Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Glen Berenger Deacon' _publ_contact_author_address ; School of Chemistry Monash University Clayton 3800 AUSTRALIA ; _publ_contact_author_email GLEN.DEACON@SCI.MONASH.EDU.AU _publ_section_title ; Manipulation of reaction pathways in redox transmetallation-ligand exchange syntheses of lanthanoid(II)/(III) aryloxide complexes. ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; loop_ _publ_author_name 'Glen Berenger Deacon' 'Gary D. Fallon' 'Craig M. Forsyth' 'Stuart C. Harris' 'Peter Junk' ; B.W.Skelton ; A.H.White #===END data_ybarth _database_code_depnum_ccdc_archive 'CCDC 281263' _audit_creation_method Xtal3.6 _audit_creation_date 05-07-19 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C46 H78 O8 Yb' _chemical_formula_moiety 'C42 H70 O7 Yb, C4 H8 O' _chemical_formula_weight 932.12 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 9.827(5) _cell_length_b 15.393(6) _cell_length_c 31.677(8) _cell_angle_alpha 90.00000 _cell_angle_beta 93.95(2) _cell_angle_gamma 90.00000 _cell_volume 4780(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.30 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 9.0 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.99 _exptl_crystal_description prism _exptl_crystal_size_max .28 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .17 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Philips PW1100 Diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SHELXTL PLUS ; _exptl_absorpt_correction_T_min .601 _exptl_absorpt_correction_T_max .723 _diffrn_reflns_number 11499 _reflns_number_total 11499 _reflns_Friedel_coverage 0 _reflns_number_gt 4874 _reflns_threshold_expression 'I > 3.00 sig(I)' _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .044 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_standards_number 3 _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .047 _refine_ls_wR_factor_gt .045 _refine_ls_goodness_of_fit_gt 1.18 _refine_ls_number_reflns 4874 _refine_ls_number_parameters 496 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .004 _refine_diff_density_min -.9 _refine_diff_density_max 1.20 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction shelx _computing_structure_solution shelx _computing_structure_refinement shelx _computing_molecular_graphics shelx _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 184 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 312 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Yb ? 0 4 .299 .973 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Yb 0.01022(4) 0.22727(3) 0.13950(1) 0.0384(1) Uani ? ? 1.0 ? ? O1 -0.1352(5) 0.2431(3) 0.0827(2) 0.046(2) Uani ? ? 1.00000 ? ? O2 0.1531(5) 0.2918(3) 0.1874(2) 0.046(2) Uani ? ? 1.00000 ? ? O3 0.2002(6) 0.2137(4) 0.0938(2) 0.057(2) Uani ? ? 1.00000 ? ? O4 -0.1797(5) 0.2550(4) 0.1844(2) 0.057(2) Uani ? ? 1.00000 ? ? O5 0.0086(7) 0.0749(4) 0.1581(2) 0.061(3) Uani ? ? 1.00000 ? ? O6 -0.4666(10) 0.2600(6) -0.06052(3) 0.123(5) Uani ? ? 1.00000 ? ? O7 0.4667(10) 0.4628(5) 0.3137(3) 0.114(4) Uani ? ? 1.00000 ? ? C1 -0.2145(8) 0.2482(5) 0.0470(3) 0.043(3) Uani ? ? 1.00000 ? ? C2 -0.2516(9) 0.3303(7) 0.0293(3) 0.046(4) Uani ? ? 1.00000 ? ? C3 -0.3365(11) 0.3350(7) -0.0080(3) 0.068(5) Uani ? ? 1.00000 ? ? C4 -0.3820(11) 0.2613(9) -0.0280(3) 0.072(5) Uani ? ? 1.00000 ? ? C5 -0.3478(10) 0.1810(8) -0.0118(3) 0.066(5) Uani ? ? 1.00000 ? ? C6 -0.2637(9) 0.1725(7) 0.0254(3) 0.048(4) Uani ? ? 1.00000 ? ? C7 -0.2299(11) 0.0811(7) 0.0415(3) 0.060(4) Uani ? ? 1.00000 ? ? C8 -0.0766(10) 0.0665(7) 0.0449(3) 0.075(5) Uani ? ? 1.00000 ? ? C9 -0.2871(11) 0.0672(7) 0.0835(3) 0.085(5) Uani ? ? 1.00000 ? ? C10 -0.2872(12) 0.0094(7) 0.0114(4) 0.095(5) Uani ? ? 1.00000 ? ? C11 -0.2025(11) 0.4161(7) 0.0499(3) 0.065(4) Uani ? ? 1.00000 ? ? C12 -0.2573(11) 0.4235(6) 0.0947(3) 0.076(5) Uani ? ? 1.00000 ? ? C13 -0.0469(11) 0.4209(7) 0.0531(3) 0.082(5) Uani ? ? 1.00000 ? ? C14 -0.2515(13) 0.4974(6) 0.0252(3) 0.102(6) Uani ? ? 1.00000 ? ? C15 -0.4822(15) 0.3328(10) -0.0872(4) 0.146(9) Uani ? ? 1.00000 ? ? C16 0.2291(8) 0.3313(6) 0.2178(3) 0.043(3) Uani ? ? 1.00000 ? ? C17 0.2588(9) 0.4223(6) 0.2159(3) 0.050(3) Uani ? ? 1.00000 ? ? C18 0.3389(10) 0.4601(6) 0.2486(3) 0.062(4) Uani ? ? 1.00000 ? ? C19 0.3919(11) 0.4157(8) 0.2832(3) 0.073(5) Uani ? ? 1.00000 ? ? C20 0.3654(9) 0.3282(7) 0.2857(3) 0.058(4) Uani ? ? 1.00000 ? ? C21 0.2874(8) 0.2843(7) 0.2536(2) 0.045(3) Uani ? ? 1.00000 ? ? C22 0.2654(11) 0.1853(8) 0.2585(3) 0.059(4) Uani ? ? 1.00000 ? ? C23 0.1150(10) 0.1650(6) 0.2601(3) 0.073(4) Uani ? ? 1.00000 ? ? C24 0.3239(11) 0.1378(6) 0.2217(3) 0.078(5) Uani ? ? 1.00000 ? ? C25 0.3377(12) 0.1473(7) 0.2984(3) 0.088(5) Uani ? ? 1.00000 ? ? C26 0.2034(10) 0.4776(6) 0.1782(3) 0.059(4) Uani ? ? 1.00000 ? ? C27 0.2633(10) 0.4460(6) 0.1372(3) 0.076(4) Uani ? ? 1.00000 ? ? C28 0.0472(10) 0.4745(6) 0.1737(3) 0.066(4) Uani ? ? 1.00000 ? ? C29 0.2426(12) 0.5736(6) 0.1820(3) 0.095(5) Uani ? ? 1.00000 ? ? C30 0.5135(12) 0.4217(8) 0.3503(3) 0.114(6) Uani ? ? 1.00000 ? ? C31 0.1925(11) 0.2216(9) 0.0483(3) 0.094(5) Uani ? ? 1.00000 ? ? C32 0.3128(13) 0.2677(10) 0.0378(4) 0.131(7) Uani ? ? 1.00000 ? ? C33 0.4132(10) 0.2602(8) 0.0739(4) 0.098(6) Uani ? ? 1.00000 ? ? C34 0.3429(10) 0.2119(7) 0.1070(3) 0.079(5) Uani ? ? 1.00000 ? ? C35 -0.3210(9) 0.2420(7) 0.1720(3) 0.070(4) Uani ? ? 1.00000 ? ? C36 -0.3943(10) 0.3185(8) 0.1912(4) 0.092(5) Uani ? ? 1.00000 ? ? C37 -0.2955(12) 0.3525(10) 0.2236(5) 0.146(8) Uani ? ? 1.00000 ? ? C38 -0.1747(10) 0.3005(7) 0.2244(3) 0.078(5) Uani ? ? 1.00000 ? ? C39 0.1054(11) 0.0101(6) 0.1454(3) 0.077(5) Uani ? ? 1.00000 ? ? C40 0.0911(15) -0.0630(7) 0.1749(5) 0.112(7) Uani ? ? 1.00000 ? ? C41 -0.0374(16) -0.0566(9) 0.1903(5) 0.134(8) Uani ? ? 1.00000 ? ? C42 -0.0858(11) 0.0304(7) 0.1840(3) 0.075(4) Uani ? ? 1.00000 ? ? O8 -0.9292(22) 0.1718(9) -0.0743(7) 0.256(11) Uani ? ? 1.00000 ? ? C43 -1.0253(26) 0.2350(21) -0.0615(7) 0.300(22) Uani ? ? 1.00000 ? ? C44 -1.0435(31) 0.2785(19) -0.0891(11) 0.354(28) Uani ? ? 1.00000 ? ? C45 -0.9175(33) 0.2992(15) -0.1042(9) 0.300(22) Uani ? ? 1.00000 ? ? C46 -0.8504(18) 0.2307(16) -0.0897(8) 0.201(14) Uani ? ? 1.00000 ? ? H3A -0.3623 0.3901 -0.0203 0.080 Uiso ? ? 1.0000 ? ? H5A -0.3835 0.1300 -0.0261 0.080 Uiso ? ? 1.0000 ? ? H8A -0.0359 0.1090 0.0640 0.080 Uiso ? ? 1.0000 ? ? H8B -0.0552 0.0093 0.0555 0.080 Uiso ? ? 1.0000 ? ? H8C -0.0417 0.0734 0.0175 0.080 Uiso ? ? 1.0000 ? ? H9A -0.3843 0.0751 0.0807 0.080 Uiso ? ? 1.0000 ? ? H9B -0.2665 0.0098 0.0939 0.080 Uiso ? ? 1.0000 ? ? H9C -0.2473 0.1092 0.1031 0.080 Uiso ? ? 1.0000 ? ? H10A -0.3847 0.0146 0.0081 0.080 Uiso ? ? 1.0000 ? ? H10B -0.2499 0.0170 -0.0156 0.080 Uiso ? ? 1.0000 ? ? H10C -0.2633 -0.0472 0.0224 0.080 Uiso ? ? 1.0000 ? ? H12A -0.2263 0.3747 0.1115 0.080 Uiso ? ? 1.0000 ? ? H12B -0.2245 0.4762 0.1080 0.080 Uiso ? ? 1.0000 ? ? H12C -0.3552 0.4241 0.0921 0.080 Uiso ? ? 1.0000 ? ? H13A -0.0104 0.3719 0.0689 0.080 Uiso ? ? 1.0000 ? ? H13B -0.0146 0.4201 0.0252 0.080 Uiso ? ? 1.0000 ? ? H13C -0.0180 0.4736 0.0672 0.080 Uiso ? ? 1.0000 ? ? H14A -0.2195 0.4952 -0.0027 0.080 Uiso ? ? 1.0000 ? ? H14B -0.3495 0.4974 0.0233 0.080 Uiso ? ? 1.0000 ? ? H14C -0.2187 0.5495 0.0392 0.080 Uiso ? ? 1.0000 ? ? H15A -0.5426 0.3260 -0.1121 0.080 Uiso ? ? 1.0000 ? ? H15B -0.5174 0.3767 -0.0694 0.080 Uiso ? ? 1.0000 ? ? H15C -0.3936 0.3498 -0.0952 0.080 Uiso ? ? 1.0000 ? ? H18A 0.3587 0.5210 0.2471 0.080 Uiso ? ? 1.0000 ? ? H20A 0.4025 0.2958 0.3098 0.080 Uiso ? ? 1.0000 ? ? H23A 0.0786 0.1958 0.2831 0.080 Uiso ? ? 1.0000 ? ? H23B 0.0672 0.1823 0.2340 0.080 Uiso ? ? 1.0000 ? ? H23C 0.1041 0.1037 0.2641 0.080 Uiso ? ? 1.0000 ? ? H24A 0.2831 0.1592 0.1953 0.080 Uiso ? ? 1.0000 ? ? H24B 0.4207 0.1469 0.2228 0.080 Uiso ? ? 1.0000 ? ? H24C 0.3053 0.0768 0.2241 0.080 Uiso ? ? 1.0000 ? ? H25A 0.3042 0.1754 0.3227 0.080 Uiso ? ? 1.0000 ? ? H25B 0.3190 0.0862 0.2995 0.080 Uiso ? ? 1.0000 ? ? H25C 0.4344 0.1563 0.2983 0.080 Uiso ? ? 1.0000 ? ? H27A 0.3611 0.4484 0.1401 0.080 Uiso ? ? 1.0000 ? ? H27B 0.2346 0.3871 0.1321 0.080 Uiso ? ? 1.0000 ? ? H27C 0.2303 0.4819 0.1139 0.080 Uiso ? ? 1.0000 ? ? H28A 0.0184 0.4151 0.1710 0.080 Uiso ? ? 1.0000 ? ? H28B 0.0106 0.4997 0.1982 0.080 Uiso ? ? 1.0000 ? ? H28C 0.0147 0.5064 0.1490 0.080 Uiso ? ? 1.0000 ? ? H29A 0.3402 0.5786 0.1850 0.080 Uiso ? ? 1.0000 ? ? H29B 0.2084 0.6045 0.1571 0.080 Uiso ? ? 1.0000 ? ? H29C 0.2042 0.5978 0.2064 0.080 Uiso ? ? 1.0000 ? ? H30A 0.5645 0.4607 0.3690 0.080 Uiso ? ? 1.0000 ? ? H30B 0.4372 0.3993 0.3642 0.080 Uiso ? ? 1.0000 ? ? H30C 0.5711 0.3745 0.3428 0.080 Uiso ? ? 1.0000 ? ? H31A 0.1081 0.2480 0.0380 0.080 Uiso ? ? 1.0000 ? ? H31B 0.1983 0.1645 0.0364 0.080 Uiso ? ? 1.0000 ? ? H32A 0.2867 0.3276 0.0346 0.080 Uiso ? ? 1.0000 ? ? H32B 0.3493 0.2482 0.0121 0.080 Uiso ? ? 1.0000 ? ? H33A 0.4426 0.3158 0.0849 0.080 Uiso ? ? 1.0000 ? ? H33B 0.4916 0.2291 0.0655 0.080 Uiso ? ? 1.0000 ? ? H34A 0.3745 0.1528 0.1082 0.080 Uiso ? ? 1.0000 ? ? H34B 0.3594 0.2379 0.1344 0.080 Uiso ? ? 1.0000 ? ? H35A -0.3520 0.1877 0.1828 0.080 Uiso ? ? 1.0000 ? ? H35B -0.3358 0.2419 0.1418 0.080 Uiso ? ? 1.0000 ? ? H36A -0.4738 0.2987 0.2044 0.080 Uiso ? ? 1.0000 ? ? H36B -0.4216 0.3606 0.1699 0.080 Uiso ? ? 1.0000 ? ? H37A -0.3331 0.3553 0.2507 0.080 Uiso ? ? 1.0000 ? ? H37B -0.2714 0.4103 0.2154 0.080 Uiso ? ? 1.0000 ? ? H38A -0.0926 0.3342 0.2285 0.080 Uiso ? ? 1.0000 ? ? H38B -0.1777 0.2592 0.2470 0.080 Uiso ? ? 1.0000 ? ? H39A 0.1962 0.0336 0.1475 0.080 Uiso ? ? 1.0000 ? ? H39B 0.0830 -0.0084 0.1169 0.080 Uiso ? ? 1.0000 ? ? H40A 0.1594 -0.0580 0.1979 0.080 Uiso ? ? 1.0000 ? ? H40B 0.1031 -0.1177 0.1610 0.080 Uiso ? ? 1.0000 ? ? H41A -0.0340 -0.0715 0.2198 0.080 Uiso ? ? 1.0000 ? ? H41B -0.0983 -0.0961 0.1750 0.080 Uiso ? ? 1.0000 ? ? H42A -0.1761 0.0314 0.1703 0.080 Uiso ? ? 1.0000 ? ? H42B -0.0876 0.0598 0.2107 0.080 Uiso ? ? 1.0000 ? ? H43A -1.0129 0.2494 -0.0320 0.080 Uiso ? ? 1.0000 ? ? H43B -1.1073 0.2013 -0.0657 0.080 Uiso ? ? 1.0000 ? ? H44A -1.0469 0.3285 -0.0711 0.080 Uiso ? ? 1.0000 ? ? H44B -1.1243 0.2770 -0.1079 0.080 Uiso ? ? 1.0000 ? ? H45A -0.8741 0.3550 -0.1019 0.080 Uiso ? ? 1.0000 ? ? H45B -0.9406 0.2874 -0.1336 0.080 Uiso ? ? 1.0000 ? ? H46A -0.8019 0.2031 -0.1113 0.080 Uiso ? ? 1.0000 ? ? H46B -0.7859 0.2547 -0.0688 0.080 Uiso ? ? 1.0000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Yb 0.0342(2) 0.0437(2) 0.0375(2) -0.0001(3) 0.0035(1) -0.0012(3) O1 0.051(3) 0.044(4) 0.042(3) 0.002(3) 0.000(3) -0.005(3) O2 0.048(3) 0.047(4) 0.042(3) -0.002(3) 0.000(3) -0.003(3) O3 0.045(4) 0.072(5) 0.056(4) -0.006(3) 0.015(3) 0.002(3) O4 0.038(3) 0.076(6) 0.058(4) 0.003(3) 0.011(3) -0.016(3) O5 0.071(5) 0.057(4) 0.054(4) -0.008(4) 0.004(4) 0.009(3) O6 0.144(8) 0.138(9) 0.078(6) -0.005(7) -0.055(6) 0.023(5) O7 0.142(8) 0.120(7) 0.076(6) -0.068(6) -0.031(6) -0.015(5) C1 0.041(5) 0.051(8) 0.036(5) -0.001(4) 0.004(4) -0.004(4) C2 0.049(6) 0.050(7) 0.039(5) 0.001(5) 0.006(5) -0.002(5) C3 0.072(8) 0.081(9) 0.049(7) 0.000(7) -0.016(6) 0.018(6) C4 0.068(7) 0.100(11) 0.045(6) 0.005(7) -0.010(5) 0.008(6) C5 0.056(7) 0.088(9) 0.054(7) -0.007(7) -0.002(6) -0.012(7) C6 0.034(5) 0.052(7) 0.058(7) 0.002(5) 0.005(5) 0.001(6) C7 0.064(7) 0.054(8) 0.061(7) 0.000(6) -0.009(6) -0.006(6) C8 0.079(8) 0.083(8) 0.060(7) 0.020(6) -0.014(6) -0.021(6) C9 0.083(9) 0.073(8) 0.098(9) -0.017(7) 0.001(8) 0.023(7) C10 0.100(10) 0.067(8) 0.114(10) 0.000(7) -0.025(8) -0.019(7) C11 0.069(8) 0.060(8) 0.068(7) -0.002(6) 0.013(6) 0.011(6) C12 0.084(8) 0.057(7) 0.088(8) -0.006(6) 0.001(7) -0.009(6) C13 0.089(9) 0.077(9) 0.078(8) -0.024(7) 0.005(7) 0.006(6) C14 0.131(12) 0.054(8) 0.117(11) -0.011(8) -0.025(9) 0.025(7) C15 0.132(14) 0.215(19) 0.083(10) 0.001(13) -0.049(9) 0.003(11) C16 0.030(5) 0.054(6) 0.049(6) -0.004(4) 0.016(4) -0.012(5) C17 0.040(5) 0.052(6) 0.058(6) -0.002(5) 0.008(5) -0.006(5) C18 0.081(8) 0.042(6) 0.062(7) -0.024(5) 0.010(6) -0.011(5) C19 0.064(7) 0.081(9) 0.073(8) -0.023(6) -0.003(6) -0.018(7) C20 0.043(6) 0.081(8) 0.051(6) -0.011(6) -0.001(5) 0.000(6) C21 0.040(5) 0.057(8) 0.039(5) 0.006(6) 0.000(4) -0.002(6) C22 0.067(7) 0.066(7) 0.043(6) 0.000(6) 0.003(5) 0.001(5) C23 0.074(8) 0.085(8) 0.059(6) -0.028(6) 0.007(6) 0.013(6) C24 0.097(9) 0.055(7) 0.083(8) 0.002(7) 0.011(7) -0.002(6) C25 0.092(9) 0.082(9) 0.085(9) -0.001(7) -0.027(8) 0.009(7) C26 0.061(7) 0.047(6) 0.067(7) -0.012(5) 0.000(5) 0.001(5) C27 0.078(8) 0.088(8) 0.063(7) 0.005(6) 0.016(6) 0.014(6) C28 0.078(8) 0.048(6) 0.072(7) 0.010(6) 0.007(6) 0.006(5) C29 0.123(11) 0.063(8) 0.098(9) -0.009(7) -0.004(8) 0.003(7) C30 0.091(10) 0.165(13) 0.082(10) -0.028(9) -0.018(8) -0.057(9) C31 0.071(7) 0.162(12) 0.051(6) -0.023(8) 0.015(6) -0.016(8) C32 0.104(10) 0.209(16) 0.083(9) -0.045(12) 0.025(8) 0.030(10) C33 0.047(6) 0.149(13) 0.097(9) -0.011(7) 0.011(6) -0.011(8) C34 0.051(6) 0.104(10) 0.085(8) 0.016(6) 0.021(6) 0.013(7) C35 0.043(6) 0.079(8) 0.089(7) -0.013(6) 0.013(5) -0.012(6) C36 0.043(6) 0.135(11) 0.100(9) 0.024(7) 0.008(6) -0.021(8) C37 0.079(10) 0.190(16) 0.166(14) 0.041(10) -0.013(10) -0.115(12) C38 0.062(7) 0.114(10) 0.058(6) 0.003(6) 0.014(5) -0.022(6) C39 0.084(8) 0.059(7) 0.087(8) 0.018(6) 0.006(7) 0.003(6) C40 0.130(13) 0.048(8) 0.159(14) 0.010(8) 0.012(11) 0.036(8) C41 0.163(16) 0.087(11) 0.163(15) 0.002(11) 0.080(13) 0.041(10) C42 0.074(8) 0.077(8) 0.075(8) -0.017(6) 0.004(6) 0.018(6) O8 0.265(20) 0.135(12) 0.381(25) 0.016(13) 0.111(19) 0.078(14) C43 0.265(28) 0.488(54) 0.168(21) 0.190(34) 0.165(22) 0.077(27) C44 0.219(38) 0.411(46) 0.439(57) 0.115(34) 0.070(38) 0.300(41) C45 0.433(53) 0.139(22) 0.346(34) -0.013(27) 0.155(35) 0.149(23) C46 0.109(15) 0.171(21) 0.323(32) -0.058(17) 0.026(17) 0.011(22) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Yb O1 . . 2.233(6) ? Yb O2 . . 2.229(5) ? Yb O3 . . 2.449(6) ? Yb O4 . . 2.461(6) ? Yb O5 . . 2.419(6) ? O1 C1 . . 1.331(10) ? O2 C16 . . 1.325(10) ? O3 C31 . . 1.443(11) ? O3 C34 . . 1.436(11) ? O4 C35 . . 1.431(10) ? O4 C38 . . 1.446(12) ? O5 C39 . . 1.454(12) ? O5 C42 . . 1.452(13) ? O6 C4 . . 1.279(11) ? O6 C15 . . 1.406(16) ? O7 C19 . . 1.379(14) ? O7 C30 . . 1.372(14) ? C1 C2 . . 1.420(13) ? C1 C6 . . 1.419(13) ? C2 C3 . . 1.401(13) ? C2 C11 . . 1.536(15) ? C3 C4 . . 1.360(16) ? C3 H3A . . .960 ? C4 C5 . . 1.371(18) ? C5 C6 . . 1.398(13) ? C5 H5A . . .961 ? C6 C7 . . 1.525(15) ? C7 C8 . . 1.520(15) ? C7 C9 . . 1.495(14) ? C7 C10 . . 1.540(15) ? C8 H8A . . .960 ? C8 H8B . . .960 ? C8 H8C . . .961 ? C9 H9A . . .961 ? C9 H9B . . .960 ? C9 H9C . . .961 ? C10 H10A . . .960 ? C10 H10B . . .961 ? C10 H10C . . .961 ? C11 C12 . . 1.556(14) ? C11 C13 . . 1.527(15) ? C11 C14 . . 1.536(14) ? C12 H12A . . .958 ? C12 H12B . . .960 ? C12 H12C . . .960 ? C13 H13A . . .961 ? C13 H13B . . .959 ? C13 H13C . . .960 ? C14 H14A . . .959 ? C14 H14B . . .961 ? C14 H14C . . .961 ? C15 H15A . . .960 ? C15 H15B . . .960 ? C15 H15C . . .960 ? C16 C17 . . 1.433(13) ? C16 C21 . . 1.431(12) ? C17 C18 . . 1.385(13) ? C17 C26 . . 1.535(13) ? C18 C19 . . 1.364(14) ? C18 H18A . . .959 ? C19 C20 . . 1.375(16) ? C20 C21 . . 1.404(12) ? C20 H20A . . .962 ? C21 C22 . . 1.548(16) ? C22 C23 . . 1.515(15) ? C22 C24 . . 1.522(15) ? C22 C25 . . 1.523(14) ? C23 H23A . . .959 ? C23 H23B . . .960 ? C23 H23C . . .959 ? C24 H24A . . .960 ? C24 H24B . . .960 ? C24 H24C . . .961 ? C25 H25A . . .961 ? C25 H25B . . .959 ? C25 H25C . . .961 ? C26 C27 . . 1.541(14) ? C26 C28 . . 1.533(14) ? C26 C29 . . 1.530(13) ? C27 H27A . . .960 ? C27 H27B . . .960 ? C27 H27C . . .960 ? C28 H28A . . .959 ? C28 H28B . . .959 ? C28 H28C . . .960 ? C29 H29A . . .960 ? C29 H29B . . .962 ? C29 H29C . . .959 ? C30 H30A . . .960 ? C30 H30B . . .959 ? C30 H30C . . .961 ? C31 C32 . . 1.437(18) ? C31 H31A . . .960 ? C31 H31B . . .960 ? C32 C33 . . 1.463(17) ? C32 H32A . . .961 ? C32 H32B . . .960 ? C33 C34 . . 1.493(16) ? C33 H33A . . .961 ? C33 H33B . . .960 ? C34 H34A . . .961 ? C34 H34B . . .959 ? C35 C36 . . 1.528(16) ? C35 H35A . . .961 ? C35 H35B . . .958 ? C36 C37 . . 1.460(18) ? C36 H36A . . .961 ? C36 H36B . . .960 ? C37 C38 . . 1.431(17) ? C37 H37A . . .959 ? C37 H37B . . .961 ? C38 H38A . . .960 ? C38 H38B . . .959 ? C39 C40 . . 1.476(16) ? C39 H39A . . .961 ? C39 H39B . . .958 ? C40 C41 . . 1.39(2) ? C40 H40A . . .959 ? C40 H40B . . .961 ? C41 C42 . . 1.431(18) ? C41 H41A . . .961 ? C41 H41B . . .961 ? C42 H42A . . .961 ? C42 H42B . . .960 ? O8 C43 . . 1.43(3) ? O8 C46 . . 1.31(3) ? C43 C44 . . 1.11(4) ? C43 H43A . . .96 ? C43 H43B . . .96 ? C44 C45 . . 1.39(5) ? C44 H44A . . .96 ? C44 H44B . . .96 ? C45 C46 . . 1.31(3) ? C45 H45A . . .96 ? C45 H45B . . .96 ? C46 H46A . . .96 ? C46 H46B . . .96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Yb O2 . . . 146.96(18) ? O1 Yb O3 . . . 90.3(2) ? O1 Yb O4 . . . 88.7(2) ? O1 Yb O5 . . . 106.7(2) ? O2 Yb O3 . . . 88.3(2) ? O2 Yb O4 . . . 89.8(2) ? O2 Yb O5 . . . 106.3(2) ? O3 Yb O4 . . . 174.9(2) ? O3 Yb O5 . . . 94.6(2) ? O4 Yb O5 . . . 90.5(2) ? Yb O1 C1 . . . 175.0(5) ? Yb O2 C16 . . . 175.2(5) ? Yb O3 C31 . . . 126.4(5) ? Yb O3 C34 . . . 126.8(5) ? C31 O3 C34 . . . 106.0(7) ? Yb O4 C35 . . . 125.3(5) ? Yb O4 C38 . . . 127.5(5) ? C35 O4 C38 . . . 106.4(7) ? Yb O5 C39 . . . 125.6(5) ? Yb O5 C42 . . . 127.6(6) ? C39 O5 C42 . . . 106.8(7) ? C4 O6 C15 . . . 120.7(11) ? C19 O7 C30 . . . 118.8(9) ? O1 C1 C2 . . . 120.5(7) ? O1 C1 C6 . . . 121.4(7) ? C2 C1 C6 . . . 118.1(8) ? C1 C2 C3 . . . 120.1(9) ? C1 C2 C11 . . . 122.2(8) ? C3 C2 C11 . . . 117.7(9) ? C2 C3 C4 . . . 120.5(10) ? C2 C3 H3A . . . 120.9 ? C4 C3 H3A . . . 118.6 ? O6 C4 C3 . . . 124.3(12) ? O6 C4 C5 . . . 114.6(11) ? C3 C4 C5 . . . 120.9(9) ? C4 C5 C6 . . . 121.0(10) ? C4 C5 H5A . . . 119.2 ? C6 C5 H5A . . . 119.8 ? C1 C6 C5 . . . 119.4(10) ? C1 C6 C7 . . . 122.5(8) ? C5 C6 C7 . . . 118.1(9) ? C6 C7 C8 . . . 110.6(9) ? C6 C7 C9 . . . 110.1(9) ? C6 C7 C10 . . . 113.1(8) ? C8 C7 C9 . . . 110.3(8) ? C8 C7 C10 . . . 104.9(9) ? C9 C7 C10 . . . 107.7(9) ? C7 C8 H8A . . . 108.2 ? C7 C8 H8B . . . 110.6 ? C7 C8 H8C . . . 109.5 ? H8A C8 H8B . . . 109.4 ? H8A C8 H8C . . . 109.6 ? H8B C8 H8C . . . 109.5 ? C7 C9 H9A . . . 109.4 ? C7 C9 H9B . . . 110.7 ? C7 C9 H9C . . . 108.5 ? H9A C9 H9B . . . 109.5 ? H9A C9 H9C . . . 109.4 ? H9B C9 H9C . . . 109.3 ? C7 C10 H10A . . . 109.1 ? C7 C10 H10B . . . 108.6 ? C7 C10 H10C . . . 110.8 ? H10A C10 H10B . . . 109.4 ? H10A C10 H10C . . . 109.4 ? H10B C10 H10C . . . 109.5 ? C2 C11 C12 . . . 109.4(8) ? C2 C11 C13 . . . 110.7(8) ? C2 C11 C14 . . . 113.9(8) ? C12 C11 C13 . . . 110.1(8) ? C12 C11 C14 . . . 106.8(8) ? C13 C11 C14 . . . 105.8(9) ? C11 C12 H12A . . . 109.4 ? C11 C12 H12B . . . 109.6 ? C11 C12 H12C . . . 109.3 ? H12A C12 H12B . . . 109.5 ? H12A C12 H12C . . . 109.5 ? H12B C12 H12C . . . 109.5 ? C11 C13 H13A . . . 109.4 ? C11 C13 H13B . . . 109.4 ? C11 C13 H13C . . . 109.6 ? H13A C13 H13B . . . 109.5 ? H13A C13 H13C . . . 109.5 ? H13B C13 H13C . . . 109.5 ? C11 C14 H14A . . . 109.2 ? C11 C14 H14B . . . 108.0 ? C11 C14 H14C . . . 111.2 ? H14A C14 H14B . . . 109.5 ? H14A C14 H14C . . . 109.5 ? H14B C14 H14C . . . 109.4 ? O6 C15 H15A . . . 116.3 ? O6 C15 H15B . . . 103.7 ? O6 C15 H15C . . . 108.2 ? H15A C15 H15B . . . 109.4 ? H15A C15 H15C . . . 109.5 ? H15B C15 H15C . . . 109.5 ? O2 C16 C17 . . . 121.6(8) ? O2 C16 C21 . . . 121.2(8) ? C17 C16 C21 . . . 117.1(8) ? C16 C17 C18 . . . 119.1(8) ? C16 C17 C26 . . . 120.8(8) ? C18 C17 C26 . . . 120.1(8) ? C17 C18 C19 . . . 123.8(9) ? C17 C18 H18A . . . 118.7 ? C19 C18 H18A . . . 117.5 ? O7 C19 C18 . . . 117.1(10) ? O7 C19 C20 . . . 124.6(9) ? C18 C19 C20 . . . 118.3(9) ? C19 C20 C21 . . . 121.7(9) ? C19 C20 H20A . . . 119.4 ? C21 C20 H20A . . . 118.9 ? C16 C21 C20 . . . 120.0(9) ? C16 C21 C22 . . . 121.7(7) ? C20 C21 C22 . . . 118.3(8) ? C21 C22 C23 . . . 110.5(8) ? C21 C22 C24 . . . 109.5(8) ? C21 C22 C25 . . . 113.6(8) ? C23 C22 C24 . . . 110.3(8) ? C23 C22 C25 . . . 107.1(9) ? C24 C22 C25 . . . 105.8(9) ? C22 C23 H23A . . . 109.8 ? C22 C23 H23B . . . 109.5 ? C22 C23 H23C . . . 109.0 ? H23A C23 H23B . . . 109.3 ? H23A C23 H23C . . . 109.6 ? H23B C23 H23C . . . 109.5 ? C22 C24 H24A . . . 110.2 ? C22 C24 H24B . . . 109.1 ? C22 C24 H24C . . . 109.0 ? H24A C24 H24B . . . 109.6 ? H24A C24 H24C . . . 109.5 ? H24B C24 H24C . . . 109.5 ? C22 C25 H25A . . . 109.0 ? C22 C25 H25B . . . 109.1 ? C22 C25 H25C . . . 110.3 ? H25A C25 H25B . . . 109.6 ? H25A C25 H25C . . . 109.4 ? H25B C25 H25C . . . 109.5 ? C17 C26 C27 . . . 110.2(8) ? C17 C26 C28 . . . 110.7(8) ? C17 C26 C29 . . . 113.6(8) ? C27 C26 C28 . . . 110.5(8) ? C27 C26 C29 . . . 105.2(8) ? C28 C26 C29 . . . 106.4(8) ? C26 C27 H27A . . . 110.2 ? C26 C27 H27B . . . 108.4 ? C26 C27 H27C . . . 109.7 ? H27A C27 H27B . . . 109.5 ? H27A C27 H27C . . . 109.5 ? H27B C27 H27C . . . 109.5 ? C26 C28 H28A . . . 109.0 ? C26 C28 H28B . . . 109.9 ? C26 C28 H28C . . . 109.6 ? H28A C28 H28B . . . 109.4 ? H28A C28 H28C . . . 109.6 ? H28B C28 H28C . . . 109.3 ? C26 C29 H29A . . . 109.2 ? C26 C29 H29B . . . 110.0 ? C26 C29 H29C . . . 109.1 ? H29A C29 H29B . . . 109.4 ? H29A C29 H29C . . . 109.6 ? H29B C29 H29C . . . 109.5 ? O7 C30 H30A . . . 111.3 ? O7 C30 H30B . . . 109.1 ? O7 C30 H30C . . . 108.0 ? H30A C30 H30B . . . 109.4 ? H30A C30 H30C . . . 109.5 ? H30B C30 H30C . . . 109.5 ? O3 C31 C32 . . . 106.6(9) ? O3 C31 H31A . . . 111.1 ? O3 C31 H31B . . . 108.3 ? C32 C31 H31A . . . 114.7 ? C32 C31 H31B . . . 106.8 ? H31A C31 H31B . . . 109.1 ? C31 C32 C33 . . . 107.5(10) ? C31 C32 H32A . . . 106.3 ? C31 C32 H32B . . . 113.8 ? C33 C32 H32A . . . 108.6 ? C33 C32 H32B . . . 111.5 ? H32A C32 H32B . . . 108.9 ? C32 C33 C34 . . . 105.6(9) ? C32 C33 H33A . . . 112.5 ? C32 C33 H33B . . . 109.5 ? C34 C33 H33A . . . 109.3 ? C34 C33 H33B . . . 111.4 ? H33A C33 H33B . . . 108.5 ? O3 C34 C33 . . . 106.0(8) ? O3 C34 H34A . . . 109.6 ? O3 C34 H34B . . . 110.9 ? C33 C34 H34A . . . 109.6 ? C33 C34 H34B . . . 111.7 ? H34A C34 H34B . . . 109.0 ? O4 C35 C36 . . . 105.0(8) ? O4 C35 H35A . . . 110.5 ? O4 C35 H35B . . . 110.6 ? C36 C35 H35A . . . 111.0 ? C36 C35 H35B . . . 110.8 ? H35A C35 H35B . . . 108.9 ? C35 C36 C37 . . . 104.3(9) ? C35 C36 H36A . . . 110.4 ? C35 C36 H36B . . . 110.9 ? C37 C36 H36A . . . 109.2 ? C37 C36 H36B . . . 113.1 ? H36A C36 H36B . . . 108.9 ? C36 C37 C38 . . . 108.8(12) ? C36 C37 H37A . . . 111.5 ? C36 C37 H37B . . . 107.8 ? C38 C37 H37A . . . 112.3 ? C38 C37 H37B . . . 107.6 ? H37A C37 H37B . . . 108.5 ? O4 C38 C37 . . . 106.1(9) ? O4 C38 H38A . . . 111.0 ? O4 C38 H38B . . . 109.4 ? C37 C38 H38A . . . 112.9 ? C37 C38 H38B . . . 108.4 ? H38A C38 H38B . . . 109.0 ? O5 C39 C40 . . . 104.8(9) ? O5 C39 H39A . . . 110.2 ? O5 C39 H39B . . . 110.6 ? C40 C39 H39A . . . 111.8 ? C40 C39 H39B . . . 110.2 ? H39A C39 H39B . . . 109.2 ? C39 C40 C41 . . . 107.3(11) ? C39 C40 H40A . . . 109.1 ? C39 C40 H40B . . . 111.0 ? C41 C40 H40A . . . 109.5 ? C41 C40 H40B . . . 111.5 ? H40A C40 H40B . . . 108.5 ? C40 C41 C42 . . . 108.6(12) ? C40 C41 H41A . . . 110.7 ? C40 C41 H41B . . . 109.1 ? C42 C41 H41A . . . 110.4 ? C42 C41 H41B . . . 109.4 ? H41A C41 H41B . . . 108.6 ? O5 C42 C41 . . . 107.5(10) ? O5 C42 H42A . . . 110.1 ? O5 C42 H42B . . . 109.1 ? C41 C42 H42A . . . 111.5 ? C41 C42 H42B . . . 110.1 ? H42A C42 H42B . . . 108.5 ? C43 O8 C46 . . . 93.1(17) ? O8 C43 C44 . . . 105(3) ? O8 C43 H43A . . . 113 ? O8 C43 H43B . . . 99 ? C44 C43 H43A . . . 129 ? C44 C43 H43B . . . 97 ? H43A C43 H43B . . . 108 ? C43 C44 C45 . . . 108(3) ? C43 C44 H44A . . . 92 ? C43 C44 H44B . . . 124 ? C45 C44 H44A . . . 95 ? C45 C44 H44B . . . 121 ? H44A C44 H44B . . . 109 ? C44 C45 C46 . . . 98(2) ? C44 C45 H45A . . . 125 ? C44 C45 H45B . . . 98 ? C46 C45 H45A . . . 119 ? C46 C45 H45B . . . 106 ? H45A C45 H45B . . . 108 ? O8 C46 C45 . . . 113(2) ? O8 C46 H46A . . . 107 ? O8 C46 H46B . . . 113 ? C45 C46 H46A . . . 112 ? C45 C46 H46B . . . 103 ? H46A C46 H46B . . . 109.0 ? _exptl_crystal_F_000 1952 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _reflns_number_observed ? _reflns_d_resolution_high .727 _reflns_d_resolution_low 13.118 _diffrn_reflns_av_sigmaI/netI .062 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .063 _refine_ls_wR_factor_ref .086 _refine_ls_goodness_of_fit_ref 1.18 _refine_ls_shift/su_mean .003 #===END #===END data_sch244 _database_code_depnum_ccdc_archive 'CCDC 281264' _audit_creation_method Xtal3.6 _audit_creation_date 05-09-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C76 H126 Er2 O14' _chemical_formula_moiety 'C68 H110 Er2 O12, 2(C4 H8 O)' _chemical_formula_weight 1598.35 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 9.894(2) _cell_length_b 25.581(8) _cell_length_c 15.606(8) _cell_angle_alpha 90.00000 _cell_angle_beta 91.63(3) _cell_angle_gamma 90.00000 _cell_volume 3948(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 16.2 _cell_measurement_temperature 300 _exptl_absorpt_coefficient_mu 2.168 _exptl_crystal_description block _exptl_crystal_size_max .23 _exptl_crystal_size_mid .23 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .63 _exptl_absorpt_correction_T_max .69 _diffrn_reflns_number 6936 _reflns_number_total 6936 _reflns_Friedel_coverage 0 _reflns_number_gt 4770 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 8 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .037 _refine_ls_wR_factor_ref .049 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_number_reflns 4770 _refine_ls_number_parameters 420 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .049 _refine_diff_density_min -.602 _refine_diff_density_max .585 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 152 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 28 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 252 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Er ? 0 4 -.723022 4.958 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Er .02946(3) .005507(10) .117031(17) .03406(17) Uani ? ? 1.00000 ? ? O0 .1256(5) -.0061(2) -.0079(3) .045(3) Uani ? ? 1.00000 ? ? O11 .0411(4) .08380(16) .1463(3) .043(3) Uani ? ? 1.00000 ? ? C11 .0738(7) .1314(2) .1792(4) .041(4) Uani ? ? 1.00000 ? ? C12 .1979(7) .1545(2) .1618(5) .044(4) Uani ? ? 1.00000 ? ? C121 .2918(7) .1337(3) .0919(5) .045(4) Uani ? ? 1.00000 ? ? C122 .2101(8) .1291(3) .0082(5) .058(5) Uani ? ? 1.00000 ? ? C123 .3591(7) .0823(3) .1157(5) .054(5) Uani ? ? 1.00000 ? ? C124 .4065(8) .1732(3) .0749(6) .067(5) Uani ? ? 1.00000 ? ? C13 .2393(7) .1992(3) .2079(5) .054(5) Uani ? ? 1.00000 ? ? C14 .1536(8) .2231(3) .2642(5) .060(5) Uani ? ? 