Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2006 data_publication_text _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Isao Azumaya' _publ_contact_author_address ; Faculty of Pharmaceutical Sciences at Kagawa Campus, Tokushima Bunri University, 1314-1, Shido, Sanuki, Kagawa, 769-2193, JAPAN ; _publ_contact_author_email azumayai@kph.bunri-u.ac.jp _publ_contact_author_phone +81-87-894-5111x6308 _publ_contact_author_fax +81-87-894-0181 _publ_section_title ; 2-D Coordination Network of Cyclic Amide with Lanthanide Metal Cation and Its Columnar Stacking ; loop_ _publ_author_name 'Isao Azumaya' 'Kosuke Katagiri' 'Takako Kato' 'Hyuma Masu' 'Masahide Tominaga' data_1-La _database_code_depnum_ccdc_archive 'CCDC 607541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H40 F9 La N3 O20.50 S3' _chemical_formula_weight 1152.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P-6 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' _cell_length_a 21.3144(5) _cell_length_b 21.3144(5) _cell_length_c 17.3882(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6841.2(4) _cell_formula_units_Z 6 _cell_measurement_temperature 150 _cell_measurement_reflns_used 7869 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 22.25 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3474 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7172 _exptl_absorpt_correction_T_max 0.8905 _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _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 ApexII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77191 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 27.75 _reflns_number_total 10971 _reflns_number_gt 7888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0496P)^2^+4.4331P] 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(13) _refine_ls_number_reflns 10971 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.1366(3) -0.0569(3) 0.2559(3) 0.0223(13) Uani 1 1 d . . . C2 C 0.0615(3) -0.1888(3) 0.2478(3) 0.0363(16) Uani 1 1 d . . . H2A H 0.0506 -0.2075 0.3005 0.055 Uiso 1 1 calc R . . H2B H 0.0630 -0.2249 0.2141 0.055 Uiso 1 1 calc R . . H2C H 0.0237 -0.1789 0.2299 0.055 Uiso 1 1 calc R . . C3 C 0.1955(3) -0.1292(3) 0.2493(3) 0.0235(13) Uani 1 1 d . . . C4 C 0.2313(3) -0.1197(3) 0.3182(3) 0.0303(13) Uani 1 1 d . . . H4 H 0.2125 -0.1113 0.3641 0.036 Uiso 1 1 calc R . . C5 C 0.2944(3) -0.1225(3) 0.3202(3) 0.0275(13) Uani 1 1 d . . . H5 H 0.3193 -0.1153 0.3675 0.033 Uiso 1 1 calc R . . C6 C 0.3221(3) -0.1359(3) 0.2532(3) 0.0208(12) Uani 1 1 d . . . C7 C 0.2831(3) -0.1493(3) 0.1856(3) 0.0321(14) Uani 1 1 d . . . H7 H 0.3000 -0.1609 0.1402 0.039 Uiso 1 1 calc R . . C8 C 0.2198(3) -0.1461(3) 0.1831(3) 0.0341(14) Uani 1 1 d . . . H8 H 0.1935 -0.1553 0.1364 0.041 Uiso 1 1 calc R . . C9 C 0.3890(3) -0.1410(3) 0.2531(3) 0.0192(12) Uani 1 1 d . . . C10 C 0.5202(3) -0.0838(3) 0.2600(3) 0.0324(14) Uani 1 1 d . . . H10A H 0.5113 -0.1306 0.2796 0.049 Uiso 1 1 calc R . . H10B H 0.5578 -0.0447 0.2911 0.049 Uiso 1 1 calc R . . H10C H 0.5363 -0.0781 0.2064 0.049 Uiso 1 1 calc R . . C11 C 0.4590(3) -0.0101(3) 0.2600(3) 0.0231(12) Uani 1 1 d . . . C12 C 0.4518(3) 0.0226(3) 0.3263(3) 0.0338(14) Uani 1 1 d . . . H12 H 0.4444 -0.0005 0.3748 0.041 Uiso 1 1 calc R . . C13 C 0.4555(3) 0.0894(3) 0.3208(3) 0.0301(13) Uani 1 1 d . . . H13 H 0.4493 0.1115 0.3654 0.036 Uiso 1 1 calc R . . C14 C 0.4680(3) 0.1238(3) 0.2505(3) 0.0217(13) Uani 1 1 d . . . C15 C 0.4786(3) 0.0928(3) 0.1856(3) 0.0344(14) Uani 1 1 d . . . H15 H 0.4895 0.1174 0.1377 0.041 Uiso 1 1 calc R . . C16 C 0.4732(3) 0.0255(3) 0.1915(3) 0.0336(14) Uani 1 1 d . . . H16 H 0.4796 0.0036 0.1468 0.040 Uiso 1 1 calc R . . C17 C 0.4730(3) 0.1970(3) 0.2442(3) 0.0242(13) Uani 1 1 d . . . C18 C 0.4164(4) 0.2709(3) 0.2472(4) 0.0366(16) Uani 1 1 d . . . H18A H 0.4078 0.2814 0.1946 0.055 Uiso 1 1 calc R . . H18B H 0.4643 0.3088 0.2644 0.055 Uiso 1 1 calc R . . H18C H 0.3792 0.2694 0.2815 0.055 Uiso 1 1 calc R . . C19 C 0.3433(3) 0.1357(3) 0.2500(3) 0.0257(13) Uani 1 1 d . . . C20 C 0.3007(3) 0.1186(3) 0.3148(3) 0.0327(13) Uani 1 1 d . . . H20 H 0.3172 0.1494 0.3586 0.039 Uiso 1 1 calc R . . C21 C 0.2330(3) 0.0555(3) 0.3155(3) 0.0321(14) Uani 1 1 d . . . H21 H 0.2031 0.0439 0.3597 0.039 Uiso 1 1 calc R . . C22 C 0.2091(3) 0.0098(3) 0.2526(3) 0.0202(12) Uani 1 1 d . . . C23 C 0.2518(3) 0.0281(3) 0.1872(3) 0.0248(12) Uani 1 1 d . . . H23 H 0.2357 -0.0028 0.1436 0.030 Uiso 1 1 calc R . . C24 C 0.3180(3) 0.0914(3) 0.1857(3) 0.0289(13) Uani 1 1 d . . . H24 H 0.3464 0.1048 0.1402 0.035 Uiso 1 1 calc R . . C25 C 0.6671(7) 0.1467(5) 0.5000 0.055(3) Uani 1 2 d S . . C28 C 0.5071(6) 0.9002(7) 0.5000 0.060(3) Uani 1 2 d S . . C27 C 0.5832(5) 0.9187(6) 0.0000 0.047(2) Uani 1 2 d S . . C29 C 0.0294(9) 0.8292(6) 0.0000 0.065(4) Uani 1 2 d S . . C30 C 0.0037(7) 0.7488(6) 0.5000 0.055(3) Uani 1 2 d S . . C31 C 0.3047(7) 0.0076(6) 0.5000 0.061(3) Uani 1 2 d S . . H31A H 0.3409 0.0204 0.4593 