Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'Peter Roesky' ; Freie Universitaet Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; 'Nils Meyer' ; Freie Universitaet Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_contact_author_name 'Peter Roesky' _publ_contact_author_address ; Fachbereich Biologie Freie Universitat Berlin Institut fur Chemia/Anorg.und Analy Fabookstrabe, 34-36 Berlin D-14195 GERMANY ; _publ_contact_author_email ROESKY@CHEMIE.FU-BERLIN.DE _publ_section_title ; Chiral Bridged Aminotroponiminate Complexes of the Lanthanides ; _publ_contact_author ; Prof. Dr. Peter Roesky Freie Universitaet Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_contact_author_fax +49/(0)3083852440 _publ_contact_author_phone +49/(0)3083854004 _publ_contact_letter ; ; _publ_requested_coeditor_name ? data_1a _database_code_depnum_ccdc_archive 'CCDC 638155' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H52 Li2 N4 O2' _chemical_formula_weight 658.76 _chemical_absolute_configuration rmad 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.581(3) _cell_length_b 10.365(3) _cell_length_c 38.296(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3803(2) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description neeldes _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.753247 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30788 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.06 _reflns_number_total 6683 _reflns_number_gt 5382 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0429P)^2^+2.9638P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.5(19) _refine_ls_number_reflns 6683 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2081(3) -0.1618(3) 0.10050(8) 0.0219(7) Uani 1 1 d . . . C2 C 0.2468(4) -0.2942(3) 0.09871(9) 0.0311(8) Uani 1 1 d . . . H2 H 0.2191 -0.3344 0.0775 0.037 Uiso 1 1 calc R . . C3 C 0.3152(4) -0.3760(3) 0.12083(10) 0.0370(9) Uani 1 1 d . . . H3 H 0.3316 -0.4597 0.1116 0.044 Uiso 1 1 calc R . . C4 C 0.3649(4) -0.3574(3) 0.15466(9) 0.0343(9) Uani 1 1 d . . . H4 H 0.4130 -0.4269 0.1655 0.041 Uiso 1 1 calc R . . C5 C 0.3489(3) -0.2449(3) 0.17342(8) 0.0302(8) Uani 1 1 d . . . H5 H 0.3860 -0.2477 0.1964 0.036 Uiso 1 1 calc R . . C6 C 0.2882(3) -0.1290(3) 0.16448(8) 0.0274(8) Uani 1 1 d . . . H6 H 0.2883 -0.0675 0.1829 0.033 Uiso 1 1 calc R . . C7 C 0.2255(3) -0.0830(3) 0.13318(8) 0.0204(7) Uani 1 1 d . . . C8 C 0.1749(3) 0.1231(3) 0.16011(7) 0.0190(7) Uani 1 1 d . . . H8 H 0.1397 0.0746 0.1809 0.023 Uiso 1 1 calc R . . C9 C 0.0712(3) 0.2341(3) 0.15167(7) 0.0173(6) Uani 1 1 d . . . H9 H 0.1178 0.2955 0.1352 0.021 Uiso 1 1 calc R . . C10 C -0.1311(3) 0.2476(3) 0.11433(7) 0.0163(6) Uani 1 1 d . . . C11 C -0.1242(3) 0.3839(3) 0.11342(8) 0.0219(7) Uani 1 1 d . . . H11 H -0.0571 0.4189 0.1290 0.026 Uiso 1 1 calc R . . C12 C -0.1947(4) 0.4762(3) 0.09463(8) 0.0291(8) Uani 1 1 d . . . H12 H -0.1681 0.5626 0.0996 0.035 Uiso 1 1 calc R . . C13 C -0.2985(4) 0.4637(3) 0.06948(9) 0.0303(8) Uani 1 1 d . . . H13 H -0.3341 0.5404 0.0592 0.036 Uiso 1 1 calc R . . C14 C -0.3540(3) 0.3468(3) 0.05831(8) 0.0256(8) Uani 1 1 d . . . H14 H -0.4238 0.3547 0.0408 0.031 Uiso 1 1 calc R . . C15 C -0.3257(3) 0.2219(3) 0.06805(8) 0.0205(7) Uani 1 1 d . . . H15 H -0.3806 0.1596 0.0561 0.025 Uiso 1 1 calc R . . C16 C -0.2300(3) 0.1670(3) 0.09261(7) 0.0157(6) Uani 1 1 d . . . C17 C -0.3090(3) -0.0477(3) 0.07918(8) 0.0224(7) Uani 1 1 d . . . H17 H -0.3117 -0.0240 0.0539 0.027 Uiso 1 1 calc R . . C18 C -0.4567(3) -0.0462(4) 0.09356(9) 0.0328(9) Uani 1 1 d . . . H18A H -0.4944 0.0415 0.0922 0.049 Uiso 1 1 calc R . . H18B H -0.4557 -0.0745 0.1180 0.049 Uiso 1 1 calc R . . H18C H -0.5154 -0.1047 0.0798 0.049 Uiso 1 1 calc R . . C19 C -0.2491(4) -0.1829(3) 0.08283(8) 0.0300(8) Uani 1 1 d . . . H19A H -0.2559 -0.2107 0.1072 0.045 Uiso 1 1 calc R . . H19B H -0.1509 -0.1825 0.0756 0.045 Uiso 1 1 calc R . . H19C H -0.3018 -0.2425 0.0680 0.045 Uiso 1 1 calc R . . C20 C 0.1315(4) -0.1600(3) 0.04012(8) 0.0263(8) Uani 1 1 d . . . H20 H 0.0904 -0.2478 0.0434 0.032 Uiso 1 1 calc R . . C21 C 0.2707(4) -0.1716(4) 0.02101(9) 0.0450(11) Uani 1 1 d . . . H21A H 0.3361 -0.2215 0.0353 0.067 Uiso 1 1 calc R . . H21B H 0.3089 -0.0853 0.0168 0.067 Uiso 1 1 calc R . . H21C H 0.2563 -0.2156 -0.0014 0.067 Uiso 1 1 calc R . . C22 C 0.0314(4) -0.0772(3) 0.01870(9) 0.0299(8) Uani 1 1 d . . . H22A H 0.0720 0.0086 0.0153 0.045 Uiso 1 1 calc R . . H22B H -0.0576 -0.0693 0.0311 0.045 Uiso 1 1 calc R . . H22C H 0.0156 -0.1180 -0.0041 0.045 Uiso 1 1 calc R . . C23 C 0.3166(3) 0.1798(3) 0.16879(8) 0.0221(7) Uani 1 1 d . . . C24 C 0.3671(4) 0.1803(4) 0.20318(9) 0.0364(9) Uani 1 1 d . . . H24 H 0.3164 0.1382 0.2212 0.044 Uiso 1 1 calc R . . C25 C 0.4920(4) 0.2428(5) 0.21071(11) 0.0553(12) Uani 1 1 d . . . H25 H 0.5264 0.2420 0.2340 0.066 Uiso 1 1 calc R . . C26 C 0.5660(4) 0.3054(4) 0.18543(10) 0.0440(10) Uani 1 1 d . . . H26 H 0.6497 0.3497 0.1912 0.053 Uiso 1 1 calc R . . C27 C 0.5184(4) 0.3036(4) 0.15153(10) 0.0350(9) Uani 1 1 d . . . H27 H 0.5704 0.3450 0.1336 0.042 Uiso 1 1 calc R . . C28 C 0.3944(3) 0.2412(3) 0.14354(8) 0.0270(8) Uani 1 1 d . . . H28 H 0.3624 0.2408 0.1201 0.032 Uiso 1 1 calc R . . C29 C 0.0348(3) 0.3067(3) 0.18517(7) 0.0201(7) Uani 1 1 d . . . C30 C 0.1116(3) 0.4142(3) 0.19488(9) 0.0272(8) Uani 1 1 d . . . H30 H 0.1832 0.4451 0.1799 0.033 Uiso 1 1 calc R . . C31 C 0.0853(4) 0.4771(4) 0.22611(9) 0.0354(9) Uani 1 1 d . . . H31 H 0.1395 0.5499 0.2327 0.042 Uiso 1 1 calc R . . C32 C -0.0204(4) 0.4331(4) 0.24773(9) 0.0343(9) Uani 1 1 d . . . H32 H -0.0395 0.4764 0.2691 0.041 Uiso 1 1 calc R . . C33 C -0.0975(4) 0.3273(4) 0.23840(8) 0.0336(9) Uani 1 1 d . . . H33 H -0.1695 0.2972 0.2534 0.040 Uiso 1 1 calc R . . C34 C -0.0708(3) 0.2631(3) 0.20690(8) 0.0260(7) Uani 1 1 d . . . H34 H -0.1249 0.1900 0.2005 0.031 Uiso 1 1 calc R . . C35 C 0.2633(4) 0.2536(4) 0.04043(11) 0.0477(11) Uani 1 1 d . . . H35A H 0.2858 0.1988 0.0200 0.057 Uiso 1 1 calc R . . H35B H 0.3340 0.2383 0.0588 0.057 Uiso 1 1 calc R . . C36 C 0.2609(4) 0.3941(4) 0.03015(12) 0.0440(10) Uani 1 1 d . . . H36A H 0.3005 0.4061 0.0065 0.053 Uiso 1 1 calc R . . H36B H 0.3151 0.4467 0.0469 0.053 Uiso 1 1 calc R . . C37 C 0.1074(4) 0.4317(4) 0.03088(11) 0.0416(10) Uani 1 1 d . . . H37A H 0.0864 0.4868 0.0513 0.050 Uiso 1 1 calc R . . H37B H 0.0809 0.4785 0.0093 0.050 Uiso 1 1 calc R . . C38 C 0.0330(3) 0.3056(3) 0.03333(8) 0.0253(8) Uani 1 1 d . . . H38A H -0.0578 0.3156 0.0454 0.030 Uiso 1 1 calc R . . H38B H 0.0164 0.2688 0.0098 0.030 Uiso 1 1 calc R . . C39 C -0.2452(4) -0.1284(4) 0.18734(9) 0.0387(9) Uani 1 1 d . . . H39A H -0.3249 -0.1120 0.1715 0.046 Uiso 1 1 calc R . . H39B H -0.2406 -0.0583 0.2049 0.046 Uiso 1 1 calc R . . C40 C -0.2599(5) -0.2585(4) 0.20502(12) 0.0593(13) Uani 1 1 d . . . H40A H -0.2138 -0.2585 0.2282 0.071 Uiso 1 1 calc R . . H40B H -0.3594 -0.2818 0.2080 0.071 Uiso 1 1 calc R . . C41 C -0.1893(4) -0.3489(4) 0.18067(11) 0.0501(11) Uani 1 1 d . . . H41A H -0.2511 -0.3733 0.1610 0.060 Uiso 1 1 calc R . . H41B H -0.1575 -0.4278 0.1929 0.060 Uiso 1 1 calc R . . C42 C -0.0671(3) -0.2684(3) 0.16827(9) 0.0322(8) Uani 1 1 d . . . H42A H 0.0131 -0.2778 0.1844 0.039 Uiso 1 1 calc R . . H42B H -0.0377 -0.2955 0.1446 0.039 Uiso 1 1 calc R . . Li1 Li 0.0948(6) 0.0825(5) 0.08497(14) 0.0292(13) Uani 1 1 d . . . Li2 Li -0.0752(6) -0.0092(5) 0.13308(15) 0.0294(13) Uani 1 1 d . . . N1 N 0.1489(3) -0.0973(3) 0.07456(6) 0.0221(6) Uani 1 1 d . . . N2 N 0.1760(3) 0.0363(2) 0.12999(6) 0.0202(6) Uani 1 1 d . . . N3 N -0.0482(2) 0.1755(2) 0.13377(6) 0.0187(6) Uani 1 1 d . . . N4 N -0.2167(3) 0.0425(2) 0.09763(6) 0.0181(6) Uani 1 1 d . . . O1 O 0.1259(2) 0.2252(2) 0.05322(5) 0.0287(5) Uani 1 1 d . . . O2 O -0.1159(2) -0.1370(2) 0.16788(6) 0.0298(6) 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 0.0249(16) 0.0205(17) 0.0204(16) 0.0006(14) 0.0036(13) -0.0016(14) C2 0.040(2) 0.0237(19) 0.0297(19) -0.0023(15) -0.0089(16) 0.0027(16) C3 0.044(2) 0.024(2) 0.042(2) -0.0027(17) -0.0055(18) 0.0063(17) C4 0.040(2) 0.027(2) 0.036(2) 0.0119(16) -0.0033(17) 0.0085(16) C5 0.0294(18) 0.038(2) 0.0232(17) 0.0110(16) -0.0009(14) 0.0098(17) C6 0.0256(17) 0.038(2) 0.0189(17) 0.0032(15) -0.0007(14) 0.0051(15) C7 0.0179(15) 0.0250(18) 0.0182(16) 0.0032(13) 0.0033(13) 0.0012(13) C8 0.0232(16) 0.0250(17) 0.0088(14) -0.0020(13) -0.0011(12) 0.0016(13) C9 0.0207(15) 0.0213(17) 0.0098(14) -0.0034(13) -0.0016(12) 0.0000(13) C10 0.0206(14) 0.0203(16) 0.0080(13) -0.0001(12) 0.0002(12) -0.0001(13) C11 0.0271(16) 0.0196(17) 0.0190(16) -0.0010(13) -0.0044(14) 0.0002(14) C12 0.042(2) 0.0212(18) 0.0244(18) 0.0000(15) -0.0095(16) 0.0015(16) C13 0.039(2) 0.0235(18) 0.0281(19) 0.0023(16) -0.0142(17) 0.0034(16) C14 0.0288(17) 0.028(2) 0.0202(17) 0.0001(14) -0.0070(14) 0.0042(15) C15 0.0239(16) 0.0202(17) 0.0173(15) -0.0021(13) -0.0037(13) 0.0021(13) C16 0.0171(15) 0.0191(16) 0.0111(14) 0.0012(12) 0.0020(12) 0.0012(13) C17 0.0240(16) 0.0224(18) 0.0208(16) 0.0001(14) -0.0033(14) -0.0038(14) C18 0.0264(18) 0.038(2) 0.034(2) 0.0000(17) -0.0038(16) -0.0111(16) C19 0.044(2) 0.0235(18) 0.0228(17) 0.0006(15) -0.0069(15) -0.0013(16) C20 0.0334(18) 0.0300(19) 0.0155(16) -0.0054(14) -0.0025(14) 0.0005(16) C21 0.042(2) 0.071(3) 0.0218(19) -0.0148(19) 0.0000(16) 0.016(2) C22 0.036(2) 0.034(2) 0.0190(18) -0.0037(15) -0.0040(15) 0.0023(16) C23 0.0220(16) 0.0286(18) 0.0157(15) -0.0064(14) -0.0031(13) 0.0038(14) C24 0.0335(19) 0.056(3) 0.0204(18) 0.0025(17) -0.0067(15) -0.0062(19) C25 0.050(2) 0.077(3) 0.039(2) -0.006(2) -0.027(2) -0.011(2) C26 0.0282(19) 0.055(3) 0.049(2) -0.006(2) -0.0069(18) -0.0067(19) C27 0.0253(18) 0.037(2) 0.042(2) -0.0092(18) 0.0051(16) -0.0028(16) C28 0.0229(17) 0.036(2) 0.0222(17) -0.0073(15) 0.0015(13) -0.0008(15) C29 0.0241(16) 0.0242(18) 0.0121(15) -0.0001(13) -0.0044(12) -0.0003(14) C30 0.0286(18) 0.030(2) 0.0226(18) -0.0028(15) -0.0033(14) -0.0016(15) C31 0.045(2) 0.035(2) 0.026(2) -0.0103(17) -0.0096(17) 0.0026(18) C32 0.046(2) 0.041(2) 0.0163(17) -0.0093(16) -0.0036(16) 0.0109(18) C33 0.0351(19) 0.047(2) 0.0184(17) 0.0043(16) 0.0073(15) 0.0088(18) C34 0.0271(17) 0.031(2) 0.0204(17) 0.0024(15) 0.0031(14) 0.0011(15) C35 0.031(2) 0.065(3) 0.047(2) 0.021(2) 0.0009(18) 0.001(2) C36 0.036(2) 0.044(2) 0.052(2) 0.001(2) 0.0082(19) -0.0095(19) C37 0.047(2) 0.033(2) 0.044(2) 0.0068(18) 0.0122(19) -0.0025(19) C38 0.0307(17) 0.032(2) 0.0132(16) 0.0039(14) 0.0001(13) 0.0033(16) C39 0.033(2) 0.059(3) 0.0241(19) -0.0011(18) 0.0061(16) 0.0089(19) C40 0.055(3) 0.071(3) 0.052(3) 0.007(3) 0.020(2) -0.018(3) C41 0.045(2) 0.050(3) 0.055(3) 0.017(2) 0.009(2) -0.008(2) C42 0.0305(18) 0.031(2) 0.035(2) 0.0157(16) 0.0020(16) 0.0008(15) Li1 0.043(3) 0.028(3) 0.017(3) -0.002(2) -0.001(2) 0.004(3) Li2 0.034(3) 0.025(3) 0.029(3) 0.005(3) -0.001(3) 0.001(2) N1 0.0253(14) 0.0247(15) 0.0164(13) -0.0022(11) 0.0019(11) -0.0002(12) N2 0.0230(13) 0.0238(15) 0.0138(13) -0.0021(11) 0.0000(11) 0.0029(12) N3 0.0185(13) 0.0246(15) 0.0129(12) -0.0017(12) -0.0019(10) -0.0012(11) N4 0.0208(13) 0.0193(14) 0.0141(13) -0.0015(11) -0.0022(11) -0.0001(11) O1 0.0295(12) 0.0319(14) 0.0247(12) 0.0098(10) 0.0034(10) -0.0015(11) O2 0.0341(13) 0.0322(14) 0.0231(12) 0.0101(10) 0.0015(10) 0.0011(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.325(4) . ? C1 C2 1.422(4) . ? C1 C7 1.504(4) . ? C2 C3 1.366(5) . ? C3 C4 1.394(5) . ? C4 C5 1.378(5) . ? C5 C6 1.378(5) . ? C6 C7 1.423(4) . ? C7 N2 1.331(4) . ? C8 N2 1.462(4) . ? C8 C23 1.516(4) . ? C8 C9 1.554(4) . ? C9 N3 1.465(4) . ? C9 C29 1.528(4) . ? C10 N3 1.321(4) . ? C10 C11 1.415(4) . ? C10 C16 1.513(4) . ? C11 C12 1.374(4) . ? C12 C13 1.391(4) . ? C13 C14 1.390(5) . ? C14 C15 1.374(4) . ? C15 C16 1.432(4) . ? C16 N4 1.311(4) . ? C17 N4 1.469(4) . ? C17 C18 1.519(4) . ? C17 C19 1.520(4) . ? C20 N1 1.479(4) . ? C20 C21 1.525(5) . ? C20 C22 1.526(5) . ? C23 C28 1.377(4) . ? C23 C24 1.403(4) . ? C24 C25 1.391(5) . ? C25 C26 1.364(6) . ? C26 C27 1.376(5) . ? C27 C28 1.387(5) . ? C29 C30 1.385(5) . ? C29 C34 1.386(4) . ? C30 C31 1.385(5) . ? C31 C32 1.385(5) . ? C32 C33 1.370(5) . ? C33 C34 1.401(5) . ? C35 O1 1.435(4) . ? C35 C36 1.508(6) . ? C36 C37 1.522(5) . ? C37 C38 1.492(5) . ? C38 O1 1.438(4) . ? C39 O2 1.449(4) . ? C39 C40 1.516(6) . ? C40 C41 1.485(6) . ? C41 C42 1.513(5) . ? C42 O2 1.441(4) . ? Li1 O1 1.937(6) . ? Li1 N2 1.951(6) . ? Li1 N1 1.976(6) . ? Li1 N3 2.510(6) . ? Li2 O2 1.919(6) . ? Li2 N3 1.932(6) . ? Li2 N4 1.992(6) . ? Li2 N2 2.456(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 N1 C1 C2 124.2(3) . . ? N1 C1 C7 113.4(3) . . ? C2 C1 C7 122.3(3) . . ? C3 C2 C1 133.9(3) . . ? C2 C3 C4 130.9(3) . . ? C5 C4 C3 124.3(3) . . ? C6 C5 C4 130.9(3) . . ? C5 C6 C7 132.8(3) . . ? N2 C7 C6 122.6(3) . . ? N2 C7 C1 112.9(3) . . ? C6 C7 C1 124.5(3) . . ? N2 C8 C23 113.9(2) . . ? N2 C8 C9 107.2(2) . . ? C23 C8 C9 109.3(2) . . ? N3 C9 C29 114.7(2) . . ? N3 C9 C8 106.8(2) . . ? C29 C9 C8 109.6(2) . . ? N3 C10 C11 123.4(3) . . ? N3 C10 C16 112.0(3) . . ? C11 C10 C16 124.5(3) . . ? C12 C11 C10 133.3(3) . . ? C11 C12 C13 130.5(3) . . ? C14 C13 C12 124.6(3) . . ? C15 C14 C13 131.5(3) . . ? C14 C15 C16 132.7(3) . . ? N4 C16 C15 123.4(3) . . ? N4 C16 C10 113.7(3) . . ? C15 C16 C10 122.9(3) . . ? N4 C17 C18 112.4(3) . . ? N4 C17 C19 108.4(2) . . ? C18 C17 C19 109.1(3) . . ? N1 C20 C21 111.4(3) . . ? N1 C20 C22 107.7(3) . . ? C21 C20 C22 109.6(3) . . ? C28 C23 C24 118.1(3) . . ? C28 C23 C8 120.7(3) . . ? C24 C23 C8 121.1(3) . . ? C25 C24 C23 119.5(3) . . ? C26 C25 C24 121.5(4) . . ? C25 C26 C27 119.4(4) . . ? C26 C27 C28 119.9(3) . . ? C23 C28 C27 121.6(3) . . ? C30 C29 C34 119.3(3) . . ? C30 C29 C9 120.0(3) . . ? C34 C29 C9 120.7(3) . . ? C31 C30 C29 120.9(3) . . ? C30 C31 C32 119.6(3) . . ? C33 C32 C31 120.1(3) . . ? C32 C33 C34 120.4(3) . . ? C29 C34 C33 119.6(3) . . ? O1 C35 C36 105.8(3) . . ? C35 C36 C37 104.9(3) . . ? C38 C37 C36 103.8(3) . . ? O1 C38 C37 104.2(3) . . ? O2 C39 C40 104.8(3) . . ? C41 C40 C39 103.8(3) . . ? C40 C41 C42 101.7(3) . . ? O2 C42 C41 105.9(3) . . ? O1 Li1 N2 132.9(3) . . ? O1 Li1 N1 123.6(3) . . ? N2 Li1 N1 80.9(2) . . ? O1 Li1 N3 105.0(3) . . ? N2 Li1 N3 69.75(19) . . ? N1 Li1 N3 131.0(3) . . ? O2 Li2 N3 134.5(3) . . ? O2 Li2 N4 121.4(3) . . ? N3 Li2 N4 80.5(2) . . ? O2 Li2 N2 111.4(3) . . ? N3 Li2 N2 71.3(2) . . ? N4 Li2 N2 125.6(3) . . ? C1 N1 C20 119.7(3) . . ? C1 N1 Li1 115.9(3) . . ? C20 N1 Li1 124.4(3) . . ? C7 N2 C8 120.1(3) . . ? C7 N2 Li1 116.8(3) . . ? C8 N2 Li1 122.9(3) . . ? C7 N2 Li2 99.6(2) . . ? C8 N2 Li2 94.2(2) . . ? Li1 N2 Li2 72.5(2) . . ? C10 N3 C9 119.9(3) . . ? C10 N3 Li2 118.2(3) . . ? C9 N3 Li2 121.5(3) . . ? C10 N3 Li1 97.2(2) . . ? C9 N3 Li1 94.7(2) . . ? Li2 N3 Li1 71.5(2) . . ? C16 N4 C17 119.8(2) . . ? C16 N4 Li2 115.5(3) . . ? C17 N4 Li2 124.5(3) . . ? C35 O1 C38 105.6(2) . . ? C35 O1 Li1 120.8(3) . . ? C38 O1 Li1 132.8(3) . . ? C42 O2 C39 109.3(3) . . ? C42 O2 Li2 126.5(3) . . ? C39 O2 Li2 119.2(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.375 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.051 #============================================================================== data_3a _database_code_depnum_ccdc_archive 'CCDC 638156' _audit_creation_date 05-02-24 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H44 Cl Ho N4 O, C4 H8 O' _chemical_formula_sum 'C42 H52 Cl Ho N4 O2' _chemical_formula_weight 845.26 _chemical_absolute_configuration rmad 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.8136(11) _cell_length_b 14.005(2) _cell_length_c 34.259(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4228.