# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1830 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-11-30 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram 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. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_yodpp # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C54 H39 O3 Y1' _chemical_formula_moiety ? _chemical_formula_weight 824.81 _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 15.907(3) _cell_length_b 13.541(3) _cell_length_c 10.966(2) _cell_angle_alpha 116.504(4) _cell_angle_beta 92.816(5) _cell_angle_gamma 103.092(4) _cell_volume 2028.1(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 2430 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.48 _exptl_crystal_description fragment _exptl_crystal_size_max .30 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .10 _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 .50 _exptl_absorpt_correction_T_max .894 _diffrn_reflns_number 23503 _reflns_number_total 6958 _reflns_Friedel_coverage ? _reflns_number_gt 4360 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 24.79 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .078 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .076 _refine_ls_wR_factor_ref .099 _refine_ls_goodness_of_fit_ref 2.937 _refine_ls_number_reflns 4360 _refine_ls_number_parameters 524 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .061 _refine_diff_density_min -.532 _refine_diff_density_max 1.622 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1356(360) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 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 ? 0 108 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 78 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 6 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Y ? 0 2 -2.951 3.542 '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 Y .27963(7) .20709(9) .22633(11) .0390(4) Uani ? ? 1.00000 ? ? O1 .2284(5) .3306(6) .2012(7) .050(3) Uani ? ? 1.00000 ? ? C11 .1847(6) .4072(9) .2712(11) .043(4) Uani ? ? 1.00000 ? ? C12 .1630(6) .4109(9) .3977(10) .044(4) Uani ? ? 1.00000 ? ? C13 .1226(9) .4912(11) .4769(12) .065(6) Uani ? ? 1.00000 ? ? C14 .0999(8) .5666(10) .4353(14) .061(6) Uani ? ? 1.00000 ? ? C15 .1200(8) .5586(11) .3123(13) .063(6) Uani ? ? 1.00000 ? ? C16 .1626(6) .4797(9) .2264(11) .046(4) Uani ? ? 1.00000 ? ? C121 .1847(6) .3243(9) .4315(11) .044(4) Uani ? ? 1.00000 ? ? C122 .2640(7) .3452(9) .5115(11) .049(5) Uani ? ? 1.00000 ? ? C123 .2852(7) .2587(11) .5269(12) .057(5) Uani ? ? 1.00000 ? ? C124 .2314(8) .1510(11) .4665(13) .058(6) Uani ? ? 