0.092 Uiso 0.50 1 calc PR . . H31B H 0.2640 -0.0412 0.4907 0.092 Uiso 0.50 1 calc PR . . H31C H 0.3267 0.0090 0.5499 0.092 Uiso 0.50 1 calc PR . . C32 C 0.3358(6) 0.9587(6) 1.0000 0.062(3) Uani 1 2 d S . . H32A H 0.3767 0.9634 1.0302 0.093 Uiso 0.50 1 calc PR . . H32B H 0.3180 0.9890 1.0227 0.093 Uiso 0.50 1 calc PR . . H32C H 0.3515 0.9744 0.9470 0.093 Uiso 0.50 1 calc PR . . F1 F 0.6118(3) 0.1602(3) 0.5000 0.0586(18) Uani 1 2 d S . . F2 F 0.6631(3) 0.1088(2) 0.4387(3) 0.0870(16) Uani 1 1 d . . . F7 F 0.5363(3) 0.9421(3) 0.4391(2) 0.100(2) Uani 1 1 d . . . F8 F 0.5284(4) 0.8514(5) 0.5000 0.103(3) Uani 1 2 d S . . F5 F 0.5743(4) 0.8528(4) 0.0000 0.099(3) Uani 1 2 d S . . F6 F 0.6219(3) 0.9521(3) 0.0612(3) 0.0911(17) Uani 1 1 d . . . F9 F -0.0348(4) 0.8298(4) 0.0000 0.077(2) Uani 1 2 d S . . F10 F 0.0292(4) 0.7945(3) 0.0621(2) 0.100(2) Uani 1 1 d . . . F11 F -0.0534(4) 0.7572(4) 0.5000 0.095(3) Uani 1 2 d S . . F12 F -0.0007(3) 0.7101(3) 0.4392(3) 0.100(2) Uani 1 1 d . . . La1 La 0.0000 0.0000 0.27325(3) 0.01766(10) Uani 1 3 d S . . La2 La 0.3333 -0.3333 0.23589(4) 0.01794(15) Uani 1 3 d S . . La3 La 0.6667 0.3333 0.23002(4) 0.02100(18) Uani 1 3 d S . . N1 N 0.1319(3) -0.1218(3) 0.2461(2) 0.0249(11) Uani 1 1 d . . . N2 N 0.4526(3) -0.0804(2) 0.2644(2) 0.0237(10) Uani 1 1 d . . . N3 N 0.4132(3) 0.2004(3) 0.2487(2) 0.0253(11) Uani 1 1 d . . . O1 O 0.0814(2) -0.0523(2) 0.2674(2) 0.0263(9) Uani 1 1 d . . . O2 O 0.3858(2) -0.1998(2) 0.2419(2) 0.0255(9) Uani 1 1 d . . . O3 O 0.5332(2) 0.2528(2) 0.2363(2) 0.0287(9) Uani 1 1 d . . . O4 O -0.06138(19) 0.0342(2) 0.16342(19) 0.0295(9) Uani 1 1 d . . . O5 O 0.0901(2) 0.0696(2) 0.3794(2) 0.0325(9) Uani 1 1 d . . . O6 O 0.27342(19) -0.29791(19) 0.3463(2) 0.0278(9) Uani 1 1 d . . . O7 O 0.2634(2) -0.3123(2) 0.1286(2) 0.0321(9) Uani 1 1 d . . . O8 O 0.6371(2) 0.2380(2) 0.1255(2) 0.0404(11) Uani 1 1 d . . . O9 O 0.6081(2) 0.3703(2) 0.3399(2) 0.0350(10) Uani 1 1 d . . . O10 O 0.7512(2) 0.2679(3) 0.4301(2) 0.0460(12) Uani 1 1 d . . . O11 O 0.8091(4) 0.2133(5) 0.5000 0.076(3) Uani 1 2 d S . . O16 O 0.3959(4) 0.9171(4) 0.5000 0.0489(18) Uani 1 2 d S . . O17 O 0.3905(2) 0.8157(2) 0.4297(2) 0.0356(10) Uani 1 1 d . . . O14 O 0.4634(3) 0.8781(3) 0.0694(3) 0.0566(14) Uani 1 1 d . . . O15 O 0.5194(4) 0.9920(3) 0.0000 0.0456(16) Uani 1 2 d S . . O18 O 0.0939(2) 0.9501(2) 0.0702(2) 0.0468(12) Uani 1 1 d . . . O19 O 0.1682(5) 0.9138(6) 0.0000 0.084(3) Uani 1 2 d S . . O12 O 0.7511(5) 0.5154(4) 0.0701(3) 0.116(3) Uani 1 1 d . . . O13 O 0.7272(5) 0.5940(5) 0.0000 0.088(3) Uani 1 2 d S . . O20 O 0.0809(3) 0.8690(3) 0.4308(3) 0.0549(14) Uani 1 1 d . . . O21 O 0.1418(4) 0.8161(4) 0.5000 0.0515(18) Uani 1 2 d S . . O22 O 0.2793(3) 0.0584(3) 0.5000 0.0408(15) Uani 1 2 d S . . O23 O 0.2803(4) 0.8864(4) 1.0000 0.0411(16) Uani 1 2 d S . . O24 O 0.1366(3) 0.0202(3) 0.5000 0.0306(13) Uani 1 2 d S . . O25 O 0.3124(3) 0.7771(3) 0.0000 0.0304(13) Uani 1 2 d S . . O26 O 0.5550(5) 0.1422(4) 0.0000 0.073(2) Uani 1 2 d S . . S1 S 0.75494(12) 0.23429(13) 0.5000 0.0338(5) Uani 1 2 d S . . S4 S 0.41087(12) 0.85825(12) 0.5000 0.0274(5) Uani 1 2 d S . . S3 S 0.49871(12) 0.91734(12) 0.0000 0.0336(5) Uani 1 2 d S . . S5 S 0.10462(14) 0.92163(15) 0.0000 0.0370(6) Uani 1 2 d S . . S2 S 0.7667(2) 0.55345(16) 0.0000 0.0676(10) Uani 1 2 d S . . S6 S 0.08594(13) 0.83455(13) 0.5000 0.0337(5) Uani 1 2 d S . . C26 C 0.8542(8) 0.6207(14) 0.0000 0.141(9) Uani 1 2 d S . . F3 F 0.8819(3) 0.6583(4) 0.0606(3) 0.118(2) Uani 1 1 d . A . F4 F 0.8884(8) 0.5725(9) 0.0000 0.152(7) Uani 0.754(13) 2 d SP A 1 F4B F 0.8317(12) 0.6995(12) 0.0000 0.064(9) Uani 0.246(13) 2 d SP A 2 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 0.017(3) 0.027(3) 0.019(2) 0.004(2) 0.0015(19) 0.008(3) C2 0.030(4) 0.026(4) 0.044(4) 0.003(2) 0.001(3) 0.007(3) C3 0.022(3) 0.020(3) 0.027(3) 0.0025(19) -0.0005(19) 0.010(3) C4 0.038(3) 0.042(4) 0.016(2) 0.003(2) 0.003(2) 0.024(3) C5 0.030(3) 0.039(3) 0.015(2) 0.000(2) -0.002(2) 0.018(3) C6 0.023(3) 0.023(3) 0.021(2) 0.0041(19) 0.0012(19) 0.015(3) C7 0.040(4) 0.046(4) 0.023(3) -0.004(2) -0.002(2) 0.032(3) C8 0.038(4) 0.050(4) 0.024(3) -0.007(2) -0.006(2) 0.029(3) C9 0.025(3) 0.017(3) 0.018(2) 0.0038(18) 0.0008(18) 0.012(3) C10 0.024(3) 0.034(4) 0.042(3) 0.002(3) 0.001(2) 0.016(3) C11 0.020(3) 0.015(3) 0.030(3) 0.005(2) 0.001(2) 0.006(3) C12 0.057(4) 0.028(3) 0.019(3) 0.002(2) 0.001(2) 0.023(3) C13 0.050(4) 0.027(3) 0.015(2) -0.004(2) 0.001(2) 0.021(3) C14 0.022(3) 0.018(3) 0.022(3) 0.0014(19) -0.0007(19) 0.009(3) C15 0.056(4) 0.030(3) 0.024(3) 0.007(2) 0.005(3) 0.027(3) C16 0.046(4) 0.028(3) 0.030(3) 0.002(2) 0.009(3) 0.021(3) C17 0.023(3) 0.022(3) 0.021(2) 0.0017(19) -0.001(2) 0.006(3) C18 0.034(4) 0.025(4) 0.056(4) 0.003(3) 0.003(3) 0.018(3) C19 0.021(3) 0.030(4) 0.026(3) -0.002(2) -0.0017(19) 0.012(3) C20 0.031(3) 0.039(4) 0.025(3) -0.009(2) -0.003(2) 0.015(3) C21 0.025(3) 0.044(4) 0.019(3) -0.004(2) 0.004(2) 0.011(3) C22 0.014(3) 0.026(3) 0.023(3) 