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow-red _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.106 _exptl_crystal_size_min 0.036 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.971 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7307 _exptl_absorpt_correction_T_max 0.9040 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13541 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.1217 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 26.71 _reflns_number_total 8667 _reflns_number_gt 6075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(18) _refine_ls_number_reflns 8667 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _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 1.0635(13) 0.2012(6) 0.4471(2) 0.0353(19) Uani 1 1 d . . . C2 C 1.1530(12) 0.2242(6) 0.4801(3) 0.037(2) Uani 1 1 d . . . H2 H 1.2197 0.2749 0.4747 0.044 Uiso 1 1 calc R . . C3 C 1.1687(12) 0.1932(9) 0.5171(3) 0.049(2) Uani 1 1 d . . . H3 H 1.2429 0.2243 0.5322 0.059 Uiso 1 1 calc R . . C4 C 1.0875(16) 0.1202(8) 0.5359(3) 0.056(3) Uani 1 1 d . . . H4 H 1.1077 0.1102 0.5625 0.067 Uiso 1 1 calc R . . C5 C 0.9799(12) 0.0614(8) 0.5184(3) 0.047(3) Uani 1 1 d . . . H5 H 0.9314 0.0178 0.5352 0.057 Uiso 1 1 calc R . . C6 C 0.9343(15) 0.0584(6) 0.4795(2) 0.039(2) Uani 1 1 d . . . H6 H 0.8609 0.0111 0.4747 0.047 Uiso 1 1 calc R . . C7 C 0.9738(10) 0.1106(6) 0.4455(3) 0.032(2) Uani 1 1 d . . . C8 C 0.8397(11) -0.0036(6) 0.4068(3) 0.030(2) Uani 1 1 d . . . H8 H 0.8886 -0.0514 0.4239 0.036 Uiso 1 1 calc R . . C9 C 0.8511(11) -0.0415(6) 0.3639(3) 0.030(2) Uani 1 1 d . . . H9 H 0.7581 -0.0791 0.3589 0.036 Uiso 1 1 calc R . . C10 C 0.8032(11) 0.0215(6) 0.2999(3) 0.031(2) Uani 1 1 d . . . C11 C 0.7395(12) -0.0655(7) 0.2887(3) 0.043(2) Uani 1 1 d . . . H11 H 0.7460 -0.1126 0.3081 0.051 Uiso 1 1 calc R . . C12 C 0.6673(13) -0.0978(7) 0.2543(3) 0.044(3) Uani 1 1 d . . . H12 H 0.6211 -0.1581 0.2564 0.052 Uiso 1 1 calc R . . C13 C 0.6536(12) -0.0557(8) 0.2186(3) 0.046(3) Uani 1 1 d . . . H13 H 0.6013 -0.0892 0.1990 0.055 Uiso 1 1 calc R . . C14 C 0.7104(16) 0.0305(8) 0.2097(3) 0.055(3) Uani 1 1 d . . . H14 H 0.6976 0.0484 0.1834 0.066 Uiso 1 1 calc R . . C15 C 0.7848(13) 0.0978(7) 0.2325(3) 0.042(2) Uani 1 1 d . . . H15 H 0.8221 0.1496 0.2180 0.051 Uiso 1 1 calc R . . C16 C 0.8168(12) 0.1055(7) 0.2730(3) 0.033(2) Uani 1 1 d . . . C17 C 0.8717(12) 0.2739(6) 0.2652(3) 0.037(2) Uani 1 1 d . . . H17 H 0.9226 0.2599 0.2401 0.044 Uiso 1 1 calc R . . C18 C 0.9626(14) 0.3478(6) 0.2866(3) 0.046(3) Uani 1 1 d . . . H18A H 0.9088 0.3668 0.3100 0.070 Uiso 1 1 calc R . . H18B H 0.9772 0.4030 0.2699 0.070 Uiso 1 1 calc R . . H18C H 1.0605 0.3213 0.2937 0.070 Uiso 1 1 calc R . . C19 C 0.7142(12) 0.3120(9) 0.2568(3) 0.051(2) Uani 1 1 d . . . H19A H 0.6555 0.2637 0.2433 0.077 Uiso 1 1 calc R . . H19B H 0.7218 0.3686 0.2406 0.077 Uiso 1 1 calc R . . H19C H 0.6645 0.3282 0.2812 0.077 Uiso 1 1 calc R . . C20 C 1.1284(14) 0.3465(7) 0.4166(3) 0.046(3) Uani 1 1 d . . . H20 H 1.2336 0.3396 0.4264 0.055 Uiso 1 1 calc R . . C21 C 1.1329(18) 0.3894(9) 0.3751(4) 0.071(4) Uani 1 1 d . . . H21A H 1.1883 0.3469 0.3579 0.106 Uiso 1 1 calc R . . H21B H 1.1831 0.4510 0.3759 0.106 Uiso 1 1 calc R . . H21C H 1.0301 0.3973 0.3655 0.106 Uiso 1 1 calc R . . C22 C 1.044(2) 0.4144(8) 0.4429(3) 0.065(4) Uani 1 1 d . . . H22A H 0.9370 0.4147 0.4358 0.097 Uiso 1 1 calc R . . H22B H 1.0849 0.4782 0.4400 0.097 Uiso 1 1 calc R . . H22C H 1.0540 0.3939 0.4698 0.097 Uiso 1 1 calc R . . C23 C 0.6743(11) 0.0047(6) 0.4193(3) 0.033(2) Uani 1 1 d . . . C24 C 0.6077(12) 0.0912(7) 0.4300(3) 0.039(2) Uani 1 1 d . . . H24 H 0.6637 0.1480 0.4275 0.046 Uiso 1 1 calc R . . C25 C 0.4640(13) 0.0950(7) 0.4438(3) 0.043(3) Uani 1 1 d . . . H25 H 0.4234 0.1539 0.4518 0.051 Uiso 1 1 calc R . . C26 C 0.3767(14) 0.0144(9) 0.4463(4) 0.059(3) Uani 1 1 d . . . H26 H 0.2777 0.0181 0.4564 0.070 Uiso 1 1 calc R . . C27 C 0.4325(17) -0.0705(8) 0.4343(3) 0.061(3) Uani 1 1 d . . . H27 H 0.3704 -0.1250 0.4339 0.074 Uiso 1 1 calc R . . C28 C 0.5852(14) -0.0761(7) 0.4223(4) 0.054(3) Uani 1 1 d . . . H28 H 0.6273 -0.1360 0.4163 0.065 Uiso 1 1 calc R . . C29 C 0.9836(10) -0.1090(6) 0.3601(3) 0.035(2) Uani 1 1 d . . . C30 C 0.9644(16) -0.2036(7) 0.3655(6) 0.096(6) Uani 1 1 d . . . H30 H 0.8672 -0.2276 0.3710 0.115 Uiso 1 1 calc R . . C31 C 1.087(2) -0.2663(9) 0.3631(7) 0.108(6) Uani 1 1 d . . . H31 H 1.0697 -0.3320 0.3663 0.130 Uiso 1 1 calc R . . C32 C 1.2296(15) -0.2360(9) 0.3563(6) 0.068(4) Uani 1 1 d . . . H32 H 1.3125 -0.2782 0.3566 0.081 Uiso 1 1 calc R . . C33 C 1.2478(18) -0.1421(10) 0.3489(5) 0.081(5) Uani 1 1 d . . . H33 H 1.3445 -0.1188 0.3424 0.097 Uiso 1 1 calc R . . C34 C 1.1282(15) -0.0801(9) 0.3509(6) 0.088(6) Uani 1 1 d . . . H34 H 1.1456 -0.0151 0.3458 0.105 Uiso 1 1 calc R . . C35 C 1.2246(14) 0.1325(10) 0.2913(3) 0.056(3) Uani 1 1 d . . . H35A H 1.1627 0.0767 0.2845 0.068 Uiso 1 1 calc R . . H35B H 1.2049 0.1830 0.2721 0.068 Uiso 1 1 calc R . . C36 C 1.3848(16) 0.1074(14) 0.2914(4) 0.090(5) Uani 1 1 d . . . H36A H 1.4431 0.1547 0.2766 0.107 Uiso 1 1 calc R . . H36B H 1.3996 0.0447 0.2793 0.107 Uiso 1 1 calc R . . C37 C 1.4376(17) 0.1051(9) 0.3329(3) 0.064(3) Uani 1 1 d . . . H37A H 1.4397 0.0396 0.3429 0.077 Uiso 1 1 calc R . . H37B H 1.5391 0.1331 0.3354 0.077 Uiso 1 1 calc R . . C38 C 1.3240(13) 0.1628(13) 0.3534(4) 0.093(5) Uani 1 1 d . . . H38A H 1.3034 0.1348 0.3791 0.111 Uiso 1 1 calc R . . H38B H 1.3628 0.2276 0.3573 0.111 Uiso 1 1 calc R . . C39 C 1.342(2) 0.1591(12) 0.1808(6) 0.109(6) Uiso 1 1 d . . . H39A H 1.2708 0.2042 0.1927 0.130 Uiso 1 1 calc R . . H39B H 1.4253 0.1485 0.1992 0.130 Uiso 1 1 calc R . . C40 C 1.264(3) 0.0689(14) 0.1737(6) 0.117(6) Uiso 1 1 d . . . H40A H 1.3168 0.0163 0.1868 0.141 Uiso 1 1 calc R . . H40B H 1.1595 0.0716 0.1832 0.141 Uiso 1 1 calc R . . C41 C 1.268(3) 0.0566(14) 0.1337(6) 0.125(7) Uiso 1 1 d . . . H41A H 1.1750 0.0817 0.1216 0.151 Uiso 1 1 calc R . . H41B H 1.2780 -0.0111 0.1269 0.151 Uiso 1 1 calc R . . C42 C 1.403(4) 0.1119(19) 0.1207(9) 0.190(12) Uiso 1 1 d . . . H42A H 1.3951 0.1305 0.0932 0.228 Uiso 1 1 calc R . . H42B H 1.4970 0.0752 0.1245 0.228 Uiso 1 1 calc R . . N1 N 1.0577(12) 0.2519(5) 0.4147(2) 0.0397(18) Uani 1 1 d . . . N2 N 0.9262(10) 0.0853(5) 0.4103(2) 0.0326(16) Uani 1 1 d . . . N3 N 0.8519(9) 0.0378(5) 0.3359(2) 0.0321(18) Uani 1 1 d . . . N4 N 0.8673(8) 0.1840(6) 0.28923(19) 0.0322(15) Uani 1 1 d . . . O1 O 1.1873(7) 0.1661(4) 0.33114(18) 0.0369(15) Uani 1 1 d . . . O2 O 1.3984(14) 0.1977(9) 0.1471(4) 0.122(4) Uiso 1 1 d . . . Cl Cl 0.7041(3) 0.29678(16) 0.36799(7) 0.0462(6) Uani 1 1 d . . . Ho Ho 0.93613(5) 0.18812(3) 0.357117(12) 0.03066(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(4) 0.038(5) 0.037(4) -0.019(4) 0.003(5) 0.005(6) C2 0.034(6) 0.038(5) 0.039(6) -0.019(4) -0.001(5) 0.002(4) C3 0.037(6) 0.053(6) 0.056(6) -0.023(6) -0.010(5) 0.004(6) C4 0.074(10) 0.068(6) 0.025(5) -0.012(5) -0.011(6) -0.001(7) C5 0.041(7) 0.058(6) 0.044(6) 0.002(5) 0.007(5) 0.002(5) C6 0.040(5) 0.053(5) 0.024(4) 0.006(4) 0.002(5) -0.001(6) C7 0.028(6) 0.038(4) 0.029(5) -0.005(4) 0.003(4) 0.002(4) C8 0.030(5) 0.033(4) 0.028(5) -0.004(4) -0.004(4) 0.003(4) C9 0.030(5) 0.031(4) 0.030(6) -0.006(4) 0.004(4) 0.006(4) C10 0.024(5) 0.032(5) 0.038(5) -0.007(4) -0.001(4) 0.010(4) C11 0.044(7) 0.042(5) 0.042(6) -0.002(4) -0.002(5) -0.008(5) C12 0.049(7) 0.044(5) 0.038(6) -0.014(4) -0.002(5) -0.007(5) C13 0.034(6) 0.055(6) 0.049(7) -0.014(5) -0.012(5) 0.002(5) C14 0.063(8) 0.064(7) 0.037(6) 0.000(5) -0.018(6) 0.007(6) C15 0.045(7) 0.051(6) 0.032(5) -0.004(4) 0.009(5) 0.005(5) C16 0.029(5) 0.047(5) 0.023(5) 0.003(4) 0.002(4) 0.002(4) C17 0.038(6) 0.031(4) 0.041(6) 0.004(4) -0.001(5) 0.006(4) C18 0.052(8) 0.044(5) 0.043(6) 0.010(4) 0.004(5) 0.001(5) C19 0.052(6) 0.045(5) 0.057(6) 0.010(6) -0.013(5) 0.004(6) C20 0.045(6) 0.051(6) 0.041(6) -0.006(5) 0.011(5) -0.016(5) C21 0.094(11) 0.068(7) 0.051(7) -0.002(6) 0.003(7) -0.038(7) C22 0.094(12) 0.058(7) 0.043(6) -0.011(5) 0.004(8) 0.008(8) C23 0.029(5) 0.032(4) 0.036(5) -0.006(4) -0.007(4) -0.005(4) C24 0.038(7) 0.043(5) 0.035(5) -0.001(4) -0.003(5) -0.001(4) C25 0.033(7) 0.049(6) 0.046(6) -0.001(4) 0.006(5) 0.000(5) C26 0.028(6) 0.081(8) 0.066(8) 0.004(7) 0.006(6) 0.004(6) C27 0.045(7) 0.061(6) 0.077(8) -0.001(6) 0.027(8) -0.019(7) C28 0.042(8) 0.040(5) 0.080(8) 0.003(5) 0.018(7) -0.003(5) C29 0.033(5) 0.041(5) 0.031(5) -0.002(5) 0.004(5) -0.002(4) C30 0.056(9) 0.039(6) 0.193(18) 0.006(8) 0.028(10) 0.012(6) C31 0.087(13) 0.041(6) 0.20(2) 0.007(9) 0.020(16) 0.017(7) C32 0.048(8) 0.068(8) 0.087(9) -0.025(9) -0.010(9) 0.022(6) C33 0.064(10) 0.084(9) 0.094(13) 0.022(8) 0.029(9) 0.022(7) C34 0.052(8) 0.051(6) 0.160(17) 0.041(9) 0.035(10) 0.026(6) C35 0.049(8) 0.093(8) 0.027(6) 0.003(6) 0.004(5) 0.015(7) C36 0.052(9) 0.177(16) 0.040(7) -0.002(9) 0.009(6) 0.047(9) C37 0.037(6) 0.089(8) 0.067(8) -0.012(6) 0.016(8) 0.001(8) C38 0.037(6) 0.186(16) 0.054(8) -0.033(11) -0.020(7) 0.021(8) N1 0.036(5) 0.049(4) 0.034(4) -0.008(3) 0.009(5) -0.015(5) N2 0.024(4) 0.036(3) 0.037(4) -0.008(3) -0.007(4) 0.002(4) N3 0.037(5) 0.031(4) 0.028(4) -0.004(3) -0.012(4) -0.005(3) N4 0.034(4) 0.039(4) 0.024(3) -0.005(4) 0.002(3) 0.001(4) O1 0.022(3) 0.050(4) 0.038(4) -0.010(3) 0.003(3) 0.002(3) Cl 0.0481(14) 0.0421(13) 0.0483(15) -0.0036(10) 0.0119(11) 0.0082(11) Ho 0.02968(18) 0.03444(16) 0.02785(16) -0.0040(2) 0.0026(2) -0.0029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.320(11) . ? C1 C2 1.416(14) . ? C1 C7 1.496(13) . ? C2 C3 1.347(15) . ? C3 C4 1.404(16) . ? C4 C5 1.392(16) . ? C5 C6 1.393(14) . ? C6 C7 1.419(12) . ? C7 N2 1.326(11) . ? C8 N2 1.464(11) . ? C8 C23 1.525(14) . ? C8 C9 1.564(12) . ? C9 N3 1.469(11) . ? C9 C29 1.508(12) . ? C10 N3 1.325(12) . ? C10 C11 1.394(13) . ? C10 C16 1.498(13) . ? C11 C12 1.414(14) . ? C12 C13 1.363(15) . ? C13 C14 1.341(16) . ? C14 C15 1.390(15) . ? C15 C16 1.420(13) . ? C16 N4 1.310(12) . ? C17 C18 1.499(14) . ? C17 N4 1.505(12) . ? C17 C19 1.514(14) . ? C20 N1 1.465(12) . ? C20 C22 1.508(16) . ? C20 C21 1.544(15) . ? C23 C28 1.381(14) . ? C23 C24 1.396(13) . ? C24 C25 1.353(15) . ? C25 C26 1.369(15) . ? C26 C27 1.350(16) . ? C27 C28 1.409(19) . ? C29 C30 1.349(13) . ? C29 C34 1.373(15) . ? C30 C31 1.396(18) . ? C31 C32 1.35(2) . ? C32 C33 1.349(17) . ? C33 C34 1.367(17) . ? C35 C36 1.456(17) . ? C35 O1 1.481(12) . ? C36 C37 1.496(18) . ? C37 C38 1.467(18) . ? C38 O1 1.427(13) . ? C39 O2 1.37(2) . ? C39 C40 1.46(2) . ? C40 C41 1.38(3) . ? C41 C42 1.49(3) . ? C42 O2 1.50(3) . ? N1 Ho 2.415(8) . ? N2 Ho 2.324(7) . ? N3 Ho 2.348(7) . ? N4 Ho 2.404(7) . ? O1 Ho 2.406(6) . ? Cl Ho 2.576(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 124.8(9) . . ? N1 C1 C7 114.0(8) . . ? C2 C1 C7 121.1(8) . . ? C3 C2 C1 137.4(10) . . ? C2 C3 C4 127.8(10) . . ? C5 C4 C3 125.6(10) . . ? C4 C5 C6 128.7(11) . . ? C5 C6 C7 134.4(11) . . ? N2 C7 C6 122.2(8) . . ? N2 C7 C1 115.3(8) . . ? C6 C7 C1 122.4(8) . . ? N2 C8 C23 114.2(7) . . ? N2 C8 C9 109.4(7) . . ? C23 C8 C9 110.6(7) . . ? N3 C9 C29 114.4(8) . . ? N3 C9 C8 111.0(7) . . ? C29 C9 C8 110.2(8) . . ? N3 C10 C11 122.5(9) . . ? N3 C10 C16 114.2(8) . . ? C11 C10 C16 123.3(9) . . ? C10 C11 C12 133.7(10) . . ? C13 C12 C11 130.5(10) . . ? C14 C13 C12 124.1(10) . . ? C13 C14 C15 131.1(11) . . ? C14 C15 C16 134.1(10) . . ? N4 C16 C15 123.0(9) . . ? N4 C16 C10 115.3(8) . . ? C15 C16 C10 121.6(9) . . ? C18 C17 N4 108.9(8) . . ? C18 C17 C19 109.8(8) . . ? N4 C17 C19 112.0(8) . . ? N1 C20 C22 112.7(10) . . ? N1 C20 C21 108.7(9) . . ? C22 C20 C21 108.5(10) . . ? C28 C23 C24 117.0(10) . . ? C28 C23 C8 120.1(9) . . ? C24 C23 C8 122.8(8) . . ? C25 C24 C23 121.3(10) . . ? C24 C25 C26 121.1(11) . . ? C27 C26 C25 120.1(11) . . ? C26 C27 C28 119.1(11) . . ? C23 C28 C27 121.2(10) . . ? C30 C29 C34 116.0(10) . . ? C30 C29 C9 120.4(9) . . ? C34 C29 C9 123.6(8) . . ? C29 C30 C31 120.8(12) . . ? C32 C31 C30 122.4(12) . . ? C31 C32 C33 116.8(13) . . ? C32 C33 C34 121.2(15) . . ? C33 C34 C29 122.6(11) . . ? C36 C35 O1 106.8(10) . . ? C35 C36 C37 108.1(10) . . ? C38 C37 C36 103.4(12) . . ? O1 C38 C37 109.7(11) . . ? O2 C39 C40 111.9(16) . . ? C41 C40 C39 105.3(19) . . ? C40 C41 C42 104(2) . . ? C41 C42 O2 102(2) . . ? C1 N1 C20 115.6(8) . . ? C1 N1 Ho 120.3(6) . . ? C20 N1 Ho 124.1(6) . . ? C7 N2 C8 117.8(7) . . ? C7 N2 Ho 122.4(6) . . ? C8 N2 Ho 118.8(5) . . ? C10 N3 C9 118.5(7) . . ? C10 N3 Ho 123.1(6) . . ? C9 N3 Ho 118.5(5) . . ? C16 N4 C17 118.7(7) . . ? C16 N4 Ho 121.0(6) . . ? C17 N4 Ho 120.2(6) . . ? C38 O1 C35 107.2(8) . . ? C38 O1 Ho 125.6(7) . . ? C35 O1 Ho 125.8(6) . . ? C39 O2 C42 101.7(16) . . ? N2 Ho N3 71.1(2) . . ? N2 Ho N4 137.2(3) . . ? N3 Ho N4 66.4(3) . . ? N2 Ho O1 104.2(3) . . ? N3 Ho O1 93.5(3) . . ? N4 Ho O1 82.6(2) . . ? N2 Ho N1 66.8(2) . . ? N3 Ho N1 136.5(2) . . ? N4 Ho N1 155.6(3) . . ? O1 Ho N1 86.6(3) . . ? N2 Ho Cl 102.9(2) . . ? N3 Ho Cl 108.9(2) . . ? N4 Ho Cl 87.34(19) . . ? O1 Ho Cl 149.29(16) . . ? N1 Ho Cl 90.9(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 171.1(12) . . . . ? C7 C1 C2 C3 -13.3(18) . . . . ? C1 C2 C3 C4 -1(2) . . . . ? C2 C3 C4 C5 4(2) . . . . ? C3 C4 C5 C6 3(2) . . . . ? C4 C5 C6 C7 -1(2) . . . . ? C5 C6 C7 N2 171.4(11) . . . . ? C5 C6 C7 C1 -12.6(18) . . . . ? N1 C1 C7 N2 12.2(13) . . . . ? C2 C1 C7 N2 -163.8(9) . . . . ? N1 C1 C7 C6 -164.1(10) . . . . ? C2 C1 C7 C6 19.9(14) . . . . ? N2 C8 C9 N3 -36.3(10) . . . . ? C23 C8 C9 N3 90.3(9) . . . . ? N2 C8 C9 C29 91.5(9) . . . . ? C23 C8 C9 C29 -141.9(8) . . . . ? N3 C10 C11 C12 172.9(11) . . . . ? C16 C10 C11 C12 -4.5(19) . . . . ? C10 C11 C12 C13 9(2) . . . . ? C11 C12 C13 C14 -1(2) . . . . ? C12 C13 C14 C15 -4(2) . . . . ? C13 C14 C15 C16 -6(2) . . . . ? C14 C15 C16 N4 -168.1(12) . . . . ? C14 C15 C16 C10 15.5(19) . . . . ? N3 C10 C16 N4 -3.3(13) . . . . ? C11 C10 C16 N4 174.3(9) . . . . ? N3 C10 C16 C15 173.4(9) . . . . ? C11 C10 C16 C15 -9.0(15) . . . . ? N2 C8 C23 C28 -171.6(9) . . . . ? C9 C8 C23 C28 64.5(12) . . . . ? N2 C8 C23 C24 5.3(13) . . . . ? C9 C8 C23 C24 -118.6(10) . . . . ? C28 C23 C24 C25 2.0(15) . . . . ? C8 C23 C24 C25 -174.9(9) . . . . ? C23 C24 C25 C26 -2.7(17) . . . . ? C24 C25 C26 C27 -1.1(19) . . . . ? C25 C26 C27 C28 5(2) . . . . ? C24 C23 C28 C27 2.2(17) . . . . ? C8 C23 C28 C27 179.2(10) . . . . ? C26 C27 C28 C23 -5.9(19) . . . . ? N3 C9 C29 C30 -142.7(13) . . . . ? C8 C9 C29 C30 91.5(14) . . . . ? N3 C9 C29 C34 37.1(17) . . . . ? C8 C9 C29 C34 -88.7(16) . . . . ? C34 C29 C30 C31 2(3) . . . . ? C9 C29 C30 C31 -178.2(15) . . . . ? C29 C30 C31 C32 2(3) . . . . ? C30 C31 C32 C33 -5(3) . . . . ? C31 C32 C33 C34 4(3) . . . . ? C32 C33 C34 C29 0(3) . . . . ? C30 C29 C34 C33 -3(3) . . . . ? C9 C29 C34 C33 177.5(15) . . . . ? O1 C35 C36 C37 12.2(17) . . . . ? C35 C36 C37 C38 -20.5(18) . . . . ? C36 C37 C38 O1 21.8(17) . . . . ? O2 C39 C40 C41 -4(3) . . . . ? C39 C40 C41 C42 26(3) . . . . ? C40 C41 C42 O2 -38(3) . . . . ? C2 C1 N1 C20 -11.4(15) . . . . ? C7 C1 N1 C20 172.8(8) . . . . ? C2 C1 N1 Ho 168.8(7) . . . . ? C7 C1 N1 Ho -7.1(12) . . . . ? C22 C20 N1 C1 -68.1(14) . . . . ? C21 C20 N1 C1 171.6(11) . . . . ? C22 C20 N1 Ho 111.8(10) . . . . ? C21 C20 N1 Ho -8.5(13) . . . . ? C6 C7 N2 C8 -4.6(14) . . . . ? C1 C7 N2 C8 179.1(8) . . . . ? C6 C7 N2 Ho 164.0(7) . . . . ? C1 C7 N2 Ho -12.3(11) . . . . ? C23 C8 N2 C7 78.2(11) . . . . ? C9 C8 N2 C7 -157.3(8) . . . . ? C23 C8 N2 Ho -90.9(8) . . . . ? C9 C8 N2 Ho 33.7(9) . . . . ? C11 C10 N3 C9 5.6(14) . . . . ? C16 C10 N3 C9 -176.8(8) . . . . ? C11 C10 N3 Ho -173.5(7) . . . . ? C16 C10 N3 Ho 4.1(11) . . . . ? C29 C9 N3 C10 80.2(11) . . . . ? C8 C9 N3 C10 -154.4(8) . . . . ? C29 C9 N3 Ho -100.6(8) . . . . ? C8 C9 N3 Ho 24.8(9) . . . . ? C15 C16 N4 C17 8.5(14) . . . . ? C10 C16 N4 C17 -174.8(8) . . . . ? C15 C16 N4 Ho -175.5(7) . . . . ? C10 C16 N4 Ho 1.1(11) . . . . ? C18 C17 N4 C16 -168.1(9) . . . . ? C19 C17 N4 C16 70.2(11) . . . . ? C18 C17 N4 Ho 15.9(10) . . . . ? C19 C17 N4 Ho -105.8(8) . . . . ? C37 C38 O1 C35 -15.0(16) . . . . ? C37 C38 O1 Ho 152.7(8) . . . . ? C36 C35 O1 C38 1.5(15) . . . . ? C36 C35 O1 Ho -166.2(10) . . . . ? C40 C39 O2 C42 -20(2) . . . . ? C41 C42 O2 C39 34(2) . . . . ? C7 N2 Ho N3 175.3(8) . . . . ? C8 N2 Ho N3 -16.2(6) . . . . ? C7 N2 Ho N4 -179.1(6) . . . . ? C8 N2 Ho N4 -10.6(9) . . . . ? C7 N2 Ho O1 86.4(8) . . . . ? C8 N2 Ho O1 -105.1(7) . . . . ? C7 N2 Ho N1 6.4(7) . . . . ? C8 N2 Ho N1 174.9(7) . . . . ? C7 N2 Ho Cl -78.9(8) . . . . ? C8 N2 Ho Cl 89.6(6) . . . . ? C10 N3 Ho N2 173.2(8) . . . . ? C9 N3 Ho N2 -5.9(6) . . . . ? C10 N3 Ho N4 -2.6(7) . . . . ? C9 N3 Ho N4 178.2(7) . . . . ? C10 N3 Ho O1 -83.0(8) . . . . ? C9 N3 Ho O1 97.9(6) . . . . ? C10 N3 Ho N1 -171.8(7) . . . . ? C9 N3 Ho N1 9.1(9) . . . . ? C10 N3 Ho Cl 75.6(8) . . . . ? C9 N3 Ho Cl -103.5(6) . . . . ? C16 N4 Ho N2 -5.2(9) . . . . ? C17 N4 Ho N2 170.7(6) . . . . ? C16 N4 Ho N3 0.6(7) . . . . ? C17 N4 Ho N3 176.5(7) . . . . ? C16 N4 Ho O1 97.7(7) . . . . ? C17 N4 Ho O1 -86.4(6) . . . . ? C16 N4 Ho N1 162.3(8) . . . . ? C17 N4 Ho N1 -21.8(11) . . . . ? C16 N4 Ho Cl -111.4(7) . . . . ? C17 N4 Ho Cl 64.5(6) . . . . ? C38 O1 Ho N2 -45.7(11) . . . . ? C35 O1 Ho N2 119.8(8) . . . . ? C38 O1 Ho N3 -117.0(11) . . . . ? C35 O1 Ho N3 48.5(8) . . . . ? C38 O1 Ho N4 177.4(11) . . . . ? C35 O1 Ho N4 -17.1(8) . . . . ? C38 O1 Ho N1 19.4(11) . . . . ? C35 O1 Ho N1 -175.1(8) . . . . ? C38 O1 Ho Cl 105.5(11) . . . . ? C35 O1 Ho Cl -89.1(8) . . . . ? C1 N1 Ho N2 1.1(8) . . . . ? C20 N1 Ho N2 -178.8(9) . . . . ? C1 N1 Ho N3 -14.4(11) . . . . ? C20 N1 Ho N3 165.7(7) . . . . ? C1 N1 Ho N4 -169.8(7) . . . . ? C20 N1 Ho N4 10.4(13) . . . . ? C1 N1 Ho O1 -105.9(9) . . . . ? C20 N1 Ho O1 74.2(8) . . . . ? C1 N1 Ho Cl 104.7(8) . . . . ? C20 N1 Ho Cl -75.