1.00000 ? ? O14 .1849(6) .2665(2) .3121(5) .096(5) Uani ? ? 1.00000 ? ? C141 .3219(10) .2822(4) .3141(7) .109(9) Uani ? ? 1.00000 ? ? C15 .0251(8) .2040(3) .2723(5) .059(5) Uani ? ? 1.00000 ? ? C16 -.0197(7) .1587(3) .2301(5) .046(4) Uani ? ? 1.00000 ? ? C161 -.1671(7) .1406(3) .2385(5) .051(4) Uani ? ? 1.00000 ? ? C162 -.2325(7) .1313(3) .1499(6) .063(5) Uani ? ? 1.00000 ? ? C163 -.1742(8) .0923(3) .2945(6) .068(6) Uani ? ? 1.00000 ? ? C164 -.2545(8) .1837(3) .2814(6) .074(6) Uani ? ? 1.00000 ? ? O21 .1627(4) -.03315(17) .2037(3) .041(3) Uani ? ? 1.00000 ? ? C21 .2367(6) -.0655(3) .2545(4) .042(4) Uani ? ? 1.00000 ? ? C22 .2700(7) -.0513(3) .3404(5) .050(4) Uani ? ? 1.00000 ? ? C221 .2244(9) -.0003(3) .3816(5) .064(5) Uani ? ? 1.00000 ? ? C222 .0718(10) .0027(4) .3828(6) .085(6) Uani ? ? 1.00000 ? ? C223 .2783(12) .0465(4) .3330(6) .093(7) Uani ? ? 1.00000 ? ? C224 .2725(12) .0067(4) .4754(6) .099(8) Uani ? ? 1.00000 ? ? C23 .3454(8) -.0865(4) .3911(5) .062(5) Uani ? ? 1.00000 ? ? O24 .4600(7) -.1714(3) .4067(5) .109(6) Uani ? ? 1.00000 ? ? C24 .3880(9) -.1336(4) .3603(6) .072(6) Uani ? ? 1.00000 ? ? C241 .4846(13) -.1628(6) .4917(7) .144(12) Uani ? ? 1.00000 ? ? C25 .3568(8) -.1471(3) .2755(5) .057(5) Uani ? ? 1.00000 ? ? C26 .2836(7) -.1139(3) .2224(4) .046(4) Uani ? ? 1.00000 ? ? C261 .2653(7) -.1286(3) .1277(5) .047(4) Uani ? ? 1.00000 ? ? C262 .1151(7) -.1298(3) .0992(5) .054(5) Uani ? ? 1.00000 ? ? C263 .3459(7) -.0892(3) .0755(5) .050(4) Uani ? ? 1.00000 ? ? C264 .3196(9) -.1827(3) .1069(6) .067(5) Uani ? ? 1.00000 ? ? O101 -.1542(5) -.0343(2) .1857(3) .054(3) Uani ? ? 1.00000 ? ? C102 -.2950(8) -.0215(3) .1725(5) .063(5) Uani ? ? 1.00000 ? ? C103 -.3637(10) -.0389(5) .2502(8) .103(8) Uani ? ? 1.00000 ? ? C104 -.2702(12) -.0745(5) .2955(8) .118(10) Uani ? ? 1.00000 ? ? C105 -.1497(9) -.0797(3) .2422(6) .071(6) Uani ? ? 1.00000 ? ? O201 .085(2) .3497(7) .0624(17) .32(2) Uani ? ? 1.00000 ? ? C202 .126(2) .3081(13) .0185(18) .27(3) Uani ? ? 1.00000 ? ? C203 .016(3) .2693(6) .0227(16) .20(2) Uani ? ? 1.00000 ? ? C204 -.0834(17) .2918(10) .0574(19) .25(3) Uani ? ? 1.00000 ? ? C205 -.032(3) .3377(11) .096(2) .34(4) Uani ? ? 1.00000 ? ? H0 .200(12) -.010(4) -.004(8) .13(5) Uiso ? ? 1.00000 ? ? H122a .26779 .11667 -.03585 .08600 Uiso ? ? 1.00000 ? ? H122b .17578 .16245 -.00837 .08600 Uiso ? ? 1.00000 ? ? H122c .13824 .10538 .01472 .08600 Uiso ? ? 1.00000 ? ? H123a .41558 .07117 .07043 .08300 Uiso ? ? 1.00000 ? ? H123b .29202 .05628 .12436 .08300 Uiso ? ? 1.00000 ? ? H123c .41283 .08623 .16665 .08300 Uiso ? ? 1.00000 ? ? H124a .46296 .15933 .03105 .10000 Uiso ? ? 1.00000 ? ? H124b .46036 .17791 .12562 .10000 Uiso ? ? 1.00000 ? ? H124c .37025 .20542 .05626 .10000 Uiso ? ? 1.00000 ? ? H13 .32660 .21329 .19998 .06800 Uiso ? ? 1.00000 ? ? H141a .33030 .31225 .34939 .16200 Uiso ? ? 1.00000 ? ? H141b .34881 .28919 .25854 .16200 Uiso ? ? 1.00000 ? ? H141c .37425 .25444 .33885 .16200 Uiso ? ? 1.00000 ? ? H15 -.03483 .22163 .30903 .07200 Uiso ? ? 1.00000 ? ? H162a -.32319 .12065 .15613 .09600 Uiso ? ? 1.00000 ? ? H162b -.18345 .10471 .12181 .09600 Uiso ? ? 1.00000 ? ? H162c -.22974 .16261 .11729 .09600 Uiso ? ? 1.00000 ? ? H163a -.26676 .08203 .29922 .10100 Uiso ? ? 1.00000 ? ? H163b -.13749 .09958 .34996 .10100 Uiso ? ? 1.00000 ? ? H163c -.12547 .06476 .26914 .10100 Uiso ? ? 1.00000 ? ? H164a -.34534 .17122 .28452 .10900 Uiso ? ? 1.00000 ? ? H164b -.25478 .21442 .24647 .10900 Uiso ? ? 1.00000 ? ? H164c -.21966 .19133 .33629 .10900 Uiso ? ? 1.00000 ? ? H222a .04634 .03520 .40961 .13600 Uiso ? ? 1.00000 ? ? H222b .03694 -.02524 .41513 .13600 Uiso ? ? 1.00000 ? ? H222c .03532 .00211 .32639 .13600 Uiso ? ? 1.00000 ? ? H223a .25073 .07818 .36056 .14200 Uiso ? ? 1.00000 ? ? H223b .24637 .04627 .27600 .14200 Uiso ? ? 1.00000 ? ? H223c .37565 .04579 .33462 .14200 Uiso ? ? 1.00000 ? ? H224a .24010 .03883 .49625 .14700 Uiso ? ? 1.00000 ? ? H224b .36807 .00585 .47898 .14700 Uiso ? ? 1.00000 ? ? H224c .23731 -.02132 .50873 .14700 Uiso ? ? 1.00000 ? ? H23 .36654 -.07802 .44893 .07800 Uiso ? ? 1.00000 ? ? H241a .40687 -.15579 .52438 .19900 Uiso ? ? 1.00000 ? ? H241b .54700 -.13286 .50275 .19900 Uiso ? ? 1.00000 ? ? H241c .52760 -.19195 .51919 .19900 Uiso ? ? 1.00000 ? ? H25 .38520 -.17989 .25516 .07100 Uiso ? ? 1.00000 ? ? H262a .10839 -.13963 .04010 .08100 Uiso ? ? 1.00000 ? ? H262b .07576 -.09658 .10640 .08100 Uiso ? ? 1.00000 ? ? H262c .06813 -.15507 .13206 .08100 Uiso ? ? 1.00000 ? ? H263a .33595 -.09763 .01608 .07400 Uiso ? ? 1.00000 ? ? H263b .43895 -.09110 .09214 .07400 Uiso ? ? 1.00000 ? ? H263c .31332 -.05492 .08478 .07400 Uiso ? ? 1.00000 ? ? H264a .30440 -.18969 .04790 .09800 Uiso ? ? 1.00000 ? ? H264b .27466 -.20836 .14005 .09800 Uiso ? ? 1.00000 ? ? H264c .41386 -.18387 .12044 .09800 Uiso ? ? 1.00000 ? ? H102a -.33208 -.03863 .12278 .08000 Uiso ? ? 1.00000 ? ? H102b -.30700 .01534 .16567 .08000 Uiso ? ? 1.00000 ? ? H103a -.44446 -.05796 .23422 .13100 Uiso ? ? 1.00000 ? ? H103b -.38515 -.01082 .28526 .13100 Uiso ? ? 1.00000 ? ? H104a -.31135 -.10786 .30286 .14600 Uiso ? ? 1.00000 ? ? H104b -.24640 -.06033 .35003 .14600 Uiso ? ? 1.00000 ? ? H105a -.07072 -.07884 .27809 .09100 Uiso ? ? 1.00000 ? ? H105b -.15404 -.11091 .21078 .09100 Uiso ? ? 1.00000 ? ? H202a .19786 .29372 .05811 .26000 Uiso ? ? 1.00000 ? ? H202b .15702 .30910 -.03524 .26000 Uiso ? ? 1.00000 ? ? H203a .03703 .23811 .05289 .22600 Uiso ? ? 1.00000 ? ? H203b -.01878 .26085 -.03321 .22600 Uiso ? ? 1.00000 ? ? H204a -.11358 .27023 .10839 .27000 Uiso ? ? 1.00000 ? ? H204b -.15781 .29884 .02456 .27000 Uiso ? ? 1.00000 ? ? H205a -.00199 .33530 .15519 .34000 Uiso ? ? 1.00000 ? ? H205b -.09537 .36669 .09242 .34000 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Er .03364(17) .03685(17) .03176(16) .00055(14) .00189(11) -.00036(14) O0 .036(3) .066(3) .034(2) .008(2) .001(2) -.000(2) O11 .036(3) .040(2) .052(3) -.0017(19) .002(2) -.007(2) C11 .037(4) .042(4) .044(4) .003(3) -.002(3) -.005(3) C12 .034(4) .044(4) .053(4) .004(3) .006(3) -.005(3) C121 .039(4) .054(4) .044(4) -.001(3) .014(3) -.011(3) C122 .057(5) .075(5) .042(4) -.006(4) .013(4) -.003(4) C123 .041(4) .058(4) .064(5) .007(3) .013(4) .001(4) C124 .043(5) .073(5) .086(7) -.007(4) .020(4) -.007(5) C13 .031(4) .064(5) .066(5) -.009(3) -.001(4) -.007(4) C14 .046(5) .070(5) .065(5) -.011(4) .005(4) -.026(4) O14 .068(4) .096(5) .123(6) -.021(3) .016(4) -.069(4) C141 .082(7) .117(9) .129(10) -.027(6) .007(7) -.075(7) C15 .054(5) .067(5) .058(5) .006(4) .015(4) -.024(4) C16 .040(4) .048(4) .050(5) .004(3) .006(3) -.010(3) C161 .039(4) .054(4) .059(5) -.002(3) .010(4) -.013(3) C162 .029(4) .082(6) .078(6) .008(4) -.000(4) -.018(5) C163 .060(5) .080(6) .065(6) -.004(4) .021(4) .001(4) C164 .052(5) .080(6) .092(7) .007(4) .029(5) -.025(5) O21 .041(3) .047(3) .035(3) .006(2) .003(2) .004(2) C21 .029(4) .055(4) .044(4) .000(3) .005(3) .012(3) C22 .043(4) .071(5) .036(4) -.001(3) .004(3) .003(3) C221 .068(5) .084(6) .041(4) .010(4) -.006(4) .003(4) C222 .074(6) .125(8) .056(5) .036(6) -.001(4) -.038(5) C223 .138(10) .091(7) .050(6) -.021(6) .011(6) -.005(5) C224 .109(8) .137(10) .049(5) .029(7) -.015(5) -.022(6) C23 .049(5) .093(6) .044(5) .004(4) -.001(4) .013(4) O24 .118(6) .131(6) .078(5) .047(5) -.016(5) .037(4) C24 .061(6) .094(7) .062(6) .017(5) .003(5) .036(5) C241 .171(14) .184(14) .076(9) .076(10) -.024(9) .051(8) C25 .046(5) .071(5) .055(5) .010(4) .008(4) .018(4) C26 .039(4) .057(4) .042(4) -.004(3) .007(3) .006(3) C261 .047(4) .050(4) .043(4) .002(3) .003(3) .009(3) C262 .047(5) .060(5) .054(5) -.006(3) .000(4) .003(4) C263 .045(4) .064(5) .041(4) .003(3) .009(3) .003(3) C264 .070(6) .056(5) .075(6) .011(4) .006(5) -.013(4) O101 .044(3) .062(3) .055(3) -.009(2) .008(2) .009(2) C102 .048(5) .078(5) .063(5) -.009(4) .004(4) .001(4) C103 .058(6) .131(10) .120(10) -.009(6) .030(6) .029(8) C104 .109(9) .152(11) .097(9) .013(8) .054(8) .049(8) C105 .065(6) .083(6) .066(6) -.019(5) .008(5) .017(5) O201 .23(2) .250(19) .49(4) -.075(16) .11(2) -.15(2) C202 .17(2) .36(4) .27(3) -.00(3) .09(2) -.09(3) C203 .23(3) .136(16) .24(3) .006(16) -.01(2) -.040(15) C204 .17(2) .18(2) .41(4) -.049(17) .08(2) -.11(2) C205 .19(2) .28(3) .57(5) -.05(2) .15(3) -.28(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Er O0 . . 2.213(5) ? Er O11 . . 2.056(4) ? Er O21 . . 2.108(4) ? Er O101 . . 2.365(5) ? Er O0 . 3 2.259(5) ? O0 H0 . . .74(12) ? O11 C11 . . 1.357(7) ? C11 C12 . . 1.396(9) ? C11 C16 . . 1.421(9) ? C12 C121 . . 1.547(10) ? C12 C13 . . 1.406(10) ? C121 C122 . . 1.520(10) ? C121 C123 . . 1.516(10) ? C121 C124 . . 1.548(10) ? C122 H122a . . .960 ? C122 H122b . . .951 ? C122 H122c . . .943 ? C123 H123a . . .956 ? C123 H123b . . .952 ? C123 H123c . . .949 ? C124 H124a . . .964 ? C124 H124b . . .950 ? C124 H124c . . .941 ? C13 C14 . . 1.381(11) ? C13 H13 . . .948 ? C14 O14 . . 1.368(10) ? C14 C15 . . 1.372(11) ? O14 C141 . . 1.413(12) ? C141 H141a . . .948 ? C141 H141b . . .932 ? C141 H141c . . .954 ? C15 C16 . . 1.398(10) ? C15 H15 . . .950 ? C16 C161 . . 1.539(10) ? C161 C162 . . 1.529(11) ? C161 C163 . . 1.517(11) ? C161 C164 . . 1.563(11) ? C162 H162a . . .945 ? C162 H162b . . .951 ? C162 H162c . . .949 ? C163 H163a . . .958 ? C163 H163b . . .947 ? C163 H163c . . .947 ? C164 H164a . . .956 ? C164 H164b . . .956 ? C164 H164c . . .935 ? O21 C21 . . 1.348(8) ? C21 C22 . . 1.418(10) ? C21 C26 . . 1.420(10) ? C22 C221 . . 1.529(11) ? C22 C23 . . 1.400(11) ? C221 C222 . . 1.512(13) ? C221 C223 . . 1.523(13) ? C221 C224 . . 1.536(12) ? C222 H222a . . .968 ? C222 H222b . . .945 ? C222 H222c . . .942 ? C223 H223a . . .961 ? C223 H223b . . .935 ? C223 H223c . . .963 ? C224 H224a . . .944 ? C224 H224b . . .946 ? C224 H224c . . .957 ? C23 C24 . . 1.368(13) ? C23 H23 . . .947 ? O24 C24 . . 1.390(12) ? O24 C241 . . 1.361(14) ? C24 C25 . . 1.394(12) ? C241 H241a . . .952 ? C241 H241b . . .996 ? C241 H241c . . .953 ? C25 C26 . . 1.378(10) ? C25 H25 . . .942 ? C26 C261 . . 1.531(10) ? C261 C262 . . 1.539(10) ? C261 C263 . . 1.534(10) ? C261 C264 . . 1.522(10) ? C262 H262a . . .957 ? C262 H262b . . .943 ? C262 H262c . . .954 ? C263 H263a . . .955 ? C263 H263b . . .950 ? C263 H263c . . .946 ? C264 H264a . . .947 ? C264 H264b . . .953 ? C264 H264c . . .951 ? O101 C102 . . 1.440(9) ? O101 C105 . . 1.459(10) ? C102 C103 . . 1.476(14) ? C102 H102a . . .955 ? C102 H102b . . .955 ? C103 C104 . . 1.464(17) ? C103 H103a . . .963 ? C103 H103b . . .932 ? C104 C105 . . 1.479(15) ? C104 H104a . . .954 ? C104 H104b . . .948 ? C105 H105a . . .949 ? C105 H105b . . .937 ? O201 C202 . . 1.33(4) ? O201 C205 . . 1.33(4) ? C202 C203 . . 1.48(4) ? C202 H202a . . 1.00 ? C202 H202b . . .90 ? C203 C204 . . 1.27(3) ? C203 H203a . . .946 ? C203 H203b . . .95 ? C204 C205 . . 1.41(4) ? C204 H204a . . 1.02 ? C204 H204b . . .90 ? C205 H205a . . .97 ? C205 H205b . . .97 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O0 Er O11 . . . 107.63(18) ? O0 Er O21 . . . 103.08(17) ? O0 Er O101 . . . 134.12(17) ? O0 Er O0 . . 3 68.67(18) ? O11 Er O21 . . . 106.52(17) ? O11 Er O101 . . . 110.94(17) ? O11 Er O0 . . 3 101.16(17) ? O21 Er O101 . . . 88.96(16) ? O21 Er O0 . . 3 152.30(17) ? O101 Er O0 . . 3 80.23(17) ? Er Er O0 3 . 3 33.93(13) ? Er O0 H0 . . . 113(9) ? Er O0 Er . . 3 111.3(2) ? H0 O0 Er . . 3 135(9) ? Er O11 C11 . . . 165.7(4) ? O11 C11 C12 . . . 120.5(6) ? O11 C11 C16 . . . 120.1(6) ? C12 C11 C16 . . . 119.4(6) ? C11 C12 C121 . . . 122.8(6) ? C11 C12 C13 . . . 119.3(6) ? C121 C12 C13 . . . 117.9(6) ? C12 C121 C122 . . . 108.5(6) ? C12 C121 C123 . . . 113.1(6) ? C12 C121 C124 . . . 110.8(6) ? C122 C121 C123 . . . 111.3(6) ? C122 C121 C124 . . . 106.1(6) ? C123 C121 C124 . . . 106.8(6) ? C121 C122 H122a . . . 109.2 ? C121 C122 H122b . . . 110.0 ? C121 C122 H122c . . . 110.0 ? H122a C122 H122b . . . 108.5 ? H122a C122 H122c . . . 109.2 ? H122b C122 H122c . . . 110.0 ? C121 C123 H123a . . . 109.8 ? C121 C123 H123b . . . 109.8 ? C121 C123 H123c . . . 110.2 ? H123a C123 H123b . . . 108.7 ? H123a C123 H123c . . . 109.0 ? H123b C123 H123c . . . 109.3 ? C121 C124 H124a . . . 108.9 ? C121 C124 H124b . . . 109.7 ? C121 C124 H124c . . . 110.5 ? H124a C124 H124b . . . 108.4 ? H124a C124 H124c . . . 109.1 ? H124b C124 H124c . . . 110.3 ? C12 C13 C14 . . . 120.7(6) ? C12 C13 H13 . . . 119.8 ? C14 C13 H13 . . . 119.5 ? C13 C14 O14 . . . 125.0(7) ? C13 C14 C15 . . . 119.2(7) ? O14 C14 C15 . . . 115.8(7) ? C14 O14 C141 . . . 116.4(7) ? O14 C141 H141a . . . 108.2 ? O14 C141 H141b . . . 109.4 ? O14 C141 H141c . . . 107.9 ? H141a C141 H141b . . . 111.2 ? H141a C141 H141c . . . 109.4 ? H141b C141 H141c . . . 110.6 ? C14 C15 C16 . . . 122.3(7) ? C14 C15 H15 . . . 118.8 ? C16 C15 H15 . . . 118.8 ? C11 C16 C15 . . . 117.9(6) ? C11 C16 C161 . . . 122.2(6) ? C15 C16 C161 . . . 119.9(6) ? C16 C161 C162 . . . 110.3(6) ? C16 C161 C163 . . . 110.7(6) ? C16 C161 C164 . . . 111.2(6) ? C162 C161 C163 . . . 111.6(6) ? C162 C161 C164 . . . 105.8(6) ? C163 C161 C164 . . . 107.1(7) ? C161 C162 H162a . . . 109.3 ? C161 C162 H162b . . . 108.7 ? C161 C162 H162c . . . 109.6 ? H162a C162 H162b . . . 109.8 ? H162a C162 H162c . . . 109.9 ? H162b C162 H162c . . . 109.5 ? C161 C163 H163a . . . 109.1 ? C161 C163 H163b . . . 110.0 ? C161 C163 H163c . . . 109.5 ? H163a C163 H163b . . . 109.0 ? H163a C163 H163c . . . 109.1 ? H163b C163 H163c . . . 110.0 ? C161 C164 H164a . . . 108.6 ? C161 C164 H164b . . . 109.2 ? C161 C164 H164c . . . 110.2 ? H164a C164 H164b . . . 108.4 ? H164a C164 H164c . . . 110.2 ? H164b C164 H164c . . . 110.2 ? Er O21 C21 . . . 170.0(4) ? O21 C21 C22 . . . 120.5(6) ? O21 C21 C26 . . . 120.3(6) ? C22 C21 C26 . . . 119.2(6) ? C21 C22 C221 . . . 123.5(6) ? C21 C22 C23 . . . 118.4(7) ? C221 C22 C23 . . . 118.1(7) ? C22 C221 C222 . . . 110.8(7) ? C22 C221 C223 . . . 110.5(7) ? C22 C221 C224 . . . 114.4(7) ? C222 C221 C223 . . . 109.3(7) ? C222 C221 C224 . . . 105.4(7) ? C223 C221 C224 . . . 106.2(7) ? C221 C222 H222a . . . 108.7 ? C221 C222 H222b . . . 110.4 ? C221 C222 H222c . . . 110.1 ? H222a C222 H222b . . . 108.4 ? H222a C222 H222c . . . 108.6 ? H222b C222 H222c . . . 110.6 ? C221 C223 H223a . . . 109.4 ? C221 C223 H223b . . . 110.8 ? C221 C223 H223c . . . 109.7 ? H223a C223 H223b . . . 109.8 ? H223a C223 H223c . . . 107.5 ? H223b C223 H223c . . . 109.6 ? C221 C224 H224a . . . 109.4 ? C221 C224 H224b . . . 109.7 ? C221 C224 H224c . . . 108.9 ? H224a C224 H224b . . . 110.3 ? H224a C224 H224c . . . 109.4 ? H224b C224 H224c . . . 109.2 ? C22 C23 C24 . . . 122.2(7) ? C22 C23 H23 . . . 119.3 ? C24 C23 H23 . . . 118.4 ? C24 O24 C241 . . . 118.2(9) ? C23 C24 O24 . . . 125.9(8) ? C23 C24 C25 . . . 119.3(8) ? O24 C24 C25 . . . 114.8(8) ? O24 C241 H241a . . . 115.3 ? O24 C241 H241b . . . 112.6 ? O24 C241 H241c . . . 112.2 ? H241a C241 H241b . . . 105.6 ? H241a C241 H241c . . . 105.3 ? H241b C241 H241c . . . 104.9 ? C24 C25 C26 . . . 121.1(7) ? C24 C25 H25 . . . 118.7 ? C26 C25 H25 . . . 120.2 ? C21 C26 C25 . . . 119.8(7) ? C21 C26 C261 . . . 121.6(6) ? C25 C26 C261 . . . 118.3(6) ? C26 C261 C262 . . . 111.7(6) ? C26 C261 C263 . . . 107.6(6) ? C26 C261 C264 . . . 113.3(6) ? C262 C261 C263 . . . 111.9(6) ? C262 C261 C264 . . . 105.3(6) ? C263 C261 C264 . . . 107.0(6) ? C261 C262 H262a . . . 108.9 ? C261 C262 H262b . . . 110.3 ? C261 C262 H262c . . . 109.9 ? H262a C262 H262b . . . 109.5 ? H262a C262 H262c . . . 108.6 ? H262b C262 H262c . . . 109.7 ? C261 C263 H263a . . . 109.0 ? C261 C263 H263b . . . 109.6 ? C261 C263 H263c . . . 110.1 ? H263a C263 H263b . . . 109.0 ? H263a C263 H263c . . . 109.4 ? H263b C263 H263c . . . 109.7 ? C261 C264 H264a . . . 109.3 ? C261 C264 H264b . . . 109.8 ? C261 C264 H264c . . . 109.4 ? H264a C264 H264b . . . 109.5 ? H264a C264 H264c . . . 109.7 ? H264b C264 H264c . . . 109.2 ? Er O101 C102 . . . 126.2(4) ? Er O101 C105 . . . 127.3(4) ? C102 O101 C105 . . . 106.2(6) ? O101 C102 C103 . . . 106.2(7) ? O101 C102 H102a . . . 111.1 ? O101 C102 H102b . . . 110.9 ? C103 C102 H102a . . . 110.7 ? C103 C102 H102b . . . 109.3 ? H102a C102 H102b . . . 108.6 ? C102 C103 C104 . . . 106.6(9) ? C102 C103 H103a . . . 109.8 ? C102 C103 H103b . . . 111.5 ? C104 C103 H103a . . . 108.6 ? C104 C103 H103b . . . 110.3 ? H103a C103 H103b . . . 109.9 ? C103 C104 C105 . . . 107.0(9) ? C103 C104 H104a . . . 110.4 ? C103 C104 H104b . . . 109.5 ? C105 C104 H104a . . . 109.9 ? C105 C104 H104b . . . 110.9 ? H104a C104 H104b . . . 109.2 ? O101 C105 C104 . . . 104.9(7) ? O101 C105 H105a . . . 110.4 ? O101 C105 H105b . . . 111.3 ? C104 C105 H105a . . . 109.2 ? C104 C105 H105b . . . 110.2 ? H105a C105 H105b . . . 110.7 ? C202 O201 C205 . . . 107(2) ? O201 C202 C203 . . . 106(2) ? O201 C202 H202a . . . 101 ? O201 C202 H202b . . . 125 ? C203 C202 H202a . . . 104 ? C203 C202 H202b . . . 109 ? H202a C202 H202b . . . 109 ? C202 C203 C204 . . . 107(2) ? C202 C203 H203a . . . 116 ? C202 C203 H203b . . . 111 ? C204 C203 H203a . . . 110 ? C204 C203 H203b . . . 103 ? H203a C203 H203b . . . 109.5 ? C203 C204 C205 . . . 107(2) ? C203 C204 H204a . . . 109 ? C203 C204 H204b . . . 118 ? C205 C204 H204a . . . 103 ? C205 C204 H204b . . . 111 ? H204a C204 H204b . . . 107.4 ? O201 C205 C204 . . . 109(2) ? O201 C205 H205a . . . 98 ? O201 C205 H205b . . . 112 ? C204 C205 H205a . . . 117 ? C204 C205 H205b . . . 113 ? H205a C205 H205b . . . 107 ? _exptl_crystal_F_000 1660 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _reflns_number_observed ? _reflns_d_resolution_high .841 _reflns_d_resolution_low 13.283 _diffrn_reflns_av_sigmaI/netI .066 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 300 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 10 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .063 _refine_ls_wR_factor_all .062 _refine_ls_goodness_of_fit_all 1.06 _refine_ls_shift/su_mean .002 #===END data_sm356ab _database_code_depnum_ccdc_archive 'CCDC 281265' _audit_creation_method SHELXL-97 _chemical_name_systematic ; pentafluorotetrakis(2,6-di-tert-butyl-4-methoxyphenolato)tetrakis (tetrahydrofuran)trierbium(III).tetrahydrofuran.hexane ; _chemical_name_common ; pentafluorotetrakis(2,6-di-tert-butyl-4- methoxyphenolato)tetrakis (tetrahydrofuran)trierbium(iii).tetrahydrofuran.hexane ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H139 Er3 F5 O13' _chemical_formula_weight 1941.72 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' 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.049(3) _cell_length_b 19.045(4) _cell_length_c 32.230(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.77(3) _cell_angle_gamma 90.00 _cell_volume 9191(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 13.7 _exptl_crystal_description tabular _exptl_crystal_colour pink _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3960 _exptl_absorpt_coefficient_mu 2.778 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.62 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Siemans/Nicolet R3m/V' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18191 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.1427 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16170 _reflns_number_gt 9509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'POVRAY 3.0' _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^)+(0.0788P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16170 _refine_ls_number_parameters 927 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1404 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.21100(4) 0.70904(3) 0.102191(17) 0.02115(15) Uani 1 1 d . . . Er2 Er 0.30846(4) 0.76196(3) 0.200916(17) 0.02214(15) Uani 1 1 d . B . Er3 Er 0.15834(4) 0.62129(3) 0.193077(17) 0.02092(15) Uani 1 1 d . . . F1 F 0.2836(4) 0.6529(4) 0.1633(2) 0.0244(16) Uani 1 1 d . . . F2 F 0.1677(4) 0.7426(4) 0.16861(19) 0.0231(16) Uani 1 1 d . . . F3 F 0.3100(4) 0.7812(4) 0.1334(2) 0.0263(17) Uani 1 1 d . . . F4 F 0.2397(4) 0.6862(4) 0.2383(2) 0.0253(16) Uani 1 1 d . . . F5 F 0.1244(5) 0.6287(4) 0.1250(2) 0.0308(18) Uani 1 1 d . . . O1 O 0.2845(5) 0.6527(4) 0.0619(2) 0.0229(19) Uani 1 1 d . . . O2 O 0.4433(7) 0.5212(5) -0.0647(3) 0.043(3) Uani 1 1 d . . . O3 O 0.1271(6) 0.7740(4) 0.0638(3) 0.029(2) Uani 1 1 d . . . O4 O -0.0966(7) 0.9427(6) -0.0412(3) 0.050(3) Uani 1 1 d . . . O5 O 0.2697(6) 0.8417(5) 0.2396(3) 0.031(2) Uani 1 1 d . . . O6 O 0.2511(6) 1.0847(5) 0.3332(3) 0.035(2) Uani 1 1 d . . . O7 O 0.2129(6) 0.5340(5) 0.2259(3) 0.030(2) Uani 1 1 d . . . O8 O 0.2949(6) 0.2754(5) 0.2971(3) 0.038(2) Uani 1 1 d . . . O9 O 0.4349(6) 0.6946(5) 0.2272(3) 0.042(3) Uani 1 1 d D . . O10 O 0.4335(6) 0.8400(5) 0.1950(3) 0.035(2) Uani 1 1 d . . . O11 O 0.0372(6) 0.5358(5) 0.1782(3) 0.031(2) Uani 1 1 d . . . O12 O 0.0388(5) 0.6772(4) 0.2216(2) 0.0236(19) Uani 1 1 d . . . O13 O -0.0161(19) 0.7420(14) 0.3556(8) 0.197(10) Uiso 1 1 d . . . C1 C 0.3258(8) 0.6197(7) 0.0322(4) 0.026(3) Uani 1 1 d . . . C2 C 0.4179(9) 0.6312(7) 0.0279(4) 0.032(3) Uani 1 1 d . . . C3 C 0.4570(9) 0.5995(7) -0.0044(4) 0.032(3) Uani 1 1 d . . . H3 H 0.5177 0.6092 -0.0079 0.038 Uiso 1 1 calc R . . C4 C 0.4095(10) 0.5539(8) -0.0318(4) 0.036(4) Uani 1 1 d . . . C5 C 0.3230(10) 0.5394(7) -0.0263(4) 0.036(4) Uani 1 1 d . . . H5 H 0.2912 0.5067 -0.0444 0.044 Uiso 1 1 calc R . . C6 C 0.2796(9) 0.5709(7) 0.0049(4) 0.031(3) Uani 1 1 d . . . C7 C 0.5309(11) 0.5372(8) -0.0719(5) 0.054(5) Uani 1 1 d . . . H7A H 0.5472 0.5105 -0.0960 0.081 Uiso 1 1 calc R . . H7B H 0.5713 0.5248 -0.0472 0.081 Uiso 1 1 calc R . . H7C H 0.5357 0.5876 -0.0775 0.081 Uiso 1 1 calc R . . C8 C 0.4750(8) 0.6799(7) 0.0584(4) 0.028(3) Uani 1 1 d . . . C9 C 0.5750(8) 0.6781(8) 0.0478(4) 0.038(4) Uani 1 1 d . . . H9A H 0.6114 0.7087 0.0671 0.057 Uiso 1 1 calc R . . H9B H 0.5781 0.6946 0.0191 0.057 Uiso 1 1 calc R . . H9C H 0.5977 0.6299 0.0504 0.057 Uiso 1 1 calc R . . C10 C 0.4424(9) 0.7559(7) 0.0537(4) 0.034(3) Uani 1 1 d . . . H10A H 0.4792 0.7860 0.0732 0.051 Uiso 1 1 calc R . . H10B H 0.3799 0.7586 0.0598 0.051 Uiso 1 1 calc R . . H10C H 0.4470 0.7719 0.0251 0.051 Uiso 1 1 calc R . . C11 C 0.4734(8) 0.6541(8) 0.1036(4) 0.035(3) Uani 1 1 d . . . H11A H 0.5100 0.6853 0.1225 0.053 Uiso 1 1 calc R . . H11B H 0.4973 0.6063 0.1061 0.053 Uiso 1 1 calc R . . H11C H 0.4117 0.6544 0.1109 0.053 Uiso 1 1 calc R . . C12 C 0.1802(10) 0.5499(8) 0.0085(4) 0.037(4) Uani 1 1 d . . . C13 C 0.1461(10) 0.4933(8) -0.0228(4) 0.049(4) Uani 1 1 d . . . H13A H 0.0838 0.4821 -0.0191 0.073 Uiso 1 1 calc R . . H13B H 0.1827 0.4509 -0.0182 0.073 Uiso 1 1 calc R . . H13C H 0.1499 0.5105 -0.0512 0.073 Uiso 1 1 calc R . . C14 C 0.1177(9) 0.6153(8) -0.0003(5) 0.049(4) Uani 1 1 d . . . H14A H 0.0557 0.6017 0.0021 0.073 Uiso 1 1 calc R . . H14B H 0.1232 0.6328 -0.0285 0.073 Uiso 1 1 calc R . . H14C H 0.1353 0.6523 0.0200 0.073 Uiso 1 1 calc R . . C15 C 0.1686(10) 0.5198(8) 0.0518(4) 0.047(4) Uani 1 1 d . . . H15A H 0.1059 0.5071 0.0533 0.071 Uiso 1 1 calc R . . H15B H 0.1866 0.5551 0.0731 0.071 Uiso 1 1 calc R . . H15C H 0.2061 0.4779 0.0567 0.071 Uiso 1 1 calc R . . C16 C 0.0736(9) 0.8156(7) 0.0380(4) 0.030(3) Uani 1 1 d . . . C17 C 0.1088(9) 0.8602(7) 0.0074(4) 0.036(3) Uani 1 1 d . . . C18 C 0.0529(9) 0.9029(8) -0.0171(4) 0.040(4) Uani 1 1 d . . . H18 H 0.0775 0.9340 -0.0359 0.047 Uiso 1 1 calc R . . C19 C -0.0360(10) 0.9023(8) -0.0154(5) 0.042(4) Uani 1 1 d . . . C20 C -0.0719(9) 0.8594(7) 0.0128(4) 0.035(3) Uani 1 1 d . . . H20 H -0.1348 0.8600 0.0139 0.042 Uiso 1 1 calc R . . C21 C -0.0201(8) 0.8148(6) 0.0401(4) 0.026(3) Uani 1 1 d . . . C22 C -0.0587(11) 0.9876(8) -0.0698(4) 0.046(4) Uani 1 1 d . . . H22A H -0.1064 1.0133 -0.0863 0.069 Uiso 1 1 calc R . . H22B H -0.0252 0.9596 -0.0884 0.069 Uiso 1 1 calc R . . H22C H -0.0183 1.0211 -0.0544 0.069 Uiso 1 1 calc R . . C23 C 0.2141(10) 0.8625(8) 0.0047(5) 0.042(4) Uani 1 1 d . . . C24 C 0.2337(10) 0.9168(10) -0.0291(5) 0.067(6) Uani 1 1 d . . . H24A H 0.2163 0.9637 -0.0204 0.100 Uiso 1 1 calc R . . H24B H 0.1996 0.9045 -0.0556 0.100 Uiso 1 1 calc R . . H24C H 0.2976 0.9164 -0.0325 0.100 Uiso 1 1 calc R . . C25 C 0.2648(9) 0.8875(8) 0.0458(5) 0.043(4) Uani 1 1 d . . . H25A H 0.2427 0.9339 0.0530 0.065 Uiso 1 1 calc R . . H25B H 0.3287 0.8905 0.0425 0.065 Uiso 1 1 calc R . . H25C H 0.2553 0.8541 0.0680 0.065 Uiso 1 1 calc R . . C26 C 0.2428(10) 0.7919(9) -0.0096(4) 0.047(4) Uani 1 1 d . . . H26A H 0.2310 0.7563 0.0111 0.071 Uiso 1 1 calc R . . H26B H 0.3068 0.7929 -0.0129 0.071 Uiso 1 1 calc R . . H26C H 0.2093 0.7804 -0.0364 0.071 Uiso 1 1 calc R . . C27 C -0.0646(9) 0.7677(9) 0.0702(4) 0.041(4) Uani 1 1 d . . . C28 C -0.0502(9) 0.6917(7) 0.0602(5) 0.037(4) Uani 1 1 d . . . H28A H -0.0787 0.6621 0.0799 0.056 Uiso 1 1 calc R . . H28B H 0.0139 0.6817 0.0624 0.056 Uiso 1 1 calc R . . H28C H -0.0766 0.6818 0.0317 0.056 Uiso 1 1 calc R . . C29 C -0.0314(9) 0.7887(8) 0.1148(4) 0.040(4) Uani 1 1 d . . . H29A H -0.0425 0.8389 0.1188 0.060 Uiso 1 1 calc R . . H29B H 0.0329 0.7794 0.1199 0.060 Uiso 1 1 calc R . . H29C H -0.0631 0.7614 0.1344 0.060 Uiso 1 1 calc R . . C30 C -0.1677(10) 0.7784(9) 0.0660(5) 0.052(4) Uani 1 1 d . . . H30A H -0.1813 0.8274 0.0722 0.078 Uiso 1 1 calc R . . H30B H -0.1942 0.7475 0.0857 0.078 Uiso 1 1 calc R . . H30C H -0.1925 0.7669 0.0375 0.078 Uiso 1 1 calc R . . C31 C 0.2623(8) 0.9011(7) 0.2634(4) 0.029(3) Uani 1 1 d . . . C32 C 0.2312(8) 0.9650(7) 0.2442(4) 0.025(3) Uani 1 1 d . . . C33 C 0.2285(8) 1.0225(7) 0.2697(4) 0.031(3) Uani 1 1 d . . . H33 H 0.2060 1.0653 0.2577 0.038 Uiso 1 1 calc R . . C34 C 0.2566(8) 1.0214(7) 0.3113(4) 0.027(3) Uani 1 1 d . . . C35 C 0.2847(9) 0.9586(7) 0.3297(4) 0.038(4) Uani 1 1 d . . . H35 H 0.3041 0.9579 0.3587 0.045 Uiso 1 1 calc R . . C36 C 0.2855(9) 0.8985(7) 0.3079(4) 0.030(3) Uani 1 1 d . . . C37 C 0.2717(10) 1.0810(8) 0.3772(4) 0.045(4) Uani 1 1 d . . . H37A H 0.2658 1.1278 0.3893 0.068 Uiso 1 1 calc R . . H37B H 0.3331 1.0642 0.3836 0.068 Uiso 1 1 calc R . . H37C H 0.2304 1.0485 0.3890 0.068 Uiso 1 1 calc R . . C38 C 0.1922(9) 0.9696(7) 0.1985(4) 0.030(3) Uani 1 1 d . . . C39 C 0.1555(10) 1.0421(7) 0.1875(4) 0.037(4) Uani 1 1 d . . . H39A H 0.2030 1.0771 0.1931 0.056 Uiso 1 1 calc R . . H39B H 0.1066 1.0527 0.2045 0.056 Uiso 1 1 calc R . . H39C H 0.1331 1.0436 0.1579 0.056 Uiso 1 1 calc R . . C40 C 0.2680(10) 0.9578(8) 0.1695(4) 0.041(4) Uani 1 1 d . . . H40A H 0.3158 0.9922 0.1764 0.061 Uiso 1 1 calc R . . H40B H 0.2438 0.9637 0.1404 0.061 Uiso 1 1 calc R . . H40C H 0.2921 0.9103 0.1737 0.061 Uiso 1 1 calc R . . C41 C 0.1162(9) 0.9170(7) 0.1890(4) 0.039(4) Uani 