0.003(2) -0.0020(18) 0.012(3) C23 0.028(3) 0.025(3) 0.018(2) 0.000(2) 0.001(2) 0.011(3) C24 0.031(3) 0.032(3) 0.019(2) 0.000(2) 0.001(2) 0.012(3) C25 0.102(10) 0.022(5) 0.036(5) 0.000 0.000 0.028(6) C28 0.036(6) 0.099(10) 0.025(5) 0.000 0.000 0.018(6) C27 0.030(6) 0.050(7) 0.057(6) 0.000 0.000 0.017(5) C29 0.131(13) 0.041(6) 0.032(5) 0.000 0.000 0.049(8) C30 0.058(8) 0.040(7) 0.062(7) 0.000 0.000 0.020(6) C31 0.074(9) 0.052(7) 0.063(7) 0.000 0.000 0.036(7) C32 0.048(7) 0.051(7) 0.086(9) 0.000 0.000 0.024(6) F1 0.052(4) 0.053(4) 0.060(4) 0.000 0.000 0.018(3) F2 0.141(5) 0.053(3) 0.061(3) -0.025(2) 0.005(3) 0.044(3) F7 0.060(3) 0.126(5) 0.043(3) 0.023(3) 0.014(2) -0.006(3) F8 0.053(5) 0.168(8) 0.118(6) 0.000 0.000 0.077(6) F5 0.046(4) 0.060(5) 0.204(10) 0.000 0.000 0.035(4) F6 0.056(3) 0.120(5) 0.094(4) -0.015(3) -0.035(3) 0.042(3) F9 0.080(5) 0.050(4) 0.070(4) 0.000 0.000 0.008(4) F10 0.191(6) 0.067(3) 0.052(3) 0.020(2) -0.007(3) 0.070(4) F11 0.032(4) 0.070(5) 0.162(8) 0.000 0.000 0.010(4) F12 0.133(5) 0.048(3) 0.085(4) -0.036(3) -0.015(3) 0.021(3) La1 0.01855(16) 0.01855(16) 0.0159(2) 0.000 0.000 0.00927(8) La2 0.01848(19) 0.01848(19) 0.0169(3) 0.000 0.000 0.00924(9) La3 0.0209(2) 0.0209(2) 0.0212(4) 0.000 0.000 0.01044(11) N1 0.019(3) 0.025(3) 0.023(2) -0.0025(17) -0.0013(16) 0.005(2) N2 0.029(3) 0.020(3) 0.026(2) 0.0010(18) 0.0014(19) 0.016(2) N3 0.025(3) 0.022(3) 0.031(2) -0.0002(17) 0.0011(17) 0.013(2) O1 0.018(2) 0.027(2) 0.036(2) 0.0073(16) -0.0007(16) 0.0122(18) O2 0.030(2) 0.023(2) 0.0284(19) 0.0035(14) 0.0013(15) 0.0163(19) O3 0.025(2) 0.022(2) 0.036(2) 0.0012(16) -0.0010(16) 0.0098(19) O4 0.027(2) 0.032(2) 0.0270(18) 0.0019(16) -0.0071(15) 0.0130(19) O5 0.039(2) 0.030(2) 0.0272(19) -0.0031(16) -0.0108(16) 0.016(2) O6 0.025(2) 0.028(2) 0.0288(19) -0.0025(15) 0.0055(15) 0.0115(18) O7 0.031(2) 0.040(2) 0.0246(19) 0.0061(16) -0.0038(16) 0.017(2) O8 0.038(3) 0.042(3) 0.039(2) -0.0169(19) -0.0095(18) 0.018(2) O9 0.037(2) 0.033(2) 0.029(2) -0.0014(17) 0.0135(17) 0.013(2) O10 0.041(3) 0.059(3) 0.036(2) 0.013(2) -0.0031(19) 0.023(2) O11 0.076(6) 0.132(8) 0.066(5) 0.000 0.000 0.086(6) O16 0.087(6) 0.049(4) 0.030(3) 0.000 0.000 0.049(4) O17 0.046(3) 0.038(3) 0.028(2) -0.0154(17) -0.0057(17) 0.025(2) O14 0.059(3) 0.052(3) 0.057(3) 0.027(2) 0.022(2) 0.027(3) O15 0.058(5) 0.036(4) 0.045(3) 0.000 0.000 0.025(3) O18 0.041(3) 0.056(3) 0.036(2) -0.013(2) 0.007(2) 0.019(2) O19 0.091(7) 0.160(9) 0.060(5) 0.000 0.000 0.106(7) O12 0.194(8) 0.134(6) 0.041(3) 0.021(4) -0.001(4) 0.098(6) O13 0.076(7) 0.101(8) 0.084(7) 0.000 0.000 0.043(6) O20 0.044(3) 0.064(3) 0.058(3) 0.033(2) 0.002(2) 0.028(3) O21 0.059(5) 0.082(5) 0.038(4) 0.000 0.000 0.054(4) O22 0.041(4) 0.045(4) 0.042(3) 0.000 0.000 0.025(3) O23 0.048(4) 0.048(4) 0.035(3) 0.000 0.000 0.030(4) O24 0.039(3) 0.033(3) 0.025(3) 0.000 0.000 0.022(3) O25 0.029(3) 0.033(3) 0.025(3) 0.000 0.000 0.013(3) O26 0.091(6) 0.066(6) 0.041(4) 0.000 0.000 0.024(5) S1 0.0372(13) 0.0557(15) 0.0207(9) 0.000 0.000 0.0323(12) S4 0.0354(12) 0.0262(11) 0.0170(9) 0.000 0.000 0.0126(10) S3 0.0330(13) 0.0309(13) 0.0333(11) 0.000 0.000 0.0132(11) S5 0.0459(15) 0.0658(17) 0.0197(9) 0.000 0.000 0.0433(14) S2 0.142(3) 0.0559(19) 0.0194(11) 0.000 0.000 0.060(2) S6 0.0407(14) 0.0345(13) 0.0316(10) 0.000 0.000 0.0231(11) C26 0.054(9) 0.31(3) 0.029(6) 0.000 0.000 0.068(14) F3 0.100(5) 0.159(6) 0.076(4) -0.007(4) -0.032(3) 0.050(4) F4 0.126(13) 0.223(18) 0.161(14) 0.000 0.000 0.127(13) F4B 0.034(15) 0.038(15) 0.12(2) 0.000 0.000 0.014(12) _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 O1 1.246(6) . ? C1 N1 1.345(7) . ? C1 C22 1.489(7) . ? C2 N1 1.467(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.379(7) . ? C3 C8 1.383(7) . ? C3 N1 1.442(7) . ? C4 C5 1.376(8) . ? C4 H4 0.9500 . ? C5 C6 1.399(7) . ? C5 H5 0.9500 . ? C6 C7 1.384(7) . ? C6 C9 1.484(8) . ? C7 C8 1.384(8) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 O2 1.237(7) . ? C9 N2 1.338(7) . ? C10 N2 1.480(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.363(7) . ? C11 C12 1.395(7) . ? C11 N2 1.437(7) . ? C12 C13 1.389(7) . ? C12 H12 0.9500 . ? C13 C14 1.381(7) . ? C13 H13 0.9500 . ? C14 C15 1.380(7) . ? C14 C17 1.515(8) . ? C15 C16 1.385(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O3 1.247(6) . ? C17 N3 1.314(7) . ? C18 N3 1.469(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.377(7) . ? C19 C24 1.386(7) . ? C19 N3 1.438(7) . ? C20 C21 1.397(8) . ? C20 H20 0.9500 . ? C21 C22 1.382(7) . ? C21 H21 0.9500 . ? C22 C23 1.385(7) . ? C23 C24 1.381(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 F2 1.313(6) . ? C25 F2 1.313(6) 4_556 ? C25 F1 1.346(13) . ? C25 S1 1.870(12) . ? C28 F7 1.324(8) 4_556 ? C28 F7 1.324(8) . ? C28 F8 1.326(14) . ? C28 S4 1.781(11) . ? C27 F6 1.316(7) . ? C27 F6 1.316(7) 4 ? C27 F5 1.321(12) . ? C27 S3 1.787(10) . ? C29 F10 1.308(7) 4 ? C29 F10 1.308(7) . ? C29 F9 1.375(15) . ? C29 S5 1.814(13) . ? C30 F12 1.314(8) . ? C30 