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.892 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.133 #============================================================================== data_4a _database_code_depnum_ccdc_archive 'CCDC 638157' _audit_creation_date 05-03-02 _audit_creation_method 'STOE X-RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H44 Cl Er N4 O, 2(C7 H8)' _chemical_formula_sum 'C52 H60 Cl Er N4 O' _chemical_formula_weight 959.75 _chemical_absolute_configuration rmad 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.0455(2) _cell_length_b 19.2532(6) _cell_length_c 26.6334(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4638.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.234 _exptl_crystal_size_min 0.051 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 1.908 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5410 _exptl_absorpt_correction_T_max 0.9378 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73070 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10649 _reflns_number_gt 9601 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0558P)^2^+1.4277P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(11) _refine_ls_number_reflns 10649 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 -0.0047(5) -0.2485(2) -0.1441(2) 0.0360(10) Uani 1 1 d . . . C2 C -0.0974(6) -0.2989(3) -0.1188(2) 0.0446(12) Uani 1 1 d . . . H2 H -0.1539 -0.3264 -0.1413 0.054 Uiso 1 1 calc R . . C3 C -0.1210(7) -0.3152(3) -0.0697(2) 0.0503(12) Uani 1 1 d . . . H3 H -0.1960 -0.3488 -0.0642 0.060 Uiso 1 1 calc R . . C4 C -0.0543(6) -0.2910(3) -0.0269(3) 0.0525(15) Uani 1 1 d . . . H4 H -0.0816 -0.3117 0.0041 0.063 Uiso 1 1 calc R . . C5 C 0.0505(6) -0.2383(3) -0.0258(2) 0.0491(13) Uani 1 1 d . . . H5 H 0.0917 -0.2292 0.0064 0.059 Uiso 1 1 calc R . . C6 C 0.1040(6) -0.1971(3) -0.06431(19) 0.0397(11) Uani 1 1 d . . . H6 H 0.1742 -0.1638 -0.0532 0.048 Uiso 1 1 calc R . . C7 C 0.0771(5) -0.1936(2) -0.1168(2) 0.0343(10) Uani 1 1 d . . . C8 C 0.2180(5) -0.0893(2) -0.12176(18) 0.0326(10) Uani 1 1 d . . . H8 H 0.1664 -0.0773 -0.0897 0.039 Uiso 1 1 calc R . . C9 C 0.2197(5) -0.0230(2) -0.15471(19) 0.0330(10) Uani 1 1 d . . . H9 H 0.3144 0.0019 -0.1476 0.040 Uiso 1 1 calc R . . C10 C 0.2773(5) 0.0039(2) -0.24112(18) 0.0328(10) Uani 1 1 d . . . C11 C 0.3402(6) 0.0679(3) -0.2256(2) 0.0435(12) Uani 1 1 d . . . H11 H 0.3237 0.0776 -0.1911 0.052 Uiso 1 1 calc R . . C12 C 0.4200(6) 0.1193(3) -0.2495(2) 0.0486(14) Uani 1 1 d . . . H12 H 0.4586 0.1543 -0.2280 0.058 Uiso 1 1 calc R . . C13 C 0.4522(7) 0.1276(3) -0.2996(3) 0.0539(15) Uani 1 1 d . . . H13 H 0.5151 0.1650 -0.3089 0.065 Uiso 1 1 calc R . . C14 C 0.3989(8) 0.0852(3) -0.3373(2) 0.0574(16) Uani 1 1 d . . . H14 H 0.4220 0.0999 -0.3705 0.069 Uiso 1 1 calc R . . C15 C 0.3183(7) 0.0254(3) -0.3343(2) 0.0532(15) Uani 1 1 d . . . H15 H 0.2907 0.0084 -0.3664 0.064 Uiso 1 1 calc R . . C16 C 0.2655(5) -0.0175(3) -0.2946(2) 0.0363(11) Uani 1 1 d . . . C17 C 0.1908(7) -0.1023(3) -0.3553(2) 0.0497(14) Uani 1 1 d . . . H17 H 0.1508 -0.0649 -0.3775 0.060 Uiso 1 1 calc R . . C18 C 0.3508(11) -0.1247(4) -0.3732(3) 0.086(3) Uani 1 1 d . . . H18A H 0.4172 -0.0845 -0.3718 0.128 Uiso 1 1 calc R . . H18B H 0.3459 -0.1422 -0.4077 0.128 Uiso 1 1 calc R . . H18C H 0.3885 -0.1614 -0.3510 0.128 Uiso 1 1 calc R . . C19 C 0.0951(9) -0.1661(3) -0.3583(2) 0.065(2) Uani 1 1 d . . . H19A H 0.1362 -0.2025 -0.3366 0.098 Uiso 1 1 calc R . . H19B H 0.0920 -0.1828 -0.3931 0.098 Uiso 1 1 calc R . . H19C H -0.0053 -0.1547 -0.3472 0.098 Uiso 1 1 calc R . . C20 C -0.0497(7) -0.3047(3) -0.2233(2) 0.0523(15) Uani 1 1 d . . . H20 H -0.1543 -0.3137 -0.2131 0.063 Uiso 1 1 calc R . . C21 C -0.0452(9) -0.2862(4) -0.2782(3) 0.0664(19) Uani 1 1 d . . . H21A H -0.1055 -0.2447 -0.2841 0.100 Uiso 1 1 calc R . . H21B H -0.0841 -0.3250 -0.2980 0.100 Uiso 1 1 calc R . . H21C H 0.0572 -0.2769 -0.2882 0.100 Uiso 1 1 calc R . . C22 C 0.0417(9) -0.3705(3) -0.2156(3) 0.070(2) Uani 1 1 d . . . H22A H 0.1440 -0.3619 -0.2260 0.105 Uiso 1 1 calc R . . H22B H 0.0000 -0.4083 -0.2358 0.105 Uiso 1 1 calc R . . H22C H 0.0398 -0.3836 -0.1800 0.105 Uiso 1 1 calc R . . C23 C 0.3756(7) -0.1105(2) -0.10838(18) 0.0373(10) Uani 1 1 d . . . C24 C 0.4384(6) -0.1738(3) -0.1246(2) 0.0421(12) Uani 1 1 d . . . H24 H 0.3823 -0.2049 -0.1447 0.051 Uiso 1 1 calc R . . C25 C 0.5824(6) -0.1903(3) -0.1111(2) 0.0507(14) Uani 1 1 d . . . H25 H 0.6245 -0.2328 -0.1224 0.061 Uiso 1 1 calc R . . C26 C 0.6650(6) -0.1462(4) -0.0818(2) 0.0580(16) Uani 1 1 d . . . H26 H 0.7633 -0.1583 -0.0727 0.070 Uiso 1 1 calc R . . C27 C 0.6048(7) -0.0848(4) -0.0656(2) 0.0574(16) Uani 1 1 d . . . H27 H 0.6618 -0.0540 -0.0456 0.069 Uiso 1 1 calc R . . C28 C 0.4614(7) -0.0677(3) -0.0784(2) 0.0497(13) Uani 1 1 d . . . H28 H 0.4205 -0.0254 -0.0663 0.060 Uiso 1 1 calc R . . C29 C 0.0945(6) 0.0258(3) -0.14072(18) 0.0382(11) Uani 1 1 d . . . C30 C 0.1242(9) 0.0838(3) -0.1114(2) 0.0563(13) Uani 1 1 d . . . H30 H 0.2234 0.0936 -0.1021 0.068 Uiso 1 1 calc R . . C31 C 0.0116(9) 0.1277(4) -0.0955(3) 0.071(2) Uani 1 1 d . . . H31 H 0.0330 0.1650 -0.0733 0.085 Uiso 1 1 calc R . . C32 C -0.1294(10) 0.1173(4) -0.1118(3) 0.074(2) Uani 1 1 d . . . H32 H -0.2056 0.1491 -0.1031 0.089 Uiso 1 1 calc R . . C33 C -0.1602(8) 0.0600(5) -0.1410(4) 0.097(3) Uani 1 1 d . . . H33 H -0.2585 0.0518 -0.1521 0.116 Uiso 1 1 calc R . . C34 C -0.0481(7) 0.0141(5) -0.1544(3) 0.078(3) Uani 1 1 d . . . H34 H -0.0717 -0.0262 -0.1734 0.093 Uiso 1 1 calc R . . C35 C -0.2468(6) -0.1368(4) -0.2220(3) 0.069(2) Uani 1 1 d . B . H35A H -0.2242 -0.1435 -0.1860 0.083 Uiso 1 1 calc R . . H35B H -0.2814 -0.1815 -0.2362 0.083 Uiso 1 1 calc R . . C36 C -0.3618(8) -0.0819(4) -0.2286(4) 0.081(2) Uani 1 1 d . . . H36A H -0.4517 -0.1021 -0.2440 0.097 Uiso 1 1 calc R A 1 H36B H -0.3890 -0.0620 -0.1956 0.097 Uiso 1 1 calc R A 1 C37A C -0.3005(15) -0.0266(7) -0.2617(6) 0.055(3) Uiso 0.50 1 d P B 1 H37A H -0.3705 -0.0153 -0.2891 0.066 Uiso 0.50 1 calc PR B 1 H37B H -0.2796 0.0161 -0.2423 0.066 Uiso 0.50 1 calc PR B 1 C37B C -0.3214(16) -0.0511(9) -0.2786(6) 0.063(4) Uiso 0.50 1 d P B 2 H37C H -0.3695 -0.0771 -0.3062 0.075 Uiso 0.50 1 calc PR B 2 H37D H -0.3529 -0.0019 -0.2804 0.075 Uiso 0.50 1 calc PR B 2 C38 C -0.1627(9) -0.0565(5) -0.2822(3) 0.077(2) Uani 1 1 d . . . H38A H -0.1801 -0.0748 -0.3164 0.093 Uiso 1 1 calc R B 1 H38B H -0.0851 -0.0203 -0.2841 0.093 Uiso 1 1 calc R B 1 C39 C 0.054(2) -0.0105(12) 0.0105(8) 0.221(9) Uiso 1 1 d . . . H39A H 0.0372 -0.0047 -0.0256 0.332 Uiso 1 1 calc R . . H39B H 0.1182 -0.0507 0.0162 0.332 Uiso 1 1 calc R . . H39C H 0.1012 0.0313 0.0240 0.332 Uiso 1 1 calc R . . C40 C -0.0782(10) -0.0208(6) 0.0341(4) 0.146(5) Uiso 1 1 d G . . C41 C -0.1577(14) 0.0396(4) 0.0436(4) 0.164(6) Uiso 1 1 d G . . H41 H -0.1204 0.0832 0.0327 0.197 Uiso 1 1 calc R . . C42 C -0.2917(13) 0.0362(6) 0.0689(4) 0.178(7) Uiso 1 1 d G . . H42 H -0.3461 0.0774 0.0754 0.214 Uiso 1 1 calc R . . C43 C -0.3463(11) -0.0276(8) 0.0849(4) 0.191(7) Uiso 1 1 d G . . H43 H -0.4379 -0.0300 0.1022 0.229 Uiso 1 1 calc R . . C44 C -0.2668(13) -0.0880(6) 0.0754(4) 0.191(8) Uiso 1 1 d G . . H44 H -0.3041 -0.1316 0.0863 0.229 Uiso 1 1 calc R . . C45 C -0.1327(12) -0.0846(5) 0.0500(4) 0.119(3) Uiso 1 1 d G . . H45 H -0.0784 -0.1259 0.0436 0.143 Uiso 1 1 calc R . . C46 C -0.141(3) 0.2210(14) 0.1336(10) 0.292(14) Uiso 1 1 d . . . H46A H -0.1087 0.2473 0.1631 0.438 Uiso 1 1 calc R . . H46B H -0.0788 0.1797 0.1297 0.438 Uiso 1 1 calc R . . H46C H -0.2443 0.2068 0.1380 0.438 Uiso 1 1 calc R . . C47 C -0.1286(11) 0.2630(4) 0.0904(3) 0.114(3) Uiso 1 1 d G . . C48 C -0.0276(10) 0.3166(5) 0.0972(3) 0.126(4) Uiso 1 1 d G . . H48 H 0.0233 0.3212 0.1282 0.151 Uiso 1 1 calc R . . C49 C -0.0010(9) 0.3635(4) 0.0585(4) 0.124(4) Uiso 1 1 d G . . H49 H 0.0680 0.4001 0.0632 0.149 Uiso 1 1 calc R . . C50 C -0.0755(13) 0.3568(5) 0.0132(3) 0.172(6) Uiso 1 1 d G . . H50 H -0.0574 0.3889 -0.0133 0.207 Uiso 1 1 calc R . . C51 C -0.1765(12) 0.3032(6) 0.0064(3) 0.207(9) Uiso 1 1 d G . . H51 H -0.2274 0.2986 -0.0246 0.248 Uiso 1 1 calc R . . C52 C -0.2031(10) 0.2563(5) 0.0450(4) 0.119(4) Uiso 1 1 d G . . H52 H -0.2721 0.2197 0.0404 0.143 Uiso 1 1 calc R . . N1 N 0.0102(5) -0.2460(2) -0.19350(17) 0.0390(9) Uani 1 1 d . B . N2 N 0.1323(4) -0.14372(19) -0.14612(13) 0.0333(7) Uani 1 1 d . B . N3 N 0.2207(4) -0.0421(2) -0.20834(15) 0.0303(8) Uani 1 1 d . B . N4 N 0.2001(5) -0.0776(2) -0.30259(17) 0.0384(9) Uani 1 1 d . B . O O -0.1160(4) -0.11221(17) -0.24897(13) 0.0419(8) Uani 1 1 d . B . Cl Cl 0.35050(17) -0.22680(7) -0.25552(6) 0.0547(3) Uani 1 1 d . B . Er Er 0.13019(2) -0.149312(10) -0.232360(8) 0.03215(6) 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 0.025(2) 0.032(2) 0.051(3) 0.007(2) 0.001(2) 0.0033(18) C2 0.034(3) 0.039(2) 0.061(3) 0.011(2) 0.002(2) -0.006(2) C3 0.036(3) 0.049(3) 0.065(3) 0.017(2) 0.009(3) -0.009(3) C4 0.040(3) 0.056(3) 0.062(4) 0.029(3) 0.007(3) 0.004(3) C5 0.043(3) 0.056(3) 0.049(3) 0.017(3) 0.000(2) -0.002(3) C6 0.033(3) 0.046(3) 0.041(2) 0.009(2) -0.003(2) -0.002(2) C7 0.025(2) 0.030(2) 0.048(3) 0.007(2) -0.0001(19) 0.0005(17) C8 0.032(2) 0.034(2) 0.032(2) 0.0011(18) -0.0028(18) -0.0031(19) C9 0.030(2) 0.033(2) 0.036(2) 0.0014(19) 0.0004(19) -0.0028(18) C10 0.0255(19) 0.035(2) 0.038(3) 0.0066(19) -0.0019(18) 0.0020(17) C11 0.044(3) 0.039(2) 0.047(3) 0.003(2) 0.004(2) -0.004(2) C12 0.044(3) 0.042(3) 0.060(3) 0.006(2) 0.002(2) -0.008(2) C13 0.050(3) 0.048(3) 0.064(4) 0.019(3) 0.010(3) -0.008(2) C14 0.068(4) 0.054(3) 0.050(3) 0.012(3) 0.012(3) -0.013(3) C15 0.069(4) 0.053(3) 0.038(3) 0.004(2) 0.011(3) -0.011(3) C16 0.026(2) 0.041(3) 0.043(3) 0.003(2) -0.001(2) 0.0054(19) C17 0.057(3) 0.055(3) 0.037(3) 0.001(2) -0.003(2) -0.006(3) C18 0.105(7) 0.085(5) 0.066(4) -0.018(4) 0.028(5) -0.009(5) C19 0.083(5) 0.067(4) 0.046(3) -0.004(3) 0.005(3) -0.023(4) C20 0.052(3) 0.043(3) 0.062(4) -0.005(3) -0.003(3) -0.012(2) C21 0.084(5) 0.055(4) 0.060(4) -0.007(3) -0.001(3) -0.025(3) C22 0.077(5) 0.038(3) 0.094(6) -0.016(3) 0.008(4) -0.005(3) C23 0.031(2) 0.039(2) 0.042(2) 0.0109(18) -0.010(2) 0.000(2) C24 0.033(2) 0.048(3) 0.045(3) 0.005(2) -0.004(2) 0.003(2) C25 0.040(3) 0.060(4) 0.053(3) 0.013(3) 0.001(2) 0.011(3) C26 0.031(3) 0.082(4) 0.061(3) 0.027(4) -0.011(2) -0.003(3) C27 0.040(3) 0.067(4) 0.065(4) 0.016(3) -0.022(3) -0.012(3) C28 0.049(3) 0.046(3) 0.054(3) 0.003(3) -0.017(3) -0.001(2) C29 0.040(3) 0.037(2) 0.038(2) 0.0039(19) 0.005(2) 0.003(2) C30 0.055(3) 0.045(3) 0.069(4) -0.009(2) -0.008(4) 0.004(3) C31 0.072(5) 0.059(4) 0.083(5) -0.024(3) 0.019(4) -0.002(3) C32 0.062(4) 0.064(4) 0.098(5) -0.019(4) 0.026(5) 0.015(4) C33 0.044(4) 0.115(7) 0.132(8) -0.060(6) -0.010(4) 0.027(4) C34 0.041(3) 0.092(5) 0.100(6) -0.056(5) -0.008(4) 0.016(3) C35 0.037(3) 0.071(4) 0.100(6) 0.035(4) 0.006(3) -0.002(3) C36 0.038(3) 0.084(5) 0.121(6) 0.022(5) 0.009(5) 0.011(3) C38 0.068(5) 0.089(5) 0.075(5) 0.032(4) -0.007(3) 0.021(4) N1 0.039(2) 0.0300(19) 0.048(2) 0.0028(18) 0.0010(19) -0.0029(17) N2 0.0271(15) 0.0302(16) 0.0426(18) 0.0064(15) -0.0023(17) 0.000(2) N3 0.0270(17) 0.0290(18) 0.035(2) 0.0007(15) -0.0036(15) -0.0001(15) N4 0.036(2) 0.040(2) 0.039(2) 0.0036(18) -0.0004(18) -0.0015(18) O 0.0295(16) 0.0433(18) 0.0528(18) 0.0066(14) -0.0046(15) -0.0007(16) Cl 0.0501(8) 0.0515(7) 0.0623(8) -0.0012(6) 0.0080(6) 0.0161(6) Er 0.02886(8) 0.03161(9) 0.03599(9) 0.00123(9) -0.00023(9) -0.00054(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 N1 1.324(7) . ? C1 C2 1.448(7) . ? C1 C7 1.480(7) . ? C2 C3 1.363(8) . ? C3 C4 1.370(9) . ? C4 C5 1.388(8) . ? C5 C6 1.385(7) . ? C6 C7 1.422(7) . ? C7 N2 1.333(6) . ? C8 N2 1.456(6) . ? C8 C23 1.526(7) . ? C8 C9 1.549(6) . ? C9 N3 1.475(6) . ? C9 C29 1.518(7) . ? C10 N3 1.345(6) . ? C10 C11 1.420(7) . ? C10 C16 1.486(7) . ? C11 C12 1.380(7) . ? C12 C13 1.376(9) . ? C13 C14 1.381(9) . ? C14 C15 1.365(8) . ? C15 C16 1.425(8) . ? C16 N4 1.317(7) . ? C17 N4 1.485(7) . ? C17 C19 1.505(9) . ? C17 C18 1.584(11) . ? C20 N1 1.483(7) . ? C20 C21 1.505(9) . ? C20 C22 1.527(9) . ? C23 C28 1.386(8) . ? C23 C24 1.411(7) . ? C24 C25 1.388(8) . ? C25 C26 1.375(10) . ? C26 C27 1.372(10) . ? C27 C28 1.381(8) . ? C29 C34 1.360(8) . ? C29 C30 1.388(7) . ? C30 C31 1.391(10) . ? C31 C32 1.362(12) . ? C32 C33 1.380(11) . ? C33 C34 1.390(9) . ? C35 O 1.462(7) . ? C35 C36 1.494(9) . ? C36 C37A 1.489(15) . ? C36 C37B 1.501(16) . ? C37A C38 1.476(15) . ? C37B C38 1.443(16) . ? C38 O 1.453(8) . ? C39 C40 1.36(2) . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C46 C47 1.41(3) . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? N1 Er 2.391(4) . ? N2 Er 2.300(4) . ? N3 Er 2.311(4) . ? N4 Er 2.409(4) . ? O Er 2.380(4) . ? Cl Er 2.5647(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.0(5) . . ? N1 C1 C7 114.3(4) . . ? C2 C1 C7 122.7(5) . . ? C3 C2 C1 133.7(6) . . ? C2 C3 C4 130.6(5) . . ? C3 C4 C5 124.6(5) . . ? C6 C5 C4 129.9(6) . . ? C5 C6 C7 134.2(5) . . ? N2 C7 C6 123.1(4) . . ? N2 C7 C1 114.5(4) . . ? C6 C7 C1 122.3(4) . . ? N2 C8 C23 114.1(4) . . ? N2 C8 C9 110.2(4) . . ? C23 C8 C9 110.1(4) . . ? N3 C9 C29 113.4(4) . . ? N3 C9 C8 110.1(4) . . ? C29 C9 C8 111.3(4) . . ? N3 C10 C11 122.4(5) . . ? N3 C10 C16 114.4(4) . . ? C11 C10 C16 123.2(4) . . ? C12 C11 C10 134.3(5) . . ? C13 C12 C11 129.9(6) . . ? C12 C13 C14 124.2(5) . . ? C15 C14 C13 129.9(6) . . ? C14 C15 C16 135.4(6) . . ? N4 C16 C15 122.7(5) . . ? N4 C16 C10 115.5(5) . . ? C15 C16 C10 121.7(5) . . ? N4 C17 C19 110.1(5) . . ? N4 C17 C18 108.6(5) . . ? C19 C17 C18 106.7(6) . . ? N1 C20 C21 109.3(5) . . ? N1 C20 C22 111.2(5) . . ? C21 C20 C22 108.2(6) . . ? C28 C23 C24 117.7(5) . . ? C28 C23 C8 119.9(5) . . ? C24 C23 C8 122.4(4) . . ? C25 C24 C23 119.8(5) . . ? C26 C25 C24 121.0(6) . . ? C27 C26 C25 119.7(5) . . ? C26 C27 C28 120.0(6) . . ? C27 C28 C23 121.8(6) . . ? C34 C29 C30 117.9(6) . . ? C34 C29 C9 122.6(5) . . ? C30 C29 C9 119.4(5) . . ? C29 C30 C31 121.3(7) . . ? C32 C31 C30 119.9(7) . . ? C31 C32 C33 119.1(7) . . ? C32 C33 C34 120.4(7) . . ? C29 C34 C33 121.2(6) . . ? O C35 C36 106.0(5) . . ? C37A C36 C35 108.4(7) . . ? C37A C36 C37B 26.2(7) . . ? C35 C36 C37B 102.4(8) . . ? C38 C37A C36 104.7(9) . . ? C38 C37B C36 105.8(10) . . ? C37B C38 O 107.6(8) . . ? C37B C38 C37A 26.8(7) . . ? O C38 C37A 108.0(7) . . ? C39 C40 C41 114.5(13) . . ? C39 C40 C45 125.5(13) . . ? C41 C40 C45 120.0 . . ? C40 C41 C42 120.0 . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C40 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 C46 111.9(14) . . ? C52 C47 C46 128.1(14) . . ? C49 C48 C47 120.0 . . ? C50 C49 C48 120.0 . