Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' #============================================================================== # (Publishing Staff Use Only) _journal_coden_Cambridge 0222 _audit_creation_method Xtal3.6 _audit_creation_date 06-05-19 _audit_update_record ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Ewan Delbridge' _publ_contact_author_address ; Department of Chemistry University of North Dakota Box 9024 Grand Forks North Dakota 58202 UNITED STATES OF AMERICA ; _publ_contact_author_email EDELBRIDGE@CHEM.UND.EDU _publ_section_title ; Synthesis, Structure and Oxidation of New Ytterbium(II) Bis(phenolate) Compounds and Catalytic Activity Towards ?-Caprolactone ; _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 'Ewan Delbridge' 'Divine T. Dugah' 'Chassidy R. Nelson' 'Brian W. Skelton' 'Allan H. White' #===END # Attachment 'edyb2.cif' ######################################## # # # CIF generated by the Xtal System # # # ######################################## #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_edyb2 _database_code_depnum_ccdc_archive 'CCDC 272546' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C74 H122 N4 O4 Yb2' _chemical_formula_moiety ' C68 H108 N4 O4 Yb2, C6 H14)' _chemical_formula_weight 1478.08 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_2/c_1 _symmetry_space_group_name_Hall -p_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z _cell_length_a 14.049(5) _cell_length_b 9.693(5) _cell_length_c 26.772(8) _cell_angle_alpha 90.00000 _cell_angle_beta 91.352(5) _cell_angle_gamma 90.00000 _cell_volume 3645(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7785 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.9 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 2.597 _exptl_crystal_description fragment _exptl_crystal_size_max .09 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour red _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .85 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 34303 _reflns_number_total 9093 _reflns_Friedel_coverage 0 _reflns_number_gt 9093 _reflns_threshold_expression 'I > 2.00 sig(I)' _diffrn_reflns_theta_max 29. _diffrn_reflns_theta_full 29. _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .063 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .063 _refine_ls_wR_factor_ref .129 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_number_reflns 9089 _refine_ls_number_parameters 366 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .045 _refine_diff_density_min -1.551 _refine_diff_density_max 3.257 _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 'Siemens SAINT' _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 ? 0 148 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 244 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 8 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' O ? 0 8 .008 .006 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Yb ? 0 4 -.884 5.548 '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 Yb .42231(2) .56143(3) .696387(11) .02660(17) Uani ? ? 1.00000 ? ? N1 .3008(4) .7310(6) .7296(2) .029(3) Uani ? ? 1.00000 ? ? C10 .3106(5) .7400(8) .7855(3) .030(4) Uani ? ? 1.00000 ? ? C11 .2918(5) .6125(8) .8146(3) .029(4) Uani ? ? 1.00000 ? ? C12 .3502(5) .4966(8) .8107(3) .028(3) Uani ? ? 1.00000 ? ? O12 .4221(4) .4983(5) .77910(18) .028(3) Uani ? ? 1.00000 ? ? C13 .3322(6) .3770(8) .8409(3) .032(4) Uani ? ? 1.00000 ? ? C131 .3919(7) .2444(8) .8356(3) .036(4) Uani ? ? 1.00000 ? ? C132 .3790(8) .1860(10) .7827(4) .049(5) Uani ? ? 1.00000 ? ? C133 .4987(7) .2682(9) .8467(3) .043(5) Uani ? ? 1.00000 ? ? C134 .3613(8) .1320(10) .8726(4) .050(5) Uani ? ? 1.00000 ? ? C14 .2593(6) .3858(9) .8749(3) .037(4) Uani ? ? 1.00000 ? ? C15 .2019(7) .5018(10) .8798(3) .041(5) Uani ? ? 1.00000 ? ? C151 .1274(8) .5028(10) .9212(4) .048(5) Uani ? ? 1.00000 ? ? C152 .0675(8) .6349(14) .9202(4) .060(6) Uani ? ? 1.00000 ? ? C153 .1768(9) .4900(13) .9728(4) .064(7) Uani ? ? 1.00000 ? ? C154 .0580(7) .3807(12) .9135(4) .055(6) Uani ? ? 1.00000 ? ? C16 .2165(6) .6133(9) .8490(3) .036(4) Uani ? ? 1.00000 ? ? C20 .3222(5) .8716(8) .7095(3) .030(4) Uani ? ? 1.00000 ? ? C21 .3305(5) .8731(8) .6543(3) .030(4) Uani ? ? 1.00000 ? ? C22 .4107(5) .8142(7) .6325(3) .027(3) Uani ? ? 1.00000 ? ? O22 .4757(4) .7533(6) .66100(18) .031(3) Uani ? ? 1.00000 ? ? C23 .4170(5) .8139(7) .5787(3) .026(3) Uani ? ? 1.00000 ? ? C231 .5012(6) .7456(8) .5535(3) .034(4) Uani ? ? 1.00000 ? ? C232 .5045(7) .5910(8) .5652(3) .037(4) Uani ? ? 1.00000 ? ? C233 .5967(6) .8100(9) .5706(3) .040(4) Uani ? ? 1.00000 ? ? C234 .4942(7) .7599(9) .4959(3) .041(4) Uani ? ? 1.00000 ? ? C24 .3430(6) .8744(8) .5511(3) .034(4) Uani ? ? 1.00000 ? ? C25 .2623(5) .9313(7) .5716(3) .029(4) Uani ? ? 1.00000 ? ? C251 .1779(6) .9850(9) .5395(3) .039(4) Uani ? ? 1.00000 ? ? C252 .1937(8) .9666(15) .4828(4) .068(7) Uani ? ? 1.00000 ? ? C253 .1596(11) 1.1308(17) .5491(6) .087(4) Uiso ? ? 1.00000 ? ? C254 .0928(9) .892(2) .5503(5) .097(10) Uani ? ? 1.00000 ? ? C26 .2599(5) .9332(7) .6229(3) .029(3) Uani ? ? 1.00000 ? ? C1 .2024(6) .6881(9) .7145(3) .038(4) Uani ? ? 1.00000 ? ? C2 .1932(7) .5332(13) .7047(3) .052(6) Uani ? ? 1.00000 ? ? N3 .2567(5) .4807(8) .6659(3) .039(4) Uani ? ? 1.00000 ? ? C41 .2466(8) .3277(13) .6655(5) .065(7) Uani ? ? 1.00000 ? ? C42 .2311(7) .5353(13) .6163(4) .057(6) Uani ? ? 1.00000 ? ? C01 .088(4) .935(7) .849(2) .264(16) Uiso ? ? .50000 ? ? C02 .078(5) 1.052(5) .824(2) .264(16) Uiso ? ? .50000 ? ? C03 .013(4) 1.032(5) .786(2) .264(16) Uiso ? ? .50000 ? ? C04 .003(6) 1.158(4) .759(3) .264(16) Uiso ? ? .50000 ? ? C05 -.064(4) 1.137(5) .719(2) .264(16) Uiso ? ? .50000 ? ? C06 -.073(5) 1.261(7) .693(2) .264(16) Uiso ? ? .50000 ? ? H10a .37391 .76799 .79337 .03800 Uiso ? ? 1.00000 ? ? H10b .26736 .80848 .79627 .03800 Uiso ? ? 1.00000 ? ? H132a .41627 .10452 .77964 .07300 Uiso ? ? 1.00000 ? ? H132b .40004 .25257 .75914 .07300 Uiso ? ? 1.00000 ? ? H132c .31417 .16528 .77623 .07300 Uiso ? ? 1.00000 ? ? H133a .53187 .18351 .84290 .06400 Uiso ? ? 1.00000 ? ? H133b .50705 .30049 .87993 .06400 Uiso ? ? 1.00000 ? ? H133c .52216 .33431 .82404 .06400 Uiso ? ? 1.00000 ? ? H134a .39937 .05224 .86826 .07500 Uiso ? ? 1.00000 ? ? H134b .29631 .10979 .86647 .07500 Uiso ? ? 1.00000 ? ? H134c .36962 .16551 .90574 .07500 Uiso ? ? 1.00000 ? ? H14 .24815 .30895 .89586 .04600 Uiso ? ? 1.00000 ? ? H152a .02270 .63175 .94614 .09100 Uiso ? ? 1.00000 ? ? H152b .03502 .64269 .88885 .09100 Uiso ? ? 1.00000 ? ? H152c .10817 .71258 .92504 .09100 Uiso ? ? 1.00000 ? ? H153a .13014 .49045 .99802 .09800 Uiso ? ? 1.00000 ? ? H153b .21915 .56507 .97796 .09800 Uiso ? ? 1.00000 ? ? H153c .21143 .40567 .97459 .09800 Uiso ? ? 1.00000 ? ? H154a .01229 .38154 .93897 .08300 Uiso ? ? 1.00000 ? ? H154b .09269 .29651 .91485 .08300 Uiso ? ? 1.00000 ? ? H154c .02675 .38895 .88177 .08300 Uiso ? ? 1.00000 ? ? H16 .17606 .69156 .85077 .04400 Uiso ? ? 1.00000 ? ? H20a .38055 .90281 .72415 .03800 Uiso ? ? 1.00000 ? ? H20b .27232 .93238 .71846 .03800 Uiso ? ? 1.00000 ? ? H232a .55744 .55069 .54928 .05600 Uiso ? ? 1.00000 ? ? H232b .44749 .54867 .55340 .05600 Uiso ? ? 1.00000 ? ? H232c .51108 .57821 .60035 .05600 Uiso ? ? 1.00000 ? ? H233a .64722 .76525 .55415 .06000 Uiso ? ? 1.00000 ? ? H233b .60485 .79973 .60566 .06000 Uiso ? ? 1.00000 ? ? H233c .59676 .90554 .56229 .06000 Uiso ? ? 1.00000 ? ? H234a .54768 .71616 .48145 .06100 Uiso ? ? 1.00000 ? ? H234b .49348 .85457 .48697 .06100 Uiso ? ? 1.00000 ? ? H234c .43744 .71682 .48373 .06100 Uiso ? ? 1.00000 ? ? H24 .34829 .87692 .51584 .04200 Uiso ? ? 1.00000 ? ? H252a .14004 1.00110 .46443 .10300 Uiso ? ? 1.00000 ? ? H252b .20172 .87137 .47542 .10300 Uiso ? ? 1.00000 ? ? H252c .24905 1.01580 .47346 .10300 Uiso ? ? 1.00000 ? ? H253a .10612 1.16210 .52947 .12500 Uiso ? ? 1.00000 ? ? H253b .21307 1.18550 .54254 .12500 Uiso ? ? 1.00000 ? ? H253c .14356 1.14300 .58400 .12500 Uiso ? ? 1.00000 ? ? H254a .03907 .91960 .53077 .13400 Uiso ? ? 1.00000 ? ? H254b .07908 .89353 .58445 .13400 Uiso ? ? 1.00000 ? ? H254c .10860 .79796 .54099 .13400 Uiso ? ? 1.00000 ? ? H26 .20767 .97747 .63808 .03600 Uiso ? ? 1.00000 ? ? H1a .18446 .73613 .68489 .04800 Uiso ? ? 1.00000 ? ? H1b .16087 .71255 .74056 .04800 Uiso ? ? 1.00000 ? ? H2a .12916 .51406 .69450 .06400 Uiso ? ? 1.00000 ? ? H2b .20736 .48521 .73504 .06400 Uiso ? ? 1.00000 ? ? H41a .28696 .28984 .64070 .09600 Uiso ? ? 1.00000 ? ? H41b .18261 .30355 .65774 .09600 Uiso ? ? 1.00000 ? ? H41c .26484 .29156 .69719 .09600 Uiso ? ? 1.00000 ? ? H42a .27280 .50025 .59241 .08400 Uiso ? ? 1.00000 ? ? H42b .23486 .63350 .61712 .08400 Uiso ? ? 1.00000 ? ? H42c .16725 .50909 .60787 .08400 Uiso ? ? 1.00000 ? ? H01a .13303 .94896 .87600 .39200 Uiso ? ? .50000 ? ? H01b .10890 .86432 .82818 .39200 Uiso ? ? .50000 ? ? H01c .02814 .91072 .86296 .39200 Uiso ? ? .50000 ? ? H02a .13746 1.07693 .81014 .32700 Uiso ? ? .50000 ? ? H02b .05670 1.12334 .84492 .32700 Uiso ? ? .50000 ? ? H03a -.04619 1.00469 .79957 .32700 Uiso ? ? .50000 ? ? H03b .03473 .96016 .76457 .32700 Uiso ? ? .50000 ? ? H04a .06202 1.18436 .74584 .32700 Uiso ? ? .50000 ? ? H04b -.01998 1.22785 .78031 .32700 Uiso ? ? .50000 ? ? H05a -.12337 1.10951 .73236 .32700 Uiso ? ? .50000 ? ? H05b -.04140 1.06557 .69794 .32700 Uiso ? ? .50000 ? ? H06a -.11224 1.24444 .66391 .39200 Uiso ? ? .50000 ? ? H06b -.01254 1.29100 .68353 .39200 Uiso ? ? .50000 ? ? H06c -.10247 1.32655 .71350 .39200 Uiso ? ? .50000 ? ? 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 .03122(18) .02744(18) .02084(16) -.00080(12) -.00584(11) -.00124(11) N1 .030(3) .027(3) .028(3) -.005(2) -.007(2) -.005(2) C10 .033(4) .030(4) .028(4) .003(3) .001(3) -.002(3) C11 .034(4) .028(4) .024(3) -.004(3) -.003(3) -.001(3) C12 .033(4) .028(4) .022(3) -.009(3) -.004(3) .002(3) O12 .035(3) .027(3) .023(2) .001(2) -.000(2) .002(2) C13 .039(4) .029(4) .028(4) .001(3) -.003(3) -.005(3) C131 .064(6) .024(4) .021(3) -.008(4) .006(3) .000(3) C132 .065(6) .038(5) .042(5) -.005(4) -.011(4) -.008(4) C133 .054(5) .038(5) .035(4) .012(4) -.007(4) -.004(4) C134 .072(7) .037(5) .041(5) -.012(5) .009(4) .002(4) C14 .044(4) .036(4) .031(4) -.008(4) -.002(3) .003(3) C15 .048(5) .043(5) .030(4) -.015(4) .004(3) -.003(3) C151 .060(6) .046(5) .038(5) -.007(5) .003(4) .006(4) C152 .052(6) .084(8) .046(6) -.011(6) .019(5) .004(6) C153 .090(8) .074(8) .029(5) -.007(7) .024(5) .003(5) C154 .044(5) .064(7) .056(6) -.007(5) .006(4) .008(5) C16 .042(4) .035(4) .030(4) -.005(3) .002(3) -.011(3) C20 .033(4) .027(3) .029(4) .003(3) -.007(3) -.002(3) C21 .026(3) .032(4) .031(4) -.004(3) -.011(3) -.001(3) C22 .024(3) .017(3) .039(4) -.004(3) -.012(3) .001(3) O22 .032(3) .040(3) .022(2) .005(2) -.008(2) -.000(2) C23 .036(4) .018(3) .025(3) .002(3) -.002(3) -.002(3) C231 .045(4) .030(4) .027(4) -.005(3) -.010(3) .005(3) C232 .052(5) .029(4) .031(4) .007(4) .001(3) .000(3) C233 .035(4) .040(4) .044(5) -.000(4) -.015(3) .000(4) C234 .051(5) .036(4) .035(4) .007(4) -.006(4) .005(4) C24 .037(4) .030(4) .034(4) -.005(3) -.002(3) .013(3) C25 .028(3) .025(3) .034(4) -.000(3) -.009(3) .014(3) C251 .041(4) .041(5) .033(4) .005(4) -.002(3) .015(4) C252 .063(7) .100(10) .040(5) .023(7) -.017(5) -.011(6) C254 .046(6) .171(16) .072(8) -.011(8) -.007(6) .065(10) C26 .031(4) .024(3) .031(4) .006(3) -.004(3) -.003(3) C1 .040(4) .039(4) .035(4) -.001(4) -.007(3) .002(4) C2 .034(4) .084(8) .037(5) -.019(5) -.011(4) .004(5) N3 .038(4) .045(4) .034(4) -.011(3) -.012(3) -.006(3) C41 .060(7) .060(7) .073(8) -.013(6) -.021(6) -.001(6) C42 .043(5) .086(8) .042(5) -.024(5) -.009(4) .022(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 #<< enter YES for value to be published Yb N1 . . 