F12 1.314(8) 4_556 ? C30 F11 1.315(13) . ? C30 S6 1.792(12) . ? C31 O22 1.433(12) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 O23 1.396(12) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? La1 O1 2.489(4) 2 ? La1 O1 2.489(4) 3 ? La1 O1 2.489(4) . ? La1 O5 2.538(3) . ? La1 O5 2.538(3) 3 ? La1 O5 2.538(3) 2 ? La1 O4 2.616(3) 2 ? La1 O4 2.616(3) . ? La1 O4 2.616(3) 3 ? La2 O2 2.485(4) . ? La2 O2 2.485(4) 2_545 ? La2 O2 2.485(4) 3_655 ? La2 O7 2.562(3) . ? La2 O7 2.562(3) 3_655 ? La2 O7 2.562(3) 2_545 ? La2 O6 2.617(3) . ? La2 O6 2.617(3) 3_655 ? La2 O6 2.617(3) 2_545 ? La3 O3 2.484(4) 2_655 ? La3 O3 2.484(4) . ? La3 O3 2.484(4) 3_665 ? La3 O8 2.558(4) . ? La3 O8 2.558(4) 2_655 ? La3 O8 2.558(4) 3_665 ? La3 O9 2.610(4) 3_665 ? La3 O9 2.610(4) 2_655 ? La3 O9 2.610(4) . ? O10 S1 1.433(4) . ? O11 S1 1.432(7) . ? O16 S4 1.440(6) . ? O17 S4 1.453(4) . ? O14 S3 1.446(4) . ? O15 S3 1.423(6) . ? O18 S5 1.430(4) . ? O19 S5 1.445(7) . ? O12 S2 1.409(6) . ? O13 S2 1.478(10) . ? O20 S6 1.441(4) . ? O21 S6 1.429(6) . ? S1 O10 1.433(4) 4_556 ? S4 O17 1.453(4) 4_556 ? S3 O14 1.446(4) 4 ? S5 O18 1.430(4) 4 ? S2 O12 1.409(6) 4 ? S2 C26 1.691(17) . ? S6 O20 1.441(4) 4_556 ? C26 F3 1.277(14) . ? C26 F3 1.277(14) 4 ? C26 F4 1.53(3) . ? C26 F4B 1.96(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N1 120.9(5) . . ? O1 C1 C22 120.0(5) . . ? N1 C1 C22 119.0(5) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 120.6(5) . . ? C4 C3 N1 120.0(5) . . ? C8 C3 N1 119.4(5) . . ? C5 C4 C3 119.8(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.6(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 118.6(5) . . ? C7 C6 C9 118.9(5) . . ? C5 C6 C9 122.3(5) . . ? C6 C7 C8 121.0(5) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C3 C8 C7 119.2(5) . . ? C3 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? O2 C9 N2 121.1(5) . . ? O2 C9 C6 120.4(5) . . ? N2 C9 C6 118.5(5) . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 119.6(5) . . ? C16 C11 N2 120.4(5) . . ? C12 C11 N2 120.1(4) . . ? C13 C12 C11 119.4(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 120.1(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.3(5) . . ? C15 C14 C17 119.4(4) . . ? C13 C14 C17 120.3(5) . . ? C14 C15 C16 119.1(5) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C11 C16 C15 121.4(5) . . ? C11 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? O3 C17 N3 121.2(5) . . ? O3 C17 C14 119.9(5) . . ? N3 C17 C14 118.8(5) . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 119.9(5) . . ? C20 C19 N3 119.7(5) . . ? C24 C19 N3 120.3(5) . . ? C19 C20 C21 119.2(5) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 120.8(5) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.4(5) . . ? C21 C22 C1 118.9(5) . . ? C23 C22 C1 121.6(5) . . ? C24 C23 C22 119.8(5) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.7(5) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? F2 C25 F2 108.4(8) . 4_556 ? F2 C25 F1 109.7(8) . . ? F2 C25 F1 109.7(8) 4_556 . ? F2 C25 S1 109.7(7) . . ? F2 C25 S1 109.7(7) 4_556 . ? F1 C25 S1 109.5(6) . . ? F7 C28 F7 106.3(10) 4_556 . ? F7 C28 F8 107.4(7) 4_556 . ? F7 C28 F8 107.4(7) . . ? F7 C28 S4 111.9(6) 4_556 . ? F7 C28 S4 111.9(6) . . ? F8 C28 S4 111.5(9) . . ? F6 C27 F6 108.0(9) . 4 ? F6 C27 F5 107.1(6) . . ? F6 C27 F5 107.1(6) 4 . ? F6 C27 S3 111.2(6) . . ? F6 C27 S3 111.2(6) 4 . ? F5 C27 S3 112.0(7) . . ? F10 C29 F10 111.3(9) 4 . ? F10 C29 F9 106.4(9) 4 . ? F10 C29 F9 106.4(9) . . ? F10 C29 S5 111.5(8) 4 . ? F10 C29 S5 111.5(8) . . ? F9 C29 S5 109.5(7) . . ? F12 C30 F12 107.0(10) . 4_556 ? F12 C30 F11 107.7(7) . . ? F12 C30 F11 107.7(7) 4_556 . ? F12 C30 S6 111.5(6) . . ? F12 C30 S6 111.5(6) 4_556 . ? F11 C30 S6 111.2(8) . . ? O22 C31 H31A 109.5 . . ? O22 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O22 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O23 C32 H32A 109.5 . . ? O23 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O23 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O1 La1 O1 119.834(12) 2 3 ? O1 La1 O1 119.834(12) 2 . ? O1 La1 O1 119.834(12) 3 . ? O1 La1 O5 65.52(12) 2 . ? O1 La1 O5 134.81(12) 3 . ? O1 La1 O5 78.40(12) . . ? O1 La1 O5 134.81(12) 2 3 ? O1 La1 O5 78.40(12) 3 3 ? O1 La1 O5 65.52(12) . 3 ? O5 La1 O5 72.98(13) . 3 ? O1 La1 O5 78.40(12) 2 2 ? O1 La1 O5 65.52(12) 3 2 ? O1 La1 O5 134.81(12) . 2 ? O5 La1 O5 72.98(13) . 2 ? O5 La1 O5 72.98(13) 3 2 ? O1 La1 O4 130.72(12) 2 2 ? O1 La1 O4 69.60(11) 3 2 ? O1 La1 O4 66.83(12) . 2 ? O5 La1 O4 145.15(12) . 2 ? O5 La1 O4 93.80(12) 3 2 ? O5 La1 O4 134.85(12) 2 2 ? O1 La1 O4 69.60(11) 2 . ? O1 La1 O4 66.83(12) 3 . ? O1 La1 O4 130.72(12) . . ? O5 La1 O4 134.85(12) . . ? O5 La1 O4 145.15(12) 3 . ? O5 La1 O4 93.80(12) 2 . ? O4 La1 O4 72.57(13) 2 . ? O1 La1 O4 66.83(12) 2 3 ? O1 La1 O4 130.72(12) 3 3 ? O1 La1 O4 69.60(11) . 3 ? O5 La1 O4 93.80(12) . 3 ? O5 La1 O4 134.85(12) 3 3 ? O5 La1 O4 145.15(12) 2 3 ? O4 La1 O4 72.57(13) 2 3 ? O4 La1 O4 72.57(13) . 