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C47 120.0 . . ? C1 N1 C20 117.9(4) . . ? C1 N1 Er 120.3(3) . . ? C20 N1 Er 121.8(4) . . ? C7 N2 C8 117.2(4) . . ? C7 N2 Er 123.2(3) . . ? C8 N2 Er 118.9(3) . . ? C10 N3 C9 117.9(4) . . ? C10 N3 Er 122.9(3) . . ? C9 N3 Er 119.2(3) . . ? C16 N4 C17 117.4(5) . . ? C16 N4 Er 119.7(4) . . ? C17 N4 Er 122.4(3) . . ? C38 O C35 107.6(5) . . ? C38 O Er 127.4(4) . . ? C35 O Er 124.7(3) . . ? N2 Er N3 71.26(14) . . ? N2 Er O 100.33(13) . . ? N3 Er O 96.60(12) . . ? N2 Er N1 66.91(15) . . ? N3 Er N1 137.44(15) . . ? O Er N1 83.65(13) . . ? N2 Er N4 138.29(14) . . ? N3 Er N4 67.06(14) . . ? O Er N4 85.96(13) . . ? N1 Er N4 154.36(15) . . ? N2 Er Cl 105.13(10) . . ? N3 Er Cl 108.11(10) . . ? O Er Cl 148.97(9) . . ? N1 Er Cl 90.22(11) . . ? N4 Er Cl 86.70(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 173.8(6) . . . . ? C7 C1 C2 C3 -8.6(9) . . . . ? C1 C2 C3 C4 -5.1(12) . . . . ? C2 C3 C4 C5 4.8(11) . . . . ? C3 C4 C5 C6 3.9(11) . . . . ? C4 C5 C6 C7 -1.5(11) . . . . ? C5 C6 C7 N2 172.9(6) . . . . ? C5 C6 C7 C1 -12.2(9) . . . . ? N1 C1 C7 N2 10.7(6) . . . . ? C2 C1 C7 N2 -167.2(4) . . . . ? N1 C1 C7 C6 -164.6(5) . . . . ? C2 C1 C7 C6 17.6(7) . . . . ? N2 C8 C9 N3 -34.5(5) . . . . ? C23 C8 C9 N3 92.3(5) . . . . ? N2 C8 C9 C29 92.1(5) . . . . ? C23 C8 C9 C29 -141.1(4) . . . . ? N3 C10 C11 C12 170.6(6) . . . . ? C16 C10 C11 C12 -10.6(9) . . . . ? C10 C11 C12 C13 7.6(11) . . . . ? C11 C12 C13 C14 4.3(11) . . . . ? C12 C13 C14 C15 -6.2(12) . . . . ? C13 C14 C15 C16 -3.9(14) . . . . ? C14 C15 C16 N4 -173.2(7) . . . . ? C14 C15 C16 C10 8.6(11) . . . . ? N3 C10 C16 N4 0.9(6) . . . . ? C11 C10 C16 N4 -178.0(4) . . . . ? N3 C10 C16 C15 179.3(5) . . . . ? C11 C10 C16 C15 0.4(8) . . . . ? N2 C8 C23 C28 -170.2(5) . . . . ? C9 C8 C23 C28 65.2(6) . . . . ? N2 C8 C23 C24 8.5(7) . . . . ? C9 C8 C23 C24 -116.1(5) . . . . ? C28 C23 C24 C25 -1.2(8) . . . . ? C8 C23 C24 C25 -179.9(5) . . . . ? C23 C24 C25 C26 0.6(9) . . . . ? C24 C25 C26 C27 -0.2(9) . . . . ? C25 C26 C27 C28 0.6(9) . . . . ? C26 C27 C28 C23 -1.3(10) . . . . ? C24 C23 C28 C27 1.6(9) . . . . ? C8 C23 C28 C27 -179.7(5) . . . . ? N3 C9 C29 C34 48.8(8) . . . . ? C8 C9 C29 C34 -76.0(7) . . . . ? N3 C9 C29 C30 -133.3(5) . . . . ? C8 C9 C29 C30 101.9(5) . . . . ? C34 C29 C30 C31 1.4(10) . . . . ? C9 C29 C30 C31 -176.5(6) . . . . ? C29 C30 C31 C32 -5.0(11) . . . . ? C30 C31 C32 C33 4.6(13) . . . . ? C31 C32 C33 C34 -1.0(15) . . . . ? C30 C29 C34 C33 2.3(13) . . . . ? C9 C29 C34 C33 -179.8(8) . . . . ? C32 C33 C34 C29 -2.6(16) . . . . ? O C35 C36 C37A 2.9(11) . . . . ? O C35 C36 C37B 29.3(10) . . . . ? C35 C36 C37A C38 11.0(13) . . . . ? C37B C36 C37A C38 -69.5(18) . . . . ? C37A C36 C37B C38 74.4(19) . . . . ? C35 C36 C37B C38 -32.3(13) . . . . ? C36 C37B C38 O 23.3(14) . . . . ? C36 C37B C38 C37A -71.9(18) . . . . ? C36 C37A C38 C37B 72.4(18) . . . . ? C36 C37A C38 O -21.1(13) . . . . ? C39 C40 C41 C42 -177.8(14) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C39 C40 C45 C44 177.5(16) . . . . ? C41 C40 C45 C44 0.0 . . . . ? C52 C47 C48 C49 0.0 . . . . ? C46 C47 C48 C49 -179.9(15) . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C52 0.0 . . . . ? C50 C51 C52 C47 0.0 . . . . ? C48 C47 C52 C51 0.0 . . . . ? C46 C47 C52 C51 179.8(18) . . . . ? C2 C1 N1 C20 -10.8(7) . . . . ? C7 C1 N1 C20 171.3(4) . . . . ? C2 C1 N1 Er 169.1(4) . . . . ? C7 C1 N1 Er -8.7(5) . . . . ? C21 C20 N1 C1 170.3(5) . . . . ? C22 C20 N1 C1 -70.3(7) . . . . ? C21 C20 N1 Er -9.6(7) . . . . ? C22 C20 N1 Er 109.8(5) . . . . ? C6 C7 N2 C8 -2.9(7) . . . . ? C1 C7 N2 C8 -178.1(4) . . . . ? C6 C7 N2 Er 167.1(4) . . . . ? C1 C7 N2 Er -8.2(5) . . . . ? C23 C8 N2 C7 78.2(5) . . . . ? C9 C8 N2 C7 -157.3(4) . . . . ? C23 C8 N2 Er -92.2(4) . . . . ? C9 C8 N2 Er 32.3(5) . . . . ? C11 C10 N3 C9 2.5(6) . . . . ? C16 C10 N3 C9 -176.3(4) . . . . ? C11 C10 N3 Er -176.3(3) . . . . ? C16 C10 N3 Er 4.8(5) . . . . ? C29 C9 N3 C10 79.3(5) . . . . ? C8 C9 N3 C10 -155.2(4) . . . . ? C29 C9 N3 Er -101.7(4) . . . . ? C8 C9 N3 Er 23.7(5) . . . . ? C15 C16 N4 C17 3.8(7) . . . . ? C10 C16 N4 C17 -177.8(5) . . . . ? C15 C16 N4 Er 175.9(4) . . . . ? C10 C16 N4 Er -5.7(6) . . . . ? C19 C17 N4 C16 -172.1(5) . . . . ? C18 C17 N4 C16 71.4(6) . . . . ? C19 C17 N4 Er 16.0(7) . . . . ? C18 C17 N4 Er -100.5(5) . . . . ? C37B C38 O C35 -4.6(11) . . . . ? C37A C38 O C35 23.6(10) . . . . ? C37B C38 O Er -177.6(8) . . . . ? C37A C38 O Er -149.4(7) . . . . ? C36 C35 O C38 -16.0(9) . . . . ? C36 C35 O Er 157.2(5) . . . . ? C7 N2 Er N3 174.9(4) . . . . ? C8 N2 Er N3 -15.3(3) . . . . ? C7 N2 Er O 81.4(4) . . . . ? C8 N2 Er O -108.8(3) . . . . ? C7 N2 Er N1 2.9(3) . . . . ? C8 N2 Er N1 172.7(4) . . . . ? C7 N2 Er N4 176.9(3) . . . . ? C8 N2 Er N4 -13.3(4) . . . . ? C7 N2 Er Cl -80.7(4) . . . . ? C8 N2 Er Cl 89.1(3) . . . . ? C10 N3 Er N2 173.0(4) . . . . ? C9 N3 Er N2 -5.9(3) . . . . ? C10 N3 Er O -88.3(3) . . . . ? C9 N3 Er O 92.8(3) . . . . ? C10 N3 Er N1 -176.1(3) . . . . ? C9 N3 Er N1 5.0(4) . . . . ? C10 N3 Er N4 -5.5(3) . . . . ? C9 N3 Er N4 175.6(4) . . . . ? C10 N3 Er Cl 72.7(3) . . . . ? C9 N3 Er Cl -106.2(3) . . . . ? C38 O Er N2 126.7(5) . . . . ? C35 O Er N2 -45.2(5) . . . . ? C38 O Er N3 54.6(6) . . . . ? C35 O Er N3 -117.3(5) . . . . ? C38 O Er N1 -168.3(6) . . . . ? C35 O Er N1 19.9(5) . . . . ? C38 O Er N4 -11.7(5) . . . . ? C35 O Er N4 176.4(5) . . . . ? C38 O Er Cl -88.5(6) . . . . ? C35 O Er Cl 99.6(5) . . . . ? C1 N1 Er N2 3.6(3) . . . . ? C20 N1 Er N2 -176.5(4) . . . . ? C1 N1 Er N3 -7.6(5) . . . . ? C20 N1 Er N3 172.3(4) . . . . ? C1 N1 Er O -100.5(4) . . . . ? C20 N1 Er O 79.4(4) . . . . ? C1 N1 Er N4 -167.2(3) . . . . ? C20 N1 Er N4 12.7(6) . . . . ? C1 N1 Er Cl 110.0(4) . . . . ? C20 N1 Er Cl -70.1(4) . . . . ? C16 N4 Er N2 3.8(5) . . . . ? C17 N4 Er N2 175.5(4) . . . . ? C16 N4 Er N3 5.9(3) . . . . ? C17 N4 Er N3 177.6(4) . . . . ? C16 N4 Er O 104.8(4) . . . . ? C17 N4 Er O -83.5(4) . . . . ? C16 N4 Er N1 171.0(3) . . . . ? C17 N4 Er N1 -17.3(6) . . . . ? C16 N4 Er Cl -105.4(4) . . . . ? C17 N4 Er Cl 66.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.054 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.087 #============================================================================== data_5a _database_code_depnum_ccdc_archive 'CCDC 638158' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H60 Cl N4 O3 Yb' _chemical_formula_weight 925.47 _chemical_absolute_configuration rmad 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' Yb Yb -0.3850 5.5486 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7538(7) _cell_length_b 15.9058(9) _cell_length_c 15.8563(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.728(7) _cell_angle_gamma 90.00 _cell_volume 2144.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.519 _exptl_crystal_size_mid 0.325 _exptl_crystal_size_min 0.134 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 950 _exptl_absorpt_coefficient_mu 2.287 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3820 _exptl_absorpt_correction_T_max 0.7311 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15281 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 29.30 _reflns_number_total 11190 _reflns_number_gt 10061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0387P)^2^+39.8963P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 11190 _refine_ls_number_parameters 368 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2188 _refine_ls_wR_factor_gt 0.2152 _refine_ls_goodness_of_fit_ref 1.273 _refine_ls_restrained_S_all 1.273 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb Yb 0.34118(6) 0.25588(7) 0.17697(3) 0.02618(13) Uani 1 1 d . . . Cl Cl 0.5494(4) 0.1701(3) 0.1255(3) 0.0437(8) Uani 1 1 d . . . O1 O 0.0895(12) 0.3162(7) 0.1534(8) 0.045(3) Uani 1 1 d . B . N1 N 0.2078(14) 0.1315(8) 0.1904(9) 0.038(3) Uani 1 1 d . . . N2 N 0.3808(13) 0.2171(6) 0.3187(7) 0.027(2) Uani 1 1 d . . . N3 N 0.4527(12) 0.3669(7) 0.2596(7) 0.025(2) Uani 1 1 d . . . N4 N 0.3937(14) 0.3690(8) 0.0914(7) 0.034(2) Uani 1 1 d . . . C1 C 0.2232(17) 0.0957(9) 0.2692(11) 0.038(3) Uani 1 1 d . . . C2 C 0.157(3) 0.0185(12) 0.2812(15) 0.067(6) Uani 1 1 d . . . H2 H 0.1096 -0.0086 0.2281 0.080 Uiso 1 1 calc R . . C3 C 0.146(2) -0.0281(12) 0.3547(17) 0.065(6) Uani 1 1 d . . . H3 H 0.0798 -0.0762 0.3425 0.078 Uiso 1 1 calc R . . C4 C 0.217(2) -0.0154(13) 0.4452(14) 0.054(4) Uiso 1 1 d . . . H4 H 0.2013 -0.0557 0.4865 0.064 Uiso 1 1 calc R . . C5 C 0.304(3) 0.0512(11) 0.4716(13) 0.057(5) Uani 1 1 d . . . H5 H 0.3426 0.0536 0.5328 0.069 Uiso 1 1 calc R . . C6 C 0.351(2) 0.1185(10) 0.4286(13) 0.051(4) Uani 1 1 d . . . H6 H 0.4176 0.1559 0.4673 0.061 Uiso 1 1 calc R . . C7 C 0.3245(17) 0.1450(9) 0.3428(10) 0.033(3) Uani 1 1 d . . . C8 C 0.4759(16) 0.2686(13) 0.3845(9) 0.039(4) Uani 1 1 d . . . H8 H 0.4287 0.2649 0.4360 0.047 Uiso 1 1 calc R . . C9 C 0.4615(15) 0.3638(8) 0.3546(8) 0.027(2) Uani 1 1 d . . . H9 H 0.5591 0.3939 0.3856 0.033 Uiso 1 1 calc R . . C10 C 0.5092(14) 0.4346(8) 0.2278(9) 0.028(2) Uani 1 1 d . . . C11 C 0.612(2) 0.4929(9) 0.2772(10) 0.040(3) Uani 1 1 d . . . H11 H 0.6453 0.4773 0.3366 0.048 Uiso 1 1 calc R . . C12 C 0.677(2) 0.5675(12) 0.2596(13) 0.053(5) Uani 1 1 d . . . H12 H 0.7505 0.5917 0.3073 0.063 Uiso 1 1 calc R . . C13 C 0.652(2) 0.6122(12) 0.1841(13) 0.054(4) Uani 1 1 d . . . H13 H 0.7044 0.6648 0.1857 0.065 Uiso 1 1 calc R . . C14 C 0.559(2) 0.5875(12) 0.1066(12) 0.051(4) Uani 1 1 d . . . H14 H 0.5440 0.6288 0.0620 0.061 Uiso 1 1 calc R . . C15 C 0.4817(19) 0.5105(10) 0.0819(10) 0.039(3) Uani 1 1 d . . . H15 H 0.4339 0.5068 0.0216 0.047 Uiso 1 1 calc R . . C16 C 0.4611(15) 0.4375(8) 0.1292(8) 0.029(2) Uani 1 1 d . . . C17 C 0.344(2) 0.3648(12) -0.0036(10) 0.050(4) Uani 1 1 d . . . H17 H 0.2917 0.4185 -0.0276 0.061 Uiso 1 1 calc R . . C18 C 0.236(2) 0.2923(13) -0.0310(11) 0.058(5) Uani 1 1 d . . . H18A H 0.2890 0.2401 -0.0080 0.087 Uiso 1 1 calc R . . H18B H 0.2053 0.2895 -0.0945 0.087 Uiso 1 1 calc R . . H18C H 0.1414 0.2996 -0.0085 0.087 Uiso 1 1 calc R . . C19 C 0.490(3) 0.3484(15) -0.0385(13) 0.074(7) Uani 1 1 d . . . H19A H 0.5580 0.3983 -0.0288 0.111 Uiso 1 1 calc R . . H19B H 0.4583 0.3365 -0.1008 0.111 Uiso 1 1 calc R . . H19C H 0.5480 0.3002 -0.0082 0.111 Uiso 1 1 calc R . . C20 C 0.128(2) 0.0897(14) 0.1082(13) 0.056(5) Uani 1 1 d . . . H20 H 0.1253 0.1330 0.0621 0.068 Uiso 1 1 calc R . . C21 C -0.047(4) 0.068(2) 0.101(2) 0.103(9) Uiso 1 1 d . . . H21A H -0.0679 0.0099 0.0803 0.154 Uiso 1 1 calc R . . H21B H -0.1147 0.1065 0.0610 0.154 Uiso 1 1 calc R . . H21C H -0.0702 0.0728 0.1589 0.154 Uiso 1 1 calc R . . C22 C 0.222(3) 0.0185(17) 0.0850(18) 0.084(7) Uiso 1 1 d . . . H22A H 0.3294 0.0375 0.0879 0.125 Uiso 1 1 calc R . . H22B H 0.1735 -0.0008 0.0259 0.125 Uiso 1 1 calc R . . H22C H 0.2241 -0.0280 0.1259 0.125 Uiso 1 1 calc R . . C23 C 0.6466(7) 0.2422(4) 0.4159(4) 0.032(3) Uani 1 1 d G . . C24 C 0.7222(9) 0.1968(5) 0.3629(5) 0.047(4) Uani 1 1 d G . . H24 H 0.6654 0.1789 0.3071 0.057 Uiso 1 1 calc R . . C25 C 0.8810(9) 0.1775(6) 0.3915(6) 0.047(4) Uani 1 1 d G . . H25 H 0.9327 0.1465 0.3552 0.056 Uiso 1 1 calc R . . C26 C 0.9641(7) 0.2037(6) 0.4731(6) 0.043(3) Uiso 1 1 d G . . H26 H 1.0726 0.1906 0.4927 0.051 Uiso 1 1 calc R . . C27 C 0.8885(9) 0.2492(7) 0.5261(5) 0.056(4) Uiso 1 1 d G . . H27 H 0.9453 0.2671 0.5819 0.067 Uiso 1 1 calc R . . C28 C 0.7297(8) 0.2685(5) 0.4975(4) 0.044(4) Uani 1 1 d G . . H28 H 0.6780 0.2995 0.5338 0.053 Uiso 1 1 calc R . . C29 C 0.3202(9) 0.4089(6) 0.3747(7) 0.032(3) Uani 1 1 d G . . C30 C 0.3278(12) 0.4954(6) 0.3902(9) 0.065(5) Uiso 1 1 d G . . H30 H 0.4200 0.5266 0.3893 0.078 Uiso 1 1 calc R . . C31 C 0.195(3) 0.5346(14) 0.4070(15) 0.055(5) Uiso 1 1 d . . . H31 H 0.1932 0.5943 0.4080 0.066 Uiso 1 1 calc R . . C32 C 0.072(2) 0.4948(12) 0.4216(12) 0.051(4) Uiso 1 1 d . . . H32 H -0.0070 0.5240 0.4418 0.062 Uiso 1 1 calc R . . C33 C 0.061(2) 0.4076(11) 0.4062(11) 0.046(4) Uiso 1 1 d . . . H33 H -0.0306 0.3778 0.4104 0.055 Uiso 1 1 calc R . . C34 C 0.1859(19) 0.3650(10) 0.3849(11) 0.041(3) Uiso 1 1 d . . . H34 H 0.1804 0.3057 0.3772 0.050 Uiso 1 1 calc R . . C35 C -0.046(3) 0.2785(16) 0.1673(17) 0.080(7) Uiso 1 1 d . B . H35A H -0.0181 0.2406 0.2181 0.096 Uiso 1 1 calc R . . H35B H -0.0964 0.2445 0.1160 0.096 Uiso 1 1 calc R . . C36 C -0.157(3) 0.3436(13) 0.1827(15) 0.064(5) Uiso 1 1 d . . . H36A H -0.1705 0.3407 0.2430 0.076 Uiso 1 1 calc R A 1 H36B H -0.2614 0.3372 0.1419 0.076 Uiso 1 1 calc R A 1 C37A C -0.077(4) 0.428(2) 0.166(2) 0.044(7) Uiso 0.50 1 d P B 1 H37A H -0.1481 0.4612 0.1203 0.053 Uiso 0.50 1 calc PR B 1 H37B H -0.0507 0.4623 0.2201 0.053 Uiso 0.50 1 calc PR B 1 C37B C -0.115(2) 0.4107(11) 0.1319(13) 0.043(7) Uiso 0.50 1 d P B 2 H37C H -0.1421 0.4657 0.1536 0.052 Uiso 0.50 1 calc PR B 2 H37D H -0.1722 0.4049 0.0704 0.052 Uiso 0.50 1 calc PR B 2 C38 C 0.062(2) 0.4051(11) 0.1401(13) 0.063(6) Uani 1 1 d R . . H38A H 0.1530 0.4380 0.1727 0.076 Uiso 1 1 d R . . H38B H 0.0477 0.4174 0.0773 0.076 Uiso 1 1 d R . . O2 O 0.765(4) -0.127(3) 0.278(3) 0.188(14) Uiso 1 1 d D . . C39 C 0.692(6) -0.171(3) 0.338(4) 0.18(2) Uiso 1 1 d D . . H39A H 0.7717 -0.1866 0.3906 0.219 Uiso 1 1 calc R . . H39B H 0.6401 -0.2226 0.3104 0.219 Uiso 1 1 calc R . . C40 C 0.575(6) -0.115(4) 0.360(4) 0.18(2) Uiso 1 1 d D . . H40A H 0.4662 -0.1304 0.3306 0.220 Uiso 1 1 calc R . . H40B H 0.5856 -0.1116 0.4238 0.220 Uiso 1 1 calc R . . C41 C 0.627(6) -0.042(3) 0.326(4) 0.19(2) Uiso 1 1 d D . . H41A H 0.6959 -0.0118 0.3753 0.223 Uiso 1 1 calc R . . H41B H 0.5339 -0.0065 0.3043 0.223 Uiso 1 1 calc R . . C42 C 0.709(10) -0.049(5) 0.260(5) 0.26(4) Uiso 1 1 d D . . H42A H 0.6381 -0.0445 0.2013 0.311 Uiso 1 1 calc R . . H42B H 0.7942 -0.0065 0.2663 0.311 Uiso 1 1 calc R . . O3 O 0.091(7) -0.271(4) 0.234(3) 0.28(3) Uiso 1 1 d D . . C43 C 0.094(6) -0.347(3) 0.184(4) 0.173(19) Uiso 1 1 d D . . H43A H -0.0130 -0.3586 0.1478 0.208 Uiso 1 1 calc R . . H43B H 0.1270 -0.3954 0.2232 0.208 Uiso 1 1 calc R . . C44 C 0.203(12) -0.334(7) 0.129(7) 0.47(8) Uiso 1 1 d D . . H44A H 0.3012 -0.3675 0.1484 0.563 Uiso 1 1 calc R . . H44B H 0.1554 -0.3456 0.0669 0.563 Uiso 1 1 calc R . . C45 C 0.225(8) -0.249(6) 0.147(5) 0.33(4) Uiso 1 1 d D . . H45A H 0.1463 -0.2171 0.1039 0.392 Uiso 1 1 calc R . . H45B H 0.3303 -0.2327 0.1394 0.392 Uiso 1 1 calc R . . C46 C 0.215(10) -0.222(6) 0.231(6) 0.40(7) Uiso 1 1 d D . . H46A H 0.3102 -0.2355 0.2768 0.484 Uiso 1 1 calc R . . H46B H 0.1906 -0.1610 0.2331 0.484 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb 0.0287(2) 0.0258(2) 0.02516(19) 0.0008(3) 0.00852(15) 0.0120(3) Cl 0.0351(18) 0.053(2) 0.047(2) -0.0050(16) 0.0168(16) 0.0075(15) O1 0.023(5) 0.057(7) 0.060(7) -0.007(5) 0.021(5) 0.002(4) N1 0.027(6) 0.034(6) 0.054(8) -0.012(5) 0.011(5) -0.008(4) N2 0.034(6) 0.024(5) 0.024(5) 0.005(4) 0.009(4) 0.001(4) N3 0.022(5) 0.029(5) 0.025(5) 0.005(4) 0.008(4) 0.000(4) N4 0.034(6) 0.043(6) 0.026(5) 0.013(5) 0.009(5) 0.005(5) C1 0.031(7) 0.036(7) 0.051(9) 0.003(6) 0.017(6) 0.001(5) C2 0.098(17) 0.038(9) 0.060(12) 0.006(8) 0.009(12) -0.021(10) C3 0.063(12) 0.040(9) 0.093(16) 0.013(10) 0.020(12) -0.027(8) C5 0.082(14) 0.047(9) 0.053(10) 0.012(8) 0.036(10) -0.001(9) C6 0.072(12) 0.036(8) 0.049(10) 0.014(7) 0.022(9) -0.004(7) C7 0.036(7) 0.033(7) 0.037(7) 0.005(6) 0.025(6) -0.003(5) C8 0.035(6) 0.053(13) 0.030(6) -0.003(7) 0.007(5) 0.005(7) C9 0.028(6) 0.031(6) 0.023(6) 0.007(5) 0.008(5) -0.004(5) C10 0.016(5) 0.037(6) 0.031(6) 0.004(5) 0.005(5) 0.004(5) C11 0.057(9) 0.031(7) 0.035(7) 0.000(5) 0.015(7) -0.013(6) C12 0.059(11) 0.054(10) 0.050(10) -0.009(8) 0.023(8) -0.031(8) C13 0.066(12) 0.047(9) 0.057(11) 0.005(8) 0.028(9) -0.010(8) C14 0.048(9) 0.055(10) 0.052(10) 0.018(8) 0.016(8) 0.003(8) C15 0.043(8) 0.047(8) 0.030(7) 0.007(6) 0.011(6) 0.000(6) C16 0.024(6) 0.036(6) 0.027(6) 0.003(5) 0.006(5) 0.005(5) C17 0.064(11) 0.058(10) 0.026(7) -0.003(7) 0.004(7) -0.013(9) C18 0.065(12) 0.074(12) 0.036(9) -0.014(8) 0.012(8) -0.013(9) C19 0.12(2) 0.073(14) 0.040(10) -0.005(9) 0.044(12) 0.001(13) C20 0.036(9) 0.075(13) 0.053(11) -0.022(9) 0.001(8) -0.005(8) C23 0.035(6) 0.025(8) 0.040(6) 0.001(5) 0.016(5) 0.003(5) C24 0.032(8) 0.073(11) 0.041(8) -0.003(8) 0.016(7) 0.017(7) C25 0.029(7) 0.046(9) 0.073(12) 0.001(8) 0.025(8) 0.000(6) C28 0.034(6) 0.045(11) 0.051(8) 0.011(7) 0.004(6) -0.007(6) C29 0.034(7) 0.042(8) 0.027(7) 0.003(6) 0.020(6) 0.004(6) C38 0.044(10) 0.060(11) 0.092(16) 0.027(11) 0.028(11) 0.030(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 Yb N2 2.276(10) . ? Yb N3 2.277(11) . ? Yb N1 2.332(12) . ? Yb O1 2.350(10) . ? Yb N4 2.363(11) . ? Yb Cl 2.561(4) . ? Yb C7 3.198(14) . ? O1 C35 1.39(3) . ? O1 C38 1.442(19) . ? N1 C1 1.35(2) . ? N1 C20 1.48(2) . ? N2 C7 1.339(16) . ? N2 C8 1.428(19) . ? N3 C10 1.334(16) . ? N3 C9 1.491(16) . ? N4 C16 1.315(18) . ? N4 C17 1.466(19) . ? C1 C2 1.39(2) . ? C1 C7 1.51(2) . ? C2 C3 1.41(3) . ? C3 C4 1.44(3) . ? C4 C5 1.31(3) . ? C5 C6 1.38(2) . ? C6 C7 1.39(2) . ? C8 C23 1.518(15) . ? C8 C9 1.58(2) . ? C9 C29 1.528(15) . ? C10 C11 1.398(19) . ? C10 C16 1.520(18) . ? C11 C12 1.37(2) . ? C12 C13 1.37(3) . ? C13 C14 1.36(3) . ? C14 C15 1.41(2) . ? C15 C16 1.42(2) . ? C17 C18 1.49(2) . ? C17 C19 1.54(3) . ? C20 C22 1.50(3) . ? C20 C21 1.55(4) . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C29 C30 1.3956 . ? C29 C34 1.410(19) . ? C30 C31 1.40(2) . ? C31 C32 1.31(3) . ? C32 C33 1.41(2) . ? C33 C34 1.39(2) . ? C35 C36 1.48(3) . ? C36 C37B 1.44(3) . ? C36 C37A 1.57(4) . ? C37A C38 1.42(4) . ? C37B C38 1.5238 . ? O2 C42 1.34(7) . ? O2 C39 1.44(5) . ? C39 C40 1.46(6) . ? C40 C41 1.40(6) . ? C41 C42 1.41(7) . ? O3 C46 1.35(7) . ? O3 C43 1.45(5) . ? C43 C44 1.46(6) . ? C44 C45 1.40(7) . ? C45 C46 1.42(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Yb N3 72.4(4) . . ? N2 Yb N1 69.0(4) . . ? N3 Yb N1 139.6(4) . . ? N2 Yb O1 100.6(4) . . ? N3 Yb O1 91.9(4) . . ? N1 Yb O1 83.7(4) . . ? N2 Yb N4 140.2(4) . . ? N3 Yb N4 68.0(4) . . ? N1 Yb N4 150.2(5) . . ? O1 Yb N4 84.3(4) . . ? N2 Yb Cl 102.5(3) . . ? N3 Yb Cl 110.9(3) . . ? N1 Yb Cl 89.2(3) . . ? O1 Yb Cl 151.5(3) . . ? N4 Yb Cl 88.4(3) . . ? N2 Yb C7 20.8(4) . . ? N3 Yb C7 93.0(4) . . ? N1 Yb C7 48.4(4) . . ? O1 Yb C7 97.6(4) . . ? N4 Yb C7 160.9(4) . . ? Cl Yb C7 98.2(3) . . ? C35 O1 C38 109.0(14) . . ? C35 O1 Yb 126.9(13) . . ? C38 O1 Yb 122.9(9) . . ? C1 N1 C20 123.2(14) . . ? C1 N1 Yb 119.9(10) . . ? C20 N1 Yb 116.3(12) . . ? C7 N2 C8 118.2(12) . . ? C7 N2 Yb 122.2(9) . . ? C8 N2 Yb 119.5(9) . . ? C10 N3 C9 118.3(11) . . ? C10 N3 Yb 123.7(9) . . ? C9 N3 Yb 117.9(7) . . ? C16 N4 C17 119.9(12) . . ? C16 N4 Yb 119.8(9) . . ? C17 N4 Yb 120.2(10) . . ? N1 C1 C2 123.0(16) . . ? N1 C1 C7 114.1(12) . . ? C2 C1 C7 122.8(16) . . ? C1 C2 C3 134(2) . . ? C2 C3 C4 130.8(17) . . ? C5 C4 C3 120.9(19) . . ? C4 C5 C6 133(2) . . ? C5 C6 C7 135.8(19) . . ? N2 C7 C6 123.5(14) . . ? N2 C7 C1 114.5(12) . . ? C6 C7 C1 122.0(14) . . ? N2 C7 Yb 37.0(6) . . ? C6 C7 Yb 160.4(12) . . ? C1 C7 Yb 77.5(8) . . ? N2 C8 C23 116.0(13) . . ? N2 C8 C9 109.8(11) . . ? C23 C8 C9 111.4(12) . . ? N3 C9 C29 110.2(10) . . ? N3 C9 C8 108.4(10) . . ? C29 C9 C8 113.4(10) . . ? N3 C10 C11 124.8(12) . . ? N3 C10 C16 112.1(11) . . ? C11 C10 C16 122.8(12) . . ? C12 C11 C10 134.6(16) . . ? C13 C12 C11 129.9(18) . . ? C14 C13 C12 125.3(17) . . ? C13 C14 C15 130.3(16) . . ? C14 C15 C16 132.7(15) . . ? N4 C16 C15 122.5(13) . . ? N4 C16 C10 115.4(11) . . ? C15 C16 C10 122.0(13) . . ? N4 C17 C18 110.5(14) . . ? N4 C17 C19 107.8(15) . . ? C18 C17 C19 106.9(17) . . ? N1 C20 C22 112.4(17) . . ? N1 C20 C21 115(2) . . ? C22 C20 C21 114(2) . . ? C24 C23 C28 120.0 . . ? C24 C23 C8 121.2(7) . . ? C28 C23 C8 118.7(7) . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C27 C28 C23 120.0 . . ? C30 C29 C34 118.4(8) . . ? C30 C29 C9 119.5(6) . . ? C34 C29 C9 122.0(11) . . ? C29 C30 C31 117.7(11) . . ? C32 C31 C30 124.8(19) . . ? C31 C32 C33 117.8(19) . . ? C34 C33 C32 119.9(17) . . ? C33 C34 C29 120.6(14) . . ? O1 C35 C36 110(2) . . ? C37B C36 C35 99.1(19) . . ? C37B C36 C37A 23.8(15) . . ? C35 C36 C37A 104(2) . . ? C38 C37A C36 106(2) . . ? C36 C37B C38 107.5(11) . . ? C37A C38 O1 110(2) . . ? C37A C38 C37B 24.4(15) . . ? O1 C38 C37B 101.6(8) . . ? C42 O2 C39 113(5) . . ? O2 C39 C40 108(4) . . ? C41 C40 C39 96(5) . . ? C40 C41 C42 120(6) . . ? O2 C42 C41 97(6) . . ? C46 O3 C43 110(5) . . ? O3 C43 C44 108(4) . . ? C45 C44 C43 95(5) . . ? C44 C45 C46 117(6) . . ? O3 C46 C45 95(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Yb O1 C35 -55.3(17) . . . . ? N3 Yb O1 C35 -127.7(16) . . . . ? N1 Yb O1 C35 12.0(16) . . . . ? N4 Yb O1 C35 164.6(17) . . . . ? Cl Yb O1 C35 88.6(18) . . . . ? C7 Yb O1 C35 -34.5(17) . . . . ? N2 Yb O1 C38 110.6(13) . . . . ? N3 Yb O1 C38 38.2(13) . . . . ? N1 Yb O1 C38 177.9(13) . . . . ? N4 Yb O1 C38 -29.4(13) . . . . ? Cl Yb O1 C38 -105.5(13) . . . . ? C7 Yb O1 C38 131.4(13) . . . . ? N2 Yb N1 C1 -3.4(10) . . . . ? N3 Yb N1 C1 -22.0(14) . . . . ? O1 Yb N1 C1 -107.4(11) . . . . ? N4 Yb N1 C1 -174.2(10) . . . . ? Cl Yb N1 C1 100.3(11) . . . . ? C7 Yb N1 C1 -1.4(9) . . . . ? N2 Yb N1 C20 -175.0(12) . . . . ? N3 Yb N1 C20 166.5(10) . . . . ? O1 Yb N1 C20 81.0(11) . . . . ? N4 Yb N1 C20 14.2(16) . . . . ? Cl Yb N1 C20 -71.2(11) . . . . ? C7 Yb N1 C20 -173.0(13) . . . . ? N3 Yb N2 C7 171.8(11) . . . . ? N1 Yb N2 C7 4.3(10) . . . . ? O1 Yb N2 C7 83.3(11) . . . . ? N4 Yb N2 C7 177.2(9) . . . . ? Cl Yb N2 C7 -80.0(11) . . . . ? N3 Yb N2 C8 -11.7(10) . . . . ? N1 Yb N2 C8 -179.2(11) . . . . ? O1 Yb N2 C8 -100.3(10) . . . . ? N4 Yb N2 C8 -6.4(13) . . . . ? Cl Yb N2 C8 96.5(10) . . . . ? C7 Yb N2 C8 176.4(17) . . . . ? N2 Yb N3 C10 168.8(11) . . . . ? N1 Yb N3 C10 -173.1(9) . . . . ? O1 Yb N3 C10 -90.7(10) . . . . ? N4 Yb N3 C10 -7.6(9) . . . . ? Cl Yb N3 C10 71.7(10) . . . . ? C7 Yb N3 C10 171.7(10) . . . . ? N2 Yb N3 C9 -11.9(8) . . . . ? N1 Yb N3 C9 6.3(12) . . . . ? O1 Yb N3 C9 88.7(9) . . . . ? N4 Yb N3 C9 171.8(9) . . . . ? Cl Yb N3 C9 -108.9(8) . . . . ? C7 Yb N3 C9 -9.0(9) . . . . ? N2 Yb N4 C16 -4.2(13) . . . . ? N3 Yb N4 C16 1.3(9) . . . . ? N1 Yb N4 C16 162.3(9) . . . . ? O1 Yb N4 C16 95.7(10) . . . . ? Cl Yb N4 C16 -112.0(10) . . . . ? C7 Yb N4 C16 -1.1(19) . . . . ? N2 Yb N4 C17 179.2(11) . . . . ? N3 Yb N4 C17 -175.3(13) . . . . ? N1 Yb N4 C17 -14.3(17) . . . . ? O1 Yb N4 C17 -81.0(13) . . . . ? Cl Yb N4 C17 71.4(12) . . . . ? C7 Yb N4 C17 -177.7(14) . . . . ? C20 N1 C1 C2 -4(3) . . . . ? Yb N1 C1 C2 -174.8(15) . . . . ? C20 N1 C1 C7 173.4(14) . . . . ? Yb N1 C1 C7 2.4(16) . . . . ? N1 C1 C2 C3 -174(2) . . . . ? C7 C1 C2 C3 9(4) . . . . ? C1 C2 C3 C4 -9(5) . . . . ? C2 C3 C4 C5 4(4) . . . . ? C3 C4 C5 C6 -2(4) . . . . ? C4 C5 C6 C7 2(4) . . . . ? C8 N2 C7 C6 2(2) . . . . ? Yb N2 C7 C6 178.0(13) . . . . ? C8 N2 C7 C1 178.9(12) . . . . ? Yb N2 C7 C1 -4.6(16) . . . . ? C8 N2 C7 Yb -176.5(17) . . . . ? C5 C6 C7 N2 177(2) . . . . ? C5 C6 C7 C1 0(3) . . . . ? C5 C6 C7 Yb -180(2) . . . . ? N1 C1 C7 N2 1.2(18) . . . . ? C2 C1 C7 N2 178.5(17) . . . . ? N1 C1 C7 C6 178.7(15) . . . . ? C2 C1 C7 C6 -4(3) . . . . ? N1 C1 C7 Yb -1.6(11) . . . . ? C2 C1 C7 Yb 175.7(18) . . . . ? N3 Yb C7 N2 -7.8(11) . . . . ? N1 Yb C7 N2 -174.6(13) . . . . ? O1 Yb C7 N2 -100.1(11) . . . . ? N4 Yb C7 N2 -5.5(18) . . . . ? Cl Yb C7 N2 103.8(10) . . . . ? N2 Yb C7 C6 -5(3) . . . . ? N3 Yb C7 C6 -13(4) . . . . ? N1 Yb C7 C6 -180(4) . . . . ? O1 Yb C7 C6 -105(4) . . . . ? N4 Yb C7 C6 -11(4) . . . . ? Cl Yb C7 C6 99(4) . . . . ? N2 Yb C7 C1 175.7(15) . . . . ? N3 Yb C7 C1 167.9(8) . . . . ? N1 Yb C7 C1 1.1(7) . . . . ? O1 Yb C7 C1 75.7(8) . . . . ? N4 Yb C7 C1 170.2(11) . . . . ? Cl Yb C7 C1 -80.5(8) . . . . ? C7 N2 C8 C23 80.0(15) . . . . ? Yb N2 C8 C23 -96.6(13) . . . . ? C7 N2 C8 C9 -152.7(12) . . . . ? Yb N2 C8 C9 30.8(13) . . . . ? C10 N3 C9 C29 84.9(13) . . . . ? Yb N3 C9 C29 -94.5(10) . . . . ? C10 N3 C9 C8 -150.4(11) . . . . ? Yb N3 C9 C8 30.2(12) . . . . ? N2 C8 C9 N3 -37.6(14) . . . . ? C23 C8 C9 N3 92.4(12) . . . . ? N2 C8 C9 C29 85.1(13) . . . . ? C23 C8 C9 C29 -145.0(10) . . . . ? C9 N3 C10 C11 17.9(19) . . . . ? Yb N3 C10 C11 -162.7(11) . . . . ? C9 N3 C10 C16 -167.7(10) . . . . ? Yb N3 C10 C16 11.7(14) . . . . ? N3 C10 C11 C12 -176(2) . . . . ? C16 C10 C11 C12 10(3) . . . . ? C10 C11 C12 C13 4(4) . . . . ? C11 C12 C13 C14 -4(4) . . . . ? C12 C13 C14 C15 -7(4) . . . . ? C13 C14 C15 C16 7(3) . . . . ? C17 N4 C16 C15 3(2) . . . . ? Yb N4 C16 C15 -173.6(11) . . . . ? C17 N4 C16 C10 -179.6(14) . . . . ? Yb N4 C16 C10 3.8(15) . . . . ? C14 C15 C16 N4 -174.5(17) . . . . ? C14 C15 C16 C10 8(3) . . . . ? N3 C10 C16 N4 -9.5(16) . . . . ? C11 C10 C16 N4 165.0(13) . . . . ? N3 C10 C16 C15 167.9(13) . . . . ? C11 C10 C16 C15 -18(2) . . . . ? C16 N4 C17 C18 -165.4(15) . . . . ? Yb N4 C17 C18 11(2) . . . . ? C16 N4 C17 C19 78.0(19) . . . . ? Yb N4 C17 C19 -105.3(14) . . . . ? C1 N1 C20 C22 -72(2) . . . . ? Yb N1 C20 C22 99(2) . . . . ? C1 N1 C20 C21 60(3) . . . . ? Yb N1 C20 C21 -128.6(18) . . . . ? N2 C8 C23 C24 26.2(16) . . . . ? C9 C8 C23 C24 -100.4(11) . . . . ? N2 C8 C23 C28 -157.3(9) . . . . ? C9 C8 C23 C28 76.1(11) . . . . ? C28 C23 C24 C25 0.0 . . . . ? C8 C23 C24 C25 176.4(10) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C23 0.0 . . . . ? C24 C23 C28 C27 0.0 . . . . ? C8 C23 C28 C27 -176.5(9) . . . . ? N3 C9 C29 C30 -87.5(10) . . . . ? C8 C9 C29 C30 150.8(8) . . . . ? N3 C9 C29 C34 97.6(13) . . . . ? C8 C9 C29 C34 -24.1(16) . . . . ? C34 C29 C30 C31 -5.9(15) . . . . ? C9 C29 C30 C31 179.1(16) . . . . ? C29 C30 C31 C32 10(3) . . . . ? C30 C31 C32 C33 -10(3) . . . . ? C31 C32 C33 C34 6(3) . . . . ? C32 C33 C34 C29 -3(2) . . . . ? C30 C29 C34 C33 2.7(18) . . . . ? C9 C29 C34 C33 177.7(13) . . . . ? C38 O1 C35 C36 -12(2) . . . . ? Yb O1 C35 C36 155.2(14) . . . . ? O1 C35 C36 C37B 30(2) . . . . ? O1 C35 C36 C37A 6(3) . . . . ? C37B C36 C37A C38 -79(4) . . . . ? C35 C36 C37A C38 3(3) . . . . ? C35 C36 C37B C38 -35.3(17) . . . . ? C37A C36 C37B C38 68(3) . . . . ? C36 C37A C38 O1 -10(3) . . . . ? C36 C37A C38 C37B 65(3) . . . . ? C35 O1 C38 C37A 14(2) . . . . ? Yb O1 C38 C37A -153.9(17) . . . . ? C35 O1 C38 C37B -9.8(15) . . . . ? Yb O1 C38 C37B -177.9(7) . . . . ? C36 C37B C38 C37A -83(4) . . . . ? C36 C37B C38 O1 29.4(11) . . . . ? C42 O2 C39 C40 0(8) . . . . ? O2 C39 C40 C41 -13(6) . . . . ? C39 C40 C41 C42 25(8) . . . . ? C39 O2 C42 C41 13(8) . . . . ? C40 C41 C42 O2 -25(9) . . . . ? C46 O3 C43 C44 -15(10) . . . . ? O3 C43 C44 C45 -9(9) . . . . ? C43 C44 C45 C46 32(10) . . . . ? C43 O3 C46 C45 30(8) . . . . ? C44 C45 C46 O3 -41(9) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 29.30 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 7.101 _refine_diff_density_min -4.522 _refine_diff_density_rms 0.245 #============================================================================== data_5b _database_code_depnum_ccdc_archive 'CCDC 638159' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H60 Cl N4 O3 Yb' _chemical_formula_weight 925.47 _chemical_absolute_configuration rmad 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' Yb Yb -0.3850 5.5486 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7575(5) _cell_length_b 15.8985(7) _cell_length_c 15.8618(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.662(5) _cell_angle_gamma 90.00 _cell_volume 2146.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.504 _exptl_crystal_size_mid 0.278 _exptl_crystal_size_min 0.132 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 950 _exptl_absorpt_coefficient_mu 2.285 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6603 _exptl_absorpt_correction_T_max 0.8753 _exptl_absorpt_process_details 'Stoe X-red' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16498 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 29.19 _reflns_number_total 11463 _reflns_number_gt 9968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'diamond 2.1e' _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^)+(0.0722P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(10) _refine_ls_number_reflns 11463 _refine_ls_number_parameters 368 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb Yb 0.658450(19) 0.744116(16) 0.822971(10) 0.02554(5) Uani 1 1 d . . . Cl Cl 0.45055(18) 0.83001(10) 0.87475(10) 0.0420(3) Uani 1 1 d . . . O1 O 0.9087(5) 0.6846(3) 0.8446(3) 0.0416(9) Uani 1 1 d . B . N1 N 0.7902(6) 0.8694(3) 0.8071(3) 0.0355(10) Uani 1 1 d . . . N2 N 0.6206(5) 0.7827(3) 0.6813(3) 0.0261(8) Uani 1 1 d . . . N3 N 0.5478(5) 0.6331(3) 0.7394(3) 0.0245(7) Uani 1 1 d . . . N4 N 0.6082(5) 0.6313(3) 0.9071(3) 0.0315(9) Uani 1 1 d . . . C1 C 0.7751(6) 0.9036(3) 0.7306(4) 0.0339(11) Uani 1 1 d . . . C2 C 0.8474(12) 0.9823(5) 0.7200(7) 0.068(2) Uani 1 1 d . . . H2 H 0.8991 1.0090 0.7726 0.082 Uiso 1 1 calc R . . C3 C 0.8543(11) 1.0274(5) 0.6423(8) 0.074(3) Uani 1 1 d . . . H3 H 0.9201 1.0756 0.6526 0.089 Uiso 1 1 calc R . . C4 C 0.7866(8) 1.0148(5) 0.5586(5) 0.0453(14) Uiso 1 1 d . . . H4 H 0.8025 1.0563 0.5185 0.054 Uiso 1 1 calc R . . C5 C 0.6977(11) 0.9482(4) 0.5270(5) 0.0576(19) Uani 1 1 d . . . H5 H 0.6654 0.9457 0.4655 0.069 Uiso 1 1 calc R . . C6 C 0.6454(9) 0.8817(4) 0.5704(5) 0.0454(14) Uani 1 1 d . . . H6 H 0.5720 0.8465 0.5327 0.055 Uiso 1 1 calc R . . C7 C 0.6763(6) 0.8552(3) 0.6566(4) 0.0299(10) Uani 1 1 d . . . C8 C 0.5253(6) 0.7293(3) 0.6148(3) 0.0259(12) Uani 1 1 d . . . H8 H 0.5717 0.7324 0.5631 0.031 Uiso 1 1 calc R . . C9 C 0.5389(6) 0.6366(3) 0.6457(3) 0.0253(9) Uani 1 1 d . . . H9 H 0.4418 0.6062 0.6148 0.030 Uiso 1 1 calc R . . C10 C 0.4904(6) 0.5659(3) 0.7730(3) 0.0269(9) Uani 1 1 d . . . C11 C 0.3854(7) 0.5077(4) 0.7226(4) 0.0384(12) Uani 1 1 d . . . H11 H 0.3513 0.5248 0.6638 0.046 Uiso 1 1 calc R . . C12 C 0.3205(10) 0.4320(5) 0.7382(5) 0.0484(16) Uani 1 1 d . . . H12 H 0.2480 0.4073 0.6905 0.058 Uiso 1 1 calc R . . C13 C 0.3499(10) 0.3867(4) 0.8175(5) 0.0548(18) Uani 1 1 d . . . H13 H 0.3023 0.3329 0.8166 0.066 Uiso 1 1 calc R . . C14 C 0.4409(8) 0.4138(4) 0.8951(5) 0.0472(15) Uani 1 1 d . . . H14 H 0.4532 0.3741 0.9410 0.057 Uiso 1 1 calc R . . C15 C 0.5174(7) 0.4890(4) 0.9178(4) 0.0391(12) Uani 1 1 d . . . H15 H 0.5676 0.4928 0.9777 0.047 Uiso 1 1 calc R . . C16 C 0.5368(6) 0.5624(3) 0.8695(3) 0.0286(9) Uani 1 1 d . . . C17 C 0.6537(8) 0.6374(4) 1.0021(4) 0.0410(13) Uani 1 1 d . . . H17 H 0.7049 0.5834 1.0257 0.049 Uiso 1 1 calc R . . C18 C 0.7709(10) 0.7076(6) 1.0289(5) 0.0576(18) Uani 1 1 d . . . H18A H 0.7162 0.7618 1.0197 0.086 Uiso 1 1 calc R . . H18B H 0.8493 0.7052 0.9939 0.086 Uiso 1 1 calc R . . H18C H 0.8232 0.7014 1.0904 0.086 Uiso 1 1 calc R . . C19 C 0.5084(9) 0.6514(6) 1.0400(4) 0.0543(17) Uani 1 1 d . . . H19A H 0.4404 0.6018 1.0286 0.081 Uiso 1 1 calc R . . H19B H 0.4502 0.7008 1.0126 0.081 Uiso 1 1 calc R . . H19C H 0.5427 0.6606 1.1027 0.081 Uiso 1 1 calc R . . C20 C 0.8733(10) 0.9119(5) 0.8887(5) 0.0563(18) Uani 1 1 d . . . H20 H 0.8763 0.8680 0.9342 0.068 Uiso 1 1 calc R . . C21 C 1.0446(17) 0.9319(10) 0.8963(10) 0.108(4) Uiso 1 1 d . . . H21A H 1.0656 0.9902 0.9157 0.162 Uiso 1 1 calc R . . H21B H 1.0694 0.9246 0.8397 0.162 Uiso 1 1 calc R . . H21C H 1.1099 0.8939 0.9386 0.162 Uiso 1 1 calc R . . C22 C 0.7784(15) 0.9818(8) 0.9157(9) 0.092(3) Uiso 1 1 d . . . H22A H 0.6692 0.9635 0.9082 0.138 Uiso 1 1 calc R . . H22B H 0.7820 1.0315 0.8797 0.138 Uiso 1 1 calc R . . H22C H 0.8225 0.9959 0.9768 0.138 Uiso 1 1 calc R . . C23 C 0.3532(3) 0.75758(15) 0.58489(17) 0.0260(10) Uani 1 1 d G . . C24 C 0.2766(4) 0.8024(2) 0.63789(19) 0.0426(13) Uani 1 1 d G . . H24 H 0.3327 0.8201 0.6939 0.051 Uiso 1 1 calc R . . C25 C 0.1179(4) 0.8215(2) 0.6090(2) 0.0528(17) Uani 1 1 d G . . H25 H 0.0656 0.8521 0.6452 0.063 Uiso 1 1 calc R . . C26 C 0.0359(3) 0.7957(2) 0.5271(2) 0.0444(13) Uiso 1 1 d G . . H26 H -0.0726 0.8087 0.5073 0.053 Uiso 1 1 calc R . . C27 C 0.1125(3) 0.7508(3) 0.47407(19) 0.0495(12) Uiso 1 1 d G . . H27 H 0.0564 0.7331 0.4181 0.059 Uiso 1 1 calc R . . C28 C 0.2712(3) 0.7318(2) 0.50297(14) 0.0382(13) Uani 1 1 d G . . H28 H 0.3235 0.7011 0.4667 0.046 Uiso 1 1 calc R . . C29 C 0.6808(4) 0.5915(2) 0.6260(3) 0.0301(10) Uani 1 1 d G . . C30 C 0.6738(5) 0.5052(2) 0.6099(4) 0.069(2) Uiso 1 1 d G . . H30 H 0.5809 0.4745 0.6103 0.082 Uiso 1 1 calc R . . C31 C 0.8069(13) 0.4635(7) 0.5930(7) 0.071(3) Uiso 1 1 d . . . H31 H 0.8070 0.4038 0.5903 0.085 Uiso 1 1 calc R . . C32 C 0.9317(10) 0.5054(5) 0.5808(5) 0.0564(17) Uiso 1 1 d . . . H32 H 1.0138 0.4766 0.5631 0.068 Uiso 1 1 calc R . . C33 C 0.9402(9) 0.5911(5) 0.5943(5) 0.0497(15) Uiso 1 1 d . . . H33 H 1.0309 0.6210 0.5883 0.060 Uiso 1 1 calc R . . C34 C 0.8155(8) 0.6346(4) 0.6168(4) 0.0449(13) Uiso 1 1 d . . . H34 H 0.8227 0.6937 0.6258 0.054 Uiso 1 1 calc R . . C35 C 1.0473(10) 0.7231(6) 0.8271(6) 0.069(2) Uiso 1 1 d . B . H35A H 1.0974 0.7603 0.8758 0.083 Uiso 1 1 calc R . . H35B H 1.0181 0.7577 0.7737 0.083 Uiso 1 1 calc R . . C36 C 1.1583(10) 0.6563(6) 0.8159(5) 0.0600(19) Uiso 1 1 d . . . H36A H 1.2617 0.6644 0.8568 0.072 Uiso 1 1 calc R A 1 H36B H 1.1732 0.6564 0.7559 0.072 Uiso 1 1 calc R A 1 C37A C 1.0807(15) 0.5712(9) 0.8356(9) 0.041(3) Uiso 0.50 1 d P B 1 H37A H 1.0560 0.5350 0.7833 0.050 Uiso 0.50 1 calc PR B 1 H37B H 1.1522 0.5402 0.8830 0.050 Uiso 0.50 1 calc PR B 1 C37B C 1.1166(8) 0.5893(4) 0.8687(5) 0.044(3) Uiso 0.50 1 d P B 2 H37C H 1.1739 0.5963 0.9300 0.053 Uiso 0.50 1 calc PR B 2 H37D H 1.1442 0.5339 0.8481 0.053 Uiso 0.50 1 calc PR B 2 C38 C 0.9399(8) 0.5949(4) 0.8605(5) 0.060(2) Uani 1 1 d R . . H38A H 0.8487 0.5620 0.8279 0.072 Uiso 1 1 d R . . H38B H 0.9540 0.5826 0.9233 0.072 Uiso 1 1 d R . . O2 O 0.2424(19) 1.1279(12) 0.7258(11) 0.170(5) Uiso 1 1 d . . . C39 C 0.296(3) 1.1680(17) 0.6598(16) 0.165(8) Uiso 1 1 d . . . H39A H 0.3498 1.2213 