1 1 d . . . H41A H 0.1381 0.8695 0.1957 0.058 Uiso 1 1 calc R . . H41B H 0.0943 0.9196 0.1593 0.058 Uiso 1 1 calc R . . H41C H 0.0674 0.9282 0.2059 0.058 Uiso 1 1 calc R . . C42 C 0.3114(10) 0.8291(8) 0.3311(4) 0.037(4) Uani 1 1 d . . . C43 C 0.3266(11) 0.8396(8) 0.3790(4) 0.052(5) Uani 1 1 d . . . H43A H 0.2727 0.8595 0.3890 0.078 Uiso 1 1 calc R . . H43B H 0.3769 0.8717 0.3856 0.078 Uiso 1 1 calc R . . H43C H 0.3399 0.7942 0.3925 0.078 Uiso 1 1 calc R . . C44 C 0.2354(11) 0.7775(7) 0.3238(5) 0.048(4) Uani 1 1 d . . . H44A H 0.1809 0.7984 0.3327 0.072 Uiso 1 1 calc R . . H44B H 0.2500 0.7346 0.3398 0.072 Uiso 1 1 calc R . . H44C H 0.2258 0.7661 0.2940 0.072 Uiso 1 1 calc R . . C45 C 0.3981(12) 0.8000(11) 0.3172(5) 0.078(6) Uani 1 1 d . . . H45A H 0.4456 0.8350 0.3224 0.117 Uiso 1 1 calc R . . H45B H 0.3896 0.7892 0.2874 0.117 Uiso 1 1 calc R . . H45C H 0.4149 0.7571 0.3329 0.117 Uiso 1 1 calc R . . C46 C 0.2359(8) 0.4720(7) 0.2448(4) 0.028(3) Uani 1 1 d . A . C47 C 0.2239(8) 0.4614(7) 0.2871(4) 0.026(3) Uani 1 1 d . . . C48 C 0.2426(8) 0.3963(6) 0.3045(4) 0.026(3) Uani 1 1 d . . . H48 H 0.2342 0.3890 0.3330 0.031 Uiso 1 1 calc R . . C49 C 0.2724(8) 0.3425(7) 0.2823(4) 0.026(3) Uani 1 1 d . . . C50 C 0.2877(9) 0.3507(8) 0.2407(4) 0.032(3) Uani 1 1 d . A . H50 H 0.3096 0.3125 0.2257 0.039 Uiso 1 1 calc R . . C51 C 0.2706(8) 0.4160(8) 0.2212(4) 0.033(3) Uani 1 1 d . . . C52 C 0.2776(12) 0.2621(9) 0.3383(5) 0.056(5) Uani 1 1 d . . . H52A H 0.2947 0.2137 0.3458 0.085 Uiso 1 1 calc R . . H52B H 0.2138 0.2685 0.3409 0.085 Uiso 1 1 calc R . . H52C H 0.3122 0.2946 0.3571 0.085 Uiso 1 1 calc R . . C53 C 0.1961(10) 0.5209(8) 0.3154(4) 0.038(4) Uani 1 1 d . . . C54 C 0.1861(13) 0.4954(9) 0.3598(4) 0.064(5) Uani 1 1 d . . . H54A H 0.2418 0.4729 0.3713 0.096 Uiso 1 1 calc R . . H54B H 0.1370 0.4614 0.3591 0.096 Uiso 1 1 calc R . . H54C H 0.1732 0.5355 0.3773 0.096 Uiso 1 1 calc R . . C55 C 0.2687(11) 0.5758(8) 0.3193(5) 0.063(5) Uani 1 1 d . . . H55A H 0.3257 0.5537 0.3293 0.094 Uiso 1 1 calc R . . H55B H 0.2541 0.6120 0.3391 0.094 Uiso 1 1 calc R . . H55C H 0.2735 0.5973 0.2920 0.094 Uiso 1 1 calc R . . C56 C 0.1090(10) 0.5551(8) 0.3001(5) 0.052(4) Uani 1 1 d . . . H56A H 0.1119 0.5726 0.2717 0.077 Uiso 1 1 calc R . . H56B H 0.0976 0.5945 0.3185 0.077 Uiso 1 1 calc R . . H56C H 0.0605 0.5208 0.3003 0.077 Uiso 1 1 calc R . . C57 C 0.2772(17) 0.4158(13) 0.1727(7) 0.035(6) Uani 0.66(3) 1 d P A 1 C57' C 0.316(3) 0.441(2) 0.1800(12) 0.012(9) Uiso 0.34(3) 1 d P A 2 C58 C 0.3330(16) 0.3563(11) 0.1594(6) 0.105(9) Uani 1 1 d . . . H58A H 0.3375 0.3594 0.1294 0.158 Uiso 1 1 calc R A 1 H58B H 0.3051 0.3116 0.1658 0.158 Uiso 1 1 calc R A 1 H58C H 0.3928 0.3589 0.1744 0.158 Uiso 1 1 calc R A 1 C59 C 0.1830(14) 0.4223(11) 0.1473(6) 0.036(6) Uani 0.66(3) 1 d P A 1 H59A H 0.1509 0.4623 0.1578 0.055 Uiso 0.66(3) 1 calc PR A 1 H59B H 0.1490 0.3792 0.1505 0.055 Uiso 0.66(3) 1 calc PR A 1 H59C H 0.1905 0.4296 0.1177 0.055 Uiso 0.66(3) 1 calc PR A 1 C59' C 0.237(3) 0.462(2) 0.1472(13) 0.037(13) Uiso 0.34(3) 1 d P A 2 H59D H 0.1937 0.4236 0.1438 0.055 Uiso 0.34(3) 1 calc PR A 2 H59E H 0.2597 0.4722 0.1204 0.055 Uiso 0.34(3) 1 calc PR A 2 H59F H 0.2073 0.5042 0.1569 0.055 Uiso 0.34(3) 1 calc PR A 2 C60 C 0.3371(16) 0.4788(13) 0.1633(9) 0.051(9) Uani 0.66(3) 1 d P A 1 H60A H 0.3949 0.4748 0.1801 0.076 Uiso 0.66(3) 1 calc PR A 1 H60B H 0.3080 0.5227 0.1703 0.076 Uiso 0.66(3) 1 calc PR A 1 H60C H 0.3463 0.4789 0.1336 0.076 Uiso 0.66(3) 1 calc PR A 1 C60' C 0.386(3) 0.497(2) 0.1872(13) 0.028(11) Uiso 0.34(3) 1 d P A 2 H60D H 0.4335 0.4812 0.2081 0.042 Uiso 0.34(3) 1 calc PR A 2 H60E H 0.3592 0.5403 0.1971 0.042 Uiso 0.34(3) 1 calc PR A 2 H60F H 0.4116 0.5073 0.1609 0.042 Uiso 0.34(3) 1 calc PR A 2 C61 C 0.5264(17) 0.7124(13) 0.2376(11) 0.063(9) Uani 0.63(2) 1 d PDU B 1 H61A H 0.5325 0.7431 0.2625 0.076 Uiso 0.50 1 calc PR B 1 H61B H 0.5492 0.7382 0.2142 0.076 Uiso 0.50 1 calc PR B 1 C61' C 0.5219(19) 0.694(3) 0.2120(14) 0.065(16) Uiso 0.37(2) 1 d PD B 2 H61C H 0.5498 0.7414 0.2152 0.077 Uiso 0.50 1 calc PR B 2 H61D H 0.5172 0.6809 0.1822 0.077 Uiso 0.50 1 calc PR B 2 C62 C 0.5799(19) 0.6461(15) 0.2463(12) 0.069(15) Uani 0.63(2) 1 d PDU B 1 H62A H 0.6416 0.6519 0.2388 0.083 Uiso 0.50 1 calc PR B 1 H62B H 0.5822 0.6332 0.2762 0.083 Uiso 0.50 1 calc PR B 1 C62' C 0.574(3) 0.643(4) 0.2375(19) 0.13(5) Uiso 0.37(2) 1 d PD B 2 H62C H 0.6369 0.6581 0.2433 0.154 Uiso 0.50 1 calc PR B 2 H62D H 0.5728 0.5965 0.2233 0.154 Uiso 0.50 1 calc PR B 2 C63 C 0.5324(19) 0.5938(13) 0.2205(9) 0.069(9) Uani 0.63(2) 1 d PDU B 1 H63A H 0.5440 0.5457 0.2314 0.083 Uiso 0.50 1 calc PR B 1 H63B H 0.5466 0.5964 0.1912 0.083 Uiso 0.50 1 calc PR B 1 C63' C 0.531(2) 0.639(3) 0.2760(13) 0.09(2) Uiso 0.37(2) 1 d PD B 2 H63C H 0.5412 0.5920 0.2892 0.114 Uiso 0.50 1 calc PR B 2 H63D H 0.5552 0.6750 0.2959 0.114 Uiso 0.50 1 calc PR B 2 C64 C 0.439(2) 0.6173(14) 0.2252(11) 0.078(10) Uani 0.63(2) 1 d PU B 1 H64A H 0.3987 0.6003 0.2012 0.093 Uiso 0.50 1 calc PR B 1 H64B H 0.4194 0.5970 0.2510 0.093 Uiso 0.50 1 calc PR B 1 C64' C 0.4353(19) 0.6498(19) 0.2657(10) 0.026(10) Uiso 0.37(2) 1 d PD B 2 H64C H 0.4084 0.6747 0.2883 0.031 Uiso 0.50 1 calc PR B 2 H64D H 0.4033 0.6049 0.2597 0.031 Uiso 0.50 1 calc PR B 2 C65 C 0.4706(10) 0.8912(8) 0.2254(4) 0.046(4) Uani 1 1 d . B . H65A H 0.5149 0.8688 0.2461 0.055 Uiso 1 1 calc R . . H65B H 0.4227 0.9122 0.2404 0.055 Uiso 1 1 calc R . . C66 C 0.5140(11) 0.9460(8) 0.2013(5) 0.050(4) Uani 1 1 d . . . H66A H 0.4814 0.9910 0.2021 0.060 Uiso 1 1 calc R B . H66B H 0.5765 0.9534 0.2132 0.060 Uiso 1 1 calc R . . C67 C 0.5115(13) 0.9204(9) 0.1580(6) 0.072(6) Uani 1 1 d . B . H67A H 0.4701 0.9494 0.1394 0.087 Uiso 1 1 calc R . . H67B H 0.5717 0.9234 0.1483 0.087 Uiso 1 1 calc R . . C68 C 0.4819(12) 0.8492(10) 0.1572(6) 0.075(6) Uani 1 1 d . B . H68A H 0.5334 0.8168 0.1580 0.091 Uiso 1 1 calc R . . H68B H 0.4417 0.8398 0.1316 0.091 Uiso 1 1 calc R . . C69 C 0.0176(9) 0.4761(7) 0.2046(4) 0.036(3) Uani 1 1 d . . . H69A H -0.0154 0.4922 0.2279 0.043 Uiso 1 1 calc R . . H69B H 0.0738 0.4535 0.2163 0.043 Uiso 1 1 calc R . . C70 C -0.0385(11) 0.4246(8) 0.1774(4) 0.051(4) Uani 1 1 d . . . H70A H -0.0094 0.3780 0.1777 0.061 Uiso 1 1 calc R . . H70B H -0.0985 0.4194 0.1871 0.061 Uiso 1 1 calc R . . C71 C -0.0450(11) 0.4560(8) 0.1347(5) 0.047(4) Uani 1 1 d . . . H71A H 0.0005 0.4355 0.1181 0.056 Uiso 1 1 calc R . . H71B H -0.1049 0.4481 0.1198 0.056 Uiso 1 1 calc R . . C72 C -0.0282(10) 0.5328(8) 0.1419(4) 0.044(4) Uani 1 1 d . . . H72A H -0.0045 0.5546 0.1174 0.053 Uiso 1 1 calc R . . H72B H -0.0839 0.5573 0.1473 0.053 Uiso 1 1 calc R . . C73 C 0.0470(10) 0.7421(9) 0.2457(6) 0.058(5) Uani 1 1 d . . . H73A H 0.0855 0.7759 0.2326 0.069 Uiso 1 1 calc R . . H73B H 0.0739 0.7324 0.2744 0.069 Uiso 1 1 calc R . . C74 C -0.0431(9) 0.7710(8) 0.2465(5) 0.045(4) Uani 1 1 d . . . H74A H -0.0608 0.7994 0.2213 0.054 Uiso 1 1 calc R . . H74B H -0.0474 0.8003 0.2716 0.054 Uiso 1 1 calc R . . C75 C -0.0986(10) 0.7064(7) 0.2476(6) 0.051(4) Uani 1 1 d . . . H75A H -0.1616 0.7160 0.2372 0.061 Uiso 1 1 calc R . . H75B H -0.0963 0.6871 0.2762 0.061 Uiso 1 1 calc R . . C76 C -0.0560(8) 0.6571(8) 0.2190(5) 0.042(4) Uani 1 1 d . . . H76A H -0.0623 0.6078 0.2281 0.050 Uiso 1 1 calc R . . H76B H -0.0842 0.6618 0.1900 0.050 Uiso 1 1 calc R . . C77 C 0.039(2) 0.7460(18) 0.3970(11) 0.166(13) Uiso 1 1 d . . . H77A H 0.0633 0.6993 0.4055 0.199 Uiso 1 1 calc R . . H77B H 0.0888 0.7795 0.3960 0.199 Uiso 1 1 calc R . . C78 C -0.0230(18) 0.7699(15) 0.4251(9) 0.122(9) Uiso 1 1 d . . . H78A H -0.0052 0.7516 0.4534 0.146 Uiso 1 1 calc R . . H78B H -0.0223 0.8219 0.4264 0.146 Uiso 1 1 calc R . . C79 C -0.1102(19) 0.7460(15) 0.4109(9) 0.130(10) Uiso 1 1 d . . . H79A H -0.1544 0.7844 0.4117 0.156 Uiso 1 1 calc R . . H79B H -0.1281 0.7065 0.4282 0.156 Uiso 1 1 calc R . . C80 C -0.103(2) 0.7222(18) 0.3661(11) 0.169(13) Uiso 1 1 d . . . H80A H -0.1106 0.6706 0.3638 0.203 Uiso 1 1 calc R . . H80B H -0.1498 0.7449 0.3469 0.203 Uiso 1 1 calc R . . C81 C -0.3630(17) 0.8976(14) 0.0501(8) 0.130(10) Uiso 1 1 d . . . H81A H -0.3482 0.8850 0.0794 0.195 Uiso 1 1 calc R . . H81B H -0.3110 0.9194 0.0393 0.195 Uiso 1 1 calc R . . H81C H -0.3798 0.8552 0.0339 0.195 Uiso 1 1 calc R . . C82 C -0.440(2) 0.9489(18) 0.0463(9) 0.195(16) Uiso 1 1 d D . . H82A H -0.4247 0.9905 0.0639 0.234 Uiso 1 1 calc R . . H82B H -0.4934 0.9264 0.0565 0.234 Uiso 1 1 calc R . . C83 C -0.4631(18) 0.9721(15) 0.0011(8) 0.178(15) Uiso 1 1 d D . . H83A H -0.4834 0.9312 -0.0163 0.214 Uiso 1 1 calc R . . H83B H -0.4092 0.9917 -0.0099 0.214 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 Er1 0.0237(3) 0.0233(3) 0.0163(3) 0.0012(3) 0.0016(2) 0.0017(3) Er2 0.0220(3) 0.0240(3) 0.0202(3) -0.0021(3) 0.0011(2) 0.0007(3) Er3 0.0247(3) 0.0202(3) 0.0178(3) 0.0022(3) 0.0022(2) 0.0028(3) F1 0.023(4) 0.027(4) 0.025(4) 0.006(3) 0.012(3) 0.011(3) F2 0.029(4) 0.025(4) 0.015(3) -0.002(3) 0.001(3) 0.005(3) F3 0.030(4) 0.027(4) 0.022(4) -0.005(3) 0.002(3) -0.010(3) F4 0.029(4) 0.026(4) 0.020(4) 0.001(3) 0.000(3) 0.002(3) F5 0.036(4) 0.034(4) 0.021(4) 0.000(3) -0.007(3) -0.001(4) O1 0.031(5) 0.021(5) 0.017(4) -0.004(4) 0.003(4) 0.005(4) O2 0.053(6) 0.048(7) 0.031(5) -0.009(5) 0.017(5) 0.010(5) O3 0.038(5) 0.026(5) 0.022(5) 0.004(4) -0.004(4) 0.005(4) O4 0.052(6) 0.051(7) 0.042(6) 0.022(6) -0.014(5) 0.016(6) O5 0.041(5) 0.032(6) 0.020(5) 0.002(4) 0.006(4) 0.013(5) O6 0.057(6) 0.026(5) 0.021(5) 0.000(4) -0.001(4) -0.004(5) O7 0.034(5) 0.034(6) 0.022(5) 0.009(4) 0.006(4) 0.003(4) O8 0.049(6) 0.027(6) 0.040(6) 0.012(5) 0.013(5) 0.001(5) O9 0.030(5) 0.030(6) 0.062(7) 0.007(5) -0.011(5) -0.004(4) O10 0.034(5) 0.028(5) 0.045(6) -0.010(5) 0.006(4) -0.004(4) O11 0.033(5) 0.032(5) 0.027(5) -0.001(4) -0.004(4) 0.002(4) O12 0.027(5) 0.019(5) 0.025(5) -0.008(4) 0.006(4) -0.004(4) C1 0.027(7) 0.024(7) 0.026(7) 0.001(6) -0.003(6) -0.005(6) C2 0.036(8) 0.038(8) 0.022(7) 0.009(6) 0.007(6) 0.020(7) C3 0.029(7) 0.034(8) 0.032(8) -0.001(7) 0.000(6) 0.005(6) C4 0.049(9) 0.050(10) 0.010(6) -0.003(7) 0.012(6) 0.003(8) C5 0.058(10) 0.033(8) 0.017(7) -0.007(6) -0.005(7) 0.013(7) C6 0.037(8) 0.033(8) 0.021(7) 0.005(6) -0.005(6) 0.008(7) C7 0.079(13) 0.047(10) 0.041(10) -0.007(8) 0.035(9) 0.009(9) C8 0.033(7) 0.032(8) 0.019(7) 0.000(6) 0.000(6) -0.006(6) C9 0.028(7) 0.047(9) 0.039(8) -0.014(8) 0.000(6) -0.003(7) C10 0.035(8) 0.024(8) 0.043(9) 0.007(7) 0.009(7) 0.012(6) C11 0.026(7) 0.040(9) 0.039(8) 0.004(7) -0.001(6) 0.002(7) C12 0.054(9) 0.035(9) 0.023(7) -0.010(7) 0.004(7) -0.006(7) C13 0.044(9) 0.061(11) 0.042(9) -0.023(9) 0.003(7) -0.012(8) C14 0.032(8) 0.060(11) 0.050(10) -0.016(9) -0.013(7) 0.005(8) C15 0.062(10) 0.051(10) 0.032(8) -0.014(8) 0.019(8) -0.028(9) C16 0.041(8) 0.024(7) 0.021(7) 0.001(6) -0.009(6) 0.002(6) C17 0.042(8) 0.028(8) 0.035(8) 0.001(7) -0.005(7) -0.003(7) C18 0.041(9) 0.036(9) 0.036(8) 0.007(7) -0.021(7) 0.003(7) C19 0.039(9) 0.037(9) 0.046(9) 0.007(8) -0.017(7) 0.007(7) C20 0.027(7) 0.039(9) 0.039(8) 0.003(7) -0.001(6) 0.000(7) C21 0.032(7) 0.016(7) 0.028(7) 0.005(6) -0.003(6) 0.010(6) C22 0.077(11) 0.032(9) 0.023(8) -0.001(7) -0.022(8) 0.011(8) C23 0.046(9) 0.043(10) 0.036(8) 0.032(8) 0.000(7) 0.002(8) C24 0.044(10) 0.086(14) 0.071(12) 0.057(11) 0.011(9) -0.017(10) C25 0.027(7) 0.048(10) 0.054(10) 0.010(8) 0.003(7) 0.006(7) C26 0.038(8) 0.078(12) 0.029(8) 0.024(9) 0.014(7) 0.003(9) C27 0.032(8) 0.054(10) 0.036(8) 0.003(8) 0.006(6) 0.004(7) C28 0.028(7) 0.032(9) 0.052(9) 0.012(7) 0.007(7) -0.007(6) C29 0.032(8) 0.058(10) 0.029(8) -0.005(8) -0.001(6) 0.003(7) C30 0.044(9) 0.070(12) 0.040(9) 0.007(9) -0.006(7) 0.001(9) C31 0.016(6) 0.041(9) 0.033(8) -0.005(7) 0.007(6) 0.009(6) C32 0.028(7) 0.032(8) 0.016(7) 0.005(6) 0.002(5) 0.004(6) C33 0.033(8) 0.030(8) 0.029(8) -0.001(7) -0.007(6) -0.001(6) C34 0.034(7) 0.023(7) 0.023(7) -0.009(6) -0.006(6) -0.008(6) C35 0.052(9) 0.035(9) 0.022(7) -0.017(7) -0.017(7) 0.006(7) C36 0.047(8) 0.022(7) 0.021(7) -0.007(6) -0.003(6) 0.009(6) C37 0.070(11) 0.046(10) 0.020(8) -0.006(7) 0.002(7) 0.010(9) C38 0.040(8) 0.027(8) 0.020(7) 0.002(6) -0.013(6) 0.011(6) C39 0.059(9) 0.028(8) 0.025(8) 0.002(6) 0.002(7) 0.019(7) C40 0.053(9) 0.047(10) 0.025(8) 0.006(7) 0.018(7) 0.020(8) C41 0.042(8) 0.023(8) 0.045(9) -0.011(7) -0.024(7) 0.006(7) C42 0.054(9) 0.032(8) 0.023(7) 0.006(7) -0.004(7) 0.008(7) C43 0.081(12) 0.042(10) 0.028(8) 0.005(8) -0.021(8) 0.010(9) C44 0.090(13) 0.026(9) 0.031(8) 0.005(7) 0.017(8) -0.005(8) C45 0.076(13) 0.097(16) 0.059(12) 0.030(12) -0.005(10) 0.044(12) C46 0.020(7) 0.023(7) 0.039(8) 0.012(7) -0.002(6) -0.006(6) C47 0.017(6) 0.040(8) 0.021(7) 0.001(6) -0.001(5) 0.003(6) C48 0.038(8) 0.022(7) 0.017(7) 0.007(6) 0.008(6) -0.001(6) C49 0.037(8) 0.019(7) 0.021(7) -0.002(6) -0.002(6) -0.002(6) C50 0.035(8) 0.036(8) 0.026(7) -0.005(7) 0.005(6) 0.005(7) C51 0.025(7) 0.043(9) 0.031(8) 0.019(7) -0.001(6) 0.012(7) C52 0.079(12) 0.041(10) 0.052(11) 0.016(9) 0.020(9) 0.002(9) C53 0.044(9) 0.032(8) 0.037(8) 0.011(7) 0.004(7) 0.002(7) C54 0.120(16) 0.052(11) 0.021(8) -0.014(8) 0.012(9) 0.018(11) C55 0.078(12) 0.038(10) 0.064(12) -0.006(9) -0.031(10) 0.010(9) C56 0.065(11) 0.051(11) 0.038(9) -0.015(8) 0.003(8) 0.031(9) C57 0.045(15) 0.023(13) 0.038(13) 0.009(11) 0.006(12) 0.006(12) C58 0.17(2) 0.097(17) 0.059(13) 0.030(12) 0.062(14) 0.095(17) C59 0.058(15) 0.029(13) 0.020(11) -0.007(10) -0.009(10) -0.020(11) C60 0.037(15) 0.039(15) 0.08(2) -0.010(15) 0.048(15) -0.004(12) C61 0.049(14) 0.048(14) 0.090(17) -0.014(13) 0.000(12) 0.016(12) C62 0.050(17) 0.046(17) 0.11(2) 0.007(14) -0.011(13) 0.005(12) C63 0.087(16) 0.048(14) 0.069(16) 0.002(13) -0.008(13) 0.016(13) C64 0.068(15) 0.036(14) 0.121(19) 0.020(14) -0.026(14) 0.001(12) C65 0.056(10) 0.053(11) 0.027(8) 0.001(8) 0.003(7) -0.022(8) C66 0.057(10) 0.040(10) 0.051(10) -0.019(8) -0.007(8) 0.004(8) C67 0.095(15) 0.045(11) 0.078(14) 0.008(10) 0.011(11) -0.038(11) C68 0.060(11) 0.089(15) 0.085(14) -0.047(13) 0.044(11) -0.034(11) C69 0.039(8) 0.036(9) 0.033(8) 0.007(7) -0.001(7) -0.004(7) C70 0.074(11) 0.029(9) 0.044(9) 0.008(8) -0.021(8) -0.010(8) C71 0.055(10) 0.038(9) 0.044(9) -0.015(8) -0.017(8) -0.005(8) C72 0.045(9) 0.050(10) 0.033(8) 0.007(8) -0.019(7) -0.002(8) C73 0.041(9) 0.066(12) 0.068(12) -0.017(10) 0.012(8) -0.008(9) C74 0.042(9) 0.045(10) 0.046(9) -0.004(8) 0.000(7) -0.008(8) C75 0.050(10) 0.024(8) 0.083(12) -0.012(9) 0.031(9) 0.004(8) C76 0.026(8) 0.038(9) 0.061(10) -0.001(8) 0.004(7) 0.001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O3 2.083(8) . ? Er1 O1 2.086(8) . ? Er1 F5 2.185(7) . ? Er1 F3 2.194(6) . ? Er1 F2 2.386(6) . ? Er1 F1 2.406(6) . ? Er1 Er2 3.5147(12) . ? Er1 Er3 3.5311(10) . ? Er2 O5 2.085(8) . ? Er2 F4 2.204(7) . ? Er2 F3 2.209(7) . ? Er2 F2 2.294(6) . ? Er2 O9 2.380(9) . ? Er2 F1 2.415(7) . ? Er2 O10 2.420(9) . ? Er2 Er3 3.4972(10) . ? Er3 O7 2.094(8) . ? Er3 F4 2.188(7) . ? Er3 F5 2.207(6) . ? Er3 F1 2.280(6) . ? Er3 O12 2.355(8) . ? Er3 F2 2.449(7) . ? Er3 O11 2.456(9) . ? O1 C1 1.349(14) . ? O2 C4 1.373(15) . ? O2 C7 1.394(17) . ? O3 C16 1.354(14) . ? O4 C19 1.401(15) . ? O4 C22 1.417(17) . ? O5 C31 1.379(15) . ? O6 C34 1.403(15) . ? O6 C37 1.422(14) . ? O7 C46 1.357(14) . ? O8 C49 1.392(15) . ? O8 C52 1.405(16) . ? O9 C61 1.43(3) . ? O9 C61' 1.442(19) . ? O9 C64 1.47(3) . ? O9 C64' 1.50(3) . ? O10 C65 1.455(16) . ? O10 C68 1.491(18) . ? O11 C72 1.452(14) . ? O11 C69 1.467(15) . ? O12 C73 1.460(17) . ? O12 C76 1.471(15) . ? O13 C80 1.43(3) . ? O13 C77 1.50(3) . ? C1 C6 1.414(17) . ? C1 C2 1.423(17) . ? C2 C3 1.385(17) . ? C2 C8 1.549(18) . ? C3 C4 1.383(18) . ? C4 C5 1.359(19) . ? C5 C6 1.389(17) . ? C6 C12 1.564(19) . ? C8 C10 1.531(17) . ? C8 C11 1.540(17) . ? C8 C9 1.577(17) . ? C12 C13 1.529(18) . ? C12 C15 1.536(18) . ? C12 C14 1.57(2) . ? C16 C21 1.419(18) . ? C16 C17 1.442(18) . ? C17 C18 1.364(18) . ? C17 C23 1.60(2) . ? C18 C19 1.344(19) . ? C19 C20 1.374(19) . ? C20 C21 1.403(17) . ? C21 C27 1.523(19) . ? C23 C26 1.50(2) . ? C23 C25 1.54(2) . ? C23 C24 1.551(18) . ? C27 C28 1.50(2) . ? C27 C29 1.528(19) . ? C27 C30 1.558(19) . ? C31 C32 1.422(18) . ? C31 C36 1.441(17) . ? C32 C33 1.372(18) . ? C32 C38 1.535(16) . ? C33 C34 1.365(17) . ? C34 C35 1.383(18) . ? C35 C36 1.344(17) . ? C36 C42 1.550(18) . ? C38 C39 1.516(17) . ? C38 C41 1.528(18) . ? C38 C40 1.560(17) . ? C42 C44 1.51(2) . ? C42 C45 1.53(2) . ? C42 C43 1.548(18) . ? C46 C47 1.406(17) . ? C46 C51 1.438(19) . ? C47 C48 1.379(17) . ? C47 C53 1.539(19) . ? C48 C49 1.353(17) . ? C49 C50 1.390(17) . ? C50 C51 1.407(18) . ? C51 C57 1.58(3) . ? C51 C57' 1.63(4) . ? C53 C56 1.502(19) . ? C53 C55 1.51(2) . ? C53 C54 1.532(19) . ? C57 C58 1.50(3) . ? C57 C60 1.55(3) . ? C57 C59 1.57(3) . ? C57' C60' 1.51(6) . ? C57' C59' 1.56(5) . ? C57' C58 1.78(4) . ? C61 C62 1.51(3) . ? C61' C62' 1.46(2) . ? C62 C63 1.44(2) . ? C62' C63' 1.46(2) . ? C63 C64 1.49(4) . ? C63' C64' 1.45(2) . ? C65 C66 1.49(2) . ? C66 C67 1.47(2) . ? C67 C68 1.43(2) . ? C69 C70 1.514(18) . ? C70 C71 1.495(19) . ? C71 C72 1.50(2) . ? C73 C74 1.47(2) . ? C74 C75 1.489(19) . ? C75 C76 1.505(19) . ? C77 C78 1.44(3) . ? C78 C79 1.42(3) . ? C79 C80 1.53(4) . ? C81 C82 1.52(3) . ? C82 C83 1.529(18) . ? C83 C83 1.534(19) 3_475 ? 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 O3 Er1 O1 105.3(3) . . ? O3 Er1 F5 105.6(3) . . ? O1 Er1 F5 102.7(3) . . ? O3 Er1 F3 104.1(3) . . ? O1 Er1 F3 103.3(3) . . ? F5 Er1 F3 133.2(2) . . ? O3 Er1 F2 99.8(3) . . ? O1 Er1 F2 154.9(3) . . ? F5 Er1 F2 70.1(2) . . ? F3 Er1 F2 69.8(2) . . ? O3 Er1 F1 161.5(3) . . ? O1 Er1 F1 93.2(3) . . ? F5 Er1 F1 69.5(2) . . ? F3 Er1 F1 70.8(2) . . ? F2 Er1 F1 61.7(2) . . ? O3 Er1 Er2 122.7(2) . . ? O1 Er1 Er2 120.8(2) . . ? F5 Er1 Er2 96.03(17) . . ? F3 Er1 Er2 37.19(17) . . ? F2 Er1 Er2 40.34(15) . . ? F1 Er1 Er2 43.30(16) . . ? O3 Er1 Er3 126.9(2) . . ? O1 Er1 Er3 116.8(2) . . ? F5 Er1 Er3 36.69(17) . . ? F3 Er1 Er3 96.58(17) . . ? F2 Er1 Er3 43.80(16) . . ? F1 Er1 Er3 39.78(15) . . ? Er2 Er1 Er3 59.52(2) . . ? O5 Er2 F4 88.6(3) . . ? O5 Er2 F3 120.0(3) . . ? F4 Er2 F3 134.3(2) . . ? O5 Er2 F2 95.0(3) . . ? F4 Er2 F2 71.3(2) . . ? F3 Er2 F2 71.3(2) . . ? O5 Er2 O9 116.2(3) . . ? F4 Er2 O9 81.7(3) . . ? F3 Er2 O9 110.7(3) . . ? F2 Er2 O9 138.0(3) . . ? O5 Er2 F1 152.6(3) . . ? F4 Er2 F1 69.7(2) . . ? F3 Er2 F1 70.4(2) . . ? F2 Er2 F1 62.9(2) . . ? O9 Er2 F1 78.0(3) . . ? O5 Er2 O10 82.3(3) . . ? F4 Er2 O10 149.0(3) . . ? F3 Er2 O10 74.7(3) . . ? F2 Er2 O10 138.8(3) . . ? O9 Er2 O10 76.1(3) . . ? F1 Er2 O10 124.8(3) . . ? O5 Er2 Er3 112.5(3) . . ? F4 Er2 Er3 37.08(17) . . ? F3 Er2 Er3 97.25(17) . . ? F2 Er2 Er3 44.25(17) . . ? O9 Er2 Er3 95.8(2) . . ? F1 Er2 Er3 40.40(15) . . ? O10 Er2 Er3 165.1(2) . . ? O5 Er2 Er1 129.3(2) . . ? F4 Er2 Er1 97.51(17) . . ? F3 Er2 Er1 36.90(17) . . ? F2 Er2 Er1 42.32(16) . . ? O9 Er2 Er1 114.4(2) . . ? F1 Er2 Er1 43.11(15) . . ? O10 Er2 Er1 111.2(2) . . ? Er3 Er2 Er1 60.47(2) . . ? O7 Er3 F4 87.0(3) . . ? O7 Er3 F5 126.4(3) . . ? F4 Er3 F5 133.2(3) . . ? O7 Er3 F1 97.1(3) . . ? F4 Er3 F1 72.6(2) . . ? F5 Er3 F1 71.6(2) . . ? O7 Er3 O12 116.0(3) . . ? F4 Er3 O12 83.3(3) . . ? F5 Er3 O12 104.5(3) . . ? F1 Er3 O12 137.8(3) . . ? O7 Er3 F2 151.5(3) . . ? F4 Er3 F2 68.6(2) . . ? F5 Er3 F2 68.6(2) . . ? F1 Er3 F2 62.5(2) . . ? O12 Er3 F2 76.7(2) . . ? O7 Er3 O11 79.5(3) . . ? F4 Er3 O11 149.2(3) . . ? F5 Er3 O11 75.8(3) . . ? F1 Er3 O11 136.2(3) . . ? O12 Er3 O11 78.1(3) . . ? F2 Er3 O11 128.9(2) . . ? O7 Er3 Er2 110.7(2) . . ? F4 Er3 Er2 37.39(17) . . ? F5 Er3 Er2 96.09(19) . . ? F1 Er3 Er2 43.35(17) . . ? O12 Er3 Er2 97.98(19) . . ? F2 Er3 Er2 40.80(15) . . ? O11 Er3 Er2 169.6(2) . . ? O7 Er3 Er1 133.3(2) . . ? F4 Er3 Er1 97.36(17) . . ? F5 Er3 Er1 36.26(18) . . ? F1 Er3 Er1 42.48(16) . . ? O12 Er3 Er1 110.7(2) . . ? F2 Er3 Er1 42.39(14) . . ? O11 Er3 Er1 112.1(2) . . ? Er2 Er3 Er1 60.01(2) . . ? Er3 F1 Er1 97.7(2) . . ? Er3 F1 Er2 96.3(2) . . ? Er1 F1 Er2 93.6(2) . . ? Er2 F2 Er1 97.3(2) . . ? Er2 F2 Er3 95.0(2) . . ? Er1 F2 Er3 93.8(2) . . ? Er1 F3 Er2 105.9(3) . . ? Er3 F4 Er2 105.5(3) . . ? Er1 F5 Er3 107.0(3) . . ? C1 O1 Er1 173.3(8) . . ? C4 O2 C7 117.3(11) . . ? C16 O3 Er1 178.4(8) . . ? C19 O4 C22 115.9(12) . . ? C31 O5 Er2 167.0(8) . . ? C34 O6 C37 116.2(10) . . ? C46 O7 Er3 170.7(8) . . ? C49 O8 C52 115.4(11) . . ? C61 O9 C61' 36(2) . . ? C61 O9 C64 101.6(16) . . ? C61' O9 C64 86(2) . . ? C61 O9 C64' 91.0(19) . . ? C61' O9 C64' 110.5(19) . . ? C64 O9 C64' 58.3(18) . . ? C61 O9 Er2 132.4(12) . . ? C61' O9 Er2 126.9(17) . . ? C64 O9 Er2 124.1(13) . . ? C64' O9 Er2 122.4(12) . . ? C65 O10 C68 106.6(10) . . ? C65 O10 Er2 127.4(8) . . ? C68 O10 Er2 125.8(8) . . ? C72 O11 C69 106.1(10) . . ? C72 O11 Er3 127.8(8) . . ? C69 O11 Er3 126.1(7) . . ? C73 O12 C76 106.3(10) . . ? C73 O12 Er3 124.3(8) . . ? C76 O12 Er3 129.4(7) . . ? C80 O13 C77 104(3) . . ? O1 C1 C6 121.0(11) . . ? O1 C1 C2 121.3(11) . . ? C6 C1 C2 117.7(12) . . ? C3 C2 C1 119.8(13) . . ? C3 C2 C8 119.2(12) . . ? C1 C2 C8 121.0(11) . . ? C4 C3 C2 121.5(13) . . ? C5 C4 O2 116.2(13) . . ? C5 C4 C3 119.0(12) . . ? O2 C4 C3 124.8(13) . . ? C4 C5 C6 122.2(13) . . ? C5 C6 C1 119.7(13) . . ? C5 C6 C12 117.8(12) . . ? C1 C6 C12 122.5(11) . . ? C10 C8 C11 111.1(11) . . ? C10 C8 C2 110.6(11) . . ? C11 C8 C2 110.4(11) . . ? C10 C8 C9 107.6(11) . . ? C11 C8 C9 107.8(10) . . ? C2 C8 C9 109.3(10) . . ? C13 C12 C15 106.0(12) . . ? C13 C12 C6 113.1(11) . . ? C15 C12 C6 111.1(11) . . ? C13 C12 C14 106.6(11) . . ? C15 C12 C14 109.9(12) . . ? C6 C12 C14 110.0(11) . . ? O3 C16 C21 119.7(12) . . ? O3 C16 C17 121.9(12) . . ? C21 C16 C17 118.3(11) . . ? C18 C17 C16 119.9(13) . . ? C18 C17 C23 120.7(13) . . ? C16 C17 C23 119.3(11) . . ? C19 C18 C17 122.1(15) . . ? C18 C19 C20 119.4(13) . . ? C18 C19 O4 124.3(14) . . ? C20 C19 O4 116.4(13) . . ? C19 C20 C21 123.1(13) . . ? C20 C21 C16 117.1(12) . . ? C20 C21 C27 120.3(12) . . ? C16 C21 C27 122.6(11) . . ? C26 C23 C25 114.2(12) . . ? C26 C23 C24 107.5(13) . . ? C25 C23 C24 106.6(13) . . ? C26 C23 C17 108.1(12) . . ? C25 C23 C17 111.8(12) . . ? C24 C23 C17 108.5(11) . . ? C28 C27 C21 110.4(11) . . ? C28 C27 C29 114.5(13) . . ? C21 C27 C29 108.7(12) . . ? C28 C27 C30 105.7(12) . . ? C21 C27 C30 111.5(12) . . ? C29 C27 C30 106.0(11) . . ? O5 C31 C32 120.1(11) . . ? O5 C31 C36 120.0(12) . . ? C32 C31 C36 119.9(12) . . ? C33 C32 C31 116.8(11) . . ? C33 C32 C38 119.8(12) . . ? C31 C32 C38 123.0(12) . . ? C34 C33 C32 123.4(13) . . ? C33 C34 C35 119.1(12) . . ? C33 C34 O6 116.9(12) . . ? C35 C34 O6 123.9(11) . . ? C36 C35 C34 122.0(12) . . ? C35 C36 C31 118.5(12) . . ? C35 C36 C42 119.2(11) . . ? C31 C36 C42 122.3(11) . . ? C39 C38 C41 107.6(11) . . ? C39 C38 C32 111.8(11) . . ? C41 C38 C32 111.1(11) . . ? C39 C38 C40 105.3(11) . . ? C41 C38 C40 111.3(11) . . ? C32 C38 C40 109.5(10) . . ? C44 C42 C45 112.1(14) . . ? C44 C42 C43 105.9(12) . . ? C45 C42 C43 107.1(13) . . ? C44 C42 C36 109.2(11) . . ? C45 C42 C36 110.4(12) . . ? C43 C42 C36 112.1(12) . . ? O7 C46 C47 120.5(12) . . ? O7 C46 C51 119.8(11) . . ? C47 C46 C51 119.6(12) . . ? C48 C47 C46 118.9(12) . . ? C48 C47 C53 118.4(11) . . ? C46 C47 C53 122.5(12) . . ? C49 C48 C47 122.0(11) . . ? C48 C49 C50 121.4(12) . . ? C48 C49 O8 126.5(11) . . ? C50 C49 O8 112.0(11) . . ? C49 C50 C51 119.3(13) . . ? C50 C51 C46 118.7(12) . . ? C50 C51 C57 114.5(14) . . ? C46 C51 C57 126.0(13) . . ? C50 C51 C57' 123.7(17) . . ? C46 C51 C57' 114.7(18) . . ? C57 C51 C57' 27.9(13) . . ? C56 C53 C55 109.1(13) . . ? C56 C53 C54 106.2(13) . . ? C55 C53 C54 106.3(13) . . ? C56 C53 C47 114.0(12) . . ? C55 C53 C47 108.7(12) . . ? C54 C53 C47 112.2(12) . . ? C58 C57 C60 100.2(18) . . ? C58 C57 C59 114(2) . . ? C60 C57 C59 110.5(18) . . ? C58 C57 C51 112.2(16) . . ? C60 C57 C51 107(2) . . ? C59 C57 C51 112.0(16) . . ? C60' C57' C59' 113(4) . . ? C60' C57' C51 115(3) . . ? C59' C57' C51 106(3) . . ? C60' C57' C58 125(3) . . ? C59' C57' C58 96(3) . . ? C51 C57' C58 97(3) . . ? C57 C58 C57' 25.6(13) . . ? O9 C61 C62 109.2(19) . . ? O9 C61' C62' 105(2) . . ? C63 C62 C61 104(2) . . ? C61' C62' C63' 105(2) . . ? C62 C63 C64 99(2) . . ? C64' C63' C62' 108(2) . . ? O9 C64 C63 111(2) . . ? C63' C64' O9 101(2) . . ? O10 C65 C66 106.0(11) . . ? C67 C66 C65 107.0(13) . . ? C68 C67 C66 108.1(15) . . ? C67 C68 O10 105.9(14) . . ? O11 C69 C70 107.4(10) . . ? C71 C70 C69 104.7(12) . . ? C72 C71 C70 104.7(12) . . ? O11 C72 C71 104.6(11) . . ? O12 C73 C74 107.4(12) . . ? C73 C74 C75 102.3(13) . . ? C74 C75 C76 103.1(12) . . ? O12 C76 C75 105.9(11) . . ? C78 C77 O13 104(3) . . ? C79 C78 C77 109(3) . . ? C78 C79 C80 104(3) . . ? O13 C80 C79 107(3) . . ? C81 C82 C83 111(2) . . ? C82 C83 C83 110(2) . 3_475 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.380 _refine_diff_density_min -1.477 _refine_diff_density_rms 0.208 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_284sch _database_code_depnum_ccdc_archive 'CCDC 281266' _audit_creation_method Xtal3.6 _audit_creation_date 05-09-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C53 H85 Ho1 O8' _chemical_formula_moiety 'C49 H77 Ho O7, C4 H8 O' _chemical_formula_weight 1015.18 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 16.852(5) _cell_length_b 16.437(6) _cell_length_c 19.084(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.94(4) _cell_angle_gamma 90.00000 _cell_volume 5285(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 10.4 _cell_measurement_theta_max 15.4 _cell_measurement_temperature 300 _exptl_absorpt_coefficient_mu 1.546 _exptl_crystal_description plate _exptl_crystal_size_max .55 _exptl_crystal_size_mid .27 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; xtal absorb ; _exptl_absorpt_correction_T_min .67 _exptl_absorpt_correction_T_max .91 _diffrn_reflns_number 11914 _reflns_number_total 9277 _reflns_Friedel_coverage 0 _reflns_number_gt 4933 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 25. _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .039 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 5 _diffrn_standards_number 6 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .059 _refine_ls_wR_factor_ref .056 _refine_ls_goodness_of_fit_ref 1.314 _refine_ls_number_reflns 4933 _refine_ls_number_parameters 583 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .02 _refine_diff_density_min -1.008 _refine_diff_density_max 1.753 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 212 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 340 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ho ? 