1.00000 ? ? C125 .1511(8) .1234(12) .3804(14) .071(6) Uani ? ? 1.00000 ? ? C126 .1286(7) .2124(11) .3655(13) .058(6) Uani ? ? 1.00000 ? ? C161 .1775(9) .4728(11) .0928(13) .062(6) Uani ? ? 1.00000 ? ? C162 .1101(11) .4383(11) -.0130(16) .085(8) Uani ? ? 1.00000 ? ? C163 .1250(18) .4364(15) -.1349(19) .125(13) Uani ? ? 1.00000 ? ? C164 .212(3) .468(3) -.154(3) .18(2) Uani ? ? 1.00000 ? ? C165 .2763(15) .494(3) -.058(3) .172(19) Uani ? ? 1.00000 ? ? C166 .2629(11) .5001(17) .069(2) .111(11) Uani ? ? 1.00000 ? ? O2 .4117(4) .2655(6) .3148(7) .048(3) Uani ? ? 1.00000 ? ? C21 .4962(6) .2747(9) .2998(11) .044(4) Uani ? ? 1.00000 ? ? C22 .5197(7) .2413(9) .1708(12) .052(5) Uani ? ? 1.00000 ? ? C23 .6080(8) .2503(11) .1581(13) .064(6) Uani ? ? 1.00000 ? ? C24 .6701(7) .2867(12) .2683(13) .067(6) Uani ? ? 1.00000 ? ? C25 .6483(7) .3199(10) .4008(13) .060(6) Uani ? ? 1.00000 ? ? C26 .5612(7) .3129(9) .4189(11) .046(5) Uani ? ? 1.00000 ? ? C221 .4515(7) .1932(9) .0474(11) .046(5) Uani ? ? 1.00000 ? ? C222 .3878(7) .2528(10) .0405(11) .052(5) Uani ? ? 1.00000 ? ? C223 .3247(8) .2023(12) -.0745(13) .063(6) Uani ? ? 1.00000 ? ? C224 .3188(9) .1007(13) -.1856(13) .071(6) Uani ? ? 1.00000 ? ? C225 .3800(11) .0442(12) -.1806(13) .080(7) Uani ? ? 1.00000 ? ? C226 .4452(8) .0883(10) -.0664(12) .061(6) Uani ? ? 1.00000 ? ? C261 .5364(7) .3409(9) .5560(11) .050(5) Uani ? ? 1.00000 ? ? C262 .5458(10) .2734(12) .6206(15) .078(7) Uani ? ? 1.00000 ? ? C263 .5188(12) .2930(14) .7431(19) .100(10) Uani ? ? 1.00000 ? ? C264 .4862(10) .3857(13) .8149(14) .080(7) Uani ? ? 1.00000 ? ? C265 .4802(8) .4533(10) .7542(13) .062(6) Uani ? ? 1.00000 ? ? C266 .5039(7) .4341(10) .6304(13) .056(5) Uani ? ? 1.00000 ? ? O3 .2200(5) .0401(6) .0810(7) .052(3) Uani ? ? 1.00000 ? ? C31 .1791(7) -.0740(9) .0091(10) .046(4) Uani ? ? 1.00000 ? ? C32 .1980(7) -.1482(9) .0581(11) .051(5) Uani ? ? 1.00000 ? ? C33 .1544(8) -.2665(10) -.0154(12) .058(5) Uani ? ? 1.00000 ? ? C34 .0953(8) -.3085(10) -.1338(14) .066(6) Uani ? ? 1.00000 ? ? C35 .0803(7) -.2363(10) -.1867(11) .053(5) Uani ? ? 1.00000 ? ? C36 .1198(7) -.1178(9) -.1148(11) .048(5) Uani ? ? 1.00000 ? ? C321 .2602(8) -.1059(9) .1885(11) .052(5) Uani ? ? 1.00000 ? ? C322 .3422(7) -.0284(10) .2165(11) .050(5) Uani ? ? 1.00000 ? ? C323 .3984(8) .0092(11) .3369(14) .066(6) Uani ? ? 1.00000 ? ? C324 .3744(9) -.0281(12) .4310(13) .068(7) Uani ? ? 1.00000 ? ? C325 .2960(10) -.1052(12) .4071(14) .073(7) Uani ? ? 1.00000 ? ? C326 .2376(9) -.1424(10) .2846(14) .068(6) Uani ? ? 1.00000 ? ? C361 .1019(7) -.0419(9) -.1716(12) .051(5) Uani ? ? 1.00000 ? ? C362 .0822(8) .0575(11) -.0926(14) .069(6) Uani ? ? 