3 ? O2 La2 O2 119.823(12) . 2_545 ? O2 La2 O2 119.823(12) . 3_655 ? O2 La2 O2 119.823(12) 2_545 3_655 ? O2 La2 O7 78.40(12) . . ? O2 La2 O7 65.70(12) 2_545 . ? O2 La2 O7 134.82(12) 3_655 . ? O2 La2 O7 65.70(12) . 3_655 ? O2 La2 O7 134.82(12) 2_545 3_655 ? O2 La2 O7 78.40(12) 3_655 3_655 ? O7 La2 O7 72.84(13) . 3_655 ? O2 La2 O7 134.82(12) . 2_545 ? O2 La2 O7 78.40(12) 2_545 2_545 ? O2 La2 O7 65.70(12) 3_655 2_545 ? O7 La2 O7 72.84(13) . 2_545 ? O7 La2 O7 72.84(13) 3_655 2_545 ? O2 La2 O6 69.14(12) . . ? O2 La2 O6 67.37(11) 2_545 . ? O2 La2 O6 130.38(11) 3_655 . ? O7 La2 O6 94.22(12) . . ? O7 La2 O6 134.62(12) 3_655 . ? O7 La2 O6 145.70(12) 2_545 . ? O2 La2 O6 67.37(11) . 3_655 ? O2 La2 O6 130.38(11) 2_545 3_655 ? O2 La2 O6 69.14(12) 3_655 3_655 ? O7 La2 O6 145.70(12) . 3_655 ? O7 La2 O6 94.22(12) 3_655 3_655 ? O7 La2 O6 134.62(12) 2_545 3_655 ? O6 La2 O6 72.12(13) . 3_655 ? O2 La2 O6 130.38(11) . 2_545 ? O2 La2 O6 69.14(12) 2_545 2_545 ? O2 La2 O6 67.37(11) 3_655 2_545 ? O7 La2 O6 134.62(12) . 2_545 ? O7 La2 O6 145.70(12) 3_655 2_545 ? O7 La2 O6 94.22(12) 2_545 2_545 ? O6 La2 O6 72.12(13) . 2_545 ? O6 La2 O6 72.12(13) 3_655 2_545 ? O3 La3 O3 119.811(13) 2_655 . ? O3 La3 O3 119.811(13) 2_655 3_665 ? O3 La3 O3 119.811(13) . 3_665 ? O3 La3 O8 67.77(13) 2_655 . ? O3 La3 O8 74.95(13) . . ? O3 La3 O8 136.98(13) 3_665 . ? O3 La3 O8 74.95(13) 2_655 2_655 ? O3 La3 O8 136.98(13) . 2_655 ? O3 La3 O8 67.77(13) 3_665 2_655 ? O8 La3 O8 75.15(15) . 2_655 ? O3 La3 O8 136.98(13) 2_655 3_665 ? O3 La3 O8 67.77(13) . 3_665 ? O3 La3 O8 74.95(13) 3_665 3_665 ? O8 La3 O8 75.15(15) . 3_665 ? O8 La3 O8 75.15(15) 2_655 3_665 ? O3 La3 O9 68.55(12) 2_655 3_665 ? O3 La3 O9 130.44(12) . 3_665 ? O3 La3 O9 67.74(12) 3_665 3_665 ? O8 La3 O9 136.30(12) . 3_665 ? O8 La3 O9 92.40(13) 2_655 3_665 ? O8 La3 O9 142.62(13) 3_665 3_665 ? O3 La3 O9 67.74(12) 2_655 2_655 ? O3 La3 O9 68.55(12) . 2_655 ? O3 La3 O9 130.44(12) 3_665 2_655 ? O8 La3 O9 92.40(13) . 2_655 ? O8 La3 O9 142.62(13) 2_655 2_655 ? O8 La3 O9 136.30(12) 3_665 2_655 ? O9 La3 O9 72.32(14) 3_665 2_655 ? O3 La3 O9 130.44(12) 2_655 . ? O3 La3 O9 67.74(12) . . ? O3 La3 O9 68.55(12) 3_665 . ? O8 La3 O9 142.62(13) . . ? O8 La3 O9 136.30(12) 2_655 . ? O8 La3 O9 92.40(13) 3_665 . ? O9 La3 O9 72.32(14) 3_665 . ? O9 La3 O9 72.32(14) 2_655 . ? C1 N1 C3 121.1(5) . . ? C1 N1 C2 120.8(5) . . ? C3 N1 C2 116.9(5) . . ? C9 N2 C11 121.4(5) . . ? C9 N2 C10 119.1(5) . . ? C11 N2 C10 117.4(5) . . ? C17 N3 C19 121.0(5) . . ? C17 N3 C18 120.3(5) . . ? C19 N3 C18 118.5(5) . . ? C1 O1 La1 160.0(4) . . ? C9 O2 La2 158.9(4) . . ? C17 O3 La3 160.2(4) . . ? O11 S1 O10 114.3(3) . 4_556 ? O11 S1 O10 114.3(3) . . ? O10 S1 O10 116.1(4) 4_556 . ? O11 S1 C25 104.5(6) . . ? O10 S1 C25 102.7(3) 4_556 . ? O10 S1 C25 102.7(3) . . ? O16 S4 O17 114.6(2) . . ? O16 S4 O17 114.6(2) . 4_556 ? O17 S4 O17 114.5(4) . 4_556 ? O16 S4 C28 105.3(6) . . ? O17 S4 C28 102.9(3) . . ? O17 S4 C28 102.9(3) 4_556 . ? O15 S3 O14 115.3(3) . 4 ? O15 S3 O14 115.3(3) . . ? O14 S3 O14 113.0(5) 4 . ? O15 S3 C27 103.6(5) . . ? O14 S3 C27 103.8(3) 4 . ? O14 S3 C27 103.8(3) . . ? O18 S5 O18 117.1(4) . 4 ? O18 S5 O19 114.0(3) . . ? O18 S5 O19 114.0(3) 4 . ? O18 S5 C29 102.6(3) . . ? O18 S5 C29 102.6(3) 4 . ? O19 S5 C29 104.2(6) . . ? O12 S2 O12 119.9(6) 4 . ? O12 S2 O13 107.2(4) 4 . ? O12 S2 O13 107.2(4) . . ? O12 S2 C26 109.3(5) 4 . ? O12 S2 C26 109.3(5) . . ? O13 S2 C26 102.4(10) . . ? O21 S6 O20 115.2(3) . . ? O21 S6 O20 115.2(3) . 4_556 ? O20 S6 O20 113.2(5) . 4_556 ? O21 S6 C30 104.1(5) . . ? O20 S6 C30 103.6(3) . . ? O20 S6 C30 103.6(3) 4_556 . ? F3 C26 F3 111.4(19) . 4 ? F3 C26 F4 101.3(11) . . ? F3 C26 F4 101.3(11) 4 . ? F3 C26 S2 120.0(7) . . ? F3 C26 S2 120.0(7) 4 . ? F4 C26 S2 97.1(16) . . ? F3 C26 F4B 72.3(13) . . ? F3 C26 F4B 72.3(13) 4 . ? F4 C26 F4B 167.9(15) . . ? S2 C26 F4B 95.0(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.418 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.104 #===END data_1-Yb _database_code_depnum_ccdc_archive 'CCDC 607542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H21 N3 O3 Yb), 3(C F3 S O3), (C2 H3 N), 3(O H2)' _chemical_formula_sum 'C29 H30 F9 N4 O15 S3 Yb' _chemical_formula_weight 1114.79 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.63000(10) _cell_length_b 11.35010(10) _cell_length_c 11.43080(10) _cell_angle_alpha 65.2210(10) _cell_angle_beta 89.7530(10) _cell_angle_gamma 82.5270(10) _cell_volume 1006.374(17) _cell_formula_units_Z 1 _cell_measurement_temperature 150 _cell_measurement_reflns_used 6281 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 23.60 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 551 _exptl_absorpt_coefficient_mu 2.591 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6972 _exptl_absorpt_correction_T_max 0.8814 _exptl_absorpt_process_details 'SADABS Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _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 