0 4 -.666016 4.678 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ho .20765(3) .39052(3) .71821(3) .0419(3) Uani ? ? 1.00000 ? ? O11 .0858(4) .3916(4) .7188(3) .048(4) Uani ? ? 1.00000 ? ? C11 .0092(8) .4145(7) .7225(8) .068(10) Uani ? ? 1.00000 ? ? C12 -.0229(8) .4461(7) .7871(7) .069(10) Uani ? ? 1.00000 ? ? C121 .0182(9) .4483(8) .8580(7) .076(10) Uani ? ? 1.00000 ? ? C122 -.0200(11) .3780(10) .9035(8) .125(14) Uani ? ? 1.00000 ? ? C123 .1068(9) .4388(9) .8624(6) .091(11) Uani ? ? 1.00000 ? ? C124 -.0021(11) .5314(9) .8966(9) .131(15) Uani ? ? 1.00000 ? ? C13 -.1027(10) .4711(9) .7832(9) .092(12) Uani ? ? 1.00000 ? ? C14 -.1476(10) .4695(10) .7247(12) .110(15) Uani ? ? 1.00000 ? ? O14 -.2230(7) .5050(8) .7265(8) .159(12) Uani ? ? 1.00000 ? ? C141 -.2833(11) .4587(11) .7209(11) .129(16) Uani ? ? 1.00000 ? ? C15 -.1177(9) .4345(8) .6638(8) .081(11) Uani ? ? 1.00000 ? ? C16 -.0402(8) .4065(7) .6628(6) .061(9) Uani ? ? 1.00000 ? ? C161 -.0112(8) .3665(8) .5947(6) .062(9) Uani ? ? 1.00000 ? ? C162 .0635(8) .4088(8) .5663(6) .083(10) Uani ? ? 1.00000 ? ? C163 .0068(8) .2781(8) .6117(6) .077(10) Uani ? ? 1.00000 ? ? C164 -.0751(8) .3674(9) .5371(7) .101(12) Uani ? ? 1.00000 ? ? O21 .2521(5) .4995(4) .7524(4) .060(5) Uani ? ? 1.00000 ? ? C21 .2922(8) .5697(7) .7652(5) .046(8) Uani ? ? 1.00000 ? ? C22 .3677(8) .5647(8) .7979(6) .059(9) Uani ? ? 1.00000 ? ? C221 .4067(8) .4850(7) .8251(7) .073(10) Uani ? ? 1.00000 ? ? C222 .3742(15) .4061(12) .7856(12) .062(8) Uiso ? ? .50000 ? ? C223 .4878(14) .4823(19) .7856(15) .108(11) Uiso ? ? .50000 ? ? C224 .419(2) .488(2) .9034(11) .132(13) Uiso ? ? .50000 ? ? C222' .4186(17) .4149(13) .7751(12) .066(8) Uiso ? ? .50000 ? ? C223' .4811(14) .4976(17) .8729(14) .088(9) Uiso ? ? .50000 ? ? C224' .3486(14) .4510(15) .8853(12) .076(8) Uiso ? ? .50000 ? ? C23 .4104(8) .6374(9) .8098(7) .076(10) Uani ? ? 1.00000 ? ? C24 .3771(10) .7120(9) .7896(7) .075(11) Uani ? ? 1.00000 ? ? O24 .4138(8) .7849(7) .8003(6) .136(11) Uani ? ? 1.00000 ? ? C241 .4655(10) .7958(9) .8511(8) .102(13) Uani ? ? 1.00000 ? ? C25 .3047(9) .7121(8) .7597(7) .068(10) Uani ? ? 1.00000 ? ? C26 .2597(8) .6449(8) .7460(6) .052(8) Uani ? ? 1.00000 ? ? C261 .1785(9) .6571(8) .7148(8) .077(11) Uani ? ? 1.00000 ? ? C262 .1125(15) .6246(16) .7622(15) .09(2) Uani ? ? .50000 ? ? C263 .159(2) .615(3) .6467(14) .10(3) Uiso ? ? .50000 ? ? C264 .1507(18) .7449(12) .702(2) .10(3) Uani ? ? .50000 ? ? C262' .125(2) .706(2) .7596(18) .12(3) Uani ? ? .50000 ? ? C263' .131(2) .5826(17) .6888(15) .10(3) Uani ? ? .50000 ? ? C264' .1959(18) .702(2) .6435(13) .14(3) Uani ? ? .50000 ? ? O31 .2716(4) .3584(4) .6285(3) .051(5) Uani ? ? 1.00000 ? ? C31 .3169(6) .3325(7) .5740(5) .048(7) Uani ? ? 1.00000 ? ? C32 .3308(7) .2484(6) .5678(5) .046(7) Uani ? ? 1.00000 ? ? C321 .2930(8) .1831(7) .6136(7) .064(9) Uani ? ? 1.00000 ? ? C322 .2032(9) .1923(7) .6088(7) .088(11) Uani ? ? 1.00000 ? ? C323 .3274(8) .1905(8) .6877(6) .083(10) Uani ? ? 1.00000 ? ? C324 .3116(10) .0959(7) .5878(8) .116(13) Uani ? ? 1.00000 ? ? C33 .3792(7) .2244(7) .5093(6) .062(9) Uani ? ? 1.00000 ? ? C34 .4127(8) .2781(8) .4655(6) .067(9) Uani ? ? 1.00000 ? ? O34 .4585(6) .2442(5) .4135(5) .094(7) Uani ? ? 1.00000 ? ? C341 .4913(9) .2970(9) .3660(8) .115(13) Uani ? ? 1.00000 ? ? C35 .4007(7) .3590(7) .4754(6) .059(8) Uani ? ? 1.00000 ? ? C36 .3525(6) .3897(7) .5284(5) .049(6) Uani ? ? 1.00000 ? ? C361 .3367(7) .4817(7) .5327(6) .053(8) Uani ? ? 1.00000 ? ? C362 .2485(8) .4988(7) .5194(7) .075(10) Uani ? ? 1.00000 ? ? C363 .3824(8) .5290(7) .4739(6) .077(10) Uani ? ? 1.00000 ? ? C364 .3657(8) .5159(7) .6026(6) .064(8) Uani ? ? 1.00000 ? ? O1 .2010(5) .2775(4) .7951(4) .056(5) Uani ? ? 1.00000 ? ? C2 .2504(9) .2580(9) .8544(7) .086(11) Uani ? ? 1.00000 ? ? C3 .2119(12) .1914(12) .8928(9) .158(18) Uani ? ? 1.00000 ? ? C4 .1319(10) .1828(9) .8639(8) .099(12) Uani ? ? 1.00000 ? ? C5 .1336(8) .2221(7) .7909(6) .070(9) Uani ? ? 1.00000 ? ? O01 .3433(18) .704(2) 1.011(2) .32(4) Uani ? ? 1.00000 ? ? C02 .270(3) .716(3) .9661(18) .24(4) Uani ? ? 1.00000 ? ? C03 .219(2) .649(3) .980(2) .24(4) Uani ? ? 1.00000 ? ? C04 .262(4) .6043(17) 1.040(3) .28(4) Uani ? ? 1.00000 ? ? C05 .326(5) .644(3) 1.059(3) .46(8) Uani ? ? 1.00000 ? ? H122a .00372 .37761 .94882 .18700 Uiso ? ? 1.00000 ? ? H122b -.01175 .32740 .88113 .18700 Uiso ? ? 1.00000 ? ? H122c -.07563 .38761 .90735 .18700 Uiso ? ? 1.00000 ? ? H123a .12377 .44197 .90991 .13700 Uiso ? ? 1.00000 ? ? H123b .13121 .48030 .83603 .13700 Uiso ? ? 1.00000 ? ? H123c .12050 .38702 .84383 .13700 Uiso ? ? 1.00000 ? ? H124a .02381 .53302 .94123 .19700 Uiso ? ? 1.00000 ? ? H124b -.05805 .53533 .90289 .19700 Uiso ? ? 1.00000 ? ? H124c .01501 .57629 .86928 .19700 Uiso ? ? 1.00000 ? ? H13 -.12585 .49193 .82469 .11800 Uiso ? ? 1.00000 ? ? H141a -.32992 .49085 .71321 .19100 Uiso ? ? 1.00000 ? ? H141b -.28872 .42814 .76246 .19100 Uiso ? ? 1.00000 ? ? H141c -.27707 .42300 .68211 .19100 Uiso ? ? 1.00000 ? ? H15 -.15021 .43055 .62318 .10200 Uiso ? ? 1.00000 ? ? H162a .07957 .38261 .52429 .12600 Uiso ? ? 1.00000 ? ? H162b .10565 .40489 .60023 .12600 Uiso ? ? 1.00000 ? ? H162c .05284 .46438 .55694 .12600 Uiso ? ? 1.00000 ? ? H163a .02509 .25126 .57100 .11700 Uiso ? ? 1.00000 ? ? H163b -.03939 .25189 .62810 .11700 Uiso ? ? 1.00000 ? ? H163c .04733 .27576 .64734 .11700 Uiso ? ? 1.00000 ? ? H164a -.05481 .34212 .49624 .15000 Uiso ? ? 1.00000 ? ? H164b -.09005 .42148 .52683 .15000 Uiso ? ? 1.00000 ? ? H164c -.12018 .33756 .55240 .15000 Uiso ? ? 1.00000 ? ? H222a .40495 .36034 .79942 .11300 Uiso ? ? .50000 ? ? H222b .37946 .41392 .73603 .11300 Uiso ? ? .50000 ? ? H222c .32056 .39798 .79612 .11300 Uiso ? ? .50000 ? ? H223a .52075 .52611 .80094 .14600 Uiso ? ? .50000 ? ? H223b .47827 .48723 .73645 .14600 Uiso ? ? .50000 ? ? H223c .51400 .43223 .79500 .14600 Uiso ? ? .50000 ? ? H224a .44200 .43779 .91878 .42100 Uiso ? ? .50000 ? ? H224b .37270 .49922 .92583 .42100 Uiso ? ? .50000 ? ? H224c .45824 .53048 .91371 .42100 Uiso ? ? .50000 ? ? H223'a .50257 .44721 .88685 .15000 Uiso ? ? .50000 ? ? H223'b .46752 .52883 .91295 .15000 Uiso ? ? .50000 ? ? H223'c .52068 .52742 .84736 .15000 Uiso ? ? .50000 ? ? H222'a .43927 .36929 .80064 .11300 Uiso ? ? .50000 ? ? H222'b .45612 .43020 .74059 .11300 Uiso ? ? .50000 ? ? H222'c .37008 .40083 .75339 .11300 Uiso ? ? .50000 ? ? H224'a .36959 .40164 .90363 .13100 Uiso ? ? .50000 ? ? H224'b .29749 .44227 .86610 .13100 Uiso ? ? .50000 ? ? H224'c .34602 .49020 .92219 .13100 Uiso ? ? .50000 ? ? H23 .46160 .63580 .83076 .09200 Uiso ? ? 1.00000 ? ? H241a .47962 .85206 .85298 .15100 Uiso ? ? 1.00000 ? ? H241b .51155 .76451 .84214 .15100 Uiso ? ? 1.00000 ? ? H241c .44336 .78004 .89412 .15100 Uiso ? ? 1.00000 ? ? H25 .28320 .76359 .74644 .08800 Uiso ? ? 1.00000 ? ? H262a .06074 .63909 .73938 .11500 Uiso ? ? .50000 ? ? H262b .11453 .64776 .80571 .11500 Uiso ? ? .50000 ? ? H262c .11391 .56701 .76361 .11500 Uiso ? ? .50000 ? ? H263a .10780 .63173 .63011 .12400 Uiso ? ? .50000 ? ? H263b .16123 .55871 .65156 .12400 Uiso ? ? .50000 ? ? H263c .19725 .63216 .61214 .12400 Uiso ? ? .50000 ? ? H264a .10783 .74521 .67061 .13600 Uiso ? ? .50000 ? ? H264b .19423 .77493 .68360 .13600 Uiso ? ? .50000 ? ? H264c .13646 .76799 .74578 .13600 Uiso ? ? .50000 ? ? H262'a .07336 .70769 .74027 .11500 Uiso ? ? .50000 ? ? H262'b .14557 .75979 .76433 .11500 Uiso ? ? .50000 ? ? H262'c .12334 .68195 .80557 .11500 Uiso ? ? .50000 ? ? H263'a .08046 .59775 .67229 .10900 Uiso ? ? .50000 ? ? H263'b .12633 .54381 .72596 .10900 Uiso ? ? .50000 ? ? H263'c .15940 .55649 .65137 .10900 Uiso ? ? .50000 ? ? H264'a .14749 .70946 .61816 .16600 Uiso ? ? .50000 ? ? H264'b .23142 .67076 .61711 .16600 Uiso ? ? .50000 ? ? H264'c .21863 .75376 .65394 .16600 Uiso ? ? .50000 ? ? H322a .17914 .15226 .63692 .13200 Uiso ? ? 1.00000 ? ? H322b .18620 .18594 .56134 .13200 Uiso ? ? 1.00000 ? ? H322c .18877 .24503 .62472 .13200 Uiso ? ? 1.00000 ? ? H323a .30452 .14995 .71661 .12100 Uiso ? ? 1.00000 ? ? H323b .31641 .24270 .70598 .12100 Uiso ? ? 1.00000 ? ? H323c .38344 .18245 .68661 .12100 Uiso ? ? 1.00000 ? ? H324a .28668 .05725 .61740 .17500 Uiso ? ? 1.00000 ? ? H324b .36699 .08702 .58820 .17500 Uiso ? ? 1.00000 ? ? H324c .29116 .08904 .54103 .17500 Uiso ? ? 1.00000 ? ? H33 .38736 .16789 .50140 .07700 Uiso ? ? 1.00000 ? ? H341a .52105 .26749 .33281 .17300 Uiso ? ? 1.00000 ? ? H341b .52484 .33483 .38973 .17300 Uiso ? ? 1.00000 ? ? H341c .44990 .32621 .34200 .17300 Uiso ? ? 1.00000 ? ? H35 .42666 .39682 .44562 .07400 Uiso ? ? 1.00000 ? ? H362a .23920 .55568 .52223 .11400 Uiso ? ? 1.00000 ? ? H362b .21848 .47156 .55394 .11400 Uiso ? ? 1.00000 ? ? H362c .23368 .47961 .47428 .11400 Uiso ? ? 1.00000 ? ? H363a .37166 .58559 .47747 .11300 Uiso ? ? 1.00000 ? ? H363b .36492 .50997 .42910 .11300 Uiso ? ? 1.00000 ? ? H363c .43763 .51976 .47930 .11300 Uiso ? ? 1.00000 ? ? H364a .35555 .57243 .60465 .09500 Uiso ? ? 1.00000 ? ? H364b .42108 .50619 .60797 .09500 Uiso ? ? 1.00000 ? ? H364c .33851 .48916 .63960 .09500 Uiso ? ? 1.00000 ? ? H2a .25587 .30474 .88335 .10900 Uiso ? ? 1.00000 ? ? H2b .30121 .24140 .83897 .10900 Uiso ? ? 1.00000 ? ? H3a .20981 .20456 .94137 .19700 Uiso ? ? 1.00000 ? ? H3b .24056 .14233 .88706 .19700 Uiso ? ? 1.00000 ? ? H4a .09482 .21003 .89283 .12000 Uiso ? ? 1.00000 ? ? H4b .11799 .12712 .86014 .12000 Uiso ? ? 1.00000 ? ? H5a .14076 .18293 .75544 .08900 Uiso ? ? 1.00000 ? ? H5b .08609 .25215 .78156 .08900 Uiso ? ? 1.00000 ? ? H02a .28097 .70764 .91581 .31200 Uiso ? ? 1.00000 ? ? H02b .24165 .76326 .97099 .31200 Uiso ? ? 1.00000 ? ? H03a .20647 .61137 .94500 .31900 Uiso ? ? 1.00000 ? ? H03b .16714 .66699 1.00018 .31900 Uiso ? ? 1.00000 ? ? H04a .27220 .55186 1.02421 .33000 Uiso ? ? 1.00000 ? ? H04b .22899 .60377 1.07974 .33000 Uiso ? ? 1.00000 ? ? H05a .37460 .60453 1.05427 .46000 Uiso ? ? 1.00000 ? ? H05b .33016 .66239 1.10448 .46000 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ho .0526(3) .0433(3) .0303(3) -.0019(4) .0107(2) -.0021(4) O11 .051(5) .058(4) .035(4) -.001(5) .015(4) .008(4) C11 .066(10) .040(8) .100(12) -.007(7) .013(10) .010(7) C12 .072(10) .059(8) .075(10) -.005(8) .028(9) .007(8) C121 .105(13) .082(10) .042(8) -.002(9) .043(9) -.008(8) C122 .166(18) .128(15) .083(11) -.025(13) .034(12) -.014(11) C123 .100(12) .131(13) .042(8) .012(11) .013(8) -.036(8) C124 .153(17) .105(13) .137(15) .024(12) .053(13) -.054(12) C13 .077(12) .096(12) .103(14) .016(10) .035(11) -.017(11) C14 .050(11) .105(14) .18(2) .011(10) -.012(13) -.010(14) O14 .077(9) .144(12) .258(17) .026(9) .031(11) -.030(11) C141 .081(13) .136(16) .171(18) -.015(13) .005(13) -.026(15) C15 .069(11) .075(10) .099(12) .015(8) .020(9) .013(9) C16 .057(8) .066(9) .060(8) -.002(7) .014(7) .012(7) C161 .064(9) .087(10) .037(7) -.010(7) .011(7) .013(7) C162 .093(11) .123(13) .032(7) -.032(9) .005(7) .013(8) C163 .087(11) .092(10) .054(9) .011(9) .013(8) .008(8) C164 .078(11) .143(15) .081(10) -.006(10) -.006(9) .034(10) O21 .073(6) .056(5) .051(5) -.006(5) .019(4) -.014(4) C21 .076(10) .046(7) .018(7) -.011(8) .022(7) -.005(5) C22 .069(10) .063(9) .046(8) -.014(8) .024(7) -.005(7) C221 .066(10) .065(9) .087(11) -.007(8) -.003(8) .007(8) C23 .070(10) .096(12) .062(9) -.004(9) .004(8) .013(8) C24 .103(13) .073(10) .048(9) -.035(10) .006(9) .002(8) O24 .184(13) .105(9) .118(10) -.070(9) -.048(9) .014(8) C241 .123(15) .098(12) .086(12) -.031(11) .022(11) -.019(10) C25 .094(12) .058(8) .053(9) -.015(9) .018(9) .001(7) C26 .068(9) .054(8) .035(7) .000(7) .003(7) .001(6) C261 .080(12) .058(9) .094(13) -.012(8) .019(11) .004(9) C262 .11(3) .07(2) .10(2) .06(2) .01(2) -.00(2) C264 .08(2) .050(17) .17(4) .021(16) -.01(2) .05(2) C262' .11(3) .14(3) .13(3) .02(3) .03(3) .03(3) C263' .13(3) .12(3) .039(18) -.00(2) .02(2) -.00(2) C264' .06(2) .23(4) .12(3) .04(3) -.00(2) -.12(3) O31 .059(5) .055(5) .039(4) -.006(4) .019(4) -.011(4) C31 .049(8) .053(7) .043(7) -.003(6) .017(6) -.017(6) C32 .068(9) .038(6) .033(7) .002(6) .012(6) -.007(6) C321 .082(10) .038(7) .073(10) .000(7) .030(8) -.005(7) C322 .095(12) .059(9) .110(12) -.016(9) .013(10) -.023(9) C323 .117(13) .085(10) .049(8) .020(9) .023(9) .030(8) C324 .177(17) .043(9) .132(13) .008(9) .096(13) -.016(9) C33 .072(9) .060(8) .056(8) .001(7) .023(7) -.022(7) C34 .080(11) .067(9) .057(9) -.010(8) .034(8) -.017(8) O34 .110(8) .090(7) .085(7) -.030(6) .069(6) -.036(6) C341 .132(15) .112(13) .103(12) -.037(11) .092(11) -.050(10) C35 .063(9) .068(8) .047(7) -.008(7) .034(7) -.001(6) C36 .054(7) .047(6) .044(6) -.011(7) -.000(6) .008(7) C361 .056(8) .051(7) .052(8) .008(6) .000(7) -.000(7) C362 .073(10) .069(9) .084(10) .006(8) .006(8) -.013(8) C363 .092(11) .073(9) .065(9) -.008(8) .026(8) .028(8) C364 .083(10) .059(8) .050(8) -.018(7) .014(7) -.020(7) O1 .078(6) .057(5) .034(5) .000(5) .013(4) .012(4) C2 .095(12) .099(11) .063(10) .002(9) -.010(9) .012(9) C3 .147(18) .20(2) .123(16) -.079(17) -.047(14) .108(15) C4 .129(15) .086(11) .082(11) -.023(11) .020(11) .037(9) C5 .087(11) .064(9) .058(9) -.017(8) .006(8) .008(7) O01 .26(3) .43(5) .28(3) -.01(3) .03(3) -.01(3) C02 .18(3) .36(5) .19(3) .06(3) .01(3) .13(3) C03 .27(4) .21(4) .24(4) -.06(3) .06(3) -.03(3) C04 .43(6) .083(17) .34(5) .10(3) .23(5) .12(3) C05 .75(14) .29(5) .33(6) -.14(6) .10(8) .20(5) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ho O11 . . 2.054(7) ? Ho O21 . . 2.044(7) ? Ho O31 . . 2.105(7) ? Ho O1 . . 2.370(7) ? O11 C11 . . 1.347(15) ? C11 C12 . . 1.45(2) ? C11 C16 . . 1.41(2) ? C12 C121 . . 1.51(2) ? C12 C13 . . 1.41(2) ? C121 C122 . . 1.59(2) ? C121 C123 . . 1.50(2) ? C121 C124 . . 1.59(2) ? C122 H122a . . .946 ? C122 H122b . . .947 ? C122 H122c . . .955 ? C123 H123a . . .948 ? C123 H123b . . .945 ? C123 H123c . . .952 ? C124 H124a . . .951 ? C124 H124b . . .955 ? C124 H124c . . .950 ? C13 C14 . . 1.34(3) ? C13 H13 . . .952 ? C14 O14 . . 1.40(2) ? C14 C15 . . 1.40(3) ? O14 C141 . . 1.27(2) ? C141 H141a . . .956 ? C141 H141b . . .94 ? C141 H141c . . .95 ? C15 C16 . . 1.38(2) ? C15 H15 . . .944 ? C16 C161 . . 1.543(17) ? C161 C162 . . 1.543(18) ? C161 C163 . . 1.518(18) ? C161 C164 . . 1.528(18) ? C162 H162a . . .953 ? C162 H162b . . .956 ? C162 H162c . . .948 ? C163 H163a . . .949 ? C163 H163b . . .947 ? C163 H163c . . .957 ? C164 H164a . . .952 ? C164 H164b . . .943 ? C164 H164c . . .954 ? O21 C21 . . 1.357(14) ? C21 C22 . . 1.410(18) ? C21 C26 . . 1.399(17) ? C22 C221 . . 1.552(18) ? C22 C23 . . 1.41(2) ? C221 C222 . . 1.59(2) ? C221 C223 . . 1.57(3) ? C221 C224 . . 1.51(3) ? C221 C222' . . 1.51(3) ? C221 C223' . . 1.55(3) ? C221 C224' . . 1.62(3) ? C222 H222a . . .95 ? C222 H222b . . .96 ? C222 H222c . . .94 ? C223 H223a . . .95 ? C223 H223b . . .95 ? C223 H223c . . .95 ? C224 H224a . . .95 ? C224 H224b . . .92 ? C224 H224c . . .98 ? C222' H222'a . . .96 ? C222' H222'b . . .95 ? C222' H222'c . . .94 ? C223' H223'a . . .94 ? C223' H223'b . . .95 ? C223' H223'c . . .97 ? C224' H224'a . . .95 ? C224' H224'b . . .94 ? C224' H224'c . . .96 ? C23 C24 . . 1.40(2) ? C23 H23 . . .946 ? C24 O24 . . 1.36(2) ? C24 C25 . . 1.34(2) ? O24 C241 . . 1.31(2) ? C241 H241a . . .956 ? C241 H241b . . .948 ? C241 H241c . . .943 ? C25 C26 . . 1.364(19) ? C25 H25 . . .953 ? C26 C261 . . 1.50(2) ? C261 C262 . . 1.54(3) ? C261 C263 . . 1.50(3) ? C261 C264 . . 1.53(3) ? C261 C262' . . 1.48(4) ? C261 C263' . . 1.54(3) ? C261 C264' . . 1.58(3) ? C262 H262a . . 1.00 ? C262 H262b . . .91 ? C262 H262c . . .95 ? C263 H263a . . .96 ? C263 H263b . . .93 ? C263 H263c . . .97 ? C264 H264a . . .94 ? C264 H264b . . .96 ? C264 H264c . . .94 ? C262' H262'a . . .94 ? C262' H262'b . . .96 ? C262' H262'c . . .96 ? C263' H263'a . . .94 ? C263' H263'b . . .96 ? C263' H263'c . . .96 ? C264' H264'a . . .95 ? C264' H264'b . . .94 ? C264' H264'c . . .96 ? O31 C31 . . 1.367(13) ? C31 C32 . . 1.408(15) ? C31 C36 . . 1.421(15) ? C32 C321 . . 1.530(16) ? C32 C33 . . 1.449(16) ? C321 C322 . . 1.52(2) ? C321 C323 . . 1.525(18) ? C321 C324 . . 1.549(17) ? C322 H322a . . .944 ? C322 H322b . . .952 ? C322 H322c . . .951 ? C323 H323a . . .951 ? C323 H323b . . .946 ? C323 H323c . . .954 ? C324 H324a . . .952 ? C324 H324b . . .944 ? C324 H324c . . .958 ? C33 C34 . . 1.347(17) ? C33 H33 . . .951 ? C34 O34 . . 1.383(16) ? C34 C35 . . 1.360(18) ? O34 C341 . . 1.377(17) ? C341 H341a . . .947 ? C341 H341b . . .950 ? C341 H341c . . .958 ? C35 C36 . . 1.400(16) ? C35 H35 . . .954 ? C36 C361 . . 1.538(16) ? C361 C362 . . 1.529(17) ? C361 C363 . . 1.575(17) ? C361 C364 . . 1.521(16) ? C362 H362a . . .950 ? C362 H362b . . .949 ? C362 H362c . . .947 ? C363 H363a . . .951 ? C363 H363b . . .951 ? C363 H363c . . .948 ? C364 H364a . . .945 ? C364 H364b . . .951 ? C364 H364c . . .956 ? O1 C2 . . 1.430(15) ? O1 C5 . . 1.458(15) ? C2 C3 . . 1.47(2) ? C2 H2a . . .950 ? C2 H2b . . .951 ? C3 C4 . . 1.45(3) ? C3 H3a . . .953 ? C3 H3b . . .95 ? C4 C5 . . 1.54(2) ? C4 H4a . . .952 ? C4 H4b . . .948 ? C5 H5a . . .943 ? C5 H5b . . .955 ? O01 C02 . . 1.51(5) ? O01 C05 . . 1.38(7) ? C02 C03 . . 1.43(7) ? C02 H02a . . .99 ? C02 H02b . . .92 ? C03 C04 . . 1.52(7) ? C03 H03a . . .93 ? C03 H03b . . 1.01 ? C04 C05 . . 1.30(9) ? C04 H04a . . .93 ? C04 H04b . . .95 ? C05 H05a . . 1.05 ? C05 H05b . . .93 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O11 Ho O21 . . . 110.6(3) ? O11 Ho O31 . . . 122.2(3) ? O11 Ho O1 . . . 86.9(3) ? O21 Ho O31 . . . 106.8(3) ? O21 Ho O1 . . . 120.7(3) ? O31 Ho O1 . . . 109.7(3) ? Ho O11 C11 . . . 164.0(7) ? O11 C11 C12 . . . 120.9(12) ? O11 C11 C16 . . . 119.2(12) ? C12 C11 C16 . . . 119.9(12) ? C11 C12 C121 . . . 126.8(12) ? C11 C12 C13 . . . 115.4(13) ? C121 C12 C13 . . . 117.6(13) ? C12 C121 C122 . . . 106.8(11) ? C12 C121 C123 . . . 119.2(11) ? C12 C121 C124 . . . 109.6(12) ? C122 C121 C123 . . . 107.8(12) ? C122 C121 C124 . . . 106.2(11) ? C123 C121 C124 . . . 106.5(12) ? C121 C122 H122a . . . 109.7 ? C121 C122 H122b . . . 109.2 ? C121 C122 H122c . . . 109.2 ? H122a C122 H122b . . . 110.1 ? H122a C122 H122c . . . 109.4 ? H122b C122 H122c . . . 109.3 ? C121 C123 H123a . . . 109.3 ? C121 C123 H123b . . . 109.7 ? C121 C123 H123c . . . 108.5 ? H123a C123 H123b . . . 110.1 ? H123a C123 H123c . . . 109.5 ? H123b C123 H123c . . . 109.7 ? C121 C124 H124a . . . 109.8 ? C121 C124 H124b . . . 109.6 ? C121 C124 H124c . . . 110.1 ? H124a C124 H124b . . . 109.0 ? H124a C124 H124c . . . 109.4 ? H124b C124 H124c . . . 109.0 ? C12 C13 C14 . . . 124.4(16) ? C12 C13 H13 . . . 117.8 ? C14 C13 H13 . . . 117.8 ? C13 C14 O14 . . . 118.2(18) ? C13 C14 C15 . . . 119.7(15) ? O14 C14 C15 . . . 122.1(17) ? C14 O14 C141 . . . 118.2(14) ? O14 C141 H141a . . . 109.6 ? O14 C141 H141b . . . 109.6 ? O14 C141 H141c . . . 109.6 ? H141a C141 H141b . . . 109.5 ? H141a C141 H141c . . . 108.8 ? H141b C141 H141c . . . 109.7 ? C14 C15 C16 . . . 120.1(14) ? C14 C15 H15 . . . 119.9 ? C16 C15 H15 . . . 120.0 ? C11 C16 C15 . . . 120.3(12) ? C11 C16 C161 . . . 122.0(11) ? C15 C16 C161 . . . 117.7(11) ? C16 C161 C162 . . . 112.0(10) ? C16 C161 C163 . . . 107.1(9) ? C16 C161 C164 . . . 111.9(11) ? C162 C161 C163 . . . 110.2(11) ? C162 C161 C164 . . . 108.1(10) ? C163 C161 C164 . . . 107.4(11) ? C161 C162 H162a . . . 109.7 ? C161 C162 H162b . . . 109.5 ? C161 C162 H162c . . . 110.4 ? H162a C162 H162b . . . 108.7 ? H162a C162 H162c . . . 109.4 ? H162b C162 H162c . . . 109.2 ? C161 C163 H163a . . . 109.7 ? C161 C163 H163b . . . 110.1 ? C161 C163 H163c . . . 109.1 ? H163a C163 H163b . . . 109.9 ? H163a C163 H163c . . . 109.0 ? H163b C163 H163c . . . 109.1 ? C161 C164 H164a . . . 109.0 ? C161 C164 H164b . . . 109.9 ? C161 C164 H164c . . . 109.2 ? H164a C164 H164b . . . 109.9 ? H164a C164 H164c . . . 109.0 ? H164b C164 H164c . . . 109.7 ? Ho O21 C21 . . . 168.8(7) ? O21 C21 C22 . . . 118.3(10) ? O21 C21 C26 . . . 120.8(11) ? C22 C21 C26 . . . 120.9(11) ? C21 C22 C221 . . . 124.8(11) ? C21 C22 C23 . . . 118.4(12) ? C221 C22 C23 . . . 116.7(11) ? C22 C221 C222 . . . 112.9(12) ? C22 C221 C223 . . . 103.3(14) ? C22 C221 C224 . . . 111.0(17) ? C22 C221 C222' . . . 119.5(13) ? C22 C221 C223' . . . 114.7(14) ? C22 C221 C224' . . . 105.7(12) ? C222 C221 C223 . . . 92.5(16) ? C222 C221 C224 . . . 122.4(18) ? C223 C221 C224 . . . 112(2) ? C222' C221 C223' . . . 111.0(16) ? C222' C221 C224' . . . 105.8(15) ? C223' C221 C224' . . . 96.9(15) ? C221 C222 H222a . . . 109 ? C221 C222 H222b . . . 108.8 ? C221 C222 H222c . . . 109.8 ? H222a C222 H222b . . . 109 ? H222a C222 H222c . . . 110 ? H222b C222 H222c . . . 110 ? C221 C223 H223a . . . 110 ? C221 C223 H223b . . . 110 ? C221 C223 H223c . . . 110 ? H223a C223 H223b . . . 109 ? H223a C223 H223c . . . 109 ? H223b C223 H223c . . . 109 ? C221 C224 H224a . . . 109 ? C221 C224 H224b . . . 111 ? C221 C224 H224c . . . 108 ? H224a C224 H224b . . . 112 ? H224a C224 H224c . . . 107 ? H224b C224 H224c . . . 109 ? C221 C222' H222'a . . . 109 ? C221 C222' H222'b . . . 109.3 ? C221 C222' H222'c . . . 110 ? H222'a C222' H222'b . . . 109 ? H222'a C222' H222'c . . . 110 ? H222'b C222' H222'c . . . 110 ? C221 C223' H223'a . . . 111 ? C221 C223' H223'b . . . 110 ? C221 C223' H223'c . . . 109 ? H223'a C223' H223'b . . . 110 ? H223'a C223' H223'c . . . 109 ? H223'b C223' H223'c . . . 108 ? C221 C224' H224'a . . . 109 ? C221 C224' H224'b . . . 110 ? C221 C224' H224'c . . . 109 ? H224'a C224' H224'b . . . 110 ? H224'a C224' H224'c . . . 109 ? H224'b C224' H224'c . . . 110 ? C22 C23 C24 . . . 119.7(13) ? C22 C23 H23 . . . 120.3 ? C24 C23 H23 . . . 120.0 ? C23 C24 O24 . . . 123.3(14) ? C23 C24 C25 . . . 118.5(14) ? O24 C24 C25 . . . 118.2(13) ? C24 O24 C241 . . . 121.9(12) ? O24 C241 H241a . . . 108.8 ? O24 C241 H241b . . . 109.2 ? O24 C241 H241c . . . 109.8 ? H241a C241 H241b . . . 109.1 ? H241a C241 H241c . . . 109.6 ? H241b C241 H241c . . . 110.2 ? C24 C25 C26 . . . 125.6(13) ? C24 C25 H25 . . . 117.1 ? C26 C25 H25 . . . 117.4 ? C21 C26 C25 . . . 116.8(12) ? C21 C26 C261 . . . 125.1(12) ? C25 C26 C261 . . . 118.0(12) ? C26 C261 C262 . . . 112.5(14) ? C26 C261 C263 . . . 117.9(17) ? C26 C261 C264 . . . 117.5(15) ? C26 C261 C262' . . . 113.7(17) ? C26 C261 C263' . . . 119.0(15) ? C26 C261 C264' . . . 103.0(15) ? C262 C261 C263 . . . 101.6(18) ? C262 C261 C264 . . . 101.2(18) ? C262' C261 C263' . . . 107(2) ? C262' C261 C264' . . . 112(2) ? C263' C261 C264' . . . 101.2(17) ? C261 C262 H262a . . . 107 ? C261 C262 H262b . . . 112 ? C261 C262 H262c . . . 110 ? H262a C262 H262b . . . 108 ? H262a C262 H262c . . . 106 ? H262b C262 H262c . . . 113 ? C261 C263 H263a . . . 110 ? C261 C263 H263b . . . 111 ? C261 C263 H263c . . . 109 ? H263a C263 H263b . . . 110 ? H263a C263 H263c . . . 107 ? H263b C263 H263c . . . 109 ? C261 C264 H264a . . . 110 ? C261 C264 H264b . . . 108 ? C261 C264 H264c . . . 109 ? H264a C264 H264b . . . 110 ? H264a C264 H264c . . . 111 ? H264b C264 H264c . . . 109 ? C261 C262' H262'a . . . 111 ? C261 C262' H262'b . . . 109 ? C261 C262' H262'c . . . 110 ? H262'a C262' H262'b . . . 109 ? H262'a C262' H262'c . . . 109 ? H262'b C262' H262'c . . . 108 ? C261 C263' H263'a . . . 111 ? C261 C263' H263'b . . . 110 ? C261 C263' H263'c . . . 110 ? H263'a C263' H263'b . . . 109 ? H263'a C263' H263'c . . . 109 ? H263'b C263' H263'c . . . 108 ? C261 C264' H264'a . . . 109 ? C261 C264' H264'b . . . 110 ? C261 C264' H264'c . . . 108 ? H264'a C264' H264'b . . . 110 ? H264'a C264' H264'c . . . 109 ? H264'b C264' H264'c . . . 110 ? Ho O31 C31 . . . 174.7(6) ? O31 C31 C32 . . . 117.7(9) ? O31 C31 C36 . . . 120.5(9) ? C32 C31 C36 . . . 121.6(10) ? C31 C32 C321 . . . 124.7(10) ? C31 C32 C33 . . . 115.5(9) ? C321 C32 C33 . . . 119.6(9) ? C32 C321 C322 . . . 108.6(10) ? C32 C321 C323 . . . 108.6(10) ? C32 C321 C324 . . . 112.3(11) ? C322 C321 C323 . . . 114.2(11) ? C322 C321 C324 . . . 106.2(11) ? C323 C321 C324 . . . 107.0(10) ? C321 C322 H322a . . . 109.4 ? C321 C322 H322b . . . 109.2 ? C321 C322 H322c . . . 109.3 ? H322a C322 H322b . . . 109.8 ? H322a C322 H322c . . . 109.9 ? H322b C322 H322c . . . 109.2 ? C321 C323 H323a . . . 109.3 ? C321 C323 H323b . . . 109.9 ? C321 C323 H323c . . . 109.2 ? H323a C323 H323b . . . 109.8 ? H323a C323 H323c . . . 109.0 ? H323b C323 H323c . . . 109.5 ? C321 C324 H324a . . . 109.6 ? C321 C324 H324b . . . 110.2 ? C321 C324 H324c . . . 109.4 ? H324a C324 H324b . . . 109.8 ? H324a C324 H324c . . . 108.6 ? H324b C324 H324c . . . 109.2 ? C32 C33 C34 . . . 123.2(11) ? C32 C33 H33 . . . 118.2 ? C34 C33 H33 . . . 118.6 ? C33 C34 O34 . . . 115.2(11) ? C33 C34 C35 . . . 119.3(12) ? O34 C34 C35 . . . 125.5(11) ? C34 O34 C341 . . . 116.9(10) ? O34 C341 H341a . . . 109.9 ? O34 C341 H341b . . . 109.9 ? O34 C341 H341c . . . 109.5 ? H341a C341 H341b . . . 109.7 ? H341a C341 H341c . . . 109.0 ? H341b C341 H341c . . . 108.8 ? C34 C35 C36 . . . 122.9(11) ? C34 C35 H35 . . . 118.8 ? C36 C35 H35 . . . 118.3 ? C31 C36 C35 . . . 117.4(10) ? C31 C36 C361 . . . 122.8(9) ? C35 C36 C361 . . . 119.7(10) ? C36 C361 C362 . . . 109.9(9) ? C36 C361 C363 . . . 111.1(9) ? C36 C361 C364 . . . 110.9(9) ? C362 C361 C363 . . . 106.0(9) ? C362 C361 C364 . . . 111.9(10) ? C363 C361 C364 . . . 106.8(9) ? C361 C362 H362a . . . 109.4 ? C361 C362 H362b . . . 109.1 ? C361 C362 H362c . . . 109.3 ? H362a C362 H362b . . . 109.5 ? H362a C362 H362c . . . 109.7 ? H362b C362 H362c . . . 109.8 ? C361 C363 H363a . . . 109.6 ? C361 C363 H363b . . . 109.3 ? C361 C363 H363c . . . 109.5 ? H363a C363 H363b . . . 109.3 ? H363a C363 H363c . . . 109.6 ? H363b C363 H363c . . . 109.5 ? C361 C364 H364a . . . 110.1 ? C361 C364 H364b . . . 109.4 ? C361 C364 H364c . . . 109.1 ? H364a C364 H364b . . . 109.8 ? H364a C364 H364c . . . 109.4 ? H364b C364 H364c . . . 108.9 ? Ho O1 C2 . . . 129.3(7) ? Ho O1 C5 . . . 120.0(6) ? C2 O1 C5 . . . 110.2(9) ? O1 C2 C3 . . . 107.8(12) ? O1 C2 H2a . . . 109.2 ? O1 C2 H2b . . . 109.5 ? C3 C2 H2a . . . 110.5 ? C3 C2 H2b . . . 110.3 ? H2a C2 H2b . . . 109.4 ? C2 C3 C4 . . . 107.2(14) ? C2 C3 H3a . . . 109.8 ? C2 C3 H3b . . . 110.2 ? C4 C3 H3a . . . 110.0 ? C4 C3 H3b . . . 110.2 ? H3a C3 H3b . . . 109.4 ? C3 C4 C5 . . . 105.8(13) ? C3 C4 H4a . . . 110.4 ? C3 C4 H4b . . . 110.4 ? C5 C4 H4a . . . 110.5 ? C5 C4 H4b . . . 110.2 ? H4a C4 H4b . . . 109.5 ? O1 C5 C4 . . . 103.8(10) ? O1 C5 H5a . . . 110.9 ? O1 C5 H5b . . . 109.7 ? C4 C5 H5a . . . 111.6 ? C4 C5 H5b . . . 111.0 ? H5a C5 H5b . . . 109.7 ? C02 O01 C05 . . . 107(4) ? O01 C02 C03 . . . 106(4) ? O01 C02 H02a . . . 112 ? O01 C02 H02b . . . 118 ? C03 C02 H02a . . . 102 ? C03 C02 H02b . . . 