0.6814 0.198 Uiso 1 1 calc R . . H39B H 0.2071 1.1809 0.6102 0.198 Uiso 1 1 calc R . . C40 C 0.409(3) 1.1087(15) 0.6324(15) 0.152(7) Uiso 1 1 d . . . H40A H 0.3838 1.1009 0.5687 0.183 Uiso 1 1 calc R . . H40B H 0.5191 1.1274 0.6530 0.183 Uiso 1 1 calc R . . C41 C 0.378(4) 1.036(2) 0.675(2) 0.224(14) Uiso 1 1 d . . . H41A H 0.4784 1.0075 0.7004 0.269 Uiso 1 1 calc R . . H41B H 0.3126 0.9979 0.6325 0.269 Uiso 1 1 calc R . . C42 C 0.294(4) 1.053(2) 0.747(2) 0.200(12) Uiso 1 1 d . . . H42A H 0.2076 1.0124 0.7454 0.241 Uiso 1 1 calc R . . H42B H 0.3675 1.0514 0.8051 0.241 Uiso 1 1 calc R . . O3 O 0.924(3) 1.2824(16) 0.7710(17) 0.257(11) Uiso 1 1 d . . . C43 C 0.837(5) 1.356(3) 0.808(3) 0.274(18) Uiso 1 1 d . . . H43A H 0.8828 1.4122 0.8018 0.329 Uiso 1 1 calc R . . H43B H 0.7221 1.3567 0.7827 0.329 Uiso 1 1 calc R . . C44 C 0.875(6) 1.327(3) 0.886(3) 0.32(2) Uiso 1 1 d . . . H44A H 0.8286 1.3581 0.9276 0.379 Uiso 1 1 calc R . . H44B H 0.9892 1.3180 0.9084 0.379 Uiso 1 1 calc R . . C45 C 0.776(4) 1.241(3) 0.8448(19) 0.238(12) Uiso 1 1 d . . . H45A H 0.8189 1.1904 0.8793 0.285 Uiso 1 1 calc R . . H45B H 0.6632 1.2461 0.8452 0.285 Uiso 1 1 calc R . . C46 C 0.793(5) 1.234(4) 0.763(3) 0.32(2) Uiso 1 1 d . . . H46A H 0.7021 1.2572 0.7198 0.381 Uiso 1 1 calc R . . H46B H 0.8117 1.1750 0.7472 0.381 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb 0.02560(8) 0.02433(8) 0.02880(8) -0.00147(16) 0.01061(5) -0.00007(17) Cl 0.0399(7) 0.0435(7) 0.0471(7) -0.0082(6) 0.0195(6) 0.0073(6) O1 0.0284(19) 0.042(2) 0.056(2) 0.0079(19) 0.0140(17) 0.0069(16) N1 0.034(2) 0.028(2) 0.046(3) -0.0100(19) 0.0140(19) -0.0051(18) N2 0.0263(19) 0.0212(18) 0.033(2) 0.0006(16) 0.0127(16) -0.0002(15) N3 0.0265(19) 0.0222(18) 0.0279(19) 0.0002(15) 0.0126(15) 0.0002(15) N4 0.031(2) 0.035(2) 0.031(2) 0.0042(17) 0.0130(17) 0.0000(17) C1 0.030(2) 0.023(2) 0.051(3) -0.004(2) 0.016(2) -0.0013(19) C2 0.084(6) 0.040(4) 0.076(6) -0.002(4) 0.009(5) -0.026(4) C3 0.075(6) 0.033(4) 0.119(8) 0.019(5) 0.031(6) -0.026(4) C5 0.089(6) 0.037(3) 0.056(4) 0.013(3) 0.037(4) 0.002(3) C6 0.057(4) 0.034(3) 0.050(4) 0.009(3) 0.023(3) -0.006(3) C7 0.031(2) 0.022(2) 0.042(3) 0.002(2) 0.019(2) 0.0043(18) C8 0.030(2) 0.021(4) 0.0285(19) -0.0004(15) 0.0123(15) 0.0021(16) C9 0.028(2) 0.025(2) 0.026(2) 0.0007(17) 0.0120(17) 0.0002(17) C10 0.024(2) 0.028(2) 0.030(2) 0.0065(18) 0.0085(17) 0.0027(18) C11 0.045(3) 0.034(3) 0.038(3) 0.000(2) 0.013(2) -0.012(2) C12 0.060(4) 0.041(3) 0.050(4) -0.003(3) 0.023(3) -0.023(3) C13 0.077(5) 0.032(3) 0.065(4) 0.010(3) 0.036(4) -0.010(3) C14 0.052(4) 0.038(3) 0.057(4) 0.014(3) 0.023(3) -0.001(3) C15 0.043(3) 0.038(3) 0.037(3) 0.010(2) 0.013(2) 0.001(2) C16 0.026(2) 0.030(2) 0.032(2) 0.0048(19) 0.0128(18) 0.0036(18) C17 0.047(3) 0.048(3) 0.029(3) 0.003(2) 0.009(2) 0.002(3) C18 0.057(4) 0.066(4) 0.049(4) -0.010(3) 0.009(3) -0.015(3) C19 0.061(4) 0.074(5) 0.035(3) -0.002(3) 0.027(3) -0.001(4) C20 0.053(4) 0.058(4) 0.057(4) -0.023(4) 0.011(3) -0.015(3) C23 0.031(2) 0.010(3) 0.038(2) 0.0045(15) 0.0113(16) 0.0050(14) C24 0.042(3) 0.043(3) 0.045(3) 0.001(3) 0.015(3) 0.008(3) C25 0.044(3) 0.051(4) 0.069(4) 0.003(3) 0.026(3) 0.017(3) C28 0.037(2) 0.034(4) 0.042(2) 0.002(2) 0.0046(19) -0.004(2) C29 0.036(3) 0.031(3) 0.026(2) -0.002(2) 0.013(2) 0.004(2) C38 0.042(4) 0.053(4) 0.088(6) 0.023(4) 0.022(4) 0.025(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 Yb N2 2.277(4) . ? Yb N3 2.281(4) . ? Yb O1 2.337(4) . ? Yb N4 2.339(4) . ? Yb N1 2.345(5) . ? Yb Cl 2.5613(14) . ? Yb C10 3.205(5) . ? O1 C35 1.445(10) . ? O1 C38 1.462(8) . ? N1 C1 1.309(8) . ? N1 C20 1.489(8) . ? N2 C7 1.345(7) . ? N2 C8 1.454(6) . ? N3 C10 1.344(6) . ? N3 C9 1.472(6) . ? N4 C16 1.330(7) . ? N4 C17 1.467(7) . ? C1 C2 1.430(9) . ? C1 C7 1.496(8) . ? C2 C3 1.440(14) . ? C3 C4 1.335(14) . ? C4 C5 1.340(11) . ? C5 C6 1.397(9) . ? C6 C7 1.394(9) . ? C8 C23 1.536(5) . ? C8 C9 1.548(6) . ? C9 C29 1.529(5) . ? C10 C11 1.413(8) . ? C10 C16 1.488(7) . ? C11 C12 1.378(8) . ? C12 C13 1.419(10) . ? C13 C14 1.369(11) . ? C14 C15 1.376(10) . ? C15 C16 1.429(7) . ? C17 C18 1.507(10) . ? C17 C19 1.546(9) . ? C20 C22 1.508(15) . ? C20 C21 1.510(16) . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C29 C30 1.3950 . ? C29 C34 1.401(8) . ? C30 C31 1.420(11) . ? C31 C32 1.333(13) . ? C32 C33 1.378(11) . ? C33 C34 1.409(10) . ? C35 C36 1.479(12) . ? C36 C37B 1.454(12) . ? C36 C37A 1.578(16) . ? C37A C38 1.432(15) . ? C37B C38 1.5246 . ? O2 C42 1.29(3) . ? O2 C39 1.40(3) . ? C39 C40 1.50(3) . ? C40 C41 1.40(4) . ? C41 C42 1.51(4) . ? O3 C46 1.36(5) . ? O3 C43 1.58(4) . ? C43 C44 1.29(5) . ? C44 C45 1.67(6) . ? C45 C46 1.35(4) . ? 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 N2 Yb N3 72.09(15) . . ? N2 Yb O1 99.60(16) . . ? N3 Yb O1 91.54(16) . . ? N2 Yb N4 140.08(16) . . ? N3 Yb N4 68.10(15) . . ? O1 Yb N4 84.38(16) . . ? N2 Yb N1 68.03(17) . . ? N3 Yb N1 138.36(16) . . ? O1 Yb N1 83.78(17) . . ? N4 Yb N1 151.18(18) . . ? N2 Yb Cl 102.95(11) . . ? N3 Yb Cl 111.22(11) . . ? O1 Yb Cl 151.88(13) . . ? N4 Yb Cl 88.96(12) . . ? N1 Yb Cl 89.23(12) . . ? N2 Yb C10 92.48(14) . . ? N3 Yb C10 20.79(13) . . ? O1 Yb C10 92.18(14) . . ? N4 Yb C10 47.61(15) . . ? N1 Yb C10 158.97(15) . . ? Cl Yb C10 103.35(10) . . ? C35 O1 C38 108.4(5) . . ? C35 O1 Yb 127.0(4) . . ? C38 O1 Yb 123.4(4) . . ? C1 N1 C20 122.6(6) . . ? C1 N1 Yb 120.5(4) . . ? C20 N1 Yb 116.4(5) . . ? C7 N2 C8 118.4(4) . . ? C7 N2 Yb 122.7(4) . . ? C8 N2 Yb 118.8(3) . . ? C10 N3 C9 119.7(4) . . ? C10 N3 Yb 122.2(3) . . ? C9 N3 Yb 118.1(3) . . ? C16 N4 C17 120.0(5) . . ? C16 N4 Yb 120.4(3) . . ? C17 N4 Yb 119.5(4) . . ? N1 C1 C2 121.5(6) . . ? N1 C1 C7 115.3(5) . . ? C2 C1 C7 123.2(6) . . ? C1 C2 C3 130.2(8) . . ? C4 C3 C2 132.7(7) . . ? C3 C4 C5 125.0(7) . . ? C4 C5 C6 130.0(8) . . ? C7 C6 C5 134.6(7) . . ? N2 C7 C6 123.0(5) . . ? N2 C7 C1 113.2(5) . . ? C6 C7 C1 123.8(5) . . ? N2 C8 C23 114.0(3) . . ? N2 C8 C9 109.8(4) . . ? C23 C8 C9 111.9(3) . . ? N3 C9 C29 109.7(4) . . ? N3 C9 C8 109.7(4) . . ? C29 C9 C8 112.8(4) . . ? N3 C10 C11 123.4(5) . . ? N3 C10 C16 113.6(4) . . ? C11 C10 C16 122.8(5) . . ? N3 C10 Yb 37.1(2) . . ? C11 C10 Yb 156.8(4) . . ? C16 C10 Yb 77.3(3) . . ? C12 C11 C10 135.3(6) . . ? C11 C12 C13 127.4(7) . . ? C14 C13 C12 125.6(6) . . ? C13 C14 C15 130.8(6) . . ? C14 C15 C16 133.0(6) . . ? N4 C16 C15 122.3(5) . . ? N4 C16 C10 114.6(4) . . ? C15 C16 C10 122.9(5) . . ? N4 C17 C18 109.9(5) . . ? N4 C17 C19 111.0(5) . . ? C18 C17 C19 110.6(6) . . ? N1 C20 C22 113.1(8) . . ? N1 C20 C21 115.9(9) . . ? C22 C20 C21 115.2(9) . . ? C24 C23 C28 120.0 . . ? C24 C23 C8 122.8(2) . . ? C28 C23 C8 117.1(2) . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? C30 C29 C34 117.6(3) . . ? C30 C29 C9 119.8(2) . . ? C34 C29 C9 122.4(4) . . ? C29 C30 C31 119.4(5) . . ? C32 C31 C30 122.2(9) . . ? C31 C32 C33 119.2(9) . . ? C32 C33 C34 120.5(7) . . ? C29 C34 C33 120.5(6) . . ? O1 C35 C36 108.9(7) . . ? C37B C36 C35 101.2(7) . . ? C37B C36 C37A 23.0(5) . . ? C35 C36 C37A 105.4(8) . . ? C38 C37A C36 105.6(9) . . ? C36 C37B C38 107.3(4) . . ? C37A C38 O1 110.3(8) . . ? C37A C38 C37B 23.8(6) . . ? O1 C38 C37B 102.5(3) . . ? C42 O2 C39 117(2) . . ? O2 C39 C40 107(2) . . ? C41 C40 C39 99(2) . . ? C40 C41 C42 114(3) . . ? O2 C42 C41 99(3) . . ? C46 O3 C43 89(3) . . ? C44 C43 O3 93(4) . . ? C43 C44 C45 86(4) . . ? C46 C45 C44 106(5) . . ? C45 C46 O3 98(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Yb O1 C35 53.2(6) . . . . ? N3 Yb O1 C35 125.3(6) . . . . ? N4 Yb O1 C35 -166.9(6) . . . . ? N1 Yb O1 C35 -13.2(6) . . . . ? Cl Yb O1 C35 -89.8(6) . . . . ? C10 Yb O1 C35 146.1(6) . . . . ? N2 Yb O1 C38 -112.8(5) . . . . ? N3 Yb O1 C38 -40.7(5) . . . . ? N4 Yb O1 C38 27.1(5) . . . . ? N1 Yb O1 C38 -179.3(5) . . . . ? Cl Yb O1 C38 104.2(5) . . . . ? C10 Yb O1 C38 -20.0(5) . . . . ? N2 Yb N1 C1 3.7(4) . . . . ? N3 Yb N1 C1 21.4(5) . . . . ? O1 Yb N1 C1 106.7(4) . . . . ? N4 Yb N1 C1 172.9(4) . . . . ? Cl Yb N1 C1 -100.6(4) . . . . ? C10 Yb N1 C1 26.9(7) . . . . ? N2 Yb N1 C20 176.3(5) . . . . ? N3 Yb N1 C20 -166.0(4) . . . . ? O1 Yb N1 C20 -80.7(5) . . . . ? N4 Yb N1 C20 -14.4(7) . . . . ? Cl Yb N1 C20 72.0(5) . . . . ? C10 Yb N1 C20 -160.5(5) . . . . ? N3 Yb N2 C7 -172.1(4) . . . . ? O1 Yb N2 C7 -83.6(4) . . . . ? N4 Yb N2 C7 -176.3(3) . . . . ? N1 Yb N2 C7 -4.4(4) . . . . ? Cl Yb N2 C7 79.4(4) . . . . ? C10 Yb N2 C7 -176.3(4) . . . . ? N3 Yb N2 C8 11.3(3) . . . . ? O1 Yb N2 C8 99.8(3) . . . . ? N4 Yb N2 C8 7.1(5) . . . . ? N1 Yb N2 C8 179.1(4) . . . . ? Cl Yb N2 C8 -97.1(3) . . . . ? C10 Yb N2 C8 7.2(3) . . . . ? N2 Yb N3 C10 -168.3(4) . . . . ? O1 Yb N3 C10 92.1(4) . . . . ? N4 Yb N3 C10 8.8(4) . . . . ? N1 Yb N3 C10 174.4(3) . . . . ? Cl Yb N3 C10 -71.0(4) . . . . ? N2 Yb N3 C9 11.3(3) . . . . ? O1 Yb N3 C9 -88.3(3) . . . . ? N4 Yb N3 C9 -171.6(4) . . . . ? N1 Yb N3 C9 -6.0(4) . . . . ? Cl Yb N3 C9 108.6(3) . . . . ? C10 Yb N3 C9 179.6(6) . . . . ? N2 Yb N4 C16 1.1(5) . . . . ? N3 Yb N4 C16 -3.2(4) . . . . ? O1 Yb N4 C16 -97.1(4) . . . . ? N1 Yb N4 C16 -163.3(4) . . . . ? Cl Yb N4 C16 110.2(4) . . . . ? C10 Yb N4 C16 1.0(3) . . . . ? N2 Yb N4 C17 -178.0(4) . . . . ? N3 Yb N4 C17 177.7(4) . . . . ? O1 Yb N4 C17 83.8(4) . . . . ? N1 Yb N4 C17 17.7(6) . . . . ? Cl Yb N4 C17 -68.9(4) . . . . ? C10 Yb N4 C17 -178.1(5) . . . . ? C20 N1 C1 C2 4.4(10) . . . . ? Yb N1 C1 C2 176.6(6) . . . . ? C20 N1 C1 C7 -174.9(6) . . . . ? Yb N1 C1 C7 -2.8(6) . . . . ? N1 C1 C2 C3 175.3(10) . . . . ? C7 C1 C2 C3 -5.4(15) . . . . ? C1 C2 C3 C4 7(2) . . . . ? C2 C3 C4 C5 -4.9(18) . . . . ? C3 C4 C5 C6 5.3(15) . . . . ? C4 C5 C6 C7 -8.1(16) . . . . ? C8 N2 C7 C6 0.7(8) . . . . ? Yb N2 C7 C6 -175.9(4) . . . . ? C8 N2 C7 C1 -178.9(4) . . . . ? Yb N2 C7 C1 4.5(6) . . . . ? C5 C6 C7 N2 -173.3(8) . . . . ? C5 C6 C7 C1 6.2(12) . . . . ? N1 C1 C7 N2 -1.0(7) . . . . ? C2 C1 C7 N2 179.7(7) . . . . ? N1 C1 C7 C6 179.5(6) . . . . ? C2 C1 C7 C6 0.1(10) . . . . ? C7 N2 C8 C23 -80.1(5) . . . . ? Yb N2 C8 C23 96.6(4) . . . . ? C7 N2 C8 C9 153.4(4) . . . . ? Yb N2 C8 C9 -29.9(5) . . . . ? C10 N3 C9 C29 -85.7(5) . . . . ? Yb N3 C9 C29 94.7(4) . . . . ? C10 N3 C9 C8 149.9(4) . . . . ? Yb N3 C9 C8 -29.7(5) . . . . ? N2 C8 C9 N3 36.9(5) . . . . ? C23 C8 C9 N3 -90.7(4) . . . . ? N2 C8 C9 C29 -85.7(4) . . . . ? C23 C8 C9 C29 146.6(4) . . . . ? C9 N3 C10 C11 -17.2(7) . . . . ? Yb N3 C10 C11 162.4(4) . . . . ? C9 N3 C10 C16 167.8(4) . . . . ? Yb N3 C10 C16 -12.6(6) . . . . ? C9 N3 C10 Yb -179.6(6) . . . . ? N2 Yb C10 N3 11.1(4) . . . . ? O1 Yb C10 N3 -88.6(4) . . . . ? N4 Yb C10 N3 -169.0(4) . . . . ? N1 Yb C10 N3 -10.3(6) . . . . ? Cl Yb C10 N3 115.0(4) . . . . ? N2 Yb C10 C11 -28.7(10) . . . . ? N3 Yb C10 C11 -39.8(9) . . . . ? O1 Yb C10 C11 -128.4(10) . . . . ? N4 Yb C10 C11 151.2(10) . . . . ? N1 Yb C10 C11 -50.2(11) . . . . ? Cl Yb C10 C11 75.2(10) . . . . ? N2 Yb C10 C16 179.3(3) . . . . ? N3 Yb C10 C16 168.2(5) . . . . ? O1 Yb C10 C16 79.6(3) . . . . ? N4 Yb C10 C16 -0.8(3) . . . . ? N1 Yb C10 C16 157.8(4) . . . . ? Cl Yb C10 C16 -76.8(3) . . . . ? N3 C10 C11 C12 173.5(7) . . . . ? C16 C10 C11 C12 -12.0(11) . . . . ? Yb C10 C11 C12 -159.0(7) . . . . ? C10 C11 C12 C13 -2.4(15) . . . . ? C11 C12 C13 C14 5.0(14) . . . . ? C12 C13 C14 C15 3.6(14) . . . . ? C13 C14 C15 C16 -3.8(13) . . . . ? C17 N4 C16 C15 -7.2(8) . . . . ? Yb N4 C16 C15 173.8(4) . . . . ? C17 N4 C16 C10 177.3(5) . . . . ? Yb N4 C16 C10 -1.7(6) . . . . ? C14 C15 C16 N4 175.1(7) . . . . ? C14 C15 C16 C10 -9.7(10) . . . . ? N3 C10 C16 N4 8.9(6) . . . . ? C11 C10 C16 N4 -166.1(5) . . . . ? Yb C10 C16 N4 1.1(4) . . . . ? N3 C10 C16 C15 -166.6(5) . . . . ? C11 C10 C16 C15 18.4(8) . . . . ? Yb C10 C16 C15 -174.4(5) . . . . ? C16 N4 C17 C18 163.8(6) . . . . ? Yb N4 C17 C18 -17.1(7) . . . . ? C16 N4 C17 C19 -73.6(7) . . . . ? Yb N4 C17 C19 105.5(6) . . . . ? C1 N1 C20 C22 75.3(10) . . . . ? Yb N1 C20 C22 -97.2(8) . . . . ? C1 N1 C20 C21 -60.9(11) . . . . ? Yb N1 C20 C21 126.6(8) . . . . ? N2 C8 C23 C24 -27.5(4) . . . . ? C9 C8 C23 C24 97.9(3) . . . . ? N2 C8 C23 C28 156.6(3) . . . . ? C9 C8 C23 C28 -78.0(4) . . . . ? C28 C23 C24 C25 0.0 . . . . ? C8 C23 C24 C25 -175.8(2) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C23 0.0 . . . . ? C24 C23 C28 C27 0.0 . . . . ? C8 C23 C28 C27 176.0(2) . . . . ? N3 C9 C29 C30 87.9(4) . . . . ? C8 C9 C29 C30 -149.5(3) . . . . ? N3 C9 C29 C34 -97.1(5) . . . . ? C8 C9 C29 C34 25.5(6) . . . . ? C34 C29 C30 C31 5.7(7) . . . . ? C9 C29 C30 C31 -179.1(7) . . . . ? C29 C30 C31 C32 -8.9(13) . . . . ? C30 C31 C32 C33 7.3(15) . . . . ? C31 C32 C33 C34 -2.9(12) . . . . ? C30 C29 C34 C33 -1.6(7) . . . . ? C9 C29 C34 C33 -176.7(5) . . . . ? C32 C33 C34 C29 0.1(10) . . . . ? C38 O1 C35 C36 10.2(9) . . . . ? Yb O1 C35 C36 -157.6(5) . . . . ? O1 C35 C36 C37B -27.6(9) . . . . ? O1 C35 C36 C37A -4.4(10) . . . . ? C37B C36 C37A C38 79.3(14) . . . . ? C35 C36 C37A C38 -3.1(10) . . . . ? C35 C36 C37B C38 34.5(6) . . . . ? C37A C36 C37B C38 -68.6(13) . . . . ? C36 C37A C38 O1 9.4(10) . . . . ? C36 C37A C38 C37B -65.1(14) . . . . ? C35 O1 C38 C37A -12.5(9) . . . . ? Yb O1 C38 C37A 155.8(6) . . . . ? C35 O1 C38 C37B 11.0(5) . . . . ? Yb O1 C38 C37B 179.3(3) . . . . ? C36 C37B C38 C37A 83.2(16) . . . . ? C36 C37B C38 O1 -29.0(4) . . . . ? C42 O2 C39 C40 -1(3) . . . . ? O2 C39 C40 C41 11(3) . . . . ? C39 C40 C41 C42 -18(3) . . . . ? C39 O2 C42 C41 -9(4) . . . . ? C40 C41 C42 O2 17(4) . . . . ? C46 O3 C43 C44 85(4) . . . . ? O3 C43 C44 C45 -60(3) . . . . ? C43 C44 C45 C46 32(5) . . . . ? C44 C45 C46 O3 21(5) . . . . ? C43 O3 C46 C45 -54(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.19 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.113 _refine_diff_density_min -1.566 _refine_diff_density_rms 0.130 #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 638160' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H68 Cl2 Li N4 O4 Yb' _chemical_formula_weight 1039.96 _chemical_absolute_configuration rmad 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' Li Li -0.0003 0.0001 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_Int_Tables_number 18 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 21.976(4) _cell_length_b 22.716(5) _cell_length_c 9.944(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4964.