2.545(6) ? Yb O12 . . 2.297(5) ? Yb O22 . . 2.225(6) ? Yb N3 . . 2.569(7) ? Yb O12 . '2 656' 2.349(5) ? N1 C10 . . 1.503(10) ? N1 C20 . . 1.498(10) ? N1 C1 . . 1.490(11) ? C10 C11 . . 1.488(11) ? C10 H10a . . .950 ? C10 H10b . . .949 ? C11 C12 . . 1.396(11) ? C11 C16 . . 1.420(11) ? C12 O12 . . 1.333(9) ? C12 C13 . . 1.439(11) ? C13 C131 . . 1.543(12) ? C13 C14 . . 1.388(12) ? C131 C132 . . 1.532(12) ? C131 C133 . . 1.540(14) ? C131 C134 . . 1.539(12) ? C132 H132a . . .953 ? C132 H132b . . .954 ? C132 H132c . . .945 ? C133 H133a . . .950 ? C133 H133b . . .948 ? C133 H133c . . .948 ? C134 H134a . . .949 ? C134 H134b . . .949 ? C134 H134c . . .950 ? C14 C15 . . 1.392(13) ? C14 H14 . . .948 ? C15 C151 . . 1.542(14) ? C15 C16 . . 1.378(12) ? C151 C152 . . 1.532(16) ? C151 C153 . . 1.537(14) ? C151 C154 . . 1.544(15) ? C152 H152a . . .949 ? C152 H152b . . .950 ? C152 H152c . . .952 ? C153 H153a . . .951 ? C153 H153b . . .948 ? C153 H153c . . .952 ? C154 H154a . . .949 ? C154 H154b . . .951 ? C154 H154c . . .950 ? C16 H16 . . .950 ? C20 C21 . . 1.487(11) ? C20 H20a . . .949 ? C20 H20b . . .950 ? C21 C22 . . 1.402(10) ? C21 C26 . . 1.410(10) ? C22 O22 . . 1.316(9) ? C22 C23 . . 1.445(10) ? C23 C231 . . 1.526(11) ? C23 C24 . . 1.390(11) ? C231 C232 . . 1.531(12) ? C231 C233 . . 1.540(12) ? C231 C234 . . 1.550(12) ? C232 H232a . . .950 ? C232 H232b . . .947 ? C232 H232c . . .951 ? C233 H233a . . .948 ? C233 H233b . . .949 ? C233 H233c . . .952 ? C234 H234a . . .952 ? C234 H234b . . .948 ? C234 H234c . . .951 ? C24 C25 . . 1.386(11) ? C24 H24 . . .950 ? C25 C251 . . 1.539(11) ? C25 C26 . . 1.375(11) ? C251 C252 . . 1.549(14) ? C251 C253 . . 1.460(19) ? C251 C254 . . 1.530(18) ? C252 H252a . . .950 ? C252 H252b . . .951 ? C252 H252c . . .951 ? C253 H253a . . .957 ? C253 H253b . . .939 ? C253 H253c . . .972 ? C254 H254a . . .947 ? C254 H254b . . .939 ? C254 H254c . . .97 ? C26 H26 . . .950 ? C1 C2 . . 1.528(15) ? C1 H1a . . .948 ? C1 H1b . . .950 ? C2 N3 . . 1.476(12) ? C2 H2a . . .953 ? C2 H2b . . .952 ? N3 C41 . . 1.490(15) ? N3 C42 . . 1.467(13) ? C41 H41a . . .956 ? C41 H41b . . .947 ? C41 H41c . . .948 ? C42 H42a . . .940 ? C42 H42b . . .954 ? C42 H42c . . .954 ? C01 C02 . . 1.33(8) ? C01 H01a . . .95 ? C01 H01b . . .95 ? C01 H01c . . .95 ? C02 C03 . . 1.36(8) ? C02 H02a . . .95 ? C02 H02b . . .95 ? C03 C04 . . 1.43(7) ? C03 H03a . . .95 ? C03 H03b . . .95 ? C04 C05 . . 1.41(9) ? C04 H04a . . .94 ? C04 H04b . . .95 ? C05 C06 . . 1.40(9) ? C05 H05a . . .95 ? C05 H05b . . .96 ? C06 H06a . . .95 ? C06 H06b . . .94 ? C06 H06c . . .94 ? 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 N1 Yb O12 . . . 79.6(2) ? N1 Yb O22 . . . 81.1(2) ? N1 Yb N3 . . . 72.4(2) ? N1 Yb O12 . . '2 656' 134.29(19) ? O12 Yb O22 . . . 129.86(18) ? O12 Yb N3 . . . 101.7(2) ? O12 Yb O12 . . '2 656' 71.56(18) ? O22 Yb N3 . . . 115.5(2) ? O22 Yb O12 . . '2 656' 90.90(19) ? N3 Yb O12 . . '2 656' 147.1(2) ? Yb N1 C10 . . . 109.8(4) ? Yb N1 C20 . . . 108.7(4) ? Yb N1 C1 . . . 110.5(5) ? C10 N1 C20 . . . 106.8(6) ? C10 N1 C1 . . . 110.4(6) ? C20 N1 C1 . . . 110.5(6) ? N1 C10 C11 . . . 117.4(6) ? N1 C10 H10a . . . 107.5 ? N1 C10 H10b . . . 107.5 ? C11 C10 H10a . . . 107.3 ? C11 C10 H10b . . . 107.4 ? H10a C10 H10b . . . 109.6 ? C10 C11 C12 . . . 121.2(7) ? C10 C11 C16 . . . 118.6(7) ? C12 C11 C16 . . . 120.0(7) ? C11 C12 O12 . . . 119.5(6) ? C11 C12 C13 . . . 119.7(7) ? O12 C12 C13 . . . 120.8(7) ? Yb O12 C12 . . . 129.4(4) ? Yb O12 Yb . . '2 656' 100.2(2) ? C12 O12 Yb . . '2 656' 122.6(4) ? C12 C13 C131 . . . 121.1(7) ? C12 C13 C14 . . . 117.4(7) ? C131 C13 C14 . . . 121.5(7) ? C13 C131 C132 . . . 109.9(7) ? C13 C131 C133 . . . 112.7(7) ? C13 C131 C134 . . . 111.7(7) ? C132 C131 C133 . . . 109.1(7) ? C132 C131 C134 . . . 107.7(7) ? C133 C131 C134 . . . 105.5(7) ? C131 C132 H132a . . . 109.4 ? C131 C132 H132b . . . 109.3 ? C131 C132 H132c . . . 110.0 ? H132a C132 H132b . . . 108.9 ? H132a C132 H132c . . . 109.7 ? H132b C132 H132c . . . 109.6 ? C131 C133 H133a . . . 109.2 ? C131 C133 H133b . . . 109.2 ? C131 C133 H133c . . . 109.3 ? H133a C133 H133b . . . 109.6 ? H133a C133 H133c . . . 109.7 ? H133b C133 H133c . . . 109.9 ? C131 C134 H134a . . . 109.4 ? C131 C134 H134b . . . 109.4 ? C131 C134 H134c . . . 109.2 ? H134a C134 H134b . . . 109.7 ? H134a C134 H134c . . . 109.6 ? H134b C134 H134c . . . 109.6 ? C13 C14 C15 . . . 123.4(8) ? C13 C14 H14 . . . 118.3 ? C15 C14 H14 . . . 118.3 ? C14 C15 C151 . . . 118.5(8) ? C14 C15 C16 . . . 118.8(8) ? C151 C15 C16 . . . 122.6(8) ? C15 C151 C152 . . . 112.0(8) ? C15 C151 C153 . . . 110.3(9) ? C15 C151 C154 . . . 109.6(8) ? C152 C151 C153 . . . 108.6(9) ? C152 C151 C154 . . . 107.1(9) ? C153 C151 C154 . . . 109.2(9) ? C151 C152 H152a . . . 109.6 ? C151 C152 H152b . . . 109.5 ? C151 C152 H152c . . . 109.4 ? H152a C152 H152b . . . 109.6 ? H152a C152 H152c . . . 109.4 ? H152b C152 H152c . . . 109.4 ? C151 C153 H153a . . . 109.5 ? C151 C153 H153b . . . 109.7 ? C151 C153 H153c . . . 109.5 ? H153a C153 H153b . . . 109.5 ? H153a C153 H153c . . . 109.2 ? H153b C153 H153c . . . 109.4 ? C151 C154 H154a . . . 109.5 ? C151 C154 H154b . . . 109.4 ? C151 C154 H154c . . . 109.4 ? H154a C154 H154b . . . 109.5 ? H154a C154 H154c . . . 109.6 ? H154b C154 H154c . . . 109.4 ? C11 C16 C15 . . . 120.5(8) ? C11 C16 H16 . . . 119.5 ? C15 C16 H16 . . . 119.9 ? N1 C20 C21 . . . 112.7(6) ? N1 C20 H20a . . . 108.7 ? N1 C20 H20b . . . 108.6 ? C21 C20 H20a . . . 108.7 ? C21 C20 H20b . . . 108.7 ? H20a C20 H20b . . . 109.5 ? C20 C21 C22 . . . 119.5(7) ? C20 C21 C26 . . . 121.7(7) ? C22 C21 C26 . . . 118.8(7) ? C21 C22 O22 . . . 119.7(7) ? C21 C22 C23 . . . 118.9(6) ? O22 C22 C23 . . . 121.3(6) ? Yb O22 C22 . . . 112.6(4) ? C22 C23 C231 . . . 120.5(6) ? C22 C23 C24 . . . 117.8(7) ? C231 C23 C24 . . . 121.8(7) ? C23 C231 C232 . . . 110.7(7) ? C23 C231 C233 . . . 111.9(6) ? C23 C231 C234 . . . 111.7(7) ? C232 C231 C233 . . . 108.3(7) ? C232 C231 C234 . . . 107.0(7) ? C233 C231 C234 . . . 107.0(7) ? C231 C232 H232a . . . 109.3 ? C231 C232 H232b . . . 109.5 ? C231 C232 H232c . . . 109.4 ? H232a C232 H232b . . . 109.6 ? H232a C232 H232c . . . 109.3 ? H232b C232 H232c . . . 109.6 ? C231 C233 H233a . . . 109.5 ? C231 C233 H233b . . . 109.5 ? C231 C233 H233c . . . 109.3 ? H233a C233 H233b . . . 109.7 ? H233a C233 H233c . . . 109.4 ? H233b C233 H233c . . . 109.4 ? C231 C234 H234a . . . 109.4 ? C231 C234 H234b . . . 109.7 ? C231 C234 H234c . . . 109.5 ? H234a C234 H234b . . . 109.4 ? H234a C234 H234c . . . 109.2 ? H234b C234 H234c . . . 109.5 ? C23 C24 C25 . . . 124.6(7) ? C23 C24 H24 . . . 117.7 ? C25 C24 H24 . . . 117.8 ? C24 C25 C251 . . . 122.8(7) ? C24 C25 C26 . . . 116.0(7) ? C251 C25 C26 . . . 121.1(7) ? C25 C251 C252 . . . 112.5(8) ? C25 C251 C253 . . . 111.4(9) ? C25 C251 C254 . . . 106.8(8) ? C252 C251 C253 . . . 108.4(10) ? C252 C251 C254 . . . 104.4(9) ? C253 C251 C254 . . . 113.2(11) ? C251 C252 H252a . . . 109.6 ? C251 C252 H252b . . . 109.6 ? C251 C252 H252c . . . 109.6 ? H252a C252 H252b . . . 109.4 ? H252a C252 H252c . . . 109.4 ? H252b C252 H252c . . . 109.3 ? C251 C253 H253a . . . 110.4 ? C251 C253 H253b . . . 111.6 ? C251 C253 H253c . . . 109.5 ? H253a C253 H253b . . . 109.8 ? H253a C253 H253c . . . 107.0 ? H253b C253 H253c . . . 108.5 ? C251 C254 H254a . . . 110.2 ? C251 C254 H254b . . . 110.8 ? C251 C254 H254c . . . 108.7 ? H254a C254 H254b . . . 110.7 ? H254a C254 H254c . . . 107.9 ? H254b C254 H254c . . . 108.5 ? C21 C26 C25 . . . 123.8(7) ? C21 C26 H26 . . . 118.1 ? C25 C26 H26 . . . 118.1 ? N1 C1 C2 . . . 113.2(7) ? N1 C1 H1a . . . 108.4 ? N1 C1 H1b . . . 108.3 ? C2 C1 H1a . . . 108.7 ? C2 C1 H1b . . . 108.7 ? H1a C1 H1b . . . 109.6 ? C1 C2 N3 . . . 114.2(8) ? C1 C2 H2a . . . 108.4 ? C1 C2 H2b . . . 108.6 ? N3 C2 H2a . . . 108.2 ? N3 C2 H2b . . . 108.3 ? H2a C2 H2b . . . 109.0 ? Yb N3 C2 . . . 103.2(5) ? Yb N3 C41 . . . 113.0(6) ? Yb N3 C42 . . . 112.3(6) ? C2 N3 C41 . . . 106.9(8) ? C2 N3 C42 . . . 111.9(8) ? C41 N3 C42 . . . 109.3(8) ? N3 C41 H41a . . . 109.2 ? N3 C41 H41b . . . 109.8 ? N3 C41 H41c . . . 109.7 ? H41a C41 H41b . . . 109.2 ? H41a C41 H41c . . . 109.1 ? H41b C41 H41c . . . 109.9 ? N3 C42 H42a . . . 110.0 ? N3 C42 H42b . . . 109.0 ? N3 C42 H42c . . . 109.1 ? H42a C42 H42b . . . 109.9 ? H42a C42 H42c . . . 109.9 ? H42b C42 H42c . . . 108.8 ? C02 C01 H01a . . . 109 ? C02 C01 H01b . . . 109 ? C02 C01 H01c . . . 110 ? H01a C01 H01b . . . 110 ? H01a C01 H01c . . . 109 ? H01b C01 H01c . . . 110 ? C01 C02 C03 . . . 109(5) ? C01 C02 H02a . . . 110 ? C01 C02 H02b . . . 109 ? C03 C02 H02a . . . 110(6) ? C03 C02 H02b . . . 109(6) ? H02a C02 H02b . . . 110(5) ? C02 C03 C04 . . . 108(5) ? C02 C03 H03a . . . 110(5) ? C02 C03 H03b . . . 109(5) ? C04 C03 H03a . . . 111(5) ? C04 C03 H03b . . . 110(5) ? H03a C03 H03b . . . 109(5) ? C03 C04 C05 . . . 108(5) ? C03 C04 H04a . . . 110(6) ? C03 C04 H04b . . . 109(6) ? C05 C04 H04a . . . 110(6) ? C05 C04 H04b . . . 109(6) ? H04a C04 H04b . . . 110(5) ? C04 C05 C06 . . . 108(5) ? C04 C05 H05a . . . 110(6) ? C04 C05 H05b . . . 109(5) ? C06 C05 H05a . . . 111(6) ? C06 C05 H05b . . . 110(6) ? H05a C05 H05b . . . 109(5) ? C05 C06 H06a . . . 108(6) ? C05 C06 H06b . . . 109(6) ? C05 C06 H06c . . . 109(6) ? H06a C06 H06b . . . 110(7) ? H06a C06 H06c . . . 110(7) ? H06b C06 H06c . . . 111(7) ? _exptl_crystal_F_000 1532 _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -35 _reflns_limit_l_max 36 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 14.006 _diffrn_reflns_av_sigmaI/netI .087 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _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 12 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .088 _refine_ls_wR_factor_all .167 _refine_ls_goodness_of_fit_all 1.217 _refine_ls_shift/su_mean .001 #===END # Attachment 'edybrt.cif' ######################################## # # # CIF generated by the Xtal System # # # ######################################## #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_edybrt _database_code_depnum_ccdc_archive 'CCDC 272547' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C74 H122 K1 N2 O10 Yb1' _chemical_formula_moiety 'C74 H122 K1 N2 O10 Yb1' _chemical_formula_weight 1411.93 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 14.0570(10) _cell_length_b 14.1370(10) _cell_length_c 23.703(2) _cell_angle_alpha 99.4510(10) _cell_angle_beta 95.457(2) _cell_angle_gamma 119.4920(10) _cell_volume 3958.5(5) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5640 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 27.94 _cell_measurement_temperature 298 _exptl_absorpt_coefficient_mu 1.285 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .25 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .77 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 36801 _reflns_number_total 19277 _reflns_Friedel_coverage ? _reflns_number_gt 16330 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 29.22 _diffrn_reflns_theta_full 29.22 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .026 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .043 _refine_ls_wR_factor_gt .084 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_number_reflns 19227 _refine_ls_number_parameters 790 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/(sig^2(F) + 14F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .028 _refine_diff_density_min -1.124 _refine_diff_density_max 1.777 _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 _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 ? 0 148 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 244 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' K ? 