109 ? H02a C02 H02b . . . 109 ? C02 C03 C04 . . . 104(4) ? C02 C03 H03a . . . 120 ? C02 C03 H03b . . . 112 ? C04 C03 H03a . . . 109 ? C04 C03 H03b . . . 106 ? H03a C03 H03b . . . 106 ? C03 C04 C05 . . . 111(4) ? C03 C04 H04a . . . 108 ? C03 C04 H04b . . . 109 ? C05 C04 H04a . . . 113 ? C05 C04 H04b . . . 105 ? H04a C04 H04b . . . 111 ? O01 C05 C04 . . . 111(5) ? O01 C05 H05a . . . 102 ? O01 C05 H05b . . . 111 ? C04 C05 H05a . . . 109 ? C04 C05 H05b . . . 119 ? H05a C05 H05b . . . 103 ? _exptl_crystal_F_000 2136 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .841 _reflns_d_resolution_low 12.423 _diffrn_reflns_av_sigmaI/netI .144 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 300 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 12 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .123 _refine_ls_wR_factor_all .067 _refine_ls_goodness_of_fit_all 1.209 _refine_ls_shift/su_mean .001 #===END data_342sch _database_code_depnum_ccdc_archive 'CCDC 281267' _audit_creation_method Xtal3.6 _audit_creation_date 05-09-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C46 H78 O8 Sm1' _chemical_formula_moiety 'C46 H78 O8 Sm1' _chemical_formula_weight 909.48 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 16.019(3) _cell_length_b 15.340(3) _cell_length_c 19.799(10) _cell_angle_alpha 90.00000 _cell_angle_beta 94.10(3) _cell_angle_gamma 90.00000 _cell_volume 4853(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 16.7 _cell_measurement_temperature 300 _exptl_absorpt_coefficient_mu 1.256 _exptl_crystal_description block _exptl_crystal_size_max .35 _exptl_crystal_size_mid .23 _exptl_crystal_size_min .13 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; xtal absorb ; _exptl_absorpt_correction_T_min .79 _exptl_absorpt_correction_T_max .85 _diffrn_reflns_number 11815 _reflns_number_total 8407 _reflns_Friedel_coverage 0 _reflns_number_gt 4127 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 8 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .062 _refine_ls_wR_factor_ref .078 _refine_ls_goodness_of_fit_ref 1.306 _refine_ls_number_reflns 4127 _refine_ls_number_parameters 497 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .049 _refine_diff_density_min -1.691 _refine_diff_density_max 2.025 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 184 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 312 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Sm ? 0 4 -.53302 3.442 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sm -.02319(4) .44504(4) .74493(3) .0522(3) Uani ? ? 1.00000 ? ? O11 .0939(4) .4574(4) .8190(3) .056(4) Uani ? ? 1.00000 ? ? C11 .1654(6) .4592(6) .8576(5) .052(6) Uani ? ? 1.00000 ? ? C12 .2075(7) .3829(7) .8814(5) .061(7) Uani ? ? 1.00000 ? ? C121 .1738(7) .2932(8) .8628(6) .070(8) Uani ? ? 1.00000 ? ? C122 .0890(9) .2803(9) .8919(7) .096(10) Uani ? ? 1.00000 ? ? C123 .1647(8) .2806(8) .7864(7) .085(9) Uani ? ? 1.00000 ? ? C124 .2333(10) .2200(9) .8919(8) .110(12) Uani ? ? 1.00000 ? ? C13 .2814(7) .3894(9) .9241(6) .077(8) Uani ? ? 1.00000 ? ? C14 .3145(8) .4689(9) .9403(7) .087(9) Uani ? ? 1.00000 ? ? O14 .3866(6) .4804(8) .9831(6) .142(9) Uani ? ? 1.00000 ? ? C141 .4295(12) .4065(18) 1.0057(13) .20(2) Uani ? ? 1.00000 ? ? C15 .2754(8) .5430(8) .9201(7) .085(9) Uani ? ? 1.00000 ? ? C16 .1992(7) .5417(7) .8772(6) .066(7) Uani ? ? 1.00000 ? ? C161 .1583(8) .6271(7) .8536(6) .073(8) Uani ? ? 1.00000 ? ? C162 .1520(9) .6343(8) .7773(7) .090(10) Uani ? ? 1.00000 ? ? C163 .0727(8) .6347(7) .8816(6) .082(9) Uani ? ? 1.00000 ? ? C164 .2095(10) .7068(9) .8788(8) .111(12) Uani ? ? 1.00000 ? ? O21 -.1198(4) .5167(5) .6736(3) .063(5) Uani ? ? 1.00000 ? ? C21 -.1808(7) .5587(7) .6371(5) .060(6) Uani ? ? 1.00000 ? ? C22 -.2524(7) .5149(7) .6075(5) .057(6) Uani ? ? 1.00000 ? ? C221 -.2638(7) .4153(7) .6141(6) .066(7) Uani ? ? 1.00000 ? ? C222 -.2678(8) .3929(9) .6889(7) .089(10) Uani ? ? 1.00000 ? ? C223 -.1892(8) .3679(8) .5852(7) .084(9) Uani ? ? 1.00000 ? ? C224 -.3438(8) .3811(9) .5769(7) .095(10) Uani ? ? 1.00000 ? ? C23 -.3163(7) .5634(8) .5714(6) .071(7) Uani ? ? 1.00000 ? ? C24 -.3099(7) .6512(8) .5638(5) .069(7) Uani ? ? 1.00000 ? ? O24 -.3715(6) .7029(6) .5307(5) .105(7) Uani ? ? 1.00000 ? ? C241 -.4419(8) .6608(10) .5008(7) .103(11) Uani ? ? 1.00000 ? ? C25 -.2404(7) .6932(8) .5895(6) .074(8) Uani ? ? 1.00000 ? ? C26 -.1756(7) .6518(7) .6253(5) .064(7) Uani ? ? 1.00000 ? ? C261 -.0996(8) .7030(8) .6549(6) .083(9) Uani ? ? 1.00000 ? ? C262 -.0192(8) .6689(10) .6231(7) .097(10) Uani ? ? 1.00000 ? ? C263 -.0907(8) .6978(8) .7313(7) .093(10) Uani ? ? 1.00000 ? ? C264 -.1062(11) .8014(10) .6349(9) .135(14) Uani ? ? 1.00000 ? ? O101 .0709(5) .4260(6) .6455(4) .086(6) Uani ? ? 1.00000 ? ? C102 .0481(11) .4158(16) .5767(7) .170(17) Uani ? ? 1.00000 ? ? C103 .1170(14) .446(2) .5430(9) .27(3) Uani ? ? 1.00000 ? ? C104 .1867(12) .4569(15) .5871(9) .173(18) Uani ? ? 1.00000 ? ? C105 .1581(11) .4447(15) .6503(9) .164(18) Uani ? ? 1.00000 ? ? O201 -.1150(5) .4695(5) .8454(4) .074(5) Uani ? ? 1.00000 ? ? C202 -.0892(10) .4544(9) .9144(6) .097(10) Uani ? ? 1.00000 ? ? C203 -.1203(10) .5284(11) .9528(7) .115(12) Uani ? ? 1.00000 ? ? C204 -.1846(14) .5697(14) .9063(9) .18(2) Uani ? ? 1.00000 ? ? C205 -.1892(9) .5158(10) .8442(7) .098(10) Uani ? ? 1.00000 ? ? O301 -.0664(6) .2852(5) .7397(4) .092(6) Uani ? ? 1.00000 ? ? C302 -.1182(9) .2444(9) .7901(7) .097(10) Uani ? ? 1.00000 ? ? C303 -.1421(12) .1581(11) .7607(9) .147(15) Uani ? ? 1.00000 ? ? C304 -.1068(12) .1460(10) .6973(9) .133(14) Uani ? ? 1.00000 ? ? C305 -.0443(8) .2213(9) .6940(7) .096(10) Uani ? ? 1.00000 ? ? O401 .4080(19) .5479(11) .7117(10) .32(3) Uani ? ? 1.00000 ? ? C402 .4410(17) .4840(18) .6711(10) .21(2) Uani ? ? 1.00000 ? ? C403 .460(2) .4183(16) .7089(18) .29(3) Uani ? ? 1.00000 ? ? C404 .4033(16) .4167(15) .7585(16) .24(3) Uani ? ? 1.00000 ? ? C405 .3809(19) .498(2) .7656(13) .27(3) Uani ? ? 1.00000 ? ? H122a .06067 .22600 .87616 .13900 Uiso ? ? 1.00000 ? ? H122b .09036 .28069 .93928 .13900 Uiso ? ? 1.00000 ? ? H122c .04921 .32630 .87610 .13900 Uiso ? ? 1.00000 ? ? H123a .21225 .30635 .76641 .12600 Uiso ? ? 1.00000 ? ? H123b .16308 .22029 .77446 .12600 Uiso ? ? 1.00000 ? ? H123c .11529 .30907 .76632 .12600 Uiso ? ? 1.00000 ? ? H124a .23896 .22393 .94089 .15600 Uiso ? ? 1.00000 ? ? H124b .28899 .22861 .87673 .15600 Uiso ? ? 1.00000 ? ? H124c .21501 .16375 .87957 .15600 Uiso ? ? 1.00000 ? ? H13 .31016 .33458 .94212 .09200 Uiso ? ? 1.00000 ? ? H141a .43416 .36922 .96972 .26500 Uiso ? ? 1.00000 ? ? H141b .40030 .38300 1.04074 .26500 Uiso ? ? 1.00000 ? ? H141c .48358 .42646 1.02346 .26500 Uiso ? ? 1.00000 ? ? H15 .29652 .60220 .93402 .11300 Uiso ? ? 1.00000 ? ? H162a .12340 .68518 .75962 .13500 Uiso ? ? 1.00000 ? ? H162b .20429 .62998 .75728 .13500 Uiso ? ? 1.00000 ? ? H162c .11969 .58442 .75768 .13500 Uiso ? ? 1.00000 ? ? H163a .07744 .63330 .92953 .11900 Uiso ? ? 1.00000 ? ? H163b .04588 .68812 .86698 .11900 Uiso ? ? 1.00000 ? ? H163c .03731 .58729 .86470 .11900 Uiso ? ? 1.00000 ? ? H164a .26871 .69617 .88212 .14600 Uiso ? ? 1.00000 ? ? H164b .19655 .72202 .92640 .14600 Uiso ? ? 1.00000 ? ? H164c .19846 .75830 .85340 .14600 Uiso ? ? 1.00000 ? ? H222a -.32080 .41101 .70642 .12600 Uiso ? ? 1.00000 ? ? H222b -.26250 .33146 .69851 .12600 Uiso ? ? 1.00000 ? ? H222c -.22574 .42251 .71668 .12600 Uiso ? ? 1.00000 ? ? H223a -.19624 .30584 .58673 .12000 Uiso ? ? 1.00000 ? ? H223b -.13805 .38246 .61034 .12000 Uiso ? ? 1.00000 ? ? H223c -.18378 .38382 .53858 .12000 Uiso ? ? 1.00000 ? ? H224a -.34081 .38927 .52759 .15000 Uiso ? ? 1.00000 ? ? H224b -.39112 .41369 .58897 .15000 Uiso ? ? 1.00000 ? ? H224c -.35195 .32157 .58445 .15000 Uiso ? ? 1.00000 ? ? H23 -.36510 .53044 .55176 .09400 Uiso ? ? 1.00000 ? ? H241a -.42554 .60865 .47962 .15000 Uiso ? ? 1.00000 ? ? H241b -.47870 .64781 .53465 .15000 Uiso ? ? 1.00000 ? ? H241c -.46916 .69820 .46780 .15000 Uiso ? ? 1.00000 ? ? H25 -.23540 .75597 .58245 .09300 Uiso ? ? 1.00000 ? ? H262a .02988 .70070 .64229 .14500 Uiso ? ? 1.00000 ? ? H262b -.02277 .67513 .57646 .14500 Uiso ? ? 1.00000 ? ? H262c -.00926 .60838 .63509 .14500 Uiso ? ? 1.00000 ? ? H263a -.08499 .63896 .74634 .13000 Uiso ? ? 1.00000 ? ? H263b -.13953 .72213 .75016 .13000 Uiso ? ? 1.00000 ? ? H263c -.04309 .73018 .74920 .13000 Uiso ? ? 1.00000 ? ? H264a -.05861 .83264 .65262 .18600 Uiso ? ? 1.00000 ? ? H264b -.15546 .82641 .65000 .18600 Uiso ? ? 1.00000 ? ? H264c -.10873 .80570 .58592 .18600 Uiso ? ? 1.00000 ? ? H102a .00035 .45071 .56396 .21000 Uiso ? ? 1.00000 ? ? H102b .03602 .35665 .56657 .21000 Uiso ? ? 1.00000 ? ? H103a .10384 .49750 .52036 .26000 Uiso ? ? 1.00000 ? ? H103b .13072 .40136 .51095 .26000 Uiso ? ? 1.00000 ? ? H104a .20671 .51526 .58332 .20500 Uiso ? ? 1.00000 ? ? H104b .22928 .41719 .57884 .20500 Uiso ? ? 1.00000 ? ? H105a .16842 .49495 .67680 .12400 Uiso ? ? 1.00000 ? ? H105b .18720 .39614 .67092 .12400 Uiso ? ? 1.00000 ? ? H202a -.02854 .44815 .92067 .12400 Uiso ? ? 1.00000 ? ? H202b -.11181 .39931 .92971 .12400 Uiso ? ? 1.00000 ? ? H203a -.07437 .56778 .96630 .13700 Uiso ? ? 1.00000 ? ? H203b -.14374 .50965 .99354 .13700 Uiso ? ? 1.00000 ? ? H204a -.16323 .62723 .89517 .22000 Uiso ? ? 1.00000 ? ? H204b -.23361 .57445 .92632 .22000 Uiso ? ? 1.00000 ? ? H205a -.19954 .55168 .80291 .12400 Uiso ? ? 1.00000 ? ? H205b -.23900 .47753 .84334 .12400 Uiso ? ? 1.00000 ? ? H302a -.16416 .28131 .79872 .13000 Uiso ? ? 1.00000 ? ? H302b -.08436 .23900 .83362 .13000 Uiso ? ? 1.00000 ? ? H303a -.20363 .15307 .75423 .17000 Uiso ? ? 1.00000 ? ? H303b -.12595 .10997 .79180 .17000 Uiso ? ? 1.00000 ? ? H304a -.14821 .14546 .65992 .17500 Uiso ? ? 1.00000 ? ? H304b -.07782 .08917 .69578 .17500 Uiso ? ? 1.00000 ? ? H305a -.04698 .24621 .64780 .11500 Uiso ? ? 1.00000 ? ? H305b .01276 .20269 .70301 .11500 Uiso ? ? 1.00000 ? ? H402a .48598 .50419 .64850 .27000 Uiso ? ? 1.00000 ? ? H402b .39794 .46186 .63949 .27000 Uiso ? ? 1.00000 ? ? H403a .51644 .43612 .73660 .28000 Uiso ? ? 1.00000 ? ? H403b .47032 .36790 .68965 .28000 Uiso ? ? 1.00000 ? ? H404a .42225 .38773 .79704 .31000 Uiso ? ? 1.00000 ? ? H404b .35590 .38553 .73603 .31000 Uiso ? ? 1.00000 ? ? H405a .41249 .51487 .80870 .33500 Uiso ? ? 1.00000 ? ? H405b .32514 .50072 .77125 .33500 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sm .0474(3) .0621(4) .0483(3) -.0002(4) .0120(2) -.0036(3) O11 .055(4) .054(4) .061(4) -.000(4) .012(3) -.005(4) C11 .054(6) .054(7) .051(6) -.007(5) .019(5) -.004(5) C12 .056(7) .068(8) .062(7) .001(6) .012(6) -.012(6) C121 .062(8) .077(8) .069(8) .011(6) -.001(6) -.003(6) C122 .088(11) .083(10) .120(12) -.019(8) .035(9) .005(9) C123 .091(10) .061(8) .105(10) .012(7) .012(8) -.015(7) C124 .137(14) .073(10) .117(12) .032(9) -.005(10) .012(9) C13 .045(7) .101(10) .084(9) -.003(7) .008(6) -.000(8) C14 .052(7) .121(12) .087(9) .002(7) -.007(7) -.001(8) O14 .072(7) .156(10) .190(11) .009(7) -.058(7) -.020(9) C141 .095(14) .27(3) .24(2) -.019(17) -.075(16) .05(2) C15 .080(9) .088(10) .087(9) -.004(8) .000(7) -.019(8) C16 .052(7) .081(9) .067(7) -.001(6) .012(5) .007(6) C161 .072(9) .059(8) .088(9) -.008(6) .013(7) -.002(6) C162 .098(11) .084(10) .089(9) -.003(8) .013(8) .027(8) C163 .099(11) .059(8) .092(9) .005(7) .027(8) -.016(7) C164 .120(13) .073(9) .141(14) -.025(9) .007(11) -.007(9) O21 .063(5) .069(5) .056(4) .004(4) .004(4) .003(4) C21 .057(7) .077(8) .048(6) .006(6) .016(5) -.006(6) C22 .055(7) .067(7) .048(6) .000(6) .008(5) .004(5) C221 .044(6) .073(8) .080(8) -.004(6) .007(6) -.003(6) C222 .087(10) .087(10) .096(10) -.024(8) .027(8) .008(8) C223 .077(9) .085(10) .089(9) .010(7) .009(7) -.019(7) C224 .069(9) .099(11) .115(11) -.023(8) -.010(8) -.015(9) C23 .052(7) .094(9) .067(7) -.007(7) .008(6) .004(7) C24 .050(7) .089(9) .067(7) .007(6) .004(6) .015(7) O24 .095(7) .109(7) .108(7) .015(6) -.015(6) .024(6) C241 .073(10) .133(13) .101(10) .020(9) -.018(8) .019(10) C25 .073(9) .070(8) .081(8) .007(7) .023(7) .012(7) C26 .055(7) .068(8) .071(7) -.013(6) .023(6) -.002(6) C261 .084(10) .080(9) .085(9) -.009(7) -.003(7) .007(7) C262 .071(9) .116(11) .107(11) -.008(9) .029(8) .011(9) C263 .075(10) .079(9) .124(11) -.008(7) -.001(8) -.034(8) C264 .128(15) .089(11) .181(17) -.036(10) -.036(13) .016(11) O101 .073(6) .127(8) .062(5) .011(5) .031(4) .001(5) C102 .125(15) .33(3) .058(9) -.079(17) .031(9) -.015(13) C103 .136(18) .60(6) .076(11) -.18(3) .028(11) -.05(2) C104 .124(15) .29(3) .110(13) -.091(16) .055(11) .022(15) C105 .102(14) .29(3) .107(13) .022(15) .041(11) .014(16) O201 .069(5) .093(6) .061(5) .020(4) .020(4) -.009(4) C202 .114(12) .115(12) .062(8) .042(9) .017(7) .007(8) C203 .112(13) .174(16) .061(8) .032(11) .025(8) -.021(9) C204 .22(2) .23(2) .101(13) .125(19) .021(14) -.053(14) C205 .092(11) .131(12) .075(9) .025(9) .032(8) .004(9) O301 .096(7) .069(6) .113(7) -.019(5) .028(5) -.006(5) C302 .106(12) .099(11) .089(10) -.027(9) .022(8) .017(8) C303 .179(19) .099(12) .173(17) -.067(12) .074(14) -.035(12) C304 .171(18) .098(12) .134(14) -.042(11) .028(12) -.037(11) C305 .079(10) .094(10) .117(12) -.013(8) .029(8) -.002(9) O401 .53(4) .193(18) .25(2) .07(2) .18(3) .065(16) C402 .27(3) .24(3) .131(17) -.00(2) .080(19) -.044(18) C403 .31(4) .16(2) .42(4) .13(2) .21(3) .16(3) C404 .20(3) .15(2) .39(4) .027(18) .16(3) .04(2) C405 .32(4) .29(3) .21(2) .08(3) .20(3) .04(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sm O11 . . 2.305(7) ? Sm O21 . . 2.299(7) ? Sm O101 . . 2.580(8) ? Sm O201 . . 2.584(8) ? Sm O301 . . 2.548(8) ? O11 C11 . . 1.331(12) ? C11 C12 . . 1.416(15) ? C11 C16 . . 1.420(15) ? C12 C121 . . 1.515(16) ? C12 C13 . . 1.407(15) ? C121 C122 . . 1.527(18) ? C121 C123 . . 1.521(17) ? C121 C124 . . 1.556(19) ? C122 H122a . . .989 ? C122 H122b . . .937 ? C122 H122c . . .986 ? C123 H123a . . .968 ? C123 H123b . . .955 ? C123 H123c . . .964 ? C124 H124a . . .970 ? C124 H124b . . .970 ? C124 H124c . . .938 ? C13 C14 . . 1.36(2) ? C13 H13 . . 1.013 ? C14 O14 . . 1.396(16) ? C14 C15 . . 1.344(19) ? O14 C141 . . 1.38(3) ? C141 H141a . . .92 ? C141 H141b . . .94 ? C141 H141c . . .96 ? C15 C16 . . 1.435(17) ? C15 H15 . . 1.002 ? C16 C161 . . 1.522(16) ? C161 C162 . . 1.512(18) ? C161 C163 . . 1.519(18) ? C161 C164 . . 1.536(18) ? C162 H162a . . .959 ? C162 H162b . . .954 ? C162 H162c . . .987 ? C163 H163a . . .946 ? C163 H163b . . .960 ? C163 H163c . . .968 ? C164 H164a . . .960 ? C164 H164b . . 1.006 ? C164 H164c . . .946 ? O21 C21 . . 1.338(12) ? C21 C22 . . 1.420(15) ? C21 C26 . . 1.451(16) ? C22 C221 . . 1.545(16) ? C22 C23 . . 1.417(15) ? C221 C222 . . 1.527(18) ? C221 C223 . . 1.543(17) ? C221 C224 . . 1.525(17) ? C222 H222a . . .980 ? C222 H222b . . .965 ? C222 H222c . . .953 ? C223 H223a . . .960 ? C223 H223b . . .954 ? C223 H223c . . .965 ? C224 H224a . . .989 ? C224 H224b . . .953 ? C224 H224c . . .936 ? C23 C24 . . 1.360(17) ? C23 H23 . . .988 ? C24 O24 . . 1.392(14) ? C24 C25 . . 1.353(16) ? O24 C241 . . 1.395(17) ? C241 H241a . . .948 ? C241 H241b . . .945 ? C241 H241c . . .952 ? C25 C26 . . 1.371(16) ? C25 H25 . . .977 ? C26 C261 . . 1.529(16) ? C261 C262 . . 1.56(2) ? C261 C263 . . 1.51(2) ? C261 C264 . . 1.56(2) ? C262 H262a . . .979 ? C262 H262b . . .926 ? C262 H262c . . .968 ? C263 H263a . . .953 ? C263 H263b . . .966 ? C263 H263c . . .956 ? C264 H264a . . .947 ? C264 H264b . . .944 ? C264 H264c . . .970 ? O101 C102 . . 1.394(16) ? O101 C105 . . 1.42(2) ? C102 C103 . . 1.41(3) ? C102 H102a . . .95 ? C102 H102b . . .95 ? C103 C104 . . 1.38(3) ? C103 H103a . . .92 ? C103 H103b . . .97 ? C104 C105 . . 1.37(3) ? C104 H104a . . .96 ? C104 H104b . . .94 ? C105 H105a . . .94 ? C105 H105b . . .95 ? O201 C202 . . 1.418(14) ? O201 C205 . . 1.384(17) ? C202 C203 . . 1.47(2) ? C202 H202a . . .976 ? C202 H202b . . .976 ? C203 C204 . . 1.47(3) ? C203 H203a . . .976 ? C203 H203b . . .958 ? C204 C205 . . 1.48(2) ? C204 H204a . . .98 ? C204 H204b . . .91 ? C205 H205a . . .989 ? C205 H205b . . .989 ? O301 C302 . . 1.481(17) ? O301 C305 . . 1.396(17) ? C302 C303 . . 1.48(2) ? C302 H302a . . .954 ? C302 H302b . . .989 ? C303 C304 . . 1.42(3) ? C303 H303a . . .99 ? C303 H303b . . .984 ? C304 C305 . . 1.53(2) ? C304 H304a . . .958 ? C304 H304b . . .989 ? C305 H305a . . .990 ? C305 H305b . . .962 ? O401 C402 . . 1.40(3) ? O401 C405 . . 1.41(4) ? C402 C403 . . 1.28(4) ? C402 H402a . . .93 ? C402 H402b . . .96 ? C403 C404 . . 1.39(5) ? C403 H403a . . 1.05 ? C403 H403b . . .88 ? C404 C405 . . 1.31(4) ? C404 H404a . . .92 ? C404 H404b . . .98 ? C405 H405a . . .99 ? C405 H405b . . .91 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O11 Sm O21 . . . 146.4(2) ? O11 Sm O101 . . . 90.1(2) ? O11 Sm O201 . . . 88.9(2) ? O11 Sm O301 . . . 108.1(2) ? O21 Sm O101 . . . 89.4(3) ? O21 Sm O201 . . . 90.5(2) ? O21 Sm O301 . . . 105.5(3) ? O101 Sm O201 . . . 178.0(3) ? O101 Sm O301 . . . 91.8(3) ? O201 Sm O301 . . . 90.2(3) ? Sm O11 C11 . . . 174.2(6) ? O11 C11 C12 . . . 122.9(9) ? O11 C11 C16 . . . 118.2(9) ? C12 C11 C16 . . . 118.9(9) ? C11 C12 C121 . . . 121.2(9) ? C11 C12 C13 . . . 120.1(10) ? C121 C12 C13 . . . 118.8(10) ? C12 C121 C122 . . . 109.7(10) ? C12 C121 C123 . . . 111.4(10) ? C12 C121 C124 . . . 111.5(10) ? C122 C121 C123 . . . 109.5(10) ? C122 C121 C124 . . . 107.8(11) ? C123 C121 C124 . . . 106.9(10) ? C121 C122 H122a . . . 113.0 ? C121 C122 H122b . . . 114.8 ? C121 C122 H122c . . . 111.1 ? H122a C122 H122b . . . 107.3 ? H122a C122 H122c . . . 103.4 ? H122b C122 H122c . . . 106.3 ? C121 C123 H123a . . . 109.3 ? C121 C123 H123b . . . 111.6 ? C121 C123 H123c . . . 111.7 ? H123a C123 H123b . . . 107.6 ? H123a C123 H123c . . . 107.1 ? H123b C123 H123c . . . 109.3 ? C121 C124 H124a . . . 109.7 ? C121 C124 H124b . . . 109.9 ? C121 C124 H124c . . . 113.3 ? H124a C124 H124b . . . 106.2 ? H124a C124 H124c . . . 108.8 ? H124b C124 H124c . . . 108.8 ? C12 C13 C14 . . . 120.2(12) ? C12 C13 H13 . . . 119.6 ? C14 C13 H13 . . . 120.2 ? C13 C14 O14 . . . 123.3(12) ? C13 C14 C15 . . . 121.5(12) ? O14 C14 C15 . . . 114.9(12) ? C14 O14 C141 . . . 117.6(14) ? O14 C141 H141a . . . 109 ? O14 C141 H141b . . . 106.9 ? O14 C141 H141c . . . 106 ? H141a C141 H141b . . . 114 ? H141a C141 H141c . . . 111 ? H141b C141 H141c . . . 110 ? C14 C15 C16 . . . 121.5(12) ? C14 C15 H15 . . . 123.0 ? C16 C15 H15 . . . 115.5 ? C11 C16 C15 . . . 117.7(10) ? C11 C16 C161 . . . 122.4(9) ? C15 C16 C161 . . . 120.0(10) ? C16 C161 C162 . . . 111.5(10) ? C16 C161 C163 . . . 109.5(9) ? C16 C161 C164 . . . 112.2(10) ? C162 C161 C163 . . . 111.2(10) ? C162 C161 C164 . . . 105.2(11) ? C163 C161 C164 . . . 107.1(10) ? C161 C162 H162a . . . 114.8 ? C161 C162 H162b . . . 114.3 ? C161 C162 H162c . . . 109.4 ? H162a C162 H162b . . . 108.4 ? H162a C162 H162c . . . 105.3 ? H162b C162 H162c . . . 103.6 ? C161 C163 H163a . . . 110.8 ? C161 C163 H163b . . . 110.6 ? C161 C163 H163c . . . 109.7 ? H163a C163 H163b . . . 108.9 ? H163a C163 H163c . . . 109.4 ? H163b C163 H163c . . . 107.3 ? C161 C164 H164a . . . 112.8 ? C161 C164 H164b . . . 110.3 ? C161 C164 H164c . . . 114.6 ? H164a C164 H164b . . . 104.2 ? H164a C164 H164c . . . 108.9 ? H164b C164 H164c . . . 105.2 ? Sm O21 C21 . . . 174.4(7) ? O21 C21 C22 . . . 122.1(10) ? O21 C21 C26 . . . 120.8(9) ? C22 C21 C26 . . . 117.0(9) ? C21 C22 C221 . . . 122.1(9) ? C21 C22 C23 . . . 119.5(10) ? C221 C22 C23 . . . 118.5(9) ? C22 C221 C222 . . . 108.5(9) ? C22 C221 C223 . . . 109.6(9) ? C22 C221 C224 . . . 113.6(9) ? C222 C221 C223 . . . 109.9(10) ? C222 C221 C224 . . . 107.4(10) ? C223 C221 C224 . . . 107.8(10) ? C221 C222 H222a . . . 112.2 ? C221 C222 H222b . . . 113.7 ? C221 C222 H222c . . . 112.1 ? H222a C222 H222b . . . 105.8 ? H222a C222 H222c . . . 104.8 ? H222b C222 H222c . . . 107.7 ? C221 C223 H223a . . . 111.1 ? C221 C223 H223b . . . 110.9 ? C221 C223 H223c . . . 111.1 ? H223a C223 H223b . . . 108.3 ? H223a C223 H223c . . . 107.4 ? H223b C223 H223c . . . 107.9 ? C221 C224 H224a . . . 109.5 ? C221 C224 H224b . . . 110.8 ? C221 C224 H224c . . . 112.3 ? H224a C224 H224b . . . 106.1 ? H224a C224 H224c . . . 107.4 ? H224b C224 H224c . . . 110.5 ? C22 C23 C24 . . . 121.3(10) ? C22 C23 H23 . . . 116.9 ? C24 C23 H23 . . . 121.8 ? C23 C24 O24 . . . 124.0(10) ? C23 C24 C25 . . . 119.7(10) ? O24 C24 C25 . . . 116.2(11) ? C24 O24 C241 . . . 117.4(10) ? O24 C241 H241a . . . 109.8 ? O24 C241 H241b . . . 108.8 ? O24 C241 H241c . . . 109.3 ? H241a C241 H241b . . . 110.0 ? H241a C241 H241c . . . 109.5 ? H241b C241 H241c . . . 109.5 ? C24 C25 C26 . . . 123.1(11) ? C24 C25 H25 . . . 119.3 ? C26 C25 H25 . . . 117.6 ? C21 C26 C25 . . . 119.3(10) ? C21 C26 C261 . . . 119.8(9) ? C25 C26 C261 . . . 120.9(10) ? C26 C261 C262 . . . 109.3(10) ? C26 C261 C263 . . . 111.8(10) ? C26 C261 C264 . . . 111.2(11) ? C262 C261 C263 . . . 111.3(10) ? C262 C261 C264 . . . 105.4(12) ? C263 C261 C264 . . . 107.7(11) ? C261 C262 H262a . . . 109.8 ? C261 C262 H262b . . . 111.9 ? C261 C262 H262c . . . 110.4 ? H262a C262 H262b . . . 109.0 ? H262a C262 H262c . . . 105.6 ? H262b C262 H262c . . . 109.9 ? C261 C263 H263a . . . 111.3 ? C261 C263 H263b . . . 110.2 ? C261 C263 H263c . . . 111.1 ? H263a C263 H263b . . . 107.8 ? H263a C263 H263c . . . 108.7 ? H263b C263 H263c . . . 107.6 ? C261 C264 H264a . . . 110.9 ? C261 C264 H264b . . . 110.9 ? C261 C264 H264c . . . 108.4 ? H264a C264 H264b . . . 110.3 ? H264a C264 H264c . . . 108.1 ? H264b C264 H264c . . . 108.2 ? Sm O101 C102 . . . 129.2(9) ? Sm O101 C105 . . . 123.4(8) ? C102 O101 C105 . . . 106.0(12) ? O101 C102 C103 . . . 105.4(15) ? O101 C102 H102a . . . 110.2 ? O101 C102 H102b . . . 110.5 ? C103 C102 H102a . . . 109 ? C103 C102 H102b . . . 112 ? H102a C102 H102b . . . 109.6 ? C102 C103 C104 . . . 111.5(16) ? C102 C103 H103a . . . 111 ? C102 C103 H103b . . . 107 ? C104 C103 H103a . . . 111 ? C104 C103 H103b . . . 107 ? H103a C103 H103b . . . 109.9 ? C103 C104 C105 . . . 104.7(17) ? C103 C104 H104a . . . 109 ? C103 C104 H104b . . . 112 ? C105 C104 H104a . . . 110 ? C105 C104 H104b . . . 111 ? H104a C104 H104b . . . 110 ? O101 C105 C104 . . . 110.9(14) ? O101 C105 H105a . . . 109.5 ? O101 C105 H105b . . . 108.5 ? C104 C105 H105a . . . 110 ? C104 C105 H105b . . . 108.1 ? H105a C105 H105b . . . 109.9 ? Sm O201 C202 . . . 125.2(8) ? Sm O201 C205 . . . 126.6(7) ? C202 O201 C205 . . . 106.9(9) ? O201 C202 C203 . . . 106.6(11) ? O201 C202 H202a . . . 110.9 ? O201 C202 H202b . . . 110.5 ? C203 C202 H202a . . . 112.4 ? C203 C202 H202b . . . 111.2 ? H202a C202 H202b . . . 105.3 ? C202 C203 C204 . . . 104.9(12) ? C202 C203 H203a . . . 110.0 ? C202 C203 H203b . . . 111.8 ? C204 C203 H203a . . . 112.6 ? C204 C203 H203b . . . 110.9 ? H203a C203 H203b . . . 106.7 ? C203 C204 C205 . . . 105.6(16) ? C203 C204 H204a . . . 106.9 ? C203 C204 H204b . . . 110.5 ? C205 C204 H204a . . . 108.3 ? C205 C204 H204b . . . 114 ? H204a C204 H204b . . . 111 ? O201 C205 C204 . . . 106.3(12) ? O201 C205 H205a . . . 113.1 ? O201 C205 H205b . . . 112.7 ? C204 C205 H205a . . . 111.8 ? C204 C205 H205b . . . 109.8 ? H205a C205 H205b . . . 103.3 ? Sm O301 C302 . . . 122.9(7) ? Sm O301 C305 . . . 128.4(8) ? C302 O301 C305 . . . 108.7(10) ? O301 C302 C303 . . . 104.7(12) ? O301 C302 H302a . . . 110.3 ? O301 C302 H302b . . . 108.8 ? C303 C302 H302a . . . 114.8 ? C303 C302 H302b . . . 112.2 ? H302a C302 H302b . . . 106.0 ? C302 C303 C304 . . . 110.7(15) ? C302 C303 H303a . . . 110.3 ? C302 C303 H303b . . . 112.0 ? C304 C303 H303a . . . 109.3 ? C304 C303 H303b . . . 110.5 ? H303a C303 H303b . . . 103.8 ? C303 C304 C305 . . . 103.9(13) ? C303 C304 H304a . . . 112.7 ? C303 C304 H304b . . . 111.0 ? C305 C304 H304a . . . 113.0 ? C305 C304 H304b . . . 110.6 ? H304a C304 H304b . . . 105.6 ? O301 C305 C304 . . . 107.7(12) ? O301 C305 H305a . . . 109.4 ? O301 C305 H305b . . . 111.8 ? C304 C305 H305a . . . 110.1 ? C304 C305 H305b . . . 112.5 ? H305a C305 H305b . . . 105.3 ? C402 O401 C405 . . . 102(2) ? O401 C402 C403 . . . 108(2) ? O401 C402 H402a . . . 113 ? O401 C402 H402b . . . 110 ? C403 C402 H402a . . . 112 ? C403 C402 H402b . . . 104 ? H402a C402 H402b . . . 110 ? C402 C403 C404 . . . 106(3) ? C402 C403 H403a . . . 105 ? C402 C403 H403b . . . 119 ? C404 C403 H403a . . . 103 ? C404 C403 H403b . . . 116 ? H403a C403 H403b . . . 106 ? C403 C404 C405 . . . 105(2) ? C403 C404 H404a . . . 114 ? C403 C404 H404b . . . 103 ? C405 C404 H404a . . . 117 ? C405 C404 H404b . . . 108 ? H404a C404 H404b . . . 110 ? O401 C405 C404 . . . 110(3) ? O401 C405 H405a . . . 110 ? O401 C405 H405b . . . 115 ? C404 C405 H405a . . . 102 ? C404 C405 H405b . . . 110 ? H405a C405 H405b . . . 109 ? _exptl_crystal_F_000 1920 _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -23 _reflns_limit_l_max 23 _reflns_number_observed ? _reflns_d_resolution_high .84 _reflns_d_resolution_low 12.847 _diffrn_reflns_av_sigmaI/netI .156 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 300 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .135 _refine_ls_wR_factor_all .107 _refine_ls_goodness_of_fit_all 1.225 _refine_ls_shift/su_mean .003 #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_sch372 _database_code_depnum_ccdc_archive 'CCDC 281268' _audit_creation_method Xtal3.6 _audit_creation_date 05-09-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C49 H79 O8 Sm1' _chemical_formula_moiety 'C49 H79 O8 Sm1' _chemical_formula_weight 946.52 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 17.111(5) _cell_length_b 18.392(3) _cell_length_c 17.722(8) _cell_angle_alpha 90.00000 _cell_angle_beta 116.88(3) _cell_angle_gamma 90.00000 _cell_volume 4975(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 16 _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 14.1 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.228 _exptl_crystal_description fragment _exptl_crystal_size_max .42 _exptl_crystal_size_mid .37 _exptl_crystal_size_min .3 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; Xray absorb ; _exptl_absorpt_correction_T_min .7 _exptl_absorpt_correction_T_max .82 _diffrn_reflns_number 12523 _reflns_number_total 8740 _reflns_Friedel_coverage 0 _reflns_number_gt 4483 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .056 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 6 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .056 _refine_ls_wR_factor_ref .069 _refine_ls_goodness_of_fit_ref 1.241 _refine_ls_number_reflns 4483 _refine_ls_number_parameters 473 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .006 _refine_diff_density_min -.978 _refine_diff_density_max 1.163 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 196 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 316 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Sm ? 