ApexII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19943 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 30.60 _reflns_number_total 11010 _reflns_number_gt 10810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+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 -0.003(5) _refine_ls_number_reflns 11010 _refine_ls_number_parameters 554 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _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 O2 O 0.7065(4) 1.1037(3) -0.0027(3) 0.0233(7) Uani 1 1 d . . . C9 C 0.6855(5) 0.9865(4) 0.0454(4) 0.0176(8) Uani 1 1 d . . . C15 C 0.5700(6) 0.5856(4) 0.0802(5) 0.0276(11) Uani 1 1 d . . . H15 H 0.4843 0.5385 0.0883 0.033 Uiso 1 1 calc R . . Yb1 Yb 0.793102(9) 0.296606(8) 0.924891(8) 0.01602(4) Uani 1 1 d . . . S2 S 0.28068(15) 0.26590(11) 0.19576(12) 0.0278(3) Uani 1 1 d . . . S1 S 0.98938(16) 0.13832(11) 0.74950(11) 0.0290(3) Uani 1 1 d . . . C5 C 0.8239(7) 0.9005(6) 0.2634(7) 0.0239(15) Uani 1 1 d . . . H5 H 0.9103 0.9429 0.2234 0.029 Uiso 1 1 calc R . . C4 C 0.8294(7) 0.8277(6) 0.3972(6) 0.0205(14) Uani 1 1 d . . . H4 H 0.9204 0.8181 0.4488 0.025 Uiso 1 1 calc R . . C3 C 0.7002(7) 0.7699(5) 0.4533(6) 0.0168(12) Uani 1 1 d . . . C6 C 0.6916(5) 0.9107(4) 0.1890(4) 0.0173(8) Uani 1 1 d . . . C8 C 0.5652(6) 0.7858(4) 0.3825(4) 0.0231(9) Uani 1 1 d . . . H8 H 0.4757 0.7500 0.4237 0.028 Uiso 1 1 calc R . . C7 C 0.5616(6) 0.8560(4) 0.2481(4) 0.0218(9) Uani 1 1 d . . . H7 H 0.4698 0.8662 0.1972 0.026 Uiso 1 1 calc R . . C26 C 0.2547(7) 0.1242(5) 0.3442(5) 0.0343(12) Uani 1 1 d . . . C22 C 0.7222(6) 0.4968(4) 0.5503(4) 0.0182(9) Uani 1 1 d . . . C21 C 0.8550(6) 0.4919(5) 0.4860(4) 0.0205(9) Uani 1 1 d . . . H21 H 0.9391 0.5341 0.4955 0.025 Uiso 1 1 calc R . . C1 C 0.7156(5) 0.5609(4) 0.6417(4) 0.0165(8) Uani 1 1 d . . . C23 C 0.5978(6) 0.4342(4) 0.5396(4) 0.0229(9) Uani 1 1 d . . . H23 H 0.5083 0.4337 0.5883 0.028 Uiso 1 1 calc R . . C24 C 0.6064(5) 0.3725(4) 0.4567(4) 0.0223(9) Uani 1 1 d . . . H24 H 0.5212 0.3320 0.4460 0.027 Uiso 1 1 calc R . . N1 N 0.7093(6) 0.6913(5) 0.5920(5) 0.0178(11) Uani 1 1 d . . . O1 O 0.7178(4) 0.4939(3) 0.7604(3) 0.0195(6) Uani 1 1 d . . . C25 C 1.1815(8) 0.1926(7) 0.7148(6) 0.0484(16) Uani 1 1 d . . . O4 O 0.8999(5) 0.2473(3) 0.7685(3) 0.0257(9) Uani 1 1 d . . . O5 O 0.9394(4) 0.1268(3) 0.6374(3) 0.0365(9) Uani 1 1 d . . . F2 F 1.1750(6) 0.3061(6) 0.6128(6) 0.0647(16) Uani 1 1 d . . . F1 F 1.2428(4) 0.2066(5) 0.8141(4) 0.0710(12) Uani 1 1 d . . . F3 F 1.2782(5) 0.1049(5) 0.6921(4) 0.0728(12) Uani 1 1 d . . . O8 O 0.3173(5) 0.2106(4) 0.1024(4) 0.0504(11) Uani 1 1 d . . . O7 O 0.4004(8) 0.3224(6) 0.2275(6) 0.0575(19) Uani 1 1 d . . . O9 O 0.1306(5) 0.3437(4) 0.1618(4) 0.0590(12) Uani 1 1 d . . . F5 F 0.1613(6) 0.0510(4) 0.3220(4) 0.0767(14) Uani 1 1 d . . . F6 F 0.1884(6) 0.1627(4) 0.4274(3) 0.0743(13) Uani 1 1 d . . . F4 F 0.3858(5) 0.0508(4) 0.3961(4) 0.0782(14) Uani 1 1 d . . . O13 O 1.0132(4) 0.1426(3) 1.0404(3) 0.0238(7) Uani 1 1 d . . . N2 N 0.6470(5) 0.9288(3) -0.0286(3) 0.0194(8) Uani 1 1 d . . . C11 C 0.6700(5) 0.7886(4) 0.0182(4) 0.0180(9) Uani 1 1 d . . . C12 C 0.8217(6) 0.7231(4) 0.0486(4) 0.0240(10) Uani 1 1 d . . . H12 H 0.9077 0.7709 0.0354 0.029 Uiso 1 1 calc R . . N3 N 0.7506(5) 0.3060(3) 0.3053(3) 0.0199(8) Uani 1 1 d . . . C17 C 0.7451(5) 0.3700(4) 0.1788(4) 0.0173(8) Uani 1 1 d . . . C19 C 0.7412(6) 0.3708(4) 0.3894(4) 0.0195(9) Uani 1 1 d . . . C14 C 0.7201(5) 0.5181(4) 0.1189(4) 0.0184(9) Uani 1 1 d . . . C13 C 0.8471(6) 0.5871(4) 0.0985(4) 0.0240(10) Uani 1 1 d . . . H13 H 0.9508 0.5415 0.1187 0.029 Uiso 1 1 calc R . . C16 C 0.5444(6) 0.7212(4) 0.0298(5) 0.0261(10) Uani 1 1 d . . . H16 H 0.4415 0.7673 0.0035 0.031 Uiso 1 1 calc R . . C18 C 0.7640(7) 0.1608(4) 0.3642(5) 0.0291(11) Uani 1 1 d . . . H18A H 0.6657 0.1347 0.3471 0.044 Uiso 1 1 calc R . . H18B H 0.7853 0.1268 0.4575 0.044 Uiso 1 1 calc R . . H18C H 0.8497 0.1250 0.3267 0.044 Uiso 1 1 calc R . . C10 C 0.6209(7) 1.0033(4) -0.1696(4) 0.0301(11) Uani 1 1 d . . . H10A H 0.5905 1.0965 -0.1905 0.045 Uiso 1 1 calc R . . H10B H 0.5374 0.9709 -0.2006 0.045 Uiso 1 1 calc R . . H10C H 0.7176 0.9921 -0.2114 0.045 Uiso 1 1 calc R . . C20 C 0.8686(6) 0.4263(4) 0.4070(4) 0.0218(9) Uani 1 1 d . . . H20 H 0.9630 0.4194 0.3658 0.026 Uiso 1 1 calc R . . C2 C 0.7113(6) 0.7586(4) 0.6783(4) 0.0275(11) Uani 1 1 d . . . H2A H 0.6933 0.6977 0.7665 0.041 Uiso 1 1 calc R . . H2B H 0.6286 0.8343 0.6486 0.041 Uiso 1 1 calc R . . H2C H 0.8132 0.7883 0.6769 0.041 Uiso 1 1 calc R . . O6 O 1.0178(5) 0.0201(3) 0.8666(3) 0.0435(10) Uani 1 1 d . . . O3 O 0.7563(5) 0.3107(3) 0.1081(3) 0.0247(8) Uani 1 1 d . . . S3 S 0.21900(18) 0.63499(13) 0.67363(18) 0.0490(4) Uani 1 1 d . . . C27 C 0.1970(9) 0.7771(7) 0.7071(9) 0.062(2) Uani 1 1 d . . . O12 O 0.0715(4) 0.5923(3) 0.6938(3) 0.0364(9) Uani 1 1 d . . . O11 O 0.3396(8) 0.5530(5) 0.7548(12) 0.199(6) Uani 1 1 d U . . O10 O 0.2567(13) 0.6834(9) 0.5440(10) 0.183(5) Uani 1 1 d U . . F9 F 0.3300(7) 0.8274(6) 