0 2 .179016 .25 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 4 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 20 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' Yb ? 0 2 -.883972 5.548 '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 .891340(10) .647420(10) .754760(10) .04081(7) Uani ? ? 1.00000 ? ? K .56802(10) .52651(10) .75672(5) .0683(5) Uani ? ? 1.00000 ? ? N11 .8939(3) .8059(3) .71729(13) .0406(12) Uani ? ? 1.00000 ? ? C110 .7964(3) .8144(4) .73095(16) .0459(15) Uani ? ? 1.00000 ? ? C111 .7990(3) .8525(3) .79459(17) .0447(15) Uani ? ? 1.00000 ? ? C112 .7988(3) .7857(3) .83274(17) .0443(14) Uani ? ? 1.00000 ? ? O112 .7993(3) .6921(2) .81133(12) .0473(11) Uani ? ? 1.00000 ? ? C113 .7947(4) .8197(4) .89212(18) .0479(16) Uani ? ? 1.00000 ? ? C1131 .7977(5) .7522(5) .9365(2) .068(2) Uani ? ? 1.00000 ? ? C1132 .9131(6) .7638(6) .9451(2) .086(3) Uani ? ? 1.00000 ? ? C1133 .7041(6) .6288(5) .9150(3) .082(3) Uani ? ? 1.00000 ? ? C1134 .7863(8) .8001(7) .9970(3) .110(4) Uani ? ? 1.00000 ? ? C114 .7895(4) .9157(4) .90873(18) .0529(17) Uani ? ? 1.00000 ? ? C115 .7870(4) .9801(4) .8709(2) .0551(18) Uani ? ? 1.00000 ? ? C1151 .7813(5) 1.0860(5) .8928(2) .064(2) Uani ? ? 1.00000 ? ? C1152 .8978(7) 1.1899(5) .8999(3) .103(4) Uani ? ? 1.00000 ? ? C1153 .7442(10) 1.0882(8) .9503(3) .145(6) Uani ? ? 1.00000 ? ? C1154 .7035(6) 1.0939(6) .8487(3) .090(3) Uani ? ? 1.00000 ? ? C116 .7929(4) .9458(4) .81382(18) .0511(17) Uani ? ? 1.00000 ? ? C120 .8761(4) .7753(4) .65322(17) .0488(16) Uani ? ? 1.00000 ? ? C121 .9681(4) .7719(4) .62604(17) .0476(16) Uani ? ? 1.00000 ? ? C122 1.0046(3) .7004(3) .64016(17) .0453(15) Uani ? ? 1.00000 ? ? O122 .9695(3) .6496(3) .68257(12) .0501(12) Uani ? ? 1.00000 ? ? C123 1.0760(3) .6834(3) .60659(17) .0463(15) Uani ? ? 1.00000 ? ? C1231 1.1136(4) .6015(4) .61639(18) .0521(17) Uani ? ? 1.00000 ? ? C1232 1.0108(4) .4839(4) .6063(2) .065(2) Uani ? ? 1.00000 ? ? C1233 1.1782(4) .6383(5) .6797(2) .066(2) Uani ? ? 1.00000 ? ? C1234 1.1893(5) .5964(6) .5760(3) .078(3) Uani ? ? 1.00000 ? ? C124 1.1088(3) .7422(4) .56282(18) .0492(16) Uani ? ? 1.00000 ? ? C125 1.0749(4) .8146(4) .54956(18) .0519(17) Uani ? ? 1.00000 ? ? C1251 1.1093(5) .8751(5) .5007(2) .069(2) Uani ? ? 1.00000 ? ? C1252 1.0038(7) .8380(7) .4557(3) .103(4) Uani ? ? 1.00000 ? ? C1253 1.1851(5) .8473(5) .4685(3) .079(3) Uani ? ? 1.00000 ? ? C1254 1.1725(8) 1.0017(6) .5262(4) .119(5) Uani ? ? 1.00000 ? ? C126 1.0034(4) .8265(4) .5823(2) .0539(18) Uani ? ? 1.00000 ? ? C11 1.0023(4) .9071(4) .7464(2) .0542(18) Uani ? ? 1.00000 ? ? C12 1.0251(5) 1.0156(5) .7296(3) .084(3) Uani ? ? 1.00000 ? ? O13 1.1225(4) 1.1074(4) .7662(3) .114(3) Uani ? ? 1.00000 ? ? C14 1.1075(8) 1.1525(7) .8192(5) .136(5) Uani ? ? 1.00000 ? ? N21 .8800(3) .4881(3) .79339(13) .0411(11) Uani ? ? 1.00000 ? ? C21 .9403(4) .4447(4) .76038(19) .0542(18) Uani ? ? 1.00000 ? ? C210 .9290(3) .5304(3) .85746(17) .0468(15) Uani ? ? 1.00000 ? ? C211 1.0536(4) .6082(3) .87393(17) .0481(15) Uani ? ? 1.00000 ? ? C212 1.1040(3) .7090(3) .85624(17) .0430(14) Uani ? ? 1.00000 ? ? O212 1.0409(2) .7290(2) .81989(12) .0491(11) Uani ? ? 1.00000 ? ? C213 1.2191(4) .7876(3) .87911(18) .0485(16) Uani ? ? 1.00000 ? ? C2131 1.2757(4) .9024(4) .8654(2) .0560(18) Uani ? ? 1.00000 ? ? C2132 1.2723(5) .8900(5) .7993(2) .070(2) Uani ? ? 1.00000 ? ? C2133 1.2177(5) .9649(4) .8857(2) .069(2) Uani ? ? 1.00000 ? ? C2134 1.3992(5) .9764(5) .8969(3) .088(3) Uani ? ? 1.00000 ? ? C214 1.2764(3) .7562(4) .91584(19) .0526(16) Uani ? ? 1.00000 ? ? C215 1.2292(4) .6553(4) .93265(19) .0562(18) Uani ? ? 1.00000 ? ? C2151 1.2947(5) .6237(5) .9733(2) .069(2) Uani ? ? 1.00000 ? ? C2152 1.2810(8) .5120(7) .9444(3) .119(5) Uani ? ? 1.00000 ? ? C2153 1.4171(7) .7128(9) .9908(5) .157(6) Uani ? ? 1.00000 ? ? C2154 1.2475(7) .6093(6) 1.0286(3) .094(3) Uani ? ? 1.00000 ? ? C216 1.1159(4) .5832(3) .9107(2) .0534(17) Uani ? ? 1.00000 ? ? C220 .7589(3) .4037(3) .78805(18) .0504(15) Uani ? ? 1.00000 ? ? C221 .6958(4) .3405(3) .7267(2) .0534(16) Uani ? ? 1.00000 ? ? C222 .6834(3) .3972(3) .68613(17) .0478(15) Uani ? ? 1.00000 ? ? O222 .7320(2) .5092(2) .70317(12) .0484(11) Uani ? ? 1.00000 ? ? C223 .6227(4) .3351(4) .62846(19) .0581(19) Uani ? ? 1.00000 ? ? C2231 .6119(4) .3923(4) .5800(2) .063(2) Uani ? ? 1.00000 ? ? C2232 .7301(5) .4626(5) .5677(2) .078(3) Uani ? ? 1.00000 ? ? C2233 .5682(5) .4693(5) .5989(3) .079(3) Uani ? ? 1.00000 ? ? C2234 .5358(7) .3074(5) .5226(3) .106(3) Uani ? ? 1.00000 ? ? C224 .5731(5) .2188(4) .6161(2) .070(2) Uani ? ? 1.00000 ? ? C225 .5813(5) .1606(4) .6561(2) .075(2) Uani ? ? 1.00000 ? ? C2251 .5239(6) .0314(4) .6413(2) .110(4) Uani ? ? 1.00000 ? ? C2252 .6320(11) .0061(10) .6502(6) .089(4) Uiso ? ? .50000 ? ? C2253 .4596(11) -.0174(10) .6834(6) .089(4) Uiso ? ? .50000 ? ? C2254 .4621(13) -.0226(12) .5796(7) .104(5) Uiso ? ? .50000 ? ? C2252' .567(2) -.0049(17) .6801(11) .288(19) Uiso ? ? .50000 ? ? C2253' .391(2) -.0132(16) .6464(9) .167(8) Uiso ? ? .50000 ? ? C2254' .5192(12) -.0166(11) .5803(6) .093(4) Uiso ? ? .50000 ? ? C226 .6434(4) .2231(4) .7118(2) .064(2) Uani ? ? 1.00000 ? ? C22 .9492(6) .3512(5) .7804(3) .087(3) Uani ? ? 1.00000 ? ? O23 1.0052(8) .3155(6) .7484(3) .179(5) Uani ? ? 1.00000 ? ? C24 .9459(15) .2375(11) .6992(5) .215(10) Uani ? ? 1.00000 ? ? O101 .5172(3) .6750(4) .7165(2) .090(2) Uani ? ? 1.00000 ? ? C101 .4839(6) .7344(6) .7553(4) .103(4) Uani ? ? 1.00000 ? ? C1011 .5053(8) .6901(8) .6596(4) .124(5) Uani ? ? 1.00000 ? ? C102 .4922(7) .7104(8) .8133(4) .110(4) Uani ? ? 1.00000 ? ? O102 .4360(5) .5939(5) .8120(2) .102(3) Uani ? ? 1.00000 ? ? C1021 .3189(7) .5374(9) .7936(4) .125(5) Uani ? ? 1.00000 ? ? O201 .4555(7) .3325(6) .7927(4) .161(5) Uani ? ? 1.00000 ? ? C2011 .4683(11) .3159(14) .8442(8) .272(12) Uani ? ? 1.00000 ? ? C201 .3913(11) .2426(11) .7423(11) .219(13) Uani ? ? 1.00000 ? ? O202 .3633(5) .3503(6) .6867(3) .143(4) Uani ? ? 1.00000 ? ? C2021 .2827(9) .3529(17) .6466(7) .263(12) Uani ? ? 1.00000 ? ? C202 .3211(16) .2541(12) .7020(8) .256(12) Uani ? ? 1.00000 ? ? H110a .79203 .86638 .71122 .05500 Uiso ? ? 1.00000 ? ? H110b .73043 .74260 .71553 .05500 Uiso ? ? 1.00000 ? ? H1132a .91916 .72347 .97239 .12400 Uiso ? ? 1.00000 ? ? H1132b .92466 .73340 .90841 .12400 Uiso ? ? 1.00000 ? ? H1132c .97206 .84033 .95849 .12400 Uiso ? ? 1.00000 ? ? H1133a .70610 .58769 .94223 .12100 Uiso ? ? 1.00000 ? ? H1133b .63288 .62333 .90937 .12100 Uiso ? ? 1.00000 ? ? H1133c .71192 .59647 .87812 .12100 Uiso ? ? 1.00000 ? ? H1134a .78659 .75843 1.02421 .15200 Uiso ? ? 1.00000 ? ? H1134b .84124 .87706 1.01245 .15200 Uiso ? ? 1.00000 ? ? H1134c .71306 .79593 .99340 .15200 Uiso ? ? 1.00000 ? ? H114 .78888 .93929 .94887 .06500 Uiso ? ? 1.00000 ? ? H1152a .89907 1.25718 .91333 .15000 Uiso ? ? 1.00000 ? ? H1152b .95130 1.18757 .92813 .15000 Uiso ? ? 1.00000 ? ? H1152c .92379 1.19109 .86383 .15000 Uiso ? ? 1.00000 ? ? H1153a .73786 1.15296 .96164 .20100 Uiso ? ? 1.00000 ? ? H1153b .66909 1.02300 .94580 .20100 Uiso ? ? 1.00000 ? ? H1153c .79229 1.08680 .97922 .20100 Uiso ? ? 1.00000 ? ? H1154a .69957 1.15917 .86085 .12600 Uiso ? ? 1.00000 ? ? H1154b .73027 1.09880 .81163 .12600 Uiso ? ? 1.00000 ? ? H1154c .62976 1.02960 .83925 .12600 Uiso ? ? 1.00000 ? ? H116 .79322 .99041 .78695 .05900 Uiso ? ? 1.00000 ? ? H120a .86360 .82884 .63877 .06000 Uiso ? ? 1.00000 ? ? H120b .81015 .70327 .63901 .06000 Uiso ? ? 1.00000 ? ? H1232a 1.03386 .43211 .61182 .09400 Uiso ? ? 1.00000 ? ? H1232b .96280 .48268 .63141 .09400 Uiso ? ? 1.00000 ? ? H1232c .97068 .45974 .56624 .09400 Uiso ? ? 1.00000 ? ? H1233a 1.20234 .58879 .68743 .09900 Uiso ? ? 1.00000 ? ? H1233b 1.24337 .71251 .68692 .09900 Uiso ? ? 1.00000 ? ? H1233c 1.13324 .64158 .70724 .09900 Uiso ? ? 1.00000 ? ? H1234a 1.21160 .54429 .58387 .11100 Uiso ? ? 1.00000 ? ? H1234b 1.15409 .57385 .53643 .11100 Uiso ? ? 1.00000 ? ? H1234c 1.25647 .66863 .58323 .11100 Uiso ? ? 1.00000 ? ? H124 1.15605 .72995 .54007 .06200 Uiso ? ? 1.00000 ? ? H1252a 1.02482 .87609 .42448 .14900 Uiso ? ? 1.00000 ? ? H1252b .96631 .75977 .43899 .14900 Uiso ? ? 1.00000 ? ? H1252c .95545 .85635 .47309 .14900 Uiso ? ? 1.00000 ? ? H1253a 1.20610 .88736 .43835 .11400 Uiso ? ? 1.00000 ? ? H1253b 1.25244 .86842 .49475 .11400 Uiso ? ? 1.00000 ? ? H1253c 1.14808 .76928 .45082 .11400 Uiso ? ? 1.00000 ? ? H1254a 1.19516 1.04090 .49718 .18100 Uiso ? ? 1.00000 ? ? H1254b 1.12619 1.02192 .54593 .18100 Uiso ? ? 1.00000 ? ? H1254c 1.23780 1.02361 .55519 .18100 Uiso ? ? 1.00000 ? ? H126 .97635 .87439 .57380 .06600 Uiso ? ? 1.00000 ? ? H11a 1.00601 .91934 .78747 .06700 Uiso ? ? 1.00000 ? ? H11b 1.05964 .89412 .73729 .06700 Uiso ? ? 1.00000 ? ? H12a 1.03170 1.00979 .68921 .10300 Uiso ? ? 1.00000 ? ? H12b .96096 1.02440 .73240 .10300 Uiso ? ? 1.00000 ? ? H14a 1.17408 1.21456 .84333 .19100 Uiso ? ? 1.00000 ? ? H14b 1.05523 1.17891 .81208 .19100 Uiso ? ? 1.00000 ? ? H14c 1.07363 1.09697 .84114 .19100 Uiso ? ? 1.00000 ? ? H21a .90281 .41700 .72000 .06700 Uiso ? ? 1.00000 ? ? H21b 1.01396 .50544 .76326 .06700 Uiso ? ? 1.00000 ? ? H22a .87483 .28893 .77653 .11200 Uiso ? ? 1.00000 ? ? H22b .98516 .37741 .82038 .11200 Uiso ? ? 1.00000 ? ? H210a .89527 .56883 .87449 .05800 Uiso ? ? 1.00000 ? ? H210b .91088 .46733 .87336 .05800 Uiso ? ? 1.00000 ? ? H2132a 1.30571 .95947 .78972 .10900 Uiso ? ? 1.00000 ? ? H2132b 1.30677 .84944 .78612 .10900 Uiso ? ? 1.00000 ? ? H2132c 1.19421 .84604 .77880 .10900 Uiso ? ? 1.00000 ? ? H2133a 1.25287 1.03692 .87773 .10200 Uiso ? ? 1.00000 ? ? H2133b 1.14158 .92312 .86621 .10200 Uiso ? ? 1.00000 ? ? H2133c 1.22149 .97355 .92691 .10200 Uiso ? ? 1.00000 ? ? H2134a 1.43090 1.04740 .88733 .12100 Uiso ? ? 1.00000 ? ? H2134b 1.40300 .98757 .93798 .12100 Uiso ? ? 1.00000 ? ? H2134c 1.43843 .94108 .88536 .12100 Uiso ? ? 1.00000 ? ? H214 1.35649 .80867 .93093 .06300 Uiso ? ? 1.00000 ? ? H2152a 1.32409 .49302 .96991 .16700 Uiso ? ? 1.00000 ? ? H2152b 1.20707 .45363 .93434 .16700 Uiso ? ? 1.00000 ? ? H2152c 1.31273 .51861 .90927 .16700 Uiso ? ? 1.00000 ? ? H2153a 1.45961 .69685 1.01580 .23400 Uiso ? ? 1.00000 ? ? H2153b 1.45021 .72593 .95597 .23400 Uiso ? ? 1.00000 ? ? H2153c 1.42800 .78594 1.00944 .23400 Uiso ? ? 1.00000 ? ? H2154a 1.28604 .58748 1.05394 .13300 Uiso ? ? 1.00000 ? ? H2154b 1.25115 .67440 1.04803 .13300 Uiso ? ? 1.00000 ? ? H2154c 1.16954 .54860 1.01793 .13300 Uiso ? ? 1.00000 ? ? H216 1.07937 .51394 .92287 .06400 Uiso ? ? 1.00000 ? ? H220a .75402 .34993 .80944 .06500 Uiso ? ? 1.00000 ? ? H220b .72416 .44078 .80478 .06500 Uiso ? ? 1.00000 ? ? H2232a .72557 .49942 .53785 .11200 Uiso ? ? 1.00000 ? ? H2232b .77989 .51693 .60171 .11200 Uiso ? ? 1.00000 ? ? H2232c .75688 .41478 .55391 .11200 Uiso ? ? 1.00000 ? ? H2233a .56266 .50451 .56897 .11100 Uiso ? ? 1.00000 ? ? H2233b .49311 .42514 .60627 .11100 Uiso ? ? 1.00000 ? ? H2233c .61328 .52452 .63392 .11100 Uiso ? ? 1.00000 ? ? H2234a .53215 .34571 .49411 .15600 Uiso ? ? 1.00000 ? ? H2234b .56311 .26019 .50904 .15600 Uiso ? ? 1.00000 ? ? H2234c .46212 .26181 .52936 .15600 Uiso ? ? 1.00000 ? ? H224 .53009 .17498 .57724 .08300 Uiso ? ? 1.00000 ? ? H2252a .60249 -.07250 .64171 .26900 Uiso ? ? .50000 ? ? H2252b .67294 .03906 .68932 .26900 Uiso ? ? .50000 ? ? H2252c .68006 .03757 .62430 .26900 Uiso ? ? .50000 ? ? H2253a .42610 -.09652 .67239 .11000 Uiso ? ? .50000 ? ? H2253b .40299 .00072 .68471 .11000 Uiso ? ? .50000 ? ? H2253c .50721 .01127 .72085 .11000 Uiso ? ? .50000 ? ? H2254a .42855 -.10149 .57314 .11800 Uiso ? ? .50000 ? ? H2254b .51236 .00412 .55422 .11800 Uiso ? ? .50000 ? ? H2254c .40571 -.00486 .57254 .11800 Uiso ? ? .50000 ? ? H2252'a .52515 -.08558 .66912 .11000 Uiso ? ? .50000 ? ? H2252'b .55226 .01706 .71786 .11000 Uiso ? ? .50000 ? ? H2252'c .64096 .02376 .68181 .11000 Uiso ? ? .50000 ? ? H2253'a .34852 -.09220 .63632 .18200 Uiso ? ? .50000 ? ? H2253'b .36009 .01241 .61749 .18200 Uiso ? ? .50000 ? ? H2253'c .38686 .01680 .68322 .18200 Uiso ? ? .50000 ? ? H2254'a .48429 -.09558 .57411 .11800 Uiso ? ? .50000 ? ? H2254'b .59447 .01301 .57452 .11800 Uiso ? ? .50000 ? ? H2254'c .48046 .00236 .55478 .11800 Uiso ? ? .50000 ? ? H226 .65319 .18612 .74134 .07800 Uiso ? ? 