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.467 _exptl_crystal_size_min 0.300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2140 _exptl_absorpt_coefficient_mu 2.037 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5907 _exptl_absorpt_correction_T_max 0.7816 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31215 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8744 _reflns_number_gt 7829 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0465P)^2^+8.1078P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(10) _refine_ls_number_reflns 8744 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.200 _refine_ls_shift/su_mean 0.008 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 Li1 Li -0.2036(6) 0.2414(4) -0.3363(14) 0.062(3) Uani 1 1 d . . . Yb1 Yb 0.0000 0.0000 0.62412(2) 0.02677(7) Uani 1 2 d S . . Yb2 Yb -0.5000 0.0000 0.34928(2) 0.03980(9) Uani 1 2 d S . . Cl1 Cl -0.03026(8) 0.10013(6) 0.72660(15) 0.0462(3) Uani 1 1 d . . . Cl2 Cl -0.41003(10) -0.06275(7) 0.4304(2) 0.0723(6) Uani 1 1 d . A . N1 N 0.1052(2) 0.02596(19) 0.6654(4) 0.0308(9) Uani 1 1 d . . . N2 N 0.05968(16) -0.0046(2) 0.4355(3) 0.0276(8) Uani 1 1 d . . . N3 N -0.4628(2) 0.04713(18) 0.1630(4) 0.0334(10) Uani 1 1 d . A . N4 N -0.4429(3) 0.0850(2) 0.4045(6) 0.0565(15) Uani 1 1 d . A . C1 C 0.1455(2) 0.0170(2) 0.5685(5) 0.0319(12) Uani 1 1 d . . . C2 C 0.2086(3) 0.0330(3) 0.5802(6) 0.0434(13) Uani 1 1 d . . . H2 H 0.2169 0.0580 0.6545 0.052 Uiso 1 1 calc R . . C3 C 0.2590(3) 0.0194(3) 0.5061(6) 0.0468(17) Uani 1 1 d . . . H3 H 0.2957 0.0364 0.5383 0.056 Uiso 1 1 calc R . . C4 C 0.2657(3) -0.0147(3) 0.3924(6) 0.0480(17) Uani 1 1 d . . . H4 H 0.3059 -0.0229 0.3631 0.058 Uiso 1 1 calc R . . C5 C 0.2189(3) -0.0376(3) 0.3187(6) 0.0453(14) Uani 1 1 d . . . H5 H 0.2307 -0.0602 0.2428 0.054 Uiso 1 1 calc R . . C6 C 0.1558(3) -0.0326(2) 0.3387(5) 0.0361(12) Uani 1 1 d . . . H6 H 0.1323 -0.0497 0.2687 0.043 Uiso 1 1 calc R . . C7 C 0.1202(2) -0.0071(3) 0.4419(4) 0.0288(11) Uani 1 1 d . . . C8 C 0.0305(2) -0.01668(18) 0.3053(5) 0.0266(11) Uani 1 1 d . . . H8 H 0.0567 0.0010 0.2336 0.032 Uiso 1 1 calc R . . C9 C 0.1278(3) 0.0482(3) 0.7960(5) 0.0420(13) Uani 1 1 d . . . H9 H 0.1702 0.0334 0.8091 0.050 Uiso 1 1 calc R . . C10 C 0.1298(3) 0.1161(3) 0.7950(7) 0.0576(18) Uani 1 1 d . . . H10A H 0.1525 0.1296 0.7160 0.086 Uiso 1 1 calc R . . H10B H 0.1499 0.1301 0.8769 0.086 Uiso 1 1 calc R . . H10C H 0.0882 0.1316 0.7915 0.086 Uiso 1 1 calc R . . C11 C 0.0888(3) 0.0245(3) 0.9091(6) 0.0556(17) Uani 1 1 d . . . H11A H 0.0468 0.0381 0.8976 0.083 Uiso 1 1 calc R . . H11B H 0.1047 0.0386 0.9954 0.083 Uiso 1 1 calc R . . H11C H 0.0897 -0.0187 0.9075 0.083 Uiso 1 1 calc R . . C12 C 0.0214(2) -0.0820(2) 0.2704(5) 0.0305(11) Uani 1 1 d . . . C13 C 0.0165(3) -0.0974(3) 0.1384(5) 0.0381(14) Uani 1 1 d . . . H13 H 0.0212 -0.0681 0.0711 0.046 Uiso 1 1 calc R . . C14 C 0.0048(4) -0.1553(2) 0.1002(6) 0.0537(15) Uani 1 1 d . . . H14 H 0.0003 -0.1649 0.0077 0.064 Uiso 1 1 calc R . . C15 C -0.0003(5) -0.1981(2) 0.1955(6) 0.0616(16) Uani 1 1 d . . . H15 H -0.0093 -0.2375 0.1708 0.074 Uiso 1 1 calc R . . C16 C 0.0081(5) -0.1829(2) 0.3302(6) 0.064(2) Uani 1 1 d . . . H16 H 0.0070 -0.2127 0.3971 0.077 Uiso 1 1 calc R . . C17 C 0.0179(3) -0.1258(2) 0.3674(6) 0.052(2) Uani 1 1 d . . . H17 H 0.0224 -0.1160 0.4597 0.062 Uiso 1 1 calc R . . C18 C -0.4192(4) 0.1190(3) 0.3098(8) 0.0590(19) Uani 1 1 d . . . C19 C -0.3888(5) 0.1715(4) 0.3437(11) 0.091(3) Uiso 1 1 d . A . H19 H -0.3879 0.1810 0.4368 0.110 Uiso 1 1 calc R . . C20 C -0.3584(7) 0.2135(6) 0.2543(16) 0.119(5) Uiso 1 1 d . . . H20 H -0.3367 0.2435 0.3003 0.142 Uiso 1 1 calc R A . C21 C -0.3554(5) 0.2176(5) 0.1210(12) 0.101(3) Uiso 1 1 d . A . H21 H -0.3385 0.2526 0.0845 0.121 Uiso 1 1 calc R . . C22 C -0.3744(4) 0.1764(4) 0.0341(10) 0.079(2) Uiso 1 1 d . . . H22 H -0.3656 0.1848 -0.0574 0.095 Uiso 1 1 calc R A . C23 C -0.4047(4) 0.1237(3) 0.0547(8) 0.0607(18) Uiso 1 1 d . A . H23 H -0.4099 0.1011 -0.0249 0.073 Uiso 1 1 calc R . . C24 C -0.4292(3) 0.0970(2) 0.1697(6) 0.0402(13) Uani 1 1 d . A . C25 C -0.4708(3) 0.0183(2) 0.0321(5) 0.0313(12) Uani 1 1 d . . . H25 H -0.4766 0.0503 -0.0358 0.038 Uiso 1 1 calc R A . C26A C -0.4522(6) 0.0911(5) 0.5619(12) 0.041(3) Uiso 0.50 1 d P A 1 H26A H -0.4913 0.0688 0.5552 0.049 Uiso 0.50 1 calc PR A 1 C27A C -0.4339(6) 0.0573(6) 0.6279(13) 0.048(3) Uiso 0.50 1 d P A 1 H27A H -0.4166 0.0758 0.7083 0.071 Uiso 0.50 1 calc PR A 1 H27B H -0.4020 0.0354 0.5805 0.071 Uiso 0.50 1 calc PR A 1 H27C H -0.4665 0.0302 0.6542 0.071 Uiso 0.50 1 calc PR A 1 C28A C -0.4867(6) 0.1452(5) 0.6048(12) 0.043(3) Uiso 0.50 1 d P A 1 H28A H -0.5277 0.1443 0.5661 0.064 Uiso 0.50 1 calc PR A 1 H28B H -0.4652 0.1804 0.5730 0.064 Uiso 0.50 1 calc PR A 1 H28C H -0.4895 0.1462 0.7031 0.064 Uiso 0.50 1 calc PR A 1 C26B C -0.4227(7) 0.1074(6) 0.5319(13) 0.046(3) Uiso 0.50 1 d P A 2 H26B H -0.3898 0.1322 0.4917 0.055 Uiso 0.50 1 calc PR A 2 C27B C -0.3880(7) 0.0853(6) 0.6219(15) 0.059(4) Uiso 0.50 1 d P A 2 H27D H -0.3853 0.0426 0.6090 0.088 Uiso 0.50 1 calc PR A 2 H27E H -0.4049 0.0936 0.7111 0.088 Uiso 0.50 1 calc PR A 2 H27F H -0.3474 0.1027 0.6147 0.088 Uiso 0.50 1 calc PR A 2 C28B C -0.4619(8) 0.1592(7) 0.5698(17) 0.060(4) Uiso 0.50 1 d P A 2 H28D H -0.4513 0.1723 0.6608 0.090 Uiso 0.50 1 calc PR A 2 H28E H -0.5048 0.1475 0.5674 0.090 Uiso 0.50 1 calc PR A 2 H28F H -0.4550 0.1914 0.5061 0.090 Uiso 0.50 1 calc PR A 2 C29 C -0.4145(3) -0.0162(2) -0.0103(5) 0.0359(13) Uani 1 1 d . A . C30 C -0.3633(3) -0.0207(2) 0.0680(6) 0.0377(13) Uani 1 1 d . . . H30 H -0.3629 -0.0030 0.1545 0.045 Uiso 1 1 calc R A . C31 C -0.3113(3) -0.0510(3) 0.0231(7) 0.0464(15) Uani 1 1 d . A . H31 H -0.2763 -0.0538 0.0788 0.056 Uiso 1 1 calc R . . C32 C -0.3116(3) -0.0766(2) -0.1029(7) 0.0491(15) Uani 1 1 d . . . H32 H -0.2768 -0.0973 -0.1344 0.059 Uiso 1 1 calc R A . C33 C -0.3628(3) -0.0721(3) -0.1827(7) 0.0539(17) Uani 1 1 d . A . H33 H -0.3634 -0.0900 -0.2689 0.065 Uiso 1 1 calc R . . C34 C -0.4121(3) -0.0419(3) -0.1382(6) 0.0441(14) Uani 1 1 d . . . H34 H -0.4464 -0.0380 -0.1959 0.053 Uiso 1 1 calc R A . C35 C -0.1297(5) 0.3234(4) -0.1606(10) 0.091(3) Uiso 1 1 d . . . H35A H -0.1614 0.3171 -0.0914 0.109 Uiso 1 1 calc R . . H35B H -0.1351 0.3632 -0.1994 0.109 Uiso 1 1 calc R . . C36 C -0.0690(7) 0.3174(6) -0.1019(15) 0.131(4) Uiso 1 1 d . . . H36A H -0.0472 0.3555 -0.1052 0.157 Uiso 1 1 calc R . . H36B H -0.0720 0.3048 -0.0068 0.157 Uiso 1 1 calc R . . C37 C -0.0367(6) 0.2734(5) -0.1802(13) 0.119(4) Uiso 1 1 d . . . H37A H -0.0313 0.2368 -0.1275 0.142 Uiso 1 1 calc R . . H37B H 0.0039 0.2882 -0.2074 0.142 Uiso 1 1 calc R . . C38 C -0.0749(4) 0.2627(4) -0.2983(9) 0.081(2) Uiso 1 1 d . . . H38A H -0.0602 0.2862 -0.3757 0.097 Uiso 1 1 calc R . . H38B H -0.0737 0.2205 -0.3233 0.097 Uiso 1 1 calc R . . C39 C -0.2267(6) 0.1124(6) -0.2920(14) 0.131(4) Uiso 1 1 d . . . H39A H -0.1897 0.0898 -0.3153 0.157 Uiso 1 1 calc R . . H39B H -0.2535 0.1141 -0.3720 0.157 Uiso 1 1 calc R . . C40 C -0.2609(5) 0.0830(5) -0.1702(11) 0.099(3) Uiso 1 1 d . . . H40A H -0.3028 0.0982 -0.1592 0.119 Uiso 1 1 calc R . . H40B H -0.2616 0.0395 -0.1768 0.119 Uiso 1 1 calc R . . C41 C -0.2197(5) 0.1039(5) -0.0639(11) 0.101(3) Uiso 1 1 d . . . H41A H -0.1909 0.0724 -0.0378 0.121 Uiso 1 1 calc R . . H41B H -0.2432 0.1158 0.0166 0.121 Uiso 1 1 calc R . . C42 C -0.1851(7) 0.1569(6) -0.1217(13) 0.122(4) Uiso 1 1 d . . . H42A H -0.1895 0.1916 -0.0623 0.146 Uiso 1 1 calc R . . H42B H -0.1413 0.1476 -0.1314 0.146 Uiso 1 1 calc R . . C43 C -0.1797(6) 0.2878(5) -0.6088(13) 0.112(4) Uiso 1 1 d . . . H43A H -0.2155 0.3140 -0.6176 0.134 Uiso 1 1 calc R . . H43B H -0.1460 0.3105 -0.5682 0.134 Uiso 1 1 calc R . . C44 C -0.1626(8) 0.2667(7) -0.7338(17) 0.159(6) Uiso 1 1 d . . . H44A H -0.1184 0.2731 -0.7463 0.191 Uiso 1 1 calc R . . H44B H -0.1843 0.2892 -0.8043 0.191 Uiso 1 1 calc R . . C45 C -0.1762(5) 0.2039(5) -0.7496(11) 0.098(3) Uiso 1 1 d . . . H45A H -0.1411 0.1822 -0.7878 0.118 Uiso 1 1 calc R . . H45B H -0.2124 0.1975 -0.8070 0.118 Uiso 1 1 calc R . . C46 C -0.1887(4) 0.1853(4) -0.5998(9) 0.078(2) Uiso 1 1 d . . . H46A H -0.2266 0.1619 -0.5936 0.093 Uiso 1 1 calc R . . H46B H -0.1546 0.1613 -0.5646 0.093 Uiso 1 1 calc R . . C47 C -0.3470(10) 0.3349(9) -0.403(2) 0.200(8) Uiso 1 1 d . . . H47A H -0.3205 0.3487 -0.4770 0.240 Uiso 1 1 calc R . . H47B H -0.3902 0.3361 -0.4316 0.240 Uiso 1 1 calc R . . C48 C -0.3364(6) 0.3685(5) -0.2741(12) 0.109(3) Uiso 1 1 d . . . H48A H -0.3188 0.4076 -0.2937 0.130 Uiso 1 1 calc R . . H48B H -0.3752 0.3741 -0.2252 0.130 Uiso 1 1 calc R . . C49 C -0.2969(10) 0.3360(9) -0.199(2) 0.207(8) Uiso 1 1 d . . . H49A H -0.3175 0.3186 -0.1194 0.248 Uiso 1 1 calc R . . H49B H -0.2620 0.3600 -0.1681 0.248 Uiso 1 1 calc R . . C50 C -0.3281(10) 0.2735(9) -0.350(2) 0.206(9) Uiso 1 1 d . . . H50A H -0.3563 0.2589 -0.2801 0.247 Uiso 1 1 calc R . . H50B H -0.3252 0.2442 -0.4237 0.247 Uiso 1 1 calc R . . O1 O -0.1338(2) 0.2792(2) -0.2641(7) 0.0674(17) Uani 1 1 d . . . O2 O -0.2118(3) 0.16803(19) -0.2497(5) 0.0656(14) Uani 1 1 d . . . O3 O -0.1944(4) 0.2384(2) -0.5259(6) 0.090(2) Uani 1 1 d . . . O4 O -0.2762(4) 0.2865(3) -0.3022(8) 0.103(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.072(8) 0.032(6) 0.083(8) -0.001(5) -0.001(6) 0.011(5) Yb1 0.02667(13) 0.03122(14) 0.02241(12) 0.000 0.000 -0.0005(2) Yb2 0.0621(2) 0.03078(15) 0.02649(14) 0.000 0.000 0.0073(2) Cl1 0.0566(9) 0.0399(7) 0.0422(7) -0.0116(6) 0.0006(7) 0.0082(7) Cl2 0.0711(13) 0.0462(9) 0.0996(15) 0.0189(9) -0.0522(12) -0.0096(9) N1 0.026(2) 0.040(2) 0.026(2) -0.0058(17) -0.0031(17) -0.0032(18) N2 0.0284(19) 0.032(2) 0.0225(16) -0.001(2) -0.0016(13) -0.003(2) N3 0.034(3) 0.027(2) 0.039(2) -0.0031(18) -0.0023(19) 0.0038(19) N4 0.083(4) 0.038(3) 0.049(3) -0.014(2) -0.025(3) 0.025(3) C1 0.028(3) 0.034(3) 0.034(3) 0.0003(18) 0.000(2) -0.0020(18) C2 0.044(3) 0.056(3) 0.030(3) -0.004(3) -0.001(3) -0.008(3) C3 0.024(3) 0.071(5) 0.046(3) 0.001(3) 0.000(3) -0.010(2) C4 0.028(3) 0.069(5) 0.046(3) 0.000(3) 0.008(2) 0.000(3) C5 0.041(4) 0.051(4) 0.044(3) -0.010(3) 0.008(3) -0.004(3) C6 0.032(3) 0.042(3) 0.035(3) -0.005(2) 0.002(2) 0.002(2) C7 0.029(2) 0.028(3) 0.029(2) 0.001(2) 0.0023(17) 0.002(2) C8 0.030(3) 0.029(3) 0.020(2) -0.0022(16) 0.0000(19) -0.0015(18) C9 0.040(3) 0.055(3) 0.030(3) -0.006(2) -0.004(2) -0.004(3) C10 0.062(5) 0.056(4) 0.054(4) -0.025(3) -0.002(3) -0.018(3) C11 0.052(4) 0.087(5) 0.028(3) -0.007(3) 0.003(3) -0.010(3) C12 0.031(3) 0.030(2) 0.031(2) -0.003(2) -0.0006(19) 0.0000(19) C13 0.044(4) 0.041(3) 0.030(3) -0.003(2) -0.001(2) 0.004(2) C14 0.068(4) 0.049(3) 0.044(3) -0.016(2) -0.013(5) 0.004(4) C15 0.089(5) 0.034(3) 0.062(3) -0.012(2) -0.003(7) -0.014(5) C16 0.107(7) 0.031(3) 0.055(3) 0.005(2) -0.001(5) -0.008(4) C17 0.087(6) 0.036(3) 0.032(3) 0.002(2) -0.001(3) -0.011(3) C18 0.073(5) 0.032(3) 0.073(5) -0.010(3) -0.025(4) 0.011(3) C24 0.037(3) 0.028(3) 0.055(3) -0.001(2) 0.000(3) -0.002(2) C25 0.039(3) 0.031(3) 0.024(2) 0.0022(17) 0.000(2) -0.002(2) C29 0.041(3) 0.035(3) 0.032(3) 0.0045(18) 0.006(2) -0.001(2) C30 0.037(3) 0.032(3) 0.044(3) 0.001(2) -0.001(3) 0.002(2) C31 0.038(4) 0.039(3) 0.062(4) 0.007(3) -0.003(3) -0.001(3) C32 0.049(4) 0.035(3) 0.063(4) 0.007(3) 0.019(3) 0.008(3) C33 0.062(5) 0.057(4) 0.042(3) -0.001(3) 0.018(3) 0.001(3) C34 0.041(3) 0.056(4) 0.036(3) -0.002(2) 0.006(2) 0.006(3) O1 0.053(3) 0.042(2) 0.107(5) -0.032(3) -0.008(3) 0.001(2) O2 0.097(4) 0.036(2) 0.064(3) 0.004(2) 0.001(3) -0.004(2) O3 0.142(6) 0.044(3) 0.085(4) 0.000(3) -0.004(4) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.885(12) . ? Li1 O3 1.898(15) . ? Li1 O1 1.899(15) . ? Li1 O4 1.924(15) . ? Yb1 N2 2.291(3) 2 ? Yb1 N2 2.291(3) . ? Yb1 N1 2.422(4) 2 ? Yb1 N1 2.422(4) . ? Yb1 Cl1 2.5796(14) 2 ? Yb1 Cl1 2.5796(14) . ? Yb1 C7 3.207(5) 2 ? Yb1 C7 3.207(5) . ? Yb2 N3 2.290(4) 2_455 ? Yb2 N3 2.290(4) . ? Yb2 N4 2.367(6) 2_455 ? Yb2 N4 2.367(6) . ? Yb2 Cl2 2.5675(18) . ? Yb2 Cl2 2.5675(18) 2_455 ? Yb2 C26A 3.139(12) 2_455 ? Yb2 C26A 3.139(12) . ? N1 C1 1.324(7) . ? N1 C9 1.479(7) . ? N2 C7 1.333(6) . ? N2 C8 1.470(6) . ? N3 C24 1.354(7) . ? N3 C25 1.468(6) . ? N4 C18 1.324(10) . ? N4 C26B 1.435(13) . ? N4 C26A 1.584(13) . ? C1 C2 1.439(8) . ? C1 C7 1.481(7) . ? C2 C3 1.364(8) . ? C3 C4 1.378(8) . ? C4 C5 1.365(9) . ? C5 C6 1.406(8) . ? C6 C7 1.413(7) . ? C8 C12 1.538(6) . ? C8 C8 1.541(10) 2 ? C9 C11 1.512(8) . ? C9 C10 1.541(9) . ? C12 C13 1.363(7) . ? C12 C17 1.386(7) . ? C13 C14 1.392(8) . ? C14 C15 1.363(8) . ? C15 C16 1.395(8) . ? C16 C17 1.366(8) . ? C18 C19 1.409(12) . ? C18 C24 1.496(9) . ? C19 C20 1.464(16) . ? C20 C21 1.330(16) . ? C21 C22 1.341(13) . ? C22 C23 1.385(11) . ? C23 C24 1.402(9) . ? C25 C29 1.525(8) . ? C25 C25 1.528(11) 2_455 ? C26A C27A 1.088(16) . ? C26A C28A 1.506(16) . ? C26B C27B 1.278(18) . ? C26B C28B 1.506(19) . ? C29 C30 1.373(8) . ? C29 C34 1.400(8) . ? C30 C31 1.406(8) . ? C31 C32 1.382(9) . ? C32 C33 1.380(10) . ? C33 C34 1.358(9) . ? C35 O1 1.441(11) . ? C35 C36 1.463(16) . ? C36 C37 1.452(16) . ? C37 C38 1.464(14) . ? C38 O1 1.391(10) . ? C39 O2 1.371(13) . ? C39 C40 1.574(16) . ? C40 C41 1.472(14) . ? C41 C42 1.535(15) . ? C42 O2 1.424(13) . ? C43 C44 1.383(18) . ? C43 O3 1.428(12) . ? C44 C45 1.467(17) . ? C45 C46 1.572(13) . ? C46 O3 1.419(10) . ? C47 C48 1.51(2) . ? C47 C50 1.55(2) . ? C48 C49 1.36(2) . ? C49 O4 1.59(2) . ? C50 O4 1.27(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 O2 Li1 O3 115.6(6) . . ? O2 Li1 O1 107.7(7) . . ? O3 Li1 O1 107.8(7) . . ? O2 Li1 O4 108.1(7) . . ? O3 Li1 O4 106.4(7) . . ? O1 Li1 O4 111.2(6) . . ? N2 Yb1 N2 70.08(18) 2 . ? N2 Yb1 N1 66.63(13) 2 2 ? N2 Yb1 N1 132.40(14) . 2 ? N2 Yb1 N1 132.40(14) 2 . ? N2 Yb1 N1 66.63(13) . . ? N1 Yb1 N1 160.5(2) 2 . ? N2 Yb1 Cl1 120.74(13) 2 2 ? N2 Yb1 Cl1 97.80(13) . 2 ? N1 Yb1 Cl1 87.96(11) 2 2 ? N1 Yb1 Cl1 84.35(11) . 2 ? N2 Yb1 Cl1 97.80(13) 2 . ? N2 Yb1 Cl1 120.74(13) . . ? N1 Yb1 Cl1 84.35(11) 2 . ? N1 Yb1 Cl1 87.96(11) . . ? Cl1 Yb1 Cl1 133.46(7) 2 . ? N2 Yb1 C7 20.57(12) 2 2 ? N2 Yb1 C7 90.64(12) . 2 ? N1 Yb1 C7 47.28(13) 2 2 ? N1 Yb1 C7 150.45(14) . 2 ? Cl1 Yb1 C7 118.69(11) 2 2 ? Cl1 Yb1 C7 88.07(10) . 2 ? N2 Yb1 C7 90.64(12) 2 . ? N2 Yb1 C7 20.57(12) . . ? N1 Yb1 C7 150.45(14) 2 . ? N1 Yb1 C7 47.28(13) . . ? Cl1 Yb1 C7 88.07(10) 2 . ? Cl1 Yb1 C7 118.69(11) . . ? C7 Yb1 C7 111.20(16) 2 . ? N3 Yb2 N3 72.1(2) 2_455 . ? N3 Yb2 N4 67.49(18) 2_455 2_455 ? N3 Yb2 N4 139.30(18) . 2_455 ? N3 Yb2 N4 139.30(18) 2_455 . ? N3 Yb2 N4 67.49(18) . . ? N4 Yb2 N4 153.2(3) 2_455 . ? N3 Yb2 Cl2 105.64(12) 2_455 . ? N3 Yb2 Cl2 103.81(12) . . ? N4 Yb2 Cl2 83.24(15) 2_455 . ? N4 Yb2 Cl2 88.39(14) . . ? N3 Yb2 Cl2 103.81(12) 2_455 2_455 ? N3 Yb2 Cl2 105.64(12) . 2_455 ? N4 Yb2 Cl2 88.39(14) 2_455 2_455 ? N4 Yb2 Cl2 83.24(15) . 2_455 ? Cl2 Yb2 Cl2 143.37(11) . 2_455 ? N3 Yb2 C26A 96.7(3) 2_455 2_455 ? N3 Yb2 C26A 166.4(2) . 2_455 ? N4 Yb2 C26A 29.4(3) 2_455 2_455 ? N4 Yb2 C26A 124.0(3) . 2_455 ? Cl2 Yb2 C26A 71.3(2) . 2_455 ? Cl2 Yb2 C26A 84.1(2) 2_455 2_455 ? N3 Yb2 C26A 166.4(2) 2_455 . ? N3 Yb2 C26A 96.7(3) . . ? N4 Yb2 C26A 124.0(3) 2_455 . ? N4 Yb2 C26A 29.4(3) . . ? Cl2 Yb2 C26A 84.1(2) . . ? Cl2 Yb2 C26A 71.3(2) 2_455 . ? C26A Yb2 C26A 95.4(5) 2_455 . ? C1 N1 C9 117.9(5) . . ? C1 N1 Yb1 118.5(3) . . ? C9 N1 Yb1 123.5(3) . . ? C7 N2 C8 118.0(4) . . ? C7 N2 Yb1 122.3(3) . . ? C8 N2 Yb1 118.7(3) . . ? C24 N3 C25 118.8(4) . . ? C24 N3 Yb2 123.1(4) . . ? C25 N3 Yb2 117.8(3) . . ? C18 N4 C26B 107.4(8) . . ? C18 N4 C26A 134.6(7) . . ? C26B N4 C26A 30.4(6) . . ? C18 N4 Yb2 121.2(4) . . ? C26B N4 Yb2 131.1(7) . . ? C26A N4 Yb2 103.4(6) . . ? N1 C1 C2 123.1(5) . . ? N1 C1 C7 115.1(4) . . ? C2 C1 C7 121.6(5) . . ? C3 C2 C1 132.9(5) . . ? C2 C3 C4 131.0(6) . . ? C5 C4 C3 125.0(5) . . ? C4 C5 C6 129.5(6) . . ? C5 C6 C7 132.9(5) . . ? N2 C7 C6 122.3(5) . . ? N2 C7 C1 113.5(4) . . ? C6 C7 C1 124.1(5) . . ? N2 C7 Yb1 37.2(2) . . ? C6 C7 Yb1 152.4(4) . . ? C1 C7 Yb1 79.1(3) . . ? N2 C8 C12 115.8(4) . . ? N2 C8 C8 106.7(3) . 2 ? C12 C8 C8 111.2(5) . 2 ? N1 C9 C11 110.0(5) . . ? N1 C9 C10 110.2(5) . . ? C11 C9 C10 112.2(5) . . ? C13 C12 C17 118.8(5) . . ? C13 C12 C8 118.3(5) . . ? C17 C12 C8 122.8(4) . . ? C12 C13 C14 121.3(5) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C16 118.7(5) . . ? C17 C16 C15 121.0(5) . . ? C16 C17 C12 120.1(5) . . ? N4 C18 C19 120.6(7) . . ? N4 C18 C24 114.3(6) . . ? C19 C18 C24 125.1(8) . . ? C18 C19 C20 128.5(10) . . ? C21 C20 C19 132.3(14) . . ? C20 C21 C22 125.3(12) . . ? C21 C22 C23 131.2(10) . . ? C22 C23 C24 132.7(7) . . ? N3 C24 C23 122.1(6) . . ? N3 C24 C18 113.9(5) . . ? C23 C24 C18 124.0(6) . . ? N3 C25 C29 112.1(5) . . ? N3 C25 C25 110.1(3) . 2_455 ? C29 C25 C25 113.6(5) . 2_455 ? C27A C26A C28A 126.3(13) . . ? C27A C26A N4 119.1(12) . . ? C28A C26A N4 114.6(9) . . ? C27A C26A Yb2 93.7(10) . . ? C28A C26A Yb2 124.1(8) . . ? N4 C26A Yb2 47.2(4) . . ? C27B C26B N4 131.6(12) . . ? C27B C26B C28B 118.1(12) . . ? N4 C26B C28B 108.7(10) . . ? C30 C29 C34 117.0(5) . . ? C30 C29 C25 123.2(5) . . ? C34 C29 C25 119.7(5) . . ? C29 C30 C31 121.5(6) . . ? C32 C31 C30 119.4(6) . . ? C33 C32 C31 119.5(6) . . ? C34 C33 C32 120.1(6) . . ? C33 C34 C29 122.4(6) . . ? O1 C35 C36 106.0(9) . . ? C37 C36 C35 107.3(12) . . ? C36 C37 C38 105.3(11) . . ? O1 C38 C37 107.0(9) . . ? O2 C39 C40 105.6(10) . . ? C41 C40 C39 97.0(9) . . ? C40 C41 C42 106.8(10) . . ? O2 C42 C41 105.7(10) . . ? C44 C43 O3 108.0(11) . . ? C43 C44 C45 112.2(14) . . ? C44 C45 C46 101.3(10) . . ? O3 C46 C45 106.1(7) . . ? C48 C47 C50 97.2(16) . . ? C49 C48 C47 107.0(15) . . ? C48 C49 O4 102.0(15) . . ? O4 C50 C47 99.2(17) . . ? C38 O1 C35 107.8(7) . . ? C38 O1 Li1 122.5(6) . . ? C35 O1 Li1 129.5(7) . . ? C39 O2 C42 102.1(8) . . ? C39 O2 Li1 134.2(8) . . ? C42 O2 Li1 121.7(7) . . ? C46 O3 C43 110.4(7) . . ? C46 O3 Li1 123.7(6) . . ? C43 O3 Li1 124.7(7) . . ? C50 O4 C49 98.6(14) . . ? C50 O4 Li1 123.7(12) . . ? C49 O4 Li1 136.6(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.885 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.081 #============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 638161' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H57 N4 O2 Yb' _chemical_formula_weight 883.01 _chemical_absolute_configuration rmad 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 monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3793(5) _cell_length_b 15.7831(11) _cell_length_c 14.0708(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.487(4) _cell_angle_gamma 90.00 _cell_volume 2007.