1.00000 ? ? C363 .0623(11) .1262(13) -.151(2) .099(9) Uani ? ? 1.00000 ? ? C364 .0680(12) .0945(17) -.285(2) .113(11) Uani ? ? 1.00000 ? ? C365 .0862(10) -.0067(17) -.3662(17) .097(8) Uani ? ? 1.00000 ? ? C366 .1042(8) -.0738(11) -.3099(14) .066(6) Uani ? ? 1.00000 ? ? H13 .10974 .49680 .56629 .08400 Uiso ? ? 1.00000 ? ? H14 .07092 .62336 .49120 .07600 Uiso ? ? 1.00000 ? ? H15 .10369 .60965 .28080 .07900 Uiso ? ? 1.00000 ? ? H122 .30430 .42232 .55690 .06400 Uiso ? ? 1.00000 ? ? H123 .34027 .27432 .58265 .07200 Uiso ? ? 1.00000 ? ? H124 .24797 .09138 .48128 .07500 Uiso ? ? 1.00000 ? ? H125 .11208 .04495 .33378 .08700 Uiso ? ? 1.00000 ? ? H126 .07340 .19605 .30753 .07600 Uiso ? ? 1.00000 ? ? H162 .04956 .41474 -.00022 .10800 Uiso ? ? 1.00000 ? ? H163 .07689 .41021 -.21241 .15600 Uiso ? ? 1.00000 ? ? H164 .22988 .47440 -.23472 .22900 Uiso ? ? 1.00000 ? ? H165 .33706 .51493 -.06894 .19600 Uiso ? ? 1.00000 ? ? H166 .31303 .52370 .14369 .13800 Uiso ? ? 1.00000 ? ? H23 .62426 .22806 .06622 .08000 Uiso ? ? 1.00000 ? ? H24 .73110 .29226 .25646 .08400 Uiso ? ? 1.00000 ? ? H25 .69336 .34743 .48017 .07500 Uiso ? ? 1.00000 ? ? H222 .38936 .32641 .11832 .06700 Uiso ? ? 1.00000 ? ? H223 .28381 .24607 -.07765 .08000 Uiso ? ? 1.00000 ? ? H224 .27109 .06616 -.26444 .09000 Uiso ? ? 1.00000 ? ? H225 .37754 -.02958 -.26033 .10000 Uiso ? ? 1.00000 ? ? H226 .48727 .04673 -.06499 .07700 Uiso ? ? 1.00000 ? ? H262 .57491 .21279 .57582 .10200 Uiso ? ? 1.00000 ? ? H263 .52069 .23928 .77883 .12200 Uiso ? ? 1.00000 ? ? H264 .46969 .40311 .90545 .09900 Uiso ? ? 1.00000 ? ? H265 .45730 .51994 .80284 .08000 Uiso ? ? 1.00000 ? ? H266 .49897 .48527 .59119 .07200 Uiso ? ? 1.00000 ? ? H33 .16731 -.31794 .01954 .07600 Uiso ? ? 1.00000 ? ? H34 .06298 -.39078 -.18329 .08300 Uiso ? ? 1.00000 ? ? H35 .04155 -.26917 -.27488 .06800 Uiso ? ? 1.00000 ? ? H322 .35891 -.00257 .14964 .06400 Uiso ? ? 1.00000 ? ? H323 .45614 .06360 .35574 .08400 Uiso ? ? 1.00000 ? ? H324 .41436 .00148 .51710 .08400 Uiso ? ? 1.00000 ? ? H325 .28211 -.13276 .47299 .09700 Uiso ? ? 1.00000 ? ? H326 .17939 -.19481 .26804 .08400 Uiso ? ? 1.00000 ? ? H362 .08145 .08301 .00803 .08900 Uiso ? ? 1.00000 ? ? H363 .04414 .19571 -.09579 .12400 Uiso ? ? 1.00000 ? ? H364 .05880 .13983 -.32989 .13400 Uiso ? ? 1.00000 ? ? H365 .08798 -.03308 -.46516 .12100 Uiso ? ? 