1.00000 ? ? H24a .98603 .21305 .67733 .29300 Uiso ? ? 1.00000 ? ? H24b .88469 .17013 .70777 .29300 Uiso ? ? 1.00000 ? ? H24c .90837 .26148 .67360 .29300 Uiso ? ? 1.00000 ? ? H1011a .43284 .67772 .64744 .16900 Uiso ? ? 1.00000 ? ? H1011b .56021 .76487 .65989 .16900 Uiso ? ? 1.00000 ? ? H1011c .51554 .63881 .63348 .16900 Uiso ? ? 1.00000 ? ? H101a .40884 .71232 .74058 .11600 Uiso ? ? 1.00000 ? ? H101b .53103 .81256 .75905 .11600 Uiso ? ? 1.00000 ? ? H102a .46073 .74377 .83716 .12900 Uiso ? ? 1.00000 ? ? H102b .56885 .74285 .83000 .12900 Uiso ? ? 1.00000 ? ? H1021a .30115 .53694 .75384 .17100 Uiso ? ? 1.00000 ? ? H1021b .29084 .57550 .81695 .17100 Uiso ? ? 1.00000 ? ? H1021c .28673 .46300 .79777 .17100 Uiso ? ? 1.00000 ? ? H2011a .54475 .34199 .85796 .41400 Uiso ? ? 1.00000 ? ? H2011b .42436 .23851 .84238 .41400 Uiso ? ? 1.00000 ? ? H2011c .44504 .35610 .87011 .41400 Uiso ? ? 1.00000 ? ? H201a .44246 .23027 .72510 .22000 Uiso ? ? 1.00000 ? ? H201b .34579 .17964 .75825 .22000 Uiso ? ? 1.00000 ? ? H202a .30356 .19585 .66814 .26500 Uiso ? ? 1.00000 ? ? H202b .25799 .23851 .71699 .26500 Uiso ? ? 1.00000 ? ? H2021a .23104 .36223 .66672 .35500 Uiso ? ? 1.00000 ? ? H2021b .31814 .41581 .62891 .35500 Uiso ? ? 1.00000 ? ? H2021c .24096 .28676 .61662 .35500 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 Yb .04716(10) .04077(9) .03999(9) .02504(8) .01106(7) .01440(7) K .0596(6) .0738(7) .0784(7) .0368(6) .0186(5) .0249(6) N11 .0455(17) .0492(17) .0391(16) .0310(15) .0147(13) .0152(13) C110 .056(2) .063(2) .0375(18) .042(2) .0154(16) .0167(17) C111 .050(2) .049(2) .041(2) .0285(18) .0127(16) .0118(16) C112 .049(2) .046(2) .0399(19) .0266(17) .0096(16) .0112(16) O112 .0615(17) .0459(14) .0459(15) .0333(14) .0189(13) .0166(12) C113 .059(2) .055(2) .044(2) .037(2) .0153(18) .0202(18) C1131 .113(4) .073(3) .048(3) .066(3) .019(3) .026(2) C1132 .122(5) .105(5) .059(3) .084(4) -.003(3) .014(3) C1133 .113(5) .075(4) .078(4) .054(4) .038(3) .041(3) C1134 .217(9) .127(6) .052(3) .126(7) .051(4) .045(4) C114 .067(3) .053(2) .045(2) .036(2) .0101(19) .0086(18) C115 .065(3) .062(3) .056(2) .044(2) .016(2) .018(2) C1151 .094(4) .073(3) .052(3) .061(3) .021(2) .017(2) C1152 .107(5) .059(3) .123(6) .040(4) -.004(4) -.004(4) C1153 .301(13) .161(8) .098(5) .189(9) .107(7) .070(5) C1154 .133(6) .096(4) .083(4) .091(5) .020(4) .018(3) C116 .068(3) .059(2) .045(2) .043(2) .0188(19) .0190(18) C120 .062(2) .062(2) .042(2) .042(2) .0200(18) .0192(18) C121 .056(2) .059(2) .043(2) .037(2) .0183(17) .0205(18) C122 .054(2) .047(2) .043(2) .0306(18) .0109(16) .0133(16) O122 .0597(17) .0600(17) .0438(15) .0370(15) .0167(13) .0218(13) C123 .049(2) .054(2) .045(2) .0338(19) .0077(16) .0123(17) C1231 .067(3) .062(3) .044(2) .045(2) .0143(19) .0131(19) C1232 .070(3) .051(2) .076(3) .037(2) .004(2) .010(2) C1233 .068(3) .088(4) .060(3) .055(3) .005(2) .017(3) C1234 .100(4) .109(5) .072(3) .083(4) .037(3) .036(3) C124 .047(2) .056(2) .045(2) .0260(19) .0153(17) .0141(18) C125 .063(3) .056(2) .046(2) .033(2) .0205(19) .0250(19) C1251 .094(4) .081(3) .060(3) .055(3) .040(3) .041(3) C1252 .126(6) .178(8) .076(4) .112(6) .051(4) .077(5) C1253 .091(4) .091(4) .066(3) .047(3) .039(3) .034(3) C1254 .187(9) .076(4) .125(6) .073(5) .083(6) .054(4) C126 .066(3) .059(3) .059(3) .044(2) .024(2) .026(2) C11 .054(2) .049(2) .063(3) .027(2) .013(2) .020(2) C12 .080(4) .064(3) .096(4) .027(3) .021(3) .024(3) O13 .085(3) .067(3) .163(5) .019(2) .042(3) .014(3) C14 .133(8) .099(6) .155(8) .054(6) .039(6) -.005(6) N21 .0467(17) .0363(15) .0381(16) .0204(14) .0053(13) .0091(12) C21 .068(3) .052(2) .052(2) .036(2) .021(2) .0161(19) C210 .055(2) .043(2) .039(2) .0240(18) .0038(16) .0091(15) C211 .054(2) .049(2) .041(2) .0266(19) .0078(17) .0140(17) C212 .048(2) .0402(18) .042(2) .0235(16) .0096(16) .0110(15) O212 .0520(16) .0427(14) .0482(16) .0216(13) .0019(12) .0147(12) C213 .053(2) .048(2) .047(2) .0290(19) .0070(17) .0119(17) C2131 .057(2) .049(2) .056(3) .022(2) .012(2) .018(2) C2132 .073(3) .069(3) .062(3) .028(3) .024(3) .027(3) C2133 .093(4) .042(2) .066(3) .033(2) .010(3) .012(2) C2134 .070(4) .062(3) .096(4) .010(3) -.004(3) .024(3) C214 .044(2) .053(2) .051(2) .0214(18) -.0010(17) .0085(18) C215 .070(3) .060(3) .046(2) .041(2) .003(2) .0081(19) C2151 .081(3) .087(4) .055(3) .056(3) .003(2) .021(3) C2152 .194(9) .148(7) .088(5) .144(7) .015(5) .028(5) C2153 .078(5) .173(9) .217(10) .052(5) -.022(6) .112(8) C2154 .136(6) .127(6) .062(3) .099(5) .012(4) .029(4) C216 .063(3) .043(2) .055(2) .027(2) .007(2) .0170(18) C220 .046(2) .047(2) .044(2) .0150(17) .0016(16) .0117(17) C221 .049(2) .040(2) .056(2) .0126(17) .0060(18) .0132(18) C222 .046(2) .045(2) .042(2) .0176(17) .0037(16) .0070(16) O222 .0534(16) .0441(14) .0473(15) .0257(13) .0056(12) .0110(12) C223 .071(3) .055(2) .045(2) .031(2) .008(2) .0098(19) C2231 .074(3) .061(3) .045(2) .031(2) .000(2) .011(2) C2232 .090(4) .091(4) .062(3) .047(3) .032(3) .028(3) C2233 .079(4) .092(4) .077(4) .051(3) .007(3) .031(3) C2234 .136(6) .074(4) .063(4) .034(4) -.033(4) .002(3) C224 .089(4) .052(3) .050(3) .029(3) -.001(2) .003(2) C225 .089(4) .045(2) .060(3) .019(2) -.006(3) .003(2) C2251 .158(7) .048(3) .065(4) .022(4) -.024(4) -.002(3) C226 .065(3) .042(2) .062(3) .014(2) .005(2) .012(2) C22 .133(6) .085(4) .079(4) .082(4) .024(4) .021(3) O23 .277(10) .174(7) .169(7) .183(7) .043(7) .023(5) C24 .43(2) .186(11) .104(7) .221(14) .071(10) .004(7) O101 .079(3) .095(3) .111(3) .057(3) .008(2) .028(3) C101 .088(5) .094(5) .140(7) .062(4) .012(4) .020(5) C1011 .126(7) .151(8) .136(7) .094(6) .017(6) .066(6) C102 .111(6) .119(6) .115(6) .077(5) .012(5) .009(5) O102 .106(4) .131(4) .096(3) .079(4) .025(3) .033(3) C1021 .099(6) .172(9) .108(6) .070(6) .025(5) .045(6) O201 .195(7) .105(5) .174(7) .052(5) .081(6) .073(5) C2011 .153(11) .262(17) .31(2) .005(11) .000(12) .217(17) C201 .105(9) .084(7) .44(3) .042(7) .023(12) .029(12) O202 .073(3) .146(6) .145(5) .019(3) .021(3) .002(4) C2021 .068(6) .39(2) .193(13) .060(10) -.035(7) -.026(14) C202 .228(18) .114(10) .217(18) -.056(11) .107(15) -.024(10) # 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 N11 . . 2.528(4) ? Yb O112 . . 2.174(4) ? Yb O122 . . 2.116(3) ? Yb N21 . . 2.508(4) ? Yb O212 . . 2.132(3) ? Yb O222 . . 2.171(2) ? K O112 . . 2.905(3) ? K O222 . . 2.827(4) ? K O101 . . 2.799(6) ? K O102 . . 2.804(7) ? K O201 . . 2.741(8) ? K O202 . . 2.813(5) ? N11 C110 . . 1.493(7) ? N11 C120 . . 1.470(5) ? N11 C11 . . 1.474(4) ? C110 C111 . . 1.507(6) ? C110 H110a . . .957 ? C110 H110b . . .954 ? C111 C112 . . 1.410(7) ? C111 C116 . . 1.370(8) ? C112 O112 . . 1.341(6) ? C112 C113 . . 1.427(6) ? C113 C1131 . . 1.543(8) ? C113 C114 . . 1.390(8) ? C1131 C1132 . . 1.538(12) ? C1131 C1133 . . 1.535(7) ? C1131 C1134 . . 1.540(9) ? C1132 H1132a . . .952 ? C1132 H1132b . . .970 ? C1132 H1132c . . .956 ? C1133 H1133a . . .943 ? C1133 H1133b . . .960 ? C1133 H1133c . . .960 ? C1134 H1134a . . .943 ? C1134 H1134b . . .950 ? C1134 H1134c . . .996 ? C114 C115 . . 1.388(8) ? C114 H114 . . .958 ? C115 C1151 . . 1.544(10) ? C115 C116 . . 1.386(7) ? C1151 C1152 . . 1.538(8) ? C1151 C1153 . . 1.507(11) ? C1151 C1154 . . 1.498(11) ? C1152 H1152a . . .943 ? C1152 H1152b . . .975 ? C1152 H1152c . . .959 ? C1153 H1153a . . .961 ? C1153 H1153b . . .981 ? C1153 H1153c . . .926 ? C1154 H1154a . . .951 ? C1154 H1154b . . .987 ? C1154 H1154c . . .955 ? C116 H116 . . .966 ? C120 C121 . . 1.516(8) ? C120 H120a . . .963 ? C120 H120b . . .953 ? C121 C122 . . 1.410(8) ? C121 C126 . . 1.377(7) ? C122 O122 . . 1.324(5) ? C122 C123 . . 1.423(7) ? C123 C1231 . . 1.530(9) ? C123 C124 . . 1.405(6) ? C1231 C1232 . . 1.532(6) ? C1231 C1233 . . 1.539(7) ? C1231 C1234 . . 1.517(9) ? C1232 H1232a . . .956 ? C1232 H1232b . . .937 ? C1232 H1232c . . .970 ? C1233 H1233a . . .949 ? C1233 H1233b . . .967 ? C1233 H1233c . . .962 ? C1234 H1234a . . .968 ? C1234 H1234b . . .941 ? C1234 H1234c . . .963 ? C124 C125 . . 1.390(9) ? C124 H124 . . .955 ? C125 C1251 . . 1.527(8) ? C125 C126 . . 1.384(8) ? C1251 C1252 . . 1.537(10) ? C1251 C1253 . . 1.531(11) ? C1251 C1254 . . 1.528(9) ? C1252 H1252a . . .969 ? C1252 H1252b . . .949 ? C1252 H1252c . . .944 ? C1253 H1253a . . .962 ? C1253 H1253b . . .960 ? C1253 H1253c . . .951 ? C1254 H1254a . . .936 ? C1254 H1254b . . .960 ? C1254 H1254c . . .969 ? C126 H126 . . .964 ? C11 C12 . . 1.535(9) ? C11 H11a . . .952 ? C11 H11b . . .946 ? C12 O13 . . 1.402(6) ? C12 H12a . . .965 ? C12 H12b . . .975 ? O13 C14 . . 1.395(13) ? C14 H14a . . .948 ? C14 H14b . . .987 ? C14 H14c . . .963 ? N21 C21 . . 1.479(7) ? N21 C210 . . 1.495(5) ? N21 C220 . . 1.499(5) ? C21 C22 . . 1.531(11) ? C21 H21a . . .962 ? C21 H21b . . .952 ? C210 C211 . . 1.504(6) ? C210 H210a . . .949 ? C210 H210b . . .953 ? C211 C212 . . 1.402(6) ? C211 C216 . . 1.383(8) ? C212 O212 . . 1.337(6) ? C212 C213 . . 1.419(5) ? C213 C2131 . . 1.525(7) ? C213 C214 . . 1.397(8) ? C2131 C2132 . . 1.539(7) ? C2131 C2133 . . 1.523(10) ? C2131 C2134 . . 1.542(7) ? C2132 H2132a . . .937 ? C2132 H2132b . . .951 ? C2132 H2132c . . .977 ? C2133 H2133a . . .951 ? C2133 H2133b . . .950 ? C2133 H2133c . . .956 ? C2134 H2134a . . .954 ? C2134 H2134b . . .953 ? C2134 H2134c . . .940 ? C214 C215 . . 1.392(7) ? C214 H214 . . .980 ? C215 C2151 . . 1.534(10) ? C215 C216 . . 1.384(6) ? C2151 C2152 . . 1.524(13) ? C2151 C2153 . . 1.510(9) ? C2151 C2154 . . 1.523(9) ? C2152 H2152a . . .973 ? C2152 H2152b . . .928 ? C2152 H2152c . . .978 ? C2153 H2153a . . .932 ? C2153 H2153b . . .986 ? C2153 H2153c . . .984 ? C2154 H2154a . . .955 ? C2154 H2154b . . .934 ? C2154 H2154c . . .976 ? C216 H216 . . .965 ? C220 C221 . . 1.500(5) ? C220 H220a . . .960 ? C220 H220b . . .944 ? C221 C222 . . 1.399(7) ? C221 C226 . . 1.406(6) ? C222 O222 . . 1.345(5) ? C222 C223 . . 1.419(5) ? C223 C2231 . . 1.545(8) ? C223 C224 . . 1.397(7) ? C2231 C2232 . . 1.548(8) ? C2231 C2233 . . 1.521(11) ? C2231 C2234 . . 1.536(7) ? C2232 H2232a . . .960 ? C2232 H2232b . . .943 ? C2232 H2232c . . .952 ? C2233 H2233a . . .949 ? C2233 H2233b . . .977 ? C2233 H2233c . . .949 ? C2234 H2234a . . .946 ? C2234 H2234b . . .949 ? C2234 H2234c . . .960 ? C224 C225 . . 1.385(9) ? C224 H224 . . .966 ? C225 C2251 . . 1.547(7) ? C225 C226 . . 1.388(6) ? C2251 C2252 . . 1.73(2) ? C2251 C2253 . . 1.441(15) ? C2251 C2254 . . 1.487(15) ? C2251 C2252' . . 1.35(3) ? C2251 C2253' . . 1.67(3) ? C2251 C2254' . . 1.472(16) ? C2252 H2252a . . .950 ? C2252 H2252b . . .949 ? C2252 H2252c . . .951 ? C2253 H2253a . . .950 ? C2253 H2253b . . .950 ? C2253 H2253c . . .949 ? C2254 H2254a . . .949 ? C2254 H2254b . . .947 ? C2254 H2254c . . .95 ? C2252' H2252'a . . .96 ? C2252' H2252'b . . .97 ? C2252' H2252'c . . .90 ? C2253' H2253'a . . .943 ? C2253' H2253'b . . .99 ? C2253' H2253'c . . .93 ? C2254' H2254'a . . .950 ? C2254' H2254'b . . .961 ? C2254' H2254'c . . .932 ? C226 H226 . . .977 ? C22 O23 . . 1.352(15) ? C22 H22a . . .962 ? C22 H22b . . .949 ? O23 C24 . . 1.327(12) ? C24 H24a . . .95 ? C24 H24b . . .989 ? C24 H24c . . .971 ? O101 C101 . . 1.410(11) ? O101 C1011 . . 1.406(12) ? C101 C102 . . 1.475(14) ? C101 H101a . . .950 ? C101 H101b . . .950 ? C1011 H1011a . . .950 ? C1011 H1011b . . .952 ? C1011 H1011c . . .951 ? C102 O102 . . 