0 4 -.53302 3.442 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sm .74909(3) .63984(3) .27961(3) .0358(2) Uani ? ? 1.00000 ? ? O11 .8156(4) .5337(4) .3106(4) .045(4) Uani ? ? 1.00000 ? ? C11 .8402(6) .4708(5) .2884(6) .041(5) Uani ? ? 1.00000 ? ? C12 .9166(6) .4668(5) .2768(6) .040(5) Uani ? ? 1.00000 ? ? C121 .9889(7) .5263(6) .3113(8) .061(7) Uani ? ? 1.00000 ? ? C122 .9570(7) .5966(7) .2610(8) .062(7) Uani ? ? 1.00000 ? ? C123 1.0169(7) .5383(6) .4050(8) .063(6) Uani ? ? 1.00000 ? ? C124 1.0716(8) .5035(7) .3041(10) .092(9) Uani ? ? 1.00000 ? ? C13 .9294(7) .4078(6) .2361(7) .053(6) Uani ? ? 1.00000 ? ? C14 .8723(7) .3492(6) .2105(7) .053(6) Uani ? ? 1.00000 ? ? O14 .8903(6) .2946(5) .1670(6) .088(6) Uani ? ? 1.00000 ? ? C141 .8354(9) .2362(7) .1397(9) .084(8) Uani ? ? 1.00000 ? ? C15 .8033(7) .3480(5) .2320(7) .050(6) Uani ? ? 1.00000 ? ? C16 .7881(6) .4067(5) .2738(6) .042(5) Uani ? ? 1.00000 ? ? C161 .7194(7) .3972(6) .3050(7) .049(6) Uani ? ? 1.00000 ? ? C162 .7616(8) .4137(7) .3998(8) .067(7) Uani ? ? 1.00000 ? ? C163 .6394(7) .4459(7) .2560(8) .068(7) Uani ? ? 1.00000 ? ? C164 .6845(8) .3190(7) .2948(10) .087(9) Uani ? ? 1.00000 ? ? O21 .7873(4) .7361(3) .3599(4) .041(3) Uani ? ? 1.00000 ? ? C21 .8133(6) .7987(5) .4057(6) .040(5) Uani ? ? 1.00000 ? ? C22 .7549(6) .8592(6) .3826(6) .042(5) Uani ? ? 1.00000 ? ? C221 .6613(7) .8593(6) .3099(7) .053(5) Uani ? ? 1.00000 ? ? C222 .6646(8) .8494(7) .2267(8) .071(7) Uani ? ? 1.00000 ? ? C223 .6081(7) .7996(6) .3237(7) .061(7) Uani ? ? 1.00000 ? ? C224 .6122(8) .9309(7) .3034(9) .079(8) Uani ? ? 1.00000 ? ? C23 .7864(8) .9250(6) .4270(7) .054(6) Uani ? ? 1.00000 ? ? C24 .8693(8) .9297(6) .4943(8) .057(7) Uani ? ? 1.00000 ? ? O24 .9031(7) .9922(5) .5431(6) .096(6) Uani ? ? 1.00000 ? ? C241 .8824(15) 1.0571(9) .5108(12) .141(14) Uani ? ? 1.00000 ? ? C25 .9217(7) .8702(6) .5194(7) .050(6) Uani ? ? 1.00000 ? ? C26 .8958(7) .8039(5) .4774(6) .040(5) Uani ? ? 1.00000 ? ? C261 .9627(7) .7415(6) .5091(6) .049(6) Uani ? ? 1.00000 ? ? C262 .9241(8) .6713(6) .5235(8) .070(7) Uani ? ? 1.00000 ? ? C263 .9969(8) .7269(7) .4447(8) .068(7) Uani ? ? 1.00000 ? ? C264 1.0430(9) .7578(8) .5938(8) .093(8) Uani ? ? 1.00000 ? ? O31 .6156(4) .6287(3) .2554(4) .045(3) Uani ? ? 1.00000 ? ? C31 .5330(8) .6276(12) .2504(11) .063(3) Uiso ? ? .50000 ? ? C32 .5190(8) .6152(11) .3212(9) .063(3) Uiso ? ? .50000 ? ? C33 .4334(9) .6125(11) .3123(8) .063(3) Uiso ? ? .50000 ? ? C34 .3620(7) .6223(8) .2325(8) .063(3) Uiso ? ? .50000 ? ? O34 .2814(8) .6197(14) .2241(12) .063(3) Uiso ? ? .50000 ? ? C35 .3761(9) .6346(11) .1617(8) .063(3) Uiso ? ? .50000 ? ? C36 .4616(10) .6373(14) .1707(9) .063(3) Uiso ? ? .50000 ? ? H33 .4235(12) .6038(17) .3601(9) .10600 Uiso ? ? .50000 ? ? H35 .3278(10) .6410(15) .1074(8) .09300 Uiso ? ? .50000 ? ? C321 .5971(7) .5983(6) .4131(6) .070(8) Uani ? ? 1.00000 ? ? C322 .6972(8) .6009(7) .4298(7) .069(7) Uani ? ? 1.00000 ? ? C323 .6015(11) .6520(9) .4833(9) .100(10) Uani ? ? 1.00000 ? ? C324 .5940(9) .5198(8) .4487(9) .088(9) Uani ? ? 1.00000 ? ? C341 .278(2) .5845(18) .3035(18) .095(10) Uiso ? ? .50000 ? ? C361 .4591(7) .6440(7) .0931(7) .065(6) Uani ? ? 1.00000 ? ? C362 .5008(8) .5785(8) .0737(8) .080(8) Uani ? ? 1.00000 ? ? C363 .5062(8) .7148(7) .0935(8) .079(8) Uani ? ? 1.00000 ? ? C364 .3649(9) .6508(10) .0182(10) .123(11) Uani ? ? 1.00000 ? ? C31' .5358(7) .6204(11) .2590(9) .048(2) Uiso ? ? .50000 ? ? C32' .5362(6) .6094(10) .3374(8) .048(2) Uiso ? ? .50000 ? ? C33' .4574(7) .6107(9) .3433(7) .048(2) Uiso ? ? .50000 ? ? C34' .3783(6) .6231(8) .2710(7) .048(2) Uiso ? ? .50000 ? ? O34' .3040(7) .6244(13) .2767(10) .048(2) Uiso ? ? .50000 ? ? C35' .3778(7) .6343(9) .1927(7) .048(2) Uiso ? ? .50000 ? ? C36' .4566(8) .6329(12) .1867(8) .048(2) Uiso ? ? .50000 ? ? H33' .4575(10) .6036(14) .3962(7) .06200 Uiso ? ? .50000 ? ? H35' .3243(8) .6433(13) .1434(7) .07400 Uiso ? ? .50000 ? ? C341' .224(2) .598(2) .234(3) .152(16) Uiso ? ? .50000 ? ? C101 .8594(8) .7886(7) .2294(8) .075(8) Uani ? ? 1.00000 ? ? O102 .7982(5) .7296(4) .1960(4) .054(4) Uani ? ? 1.00000 ? ? C103 .7872(8) .7085(7) .1131(7) .063(7) Uani ? ? 1.00000 ? ? C104 .7119(8) .6585(6) .0734(7) .060(6) Uani ? ? 1.00000 ? ? O105 .7201(5) .6033(4) .1327(4) .059(4) Uani ? ? 1.00000 ? ? C106 .7165(8) .5317(6) .0998(7) .062(7) Uani ? ? 1.00000 ? ? H122a .94010 .59005 .20214 .09200 Uiso ? ? 1.00000 ? ? H122b .90551 .61495 .26519 .09200 Uiso ? ? 1.00000 ? ? H122c .99973 .63497 .28136 .09200 Uiso ? ? 1.00000 ? ? H123a .96981 .55414 .41715 .09500 Uiso ? ? 1.00000 ? ? H123b 1.04128 .49479 .43935 .09500 Uiso ? ? 1.00000 ? ? H123c 1.06306 .57533 .43091 .09500 Uiso ? ? 1.00000 ? ? H124a 1.09536 .45775 .33633 .13000 Uiso ? ? 1.00000 ? ? H124b 1.05935 .49171 .24673 .13000 Uiso ? ? 1.00000 ? ? H124c 1.11800 .53736 .32559 .13000 Uiso ? ? 1.00000 ? ? H13 .97933 .40573 .22355 .06500 Uiso ? ? 1.00000 ? ? H141a .83401 .21258 .19077 .12600 Uiso ? ? 1.00000 ? ? H141b .77488 .25150 .10632 .12600 Uiso ? ? 1.00000 ? ? H141c .85679 .20219 .11297 .12600 Uiso ? ? 1.00000 ? ? H15 .76371 .30600 .21682 .05800 Uiso ? ? 1.00000 ? ? H162a .81035 .38157 .43135 .09200 Uiso ? ? 1.00000 ? ? H162b .78579 .46294 .41151 .09200 Uiso ? ? 1.00000 ? ? H162c .72102 .40986 .42253 .09200 Uiso ? ? 1.00000 ? ? H163a .65619 .49686 .25993 .09900 Uiso ? ? 1.00000 ? ? H163b .61203 .43409 .19625 .09900 Uiso ? ? 1.00000 ? ? H163c .59482 .44285 .27436 .09900 Uiso ? ? 1.00000 ? ? H164a .65615 .30798 .23369 .13000 Uiso ? ? 1.00000 ? ? H164b .72911 .28603 .32207 .13000 Uiso ? ? 1.00000 ? ? H164c .63981 .31417 .31255 .13000 Uiso ? ? 1.00000 ? ? H222a .69585 .89117 .21767 .10400 Uiso ? ? 1.00000 ? ? H222b .69380 .80716 .22442 .10400 Uiso ? ? 1.00000 ? ? H222c .60686 .85038 .17950 .10400 Uiso ? ? 1.00000 ? ? H223a .63175 .75207 .32781 .08700 Uiso ? ? 1.00000 ? ? H223b .60258 .80768 .37591 .08700 Uiso ? ? 1.00000 ? ? H223c .54718 .79733 .27925 .08700 Uiso ? ? 1.00000 ? ? H224a .60751 .93889 .35391 .12500 Uiso ? ? 1.00000 ? ? H224b .64205 .96995 .29324 .12500 Uiso ? ? 1.00000 ? ? H224c .55275 .93048 .25721 .12500 Uiso ? ? 1.00000 ? ? H23 .74825 .96870 .40994 .07200 Uiso ? ? 1.00000 ? ? H241a .89173 1.05936 .46232 .19500 Uiso ? ? 1.00000 ? ? H241b .82455 1.06679 .49823 .19500 Uiso ? ? 1.00000 ? ? H241c .92101 1.09083 .55234 .19500 Uiso ? ? 1.00000 ? ? H25 .97830 .87467 .56830 .06100 Uiso ? ? 1.00000 ? ? H262a .90010 .67718 .56039 .09700 Uiso ? ? 1.00000 ? ? H262b .87361 .65649 .46708 .09700 Uiso ? ? 1.00000 ? ? H262c .96185 .63025 .53841 .09700 Uiso ? ? 1.00000 ? ? H263a .95021 .71479 .38868 .10000 Uiso ? ? 1.00000 ? ? H263b 1.02587 .76938 .43612 .10000 Uiso ? ? 1.00000 ? ? H263c 1.03839 .68765 .46043 .10000 Uiso ? ? 1.00000 ? ? H264a 1.07436 .80149 .58797 .12800 Uiso ? ? 1.00000 ? ? H264b 1.02777 .76949 .63798 .12800 Uiso ? ? 1.00000 ? ? H264c 1.08716 .72059 .61466 .12800 Uiso ? ? 1.00000 ? ? H322a .73904 .59132 .48725 .09300 Uiso ? ? 1.00000 ? ? H322b .70834 .64898 .41389 .09300 Uiso ? ? 1.00000 ? ? H322c .70466 .56527 .39443 .09300 Uiso ? ? 1.00000 ? ? H323a .60413 .70021 .46650 .13600 Uiso ? ? 1.00000 ? ? H323b .55122 .64540 .49193 .13600 Uiso ? ? 1.00000 ? ? H323c .65273 .64130 .53459 .13600 Uiso ? ? 1.00000 ? ? H324a .53724 .51474 .45028 .12700 Uiso ? ? 1.00000 ? ? H324b .59534 .48387 .41135 .12700 Uiso ? ? 1.00000 ? ? H324c .63811 .50968 .50494 .12700 Uiso ? ? 1.00000 ? ? H341a .32328 .55019 .33410 .11600 Uiso ? ? .50000 ? ? H341b .22236 .56022 .29083 .11600 Uiso ? ? .50000 ? ? H341c .28354 .62126 .34668 .11600 Uiso ? ? .50000 ? ? H341'a .18675 .63883 .20429 .16400 Uiso ? ? .50000 ? ? H341'b .22472 .56633 .19016 .16400 Uiso ? ? .50000 ? ? H341'c .20527 .57510 .26745 .16400 Uiso ? ? .50000 ? ? H362a .56097 .57439 .11605 .10600 Uiso ? ? 1.00000 ? ? H362b .47056 .53621 .07105 .10600 Uiso ? ? 1.00000 ? ? H362c .50381 .58401 .01984 .10600 Uiso ? ? 1.00000 ? ? H363a .47322 .75694 .10095 .11500 Uiso ? ? 1.00000 ? ? H363b .56373 .71863 .13805 .11500 Uiso ? ? 1.00000 ? ? H363c .50696 .72336 .04053 .11500 Uiso ? ? 1.00000 ? ? H364a .33017 .61095 .01517 .15600 Uiso ? ? 1.00000 ? ? H364b .33814 .69461 .02747 .15600 Uiso ? ? 1.00000 ? ? H364c .36533 .65764 -.03554 .15600 Uiso ? ? 1.00000 ? ? H101a .91590 .77440 .23697 .09800 Uiso ? ? 1.00000 ? ? H101b .83979 .82966 .19498 .09800 Uiso ? ? 1.00000 ? ? H101c .86741 .80315 .28619 .09800 Uiso ? ? 1.00000 ? ? H103a .78119 .75028 .07877 .07700 Uiso ? ? 1.00000 ? ? H103b .83972 .68269 .11849 .07700 Uiso ? ? 1.00000 ? ? H104a .65820 .68664 .05716 .08800 Uiso ? ? 1.00000 ? ? H104b .70794 .63952 .02025 .08800 Uiso ? ? 1.00000 ? ? H106a .66036 .52453 .05028 .09800 Uiso ? ? 1.00000 ? ? H106b .76096 .52514 .08170 .09800 Uiso ? ? 1.00000 ? ? H106c .72210 .49287 .13758 .09800 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sm .0406(3) .0345(3) .0347(3) .0004(3) .0192(2) -.0014(3) O11 .047(4) .046(4) .045(4) .001(3) .025(4) -.005(3) C11 .042(6) .043(6) .035(6) .006(5) .016(5) .003(5) C12 .039(6) .035(6) .044(6) .004(5) .016(5) .015(5) C121 .050(7) .051(7) .089(10) -.003(6) .037(7) .003(7) C122 .058(7) .067(8) .070(9) -.006(6) .036(7) .009(7) C123 .051(7) .061(8) .052(8) .002(6) .003(6) .006(6) C124 .056(8) .070(9) .159(15) -.022(7) .058(9) -.018(10) C13 .047(7) .053(7) .066(8) -.001(6) .031(6) -.005(6) C14 .056(7) .045(7) .056(7) -.002(6) .024(6) -.001(6) O14 .101(7) .073(6) .113(8) -.006(5) .068(6) -.035(6) C141 .089(10) .058(9) .103(11) -.002(8) .041(9) -.030(8) C15 .048(6) .038(7) .062(7) -.006(5) .023(6) -.001(5) C16 .042(6) .038(6) .034(6) .008(5) .007(5) .005(5) C161 .041(6) .053(7) .059(8) -.001(6) .030(6) .004(6) C162 .074(8) .066(8) .074(9) .021(7) .044(7) .029(7) C163 .047(7) .075(9) .087(10) .002(6) .035(7) .009(8) C164 .071(9) .055(8) .151(14) -.002(7) .063(10) .008(9) O21 .050(4) .034(4) .037(4) -.002(3) .019(3) -.008(3) C21 .050(6) .039(6) .041(6) .006(5) .029(6) .008(5) C22 .061(6) .032(5) .042(6) .001(6) .030(5) .001(6) C221 .058(7) .036(6) .060(7) .014(6) .022(6) .006(6) C222 .075(8) .064(9) .062(8) .018(7) .020(7) .011(7) C223 .065(8) .050(7) .068(8) -.003(6) .030(7) -.003(6) C224 .067(8) .056(8) .100(11) .023(7) .026(8) .003(8) C23 .070(8) .044(7) .059(8) .013(6) .038(7) .009(6) C24 .088(9) .041(7) .056(8) -.011(7) .045(7) -.013(6) O24 .147(9) .053(6) .078(7) -.008(6) .043(6) -.020(5) C241 .25(2) .062(11) .139(17) -.038(13) .116(17) -.007(11) C25 .059(7) .051(7) .044(6) -.011(6) .028(6) -.016(6) C26 .054(7) .039(6) .034(6) .005(5) .027(5) .003(5) C261 .053(7) .050(7) .041(7) -.008(6) .019(6) -.011(5) C262 .093(9) .056(7) .079(9) .017(7) .053(8) .031(7) C263 .062(8) .066(8) .085(10) .007(6) .040(7) .007(7) C264 .078(9) .090(10) .062(9) .025(8) -.011(7) .001(8) O31 .042(4) .047(4) .048(4) -.006(3) .022(3) -.004(4) C321 .107(10) .046(7) .095(10) -.017(7) .078(9) -.018(7) C322 .084(9) .080(9) .042(7) .003(7) .029(7) .015(7) C323 .131(13) .103(12) .089(11) -.012(10) .069(10) -.028(9) C324 .097(11) .092(11) .095(11) .002(9) .060(9) .022(9) C361 .045(6) .063(8) .063(8) -.002(7) .004(6) -.016(7) C362 .083(9) .087(10) .053(8) .009(8) .015(7) -.016(8) C363 .083(9) .073(9) .069(9) .007(8) .024(8) .016(8) C364 .069(9) .150(16) .096(12) .034(10) -.010(9) -.007(12) C101 .090(9) .076(9) .065(9) -.019(8) .039(8) .004(7) O102 .063(5) .053(5) .055(5) -.009(4) .034(4) -.007(4) C103 .102(10) .064(8) .040(7) .012(7) .046(7) .014(6) C104 .092(9) .052(8) .030(6) -.001(6) .022(6) -.005(5) O105 .081(5) .055(5) .043(5) -.007(4) .029(4) -.003(4) C106 .086(9) .052(7) .049(7) .002(7) .030(7) -.007(6) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sm O11 . . 2.201(6) ? Sm O21 . . 2.179(6) ? Sm O31 . . 2.135(7) ? Sm O102 . . 2.599(9) ? Sm O105 . . 2.512(8) ? O11 C11 . . 1.348(13) ? C11 C12 . . 1.414(17) ? C11 C16 . . 1.429(14) ? C12 C121 . . 1.555(14) ? C12 C13 . . 1.374(16) ? C121 C122 . . 1.525(17) ? C121 C123 . . 1.52(2) ? C121 C124 . . 1.54(2) ? C122 H122a . . .955 ? C122 H122b . . .977 ? C122 H122c . . .961 ? C123 H123a . . .969 ? C123 H123b . . .978 ? C123 H123c . . .985 ? C124 H124a . . .995 ? C124 H124b . . .965 ? C124 H124c . . .942 ? C13 C14 . . 1.387(15) ? C13 H13 . . .977 ? C14 O14 . . 1.382(17) ? C14 C15 . . 1.39(2) ? O14 C141 . . 1.363(16) ? C141 H141a . . 1.014 ? C141 H141b . . .974 ? C141 H141c . . .951 ? C15 C16 . . 1.399(16) ? C15 H15 . . .982 ? C16 C161 . . 1.52(2) ? C161 C162 . . 1.529(17) ? C161 C163 . . 1.534(15) ? C161 C164 . . 1.537(17) ? C162 H162a . . .967 ? C162 H162b . . .978 ? C162 H162c . . .949 ? C163 H163a . . .974 ? C163 H163b . . .968 ? C163 H163c . . .958 ? C164 H164a . . .988 ? C164 H164b . . .922 ? C164 H164c . . .952 ? O21 C21 . . 1.362(11) ? C21 C22 . . 1.426(14) ? C21 C26 . . 1.412(12) ? C22 C221 . . 1.536(12) ? C22 C23 . . 1.410(15) ? C221 C222 . . 1.51(2) ? C221 C223 . . 1.517(18) ? C221 C224 . . 1.538(17) ? C222 H222a . . .989 ? C222 H222b . . .935 ? C222 H222c . . .964 ? C223 H223a . . .952 ? C223 H223b . . .983 ? C223 H223c . . .983 ? C224 H224a . . .945 ? C224 H224b . . .946 ? C224 H224c . . .975 ? C23 C24 . . 1.382(15) ? C23 H23 . . .992 ? C24 O24 . . 1.397(14) ? C24 C25 . . 1.356(16) ? O24 C241 . . 1.302(19) ? C241 H241a . . .94 ? C241 H241b . . .93 ? C241 H241c . . .961 ? C25 C26 . . 1.392(14) ? C25 H25 . . .968 ? C26 C261 . . 1.536(14) ? C261 C262 . . 1.524(18) ? C261 C263 . . 1.52(2) ? C261 C264 . . 1.539(14) ? C262 H262a . . .921 ? C262 H262b . . 1.019 ? C262 H262c . . .950 ? C263 H263a . . .978 ? C263 H263b . . .974 ? C263 H263c . . .962 ? C264 H264a . . .998 ? C264 H264b . . .954 ? C264 H264c . . .961 ? O31 C31 . . 1.374(17) ? O31 C31' . . 1.403(16) ? C31 C32 . . 1.40(3) ? C31 C36 . . 1.400(19) ? C32 C33 . . 1.40(2) ? C32 C321 . . 1.603(14) ? C33 C34 . . 1.401(15) ? C33 H33 . . .95 ? C34 O34 . . 1.32(2) ? C34 C35 . . 1.40(2) ? O34 C341 . . 1.57(4) ? C35 C36 . . 1.40(2) ? C35 H35 . . .950 ? C36 C361 . . 1.36(2) ? C321 C322 . . 1.601(18) ? C321 C323 . . 1.56(2) ? C321 C324 . . 1.59(2) ? C321 C32' . . 1.291(13) ? C322 H322a . . .959 ? C322 H322b . . .974 ? C322 H322c . . .955 ? C323 H323a . . .942 ? C323 H323b . . .95 ? C323 H323c . . .956 ? C324 H324a . . .990 ? C324 H324b . . .943 ? C324 H324c . . .958 ? C341 H341a . . .96 ? C341 H341b . . .98 ? C341 H341c . . .99 ? C361 C362 . . 1.52(2) ? C361 C363 . . 1.53(2) ? C361 C364 . . 1.562(15) ? C361 C36' . . 1.69(2) ? C362 H362a . . .964 ? C362 H362b . . .925 ? C362 H362c . . .983 ? C363 H363a . . 1.002 ? C363 H363b . . .946 ? C363 H363c . . .959 ? C364 H364a . . .930 ? C364 H364b . . .977 ? C364 H364c . . .96 ? C31' C32' . . 1.40(2) ? C31' C36' . . 1.400(15) ? C32' C33' . . 1.398(19) ? C33' C34' . . 1.400(13) ? C33' H33' . . .95 ? C34' O34' . . 1.32(2) ? C34' C35' . . 1.40(2) ? O34' C341' . . 1.32(4) ? C35' C36' . . 1.40(2) ? C35' H35' . . .952 ? C341' H341'a . . .97 ? C341' H341'b . . .97 ? C341' H341'c . . .91 ? C101 O102 . . 1.437(15) ? C101 H101a . . .951 ? C101 H101b . . .932 ? C101 H101c . . .989 ? O102 C103 . . 1.447(15) ? C103 C104 . . 1.477(17) ? C103 H103a . . .957 ? C103 H103b . . .981 ? C104 O105 . . 1.422(14) ? C104 H104a . . .977 ? C104 H104b . . .978 ? O105 C106 . . 1.431(14) ? C106 H106a . . .973 ? C106 H106b . . .958 ? C106 H106c . . .953 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O11 Sm O21 . . . 126.1(2) ? O11 Sm O31 . . . 110.6(3) ? O11 Sm O102 . . . 116.2(3) ? O11 Sm O105 . . . 81.9(3) ? O21 Sm O31 . . . 100.8(3) ? O21 Sm O102 . . . 77.1(3) ? O21 Sm O105 . . . 139.0(3) ? O31 Sm O102 . . . 122.6(2) ? O31 Sm O105 . . . 94.3(3) ? O102 Sm O105 . . . 62.7(2) ? Sm O11 C11 . . . 152.0(6) ? O11 C11 C12 . . . 121.2(9) ? O11 C11 C16 . . . 120.6(10) ? C12 C11 C16 . . . 118.2(10) ? C11 C12 C121 . . . 122.0(10) ? C11 C12 C13 . . . 119.7(9) ? C121 C12 C13 . . . 118.3(11) ? C12 C121 C122 . . . 110.9(8) ? C12 C121 C123 . . . 109.4(11) ? C12 C121 C124 . . . 112.0(10) ? C122 C121 C123 . . . 111.6(10) ? C122 C121 C124 . . . 106.4(12) ? C123 C121 C124 . . . 106.4(9) ? C121 C122 H122a . . . 112.5 ? C121 C122 H122b . . . 110.2 ? C121 C122 H122c . . . 113.1 ? H122a C122 H122b . . . 106.8 ? H122a C122 H122c . . . 107.9 ? H122b C122 H122c . . . 106.1 ? C121 C123 H123a . . . 113.8 ? C121 C123 H123b . . . 113.4 ? C121 C123 H123c . . . 113.6 ? H123a C123 H123b . . . 105.7 ? H123a C123 H123c . . . 105.1 ? H123b C123 H123c . . . 104.5 ? C121 C124 H124a . . . 109.6 ? C121 C124 H124b . . . 112.2 ? C121 C124 H124c . . . 115.2 ? H124a C124 H124b . . . 104.6 ? H124a C124 H124c . . . 106.0 ? H124b C124 H124c . . . 108.5 ? C12 C13 C14 . . . 122.0(12) ? C12 C13 H13 . . . 121.0 ? C14 C13 H13 . . . 117.0 ? C13 C14 O14 . . . 116.5(12) ? C13 C14 C15 . . . 118.7(11) ? O14 C14 C15 . . . 124.8(10) ? C14 O14 C141 . . . 118.7(12) ? O14 C141 H141a . . . 108.1 ? O14 C141 H141b . . . 111.1 ? O14 C141 H141c . . . 109.7 ? H141a C141 H141b . . . 102.6 ? H141a C141 H141c . . . 109.4 ? H141b C141 H141c . . . 115.5 ? C14 C15 C16 . . . 121.1(10) ? C14 C15 H15 . . . 120.1 ? C16 C15 H15 . . . 118.8 ? C11 C16 C15 . . . 118.8(11) ? C11 C16 C161 . . . 123.4(10) ? C15 C16 C161 . . . 117.7(10) ? C16 C161 C162 . . . 108.6(9) ? C16 C161 C163 . . . 111.4(10) ? C16 C161 C164 . . . 112.9(11) ? C162 C161 C163 . . . 111.4(11) ? C162 C161 C164 . . . 106.3(11) ? C163 C161 C164 . . . 106.3(9) ? C161 C162 H162a . . . 111.6 ? C161 C162 H162b . . . 111.1 ? C161 C162 H162c . . . 112.2 ? H162a C162 H162b . . . 105.8 ? H162a C162 H162c . . . 108.4 ? H162b C162 H162c . . . 107.5 ? C161 C163 H163a . . . 111.3 ? C161 C163 H163b . . . 110.9 ? C161 C163 H163c . . . 114.6 ? H163a C163 H163b . . . 106.0 ? H163a C163 H163c . . . 106.6 ? H163b C163 H163c . . . 107.0 ? C161 C164 H164a . . . 107.0 ? C161 C164 H164b . . . 111.6 ? C161 C164 H164c . . . 112.0 ? H164a C164 H164b . . . 108.6 ? H164a C164 H164c . . . 105.9 ? H164b C164 H164c . . . 111.4 ? Sm O21 C21 . . . 175.4(8) ? O21 C21 C22 . . . 119.4(7) ? O21 C21 C26 . . . 121.1(9) ? C22 C21 C26 . . . 119.4(9) ? C21 C22 C221 . . . 124.8(9) ? C21 C22 C23 . . . 117.9(8) ? C221 C22 C23 . . . 117.2(9) ? C22 C221 C222 . . . 109.5(10) ? C22 C221 C223 . . . 109.8(9) ? C22 C221 C224 . . . 113.1(9) ? C222 C221 C223 . . . 111.1(9) ? C222 C221 C224 . . . 106.9(10) ? C223 C221 C224 . . . 106.5(11) ? C221 C222 H222a . . . 109.0 ? C221 C222 H222b . . . 113.5 ? C221 C222 H222c . . . 111.7 ? H222a C222 H222b . . . 107.4 ? H222a C222 H222c . . . 105.2 ? H222b C222 H222c . . . 109.6 ? C221 C223 H223a . . . 114.3 ? C221 C223 H223b . . . 111.2 ? C221 C223 H223c . . . 113.4 ? H223a C223 H223b . . . 106.6 ? H223a C223 H223c . . . 106.4 ? H223b C223 H223c . . . 104.1 ? C221 C224 H224a . . . 109.9 ? C221 C224 H224b . . . 109.8 ? C221 C224 H224c . . . 112.6 ? H224a C224 H224b . . . 110.2 ? H224a C224 H224c . . . 107.1 ? H224b C224 H224c . . . 107.1 ? C22 C23 C24 . . . 121.2(10) ? C22 C23 H23 . . . 119.5 ? C24 C23 H23 . . . 119.3 ? C23 C24 O24 . . . 124.2(11) ? C23 C24 C25 . . . 120.1(10) ? O24 C24 C25 . . . 115.7(9) ? C24 O24 C241 . . . 121.8(11) ? O24 C241 H241a . . . 108.6 ? O24 C241 H241b . . . 109 ? O24 C241 H241c . . . 107.4 ? H241a C241 H241b . . . 111.9 ? H241a C241 H241c . . . 109 ? H241b C241 H241c . . . 110 ? C24 C25 C26 . . . 121.9(9) ? C24 C25 H25 . . . 118.1 ? C26 C25 H25 . . . 120.0 ? C21 C26 C25 . . . 119.1(9) ? C21 C26 C261 . . . 123.7(9) ? C25 C26 C261 . . . 117.1(8) ? C26 C261 C262 . . . 112.7(10) ? C26 C261 C263 . . . 109.5(9) ? C26 C261 C264 . . . 113.6(9) ? C262 C261 C263 . . . 108.6(10) ? C262 C261 C264 . . . 105.3(9) ? C263 C261 C264 . . . 106.8(10) ? C261 C262 H262a . . . 112.6 ? C261 C262 H262b . . . 107.4 ? C261 C262 H262c . . . 115.3 ? H262a C262 H262b . . . 106.1 ? H262a C262 H262c . . . 111.2 ? H262b C262 H262c . . . 103.2 ? C261 C263 H263a . . . 112.8 ? C261 C263 H263b . . . 111.8 ? C261 C263 H263c . . . 113.5 ? H263a C263 H263b . . . 105.3 ? H263a C263 H263c . . . 106.2 ? H263b C263 H263c . . . 106.6 ? C261 C264 H264a . . . 109.9 ? C261 C264 H264b . . . 113.0 ? C261 C264 H264c . . . 115.9 ? H264a C264 H264b . . . 105.2 ? H264a C264 H264c . . . 104.2 ? H264b C264 H264c . . . 107.8 ? Sm O31 C31 . . . 171.6(9) ? Sm O31 C31' . . . 167.4(7) ? O31 C31 C32 . . . 122.2(11) ? O31 C31 C36 . . . 117.8(17) ? C32 C31 C36 . . . 120.0(14) ? C31 C32 C33 . . . 120.0(11) ? C31 C32 C321 . . . 122.7(11) ? C33 C32 C321 . . . 117.2(13) ? C321 C32 C31' . . . 119.2(12) ? C321 C32 C33' . . . 95.7(12) ? C32 C33 C34 . . . 120.0(14) ? C32 C33 H33 . . . 120.3 ? C34 C33 H33 . . . 119.7 ? C33 C34 O34 . . . 120.0(16) ? C33 C34 C35 . . . 120.0(13) ? O34 C34 C35 . . . 120.0(13) ? C34 O34 C341 . . . 111.9(16) ? C34 C35 C36 . . . 119.9(11) ? C34 C35 H35 . . . 120.3(19) ? C36 C35 H35 . . . 120(2) ? C31 C36 C35 . . . 120.1(17) ? C31 C36 C361 . . . 130.1(17) ? C35 C36 C361 . . . 109.6(11) ? C32 C321 C322 . . . 120.9(11) ? C32 C321 C323 . . . 113.8(11) ? C32 C321 C324 . . . 114.7(10) ? C322 C321 C323 . . . 99.9(9) ? C322 C321 C324 . . . 100.2(9) ? C322 C321 C32' . . . 118.8(11) ? C323 C321 C324 . . . 104.9(11) ? C323 C321 C32' . . . 117.0(12) ? C324 C321 C32' . . . 113.6(11) ? C321 C322 H322a . . . 114.5 ? C321 C322 H322b . . . 107.9 ? C321 C322 H322c . . . 108.0 ? H322a C322 H322b . . . 108.9 ? H322a C322 H322c . . . 108.3 ? H322b C322 H322c . . . 109.3 ? C321 C323 H323a . . . 109.5 ? C321 C323 H323b . . . 109.1 ? C321 C323 H323c . . . 108.6 ? H323a C323 H323b . . . 110.5 ? H323a C323 H323c . . . 109.9 ? H323b C323 H323c . . . 109.3 ? C321 C324 H324a . . . 107.9 ? C321 C324 H324b . . . 110.2 ? C321 C324 H324c . . . 116.0 ? H324a C324 H324b . . . 106.8 ? H324a C324 H324c . . . 105.8 ? H324b C324 H324c . . . 109.6 ? O34 C341 H341a . . . 115 ? O34 C341 H341b . . . 114 ? O34 C341 H341c . . . 112 ? H341a C341 H341b . . . 106 ? H341a C341 H341c . . . 104 ? H341b C341 H341c . . . 104 ? C36 C361 C362 . . . 110.8(14) ? C36 C361 C363 . . . 107.2(13) ? C36 C361 C364 . . . 114.5(13) ? C362 C361 C363 . . . 112.1(12) ? C362 C361 C364 . . . 106.4(11) ? C362 C361 C36' . . . 110.5(11) ? C363 C361 C364 . . . 105.9(11) ? C363 C361 C36' . . . 110.2(11) ? C364 C361 C36' . . . 111.7(12) ? C361 C362 H362a . . . 109.4 ? C361 C362 H362b . . . 111.7 ? C361 C362 H362c . . . 112.0 ? H362a C362 H362b . . . 110.4 ? H362a C362 H362c . . . 105.0 ? H362b C362 H362c . . . 108.1 ? C361 C363 H363a . . . 109.5 ? C361 C363 H363b . . . 114.6 ? C361 C363 H363c . . . 112.1 ? H363a C363 H363b . . . 105.6 ? H363a C363 H363c . . . 105.0 ? H363b C363 H363c . . . 109.5 ? C361 C364 H364a . . . 111.9 ? C361 C364 H364b . . . 107.8 ? C361 C364 H364c . . . 112.6 ? H364a C364 H364b . . . 108.8 ? H364a C364 H364c . . . 109.6 ? H364b C364 H364c . . . 105.8 ? O31 C31' C32' . . . 119.5(9) ? O31 C31' C36' . . . 120.0(15) ? C31 C31' C32' . . . 141(9) ? C31 C31' C36' . . . 51(5) ? C32' C31' C36' . . . 120.0(13) ? C31' C32' C33' . . . 120.0(9) ? C321 C32' C31' . . . 133.9(12) ? C321 C32' C33' . . . 106.1(13) ? C32' C33' C34' . . . 120.0(12) ? C32' C33' H33' . . . 120.2(13) ? C34' C33' H33' . . . 119.8 ? C33' C34' O34' . . . 120.0(13) ? C33' C34' C35' . . . 120.1(11) ? O34' C34' C35' . . . 120.0(10) ? C34' O34' C341' . . . 137(3) ? C34' C35' C36' . . . 120.0(9) ? C34' C35' H35' . . . 120.4 ? C36' C35' H35' . . . 119.6 ? C31' C36' C35' . . . 120.0(14) ? C361 C36' C31' . . . 118.3(13) ? C361 C36' C35' . . . 121.7(9) ? O34' C341' H341'a . . . 107 ? O34' C341' H341'b . . . 108 ? O34' C341' H341'c . . . 112 ? H341b C341' H341'a . . . 128 ? H341b C341' H341'b . . . 109 ? H341'a C341' H341'b . . . 106 ? H341'a C341' H341'c . . . 111 ? H341'b C341' H341'c . . . 112 ? O102 C101 H101a . . . 110.8 ? O102 C101 H101b . . . 111.3 ? O102 C101 H101c . . . 111.3 ? H101a C101 H101b . . . 110.9 ? H101a C101 H101c . . . 105.4 ? H101b C101 H101c . . . 106.9 ? Sm O102 C101 . . . 127.4(7) ? Sm O102 C103 . . . 118.8(6) ? C101 O102 C103 . . . 110.9(10) ? O102 C103 C104 . . . 109.6(12) ? O102 C103 H103a . . . 110.9 ? O102 C103 H103b . . . 109.7 ? C104 C103 H103a . . . 112.2 ? C104 C103 H103b . . . 108.0 ? H103a C103 H103b . . . 106.3 ? C103 C104 O105 . . . 108.6(8) ? C103 C104 H104a . . . 108.2 ? C103 C104 H104b . . . 110.2 ? O105 C104 H104a . . . 111.2 ? O105 C104 H104b . . . 113.4 ? H104a C104 H104b . . . 105.0 ? Sm O105 C104 . . . 118.8(6) ? Sm O105 C106 . . . 128.4(7) ? C104 O105 C106 . . . 112.6(9) ? O105 C106 H106a . . . 109.6 ? O105 C106 H106b . . . 110.9 ? O105 C106 H106c . . . 115.5 ? H106a C106 H106b . . . 106.9 ? H106a C106 H106c . . . 106.1 ? H106b C106 H106c . . . 107.4 ? C341 H341b C341' . . . 63(2) ? _exptl_crystal_F_000 1996 _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min -21 _reflns_limit_l_max 18 _reflns_number_observed ? _reflns_d_resolution_high .841 _reflns_d_resolution_low 15.216 _diffrn_reflns_av_sigmaI/netI .158 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 2 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .127 _refine_ls_wR_factor_all .095 _refine_ls_goodness_of_fit_all 1.21 _refine_ls_shift/su_mean .0003 #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_244sch _database_code_depnum_ccdc_archive 'CCDC 281269' _audit_creation_method Xtal3.6 _audit_creation_date 05-01-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C47.5 H70.5 Er1 O6' _chemical_formula_moiety 'C47 H67 Er O6, 0.25( C6 H14)' _chemical_formula_weight 904.94 _chemical_melting_point ? _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P_61 _symmetry_space_group_name_Hall p_61 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,1/2+z -y,+x-y,1/3+z +y,-x+y,5/6+z -x+y,-x,2/3+z +x-y,+x,1/6+z _cell_length_a 28.49(3) _cell_length_b 28.49(3) _cell_length_c 10.210(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 120.0000 _cell_volume 7177(13) _cell_formula_units_Z 6 _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 16.4 _cell_measurement_temperature 300(2) _exptl_absorpt_coefficient_mu 1.796 _exptl_crystal_description plate _exptl_crystal_size_max .25 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .68 _exptl_absorpt_correction_T_max .87 _diffrn_reflns_number 12834 _reflns_number_total 3347 _reflns_Friedel_coverage ? _reflns_number_gt 2266 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .131 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 3 _diffrn_standards_number 8 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_ref .041 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_number_reflns 2266 _refine_ls_number_parameters 497 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .105 _refine_diff_density_min -.69 _refine_diff_density_max .742 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 285 .002014 .002014 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' O ? 