1.00000 ? ? H366 .12002 -.14513 -.36739 .08900 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 Y .0355(5) .0365(5) .0403(6) .0098(4) .0069(4) .0141(4) O1 .052(4) .046(4) .056(5) .023(4) .020(4) .022(4) C11 .041(6) .042(6) .054(7) .012(5) .024(5) .027(5) C12 .042(6) .046(6) .033(6) .014(5) .006(5) .010(5) C13 .081(9) .064(8) .049(7) .036(7) .017(6) .018(6) C14 .055(7) .057(7) .083(9) .031(6) .027(7) .033(7) C15 .064(8) .067(8) .072(9) .040(7) .019(7) .033(7) C16 .038(6) .044(6) .051(7) .009(5) .012(5) .019(5) C121 .039(6) .052(6) .050(6) .017(5) .015(5) .030(6) C122 .049(7) .044(6) .038(6) .001(5) .007(5) .011(5) C123 .041(6) .073(8) .060(8) .015(6) .013(6) .033(7) C124 .053(7) .068(8) .076(9) .025(6) .014(6) .049(7) C125 .050(8) .074(9) .086(10) .001(7) .019(7) .042(8) C126 .037(6) .071(8) .075(9) .008(6) .017(6) .043(7) C161 .088(9) .068(8) .058(8) .048(7) .029(7) .040(7) C162 .118(13) .054(8) .071(10) .018(8) -.006(9) .024(7) C163 .24(3) .079(11) .067(12) .071(15) -.006(14) .035(10) C164 .35(4) .21(3) .15(2) .23(3) .18(3) .13(2) C165 .15(2) .35(4) .21(3) .19(2) .14(2) .23(3) C166 .091(12) .183(19) .149(17) .082(13) .063(12) .129(16) O2 .035(4) .062(5) .047(4) .016(3) .011(3) .023(4) C21 .036(6) .044(6) .048(6) .005(5) .008(5) .021(5) C22 .046(7) .053(7) .065(8) .016(5) .016(6) .033(6) C23 .057(8) .074(8) .060(8) .018(7) .023(6) .029(7) C24 .038(7) .090(10) .061(8) .016(6) .017(6) .025(7) C25 .040(7) .071(8) .068(8) .016(6) -.005(6) .034(7) C26 .041(6) .042(6) .045(6) .007(5) .004(5) .015(5) C221 .048(6) .054(7) .037(6) .016(5) .011(5) .021(5) C222 .050(7) .063(7) .040(6) .005(6) .010(5) .026(6) C223 .056(8) .079(9) .065(9) .022(7) .012(7) .041(8) C224 .066(9) .090(10) .051(8) .013(8) -.005(7) .033(8) C225 .107(12) .066(9) .039(7) .002(8) .010(8) .012(7) C226 .069(8) .058(7) .056(8) .031(6) .015(6) .021(6) C261 .047(6) .049(6) .048(7) -.001(5) -.006(5) .025(6) C262 .102(11) .068(9) .066(9) .023(8) -.003(8) .035(8) C263 .144(16) .088(11) .099(13) .040(11) .011(11) .069(11) C264 .094(11) .075(10) .052(8) -.010(8) .006(7) .030(8) C265 .063(8) .054(7) .064(8) .013(6) .015(7) .024(7) C266 .052(7) .053(7) .063(8) .012(6) .014(6) .029(6) O3 .070(5) .043(4) .039(4) .012(4) .003(4) .020(4) C31 .054(7) .038(6) .031(6) .003(5) .010(5) .007(5) C32 .052(7) .051(7) .050(7) .017(5) .012(5) .023(6) C33 .061(8) .052(7) .058(8) .019(6) .011(6) .021(6) C34 .059(8) .042(7) .083(10) .004(6) .010(7) .022(7) C35 .050(7) .053(7) .044(6) .011(6) .005(5) .015(6) C36 .046(6) .046(6) .049(7) .013(5) .006(5) .021(5) C321 .067(8) .040(6) .046(7) .019(6) .015(6) .016(5) C322 .044(6) .062(7) .047(7) .018(6) .011(5) .025(6) C323 .056(8) .072(8) .083(10) .026(7) .006(7) .045(8) C324 .074(9) .083(10) .058(8) .043(8) .006(7) .033(8) C325 .096(11) .071(9) .070(9) .040(8) .021(8) .039(8) C326 .074(9) .054(7) .074(9) .014(6) .000(7) .032(7) C361 .044(6) .046(7) .054(7) .001(5) .004(5) .023(6) C362 .072(9) .056(8) .077(9) .009(7) -.013(7) .035(7) C363 .106(13) .065(10) .114(14) .020(9) -.023(11) .039(10) C364 .109(14) .091(13) .135(18) -.019(11) -.049(13) .079(14) C365 .077(10) .116(14) .089(12) -.021(10) -.013(9) .065(12) C366 .051(7) .079(9) .072(9) .010(6) .011(6) .043(8) # 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 Y O1 . . 