1.427(11) ? C102 H102a . . .950 ? C102 H102b . . .950 ? O102 C1021 . . 1.411(10) ? C1021 H1021a . . .950 ? C1021 H1021b . . .951 ? C1021 H1021c . . .946 ? O201 C2011 . . 1.29(2) ? O201 C201 . . 1.42(2) ? C2011 H2011a . . .949 ? C2011 H2011b . . .946 ? C2011 H2011c . . .96 ? C201 C202 . . 1.39(3) ? C201 H201a . . .93 ? C201 H201b . . .97 ? O202 C2021 . . 1.43(2) ? O202 C202 . . 1.32(2) ? C2021 H2021a . . .954 ? C2021 H2021b . . .97 ? C2021 H2021c . . .942 ? C202 H202a . . .964 ? C202 H202b . . .92 ? 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 N11 Yb O112 . . . 78.70(12) ? N11 Yb O122 . . . 77.61(14) ? N11 Yb N21 . . . 177.21(12) ? N11 Yb O212 . . . 103.73(11) ? N11 Yb O222 . . . 99.30(12) ? O112 Yb O122 . . . 155.88(15) ? O112 Yb N21 . . . 98.85(13) ? O112 Yb O212 . . . 94.13(12) ? O112 Yb O222 . . . 87.95(11) ? O122 Yb N21 . . . 104.73(14) ? O122 Yb O212 . . . 95.78(12) ? O122 Yb O222 . . . 91.45(10) ? N21 Yb O212 . . . 77.68(11) ? N21 Yb O222 . . . 79.21(12) ? O212 Yb O222 . . . 156.85(13) ? O112 K O222 . . . 63.51(9) ? O112 K O101 . . . 96.19(11) ? O112 K O102 . . . 106.97(12) ? O112 K O201 . . . 120.7(2) ? O112 K O202 . . . 168.12(18) ? O222 K O101 . . . 111.47(13) ? O222 K O102 . . . 167.46(13) ? O222 K O201 . . . 105.4(2) ? O222 K O202 . . . 104.63(17) ? O101 K O102 . . . 59.79(17) ? O101 K O201 . . . 136.7(2) ? O101 K O202 . . . 87.7(2) ? O102 K O201 . . . 86.4(3) ? O102 K O202 . . . 84.7(2) ? O201 K O202 . . . 61.1(2) ? Yb N11 C110 . . . 108.9(2) ? Yb N11 C120 . . . 107.7(3) ? Yb N11 C11 . . . 105.9(3) ? C110 N11 C120 . . . 106.3(3) ? C110 N11 C11 . . . 113.1(4) ? C120 N11 C11 . . . 114.7(3) ? N11 C110 C111 . . . 116.4(4) ? N11 C110 H110a . . . 107.6 ? N11 C110 H110b . . . 108.2 ? C111 C110 H110a . . . 107.7 ? C111 C110 H110b . . . 108.2 ? H110a C110 H110b . . . 108.5 ? C110 C111 C112 . . . 118.8(4) ? C110 C111 C116 . . . 120.2(5) ? C112 C111 C116 . . . 120.8(4) ? C111 C112 O112 . . . 118.7(4) ? C111 C112 C113 . . . 118.1(5) ? O112 C112 C113 . . . 123.2(4) ? Yb O112 K . . . 102.97(9) ? Yb O112 C112 . . . 135.8(3) ? K O112 C112 . . . 104.7(3) ? C112 C113 C1131 . . . 120.6(5) ? C112 C113 C114 . . . 118.1(5) ? C1131 C113 C114 . . . 121.3(4) ? C113 C1131 C1132 . . . 107.8(5) ? C113 C1131 C1133 . . . 110.9(4) ? C113 C1131 C1134 . . . 111.8(6) ? C1132 C1131 C1133 . . . 111.1(6) ? C1132 C1131 C1134 . . . 106.3(5) ? C1133 C1131 C1134 . . . 108.8(5) ? C1131 C1132 H1132a . . . 111.0 ? C1131 C1132 H1132b . . . 110.2 ? C1131 C1132 H1132c . . . 111.8 ? H1132a C1132 H1132b . . . 107.6 ? H1132a C1132 H1132c . . . 108.8 ? H1132b C1132 H1132c . . . 107.3 ? C1131 C1133 H1133a . . . 110.8 ? C1131 C1133 H1133b . . . 109.8 ? C1131 C1133 H1133c . . . 110.0 ? H1133a C1133 H1133b . . . 109.2 ? H1133a C1133 H1133c . . . 109.2 ? H1133b C1133 H1133c . . . 107.8 ? C1131 C1134 H1134a . . . 112.4 ? C1131 C1134 H1134b . . . 112.9 ? C1131 C1134 H1134c . . . 109.2 ? H1134a C1134 H1134b . . . 110.1 ? H1134a C1134 H1134c . . . 106.2 ? H1134b C1134 H1134c . . . 105.7 ? C113 C114 C115 . . . 124.0(4) ? C113 C114 H114 . . . 117.7 ? C115 C114 H114 . . . 118.3 ? C114 C115 C1151 . . . 120.9(4) ? C114 C115 C116 . . . 116.4(5) ? C1151 C115 C116 . . . 122.7(5) ? C115 C1151 C1152 . . . 108.7(6) ? C115 C1151 C1153 . . . 112.2(6) ? C115 C1151 C1154 . . . 110.7(4) ? C1152 C1151 C1153 . . . 109.2(5) ? C1152 C1151 C1154 . . . 107.0(6) ? C1153 C1151 C1154 . . . 109.0(8) ? C1151 C1152 H1152a . . . 112.2 ? C1151 C1152 H1152b . . . 109.5 ? C1151 C1152 H1152c . . . 111.2 ? H1152a C1152 H1152b . . . 107.9 ? H1152a C1152 H1152c . . . 109.3 ? H1152b C1152 H1152c . . . 106.6 ? C1151 C1153 H1153a . . . 110.1 ? C1151 C1153 H1153b . . . 109.6 ? C1151 C1153 H1153c . . . 111.6 ? H1153a C1153 H1153b . . . 106.0 ? H1153a C1153 H1153c . . . 110.6 ? H1153b C1153 H1153c . . . 108.9 ? C1151 C1154 H1154a . . . 112.3 ? C1151 C1154 H1154b . . . 110.0 ? C1151 C1154 H1154c . . . 112.9 ? H1154a C1154 H1154b . . . 106.3 ? H1154a C1154 H1154c . . . 109.0 ? H1154b C1154 H1154c . . . 106.0 ? C111 C116 C115 . . . 122.7(5) ? C111 C116 H116 . . . 119.4 ? C115 C116 H116 . . . 117.9 ? N11 C120 C121 . . . 118.4(4) ? N11 C120 H120a . . . 107.4 ? N11 C120 H120b . . . 108.4 ? C121 C120 H120a . . . 106.7 ? C121 C120 H120b . . . 107.5 ? H120a C120 H120b . . . 108.2 ? C120 C121 C122 . . . 119.0(4) ? C120 C121 C126 . . . 119.4(5) ? C122 C121 C126 . . . 121.0(5) ? C121 C122 O122 . . . 119.5(5) ? C121 C122 C123 . . . 118.0(4) ? O122 C122 C123 . . . 122.6(5) ? Yb O122 C122 . . . 144.5(4) ? C122 C123 C1231 . . . 121.4(4) ? C122 C123 C124 . . . 117.9(5) ? C1231 C123 C124 . . . 120.7(5) ? C123 C1231 C1232 . . . 109.4(5) ? C123 C1231 C1233 . . . 109.3(4) ? C123 C1231 C1234 . . . 112.7(5) ? C1232 C1231 C1233 . . . 108.9(4) ? C1232 C1231 C1234 . . . 108.6(4) ? C1233 C1231 C1234 . . . 107.9(5) ? C1231 C1232 H1232a . . . 109.8 ? C1231 C1232 H1232b . . . 111.4 ? C1231 C1232 H1232c . . . 109.2 ? H1232a C1232 H1232b . . . 110.1 ? H1232a C1232 H1232c . . . 107.3 ? H1232b C1232 H1232c . . . 108.9 ? C1231 C1233 H1233a . . . 111.6 ? C1231 C1233 H1233b . . . 110.1 ? C1231 C1233 H1233c . . . 111.3 ? H1233a C1233 H1233b . . . 108.1 ? H1233a C1233 H1233c . . . 108.5 ? H1233b C1233 H1233c . . . 107.1 ? C1231 C1234 H1234a . . . 110.1 ? C1231 C1234 H1234b . . . 111.9 ? C1231 C1234 H1234c . . . 109.9 ? H1234a C1234 H1234b . . . 108.7 ? H1234a C1234 H1234c . . . 106.9 ? H1234b C1234 H1234c . . . 109.1 ? C123 C124 C125 . . . 124.4(5) ? C123 C124 H124 . . . 117.7 ? C125 C124 H124 . . . 117.9 ? C124 C125 C1251 . . . 123.4(5) ? C124 C125 C126 . . . 115.8(4) ? C1251 C125 C126 . . . 120.8(6) ? C125 C1251 C1252 . . . 108.8(5) ? C125 C1251 C1253 . . . 112.5(6) ? C125 C1251 C1254 . . . 109.7(5) ? C1252 C1251 C1253 . . . 107.4(5) ? C1252 C1251 C1254 . . . 110.6(8) ? C1253 C1251 C1254 . . . 107.9(6) ? C1251 C1252 H1252a . . . 109.4 ? C1251 C1252 H1252b . . . 110.2 ? C1251 C1252 H1252c . . . 110.8 ? H1252a C1252 H1252b . . . 107.9 ? H1252a C1252 H1252c . . . 108.4 ? H1252b C1252 H1252c . . . 110.1 ? C1251 C1253 H1253a . . . 110.5 ? C1251 C1253 H1253b . . . 110.9 ? C1251 C1253 H1253c . . . 110.7 ? H1253a C1253 H1253b . . . 107.7 ? H1253a C1253 H1253c . . . 108.4 ? H1253b C1253 H1253c . . . 108.6 ? C1251 C1254 H1254a . . . 111.4 ? C1251 C1254 H1254b . . . 109.8 ? C1251 C1254 H1254c . . . 109.6 ? H1254a C1254 H1254b . . . 109.8 ? H1254a C1254 H1254c . . . 109.1 ? H1254b C1254 H1254c . . . 107.0 ? C121 C126 C125 . . . 123.0(6) ? C121 C126 H126 . . . 118.6 ? C125 C126 H126 . . . 118.3 ? N11 C11 C12 . . . 115.8(5) ? N11 C11 H11a . . . 108.3 ? N11 C11 H11b . . . 108.3 ? C12 C11 H11a . . . 107.2 ? C12 C11 H11b . . . 107.5 ? H11a C11 H11b . . . 109.6 ? C11 C12 O13 . . . 110.0(6) ? C11 C12 H12a . . . 109.6 ? C11 C12 H12b . . . 109.2 ? O13 C12 H12a . . . 110.8 ? O13 C12 H12b . . . 111.0 ? H12a C12 H12b . . . 106.2 ? C12 O13 C14 . . . 115.1(6) ? O13 C14 H14a . . . 114.0 ? O13 C14 H14b . . . 110.2 ? O13 C14 H14c . . . 111.7 ? H14a C14 H14b . . . 106.6 ? H14a C14 H14c . . . 108.6 ? H14b C14 H14c . . . 105.4 ? Yb N21 C21 . . . 107.9(3) ? Yb N21 C210 . . . 108.3(2) ? Yb N21 C220 . . . 107.7(3) ? C21 N21 C210 . . . 112.7(4) ? C21 N21 C220 . . . 114.3(3) ? C210 N21 C220 . . . 105.8(3) ? N21 C21 C22 . . . 115.8(5) ? N21 C21 H21a . . . 107.9 ? N21 C21 H21b . . . 108.2 ? C22 C21 H21a . . . 108.4 ? C22 C21 H21b . . . 108.0 ? H21a C21 H21b . . . 108.3 ? N21 C210 C211 . . . 115.8(4) ? N21 C210 H210a . . . 107.8 ? N21 C210 H210b . . . 107.9 ? C211 C210 H210a . . . 108.2 ? C211 C210 H210b . . . 107.8 ? H210a C210 H210b . . . 109.3 ? C210 C211 C212 . . . 120.2(5) ? C210 C211 C216 . . . 118.8(4) ? C212 C211 C216 . . . 120.8(4) ? C211 C212 O212 . . . 118.8(3) ? C211 C212 C213 . . . 118.7(5) ? O212 C212 C213 . . . 122.4(4) ? Yb O212 C212 . . . 142.5(2) ? C212 C213 C2131 . . . 120.8(5) ? C212 C213 C214 . . . 117.0(4) ? C2131 C213 C214 . . . 122.1(4) ? C213 C2131 C2132 . . . 110.4(4) ? C213 C2131 C2133 . . . 109.9(4) ? C213 C2131 C2134 . . . 112.3(5) ? C2132 C2131 C2133 . . . 110.0(5) ? C2132 C2131 C2134 . . . 107.4(4) ? C2133 C2131 C2134 . . . 106.8(4) ? C2131 C2132 H2132a . . . 112.0 ? C2131 C2132 H2132b . . . 110.4 ? C2131 C2132 H2132c . . . 108.4 ? H2132a C2132 H2132b . . . 110.5 ? H2132a C2132 H2132c . . . 108.3 ? H2132b C2132 H2132c . . . 107.1 ? C2131 C2133 H2133a . . . 110.5 ? C2131 C2133 H2133b . . . 109.5 ? C2131 C2133 H2133c . . . 109.4 ? H2133a C2133 H2133b . . . 109.4 ? H2133a C2133 H2133c . . . 108.9 ? H2133b C2133 H2133c . . . 109.0 ? C2131 C2134 H2134a . . . 109.4 ? C2131 C2134 H2134b . . . 108.7 ? C2131 C2134 H2134c . . . 109.6 ? H2134a C2134 H2134b . . . 108.9 ? H2134a C2134 H2134c . . . 110.0 ? H2134b C2134 H2134c . . . 110.1 ? C213 C214 C215 . . . 125.3(4) ? C213 C214 H214 . . . 117.9 ? C215 C214 H214 . . . 116.8 ? C214 C215 C2151 . . . 123.9(4) ? C214 C215 C216 . . . 115.4(5) ? C2151 C215 C216 . . . 120.8(5) ? C215 C2151 C2152 . . . 110.5(5) ? C215 C2151 C2153 . . . 112.0(7) ? C215 C2151 C2154 . . . 109.1(6) ? C2152 C2151 C2153 . . . 109.8(8) ? C2152 C2151 C2154 . . . 107.1(6) ? C2153 C2151 C2154 . . . 108.1(6) ? C2151 C2152 H2152a . . . 110.4 ? C2151 C2152 H2152b . . . 113.0 ? C2151 C2152 H2152c . . . 109.6 ? H2152a C2152 H2152b . . . 109.3 ? H2152a C2152 H2152c . . . 105.3 ? H2152b C2152 H2152c . . . 108.9 ? C2151 C2153 H2153a . . . 114.5 ? C2151 C2153 H2153b . . . 110.5 ? C2151 C2153 H2153c . . . 111.2 ? H2153a C2153 H2153b . . . 108.0 ? H2153a C2153 H2153c . . . 108.2 ? H2153b C2153 H2153c . . . 103.9 ? C2151 C2154 H2154a . . . 110.2 ? C2151 C2154 H2154b . . . 111.8 ? C2151 C2154 H2154c . . . 108.7 ? H2154a C2154 H2154b . . . 110.4 ? H2154a C2154 H2154c . . . 106.9 ? H2154b C2154 H2154c . . . 108.7 ? C211 C216 C215 . . . 122.7(4) ? C211 C216 H216 . . . 119.5 ? C215 C216 H216 . . . 117.8 ? N21 C220 C221 . . . 114.7(4) ? N21 C220 H220a . . . 108.1 ? N21 C220 H220b . . . 108.8 ? C221 C220 H220a . . . 107.5 ? C221 C220 H220b . . . 108.5 ? H220a C220 H220b . . . 109.1 ? C220 C221 C222 . . . 120.2(4) ? C220 C221 C226 . . . 118.9(5) ? C222 C221 C226 . . . 120.7(4) ? C221 C222 O222 . . . 118.4(3) ? C221 C222 C223 . . . 118.9(4) ? O222 C222 C223 . . . 122.6(5) ? Yb O222 K . . . 105.54(12) ? Yb O222 C222 . . . 136.0(3) ? K O222 C222 . . . 100.6(3) ? C222 C223 C2231 . . . 122.1(4) ? C222 C223 C224 . . . 117.7(5) ? C2231 C223 C224 . . . 120.1(4) ? C223 C2231 C2232 . . . 107.0(5) ? C223 C2231 C2233 . . . 111.8(5) ? C223 C2231 C2234 . . . 112.5(5) ? C2232 C2231 C2233 . . . 109.1(5) ? C2232 C2231 C2234 . . . 107.5(5) ? C2233 C2231 C2234 . . . 108.8(6) ? C2231 C2232 H2232a . . . 108.6 ? C2231 C2232 H2232b . . . 110.7 ? C2231 C2232 H2232c . . . 109.9 ? H2232a C2232 H2232b . . . 109.2 ? H2232a C2232 H2232c . . . 108.5 ? H2232b C2232 H2232c . . . 109.9 ? C2231 C2233 H2233a . . . 110.9 ? C2231 C2233 H2233b . . . 109.4 ? C2231 C2233 H2233c . . . 112.1 ? H2233a C2233 H2233b . . . 107.2 ? H2233a C2233 H2233c . . . 109.7 ? H2233b C2233 H2233c . . . 107.3 ? C2231 C2234 H2234a . . . 109.8 ? C2231 C2234 H2234b . . . 110.5 ? C2231 C2234 H2234c . . . 109.1 ? H2234a C2234 H2234b . . . 109.9 ? H2234a C2234 H2234c . . . 108.9 ? H2234b C2234 H2234c . . . 108.7 ? C223 C224 C225 . . . 124.2(4) ? C223 C224 H224 . . . 118.9 ? C225 C224 H224 . . . 116.9 ? C224 C225 C2251 . . . 123.0(4) ? C224 C225 C226 . . . 117.2(5) ? C2251 C225 C226 . . . 119.8(5) ? C225 C2251 C2252 . . . 104.9(6) ? C225 C2251 C2253 . . . 112.7(7) ? C225 C2251 C2254 . . . 113.0(8) ? C225 C2251 C2252' . . . 112.6(9) ? C225 C2251 C2253' . . . 104.2(9) ? C225 C2251 C2254' . . . 112.8(7) ? C2252 C2251 C2253 . . . 104.0(9) ? C2252 C2251 C2254 . . . 107.4(10) ? C2253 C2251 C2254 . . . 113.8(8) ? C2252' C2251 C2253' . . . 108.4(14) ? C2252' C2251 C2254' . . . 