0 36 .007996 .005981 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 423 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Er ? 0 6 -.723022 4.958 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Er .27161(3) .41507(3) .00000 .0565(3) Uani ? ? 1.00000 ? ? O11 .3421(3) .4539(3) .1270(8) .051(5) Uani ? ? 1.00000 ? ? C11 .3841(5) .4789(5) .2098(15) .063(9) Uani ? ? 1.00000 ? ? C12 .4267(5) .5326(5) .1822(16) .063(8) Uani ? ? 1.00000 ? ? C121 .4280(5) .5634(5) .0580(15) .064(9) Uani ? ? 1.00000 ? ? C122 .4282(7) .5332(7) -.0626(14) .080(10) Uani ? ? 1.00000 ? ? C123 .3794(6) .5738(5) .0536(14) .065(9) Uani ? ? 1.00000 ? ? C124 .4783(7) .6202(6) .0585(16) .087(11) Uani ? ? 1.00000 ? ? C13 .4668(5) .5585(5) .2777(14) .061(9) Uani ? ? 1.00000 ? ? C14 .4682(5) .5335(6) .3935(14) .064(9) Uani ? ? 1.00000 ? ? O14 .5095(4) .5647(5) .4739(11) .095(7) Uani ? ? 1.00000 ? ? C141 .5040(7) .5476(8) .6049(15) .101(12) Uani ? ? 1.00000 ? ? C15 .4284(6) .4804(6) .4125(14) .068(9) Uani ? ? 1.00000 ? ? C16 .3859(5) .4525(5) .3253(14) .044(7) Uani ? ? 1.00000 ? ? C161 .3435(6) .3933(6) .3565(16) .079(10) Uani ? ? 1.00000 ? ? C162 .2872(6) .3873(8) .3721(16) .099(11) Uani ? ? 1.00000 ? ? C163 .3444(7) .3557(6) .2566(15) .079(10) Uani ? ? 1.00000 ? ? C164 .3544(8) .3751(6) .4882(18) .108(12) Uani ? ? 1.00000 ? ? O21 .1943(4) .3464(4) -.0224(9) .064(6) Uani ? ? 1.00000 ? ? C21 .1449(6) .3038(6) -.0473(15) .075(10) Uani ? ? 1.00000 ? ? C22 .1190(6) .2616(6) .0455(17) .076(10) Uani ? ? 1.00000 ? ? C221 .1404(7) .2625(7) .1883(17) .088(11) Uani ? ? 1.00000 ? ? C222 .1954(7) .2633(8) .170(2) .117(13) Uani ? ? 1.00000 ? ? C223 .1025(10) .2136(10) .269(2) .20(2) Uani ? ? 1.00000 ? ? C224 .1478(7) .3129(8) .2564(17) .114(13) Uani ? ? 1.00000 ? ? C23 .0674(6) .2174(6) .012(2) .098(11) Uani ? ? 1.00000 ? ? C24 .0446(6) .2135(8) -.1074(18) .100(11) Uani ? ? 1.00000 ? ? O24 -.0061(5) .1719(5) -.1469(17) .165(10) Uani ? ? 1.00000 ? ? C241 -.0376(11) .1342(10) -.083(3) .27(3) Uani ? ? 1.00000 ? ? C25 .0717(6) .2558(7) -.2010(16) .093(12) Uani ? ? 1.00000 ? ? C26 .1218(5) .3013(6) -.178(2) .083(10) Uani ? ? 1.00000 ? ? C261 .1475(6) .3443(7) -.2794(14) .078(10) Uani ? ? 1.00000 ? ? C262 .2001(6) .3508(7) -.3315(17) .088(10) Uani ? ? 1.00000 ? ? C263 .1111(7) .3306(10) -.4023(17) .135(15) Uani ? ? 1.00000 ? ? C264 .1523(7) .3963(7) -.2247(16) .096(12) Uani ? ? 1.00000 ? ? C01 .2916(6) .4745(6) -.172(2) .086(10) Uani ? ? 1.00000 ? ? C02 .3049(6) .5077(6) -.2540(14) .068(9) Uani ? ? 1.00000 ? ? C021 .3210(5) .5463(6) -.3641(13) .056(8) Uani ? ? 1.00000 ? ? C022 .2966(6) .5776(6) -.3746(13) .072(10) Uani ? ? 1.00000 ? ? C023 .3125(7) .6148(6) -.4714(19) .089(11) Uani ? ? 1.00000 ? ? C024 .3528(7) .6231(8) -.5511(17) .105(13) Uani ? ? 1.00000 ? ? C025 .3762(9) .5889(9) -.5472(15) .117(15) Uani ? ? 1.00000 ? ? C026 .3602(7) .5530(8) -.4467(14) .085(11) Uani ? ? 1.00000 ? ? O101 .3080(4) .3657(4) -.0865(10) .073(6) Uani ? ? 1.00000 ? ? C102 .3649(6) .3898(6) -.1135(14) .076(10) Uani ? ? 1.00000 ? ? C103 .3718(7) .3402(7) -.134(2) .114(13) Uani ? ? 1.00000 ? ? C104 .3192(8) .2937(7) -.117(2) .129(15) Uani ? ? 1.00000 ? ? C105 .2822(7) .3124(6) -.1343(18) .100(12) Uani ? ? 1.00000 ? ? O201 .2331(3) .4552(4) .1355(10) .074(6) Uani ? ? 1.00000 ? ? C202 .2568(8) .4928(8) .2433(17) .121(13) Uani ? ? 1.00000 ? ? C203 .2186(8) .4940(12) .322(2) .189(19) Uani ? ? 1.00000 ? ? C204 .1672(9) .4645(11) .250(2) .17(2) Uani ? ? 1.00000 ? ? C205 .1814(8) .4519(8) .1141(16) .110(14) Uani ? ? 1.00000 ? ? H122a .46194 .53008 -.06510 .10000 Uiso ? ? 1.00000 ? ? H122b .39912 .49811 -.07127 .10000 Uiso ? ? 1.00000 ? ? H122c .43145 .55150 -.14831 .10000 Uiso ? ? 1.00000 ? ? H123a .34654 .54146 .05651 .13200 Uiso ? ? 1.00000 ? ? H123b .38228 .59681 .12500 .13200 Uiso ? ? 1.00000 ? ? H123c .38089 .59311 -.02650 .13200 Uiso ? ? 1.00000 ? ? H124a .47751 .64213 .12908 .12500 Uiso ? ? 1.00000 ? ? H124b .51117 .61955 .06295 .12500 Uiso ? ? 1.00000 ? ? H124c .48047 .64053 -.02235 .12500 Uiso ? ? 1.00000 ? ? H13 .49622 .59683 .25861 .07500 Uiso ? ? 1.00000 ? ? H141a .47138 .54401 .64314 .13000 Uiso ? ? 1.00000 ? ? H141b .50065 .51220 .60731 .13000 Uiso ? ? 1.00000 ? ? H141c .53235 .56901 .66725 .13000 Uiso ? ? 1.00000 ? ? H15 .43018 .46112 .48796 .07700 Uiso ? ? 1.00000 ? ? H162a .28737 .41117 .44232 .13600 Uiso ? ? 1.00000 ? ? H162b .27653 .39790 .29426 .13600 Uiso ? ? 1.00000 ? ? H162c .25963 .35139 .39516 .13600 Uiso ? ? 1.00000 ? ? H163a .33717 .36583 .16945 .12000 Uiso ? ? 1.00000 ? ? H163b .38028 .35981 .24895 .12000 Uiso ? ? 1.00000 ? ? H163c .31888 .31966 .27265 .12000 Uiso ? ? 1.00000 ? ? H164a .38776 .37688 .48773 .15000 Uiso ? ? 1.00000 ? ? H164b .35264 .39719 .55644 .15000 Uiso ? ? 1.00000 ? ? H164c .32676 .33767 .51098 .15000 Uiso ? ? 1.00000 ? ? H222a .21057 .26389 .25306 .15700 Uiso ? ? 1.00000 ? ? H222b .21991 .29465 .12162 .15700 Uiso ? ? 1.00000 ? ? H222c .18900 .23082 .12185 .15700 Uiso ? ? 1.00000 ? ? H224a .16112 .31429 .34548 .15700 Uiso ? ? 1.00000 ? ? H224b .11409 .31208 .25976 .15700 Uiso ? ? 1.00000 ? ? H224c .17333 .34407 .20924 .15700 Uiso ? ? 1.00000 ? ? H223a .11798 .21657 .35596 .22500 Uiso ? ? 1.00000 ? ? H223b .09767 .18078 .22561 .22500 Uiso ? ? 1.00000 ? ? H223c .06845 .21185 .27630 .22500 Uiso ? ? 1.00000 ? ? H23 .04624 .18814 .07276 .10500 Uiso ? ? 1.00000 ? ? H241a -.06971 .11300 -.13221 .36000 Uiso ? ? 1.00000 ? ? H241b -.04622 .14687 -.00549 .36000 Uiso ? ? 1.00000 ? ? H241c -.02204 .11260 -.05978 .36000 Uiso ? ? 1.00000 ? ? H25 .05115 .25101 -.28177 .10500 Uiso ? ? 1.00000 ? ? H262a .22592 .35678 -.26240 .14000 Uiso ? ? 1.00000 ? ? H262b .19371 .31715 -.37517 .14000 Uiso ? ? 1.00000 ? ? H262c .21858 .37893 -.39445 .14000 Uiso ? ? 1.00000 ? ? H263a .10871 .29880 -.44904 .19300 Uiso ? ? 1.00000 ? ? H263b .07629 .32457 -.39228 .19300 Uiso ? ? 1.00000 ? ? H263c .12837 .35947 -.47288 .19300 Uiso ? ? 1.00000 ? ? H264a .11743 .39333 -.20323 .12600 Uiso ? ? 1.00000 ? ? H264b .17376 .40866 -.14598 .12600 Uiso ? ? 1.00000 ? ? H264c .16925 .42767 -.28463 .12600 Uiso ? ? 1.00000 ? ? H022 .26810 .57230 -.31293 .09200 Uiso ? ? 1.00000 ? ? H023 .29453 .63555 -.48204 .11300 Uiso ? ? 1.00000 ? ? H024 .36902 .65401 -.61474 .13900 Uiso ? ? 1.00000 ? ? H025 .40216 .59165 -.61588 .12800 Uiso ? ? 1.00000 ? ? H026 .37742 .53117 -.43908 .10400 Uiso ? ? 1.00000 ? ? H102a .37560 .41355 -.19037 .09000 Uiso ? ? 1.00000 ? ? H102b .38689 .41169 -.04237 .09000 Uiso ? ? 1.00000 ? ? H103a .39625 .34003 -.07092 .11600 Uiso ? ? 1.00000 ? ? H103b .38501 .34063 -.21941 .11600 Uiso ? ? 1.00000 ? ? H104a .31303 .26515 -.17826 .13200 Uiso ? ? 1.00000 ? ? H104b .31764 .27883 -.03009 .13200 Uiso ? ? 1.00000 ? ? H105a .27192 .30866 -.22069 .09600 Uiso ? ? 1.00000 ? ? H105b .25063 .28930 -.07981 .09600 Uiso ? ? 1.00000 ? ? H202a .28062 .48548 .29353 .14000 Uiso ? ? 1.00000 ? ? H202b .27894 .52979 .20865 .14000 Uiso ? ? 1.00000 ? ? H203a .21314 .47286 .40468 .20600 Uiso ? ? 1.00000 ? ? H203b .22417 .52808 .34869 .20600 Uiso ? ? 1.00000 ? ? H204a .14194 .43296 .29245 .20500 Uiso ? ? 1.00000 ? ? H204b .15315 .48816 .23584 .20500 Uiso ? ? 1.00000 ? ? H205a .15494 .41668 .08575 .13900 Uiso ? ? 1.00000 ? ? H205b .18446 .47790 .05129 .13900 Uiso ? ? 1.00000 ? ? C1 .000(10) .058(6) .218(6) .35(5) Uiso ? ? .25000 ? ? C2 .009(2) .0109(11) .201(2) .35(5) Uiso ? ? .25000 ? ? C3 .0244(12) -.0022(7) .330(3) .35(5) Uiso ? ? .25000 ? ? C4 .0625(6) .0497(10) .399(3) .35(5) Uiso ? ? .25000 ? ? C5 .0304(12) .0732(7) .458(6) .35(5) Uiso ? ? .25000 ? ? C6 -.023(4) .0279(17) .51(2) .35(5) Uiso ? ? .25000 ? ? H1a -.02396 .04961 .28784 .60000 Uiso ? ? .25000 ? ? H1b .03707 .08625 .25557 .60000 Uiso ? ? .25000 ? ? H1c -.00559 .06614 .14386 .60000 Uiso ? ? .25000 ? ? H2a -.02442 -.02156 .17794 .52000 Uiso ? ? .25000 ? ? H2b .03661 .01508 .14567 .52000 Uiso ? ? .25000 ? ? H3a .04232 -.02346 .31545 .52000 Uiso ? ? .25000 ? ? H3b -.00802 -.02320 .38390 .52000 Uiso ? ? .25000 ? ? H4a .08857 .07538 .33571 .52000 Uiso ? ? .25000 ? ? H4b .08187 .04243 .46775 .52000 Uiso ? ? .25000 ? ? H5a .02423 .09451 .39239 .52000 Uiso ? ? .25000 ? ? H5b .05049 .09659 .53217 .52000 Uiso ? ? .25000 ? ? H6a -.04468 -.00034 .44693 .60000 Uiso ? ? .25000 ? ? H6b -.01804 .00814 .58389 .60000 Uiso ? ? .25000 ? ? H6c -.04559 .04119 .54379 .60000 Uiso ? ? .25000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Er .0499(4) .0551(5) .0669(4) .0281(4) -.0024(5) -.0017(5) O11 .049(6) .048(5) .060(7) .026(5) .001(5) .005(5) C11 .047(8) .056(9) .099(14) .036(8) -.012(10) -.016(10) C12 .056(9) .048(8) .082(11) .025(7) .025(11) -.014(11) C121 .046(9) .040(8) .087(13) .008(7) -.012(9) -.003(9) C122 .090(12) .099(13) .053(11) .048(11) .001(11) -.008(11) C123 .082(11) .045(9) .078(12) .039(8) -.007(11) .012(9) C124 .102(14) .068(11) .093(14) .043(10) -.018(12) .014(11) C13 .045(9) .068(10) .079(12) .036(8) -.008(9) -.021(10) C14 .046(8) .080(11) .074(12) .036(8) -.018(9) .004(10) O14 .083(8) .098(8) .087(9) .032(7) -.022(8) -.001(8) C141 .068(11) .114(15) .104(16) .033(11) -.042(12) .002(13) C15 .063(10) .088(12) .062(11) .044(9) .007(10) .035(10) C16 .041(7) .045(7) .056(9) .029(6) -.008(9) -.006(9) C161 .080(11) .078(11) .079(13) .039(9) -.008(12) -.006(12) C162 .048(10) .112(14) .079(13) -.004(10) .037(11) -.008(12) C163 .086(12) .070(11) .080(12) .037(9) .003(11) .020(11) C164 .136(17) .073(12) .075(12) .021(11) -.019(15) .025(13) O21 .057(6) .075(7) .055(7) .029(5) .004(6) -.015(6) C21 .050(9) .079(11) .108(16) .041(9) -.003(10) -.009(11) C22 .058(10) .059(10) .107(16) .025(8) .005(11) .019(11) C221 .095(13) .107(14) .060(12) .048(11) -.027(12) -.029(12) C222 .096(13) .113(15) .138(16) .049(12) -.029(17) .025(17) C223 .13(2) .16(2) .21(3) -.003(17) -.01(2) .08(2) C224 .063(12) .16(2) .089(14) .030(12) .014(12) -.003(15) C23 .080(12) .070(11) .129(16) .027(10) .019(14) -.020(15) C24 .067(11) .108(14) .112(16) .033(11) -.034(12) -.012(14) O24 .072(8) .123(11) .202(15) -.025(8) -.014(12) -.026(13) C241 .13(2) .14(2) .46(6) .009(19) .04(3) .01(3) C25 .074(11) .148(17) .082(14) .074(12) -.005(11) -.035(14) C26 .035(8) .103(12) .121(15) .041(9) -.036(12) -.039(14) C261 .058(10) .124(15) .044(10) .041(11) .003(9) .008(11) C262 .070(10) .122(14) .066(11) .044(11) .009(13) .002(14) C263 .081(13) .22(3) .099(15) .072(16) -.034(13) -.001(18) C264 .099(14) .097(14) .099(15) .055(12) -.002(13) -.017(13) C01 .074(11) .053(9) .118(14) .023(8) -.012(14) .015(13) C02 .064(10) .056(10) .088(12) .033(8) -.024(10) -.012(10) C021 .050(9) .079(11) .041(10) .033(8) -.001(8) .002(9) C022 .094(12) .084(12) .055(11) .057(10) .031(10) .020(10) C023 .089(12) .087(12) .097(14) .048(10) .027(13) .014(13) C024 .101(14) .106(15) .103(16) .049(13) -.006(13) .014(13) C025 .143(18) .19(2) .066(14) .116(17) .037(13) .006(15) C026 .109(13) .141(16) .048(11) .094(13) .000(11) .013(12) O101 .051(6) .061(6) .101(8) .025(5) -.005(6) -.019(7) C102 .067(11) .079(11) .079(13) .035(10) .014(10) .007(11) C103 .084(12) .101(14) .17(2) .056(11) .002(16) -.055(16) C104 .135(17) .059(11) .19(2) .045(12) -.013(18) -.038(15) C105 .098(13) .071(11) .136(18) .045(11) .026(15) -.024(14) O201 .053(6) .091(8) .086(9) .043(6) -.009(6) -.018(7) C202 .085(14) .145(18) .112(16) .041(14) -.028(13) -.064(16) C203 .075(13) .31(3) .135(19) .061(19) -.044(17) -.12(2) C204 .124(18) .26(3) .16(2) .11(2) .001(18) -.09(2) C205 .120(16) .16(2) .099(15) .105(16) -.016(14) -.035(15) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Er O11 . . 2.172(8) ? Er O21 . . 2.102(9) ? Er C01 . . 2.307(17) ? Er O101 . . 2.302(9) ? Er O201 . . 2.382(10) ? O11 C11 . . 1.342(16) ? C11 C12 . . 1.428(18) ? C11 C16 . . 1.41(2) ? C12 C121 . . 1.53(2) ? C12 C13 . . 1.40(2) ? C121 C122 . . 1.50(2) ? C121 C123 . . 1.55(2) ? C121 C124 . . 1.53(2) ? C122 H122a . . 1.009 ? C122 H122b . . .929 ? C122 H122c . . 1.000 ? C123 H123a . . .929 ? C123 H123b . . .957 ? C123 H123c . . .976 ? C124 H124a . . .960 ? C124 H124b . . .948 ? C124 H124c . . .992 ? C13 C14 . . 1.39(2) ? C13 H13 . . 1.010 ? C14 O14 . . 1.342(18) ? C14 C15 . . 1.38(2) ? O14 C141 . . 1.40(2) ? C141 H141a . . .965 ? C141 H141b . . .964 ? C141 H141c . . .969 ? C15 C16 . . 1.39(2) ? C15 H15 . . .962 ? C16 C161 . . 1.54(2) ? C161 C162 . . 1.53(2) ? C161 C163 . . 1.49(2) ? C161 C164 . . 1.53(2) ? C162 H162a . . .987 ? C162 H162b . . .953 ? C162 H162c . . .957 ? C163 H163a . . .988 ? C163 H163b . . .973 ? C163 H163c . . .929 ? C164 H164a . . .93 ? C164 H164b . . .957 ? C164 H164c . . .987 ? O21 C21 . . 1.346(17) ? C21 C22 . . 1.41(2) ? C21 C26 . . 1.47(2) ? C22 C221 . . 1.58(2) ? C22 C23 . . 1.42(2) ? C221 C222 . . 1.57(2) ? C221 C223 . . 1.51(3) ? C221 C224 . . 1.51(3) ? C222 H222a . . .95 ? C222 H222b . . .95 ? C222 H222c . . .98 ? C223 H223a . . .98 ? C223 H223b . . .98 ? C223 H223c . . .95 ? C224 H224a . . .979 ? C224 H224b . . .950 ? C224 H224c . . .950 ? C23 C24 . . 1.36(3) ? C23 H23 . . .971 ? C24 O24 . . 1.39(2) ? C24 C25 . . 1.42(3) ? O24 C241 . . 1.19(3) ? C241 H241a . . .95 ? C241 H241b . . .95 ? C241 H241c . . .95 ? C25 C26 . . 1.39(2) ? C25 H25 . . .980 ? C26 C261 . . 1.49(2) ? C261 C262 . . 1.51(2) ? C261 C263 . . 1.55(2) ? C261 C264 . . 1.53(2) ? C262 H262a . . .972 ? C262 H262b . . .990 ? C262 H262c . . .954 ? C263 H263a . . 1.00 ? C263 H263b . . .924 ? C263 H263c . . 1.02 ? C264 H264a . . .979 ? C264 H264b . . .963 ? C264 H264c . . .987 ? C01 C02 . . 1.17(2) ? C02 C021 . . 1.48(2) ? C021 C022 . . 1.38(2) ? C021 C026 . . 1.33(2) ? C022 C023 . . 1.35(2) ? C022 H022 . . .977 ? C023 C024 . . 1.33(2) ? C023 H023 . . .962 ? C024 C025 . . 1.43(3) ? C024 H024 . . 1.002 ? C025 C026 . . 1.36(2) ? C025 H025 . . .994 ? C026 H026 . . .971 ? O101 C102 . . 1.437(18) ? O101 C105 . . 1.403(18) ? C102 C103 . . 1.53(2) ? C102 H102a . . .980 ? C102 H102b . . .958 ? C103 C104 . . 1.43(2) ? C103 H103a . . .950 ? C103 H103b . . .95 ? C104 C105 . . 1.41(2) ? C104 H104a . . .969 ? C104 H104b . . .98 ? C105 H105a . . .919 ? C105 H105b . . .979 ? O201 C202 . . 1.45(2) ? O201 C205 . . 1.45(2) ? C202 C203 . . 1.37(3) ? C202 H202a . . .954 ? C202 H202b . . .98 ? C203 C204 . . 1.47(3) ? C203 H203a . . 1.00 ? C203 H203b . . .94 ? C204 C205 . . 1.54(3) ? C204 H204a . . .93 ? C204 H204b . . .95 ? C205 H205a . . .95 ? C205 H205b . . .950 ? C1 C2 . . 1.49(18) ? C1 H1a . . .93 ? C1 H1b . . 1.0 ? C1 H1c . . .83 ? C2 C3 . . 1.50(4) ? C2 H2a . . .96 ? C2 H2b . . .94 ? C3 C4 . . 1.50(3) ? C3 H3a . . .98 ? C3 H3b . . .98 ? C4 C5 . . 1.51(4) ? C4 H4a . . .98 ? C4 H4b . . .98 ? C5 C6 . . 1.50(10) ? C5 H5a . . .98 ? C5 H5b . . .98 ? C6 H6a . . .94 ? C6 H6b . . .99 ? C6 H6c . . .98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O11 Er O21 . . . 144.1(3) ? O11 Er C01 . . . 104.8(4) ? O11 Er O101 . . . 87.5(4) ? O11 Er O201 . . . 86.5(4) ? O21 Er C01 . . . 111.1(5) ? O21 Er O101 . . . 88.4(4) ? O21 Er O201 . . . 89.4(4) ? C01 Er O101 . . . 97.7(6) ? C01 Er O201 . . . 95.5(6) ? O101 Er O201 . . . 166.5(4) ? Er O11 C11 . . . 176.7(10) ? O11 C11 C12 . . . 119.9(14) ? O11 C11 C16 . . . 120.2(10) ? C12 C11 C16 . . . 119.8(12) ? C11 C12 C121 . . . 122.8(12) ? C11 C12 C13 . . . 117.4(14) ? C121 C12 C13 . . . 119.7(10) ? C12 C121 C122 . . . 110.8(14) ? C12 C121 C123 . . . 111.3(12) ? C12 C121 C124 . . . 110.1(12) ? C122 C121 C123 . . . 110.1(13) ? C122 C121 C124 . . . 109.8(12) ? C123 C121 C124 . . . 104.5(14) ? C121 C122 H122a . . . 110.3 ? C121 C122 H122b . . . 116.0 ? C121 C122 H122c . . . 116.3 ? H122a C122 H122b . . . 106 ? H122a C122 H122c . . . 100.3 ? H122b C122 H122c . . . 106.2 ? C121 C123 H123a . . . 111.4 ? C121 C123 H123b . . . 109.3 ? C121 C123 H123c . . . 109.9 ? H123a C123 H123b . . . 110.7 ? H123a C123 H123c . . . 108.9 ? H123b C123 H123c . . . 106.6 ? C121 C124 H124a . . . 112.1 ? C121 C124 H124b . . . 113.0 ? C121 C124 H124c . . . 111.4 ? H124a C124 H124b . . . 108.7 ? H124a C124 H124c . . . 105.1 ? H124b C124 H124c . . . 106.1 ? C12 C13 C14 . . . 123.3(11) ? C12 C13 H13 . . . 116.9 ? C14 C13 H13 . . . 119.8 ? C13 C14 O14 . . . 115.0(11) ? C13 C14 C15 . . . 117.5(12) ? O14 C14 C15 . . . 127.5(14) ? C14 O14 C141 . . . 116.4(10) ? O14 C141 H141a . . . 110.9 ? O14 C141 H141b . . . 108.9 ? O14 C141 H141c . . . 119.6 ? H141a C141 H141b . . . 107.0 ? H141a C141 H141c . . . 104.8 ? H141b C141 H141c . . . 105 ? C14 C15 C16 . . . 122.8(15) ? C14 C15 H15 . . . 119.3 ? C16 C15 H15 . . . 117.9 ? C11 C16 C15 . . . 119.0(10) ? C11 C16 C161 . . . 122.6(11) ? C15 C16 C161 . . . 118.4(13) ? C16 C161 C162 . . . 110.3(16) ? C16 C161 C163 . . . 111.1(13) ? C16 C161 C164 . . . 111.9(12) ? C162 C161 C163 . . . 112.6(13) ? C162 C161 C164 . . . 104.5(14) ? C163 C161 C164 . . . 106.2(17) ? C161 C162 H162a . . . 110.8 ? C161 C162 H162b . . . 111.1 ? C161 C162 H162c . . . 114 ? H162a C162 H162b . . . 106 ? H162a C162 H162c . . . 106.0 ? H162b C162 H162c . . . 108.8 ? C161 C163 H163a . . . 109.1 ? C161 C163 H163b . . . 111.3 ? C161 C163 H163c . . . 112.9 ? H163a C163 H163b . . . 104.5 ? H163a C163 H163c . . . 108.7 ? H163b C163 H163c . . . 110 ? C161 C164 H164a . . . 110.8 ? C161 C164 H164b . . . 109 ? C161 C164 H164c . . . 112.7 ? H164a C164 H164b . . . 111.0 ? H164a C164 H164c . . . 108 ? H164b C164 H164c . . . 105.2 ? Er O21 C21 . . . 175.2(10) ? O21 C21 C22 . . . 120.5(14) ? O21 C21 C26 . . . 117.1(12) ? C22 C21 C26 . . . 122.3(11) ? C21 C22 C221 . . . 124.9(11) ? C21 C22 C23 . . . 117.5(16) ? C221 C22 C23 . . . 117.3(14) ? C22 C221 C222 . . . 105.3(15) ? C22 C221 C223 . . . 113.3(13) ? C22 C221 C224 . . . 108.2(17) ? C222 C221 C223 . . . 109(2) ? C222 C221 C224 . . . 112.2(13) ? C223 C221 C224 . . . 108.9(17) ? C221 C222 H222a . . . 109 ? C221 C222 H222b . . . 109 ? C221 C222 H222c . . . 109.5 ? H222a C222 H222b . . . 109.5 ? H222a C222 H222c . . . 109 ? H222b C222 H222c . . . 109 ? C221 C223 H223a . . . 109.5 ? C221 C223 H223b . . . 109 ? C221 C223 H223c . . . 109 ? H223a C223 H223b . . . 109 ? H223a C223 H223c . . . 109 ? H223b C223 H223c . . . 109 ? C221 C224 H224a . . . 109 ? C221 C224 H224b . . . 109.5 ? C221 C224 H224c . . . 109.5 ? H224a C224 H224b . . . 109.5 ? H224a C224 H224c . . . 109.5 ? H224b C224 H224c . . . 109 ? C22 C23 C24 . . . 122.0(16) ? C22 C23 H23 . . . 122 ? C24 C23 H23 . . . 115.9 ? C23 C24 O24 . . . 125.4(15) ? C23 C24 C25 . . . 119.8(13) ? O24 C24 C25 . . . 114.7(16) ? C24 O24 C241 . . . 127(2) ? O24 C241 H241a . . . 109 ? O24 C241 H241b . . . 109 ? O24 C241 H241c . . . 109 ? H241a C241 H241b . . . 109 ? H241a C241 H241c . . . 109 ? H241b C241 H241c . . . 109 ? C24 C25 C26 . . . 122.9(16) ? C24 C25 H25 . . . 114.4 ? C26 C25 H25 . . . 122.5 ? C21 C26 C25 . . . 115.3(14) ? C21 C26 C261 . . . 124.6(11) ? C25 C26 C261 . . . 120.1(16) ? C26 C261 C262 . . . 113.3(18) ? C26 C261 C263 . . . 111.5(12) ? C26 C261 C264 . . . 108.3(14) ? C262 C261 C263 . . . 104.1(14) ? C262 C261 C264 . . . 114.0(13) ? C263 C261 C264 . . . 105.4(19) ? C261 C262 H262a . . . 112.7 ? C261 C262 H262b . . . 110.5 ? C261 C262 H262c . . . 116 ? H262a C262 H262b . . . 104 ? H262a C262 H262c . . . 106.8 ? H262b C262 H262c . . . 105.4 ? C261 C263 H263a . . . 111 ? C261 C263 H263b . . . 118.6 ? C261 C263 H263c . . . 112.3 ? H263a C263 H263b . . . 107.7 ? H263a C263 H263c . . . 100.5 ? H263b C263 H263c . . . 106 ? C261 C264 H264a . . . 113.8 ? C261 C264 H264b . . . 113 ? C261 C264 H264c . . . 114.7 ? H264a C264 H264b . . . 106.0 ? H264a C264 H264c . . . 104 ? H264b C264 H264c . . . 104.7 ? Er C01 C02 . . . 174.8(13) ? C01 C02 C021 . . . 175.6(17) ? C02 C021 C022 . . . 118.0(14) ? C02 C021 C026 . . . 121.0(18) ? C022 C021 C026 . . . 120.9(15) ? C021 C022 C023 . . . 118.9(16) ? C021 C022 H022 . . . 119.9 ? C023 C022 H022 . . . 121 ? C022 C023 C024 . . . 121(2) ? C022 C023 H023 . . . 119.6 ? C024 C023 H023 . . . 119.8 ? C023 C024 C025 . . . 121.1(17) ? C023 C024 H024 . . . 122 ? C025 C024 H024 . . . 116.6 ? C024 C025 C026 . . . 116(2) ? C024 C025 H025 . . . 120.7 ? C026 C025 H025 . . . 123 ? C021 C026 C025 . . . 122(2) ? C021 C026 H026 . . . 120.9 ? C025 C026 H026 . . . 117 ? Er O101 C102 . . . 121.8(9) ? Er O101 C105 . . . 130.0(10) ? C102 O101 C105 . . . 107.9(14) ? O101 C102 C103 . . . 102.6(11) ? O101 C102 H102a . . . 111.8 ? O101 C102 H102b . . . 112.3 ? C103 C102 H102a . . . 112.9 ? C103 C102 H102b . . . 111.1 ? H102a C102 H102b . . . 106.4 ? C102 C103 C104 . . . 106.3(18) ? C102 C103 H103a . . . 110.3 ? C102 C103 H103b . . . 110.2 ? C104 C103 H103a . . . 110.3 ? C104 C103 H103b . . . 110.3 ? H103a C103 H103b . . . 109 ? C103 C104 C105 . . . 105.7(17) ? C103 C104 H104a . . . 112 ? C103 C104 H104b . . . 108.0 ? C105 C104 H104a . . . 112.4 ? C105 C104 H104b . . . 113 ? H104a C104 H104b . . . 106 ? O101 C105 C104 . . . 106.2(14) ? O101 C105 H105a . . . 115.0 ? O101 C105 H105b . . . 109.7 ? C104 C105 H105a . . . 109 ? C104 C105 H105b . . . 106.6 ? H105a C105 H105b . . . 109.6 ? Er O201 C202 . . . 130.0(11) ? Er O201 C205 . . . 125.4(9) ? C202 O201 C205 . . . 104.2(15) ? O201 C202 C203 . . . 112.7(15) ? O201 C202 H202a . . . 111 ? O201 C202 H202b . . . 109.4 ? C203 C202 H202a . . . 110.6 ? C203 C202 H202b . . . 106 ? H202a C202 H202b . . . 106.3 ? C202 C203 C204 . . . 106(2) ? C202 C203 H203a . . . 111 ? C202 C203 H203b . . . 118 ? C204 C203 H203a . . . 105.5 ? C204 C203 H203b . . . 110 ? H203a C203 H203b . . . 106 ? C203 C204 C205 . . . 106(2) ? C203 C204 H204a . . . 113 ? C203 C204 H204b . . . 109 ? C205 C204 H204a . . . 111 ? C205 C204 H204b . . . 106 ? H204a C204 H204b . . . 111 ? O201 C205 C204 . . . 103.1(15) ? O201 C205 H205a . . . 111 ? O201 C205 H205b . . . 111.0 ? C204 C205 H205a . . . 111.0 ? C204 C205 H205b . . . 111 ? H205a C205 H205b . . . 109.5 ? C2 C1 H1a . . . 106 ? C2 C1 H1b . . . 101 ? C2 C1 H1c . . . 106 ? H1a C1 H1b . . . 105 ? H1a C1 H1c . . . 123 ? H1b C1 H1c . . . 113 ? C1 C2 C3 . . . 109(4) ? C1 C2 H2a . . . 112 ? C1 C2 H2b . . . 118 ? C3 C2 H2a . . . 104 ? C3 C2 H2b . . . 103 ? H2a C2 H2b . . . 110 ? C2 C3 H3a . . . 110 ? C2 C3 H3b . . . 110 ? C4 C3 H3a . . . 110 ? C4 C3 H3b . . . 110 ? H3a C3 H3b . . . 109 ? C3 C4 C5 . . . 109(2) ? C3 C4 H4a . . . 110 ? C3 C4 H4b . . . 110 ? C5 C4 H4a . . . 110 ? C5 C4 H4b . . . 110 ? H4a C4 H4b . . . 109.5 ? C4 C5 C6 . . . 109(4) ? C4 C5 H5a . . . 110 ? C4 C5 H5b . . . 110 ? C6 C5 H5a . . . 110 ? C6 C5 H5b . . . 110 ? H5a C5 H5b . . . 109 ? C5 C6 H6a . . . 115 ? C5 C6 H6b . . . 111 ? C5 C6 H6c . . . 112 ? H6a C6 H6b . . . 104 ? H6a C6 H6c . . . 108 ? H6b C6 H6c . . . 105 ? _exptl_crystal_F_000 2829 _reflns_limit_h_min 0 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _reflns_number_observed 3347 _reflns_d_resolution_high .843 _reflns_d_resolution_low 14.245 _diffrn_reflns_av_sigmaI/netI .097 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 300(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type atom_block _refine_ls_number_restraints 9 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .080 _refine_ls_wR_factor_all .052 _refine_ls_goodness_of_fit_all 1.076 _refine_ls_shift/su_mean .005 #===END data_gbdsch _database_code_depnum_ccdc_archive 'CCDC 282031' _audit_creation_method Xtal3.6 _audit_creation_date 05-09-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C53 H85 Nd1 O8' _chemical_formula_moiety 'C49 H77 Nd O7, C4 H8 O' _chemical_formula_weight 994.49 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 16.824(6) _cell_length_b 16.409(9) _cell_length_c 19.187(5) _cell_angle_alpha 90.00000 _cell_angle_beta 90.97(2) _cell_angle_gamma 90.00000 _cell_volume 5296(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 10.5 _cell_measurement_theta_max 17.7 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.029 _exptl_crystal_description plate _exptl_crystal_size_max .55 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; xtal absorb ; _exptl_absorpt_correction_T_min .67 _exptl_absorpt_correction_T_max .88 _diffrn_reflns_number 9299 _reflns_number_total 9299 _reflns_Friedel_coverage 0 _reflns_number_gt 4464 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 25. _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 8 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .045 _refine_ls_wR_factor_ref .045 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_number_reflns 4463 _refine_ls_number_parameters 598 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .003 _refine_diff_density_min -.627 _refine_diff_density_max .575 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal DIFDAT ABSORB SORTRF ADDREF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 212 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 340 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Nd ? 0 4 -.535 3.018 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Nd .20680(3) .38896(3) .71885(2) .0425(2) Uani ? ? 1.00000 ? ? O11 .0797(3) .3920(4) .7219(2) .050(3) Uani ? ? 1.00000 ? ? C11 .0024(5) .4151(5) .7255(5) .055(6) Uani ? ? 1.00000 ? ? C12 -.0296(6) .4466(6) .7873(5) .069(7) Uani ? ? 1.00000 ? ? C121 .0109(6) .4497(7) .8600(5) .080(8) Uani ? ? 1.00000 ? ? C122 .1017(7) .4373(7) .8626(5) .096(8) Uani ? ? 1.00000 ? ? C123 -.0237(8) .3824(8) .9031(6) .121(10) Uani ? ? 1.00000 ? ? C124 -.0056(8) .5303(8) .8967(7) .134(12) Uani ? ? 1.00000 ? ? C13 -.1084(7) .4731(7) .7849(7) .098(9) Uani ? ? 1.00000 ? ? C14 -.1542(6) .4693(7) .7253(8) .100(10) Uani ? ? 1.00000 ? ? O14 -.2299(5) .5065(6) .7262(6) .162(9) Uani ? ? 1.00000 ? ? C141 -.2875(8) .4590(8) .7244(9) .147(12) Uani ? ? 1.00000 ? ? C15 -.1243(6) .4363(6) .6658(6) .079(7) Uani ? ? 1.00000 ? ? C16 -.0467(5) .4089(5) .6637(5) .056(6) Uani ? ? 1.00000 ? ? C161 -.0146(5) .3693(6) .5968(4) .059(6) Uani ? ? 1.00000 ? ? C162 .0570(6) .4137(7) .5693(5) .088(8) Uani ? ? 1.00000 ? ? C163 -.0780(6) .3686(7) .5371(5) .103(9) Uani ? ? 1.00000 ? ? C164 .0049(6) .2810(7) .6110(5) .077(7) Uani ? ? 1.00000 ? ? O21 .2528(3) .5019(3) .7538(3) .058(4) Uani ? ? 1.00000 ? ? C21 .2950(5) .5706(5) .7673(4) .047(5) Uani ? ? 1.00000 ? ? C22 .3701(5) .5668(6) .8008(5) .060(6) Uani ? ? 1.00000 ? ? C221 .4050(6) .4869(6) .8274(5) .074(7) Uani ? ? 