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.570 _exptl_crystal_size_mid 0.236 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 2.373 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4669 _exptl_absorpt_correction_T_max 0.8917 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'area dectecor' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13718 _diffrn_reflns_av_R_equivalents 0.1014 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9047 _reflns_number_gt 8140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.1515P)^2^+1.4724P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 9047 _refine_ls_number_parameters 462 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.1995 _refine_ls_wR_factor_gt 0.1949 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2321(11) 0.1800(6) -0.0522(7) 0.0280(19) Uani 1 1 d . . . C2 C 0.1780(13) 0.1502(7) -0.1509(8) 0.034(2) Uani 1 1 d . . . H2 H 0.2491 0.1521 -0.1879 0.041 Uiso 1 1 calc R . . C3 C 0.0429(14) 0.1191(7) -0.2029(8) 0.034(2) Uani 1 1 d . . . H3 H 0.0362 0.1017 -0.2686 0.041 Uiso 1 1 calc R . . C4 C -0.0890(14) 0.1093(9) -0.1714(10) 0.035(3) Uani 1 1 d . . . H4 H -0.1770 0.0940 -0.2197 0.042 Uiso 1 1 calc R . . C5 C -0.0970(11) 0.1202(7) -0.0791(9) 0.035(2) Uani 1 1 d . . . H5 H -0.1941 0.1164 -0.0710 0.041 Uiso 1 1 calc R . . C6 C 0.0137(11) 0.1363(7) 0.0084(8) 0.0286(19) Uani 1 1 d . . . H6 H -0.0212 0.1365 0.0659 0.034 Uiso 1 1 calc R . . C7 C 0.1652(11) 0.1522(6) 0.0270(7) 0.0255(18) Uani 1 1 d . . . C8 C 0.1935(11) 0.1237(7) 0.1988(7) 0.0239(19) Uani 1 1 d . . . H8 H 0.1080 0.1614 0.1995 0.029 Uiso 1 1 calc R . . C9 C 0.3118(10) 0.1332(6) 0.3011(7) 0.0250(17) Uani 1 1 d . . . H9 H 0.3766 0.0818 0.3131 0.030 Uiso 1 1 calc R . . C10 C 0.5065(10) 0.2245(6) 0.3830(7) 0.025(2) Uani 1 1 d . . . C11 C 0.5386(12) 0.1750(7) 0.4674(8) 0.032(2) Uani 1 1 d . . . H11 H 0.4776 0.1262 0.4612 0.039 Uiso 1 1 calc R . . C12 C 0.6436(13) 0.1815(9) 0.5616(9) 0.046(3) Uani 1 1 d . . . H12 H 0.6520 0.1325 0.6020 0.055 Uiso 1 1 calc R . . C13 C 0.7320(16) 0.2462(11) 0.6018(9) 0.045(3) Uani 1 1 d . . . H13 H 0.7830 0.2417 0.6697 0.054 Uiso 1 1 calc R . . C14 C 0.7549(16) 0.3166(8) 0.5545(9) 0.045(3) Uani 1 1 d . . . H14 H 0.8189 0.3568 0.5947 0.054 Uiso 1 1 calc R . . C15 C 0.7010(14) 0.3399(8) 0.4581(9) 0.040(2) Uani 1 1 d . . . H15 H 0.7423 0.3914 0.4427 0.048 Uiso 1 1 calc R . . C16 C 0.5965(11) 0.3038(7) 0.3754(9) 0.033(2) Uani 1 1 d . . . C17 C 0.4006(11) 0.2701(8) -0.1063(8) 0.033(2) Uani 1 1 d . . . H17 H 0.3106 0.2792 -0.1624 0.039 Uiso 1 1 calc R . . C18 C 0.5086(13) 0.2150(8) -0.1447(9) 0.039(3) Uani 1 1 d . . . H18A H 0.6003 0.2073 -0.0922 0.046 Uiso 1 1 calc R . . H18B H 0.5309 0.2430 -0.2012 0.046 Uiso 1 1 calc R . . H18C H 0.4634 0.1596 -0.1651 0.046 Uiso 1 1 calc R . . C19 C 0.4660(17) 0.3555(8) -0.0746(11) 0.048(3) Uani 1 1 d . . . H19A H 0.4881 0.3842 -0.1308 0.058 Uiso 1 1 calc R . . H19B H 0.5574 0.3487 -0.0217 0.058 Uiso 1 1 calc R . . H19C H 0.3954 0.3895 -0.0506 0.058 Uiso 1 1 calc R . . C20 C 0.6465(15) 0.4135(8) 0.2704(9) 0.040(3) Uani 1 1 d . . . H20 H 0.7531 0.4087 0.3077 0.048 Uiso 1 1 calc R . . C21 C 0.6352(18) 0.4247(9) 0.1606(10) 0.047(3) Uani 1 1 d . . . H21A H 0.6908 0.4752 0.1512 0.056 Uiso 1 1 calc R . . H21B H 0.5312 0.4313 0.1240 0.056 Uiso 1 1 calc R . . H21C H 0.6766 0.3747 0.1362 0.056 Uiso 1 1 calc R . . C22 C 0.5796(16) 0.4931(8) 0.3054(11) 0.047(3) Uani 1 1 d . . . H22A H 0.4759 0.4989 0.2678 0.057 Uiso 1 1 calc R . . H22B H 0.6351 0.5433 0.2951 0.057 Uiso 1 1 calc R . . H22C H 0.5853 0.4876 0.3757 0.057 Uiso 1 1 calc R . . C23 C 0.1386(11) 0.0340(7) 0.1891(7) 0.0282(19) Uani 1 1 d . . . C24 C -0.0016(12) 0.0150(7) 0.2031(8) 0.033(2) Uani 1 1 d . . . H24 H -0.0630 0.0599 0.2138 0.040 Uiso 1 1 calc R . . C25 C -0.0522(16) -0.0693(8) 0.2016(9) 0.044(3) Uani 1 1 d . . . H25 H -0.1472 -0.0814 0.2102 0.052 Uiso 1 1 calc R . . C26 C 0.0416(14) -0.1350(8) 0.1870(9) 0.031(3) Uani 1 1 d . . . H26 H 0.0108 -0.1924 0.1870 0.038 Uiso 1 1 calc R . . C27 C 0.1774(13) -0.1161(7) 0.1729(9) 0.037(2) Uani 1 1 d . . . H27 H 0.2398 -0.1606 0.1626 0.045 Uiso 1 1 calc R . . C28 C 0.2256(12) -0.0312(7) 0.1733(8) 0.034(2) Uani 1 1 d . . . H28 H 0.3193 -0.0193 0.1626 0.041 Uiso 1 1 calc R . . C29 C 0.2220(12) 0.1362(7) 0.3787(8) 0.032(2) Uani 1 1 d . . . C30 C 0.1532(14) 0.2122(8) 0.3946(9) 0.039(3) Uani 1 1 d . . . H30 H 0.1703 0.2631 0.3634 0.047 Uiso 1 1 calc R . . C31 C 0.0589(16) 0.2115(9) 0.4571(9) 0.048(3) Uani 1 1 d . . . H31 H 0.0073 0.2617 0.4648 0.058 Uiso 1 1 calc R . . C32 C 0.0399(14) 0.1399(12) 0.5072(11) 0.052(3) Uani 1 1 d . . . H32 H -0.0218 0.1404 0.5510 0.062 Uiso 1 1 calc R . . C33 C 0.1139(15) 0.0652(9) 0.4925(10) 0.046(3) Uani 1 1 d . . . H33 H 0.1028 0.0150 0.5272 0.055 Uiso 1 1 calc R . . C34 C 0.2017(15) 0.0642(8) 0.4287(9) 0.042(3) Uani 1 1 d . . . H34 H 0.2493 0.0130 0.4189 0.050 Uiso 1 1 calc R . . C35 C 0.1638(15) 0.3796(9) 0.0462(9) 0.044(3) Uani 1 1 d . . . H35A H 0.1538 0.3402 -0.0099 0.052 Uiso 1 1 calc R . . H35B H 0.1908 0.4362 0.0262 0.052 Uiso 1 1 calc R . . C36 C 0.0214(13) 0.3845(10) 0.0745(10) 0.047(3) Uani 1 1 d . . . H36A H -0.0275 0.4398 0.0553 0.056 Uiso 1 1 calc R . . H36B H -0.0467 0.3387 0.0424 0.056 Uiso 1 1 calc R . . C37 C 0.0653(14) 0.3741(10) 0.1851(10) 0.046(3) Uani 1 1 d . . . H37A H 0.0172 0.4177 0.2167 0.055 Uiso 1 1 calc R . . H37B H 0.0374 0.3173 0.2040 0.055 Uiso 1 1 calc R . . C38 C 0.2299(12) 0.3850(9) 0.2145(9) 0.036(2) Uani 1 1 d . . . H38A H 0.2567 0.4456 0.2235 0.043 Uiso 1 1 calc R . . H38B H 0.2749 0.3545 0.2768 0.043 Uiso 1 1 calc R . . C39 C 0.7093(14) 0.1969(8) 0.1064(10) 0.042(3) Uani 1 1 d . . . H39A H 0.7277 0.2342 0.0580 0.051 Uiso 1 1 calc R . . C40 C 0.6297(12) 0.1221(8) 0.0893(9) 0.037(2) Uani 1 1 d . . . H40A H 0.5907 0.0971 0.0263 0.044 Uiso 1 1 calc R . . C41 C 0.6151(12) 0.0892(8) 0.1765(11) 0.039(3) Uani 1 1 d . . . H41A H 0.5593 0.0406 0.1839 0.047 Uiso 1 1 calc R . . C42 C 0.6999(14) 0.1419(8) 0.2545(10) 0.040(3) Uani 1 1 d . . . H42A H 0.7139 0.1339 0.3233 0.048 Uiso 1 1 calc R . . C43 C 0.7576(12) 0.2071(8) 0.2089(10) 0.042(3) Uani 1 1 d . . . H43A H 0.8198 0.2514 0.2421 0.050 Uiso 1 1 calc R . . C44 C -0.330(3) -0.095(2) 0.335(2) 0.099(7) Uiso 1 1 d . . . H44B H -0.3862 -0.0444 0.3055 0.119 Uiso 1 1 calc R . . H44A H -0.3165 -0.1334 0.2823 0.119 Uiso 1 1 calc R . . C45 C -0.184(4) -0.073(2) 0.408(2) 0.115(9) Uiso 1 1 d . . . H45A H -0.1153 -0.1214 0.4196 0.138 Uiso 1 1 calc R . . H45B H -0.1369 -0.0240 0.3840 0.138 Uiso 1 1 calc R . . C46 C -0.230(3) -0.050(2) 0.499(2) 0.102(8) Uiso 1 1 d . . . H46A H -0.1630 -0.0767 0.5582 0.123 Uiso 1 1 calc R . . H46B H -0.2295 0.0119 0.5086 0.123 Uiso 1 1 calc R . . C47 C -0.377(3) -0.084(2) 0.480(2) 0.099(7) Uiso 1 1 d . . . H47B H -0.4513 -0.0380 0.4695 0.119 Uiso 1 1 calc R . . H47A H -0.3873 -0.1202 0.5354 0.119 Uiso 1 1 calc R . . N1 N 0.3509(9) 0.2282(8) -0.0244(6) 0.0251(18) Uani 1 1 d . . . N2 N 0.2519(10) 0.1508(7) 0.1175(8) 0.026(2) Uani 1 1 d . . . N3 N 0.4016(10) 0.2068(5) 0.3009(7) 0.0289(17) Uani 1 1 d . . . N4 N 0.5685(10) 0.3356(5) 0.2844(7) 0.0319(18) Uani 1 1 d . . . O1 O 0.2797(9) 0.3488(6) 0.1330(6) 0.0301(18) Uani 1 1 d . . . O2 O -0.391(6) -0.133(3) 0.392(4) 0.226(17) Uiso 1 1 d . . . Yb Yb 0.46425(3) 0.23741(4) 0.15396(2) 0.02588(13) 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 0.024(4) 0.026(4) 0.034(5) -0.002(4) 0.007(4) 0.005(3) C2 0.037(6) 0.031(5) 0.036(5) -0.002(4) 0.014(4) -0.004(4) C3 0.035(6) 0.036(5) 0.027(5) 0.001(4) 0.000(4) -0.008(4) C4 0.012(5) 0.044(6) 0.040(7) 0.008(5) -0.010(4) -0.002(5) C5 0.015(4) 0.034(5) 0.047(6) 0.011(4) -0.005(4) 0.003(4) C6 0.023(4) 0.031(5) 0.029(5) -0.001(4) 0.003(4) -0.002(4) C7 0.020(4) 0.025(5) 0.030(5) -0.001(3) 0.003(3) -0.001(3) C8 0.010(4) 0.029(5) 0.030(5) 0.002(4) 0.002(3) 0.008(3) C9 0.017(4) 0.025(4) 0.031(4) -0.003(3) 0.004(3) -0.004(3) C10 0.025(4) 0.015(7) 0.031(4) -0.010(3) 0.001(3) 0.001(3) C11 0.026(5) 0.030(5) 0.033(5) -0.006(4) -0.004(4) -0.002(4) C12 0.028(5) 0.056(7) 0.040(6) -0.002(5) -0.015(5) 0.023(5) C13 0.064(7) 0.025(7) 0.040(5) -0.009(6) 0.006(5) 0.001(6) C14 0.047(7) 0.036(6) 0.040(6) -0.011(5) -0.006(5) -0.003(5) C15 0.037(6) 0.034(5) 0.048(6) -0.002(5) 0.008(5) -0.003(5) C16 0.018(4) 0.031(5) 0.051(6) -0.009(4) 0.012(4) -0.006(4) C17 0.019(4) 0.043(5) 0.036(5) -0.001(4) 0.006(4) -0.001(4) C18 0.026(4) 0.046(8) 0.047(6) 0.004(4) 0.016(4) 0.002(4) C19 0.052(7) 0.040(6) 0.055(7) -0.002(5) 0.019(6) -0.005(5) C20 0.043(6) 0.035(5) 0.041(6) -0.002(4) 0.007(5) -0.014(5) C21 0.058(9) 0.033(6) 0.048(7) 0.003(5) 0.011(6) -0.013(6) C22 0.039(6) 0.034(6) 0.063(8) 0.004(5) 0.003(6) -0.010(5) C23 0.023(4) 0.036(5) 0.026(4) 0.002(4) 0.007(3) -0.001(4) C24 0.022(5) 0.034(5) 0.042(6) 0.000(4) 0.006(4) -0.004(4) C25 0.052(7) 0.038(6) 0.041(6) 0.005(5) 0.012(5) -0.009(5) C26 0.020(6) 0.032(5) 0.035(6) 0.003(4) -0.004(5) -0.007(5) C27 0.020(5) 0.033(5) 0.053(7) -0.002(5) -0.001(4) 0.005(4) C28 0.029(5) 0.030(5) 0.041(5) -0.003(4) 0.004(4) -0.004(4) C29 0.033(5) 0.030(5) 0.033(5) 0.000(4) 0.008(4) 0.003(4) C30 0.044(6) 0.040(6) 0.037(5) 0.003(4) 0.017(5) 0.008(4) C31 0.047(7) 0.063(9) 0.038(6) 0.005(5) 0.017(5) 0.017(5) C32 0.023(5) 0.085(10) 0.046(7) 0.008(7) 0.009(5) 0.000(6) C33 0.037(6) 0.056(7) 0.047(7) 0.019(6) 0.015(5) -0.007(5) C34 0.043(6) 0.040(6) 0.044(6) 0.010(5) 0.013(5) 0.000(5) C35 0.043(6) 0.044(7) 0.042(6) 0.008(5) 0.008(5) 0.016(5) C36 0.020(5) 0.059(8) 0.052(7) 0.000(6) -0.006(5) -0.001(5) C37 0.029(6) 0.053(7) 0.052(7) 0.003(6) 0.005(5) -0.003(5) C38 0.015(5) 0.045(7) 0.040(6) -0.004(5) -0.005(4) 0.000(5) C39 0.033(5) 0.041(6) 0.057(7) 0.003(5) 0.019(5) -0.001(5) C40 0.019(4) 0.042(6) 0.045(6) -0.007(5) 0.001(4) 0.013(4) C41 0.016(4) 0.029(6) 0.067(8) 0.000(5) 0.003(5) 0.001(4) C42 0.033(6) 0.041(6) 0.047(6) 0.003(5) 0.011(5) 0.016(5) C43 0.017(4) 0.051(6) 0.056(7) -0.002(5) 0.007(4) 0.000(4) N1 0.024(3) 0.019(5) 0.032(3) 0.001(4) 0.007(2) -0.001(4) N2 0.009(4) 0.034(5) 0.030(5) 0.004(4) -0.003(3) 0.009(3) N3 0.026(4) 0.026(3) 0.036(4) -0.006(3) 0.010(3) -0.006(3) N4 0.025(4) 0.024(4) 0.045(5) 0.002(3) 0.007(4) -0.003(3) O1 0.017(4) 0.039(5) 0.028(4) 0.004(3) -0.003(3) -0.002(3) Yb 0.02172(18) 0.02535(18) 0.02979(19) -0.0001(3) 0.00552(11) -0.0013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.319(14) . ? C1 C2 1.426(15) . ? C1 C7 1.484(15) . ? C2 C3 1.373(16) . ? C3 C4 1.429(19) . ? C4 C5 1.33(2) . ? C5 C6 1.406(14) . ? C6 C7 1.397(14) . ? C7 N2 1.316(14) . ? C7 Yb 3.193(10) . ? C8 N2 1.457(15) . ? C8 C23 1.500(15) . ? C8 C9 1.572(13) . ? C9 N3 1.436(12) . ? C9 C29 1.549(15) . ? C10 N3 1.332(12) . ? C10 C11 1.385(15) . ? C10 C16 1.529(14) . ? C10 Yb 3.147(9) . ? C11 C12 1.428(14) . ? C12 C13 1.34(2) . ? C13 C14 1.34(2) . ? C14 C15 1.366(18) . ? C15 C16 1.425(16) . ? C16 N4 1.334(16) . ? C16 Yb 3.206(11) . ? C17 C19 1.498(17) . ? C17 N1 1.507(15) . ? C17 C18 1.539(16) . ? C20 N4 1.471(14) . ? C20 C21 1.531(18) . ? C20 C22 1.54(2) . ? C23 C28 1.368(16) . ? C23 C24 1.413(14) . ? C24 C25 1.410(16) . ? C25 C26 1.41(2) . ? C26 C27 1.374(18) . ? C27 C28 1.413(16) . ? C29 C34 1.377(16) . ? C29 C30 1.407(16) . ? C30 C31 1.405(17) . ? C31 C32 1.37(2) . ? C32 C33 1.41(2) . ? C33 C34 1.370(19) . ? C35 O1 1.483(14) . ? C35 C36 1.494(19) . ? C36 C37 1.509(19) . ? C37 C38 1.497(17) . ? C38 O1 1.466(16) . ? C39 C40 1.383(18) . ? C39 C43 1.40(2) . ? C39 Yb 2.639(12) . ? C40 C41 1.373(19) . ? C40 Yb 2.702(10) . ? C41 C42 1.436(19) . ? C41 Yb 2.708(13) . ? C42 C43 1.396(19) . ? C42 Yb 2.737(11) . ? C43 Yb 2.695(11) . ? C44 O2 1.25(5) . ? C44 C45 1.52(4) . ? C45 C46 1.50(4) . ? C46 C47 1.43(4) . ? C47 O2 1.43(5) . ? N1 Yb 2.454(8) . ? N2 Yb 2.357(10) . ? N3 Yb 2.346(9) . ? N4 Yb 2.402(9) . ? O1 Yb 2.429(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.2(10) . . ? N1 C1 C7 116.2(9) . . ? C2 C1 C7 121.4(9) . . ? C3 C2 C1 132.4(11) . . ? C2 C3 C4 128.7(11) . . ? C5 C4 C3 124.5(11) . . ? C4 C5 C6 131.1(11) . . ? C7 C6 C5 132.2(10) . . ? N2 C7 C6 120.9(10) . . ? N2 C7 C1 117.1(9) . . ? C6 C7 C1 121.7(9) . . ? N2 C7 Yb 40.7(6) . . ? C6 C7 Yb 151.4(7) . . ? C1 C7 Yb 79.1(5) . . ? N2 C8 C23 113.4(9) . . ? N2 C8 C9 111.7(8) . . ? C23 C8 C9 108.3(8) . . ? N3 C9 C29 114.0(8) . . ? N3 C9 C8 110.3(8) . . ? C29 C9 C8 105.4(8) . . ? N3 C10 C11 124.5(9) . . ? N3 C10 C16 113.8(9) . . ? C11 C10 C16 121.6(9) . . ? N3 C10 Yb 42.6(5) . . ? C11 C10 Yb 148.6(7) . . ? C16 C10 Yb 78.2(6) . . ? C10 C11 C12 133.9(11) . . ? C13 C12 C11 129.9(14) . . ? C14 C13 C12 125.8(12) . . ? C13 C14 C15 130.5(12) . . ? C14 C15 C16 134.0(12) . . ? N4 C16 C15 123.3(10) . . ? N4 C16 C10 113.9(9) . . ? C15 C16 C10 122.9(10) . . ? N4 C16 Yb 42.7(5) . . ? C15 C16 Yb 158.0(8) . . ? C10 C16 Yb 73.9(5) . . ? C19 C17 N1 110.7(10) . . ? C19 C17 C18 110.9(10) . . ? N1 C17 C18 112.8(10) . . ? N4 C20 C21 109.2(10) . . ? N4 C20 C22 112.2(11) . . ? C21 C20 C22 107.7(11) . . ? C28 C23 C24 118.7(10) . . ? C28 C23 C8 121.3(9) . . ? C24 C23 C8 119.8(9) . . ? C25 C24 C23 121.3(11) . . ? C26 C25 C24 118.4(12) . . ? C27 C26 C25 119.9(11) . . ? C26 C27 C28 120.9(11) . . ? C23 C28 C27 120.7(11) . . ? C34 C29 C30 119.4(11) . . ? C34 C29 C9 120.7(10) . . ? C30 C29 C9 119.8(9) . . ? C31 C30 C29 119.0(11) . . ? C32 C31 C30 121.3(13) . . ? C31 C32 C33 118.5(12) . . ? C34 C33 C32 120.8(12) . . ? C33 C34 C29 120.9(13) . . ? O1 C35 C36 108.0(10) . . ? C37 C36 C35 104.6(10) . . ? C38 C37 C36 104.5(11) . . ? O1 C38 C37 105.1(10) . . ? C40 C39 C43 106.8(11) . . ? C40 C39 Yb 77.5(7) . . ? C43 C39 Yb 77.0(7) . . ? C41 C40 C39 110.2(11) . . ? C41 C40 Yb 75.6(7) . . ? C39 C40 Yb 72.5(7) . . ? C40 C41 C42 107.3(11) . . ? C40 C41 Yb 75.0(7) . . ? C42 C41 Yb 75.8(7) . . ? C43 C42 C41 106.2(11) . . ? C43 C42 Yb 73.4(7) . . ? C41 C42 Yb 73.6(7) . . ? C39 C43 C42 109.3(11) . . ? C39 C43 Yb 72.6(7) . . ? C42 C43 Yb 76.8(7) . . ? O2 C44 C45 99(3) . . ? C46 C45 C44 103(3) . . ? C47 C46 C45 103(3) . . ? C46 C47 O2 103(3) . . ? C1 N1 C17 115.8(8) . . ? C1 N1 Yb 116.0(7) . . ? C17 N1 Yb 128.2(6) . . ? C7 N2 C8 120.0(9) . . ? C7 N2 Yb 118.0(8) . . ? C8 N2 Yb 118.2(7) . . ? C10 N3 C9 117.8(9) . . ? C10 N3 Yb 114.9(7) . . ? C9 N3 Yb 116.9(6) . . ? C16 N4 C20 117.8(9) . . ? C16 N4 Yb 115.2(7) . . ? C20 N4 Yb 123.5(7) . . ? C35 O1 C38 101.5(9) . . ? C35 O1 Yb 132.8(8) . . ? C38 O1 Yb 123.6(6) . . ? C44 O2 C47 111(4) . . ? N2 Yb N3 71.1(3) . . ? N2 Yb N4 133.5(3) . . ? N3 Yb N4 66.8(3) . . ? N2 Yb O1 82.0(4) . . ? N3 Yb O1 85.3(3) . . ? N4 Yb O1 76.0(3) . . ? N2 Yb N1 68.5(3) . . ? N3 Yb N1 138.3(3) . . ? N4 Yb N1 142.8(4) . . ? O1 Yb N1 79.6(3) . . ? N2 Yb C39 123.2(4) . . ? N3 Yb C39 127.9(4) . . ? N4 Yb C39 98.4(4) . . ? O1 Yb C39 141.7(4) . . ? N1 Yb C39 84.0(4) . . ? N2 Yb C43 134.3(4) . . ? N3 Yb C43 100.8(4) . . ? N4 Yb C43 73.7(4) . . ? O1 Yb C43 143.4(4) . . ? N1 Yb C43 114.4(3) . . ? C39 Yb C43 30.4(4) . . ? N2 Yb C40 93.7(4) . . ? N3 Yb C40 117.4(4) . . ? N4 Yb C40 122.6(3) . . ? O1 Yb C40 154.3(3) . . ? N1 Yb C40 75.3(3) . . ? C39 Yb C40 30.0(4) . . ? C43 Yb C40 48.9(4) . . ? N2 Yb C41 84.8(3) . . ? N3 Yb C41 88.0(4) . . ? N4 Yb C41 112.0(3) . . ? O1 Yb C41 166.5(3) . . ? N1 Yb C41 98.0(4) . . ? C39 Yb C41 50.0(4) . . ? C43 Yb C41 49.6(4) . . ? C40 Yb C41 29.4(4) . . ? N2 Yb C42 108.2(4) . . ? N3 Yb C42 77.8(4) . . ? N4 Yb C42 81.5(4) . . ? O1 Yb C42 155.9(3) . . ? N1 Yb C42 124.4(4) . . ? C39 Yb C42 50.2(4) . . ? C43 Yb C42 29.8(4) . . ? C40 Yb C42 49.1(4) . . ? C41 Yb C42 30.6(4) . . ? N2 Yb C10 93.1(3) . . ? N3 Yb C10 22.6(3) . . ? N4 Yb C10 49.1(3) . . ? O1 Yb C10 93.6(3) . . ? N1 Yb C10 160.9(3) . . ? C39 Yb C10 111.3(3) . . ? C43 Yb C10 81.7(3) . . ? C40 Yb C10 112.0(3) . . ? C41 Yb C10 84.5(4) . . ? C42 Yb C10 64.6(3) . . ? N2 Yb C16 119.1(3) . . ? N3 Yb C16 48.2(3) . . ? N4 Yb C16 22.1(3) . . ? O1 Yb C16 87.7(3) . . ? N1 Yb C16 164.3(3) . . ? C39 Yb C16 100.9(3) . . ? C43 Yb C16 71.3(3) . . ? C40 Yb C16 116.1(3) . . ? C41 Yb C16 96.5(4) . . ? C42 Yb C16 68.2(3) . . ? C10 Yb C16 27.8(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 6.221 _refine_diff_density_min -2.712 _refine_diff_density_rms 0.286 _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END===========================================================================