112.5(15) ? C2253' C2251 C2254' . . . 105.5(9) ? C2251 C2252 H2252a . . . 109.4 ? C2251 C2252 H2252b . . . 109.5 ? C2251 C2252 H2252c . . . 109.4 ? C2251 C2252 H2252'c . . . 90.9(15) ? H2252a C2252 H2252b . . . 109.5 ? H2252a C2252 H2252c . . . 109.4 ? H2252b C2252 H2252c . . . 109.5 ? C2251 C2253 H2253a . . . 109.4 ? C2251 C2253 H2253b . . . 109.4 ? C2251 C2253 H2253c . . . 109.4 ? H2253a C2253 H2253b . . . 109.5 ? H2253a C2253 H2253c . . . 109.5 ? H2253b C2253 H2253c . . . 109.5 ? C2251 C2254 H2254a . . . 109.4 ? C2251 C2254 H2254b . . . 109.5 ? C2251 C2254 H2254c . . . 109.3 ? H2254a C2254 H2254b . . . 109.7 ? H2254a C2254 H2254c . . . 109.4 ? H2254b C2254 H2254c . . . 109.6 ? C2251 C2252' H2252'a . . . 108 ? C2251 C2252' H2252'b . . . 107 ? C2251 C2252' H2252'c . . . 112 ? H2252'a C2252' H2252'b . . . 106 ? H2252'a C2252' H2252'c . . . 112 ? H2252'b C2252' H2252'c . . . 111 ? C2251 C2253' H2253'a . . . 110 ? C2251 C2253' H2253'b . . . 108.0 ? C2251 C2253' H2253'c . . . 111.3 ? H2253'a C2253' H2253'b . . . 106.8 ? H2253'a C2253' H2253'c . . . 112 ? H2253'b C2253' H2253'c . . . 108 ? C2251 C2254' H2254'a . . . 108.9 ? C2251 C2254' H2254'b . . . 108.2 ? C2251 C2254' H2254'c . . . 110.2 ? H2254'a C2254' H2254'b . . . 108.5 ? H2254'a C2254' H2254'c . . . 111.0 ? H2254'b C2254' H2254'c . . . 110.0 ? C221 C226 C225 . . . 121.1(5) ? C221 C226 H226 . . . 118.6 ? C225 C226 H226 . . . 120.3 ? C21 C22 O23 . . . 112.7(6) ? C21 C22 H22a . . . 108.2 ? C21 C22 H22b . . . 108.9 ? O23 C22 H22a . . . 108.5 ? O23 C22 H22b . . . 109.8 ? H22a C22 H22b . . . 108.6 ? C22 O23 C24 . . . 116.4(12) ? O23 C24 H24a . . . 115.5 ? O23 C24 H24b . . . 109.9 ? O23 C24 H24c . . . 111.7 ? H24a C24 H24b . . . 106.5 ? H24a C24 H24c . . . 107.9 ? H24b C24 H24c . . . 104.6 ? K O101 C101 . . . 117.7(5) ? K O101 C1011 . . . 129.3(6) ? C101 O101 C1011 . . . 112.4(8) ? O101 C101 C102 . . . 110.0(9) ? O101 C101 H101a . . . 109.4 ? O101 C101 H101b . . . 109.4 ? C102 C101 H101a . . . 109.3 ? C102 C101 H101b . . . 109.2 ? H101a C101 H101b . . . 109.5 ? O101 C1011 H1011a . . . 109.8 ? O101 C1011 H1011b . . . 108.6 ? O101 C1011 H1011c . . . 109.7 ? H1011a C1011 H1011b . . . 109.7 ? H1011a C1011 H1011c . . . 109.4 ? H1011b C1011 H1011c . . . 109.7 ? C101 C102 O102 . . . 114.2(6) ? C101 C102 H102a . . . 108.4 ? C101 C102 H102b . . . 108.4 ? O102 C102 H102a . . . 108.2 ? O102 C102 H102b . . . 108.2 ? H102a C102 H102b . . . 109.5 ? K O102 C102 . . . 101.9(5) ? K O102 C1021 . . . 122.6(5) ? C102 O102 C1021 . . . 114.1(9) ? O102 C1021 H1021a . . . 109.3 ? O102 C1021 H1021b . . . 109.2 ? O102 C1021 H1021c . . . 109.5 ? H1021a C1021 H1021b . . . 109.4 ? H1021a C1021 H1021c . . . 109.8 ? H1021b C1021 H1021c . . . 109.7 ? K O201 C2011 . . . 128.6(7) ? K O201 C201 . . . 108.2(10) ? C2011 O201 C201 . . . 122.3(13) ? O201 C2011 H2011a . . . 109.4 ? O201 C2011 H2011b . . . 109.5 ? O201 C2011 H2011c . . . 109 ? H2011a C2011 H2011b . . . 110 ? H2011a C2011 H2011c . . . 109.5 ? H2011b C2011 H2011c . . . 109.3 ? O201 C201 C202 . . . 117.6(15) ? O201 C201 H201a . . . 105.7 ? O201 C201 H201b . . . 104 ? C202 C201 H201a . . . 112 ? C202 C201 H201b . . . 108.5 ? H201a C201 H201b . . . 109.3 ? K O202 C2021 . . . 130.2(9) ? K O202 C202 . . . 115.9(9) ? C2021 O202 C202 . . . 111.8(12) ? O202 C2021 H2021a . . . 110.0 ? O202 C2021 H2021b . . . 111.0 ? O202 C2021 H2021c . . . 113 ? H2021a C2021 H2021b . . . 107 ? H2021a C2021 H2021c . . . 107.2 ? H2021b C2021 H2021c . . . 108.5 ? C201 C202 O202 . . . 117.1(13) ? C201 C202 H202a . . . 103 ? C201 C202 H202b . . . 106.9 ? O202 C202 H202a . . . 108.4 ? O202 C202 H202b . . . 111 ? H202a C202 H202b . . . 110.5 ? _exptl_crystal_F_000 1498 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 19 _reflns_limit_k_min -18 _reflns_limit_k_max 16 _reflns_limit_l_min -32 _reflns_limit_l_max 32 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 12.137 _diffrn_reflns_av_sigmaI/netI .048 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 298(2) _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 18 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .054 _refine_ls_wR_factor_all .114 _refine_ls_goodness_of_fit_all 1.135 _refine_ls_shift/su_mean .001 #===END #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_edbb _database_code_depnum_ccdc_archive 'CCDC 621007' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C43 H72 F3 N2 O8 S1 Yb1' _chemical_formula_moiety 'C39 H62 F3 N2 O6 Yb, C4 H10 O2' _chemical_formula_weight 1007.15 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_21_21_21 _symmetry_space_group_name_Hall p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 11.1100(10) _cell_length_b 14.063(2) _cell_length_c 31.033(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 4848.6(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.38 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6616 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 33.38 _cell_measurement_temperature 170 _exptl_absorpt_coefficient_mu 2.032 _exptl_crystal_description prism _exptl_crystal_size_max .45 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .16 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .74 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 27152 _reflns_number_total 15915 _reflns_Friedel_coverage .850 _reflns_number_gt 14028 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 32.21 _diffrn_reflns_theta_full 32.2 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .031 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .058 _refine_ls_wR_factor_ref .093 _refine_ls_goodness_of_fit_ref 1.451 _refine_ls_number_reflns 7777 _refine_ls_number_parameters 538 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/(sig^2(F) + .001F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .013 _refine_diff_density_min -2.578 _refine_diff_density_max 2.379 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack -.007(14) # 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 ? 0 172 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 288 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 12 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 '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' S ? 0 4 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' Yb ? 0 4 -.884 5.548 '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 .19198(3) .57859(3) .294110(11) .02026(12) Uani ? ? 1.00000 ? ? N1 .4119(5) .5742(6) .2951(2) .023(3) Uani ? ? 1.00000 ? ? C10 .4535(7) .6057(7) .3392(3) .027(4) Uani ? ? 1.00000 ? ? C11 .4231(7) .5427(6) .3772(3) .023(4) Uani ? ? 1.00000 ? ? C12 .3017(8) .5220(5) .3883(2) .021(3) Uani ? ? 1.00000 ? ? O12 .2154(4) .5432(5) .3591(2) .025(3) Uani ? ? 1.00000 ? ? C13 .2789(7) .4780(6) .4286(3) .020(4) Uani ? ? 1.00000 ? ? C131 .1496(7) .4579(7) .4429(3) .025(4) Uani ? ? 1.00000 ? ? C132 .0875(8) .3871(8) .4126(3) .033(5) Uani ? ? 1.00000 ? ? C133 .0769(9) .5507(8) .4445(4) .038(5) Uani ? ? 1.00000 ? ? C134 .1444(8) .4144(11) .4887(3) .041(5) Uani ? ? 1.00000 ? ? C14 .3757(8) .4574(6) .4550(3) .024(4) Uani ? ? 1.00000 ? ? C15 .4957(8) .4768(7) .4446(3) .026(4) Uani ? ? 1.00000 ? ? C151 .5973(8) .4531(7) .4763(3) .032(5) Uani ? ? 1.00000 ? ? C152 .5782(15) .5170(16) .5178(6) .051(10) Uani ? ? .707(12) ? ? C153 .5897(15) .3506(12) .4918(6) .044(9) Uani ? ? .707(12) ? ? C154 .7196(13) .4723(15) .4596(6) .051(10) Uani ? ? .707(12) ? ? C152' .568(3) .402(2) .5123(10) .026(6) Uiso ? ? .293(12) ? ? C153' .695(4) .388(2) .4478(11) .037(7) Uiso ? ? .293(12) ? ? C154' .666(3) .542(2) .4843(11) .034(7) Uiso ? ? .293(12) ? ? C16 .5167(8) .5210(7) .4054(3) .027(4) Uani ? ? 1.00000 ? ? C20 .4651(8) .6441(7) .2646(3) .026(4) Uani ? ? 1.00000 ? ? C21 .4363(8) .6323(7) .2174(3) .027(4) Uani ? ? 1.00000 ? ? C22 .3164(7) .6343(5) .2029(3) .023(3) Uani ? ? 1.00000 ? ? O22 .2281(5) .6313(5) .2326(2) .028(3) Uani ? ? 1.00000 ? ? C23 .2923(8) .6380(6) .1582(3) .026(4) Uani ? ? 1.00000 ? ? C231 .1614(8) .6487(7) .1418(3) .027(4) Uani ? ? 1.00000 ? ? C232 .1587(10) .6567(10) .0926(4) .045(6) Uani ? ? 1.00000 ? ? C233 .1042(10) .7385(10) .1606(4) .048(7) Uani ? ? 1.00000 ? ? C234 .0855(9) .5622(10) .1540(3) .042(6) Uani ? ? 1.00000 ? ? C24 .3897(8) .6338(7) .1305(3) .026(4) Uani ? ? 1.00000 ? ? C25 .5111(8) .6280(6) .1438(3) .026(4) Uani ? ? 1.00000 ? ? C251 .6104(8) .6218(8) .1100(3) .034(5) Uani ? ? 1.00000 ? ? C252 .7349(9) .6238(10) .1298(4) .045(6) Uani ? ? 1.00000 ? ? C253 .6007(12) .7064(13) .0789(5) .063(9) Uani ? ? 1.00000 ? ? C255 .5969(11) .5314(11) .0841(4) .050(7) Uani ? ? 1.00000 ? ? C26 .5304(7) .6287(6) .1877(3) .025(4) Uani ? ? 1.00000 ? ? C1 .4609(7) .4773(7) .2856(3) .029(4) Uani ? ? 1.00000 ? ? C2 .3743(10) .3975(8) .2960(5) .025(5) Uani ? ? .707(12) ? ? N3 .2545(6) .4139(6) .2742(3) .029(4) Uani ? ? 1.00000 ? ? C31 .2593(13) .3978(11) .2290(4) .034(7) Uani ? ? .707(12) ? ? C32 .1726(10) .3380(9) .2932(5) .030(6) Uani ? ? .707(12) ? ? C2' .388(3) .424(3) .2557(10) .031(6) Uiso ? ? .293(12) ? ? C31' .183(4) .380(3) .2324(12) .042(8) Uiso ? ? .293(12) ? ? C32' .244(4) .348(3) .3060(13) .038(8) Uiso ? ? .293(12) ? ? O101 .0055(6) .5030(6) .2729(3) .047(5) Uani ? ? 1.00000 ? ? O102 -.0059(6) .6613(5) .2956(3) .044(4) Uani ? ? 1.00000 ? ? O103 -.1625(6) .6006(8) .2468(3) .056(5) Uani ? ? 1.00000 ? ? C101 -.1649(9) .5481(13) .3260(4) .064(9) Uani ? ? 1.00000 ? ? S101 -.07549(18) .5820(2) .27971(7) .0311(10) Uani ? ? 1.00000 ? ? F101 -.2364(7) .6190(10) .3371(3) .098(8) Uani ? ? 1.00000 ? ? F102 -.0972(7) .5239(11) .3583(3) .120(9) Uani ? ? 1.00000 ? ? F103 -.2339(7) .4730(8) .3158(4) .107(8) Uani ? ? 1.00000 ? ? O201 .2206(6) .7371(5) .3176(2) .035(4) Uani ? ? 1.00000 ? ? C202 .2047(12) .8184(7) .2892(5) .049(6) Uani ? ? 1.00000 ? ? C203 .110(2) .879(2) .3199(9) .050(6) Uiso ? ? .50000 ? ? C203' .206(3) .898(2) .3103(9) .060(7) Uiso ? ? .50000 ? ? C204 .122(3) .857(2) .3594(11) .051(7) Uiso ? ? .50000 ? ? C204' .164(4) .864(4) .3593(16) .089(15) Uiso ? ? .50000 ? ? C205 .1888(18) .7648(10) .3606(4) .063(8) Uani ? ? 1.00000 ? ? C01 .170(11) .654(12) .611(3) .34(4) Uiso ? ? .50000 ? ? O02 .192(5) .681(4) .5681(17) .197(17) Uiso ? ? .50000 ? ? C03 .305(8) .649(6) .556(3) .36(4) Uiso ? ? .50000 ? ? C04 .372(7) .729(8) .5333(18) .25(5) Uiso ? ? .50000 ? ? O05 .310(5) .754(7) .496(2) .36(4) Uiso ? ? .50000 ? ? C06 .389(5) .759(4) .4627(16) .114(17) Uiso ? ? .50000 ? ? C01' .110(5) .657(6) .636(2) .207(18) Uiso ? ? .50000 ? ? O02' .163(4) .699(4) .6014(17) .20(2) Uiso ? ? .50000 ? ? C03' .293(4) .678(3) .6011(13) .132(19) Uiso ? ? .50000 ? ? C04' .354(4) .734(3) .5641(14) .13(2) Uiso ? ? .50000 ? ? O05' .315(6) .696(4) .5237(14) .21(2) Uiso ? ? .50000 ? ? C06' .382(6) .743(5) .4888(16) .14(2) Uiso ? ? .50000 ? ? H10a .41886 .66632 .34456 .03400 Uiso ? ? 1.00000 ? ? H10b .53861 .61139 .33812 .03400 Uiso ? ? 1.00000 ? ? H132a .00761 .37600 .42227 .05000 Uiso ? ? 1.00000 ? ? H132b .13090 .32889 .41251 .05000 Uiso ? ? 1.00000 ? ? H132c .08560 .41256 .38426 .05000 Uiso ? ? 1.00000 ? ? H133a -.00312 .53729 .45343 .05800 Uiso ? ? 1.00000 ? ? H133b .07557 .57884 .41667 .05800 Uiso ? ? 1.00000 ? ? H133c .11322 .59332 .46436 .05800 Uiso ? ? 1.00000 ? ? H134a .06289 .40300 .49636 .06200 Uiso ? ? 1.00000 ? ? H134b .17943 .45734 .50869 .06200 Uiso ? ? 1.00000 ? ? H134c .18763 .35613 .48903 .06200 Uiso ? ? 1.00000 ? ? H14 .35968 .42821 .48202 .03000 Uiso ? ? 