ? C42 C43 1.368(10) . ? C43 C44 1.384(9) . ? C45 N5 1.317(9) . ? C45 C46 1.380(11) . ? C46 C47 1.342(14) . ? C47 C48 1.427(13) . ? C48 C49 1.387(10) . ? C48 C50 1.409(13) . ? C49 N5 1.367(10) . ? C49 C54 1.432(10) . ? C50 C52 1.343(14) . ? C52 C53 1.479(12) . ? C53 C54 1.393(11) . ? C53 C55 1.403(12) . ? C54 N6 1.356(9) . ? C55 C56 1.348(13) . ? C56 C57 1.424(12) . ? C57 N6 1.328(9) . ? N1 Yb1 2.356(5) . ? N2 Yb1 2.343(5) . ? N3 Yb1 2.348(6) . ? N4 Yb1 2.354(5) . ? N5 Yb1 2.514(6) . ? N6 Yb1 2.497(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 C23 C22 C21 121.4(8) . . ? O2 C58 O1 121.2(8) . . ? O2 C58 C59 119.2(11) . . ? O1 C58 C59 119.5(13) . . ? O2 C58 Yb1 60.2(4) . . ? O1 C58 Yb1 61.3(4) . . ? C59 C58 Yb1 174.5(7) . . ? C58 O1 Yb1 90.7(6) . . ? C58 O2 Yb1 92.3(5) . . ? C20 C1 C2 125.4(6) . . ? C20 C1 C21 116.5(6) . . ? C2 C1 C21 117.8(6) . . ? N2 C2 C1 126.6(6) . . ? N2 C2 C3 108.7(6) . . ? C1 C2 C3 124.7(7) . . ? C4 C3 C2 108.3(7) . . ? C3 C4 C5 107.0(6) . . ? N2 C5 C6 125.2(6) . . ? N2 C5 C4 109.4(6) . . ? C6 C5 C4 125.3(6) . . ? C7 C6 C5 126.5(6) . . ? C7 C6 C27 116.1(6) . . ? C5 C6 C27 117.2(6) . . ? N3 C7 C6 125.4(6) . . ? N3 C7 C8 109.3(6) . . ? C6 C7 C8 125.2(6) . . ? C9 C8 C7 108.2(6) . . ? C8 C9 C10 106.1(7) . . ? N3 C10 C11 126.2(6) . . ? N3 C10 C9 109.6(6) . . ? C11 C10 C9 124.2(6) . . ? C12 C11 C10 124.9(6) . . ? C12 C11 C33 117.6(6) . . ? C10 C11 C33 117.3(6) . . ? N4 C12 C11 125.7(6) . . ? N4 C12 C13 109.1(6) . . ? C11 C12 C13 125.1(6) . . ? C14 C13 C12 108.0(6) . . ? C13 C14 C15 106.9(6) . . ? N4 C15 C16 124.9(6) . . ? N4 C15 C14 109.8(6) . . ? C16 C15 C14 125.3(6) . . ? C17 C16 C15 125.5(6) . . ? C17 C16 C39 116.9(6) . . ? C15 C16 C39 117.5(6) . . ? N1 C17 C16 125.6(6) . . ? N1 C17 C18 109.8(5) . . ? C16 C17 C18 124.5(6) . . ? C19 C18 C17 107.7(6) . . ? C18 C19 C20 106.9(6) . . ? C1 C20 N1 125.4(6) . . ? C1 C20 C19 124.8(6) . . ? N1 C20 C19 109.6(5) . . ? C26 C21 C22 118.0(7) . . ? C26 C21 C1 122.7(7) . . ? C22 C21 C1 119.4(7) . . ? C24 C23 C22 120.4(9) . . ? C23 C24 C25 118.9(8) . . ? C24 C25 C26 121.3(8) . . ? C21 C26 C25 120.1(9) . . ? C28 C27 C32 118.7(7) . . ? C28 C27 C6 120.9(6) . . ? C32 C27 C6 120.3(6) . . ? C27 C28 C29 120.9(7) . . ? C30 C29 C28 120.3(7) . . ? C29 C30 C31 119.1(7) . . ? C30 C31 C32 121.2(7) . . ? C31 C32 C27 119.8(7) . . ? C38 C33 C34 118.1(7) . . ? C38 C33 C11 119.5(7) . . ? C34 C33 C11 122.5(7) . . ? C35 C34 C33 