2.132(9) ? Y O2 . . 2.085(6) ? Y O3 . . 2.053(6) ? O1 C11 . . 1.349(13) ? C11 C12 . . 1.428(17) ? C11 C16 . . 1.38(2) ? C12 C13 . . 1.370(17) ? C12 C121 . . 1.48(2) ? C13 C14 . . 1.40(2) ? C13 H13 . . .984(14) ? C14 C15 . . 1.37(2) ? C14 H14 . . .972(13) ? C15 C16 . . 1.407(17) ? C15 H15 . . .974(17) ? C16 C161 . . 1.46(2) ? C121 C122 . . 1.396(16) ? C121 C126 . . 1.401(14) ? C122 C123 . . 1.36(2) ? C122 H122 . . .975(9) ? C123 C124 . . 1.347(16) ? C123 H123 . . .966(12) ? C124 C125 . . 1.420(19) ? C124 H124 . . .978(17) ? C125 C126 . . 1.40(2) ? C125 H125 . . .980(12) ? C126 H126 . . .978(12) ? C161 C162 . . 1.37(2) ? C161 C166 . . 1.39(2) ? C162 C163 . . 1.36(3) ? C162 H162 . . .982(17) ? C163 C164 . . 1.41(5) ? C163 H163 . . .99(2) ? C164 C165 . . 1.30(5) ? C164 H164 . . .98(4) ? C165 C166 . . 1.39(4) ? C165 H165 . . .97(3) ? C166 H166 . . 1.00(2) ? O2 C21 . . 1.346(12) ? C21 C22 . . 1.379(17) ? C21 C26 . . 1.437(15) ? C22 C23 . . 1.401(17) ? C22 C221 . . 1.477(15) ? C23 C24 . . 1.346(18) ? C23 H23 . . .981(14) ? C24 C25 . . 1.40(2) ? C24 H24 . . .975(12) ? C25 C26 . . 1.397(16) ? C25 H25 . . .969(12) ? C26 C261 . . 1.476(17) ? C221 C222 . . 1.45(2) ? C221 C226 . . 1.387(14) ? C222 C223 . . 1.365(16) ? C222 H222 . . .975(10) ? C223 C224 . . 1.348(17) ? C223 H223 . . .983(16) ? C224 C225 . . 1.38(3) ? C224 H224 . . .978(13) ? C225 C226 . . 1.386(19) ? C225 H225 . . .981(12) ? C226 H226 . . .971(15) ? C261 C262 . . 1.41(2) ? C261 C266 . . 1.394(17) ? C262 C263 . . 1.36(3) ? C262 H262 . . .982(16) ? C263 C264 . . 1.39(2) ? C263 H263 . . .97(2) ? C264 C265 . . 1.37(3) ? C264 H264 . . .977(15) ? C265 C266 . . 1.35(2) ? C265 H265 . . .985(13) ? C266 H266 . . .979(16) ? O3 C31 . . 1.356(11) ? C31 C32 . . 1.41(2) ? C31 C36 . . 1.410(15) ? C32 C33 . . 1.410(15) ? C32 C321 . . 1.492(16) ? C33 C34 . . 1.368(18) ? C33 H33 . . .985(16) ? C34 C35 . . 1.40(2) ? C34 H34 . . .986(11) ? C35 C36 . . 1.398(14) ? C35 H35 . . .973(11) ? C36 C361 . . 1.49(2) ? C321 C322 . . 1.397(15) ? C321 C326 . . 1.38(2) ? C322 C323 . . 1.371(18) ? C322 H322 . . .967(14) ? C323 C324 . . 1.37(2) ? C323 H323 . . .984(12) ? C324 C325 . . 1.36(2) ? C324 H324 . . .971(13) ? C325 C326 . . 1.41(2) ? C325 H325 . . .964(18) ? C326 H326 . . .982(12) ? C361 C362 . . 1.356(17) ? C361 C366 . . 1.38(2) ? C362 C363 . . 1.42(3) ? C362 H362 . . 1.000(15) ? C363 C364 . . 1.36(3) ? C363 H363 . . .983(17) ? C364 C365 . . 