1.00000 ? ? H152a .63989 .50380 .53814 .08100 Uiso ? ? .707(12) ? ? H152b .50201 .50302 .53024 .08100 Uiso ? ? .707(12) ? ? H152c .58108 .58213 .50993 .08100 Uiso ? ? .707(12) ? ? H153a .65381 .33843 .51134 .06600 Uiso ? ? .707(12) ? ? H153b .59581 .30892 .46788 .06600 Uiso ? ? .707(12) ? ? H153c .51500 .34083 .50599 .06600 Uiso ? ? .707(12) ? ? H154a .77743 .45601 .48088 .08200 Uiso ? ? .707(12) ? ? H154b .72675 .53800 .45279 .08200 Uiso ? ? .707(12) ? ? H154c .73313 .43556 .43439 .08200 Uiso ? ? .707(12) ? ? H152'a .63834 .39244 .52913 .03900 Uiso ? ? .293(12) ? ? H152'b .53512 .34280 .50408 .03900 Uiso ? ? .293(12) ? ? H152'c .51054 .43686 .52867 .03900 Uiso ? ? .293(12) ? ? H153'a .76093 .37027 .46570 .05500 Uiso ? ? .293(12) ? ? H153'b .72359 .42364 .42404 .05500 Uiso ? ? .293(12) ? ? H153'c .65608 .33186 .43765 .05500 Uiso ? ? .293(12) ? ? H154'a .73021 .52870 .50379 .05000 Uiso ? ? .293(12) ? ? H154'b .61479 .58843 .49611 .05000 Uiso ? ? .293(12) ? ? H154'c .69894 .56403 .45778 .05000 Uiso ? ? .293(12) ? ? H16 .59691 .53673 .39749 .03400 Uiso ? ? 1.00000 ? ? H20a .55015 .64065 .26751 .03200 Uiso ? ? 1.00000 ? ? H20b .43824 .70552 .27296 .03200 Uiso ? ? 1.00000 ? ? H232a .07776 .66315 .08311 .06800 Uiso ? ? 1.00000 ? ? H232b .19281 .60095 .08025 .06800 Uiso ? ? 1.00000 ? ? H232c .20378 .71064 .08378 .06800 Uiso ? ? 1.00000 ? ? H233a .02401 .74438 .15030 .07300 Uiso ? ? 1.00000 ? ? H233b .14954 .79255 .15200 .07300 Uiso ? ? 1.00000 ? ? H233c .10354 .73433 .19114 .07300 Uiso ? ? 1.00000 ? ? H234a .00573 .57040 .14365 .06100 Uiso ? ? 1.00000 ? ? H234b .08397 .55578 .18452 .06100 Uiso ? ? 1.00000 ? ? H234c .11955 .50666 .14161 .06100 Uiso ? ? 1.00000 ? ? H24 .37384 .63504 .10041 .03300 Uiso ? ? 1.00000 ? ? H252a .79365 .61977 .10763 .07000 Uiso ? ? 1.00000 ? ? H252b .74375 .57136 .14885 .07000 Uiso ? ? 1.00000 ? ? H252c .74537 .68139 .14532 .07000 Uiso ? ? 1.00000 ? ? H253a .66265 .70213 .05790 .09200 Uiso ? ? 1.00000 ? ? H253b .60884 .76397 .09454 .09200 Uiso ? ? 1.00000 ? ? H253c .52448 .70494 .06502 .09200 Uiso ? ? 1.00000 ? ? H255a .65897 .52809 .06307 .07700 Uiso ? ? 1.00000 ? ? H255b .52077 .53130 .07006 .07700 Uiso ? ? 1.00000 ? ? H255c .60220 .47800 .10270 .07700 Uiso ? ? 1.00000 ? ? H26 .61077 .62658 .19805 .03100 Uiso ? ? 1.00000 ? ? H1a .53208 .46840 .30207 .03700 Uiso ? ? .707(12) ? ? H1b .47995 .47419 .25577 .03700 Uiso ? ? .707(12) ? ? H2a .36254 .39485 .32634 .03400 Uiso ? ? .707(12) ? ? H2b .40714 .33903 .28629 .03400 Uiso ? ? .707(12) ? ? H31a .18220 .40903 .21679 .05300 Uiso ? ? .707(12) ? ? H31b .28273 .33398 .22365 .05300 Uiso ? ? .707(12) ? ? H31c .31626 .43986 .21638 .05300 Uiso ? ? .707(12) ? ? H32a .09460 .34355 .28095 .04600 Uiso ? ? .707(12) ? ? H32b .16776 .34603 .32352 .04600 Uiso ? ? .707(12) ? ? H32c .20459 .27686 .28688 .04600 Uiso ? ? .707(12) ? ? H1'a .46614 .44281 .31183 .03700 Uiso ? ? .293(12) ? ? H1'b .53907 .48425 .27356 .03700 Uiso ? ? .293(12) ? ? H2'a .42122 .36202 .25195 .03900 Uiso ? ? .293(12) ? ? H2'b .38519 .45550 .22875 .03900 Uiso ? ? .293(12) ? ? H31'a .10034 .37182 .23953 .06200 Uiso ? ? .293(12) ? ? H31'b .21538 .32179 .22254 .06200 Uiso ? ? .293(12) ? ? H31'c .19024 .42706 .21061 .06200 Uiso ? ? .293(12) ? ? H32'a .16333 .34538 .31560 .05700 Uiso ? ? .293(12) ? ? H32'b .29548 .36450 .32922 .05700 Uiso ? ? .293(12) ? ? H32'c .26716 .28737 .29495 .05700 Uiso ? ? .293(12) ? ? H202a .17032 .80112 .26231 .06000 Uiso ? ? .50000 ? ? H202b .27782 .85178 .28447 .06000 Uiso ? ? .50000 ? ? H203a .03004 .86500 .31092 .06000 Uiso ? ? .50000 ? ? H203b .12529 .94474 .31642 .06000 Uiso ? ? .50000 ? ? H204a .04514 .84900 .37296 .07800 Uiso ? ? .50000 ? ? H204b .16597 .90416 .37468 .07800 Uiso ? ? .50000 ? ? H205a .26005 .77195 .37724 .08100 Uiso ? ? .50000 ? ? H205b .13960 .71688 .37313 .08100 Uiso ? ? .50000 ? ? H202'a .12967 .81246 .27480 .06100 Uiso ? ? .50000 ? ? H202'b .26801 .81885 .26865 .06100 Uiso ? ? .50000 ? ? H205'a .25376 .75252 .37976 .07900 Uiso ? ? .50000 ? ? H205'b .11960 .73087 .36996 .07900 Uiso ? ? .50000 ? ? H203'a .15091 .94266 .29836 .07500 Uiso ? ? .50000 ? ? H203'b .28444 .92537 .31071 .07500 Uiso ? ? .50000 ? ? H204'a .08069 .87599 .36278 .10700 Uiso ? ? .50000 ? ? H204'b .20884 .89741 .38009 .10700 Uiso ? ? .50000 ? ? H01a .09340 .67507 .61954 .20900 Uiso ? ? .50000 ? ? H01b .23051 .67590 .62900 .20900 Uiso ? ? .50000 ? ? H01c .16967 .58434 .61160 .20900 Uiso ? ? .50000 ? ? H03a .29211 .59664 .53542 .42300 Uiso ? ? .50000 ? ? H03b .34712 .62669 .57930 .42300 Uiso ? ? .50000 ? ? H04a .44930 .70586 .52543 .22500 Uiso ? ? .50000 ? ? H04b .37689 .78023 .55173 .22500 Uiso ? ? .50000 ? ? H06a .34733 .77701 .43686 .14800 Uiso ? ? .50000 ? ? H06b .42534 .69858 .45821 .14800 Uiso ? ? .50000 ? ? H06c .44887 .80479 .46878 .14800 Uiso ? ? .50000 ? ? H01'a .02648 .66999 .63606 .31200 Uiso ? ? .50000 ? ? H01'b .14533 .68117 .66181 .31200 Uiso ? ? .50000 ? ? H01'c .12239 .58986 .63499 .31200 Uiso ? ? .50000 ? ? H03'a .30535 .61188 .59718 .16600 Uiso ? ? .50000 ? ? H03'b .32681 .69725 .62790 .16600 Uiso ? ? .50000 ? ? H04'a .43893 .72742 .56605 .15700 Uiso ? ? .50000 ? ? H04'b .33290 .79920 .56580 .15700 Uiso ? ? .50000 ? ? H06'a .35619 .71871 .46180 .21800 Uiso ? ? .50000 ? ? H06'b .46564 .73096 .49234 .21800 Uiso ? ? .50000 ? ? H06'c .36824 .80979 .48967 .21800 Uiso ? ? .50000 ? ? 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 .01264(10) .02841(13) .01972(13) .00114(15) .00094(14) .00466(15) N1 .021(3) .034(3) .015(3) -.005(3) .004(3) .007(4) C10 .014(3) .042(5) .026(4) -.015(3) -.003(3) .006(3) C11 .019(3) .027(4) .023(4) -.002(3) -.001(3) .006(3) C12 .016(3) .030(3) .016(3) .002(3) -.003(3) -.001(3) O12 .006(2) .049(4) .022(3) -.003(2) .0009(18) -.002(3) C13 .015(3) .025(4) .021(4) -.003(2) -.000(2) .001(3) C131 .016(3) .035(4) .024(4) .001(3) .003(3) .004(3) C132 .013(3) .048(5) .039(5) -.010(3) .001(3) -.001(4) C133 .025(4) .044(6) .045(6) .004(4) .010(4) -.004(4) C134 .020(4) .076(8) .028(5) -.006(5) .002(3) .014(6) C14 .021(4) .031(4) .018(4) -.003(3) -.001(3) .008(3) C15 .016(3) .039(5) .023(4) -.005(3) -.003(3) .001(3) C151 .026(4) .034(4) .037(5) -.002(3) -.011(4) .009(4) C152 .028(7) .082(14) .043(10) .003(8) -.010(7) -.008(9) C153 .036(8) .038(8) .057(11) .003(6) -.015(7) .010(7) C154 .024(7) .089(14) .040(9) -.003(7) -.009(6) .023(9) C16 .019(4) .037(5) .026(4) .001(3) -.002(3) .006(3) C20 .020(4) .033(4) .024(4) -.006(3) -.001(3) .008(3) C21 .026(4) .033(4) .021(4) .001(3) .002(3) .007(3) C22 .018(3) .027(3) .024(4) .000(3) .001(4) .005(3) O22 .017(2) .047(4) .019(3) .008(2) .005(2) .012(3) C23 .024(4) .024(3) .030(4) .005(3) .002(3) .005(3) C231 .024(4) .039(5) .018(4) .005(3) -.004(3) .004(3) C232 .030(5) .076(8) .027(5) .010(5) -.002(4) .007(5) C233 .034(5) .063(8) .047(7) .028(5) -.003(5) .004(6) C234 .021(4) .068(8) .036(5) -.002(5) -.007(4) .007(5) C24 .023(4) .034(4) .022(4) .006(3) .003(3) .004(3) C25 .018(4) .027(4) .032(5) .005(3) .005(3) .004(3) C251 .019(4) .059(6) .024(5) -.001(4) .006(3) -.002(4) C252 .018(4) .085(9) .033(6) -.001(5) .006(4) -.010(6) C253 .044(7) .097(12) .047(8) -.000(7) .019(6) .025(7) C255 .032(6) .071(9) .048(7) -.001(5) .007(5) -.023(6) C26 .015(3) .031(4) .031(4) -.000(3) .005(3) .004(3) C1 .016(3) .036(4) .036(6) .006(3) .006(3) .003(4) C2 .020(5) .026(5) .029(6) .002(4) -.000(5) -.001(5) N3 .023(3) .033(4) .032(4) -.001(3) -.003(3) .002(4) C31 .036(7) .043(8) .023(7) .012(6) -.005(5) -.000(5) C32 .020(5) .041(6) .028(6) -.007(4) -.000(5) .008(6) O101 .016(3) .038(4) .086(6) .003(3) -.003(3) -.005(4) O102 .022(3) .040(4) .071(5) .002(3) -.002(4) -.006(5) O103 .020(3) .098(8) .050(5) .002(4) -.014(3) .012(5) C101 .017(4) .126(15) .048(7) .007(6) .004(4) .031(8) S101 .0172(8) .0393(11) .0367(11) .0022(10) -.0020(7) .0057(11) F101 .032(4) .186(13) .075(6) .018(6) .024(4) -.010(7) F102 .032(4) .265(17) .063(6) .001(6) -.003(4) .083(8) F103 .029(4) .116(8) .174(12) -.016(5) -.003(5) .085(8) O201 .035(4) .029(3) .041(4) .002(3) -.004(3) .002(3) C202 .052(7) .029(4) .065(8) .008(5) -.009(7) .012(5) C205 .085(10) .052(7) .052(7) .021(9) .000(9) -.011(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 Yb N1 . . 2.444(6) ? Yb O12 . . 2.092(6) ? Yb O22 . . 2.087(6) ? Yb N3 . . 2.495(9) ? Yb O101 . . 2.419(7) ? Yb O102 . . 2.487(7) ? Yb O201 . . 2.366(7) ? N1 C10 . . 1.509(12) ? N1 C20 . . 1.489(12) ? N1 C1 . . 1.498(12) ? C10 C11 . . 1.514(12) ? C10 H10a . . .950 ? C10 H10b . . .950 ? C11 C12 . . 1.422(12) ? C11 C16 . . 1.391(12) ? C12 O12 . . 1.354(10) ? C12 C13 . . 1.416(11) ? C13 C131 . . 1.530(11) ? C13 C14 . . 1.384(11) ? C131 C132 . . 1.534(14) ? C131 C133 . . 1.535(14) ? C131 C134 . . 1.547(14) ? C132 H132a . . .950 ? C132 H132b . . .950 ? C132 H132c . . .950 ? C133 H133a . . .950 ? C133 H133b . . .950 ? C133 H133c . . .950 ? C134 H134a . . .950 ? C134 H134b . . .950 ? C134 H134c . . .950 ? C14 C15 . . 1.399(12) ? C14 H14 . . .950 ? C15 C151 . . 1.534(13) ? C15 C16 . . 1.387(13) ? C151 C152 . . 1.59(2) ? C151 C153 . . 1.52(2) ? C151 C154 . . 1.480(18) ? C151 C152' . . 1.36(3) ? C151 C153' . . 1.68(4) ? C151 C154' . . 1.48(4) ? C152 C152' . . 1.62(4) ? C152 C154' . . 1.47(4) ? C152 H152a . . .950 ? C152 H152b . . .951 ? C152 H152c . . .95 ? C153 H153a . . .950 ? C153 H153b . . .950 ? C153 H153c . . .949 ? C154 H154a . . .950 ? C154 H154b . . .95 ? C154 H154c . . .949 ? C152' H152'a . . .95 ? C152' H152'b . . .95 ? C152' H152'c . . .95 ? C153' H153'a . . .95 ? C153' H153'b . . .95 ? C153' H153'c . . .95 ? C154' H154'a . . .95 ? C154' H154'b . . .95 ? C154' H154'c . . .95 ? C16 H16 . . .950 ? C20 C21 . . 1.507(12) ? C20 H20a . . .950 ? C20 H20b . . .950 ? C21 C22 . . 1.407(12) ? C21 C26 . . 1.395(12) ? C22 O22 . . 1.348(10) ? C22 C23 . . 1.412(12) ? C23 C231 . . 1.549(12) ? C23 C24 . . 1.384(13) ? C231 C232 . . 1.532(14) ? C231 C233 . . 1.529(16) ? C231 C234 . . 1.528(16) ? C232 H232a . . .950 ? C232 H232b . . .951 ? C232 H232c . . .950 ? C233 H233a . . .950 ? C233 H233b . . .950 ? C233 H233c . . .950 ? C234 H234a . . .950 ? C234 H234b . . .950 ? C234 H234c . . .950 ? C24 C25 . . 1.414(12) ? C24 H24 . . .950 ? C25 C251 . . 1.525(13) ? C25 C26 . . 1.376(13) ? C251 C252 . . 1.514(14) ? C251 C253 . . 1.54(2) ? C251 C255 . . 1.512(18) ? C252 H252a . . .950 ? C252 H252b . . .951 ? C252 H252c . . .949 ? C253 H253a . . .950 ? C253 H253b . . .949 ? C253 H253c . . .950 ? C255 H255a . . .950 ? C255 H255b . . .950 ? C255 H255c . . .950 ? C26 H26 . . .950 ? C1 C2 . . 1.513(14) ? C1 C2' . . 1.44(3) ? C1 H1a . . .950 ? C1 H1b . . .950 ? C1 H1'a . . .950 ? C1 H1'b . . .950 ? C2 N3 . . 1.510(14) ? C2 H2a . . .951 ? C2 H2b . . .949 ? N3 C31 . . 1.424(16) ? N3 C32 . . 1.520(15) ? N3 C2' . . 1.59(3) ? N3 C31' . . 1.59(4) ? N3 C32' . . 1.36(4) ? C31 H31a . . .950 ? C31 H31b . . .949 ? C31 H31c . . .951 ? C32 H32a . . .950 ? C32 H32b . . .950 ? C32 H32c . . .950 ? C2' H2'a . . .95 ? C2' H2'b . . .95 ? C31' H31'a . . .95 ? C31' H31'b . . .95 ? C31' H31'c . . .95 ? C32' H32'a . . .95 ? C32' H32'b . . .95 ? C32' H32'c . . .95 ? O101 S101 . . 1.445(8) ? O102 S101 . . 1.444(8) ? O103 S101 . . 1.431(8) ? C101 S101 . . 1.810(13) ? C101 F101 . . 1.32(2) ? C101 F102 . . 1.299(16) ? C101 F103 . . 1.34(2) ? O201 C202 . . 1.453(14) ? O201 C205 . . 1.436(16) ? C202 C203 . . 1.65(3) ? C202 C203' . . 1.30(3) ? C202 H202a . . .950 ? C202 H202b . . .950 ? C202 H202'a . . .950 ? C202 H202'b . . .951 ? C203 C204 . . 1.27(4) ? C203 H203a . . .95 ? C203 H203b . . .95 ? C203' C204' . . 1.66(6) ? C203' H203'a . . .95 ? C203' H203'b . . .95 ? C204 C205 . . 1.49(4) ? C204 H204a . . .96 ? C204 H204b . . .95 ? C204' C205 . . 1.42(5) ? C204' H204'a . . .95 ? C204' H204'b . . .94 ? C205 H205a . . .950 ? C205 H205b . . .951 ? C205 H205'a . . .950 ? C205 H205'b . . .950 ? C01 O02 . . 1.41(11) ? C01 H01a . . .94 ? C01 H01b . . .93 ? C01 H01c . . .98 ? O02 C03 . . 1.38(10) ? C03 C04 . . 1.52(12) ? C03 H03a . . .99 ? C03 H03b . . .92 ? C04 O05 . . 1.39(10) ? C04 H04a . . .95 ? C04 H04b . . .92 ? O05 C06 . . 