121.8(9) . . ? C34 C35 C36 119.3(9) . . ? C37 C36 C35 118.9(8) . . ? C38 C37 C36 120.8(10) . . ? C33 C38 C37 121.1(9) . . ? C40 C39 C44 118.7(6) . . ? C40 C39 C16 121.2(6) . . ? C44 C39 C16 120.1(6) . . ? C39 C40 C41 120.1(6) . . ? C42 C41 C40 120.3(6) . . ? C43 C42 C41 120.3(6) . . ? C42 C43 C44 120.0(6) . . ? C43 C44 C39 120.6(6) . . ? N5 C45 C46 123.7(9) . . ? C47 C46 C45 118.6(8) . . ? C46 C47 C48 120.7(8) . . ? C49 C48 C50 120.6(8) . . ? C49 C48 C47 116.3(9) . . ? C50 C48 C47 123.0(8) . . ? N5 C49 C48 122.3(7) . . ? N5 C49 C54 116.3(6) . . ? C48 C49 C54 121.3(8) . . ? C52 C50 C48 118.8(8) . . ? C52 C50 C51 118.8(11) . . ? C48 C50 C51 122.4(10) . . ? C50 C52 C53 122.6(9) . . ? C54 C53 C55 117.9(8) . . ? C54 C53 C52 117.6(8) . . ? C55 C53 C52 124.4(8) . . ? N6 C54 C53 123.2(7) . . ? N6 C54 C49 118.1(7) . . ? C53 C54 C49 118.5(7) . . ? C56 C55 C53 119.5(9) . . ? C55 C56 C57 119.1(8) . . ? N6 C57 C56 122.6(8) . . ? C17 N1 C20 105.8(5) . . ? C17 N1 Yb1 125.1(4) . . ? C20 N1 Yb1 124.9(4) . . ? C5 N2 C2 106.5(5) . . ? C5 N2 Yb1 123.8(4) . . ? C2 N2 Yb1 125.7(4) . . ? C10 N3 C7 106.9(6) . . ? C10 N3 Yb1 125.2(4) . . ? C7 N3 Yb1 123.9(4) . . ? C12 N4 C15 105.9(5) . . ? C12 N4 Yb1 122.4(4) . . ? C15 N4 Yb1 123.6(4) . . ? C45 N5 C49 118.2(7) . . ? C45 N5 Yb1 123.7(6) . . ? C49 N5 Yb1 117.5(4) . . ? C57 N6 C54 117.4(7) . . ? C57 N6 Yb1 124.2(5) . . ? C54 N6 Yb1 117.5(4) . . ? N2 Yb1 N3 76.53(19) . . ? N2 Yb1 N4 120.94(18) . . ? N3 Yb1 N4 76.01(18) . . ? N2 Yb1 N1 76.45(18) . . ? N3 Yb1 N1 121.81(18) . . ? N4 Yb1 N1 75.55(17) . . ? N2 Yb1 O2 83.9(2) . . ? N3 Yb1 O2 78.88(19) . . ? N4 Yb1 O2 138.3(2) . . ? N1 Yb1 O2 146.0(2) . . ? N2 Yb1 O1 134.9(2) . . ? N3 Yb1 O1 77.14(19) . . ? N4 Yb1 O1 86.6(2) . . ? N1 Yb1 O1 148.46(19) . . ? O2 Yb1 O1 55.4(2) . . ? N2 Yb1 N6 82.32(18) . . ? N3 Yb1 N6 146.06(18) . . ? N4 Yb1 N6 137.93(18) . . ? N1 Yb1 N6 77.35(18) . . ? O2 Yb1 N6 72.7(2) . . ? O1 Yb1 N6 100.7(2) . . ? N2 Yb1 N5 142.7(2) . . ? N3 Yb1 N5 140.8(2) . . ? N4 Yb1 N5 79.35(19) . . ? N1 Yb1 N5 79.77(18) . . ? O2 Yb1 N5 101.0(2) . . ? O1 Yb1 N5 71.4(2) . . ? N6 Yb1 N5 64.55(19) . . ? N2 Yb1 C58 109.1(3) . . ? N3 Yb1 C58 75.0(2) . . ? N4 Yb1 C58 112.5(3) . . ? N1 Yb1 C58 163.2(2) . . ? O2 Yb1 C58 27.6(3) . . ? O1 Yb1 C58 27.9(3) . . ? N6 Yb1 C58 87.5(3) . . ? N5 Yb1 C58 87.2(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.816 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.137