1.00000 ? ? C222' .4182(12) .4213(10) .7738(9) .108(14) Uani ? ? .75000 ? ? C223' .4812(11) .4941(12) .8735(11) .141(17) Uani ? ? .75000 ? ? C224' .3479(10) .4499(10) .8841(8) .125(15) Uani ? ? .75000 ? ? C222 .369(3) .409(2) .797(3) .10(2) Uiso ? ? .25000 ? ? C223 .4864(15) .484(2) .7867(18) .068(11) Uiso ? ? .25000 ? ? C224 .431(3) .497(3) .9026(13) .085(17) Uiso ? ? .25000 ? ? C23 .4118(6) .6380(6) .8125(5) .069(7) Uani ? ? 1.00000 ? ? C24 .3824(7) .7115(7) .7923(5) .080(8) Uani ? ? 1.00000 ? ? O24 .4211(6) .7848(5) .8016(5) .151(8) Uani ? ? 1.00000 ? ? C241 .4672(7) .7999(7) .8550(6) .108(10) Uani ? ? 1.00000 ? ? C25 .3089(7) .7159(6) .7610(5) .074(7) Uani ? ? 1.00000 ? ? C26 .2627(5) .6471(6) .7473(4) .053(6) Uani ? ? 1.00000 ? ? C261 .1810(5) .6609(5) .7127(5) .064(7) Uani ? ? 1.00000 ? ? C262 .1171(13) .6206(14) .7608(13) .098(18) Uani ? ? .50000 ? ? C263 .1727(17) .6226(18) .6427(10) .10(2) Uani ? ? .50000 ? ? C264 .1543(17) .7503(11) .7097(15) .11(2) Uani ? ? .50000 ? ? C262' .1273(16) .700(3) .7638(15) .15(3) Uani ? ? .50000 ? ? C263' .1425(14) .5850(12) .6803(13) .08(2) Uani ? ? .50000 ? ? C264' .1943(15) .7145(16) .6459(11) .12(2) Uani ? ? .50000 ? ? O31 .2727(3) .3601(3) .6256(2) .046(3) Uani ? ? 1.00000 ? ? C31 .3181(4) .3337(5) .5723(4) .042(5) Uani ? ? 1.00000 ? ? C32 .3313(5) .2491(5) .5638(4) .048(5) Uani ? ? 1.00000 ? ? C321 .2941(5) .1853(5) .6113(5) .062(6) Uani ? ? 1.00000 ? ? C322 .2038(6) .1933(6) .6103(5) .073(7) Uani ? ? 1.00000 ? ? C323 .3274(6) .1940(6) .6858(5) .078(7) Uani ? ? 1.00000 ? ? C324 .3115(7) .0971(6) .5894(6) .103(9) Uani ? ? 1.00000 ? ? C33 .3803(5) .2223(5) .5108(4) .054(6) Uani ? ? 1.00000 ? ? C34 .4153(5) .2772(6) .4666(5) .061(6) Uani ? ? 1.00000 ? ? O34 .4602(4) .2418(4) .4149(4) .085(5) Uani ? ? 1.00000 ? ? C341 .4939(7) .2922(7) .3651(6) .102(9) Uani ? ? 1.00000 ? ? C35 .4015(5) .3592(5) .4732(4) .052(6) Uani ? ? 1.00000 ? ? C36 .3535(4) .3891(6) .5262(4) .048(5) Uani ? ? 1.00000 ? ? C361 .3389(5) .4817(5) .5293(4) .053(6) Uani ? ? 1.00000 ? ? C362 .2494(5) .4977(5) .5180(4) .063(6) Uani ? ? 1.00000 ? ? C363 .3813(6) .5286(5) .4724(5) .072(7) Uani ? ? 1.00000 ? ? C364 .3672(5) .5156(5) .5988(5) .065(6) Uani ? ? 1.00000 ? ? O101 .1968(3) .2687(4) .7984(3) .060(4) Uani ? ? 1.00000 ? ? C102 .2446(6) .2480(7) .8593(6) .094(9) Uani ? ? 1.00000 ? ? C103 .1987(10) .1932(10) .8989(7) .184(16) Uani ? ? 1.00000 ? ? C104 .1237(7) .1767(7) .8668(6) .099(9) Uani ? ? 1.00000 ? ? C105 .1291(6) .2141(6) .7955(5) .075(7) Uani ? ? 1.00000 ? ? O201 .3376(16) .704(2) 1.0107(14) .33(3) Uani ? ? 1.00000 ? ? C202 .271(2) .715(2) .9645(16) .22(3) Uani ? ? 1.00000 ? ? C203 .2266(14) .647(3) .9793(18) .23(3) Uani ? ? 1.00000 ? ? C204 .254(2) .6081(14) 1.037(2) .21(2) Uani ? ? 1.00000 ? ? C205 .328(2) .636(3) 1.0481(19) .26(3) Uani ? ? 1.00000 ? ? H122a .11513 .38637 .83979 .13400 Uiso ? ? 1.00000 ? ? H122b .12547 .48009 .83448 .13400 Uiso ? ? 1.00000 ? ? H122c .11862 .43629 .91006 .13400 Uiso ? ? 1.00000 ? ? H123a -.08117 .38767 .90925 .17500 Uiso ? ? 1.00000 ? ? H123b -.01833 .32673 .88217 .17500 Uiso ? ? 1.00000 ? ? H123c .00006 .37824 .94886 .17500 Uiso ? ? 1.00000 ? ? H124a .01310 .57557 .87085 .18000 Uiso ? ? 1.00000 ? ? H124b -.06155 .53704 .90393 .18000 Uiso ? ? 1.00000 ? ? H124c .02018 .53225 .94275 .18000 Uiso ? ? 1.00000 ? ? H13 -.13221 .49601 .82686 .12700 Uiso ? ? 1.00000 ? ? H141a -.28614 .42811 .68251 .24000 Uiso ? ? 1.00000 ? ? H141b -.28472 .42146 .76518 .24000 Uiso ? ? 1.00000 ? ? H141c -.33474 .49011 .72461 .24000 Uiso ? ? 1.00000 ? ? H15 -.15779 .43364 .62280 .09900 Uiso ? ? 1.00000 ? ? H162a .07437 .38710 .52827 .11700 Uiso ? ? 1.00000 ? ? H162b .09812 .41287 .60357 .11700 Uiso ? ? 1.00000 ? ? H162c .04264 .46816 .55875 .11700 Uiso ? ? 1.00000 ? ? H163a -.05607 .34408 .49696 .13700 Uiso ? ? 1.00000 ? ? H163b -.09308 .42314 .52663 .13700 Uiso ? ? 1.00000 ? ? H163c -.12292 .33871 .55148 .13700 Uiso ? ? 1.00000 ? ? H164a .02460 .25698 .56980 .10800 Uiso ? ? 1.00000 ? ? H164b -.04181 .25371 .62484 .10800 Uiso ? ? 1.00000 ? ? H164c .04402 .27815 .64702 .10800 Uiso ? ? 1.00000 ? ? H222a .40017 .36283 .81355 .13800 Uiso ? ? .25000 ? ? H222b .36889 .40997 .74858 .13800 Uiso ? ? .25000 ? ? H222c .31625 .40200 .81384 .13800 Uiso ? ? .25000 ? ? H223a .51732 .43872 .80563 .09300 Uiso ? ? .25000 ? ? H223b .51482 .53244 .79519 .09300 Uiso ? ? .25000 ? ? H223c .47662 .47533 .73958 .09300 Uiso ? ? .25000 ? ? H224a .45665 .45444 .92047 .08300 Uiso ? ? .25000 ? ? H224b .39329 .52228 .92883 .08300 Uiso ? ? .25000 ? ? H224c .47624 .54350 .89973 .08300 Uiso ? ? .25000 ? ? H222'a .47008 .39934 .77966 .28900 Uiso ? ? .75000 ? ? H222'b .41319 .44444 .72820 .28900 Uiso ? ? .75000 ? ? H222'c .37991 .37950 .77871 .28900 Uiso ? ? .75000 ? ? H223'a .49586 .43859 .88744 .29100 Uiso ? ? .75000 ? ? H223'b .46958 .52365 .91380 .29100 Uiso ? ? .75000 ? ? H223'c .52172 .51660 .84816 .29100 Uiso ? ? .75000 ? ? H224'a .36761 .39806 .89875 .29000 Uiso ? ? .75000 ? ? H224'b .29598 .44250 .86378 .29000 Uiso ? ? .75000 ? ? H224'c .34482 .48521 .92256 .29000 Uiso ? ? .75000 ? ? H23 .46498 .63599 .83599 .08800 Uiso ? ? 1.00000 ? ? H241a .43903 .79150 .89694 .16000 Uiso ? ? 1.00000 ? ? H241b .51260 .76801 .85340 .16000 Uiso ? ? 1.00000 ? ? H241c .48158 .85704 .85260 .16000 Uiso ? ? 1.00000 ? ? H25 .28700 .77064 .74753 .09200 Uiso ? ? 1.00000 ? ? H262a .12042 .56409 .76943 .13000 Uiso ? ? .50000 ? ? H262b .11342 .64691 .80783 .13000 Uiso ? ? .50000 ? ? H262c .06066 .62948 .74221 .13000 Uiso ? ? .50000 ? ? H263a .21134 .64232 .61570 .13500 Uiso ? ? .50000 ? ? H263b .17935 .56458 .65168 .13500 Uiso ? ? .50000 ? ? H263c .12110 .63016 .62416 .13500 Uiso ? ? .50000 ? ? H264a .15457 .77507 .75422 .15000 Uiso ? ? .50000 ? ? H264b .19435 .78231 .68214 .15000 Uiso ? ? .50000 ? ? H264c .10496 .76258 .68673 .15000 Uiso ? ? .50000 ? ? H262'a .12282 .67481 .80239 .20000 Uiso ? ? .50000 ? ? H262'b .15226 .75678 .77190 .20000 Uiso ? ? .50000 ? ? H262'c .07799 .71407 .73936 .20000 Uiso ? ? .50000 ? ? H263'a .17569 .56389 .64180 .09200 Uiso ? ? .50000 ? ? H263'b .13483 .54320 .71149 .09200 Uiso ? ? .50000 ? ? H263'c .09007 .59180 .65480 .09200 Uiso ? ? .50000 ? ? H264'a .21822 .76627 .65198 .16500 Uiso ? ? .50000 ? ? H264'b .22880 .68702 .60904 .16500 Uiso ? ? .50000 ? ? H264'c .14425 .72378 .61822 .16500 Uiso ? ? .50000 ? ? H322a .18605 .24751 .62444 .10400 Uiso ? ? 1.00000 ? ? H322b .18130 .18519 .56371 .10400 Uiso ? ? 1.00000 ? ? H322c .17753 .15515 .64035 .10400 Uiso ? ? 1.00000 ? ? H323a .38454 .18742 .68921 .10600 Uiso ? ? 1.00000 ? ? H323b .31648 .24786 .70566 .10600 Uiso ? ? 1.00000 ? ? H323c .30580 .15565 .71975 .10600 Uiso ? ? 1.00000 ? ? H324a .29092 .08772 .54318 .14100 Uiso ? ? 1.00000 ? ? H324b .36835 .08754 .58824 .14100 Uiso ? ? 1.00000 ? ? H324c .28970 .05636 .61916 .14100 Uiso ? ? 1.00000 ? ? H33 .38979 .16229 .50545 .06900 Uiso ? ? 1.00000 ? ? H341a .45115 .32224 .33977 .15200 Uiso ? ? 1.00000 ? ? H341b .52862 .32967 .38834 .15200 Uiso ? ? 1.00000 ? ? H341c .52335 .25983 .33396 .15200 Uiso ? ? 1.00000 ? ? H35 .42577 .39753 .43999 .06600 Uiso ? ? 1.00000 ? ? H362a .23047 .47912 .47365 .09000 Uiso ? ? 1.00000 ? ? H362b .21780 .47260 .55336 .09000 Uiso ? ? 1.00000 ? ? H362c .23808 .55638 .52022 .09000 Uiso ? ? 1.00000 ? ? H363a .43884 .52010 .47626 .09700 Uiso ? ? 1.00000 ? ? H363b .36523 .51080 .42711 .09700 Uiso ? ? 1.00000 ? ? H363c .37460 .58738 .47339 .09700 Uiso ? ? 1.00000 ? ? H364a .34153 .49009 .63792 .09100 Uiso ? ? 1.00000 ? ? H364b .42465 .50543 .60669 .09100 Uiso ? ? 1.00000 ? ? H364c .36055 .57341 .60376 .09100 Uiso ? ? 1.00000 ? ? H102a .25787 .29628 .88763 .11400 Uiso ? ? 1.00000 ? ? H102b .29688 .22598 .84633 .11400 Uiso ? ? 1.00000 ? ? H103a .19527 .21020 .94391 .20000 Uiso ? ? 1.00000 ? ? H103b .22923 .14057 .89853 .20000 Uiso ? ? 1.00000 ? ? H104a .08150 .20171 .89433 .11400 Uiso ? ? 1.00000 ? ? H104b .11040 .11927 .86435 .11400 Uiso ? ? 1.00000 ? ? H105a .07825 .24493 .78427 .09600 Uiso ? ? 1.00000 ? ? H105b .13131 .17347 .75980 .09600 Uiso ? ? 1.00000 ? ? H202a .23878 .76461 .97456 .25000 Uiso ? ? 1.00000 ? ? H202b .28243 .71919 .91551 .25000 Uiso ? ? 1.00000 ? ? H203a .16770 .65968 .98275 .27000 Uiso ? ? 1.00000 ? ? H203b .22547 .60882 .93800 .27000 Uiso ? ? 1.00000 ? ? H204a .21391 .61799 1.07224 .24000 Uiso ? ? 1.00000 ? ? H204b .24698 .54831 1.02641 .24000 Uiso ? ? 1.00000 ? ? H205a .32558 .63830 1.10062 .30000 Uiso ? ? 1.00000 ? ? H205b .35800 .58554 1.04033 .30000 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nd .0411(2) .0431(2) .0434(2) -.0023(3) -.00001(16) -.0023(3) O11 .038(3) .061(3) .051(3) .002(3) .001(2) .002(3) C11 .049(6) .047(6) .068(6) .003(4) .002(5) .013(4) C12 .070(7) .062(7) .076(7) .007(5) .018(6) .001(5) C121 .081(8) .089(9) .071(7) -.007(7) .030(6) -.017(6) C122 .094(9) .127(10) .067(7) .013(8) -.005(6) -.028(7) C123 .143(11) .127(11) .094(8) -.026(10) .009(8) .026(9) C124 .151(13) .110(11) .140(12) .036(9) -.000(9) -.065(9) C13 .067(8) .093(9) .135(11) .008(7) .039(8) -.021(8) C14 .041(7) .100(10) .160(14) .026(7) .014(8) -.007(9) O14 .080(7) .142(9) .263(12) .039(7) .025(8) -.018(8) C141 .068(9) .123(11) .250(17) -.040(9) -.022(10) .001(13) C15 .059(7) .087(8) .091(8) .024(6) -.010(6) .012(6) C16 .037(5) .050(6) .081(6) -.003(4) -.001(5) .023(5) C161 .047(5) .071(7) .059(6) -.001(5) -.015(4) .014(5) C162 .084(7) .121(10) .060(6) -.026(7) -.004(5) .020(6) C163 .067(7) .154(12) .086(7) -.006(7) -.029(6) .013(8) C164 .068(7) .092(8) .069(7) -.004(6) -.000(5) -.008(6) O21 .057(4) .048(4) .068(4) -.012(3) -.002(3) -.004(3) C21 .043(5) .055(5) .042(6) .003(5) .003(4) -.003(4) C22 .060(6) .053(6) .066(6) -.001(5) -.001(5) -.007(5) C221 .060(7) .069(7) .091(8) .011(6) -.022(6) -.009(6) C222' .116(16) .082(12) .125(15) .050(11) -.038(13) -.024(10) C223' .15(2) .131(17) .143(16) .043(16) -.081(15) -.020(14) C224' .155(17) .104(14) .117(14) .018(13) -.009(12) .044(12) C23 .070(7) .069(8) .069(7) -.010(6) -.020(5) .001(5) C24 .095(9) .067(8) .078(8) -.043(7) -.011(6) .001(6) O24 .194(10) .091(6) .166(9) -.089(7) -.090(7) .031(6) C241 .102(10) .106(10) .116(10) -.040(8) -.022(8) -.034(8) C25 .102(9) .044(6) .075(8) -.015(6) -.003(6) .008(5) C26 .062(6) .050(6) .048(6) .003(5) .003(4) .008(5) C261 .066(7) .042(6) .084(8) .004(5) -.012(6) .015(6) C262 .094(17) .052(14) .15(2) .013(15) .022(15) .024(17) C263 .11(2) .12(3) .072(17) .02(2) -.039(16) -.021(18) C264 .13(2) .10(2) .09(2) .055(18) -.022(18) -.013(16) C262' .09(2) .23(4) .11(2) .08(3) .009(18) -.07(3) C263' .076(18) .10(2) .080(19) .015(14) -.027(15) -.013(15) C264' .14(2) .09(2) .11(2) -.041(17) -.080(18) .053(17) O31 .044(3) .048(3) .048(3) .003(3) .009(3) -.004(3) C31 .029(4) .047(5) .049(5) -.002(4) -.006(4) -.003(4) C32 .046(5) .054(6) .045(5) -.000(4) .002(4) .001(4) C321 .067(7) .043(6) .078(7) -.004(5) .018(5) -.003(5) C322 .070(7) .067(7) .083(7) -.021(6) .011(6) -.006(6) C323 .079(7) .089(8) .066(7) .013(6) .009(5) .013(6) C324 .142(11) .055(8) .113(9) -.001(7) .042(8) .013(6) C33 .051(6) .048(5) .063(6) .002(5) .006(5) -.008(5) C34 .053(6) .070(7) .059(6) -.012(5) .009(5) -.019(5) O34 .083(5) .076(5) .096(5) -.015(4) .045(4) -.027(4) C341 .104(9) .097(9) .108(9) -.030(7) .044(7) -.035(7) C35 .049(5) .058(6) .050(5) -.013(4) .001(4) .000(4) C36 .036(4) .058(5) .049(5) -.005(5) -.006(4) -.005(5) C361 .044(5) .055(6) .060(6) -.001(4) -.000(4) .009(5) C362 .048(6) .070(6) .070(6) .014(5) -.003(5) .002(5) C363 .081(7) .063(7) .072(7) .004(6) .010(6) .021(5) C364 .060(6) .059(6) .077(7) -.015(5) .006(5) -.010(5) O101 .057(4) .065(4) .057(4) .002(3) -.005(3) .010(3) C102 .078(8) .118(10) .085(8) -.003(7) -.025(6) .039(7) C103 .167(15) .235(19) .147(13) -.091(14) -.077(12) .138(13) C104 .112(10) .093(9) .091(9) -.022(8) .011(7) .039(7) C105 .085(8) .075(7) .066(7) -.011(6) -.001(6) .007(6) O201 .31(3) .38(3) .30(3) -.07(3) -.03(2) .12(2) C202 .18(2) .27(3) .21(3) .08(2) .04(2) .14(2) C203 .18(2) .30(4) .21(3) -.07(2) -.01(2) .03(2) C204 .19(2) .131(15) .30(3) .028(18) .11(2) .114(18) C205 .22(3) .27(4) .28(3) .04(3) .01(3) .12(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nd O11 . . 2.140(5) ? Nd O21 . . 2.113(6) ? Nd O31 . . 2.173(5) ? Nd O101 . . 2.502(6) ? O11 C11 . . 1.358(10) ? C11 C12 . . 1.409(13) ? C11 C16 . . 1.436(12) ? C12 C121 . . 1.543(14) ? C12 C13 . . 1.395(16) ? C121 C122 . . 1.540(16) ? C121 C123 . . 1.503(17) ? C121 C124 . . 1.526(17) ? C122 H122a . . .971 ? C122 H122b . . .975 ? C122 H122c . . .950 ? C123 H123a . . .980 ? C123 H123b . . 1.002 ? C123 H123c . . .960 ? C124 H124a . . .949 ? C124 H124b . . .961 ? C124 H124c . . .978 ? C13 C14 . . 1.37(2) ? C13 H13 . . .979 ? C14 O14 . . 1.412(14) ? C14 C15 . . 1.367(18) ? O14 C141 . . 1.244(17) ? C141 H141a . . .951 ? C141 H141b . . .996 ? C141 H141c . . .945 ? C15 C16 . . 1.383(13) ? C15 H15 . . .992 ? C16 C161 . . 1.545(12) ? C161 C162 . . 1.511(13) ? C161 C163 . . 1.552(13) ? C161 C164 . . 1.509(14) ? C162 H162a . . .950 ? C162 H162b . . .947 ? C162 H162c . . .947 ? C163 H163a . . .949 ? C163 H163b . . .951 ? C163 H163c . . .946 ? C164 H164a . . .948 ? C164 H164b . . .946 ? C164 H164c . . .948 ? O21 C21 . . 1.354(10) ? C21 C22 . . 1.410(12) ? C21 C26 . . 1.418(13) ? C22 C221 . . 1.522(14) ? C22 C23 . . 1.378(14) ? C221 C222' . . 1.51(2) ? C221 C223' . . 1.55(2) ? C221 C224' . . 1.58(2) ? C221 C222 . . 1.53(4) ? C221 C223 . . 1.59(3) ? C221 C224 . . 1.51(3) ? C222' H222'a . . .95 ? C222' H222'b . . .956 ? C222' H222'c . . .947 ? C223' H223'a . . .98 ? C223' H223'b . . .94 ? C223' H223'c . . .92 ? C224' H224'a . . .953 ? C224' H224'b . . .959 ? C224' H224'c . . .941 ? C222 H222a . . .97 ? C222 H222b . . .92 ? C222 H222c . . .96 ? C223 H223a . . .97 ? C223 H223b . . .94 ? C223 H223c . . .93 ? C224 H224a . . .88 ? C224 H224b . . .92 ? C224 H224c . . 1.08 ? C23 C24 . . 1.359(15) ? C23 H23 . . .994 ? C24 O24 . . 1.378(14) ? C24 C25 . . 1.368(16) ? O24 C241 . . 1.297(15) ? C241 H241a . . .951 ? C241 H241b . . .927 ? C241 H241c . . .970 ? C25 C26 . . 1.392(13) ? C25 H25 . . 1.003 ? C26 C261 . . 1.534(12) ? C261 C262 . . 1.57(3) ? C261 C263 . . 1.49(2) ? C261 C264 . . 1.54(2) ? C261 C262' . . 1.49(3) ? C261 C263' . . 1.53(2) ? C261 C264' . . 1.57(3) ? C262 H262a . . .94 ? C262 H262b . . 1.00 ? C262 H262c . . 1.02 ? C263 H263a . . .90 ? C263 H263b . . .97 ? C263 H263c . . .94 ? C264 H264a . . .95 ? C264 H264b . . 1.01 ? C264 H264c . . .95 ? C262' H262'a . . .85 ? C262' H262'b . . 1.04 ? C262' H262'c . . .97 ? C263' H263'a . . 1.00 ? C263' H263'b . . .92 ? C263' H263'c . . 1.01 ? C264' H264'a . . .95 ? C264' H264'b . . 1.03 ? C264' H264'c . . 1.00 ? O31 C31 . . 1.357(9) ? C31 C32 . . 1.417(12) ? C31 C36 . . 1.408(11) ? C32 C321 . . 1.529(12) ? C32 C33 . . 1.391(12) ? C321 C322 . . 1.524(13) ? C321 C323 . . 1.532(13) ? C321 C324 . . 1.537(13) ? C322 H322a . . .979 ? C322 H322b . . .974 ? C322 H322c . . .964 ? C323 H323a . . .968 ? C323 H323b . . .982 ? C323 H323c . . .980 ? C324 H324a . . .959 ? C324 H324b . . .970 ? C324 H324c . . .956 ? C33 C34 . . 1.376(13) ? C33 H33 . . 1.003 ? C34 O34 . . 1.385(11) ? C34 C35 . . 1.372(13) ? O34 C341 . . 1.391(13) ? C341 H341a . . .992 ? C341 H341b . . .954 ? C341 H341c . . .945 ? C35 C36 . . 1.397(11) ? C35 H35 . . .989 ? C36 C361 . . 1.541(13) ? C361 C362 . . 1.540(11) ? C361 C363 . . 1.522(12) ? C361 C364 . . 1.514(12) ? C362 H362a . . .954 ? C362 H362b . . .962 ? C362 H362c . . .982 ? C363 H363a . . .980 ? C363 H363b . . .952 ? C363 H363c . . .971 ? C364 H364a . . .968 ? C364 H364b . . .991 ? C364 H364c . . .959 ? O101 C102 . . 1.449(12) ? O101 C105 . . 1.449(12) ? C102 C103 . . 1.42(2) ? C102 H102a . . .984 ? C102 H102b . . .986 ? C103 C104 . . 1.42(2) ? C103 H103a . . .910 ? C103 H103b . . 1.005 ? C104 C105 . . 1.504(15) ? C104 H104a . . .983 ? C104 H104b . . .969 ? C105 H105a . . 1.013 ? C105 H105b . . .957 ? O201 C202 . . 1.44(4) ? O201 C205 . . 1.34(5) ? C202 C203 . . 1.37(6) ? C202 H202a . . .99 ? C202 H202b . . .97 ? C203 C204 . . 1.35(5) ? C203 H203a . . 1.02 ? C203 H203b . . 1.01 ? C204 C205 . . 1.33(5) ? C204 H204a . . .97 ? C204 H204b . . 1.01 ? C205 H205a . . 1.01 ? C205 H205b . . .98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O11 Nd O21 . . . 109.4(2) ? O11 Nd O31 . . . 123.47(18) ? O11 Nd O101 . . . 85.6(2) ? O21 Nd O31 . . . 105.2(2) ? O21 Nd O101 . . . 121.7(2) ? O31 Nd O101 . . . 111.80(18) ? Nd O11 C11 . . . 165.0(5) ? O11 C11 C12 . . . 121.7(8) ? O11 C11 C16 . . . 118.5(7) ? C12 C11 C16 . . . 119.8(8) ? C11 C12 C121 . . . 127.1(9) ? C11 C12 C13 . . . 117.6(9) ? C121 C12 C13 . . . 115.1(9) ? C12 C121 C122 . . . 116.6(8) ? C12 C121 C123 . . . 107.7(9) ? C12 C121 C124 . . . 111.4(9) ? C122 C121 C123 . . . 106.1(9) ? C122 C121 C124 . . . 106.7(9) ? C123 C121 C124 . . . 107.9(9) ? C121 C122 H122a . . . 109.8 ? C121 C122 H122b . . . 107.6 ? C121 C122 H122c . . . 108.3 ? H122a C122 H122b . . . 105.7 ? H122a C122 H122c . . . 110.4 ? H122b C122 H122c . . . 115.0 ? C121 C123 H123a . . . 113.1 ? C121 C123 H123b . . . 114.2 ? C121 C123 H123c . . . 113.3 ? H123a C123 H123b . . . 102.9 ? H123a C123 H123c . . . 107.0 ? H123b C123 H123c . . . 105.3 ? C121 C124 H124a . . . 111.9 ? C121 C124 H124b . . . 110.6 ? C121 C124 H124c . . . 111.3 ? H124a C124 H124b . . . 108.6 ? H124a C124 H124c . . . 107.6 ? H124b C124 H124c . . . 106.6 ? C12 C13 C14 . . . 122.2(12) ? C12 C13 H13 . . . 119.6 ? C14 C13 H13 . . . 118.2 ? C13 C14 O14 . . . 117.7(12) ? C13 C14 C15 . . . 120.4(10) ? O14 C14 C15 . . . 121.7(12) ? C14 O14 C141 . . . 115.5(11) ? O14 C141 H141a . . . 109.1 ? O14 C141 H141b . . . 109.9 ? O14 C141 H141c . . . 108.4 ? H141a C141 H141b . . . 109.5 ? H141a C141 H141c . . . 108.9 ? H141b C141 H141c . . . 111.0 ? C14 C15 C16 . . . 121.0(10) ? C14 C15 H15 . . . 120.0 ? C16 C15 H15 . . . 119.0 ? C11 C16 C15 . . . 118.9(8) ? C11 C16 C161 . . . 120.8(7) ? C15 C16 C161 . . . 120.3(8) ? C16 C161 C162 . . . 112.3(7) ? C16 C161 C163 . . . 111.8(7) ? C16 C161 C164 . . . 109.4(7) ? C162 C161 C163 . . . 106.7(7) ? C162 C161 C164 . . . 110.7(8) ? C163 C161 C164 . . . 105.7(8) ? C161 C162 H162a . . . 109.0 ? C161 C162 H162b . . . 109.1 ? C161 C162 H162c . . . 109.1 ? H162a C162 H162b . . . 109.7 ? H162a C162 H162c . . . 109.7 ? H162b C162 H162c . . . 110.0 ? C161 C163 H163a . . . 109.3 ? C161 C163 H163b . . . 109.1 ? C161 C163 H163c . . . 109.3 ? H163a C163 H163b . . . 109.5 ? H163a C163 H163c . . . 109.9 ? H163b C163 H163c . . . 109.7 ? C161 C164 H164a . . . 109.1 ? C161 C164 H164b . . . 109.0 ? C161 C164 H164c . . . 109.0 ? H164a C164 H164b . . . 109.9 ? H164a C164 H164c . . . 109.8 ? H164b C164 H164c . . . 110.0 ? Nd O21 C21 . . . 168.1(5) ? O21 C21 C22 . . . 120.9(8) ? O21 C21 C26 . . . 119.3(7) ? C22 C21 C26 . . . 119.8(8) ? C21 C22 C221 . . . 121.9(8) ? C21 C22 C23 . . . 119.2(9) ? C221 C22 C23 . . . 118.9(8) ? C22 C221 C222' . . . 116.6(10) ? C22 C221 C223' . . . 115.8(10) ? C22 C221 C224' . . . 109.0(9) ? C22 C221 C222 . . . 117(2) ? C22 C221 C223 . . . 101.1(15) ? C22 C221 C224 . . . 109(2) ? C222' C221 C223' . . . 108.3(12) ? C222' C221 C224' . . . 107.1(11) ? C223' C221 C224' . . . 98.2(11) ? C222 C221 C223 . . . 97(2) ? C222 C221 C224 . . . 124(3) ? C223 C221 C224 . . . 103(2) ? C221 C222' H222'a . . . 109.6 ? C221 C222' H222'b . . . 109.1 ? C221 C222' H222'c . . . 109.9 ? H222'a C222' H222'b . . . 109.1 ? H222'a C222' H222'c . . . 109.9 ? H222'b C222' H222'c . . . 109.3 ? C221 C223' H223'a . . . 106.6 ? C221 C223' H223'b . . . 109.2 ? C221 C223' H223'c . . . 109.9 ? H223'a C223' H223'b . . . 108 ? H223'a C223' H223'c . . . 109 ? H223'b C223' H223'c . . . 113 ? C221 C224' H224'a . . . 109.4 ? C221 C224' H224'b . . . 109.2 ? C221 C224' H224'c . . . 110.2 ? H224'a C224' H224'b . . . 108.4 ? H224'a C224' H224'c . . . 110.0 ? H224'b C224' H224'c . . . 109.5 ? C221 C222 H222a . . . 109 ? C221 C222 H222b . . . 111 ? C221 C222 H222c . . . 109 ? H222a C222 H222b . . . 110 ? H222a C222 H222c . . . 107 ? H222b C222 H222c . . . 110 ? C221 C223 H223a . . . 107 ? C221 C223 H223b . . . 109 ? C221 C223 H223c . . . 110 ? H223a C223 H223b . . . 108 ? H223a C223 H223c . . . 109 ? H223b C223 H223c . . . 112 ? C221 C224 H224a . . . 115 ? C221 C224 H224b . . . 112 ? C221 C224 H224c . . . 103 ? H224a C224 H224b . . . 119 ? H224a C224 H224c . . . 104 ? H224b C224 H224c . . . 101 ? C22 C23 C24 . . . 121.5(9) ? C22 C23 H23 . . . 119.8 ? C24 C23 H23 . . . 118.6 ? C23 C24 O24 . . . 124.7(10) ? C23 C24 C25 . . . 119.7(10) ? O24 C24 C25 . . . 115.6(10) ? C24 O24 C241 . . . 123.0(9) ? O24 C241 H241a . . . 109.9 ? O24 C241 H241b . . . 110.4 ? O24 C241 H241c . . . 107.1 ? H241a C241 H241b . . . 111.6 ? H241a C241 H241c . . . 107.9 ? H241b C241 H241c . . . 109.8 ? C24 C25 C26 . . . 122.5(9) ? C24 C25 H25 . . . 119.1 ? C26 C25 H25 . . . 118.4 ? C21 C26 C25 . . . 117.2(8) ? C21 C26 C261 . . . 125.7(8) ? C25 C26 C261 . . . 117.1(8) ? C26 C261 C262 . . . 107.5(11) ? C26 C261 C263 . . . 113.4(13) ? C26 C261 C264 . . . 114.6(12) ? C26 C261 C262' . . . 109.2(12) ? C26 C261 C263' . . . 115.2(11) ? C26 C261 C264' . . . 107.1(11) ? C262 C261 C263 . . . 107.3(15) ? C262 C261 C264 . . . 102.8(15) ? C263 C261 C264 . . . 110.3(16) ? C262' C261 C263' . . . 111.0 ? C262' C261 C264' . . . 113.2 ? C263' C261 C264' . . . 100.9 ? C261 C262 H262a . . . 118 ? C261 C262 H262b . . . 113.6 ? C261 C262 H262c . . . 112 ? H262a C262 H262b . . . 106 ? H262a C262 H262c . . . 105 ? H262b C262 H262c . . . 100 ? C261 C263 H263a . . . 108 ? C261 C263 H263b . . . 104.1 ? C261 C263 H263c . . . 111 ? H263a C263 H263b . . . 112 ? H263a C263 H263c . . . 114 ? H263b C263 H263c . . . 107 ? C261 C264 H264a . . . 112 ? C261 C264 H264b . . . 109 ? C261 C264 H264c . . . 118 ? H264a C264 H264b . . . 105 ? H264a C264 H264c . . . 108 ? H264b C264 H264c . . . 103 ? C261 C262' H262'a . . . 115 ? C261 C262' H262'b . . . 104 ? C261 C262' H262'c . . . 108 ? H262'a C262' H262'b . . . 110 ? H262'a C262' H262'c . . . 117 ? H262'b C262' H262'c . . . 101 ? C261 C263' H263'a . . . 110.2 ? C261 C263' H263'b . . . 114 ? C261 C263' H263'c . . . 117.9 ? H263'a C263' H263'b . . . 108 ? H263'a C263' H263'c . . . 100 ? H263'b C263' H263'c . . . 105 ? C261 C264' H264'a . . . 117.8 ? C261 C264' H264'b . . . 114 ? C261 C264' H264'c . . . 113 ? H264'a C264' H264'b . . . 104 ? H264'a C264' H264'c . . . 106 ? H264'b C264' H264'c . . . 101 ? Nd O31 C31 . . . 172.3(5) ? O31 C31 C32 . . . 119.4(7) ? O31 C31 C36 . . . 121.2(7) ? C32 C31 C36 . . . 119.4(7) ? C31 C32 C321 . . . 122.4(7) ? C31 C32 C33 . . . 119.4(7) ? C321 C32 C33 . . . 118.3(7) ? C32 C321 C322 . . . 110.6(7) ? C32 C321 C323 . . . 110.2(7) ? C32 C321 C324 . . . 113.5(8) ? C322 C321 C323 . . . 110.7(8) ? C322 C321 C324 . . . 105.8(8) ? C323 C321 C324 . . . 105.9(8) ? C321 C322 H322a . . . 112.5 ? C321 C322 H322b . . . 111.9 ? C321 C322 H322c . . . 113.8 ? H322a C322 H322b . . . 105.2 ? H322a C322 H322c . . . 106.2 ? H322b C322 H322c . . . 106.6 ? C321 C323 H323a . . . 113.6 ? C321 C323 H323b . . . 112.2 ? C321 C323 H323c . . . 115.2 ? H323a C323 H323b . . . 105.4 ? H323a C323 H323c . . . 105.3 ? H323b C323 H323c . . . 104.2 ? C321 C324 H324a . . . 109.7 ? C321 C324 H324b . . . 110.6 ? C321 C324 H324c . . . 114.8 ? H324a C324 H324b . . . 107.0 ? H324a C324 H324c . . . 107.7 ? H324b C324 H324c . . . 106.8 ? C32 C33 C34 . . . 120.6(8) ? C32 C33 H33 . . . 118.8 ? C34 C33 H33 . . . 120.6 ? C33 C34 O34 . . . 114.3(8) ? C33 C34 C35 . . . 120.7(8) ? O34 C34 C35 . . . 124.9(8) ? C34 O34 C341 . . . 118.5(8) ? O34 C341 H341a . . . 109.4 ? O34 C341 H341b . . . 108.3 ? O34 C341 H341c . . . 109.0 ? H341a C341 H341b . . . 109.9 ? H341a C341 H341c . . . 110.7 ? H341b C341 H341c . . . 109.5 ? C34 C35 C36 . . . 120.8(8) ? C34 C35 H35 . . . 119.5 ? C36 C35 H35 . . . 119.7 ? C31 C36 C35 . . . 119.1(8) ? C31 C36 C361 . . . 122.9(7) ? C35 C36 C361 . . . 117.9(7) ? C36 C361 C362 . . . 108.6(7) ? C36 C361 C363 . . . 113.2(7) ? C36 C361 C364 . . . 110.4(7) ? C362 C361 C363 . . . 106.4(7) ? C362 C361 C364 . . . 110.6(7) ? C363 C361 C364 . . . 107.5(7) ? C361 C362 H362a . . . 112.4 ? C361 C362 H362b . . . 112.3 ? C361 C362 H362c . . . 110.5 ? H362a C362 H362b . . . 108.2 ? H362a C362 H362c . . . 106.9 ? H362b C362 H362c . . . 106.3 ? C361 C363 H363a . . . 110.4 ? C361 C363 H363b . . . 111.7 ? C361 C363 H363c . . . 115.7 ? H363a C363 H363b . . . 106.8 ? H363a C363 H363c . . . 104.7 ? H363b C363 H363c . . . 106.9 ? C361 C364 H364a . . . 112.7 ? C361 C364 H364b . . . 111.4 ? C361 C364 H364c . . . 114.6 ? H364a C364 H364b . . . 104.8 ? H364a C364 H364c . . . 107.3 ? H364b C364 H364c . . . 105.5 ? Nd O101 C102 . . . 129.4(6) ? Nd O101 C105 . . . 121.7(5) ? C102 O101 C105 . . . 108.2(7) ? O101 C102 C103 . . . 106.3(9) ? O101 C102 H102a . . . 112.0 ? O101 C102 H102b . . . 111.6 ? C103 C102 H102a . . . 109.6 ? C103 C102 H102b . . . 113.6 ? H102a C102 H102b . . . 103.9 ? C102 C103 C104 . . . 112.2(12) ? C102 C103 H103a . . . 111.0 ? C102 C103 H103b . . . 105.0 ? C104 C103 H103a . . . 113.6 ? C104 C103 H103b . . . 106.4 ? H103a C103 H103b . . . 108.1 ? C103 C104 C105 . . . 104.5(10) ? C103 C104 H104a . . . 109.4 ? C103 C104 H104b . . . 114.2 ? C105 C104 H104a . . . 111.9 ? C105 C104 H104b . . . 111.7 ? H104a C104 H104b . . . 105.3 ? O101 C105 C104 . . . 106.1(8) ? O101 C105 H105a . . . 111.1 ? O101 C105 H105b . . . 114.7 ? C104 C105 H105a . . . 109.5 ? C104 C105 H105b . . . 111.7 ? H105a C105 H105b . . . 103.8 ? C202 O201 C205 . . . 109(3) ? O201 C202 C203 . . . 101(3) ? O201 C202 H202a . . . 114 ? O201 C202 H202b . . . 116 ? C203 C202 H202a . . . 109 ? C203 C202 H202b . . . 112 ? H202a C202 H202b . . . 105 ? C202 C203 C204 . . . 112(3) ? C202 C203 H203a . . . 112 ? C202 C203 H203b . . . 110 ? C204 C203 H203a . . . 111 ? C204 C203 H203b . . . 111 ? H203a C203 H203b . . . 100 ? C203 C204 C205 . . . 106(3) ? C203 C204 H204a . . . 105 ? C203 C204 H204b . . . 105 ? C205 C204 H204a . . . 119 ? C205 C204 H204b . . . 118 ? H204a C204 H204b . . . 103 ? O201 C205 C204 . . . 109(3) ? O201 C205 H205a . . . 120 ? O201 C205 H205b . . . 123 ? C204 C205 H205a . . . 97 ? C204 C205 H205b . . . 100 ? H205a C205 H205b . . . 102 ? _exptl_crystal_F_000 2108 _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .841 _reflns_d_resolution_low 12.47 _diffrn_reflns_av_sigmaI/netI .08 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_reduction_process 'equatorial monochr Lp' _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 12 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .128 _refine_ls_wR_factor_all .067 _refine_ls_goodness_of_fit_all 1.173 _refine_ls_shift/su_mean .0001