1.36(9) ? C06 H06a . . .96 ? C06 H06b . . .95 ? C06 H06c . . .95 ? C01' O02' . . 1.37(9) ? C01' H01'a . . .94 ? C01' H01'b . . .95 ? C01' H01'c . . .95 ? O02' C03' . . 1.47(7) ? C03' C04' . . 1.55(6) ? C03' H03'a . . .95 ? C03' H03'b . . .95 ? C04' O05' . . 1.43(6) ? C04' H04'a . . .95 ? C04' H04'b . . .95 ? O05' C06' . . 1.47(8) ? C06' H06'a . . .95 ? C06' H06'b . . .95 ? C06' H06'c . . .95 ? 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 N1 Yb O12 . . . 81.8(2) ? N1 Yb O22 . . . 80.2(2) ? N1 Yb N3 . . . 72.7(3) ? N1 Yb O101 . . . 148.0(3) ? N1 Yb O102 . . . 153.5(3) ? N1 Yb O201 . . . 83.4(3) ? O12 Yb O22 . . . 160.4(2) ? O12 Yb N3 . . . 89.0(3) ? O12 Yb O101 . . . 105.3(3) ? O12 Yb O102 . . . 101.7(3) ? O12 Yb O201 . . . 84.9(3) ? O22 Yb N3 . . . 92.9(3) ? O22 Yb O101 . . . 94.1(3) ? O22 Yb O102 . . . 91.2(3) ? O22 Yb O201 . . . 85.5(3) ? N3 Yb O101 . . . 76.3(2) ? N3 Yb O102 . . . 133.2(2) ? N3 Yb O201 . . . 155.9(2) ? O101 Yb O102 . . . 56.9(3) ? O101 Yb O201 . . . 127.8(3) ? O102 Yb O201 . . . 70.9(2) ? Yb N1 C10 . . . 108.1(5) ? Yb N1 C20 . . . 111.9(5) ? Yb N1 C1 . . . 112.6(5) ? C10 N1 C20 . . . 105.2(7) ? C10 N1 C1 . . . 109.6(7) ? C20 N1 C1 . . . 109.3(7) ? N1 C10 C11 . . . 117.8(7) ? N1 C10 H10a . . . 107.3 ? N1 C10 H10b . . . 107.3 ? C11 C10 H10a . . . 107.4 ? C11 C10 H10b . . . 107.4 ? H10a C10 H10b . . . 109.5 ? C10 C11 C12 . . . 121.3(7) ? C10 C11 C16 . . . 116.8(7) ? C12 C11 C16 . . . 120.7(8) ? C11 C12 O12 . . . 117.6(7) ? C11 C12 C13 . . . 118.2(7) ? O12 C12 C13 . . . 124.1(7) ? Yb O12 C12 . . . 141.9(5) ? C12 C13 C131 . . . 120.3(7) ? C12 C13 C14 . . . 118.4(7) ? C131 C13 C14 . . . 121.3(7) ? C13 C131 C132 . . . 111.4(7) ? C13 C131 C133 . . . 110.3(8) ? C13 C131 C134 . . . 112.0(7) ? C132 C131 C133 . . . 109.5(8) ? C132 C131 C134 . . . 106.8(8) ? C133 C131 C134 . . . 106.7(8) ? C131 C132 H132a . . . 109.5 ? C131 C132 H132b . . . 109.5 ? C131 C132 H132c . . . 109.5 ? H132a C132 H132b . . . 109.5 ? H132a C132 H132c . . . 109.5 ? H132b C132 H132c . . . 109.4 ? C131 C133 H133a . . . 109.5 ? C131 C133 H133b . . . 109.4 ? C131 C133 H133c . . . 109.5 ? H133a C133 H133b . . . 109.5 ? H133a C133 H133c . . . 109.5 ? H133b C133 H133c . . . 109.5 ? C131 C134 H134a . . . 109.5 ? C131 C134 H134b . . . 109.5 ? C131 C134 H134c . . . 109.5 ? H134a C134 H134b . . . 109.5 ? H134a C134 H134c . . . 109.5 ? H134b C134 H134c . . . 109.5 ? C13 C14 C15 . . . 124.2(8) ? C13 C14 H14 . . . 117.9 ? C15 C14 H14 . . . 117.9 ? C14 C15 C151 . . . 120.7(8) ? C14 C15 C16 . . . 116.8(8) ? C151 C15 C16 . . . 122.5(8) ? C15 C151 C152 . . . 107.4(9) ? C15 C151 C153 . . . 111.6(10) ? C15 C151 C154 . . . 114.3(10) ? C15 C151 C152' . . . 117.6(15) ? C15 C151 C153' . . . 105.0(15) ? C15 C151 C154' . . . 107.8(15) ? C152 C151 C153 . . . 105.7(12) ? C152 C151 C154 . . . 107.7(11) ? C153 C151 C154 . . . 109.6(12) ? C151 C152 H152a . . . 109.5 ? C151 C152 H152b . . . 109.4 ? C151 C152 H152c . . . 109.5 ? H152a C152 H152b . . . 109.4 ? H152a C152 H152c . . . 110 ? H152b C152 H152c . . . 109(2) ? C151 C153 H153a . . . 109.4 ? C151 C153 H153b . . . 109.4 ? C151 C153 H153c . . . 109.4 ? H153a C153 H153b . . . 109.5 ? H153a C153 H153c . . . 109.5 ? H153b C153 H153c . . . 109.6 ? C151 C154 H154a . . . 109.5 ? C151 C154 H154b . . . 109.4 ? C151 C154 H154c . . . 109.5 ? H154a C154 H154b . . . 109.4 ? H154a C154 H154c . . . 109.5 ? H154b C154 H154c . . . 109.5 ? C151 C152' H152'a . . . 109 ? C151 C152' H152'b . . . 109 ? C151 C152' H152'c . . . 109 ? H152'a C152' H152'b . . . 109 ? H152'a C152' H152'c . . . 110 ? H152'b C152' H152'c . . . 110 ? C151 C153' H153'a . . . 109 ? C151 C153' H153'b . . . 109 ? C151 C153' H153'c . . . 109 ? H153'a C153' H153'b . . . 110 ? H153'a C153' H153'c . . . 110 ? H153'b C153' H153'c . . . 110 ? C151 C154' H154'a . . . 109 ? C151 C154' H154'b . . . 110 ? C151 C154' H154'c . . . 109 ? H154'a C154' H154'b . . . 110 ? H154'a C154' H154'c . . . 109 ? H154'b C154' H154'c . . . 109 ? C11 C16 C15 . . . 121.6(8) ? C11 C16 H16 . . . 119.2 ? C15 C16 H16 . . . 119.2 ? N1 C20 C21 . . . 117.5(7) ? N1 C20 H20a . . . 107.4 ? N1 C20 H20b . . . 107.5 ? C21 C20 H20a . . . 107.4 ? C21 C20 H20b . . . 107.4 ? H20a C20 H20b . . . 109.5 ? C20 C21 C22 . . . 120.7(8) ? C20 C21 C26 . . . 119.2(8) ? C22 C21 C26 . . . 119.8(8) ? C21 C22 O22 . . . 118.0(7) ? C21 C22 C23 . . . 119.7(8) ? O22 C22 C23 . . . 122.3(7) ? Yb O22 C22 . . . 141.0(5) ? C22 C23 C231 . . . 120.3(8) ? C22 C23 C24 . . . 117.4(8) ? C231 C23 C24 . . . 122.3(8) ? C23 C231 C232 . . . 110.7(7) ? C23 C231 C233 . . . 110.2(8) ? C23 C231 C234 . . . 111.0(8) ? C232 C231 C233 . . . 108.2(9) ? C232 C231 C234 . . . 107.2(8) ? C233 C231 C234 . . . 109.5(8) ? C231 C232 H232a . . . 109.5 ? C231 C232 H232b . . . 109.4 ? C231 C232 H232c . . . 109.5 ? H232a C232 H232b . . . 109.4 ? H232a C232 H232c . . . 109.5 ? H232b C232 H232c . . . 109.4 ? C231 C233 H233a . . . 109.5 ? C231 C233 H233b . . . 109.5 ? C231 C233 H233c . . . 109.5 ? H233a C233 H233b . . . 109.4 ? H233a C233 H233c . . . 109.5 ? H233b C233 H233c . . . 109.5 ? C231 C234 H234a . . . 109.5 ? C231 C234 H234b . . . 109.4 ? C231 C234 H234c . . . 109.5 ? H234a C234 H234b . . . 109.4 ? H234a C234 H234c . . . 109.5 ? H234b C234 H234c . . . 109.5 ? C23 C24 C25 . . . 124.5(8) ? C23 C24 H24 . . . 117.7 ? C25 C24 H24 . . . 117.8 ? C24 C25 C251 . . . 119.4(8) ? C24 C25 C26 . . . 116.0(8) ? C251 C25 C26 . . . 124.6(8) ? C25 C251 C252 . . . 112.4(8) ? C25 C251 C253 . . . 109.7(9) ? C25 C251 C255 . . . 110.1(9) ? C252 C251 C253 . . . 107.7(10) ? C252 C251 C255 . . . 108.8(10) ? C253 C251 C255 . . . 108.0(10) ? C251 C252 H252a . . . 109.5 ? C251 C252 H252b . . . 109.4 ? C251 C252 H252c . . . 109.5 ? H252a C252 H252b . . . 109.4 ? H252a C252 H252c . . . 109.5 ? H252b C252 H252c . . . 109.5 ? C251 C253 H253a . . . 109.4 ? C251 C253 H253b . . . 109.5 ? C251 C253 H253c . . . 109.3 ? H253a C253 H253b . . . 109.6 ? H253a C253 H253c . . . 109.5 ? H253b C253 H253c . . . 109.6 ? C251 C255 H255a . . . 109.5 ? C251 C255 H255b . . . 109.4 ? C251 C255 H255c . . . 109.5 ? H255a C255 H255b . . . 109.4 ? H255a C255 H255c . . . 109.5 ? H255b C255 H255c . . . 109.5 ? C21 C26 C25 . . . 122.5(8) ? C21 C26 H26 . . . 118.7 ? C25 C26 H26 . . . 118.8 ? N1 C1 C2 . . . 113.6(7) ? N1 C1 C2' . . . 113.4(16) ? N1 C1 H1a . . . 108.4 ? N1 C1 H1b . . . 108.4 ? N1 C1 H1'a . . . 108.5 ? N1 C1 H1'b . . . 108.4 ? C2 C1 H1a . . . 108.5 ? C2 C1 H1b . . . 108.4 ? C2' C1 H1'a . . . 108.6 ? C2' C1 H1'b . . . 108.4 ? H1a C1 H1b . . . 109.5 ? H1'a C1 H1'b . . . 109.5 ? C1 C2 N3 . . . 110.6(9) ? C1 C2 H2a . . . 109.2 ? C1 C2 H2b . . . 109.3 ? N3 C2 H2a . . . 109.1 ? N3 C2 H2b . . . 109.2 ? H2a C2 H2b . . . 109.4 ? Yb N3 C2 . . . 106.0(6) ? Yb N3 C31 . . . 113.7(8) ? Yb N3 C32 . . . 113.0(6) ? Yb N3 C2' . . . 105.5(15) ? Yb N3 C31' . . . 109.7(15) ? Yb N3 C32' . . . 115.6(17) ? C2 N3 C31 . . . 112.6(9) ? C2 N3 C32 . . . 104.3(8) ? C31 N3 C32 . . . 107.0(10) ? C2' N3 C31' . . . 101(2) ? C2' N3 C32' . . . 113(2) ? C31' N3 C32' . . . 110(2) ? N3 C31 H31a . . . 109.5 ? N3 C31 H31b . . . 109.4 ? N3 C31 H31c . . . 109.4 ? H31a C31 H31b . . . 109.6 ? H31a C31 H31c . . . 109.5 ? H31b C31 H31c . . . 109.5 ? N3 C32 H32a . . . 109.5 ? N3 C32 H32b . . . 109.5 ? N3 C32 H32c . . . 109.4 ? H32a C32 H32b . . . 109.5 ? H32a C32 H32c . . . 109.5 ? H32b C32 H32c . . . 109.5 ? C1 C2' N3 . . . 110(2) ? C1 C2' H2'a . . . 110 ? C1 C2' H2'b . . . 110 ? N3 C2' H2'a . . . 109 ? N3 C2' H2'b . . . 109 ? H2'a C2' H2'b . . . 109 ? N3 C31' H31'a . . . 109 ? N3 C31' H31'b . . . 109 ? N3 C31' H31'c . . . 109 ? H31'a C31' H31'b . . . 110 ? H31'a C31' H31'c . . . 110 ? H31'b C31' H31'c . . . 110 ? N3 C32' H32'a . . . 109 ? N3 C32' H32'b . . . 110 ? N3 C32' H32'c . . . 109 ? H32'a C32' H32'b . . . 110 ? H32'a C32' H32'c . . . 109 ? H32'b C32' H32'c . . . 110 ? Yb O101 S101 . . . 99.0(4) ? Yb O102 S101 . . . 96.1(4) ? S101 C101 F101 . . . 109.8(12) ? S101 C101 F102 . . . 111.4(8) ? S101 C101 F103 . . . 109.4(10) ? F101 C101 F102 . . . 110.1(13) ? F101 C101 F103 . . . 108.1(9) ? F102 C101 F103 . . . 107.9(15) ? O101 S101 O102 . . . 108.0(4) ? O101 S101 O103 . . . 117.2(6) ? O101 S101 C101 . . . 104.8(7) ? O102 S101 O103 . . . 117.7(6) ? O102 S101 C101 . . . 103.1(7) ? O103 S101 C101 . . . 104.1(5) ? Yb O201 C202 . . . 122.6(6) ? Yb O201 C205 . . . 120.6(7) ? C202 O201 C205 . . . 108.6(9) ? O201 C202 C203 . . . 97.7(12) ? O201 C202 C203' . . . 112.0(16) ? O201 C202 H202a . . . 112.3 ? O201 C202 H202b . . . 112.3 ? O201 C202 H202'a . . . 108.8 ? O201 C202 H202'b . . . 108.8 ? C203 C202 H202a . . . 112.4 ? C203 C202 H202b . . . 112.4 ? C203' C202 H202'a . . . 109.0 ? C203' C202 H202'b . . . 108.8 ? H202a C202 H202b . . . 109.4 ? H202'a C202 H202'b . . . 109.4(14) ? C202 C203 C204 . . . 111(2) ? C202 C203 H203a . . . 109 ? C202 C203 H203b . . . 109 ? C204 C203 H203a . . . 109 ? C204 C203 H203b . . . 109 ? H203a C203 H203b . . . 109 ? C202 C203' C204' . . . 102(2) ? C202 C203' H203'a . . . 111 ? C202 C203' H203'b . . . 112 ? C204' C203' H203'a . . . 111 ? C204' C203' H203'b . . . 111 ? H203'a C203' H203'b . . . 110 ? C203 C204 C205 . . . 107(3) ? C203 C204 H204a . . . 111 ? C203 C204 H204b . . . 111 ? C205 C204 H204a . . . 110 ? C205 C204 H204b . . . 110 ? H204a C204 H204b . . . 109 ? H204'a C204 H204'b . . . 108 ? C203' C204' C205 . . . 105(3) ? C203' C204' H204'a . . . 109 ? C203' C204' H204'b . . . 109 ? C205 C204' H204'a . . . 111 ? C205 C204' H204'b . . . 112 ? H204'a C204' H204'b . . . 110 ? O201 C205 C204 . . . 109.6(16) ? O201 C205 C204' . . . 107(2) ? O201 C205 H205a . . . 109.3 ? O201 C205 H205b . . . 109.2 ? O201 C205 H205'a . . . 110.3 ? O201 C205 H205'b . . . 110.3 ? C204 C205 H205a . . . 109.7 ? C204 C205 H205b . . . 110 ? C204' C205 H205'a . . . 110 ? C204' C205 H205'b . . . 110 ? H205a C205 H205b . . . 109.4 ? H205'a C205 H205'b . . . 109.4 ? O02 C01 H01a . . . 110 ? O02 C01 H01b . . . 110 ? O02 C01 H01c . . . 107 ? H01a C01 H01b . . . 113 ? H01a C01 H01c . . . 108 ? H01b C01 H01c . . . 109 ? C01 O02 C03 . . . 109(7) ? O02 C03 C04 . . . 109(6) ? O02 C03 H03a . . . 107 ? O02 C03 H03b . . . 111 ? C04 C03 H03a . . . 109 ? C04 C03 H03b . . . 112 ? H03a C03 H03b . . . 109 ? C03 C04 O05 . . . 109(7) ? C03 C04 H04a . . . 108 ? C03 C04 H04b . . . 109 ? O05 C04 H04a . . . 109 ? O05 C04 H04b . . . 111 ? H04a C04 H04b . . . 112 ? C04 O05 C06 . . . 109(5) ? O05 C06 H06a . . . 110 ? O05 C06 H06b . . . 110 ? O05 C06 H06c . . . 110 ? H06a C06 H06b . . . 109 ? H06a C06 H06c . . . 109 ? H06b C06 H06c . . . 110 ? H01'a C01' H01'b . . . 110 ? H01'a C01' H01'c . . . 110 ? H01'b C01' H01'c . . . 109 ? C01' O02' C03' . . . 110(5) ? O02' C03' C04' . . . 109(4) ? O02' C03' H03'a . . . 110 ? O02' C03' H03'b . . . 109 ? C04' C03' H03'a . . . 110 ? C04' C03' H03'b . . . 109 ? H03'a C03' H03'b . . . 109 ? C03' C04' O05' . . . 110(4) ? C03' C04' H04'a . . . 110 ? C03' C04' H04'b . . . 110 ? O05' C04' H04'a . . . 109 ? O05' C04' H04'b . . . 109 ? H04'a C04' H04'b . . . 109 ? C04' O05' C06' . . . 109(5) ? O05' C06' H06'a . . . 109 ? O05' C06' H06'b . . . 109 ? O05' C06' H06'c . . . 110 ? H06'a C06' H06'b . . . 110 ? H06'a C06' H06'c . . . 109 ? H06'b C06' H06'c . . . 110 ? _exptl_crystal_F_000 2084 _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 43 _reflns_number_observed ? _reflns_d_resolution_high .667 _reflns_d_resolution_low 12.776 _diffrn_reflns_av_sigmaI/netI .053 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 170 _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 18 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .054 _refine_ls_wR_factor_all .062 _refine_ls_goodness_of_fit_all 1.318 _refine_ls_shift/su_mean .001