0.6969(9) 0.130(3) Uani 1 1 d . . . F8 F 0.0956(6) 0.8683(4) 0.6221(7) 0.114(2) Uani 1 1 d . . . F7 F 0.1491(12) 0.7546(9) 0.8155(8) 0.191(5) Uani 1 1 d . . . O14 O 0.9847(4) 0.4190(3) 0.9204(3) 0.0298(8) Uani 1 1 d . . . O15 O 0.5240(4) 0.3344(3) 0.9097(3) 0.0329(8) Uani 1 1 d . . . N4 N 0.1699(7) 0.8440(7) 0.1459(6) 0.0604(16) Uani 1 1 d . . . C29 C 0.2013(8) 0.7377(9) 0.2140(7) 0.0491(19) Uani 1 1 d . . . C28 C 0.2433(10) 0.6002(7) 0.3010(9) 0.076(2) Uani 1 1 d . . . H28A H 0.2050 0.5458 0.2629 0.114 Uiso 1 1 calc R . . H28B H 0.1957 0.5827 0.3837 0.114 Uiso 1 1 calc R . . H28C H 0.3574 0.5794 0.3152 0.114 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 O2 0.038(2) 0.0129(13) 0.0179(15) -0.0048(12) 0.0057(14) -0.0063(13) C9 0.018(2) 0.0174(18) 0.017(2) -0.0062(16) 0.0041(17) -0.0035(16) C15 0.021(3) 0.023(2) 0.041(3) -0.015(2) 0.002(2) -0.0081(19) Yb1 0.02321(9) 0.01355(6) 0.01129(7) -0.00509(5) 0.00306(5) -0.00319(5) S2 0.0256(7) 0.0261(5) 0.0305(6) -0.0101(5) 0.0004(5) -0.0062(5) S1 0.0354(7) 0.0312(6) 0.0204(6) -0.0148(5) -0.0011(5) 0.0092(5) C5 0.026(3) 0.022(2) 0.023(3) -0.008(2) 0.001(2) -0.006(2) C4 0.020(3) 0.025(3) 0.018(3) -0.009(2) -0.004(2) -0.007(2) C3 0.025(3) 0.0116(19) 0.013(2) -0.0044(17) 0.007(2) -0.005(2) C6 0.024(2) 0.0118(16) 0.0153(19) -0.0053(15) 0.0023(17) -0.0004(16) C8 0.021(2) 0.026(2) 0.020(2) -0.0070(18) 0.0073(18) -0.0049(18) C7 0.024(2) 0.0215(19) 0.016(2) -0.0038(17) -0.0023(18) -0.0037(18) C26 0.045(4) 0.036(3) 0.025(3) -0.015(2) 0.005(2) -0.010(3) C22 0.029(3) 0.0150(17) 0.0093(18) -0.0036(15) -0.0005(17) -0.0027(17) C21 0.023(3) 0.027(2) 0.017(2) -0.0123(19) 0.0039(18) -0.0091(19) C1 0.019(2) 0.0170(18) 0.0124(18) -0.0047(15) -0.0003(16) -0.0028(16) C23 0.023(3) 0.027(2) 0.022(2) -0.0127(18) 0.0056(18) -0.0047(19) C24 0.023(2) 0.026(2) 0.021(2) -0.0122(18) -0.0003(18) -0.0078(19) N1 0.031(3) 0.0154(18) 0.0098(19) -0.0073(15) 0.0017(19) -0.0056(19) O1 0.0311(19) 0.0164(13) 0.0096(13) -0.0044(11) 0.0019(12) -0.0021(12) C25 0.037(4) 0.074(4) 0.039(4) -0.034(3) -0.005(3) 0.013(3) O4 0.038(2) 0.0225(17) 0.0146(17) -0.0080(14) 0.0039(16) 0.0032(15) O5 0.040(2) 0.047(2) 0.031(2) -0.0281(17) -0.0029(16) 0.0079(17) F2 0.033(3) 0.087(4) 0.066(3) -0.025(3) 0.017(2) -0.008(2) F1 0.038(2) 0.138(4) 0.060(2) -0.064(3) 0.0014(18) -0.011(2) F3 0.036(2) 0.118(3) 0.069(3) -0.056(3) -0.0023(18) 0.031(2) O8 0.069(3) 0.049(2) 0.043(2) -0.025(2) 0.023(2) -0.020(2) O7 0.076(4) 0.049(3) 0.048(3) -0.015(3) -0.016(3) -0.032(3) O9 0.040(3) 0.071(3) 0.042(2) -0.004(2) -0.010(2) 0.007(2) F5 0.123(4) 0.068(2) 0.043(2) -0.0109(19) 0.015(2) -0.067(3) F6 0.103(4) 0.085(3) 0.029(2) -0.0235(19) 0.019(2) 0.004(2) F4 0.060(3) 0.047(2) 0.082(3) 0.013(2) -0.009(2) 0.0091(19) O13 0.0270(19) 0.0208(14) 0.0207(16) -0.0070(12) -0.0043(13) 0.0004(13) N2 0.027(2) 0.0129(15) 0.0172(18) -0.0049(13) 0.0008(15) -0.0036(14) C11 0.027(3) 0.0160(18) 0.0136(19) -0.0082(15) 0.0025(17) -0.0058(17) C12 0.028(3) 0.021(2) 0.026(2) -0.0115(18) -0.0002(19) -0.0057(19) N3 0.029(2) 0.0163(16) 0.0171(18) -0.0100(14) 0.0009(15) -0.0019(15) C17 0.019(2) 0.0170(18) 0.020(2) -0.0110(16) 0.0026(17) -0.0057(16) C19 0.033(3) 0.0140(17) 0.0131(19) -0.0078(15) 0.0015(18) -0.0033(17) C14 0.028(3) 0.0172(18) 0.0142(19) -0.0101(16) 0.0030(17) -0.0034(17) C13 0.021(3) 0.023(2) 0.028(2) -0.0120(19) -0.001(2) -0.0003(18) C16 0.025(3) 0.023(2) 0.036(3) -0.018(2) -0.001(2) -0.0011(19) C18 0.042(3) 0.018(2) 0.028(3) -0.010(2) -0.003(2) -0.003(2) C10 0.048(3) 0.024(2) 0.017(2) -0.0077(18) -0.008(2) -0.006(2) C20 0.025(3) 0.023(2) 0.019(2) -0.0111(18) 0.0068(19) -0.0041(18) C2 0.045(3) 0.023(2) 0.021(2) -0.0154(18) 0.006(2) -0.006(2) O6 0.068(3) 0.0314(18) 0.0260(19) -0.0143(16) -0.0091(18) 0.0171(18) O3 0.041(2) 0.0215(17) 0.0200(18) -0.0149(15) 0.0104(16) -0.0103(16) S3 0.0263(8) 0.0311(7) 0.0875(13) -0.0225(8) 0.0192(8) -0.0064(6) C27 0.061(5) 0.047(4) 0.080(6) -0.027(4) -0.004(4) -0.014(4) O12 0.035(2) 0.0407(19) 0.031(2) -0.0101(16) 0.0092(16) -0.0136(17) O11 0.081(5) 0.045(3) 0.417(16) -0.055(6) -0.142(8) 0.029(3) O10 0.241(11) 0.190(8) 0.211(9) -0.142(8) 0.211(9) -0.158(8) F9 0.055(4) 0.073(3) 0.273(10) -0.083(5) -0.029(5) -0.015(3) F8 0.090(4) 0.047(2) 0.204(7) -0.056(3) -0.048(4) 0.013(2) F7 0.285(11) 0.263(9) 0.160(7) -0.182(8) 0.113(7) -0.173(9) O14 0.032(2) 0.0264(16) 0.0294(18) -0.0073(14) -0.0001(15) -0.0134(15) O15 0.0212(19) 0.0300(17) 0.034(2) -0.0006(15) 0.0075(15) -0.0040(14) N4 0.038(4) 0.073(4) 0.060(4) -0.022(3) -0.009(3) 0.005(3) C29 0.023(4) 0.082(6) 0.056(4) -0.041(4) 0.006(3) -0.012(4) C28 0.069(6) 0.069(5) 0.084(6) -0.023(4) 0.017(4) -0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C9 1.246(4) . ? O2 Yb1 2.222(3) 1_564 ? C9 N2 1.334(5) . ? C9 C6 1.498(6) . ? C15 C16 1.385(6) . ? C15 C14 1.387(7) . ? C15 H15 0.9500 . ? Yb1 O3 2.185(4) 1_556 ? Yb1 O2 2.222(3) 1_546 ? Yb1 O4 2.248(4) . ? Yb1 O1 2.253(3) . ? Yb1 O14 2.281(3) . ? Yb1 O15 2.300(3) . ? Yb1 O13 2.373(3) . ? S2 O7 1.407(6) . ? S2 O9 1.424(5) . ? S2 O8 1.463(4) . ? S2 C26 1.822(5) . ? S1 O5 1.416(4) . ? S1 O6 1.437(4) . ? S1 O4 1.465(4) . ? S1 C25 1.828(7) . ? C5 C6 1.389(8) . ? C5 C4 1.399(9) . ? C5 H5 0.9500 . ? C4 C3 1.385(7) . ? C4 H4 0.9500 . ? C3 C8 1.369(8) . ? C3 N1 1.453(8) . ? C6 C7 1.386(6) . ? C8 C7 1.401(6) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? C26 F4 1.294(7) . ? C26 F6 1.304(6) . ? C26 F5 1.326(6) . ? C22 C21 1.366(6) . ? C22 C23 1.395(6) . ? C22 C1 1.499(6) . ? C21 C20 1.387(6) . ? C21 H21 0.9500 . ? C1 O1 1.245(5) . ? C1 N1 1.338(6) . ? C23 C24 1.391(6) . ? C23 H23 0.9500 . ? C24 C19 1.394(7) . ? C24 H24 0.9500 . ? N1 C2 1.481(7) . ? C25 F2 1.321(8) . ? C25 F3 1.324(7) . ? C25 F1 1.331(7) . ? N2 C11 1.436(5) . ? N2 C10 1.475(5) . ? C11 C16 1.381(6) . ? C11 C12 1.386(6) . ? C12 C13 1.390(6) . ? C12 H12 0.9500 . ? N3 C17 1.316(5) . ? N3 C19 1.432(5) . ? N3 C18 1.485(5) . ? C17 O3 1.246(5) . ? C17 C14 1.511(5) . ? C19 C20 1.391(6) . ? C14 C13 1.392(6) . ? C13 H13 0.9500 . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C20 H20 0.9500 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 Yb1 2.185(4) 1_554 ? S3 O11 1.358(6) . ? S3 O10 1.401(8) . ? S3 O12 1.404(4) . ? S3 C27 1.794(7) . ? C27 F7 1.237(10) . ? C27 F8 1.308(9) . ? C27 F9 1.330(9) . ? N4 C29 1.124(10) . ? C29 C28 1.453(11) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 O2 Yb1 168.7(3) . 1_564 ? O2 C9 N2 121.1(4) . . ? O2 C9 C6 120.1(4) . . ? N2 C9 C6 118.7(3) . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? O3 Yb1 O2 92.10(12) 1_556 1_546 ? O3 Yb1 O4 162.58(11) 1_556 . ? O2 Yb1 O4 86.50(12) 1_546 . ? O3 Yb1 O1 109.51(12) 1_556 . ? O2 Yb1 O1 134.37(11) 1_546 . ? O4 Yb1 O1 83.35(11) . . ? O3 Yb1 O14 80.80(13) 1_556 . ? O2 Yb1 O14 150.00(11) 1_546 . ? O4 Yb1 O14 91.78(13) . . ? O1 Yb1 O14 74.87(11) . . ? O3 Yb1 O15 81.74(14) 1_556 . ? O2 Yb1 O15 72.09(12) 1_546 . ? O4 Yb1 O15 114.13(14) . . ? O1 Yb1 O15 71.99(11) . . ? O14 Yb1 O15 134.43(13) . . ? O3 Yb1 O13 83.77(13) 1_556 . ? O2 Yb1 O13 75.57(11) 1_546 . ? O4 Yb1 O13 79.06(12) . . ? O1 Yb1 O13 144.14(11) . . ? O14 Yb1 O13 74.71(11) . . ? O15 Yb1 O13 143.86(11) . . ? O7 S2 O9 115.9(4) . . ? O7 S2 O8 116.2(4) . . ? O9 S2 O8 109.5(3) . . ? O7 S2 C26 105.0(3) . . ? O9 S2 C26 104.8(3) . . ? O8 S2 C26 104.0(2) . . ? O5 S1 O6 117.2(2) . . ? O5 S1 O4 113.7(2) . . ? O6 S1 O4 112.8(2) . . ? O5 S1 C25 104.9(3) . . ? O6 S1 C25 104.2(3) . . ? O4 S1 C25 101.8(3) . . ? C6 C5 C4 119.8(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C3 C4 C5 118.9(5) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C8 C3 C4 122.0(4) . . ? C8 C3 N1 119.7(5) . . ? C4 C3 N1 118.3(5) . . ? C7 C6 C5 120.1(4) . . ? C7 C6 C9 119.6(4) . . ? C5 C6 C9 120.2(4) . . ? C3 C8 C7 118.8(4) . . ? C3 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C6 C7 C8 120.2(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? F4 C26 F6 108.8(5) . . ? F4 C26 F5 107.8(5) . . ? F6 C26 F5 107.1(5) . . ? F4 C26 S2 112.3(4) . . ? F6 C26 S2 110.0(4) . . ? F5 C26 S2 110.7(4) . . ? C21 C22 C23 120.8(4) . . ? C21 C22 C1 119.4(4) . . ? C23 C22 C1 119.6(4) . . ? C22 C21 C20 120.9(4) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? O1 C1 N1 121.3(4) . . ? O1 C1 C22 120.6(3) . . ? N1 C1 C22 118.1(4) . . ? C24 C23 C22 119.2(4) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C19 119.4(4) . . ? C23 C24 H24 120.3 . . ? C19 C24 H24 120.3 . . ? C1 N1 C3 121.2(5) . . ? C1 N1 C2 120.2(4) . . ? C3 N1 C2 118.5(4) . . ? C1 O1 Yb1 146.0(3) . . ? F2 C25 F3 107.9(6) . . ? F2 C25 F1 107.5(6) . . ? F3 C25 F1 108.2(5) . . ? F2 C25 S1 112.2(4) . . ? F3 C25 S1 109.8(5) . . ? F1 C25 S1 111.1(5) . . ? S1 O4 Yb1 141.0(2) . . ? C9 N2 C11 121.2(3) . . ? C9 N2 C10 121.0(3) . . ? C11 N2 C10 115.8(3) . . ? C16 C11 C12 120.9(4) . . ? C16 C11 N2 120.8(4) . . ? C12 C11 N2 118.3(4) . . ? C11 C12 C13 119.5(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C17 N3 C19 122.7(3) . . ? C17 N3 C18 119.2(4) . . ? C19 N3 C18 118.1(4) . . ? O3 C17 N3 121.2(4) . . ? O3 C17 C14 119.8(4) . . ? N3 C17 C14 119.0(3) . . ? C20 C19 C24 120.9(4) . . ? C20 C19 N3 119.7(4) . . ? C24 C19 N3 119.3(4) . . ? C15 C14 C13 119.9(4) . . ? C15 C14 C17 119.6(4) . . ? C13 C14 C17 120.5(4) . . ? C12 C13 C14 119.7(4) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C11 C16 C15 119.3(4) . . ? C11 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C21 C20 C19 118.6(4) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C17 O3 Yb1 153.8(3) . 1_554 ? O11 S3 O10 112.4(8) . . ? O11 S3 O12 116.6(4) . . ? O10 S3 O12 113.1(5) . . ? O11 S3 C27 104.9(5) . . ? O10 S3 C27 103.8(4) . . ? O12 S3 C27 104.5(3) . . ? F7 C27 F8 107.8(9) . . ? F7 C27 F9 108.4(8) . . ? F8 C27 F9 106.6(6) . . ? F7 C27 S3 112.6(6) . . ? F8 C27 S3 109.0(6) . . ? F9 C27 S3 112.1(6) . . ? N4 C29 C28 179.3(9) . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.077 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.128 #===END