1.37(3) ? C364 H364 . . .97(3) ? C365 C366 . . 1.37(3) ? C365 H365 . . .984(19) ? C366 H366 . . .988(14) ? 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 O1 Y O2 . . . 114.8(3) ? O1 Y O3 . . . 114.2(3) ? O2 Y O3 . . . 123.0(3) ? Y O1 C11 . . . 137.6(8) ? O1 C11 C12 . . . 116.1(12) ? O1 C11 C16 . . . 123.0(11) ? C12 C11 C16 . . . 120.9(10) ? C11 C12 C13 . . . 118.7(13) ? C11 C12 C121 . . . 116.4(10) ? C13 C12 C121 . . . 124.8(12) ? C12 C13 C14 . . . 121.9(13) ? C12 C13 H13 . . . 119.4(15) ? C14 C13 H13 . . . 118.7(13) ? C13 C14 C15 . . . 117.6(12) ? C13 C14 H14 . . . 122.0(15) ? C15 C14 H14 . . . 120.4(16) ? C14 C15 C16 . . . 123.8(15) ? C14 C15 H15 . . . 118.7(13) ? C16 C15 H15 . . . 117.5(14) ? C11 C16 C15 . . . 117.1(12) ? C11 C16 C161 . . . 122.7(11) ? C15 C16 C161 . . . 120.2(14) ? C12 C121 C122 . . . 122.7(9) ? C12 C121 C126 . . . 118.3(10) ? C122 C121 C126 . . . 118.4(13) ? C121 C122 C123 . . . 120.5(9) ? C121 C122 H122 . . . 119.5(13) ? C123 C122 H122 . . . 120.0(11) ? C122 C123 C124 . . . 122.0(12) ? C122 C123 H123 . . . 119.7(11) ? C124 C123 H123 . . . 118.4(16) ? C123 C124 C125 . . . 120.3(15) ? C123 C124 H124 . . . 119.9(12) ? C125 C124 H124 . . . 119.8(11) ? C124 C125 C126 . . . 117.9(11) ? C124 C125 H125 . . . 121.1(17) ? C126 C125 H125 . . . 121.0(13) ? C121 C126 C125 . . . 120.9(11) ? C121 C126 H126 . . . 119.4(15) ? C125 C126 H126 . . . 119.7(11) ? C16 C161 C162 . . . 122.5(13) ? C16 C161 C166 . . . 119.7(14) ? C162 C161 C166 . . . 117.8(16) ? C161 C162 C163 . . . 121.8(18) ? C161 C162 H162 . . . 119.1(17) ? C163 C162 H162 . . . 119.1(18) ? C162 C163 C164 . . . 119(2) ? C162 C163 H163 . . . 122(2) ? C164 C163 H163 . . . 119(2) ? C163 C164 C165 . . . 120(3) ? C163 C164 H164 . . . 126(3) ? C165 C164 H164 . . . 115(4) ? C164 C165 C166 . . . 122(3) ? C164 C165 H165 . . . 122(4) ? C166 C165 H165 . . . 116(3) ? C161 C166 C165 . . . 119.2(18) ? C161 C166 H166 . . . 119(2) ? C165 C166 H166 . . . 121.4(19) ? Y O2 C21 . . . 149.6(6) ? O2 C21 C22 . . . 120.7(9) ? O2 C21 C26 . . . 119.1(10) ? C22 C21 C26 . . . 120.1(10) ? C21 C22 C23 . . . 119.4(11) ? C21 C22 C221 . . . 119.8(10) ? C23 C22 C221 . . . 120.7(11) ? C22 C23 C24 . . . 121.5(13) ? C22 C23 H23 . . . 118.9(12) ? C24 C23 H23 . . . 119.7(13) ? C23 C24 C25 . . . 120.5(11) ? C23 C24 H24 . . . 119.7(14) ? C25 C24 H24 . . . 119.7(12) ? C24 C25 C26 . . . 120.2(11) ? C24 C25 H25 . . . 120.3(11) ? C26 C25 H25 . . . 119.5(13) ? C21 C26 C25 . . . 118.2(11) ? C21 C26 C261 . . . 120.9(10) ? C25 C26 C261 . . . 120.8(10) ? C22 C221 C222 . . . 121.5(9) ? C22 C221 C226 . . . 121.4(12) ? C222 C221 C226 . . . 117.2(10) ? C221 C222 C223 . . . 118.8(10) ? C221 C222 H222 . . . 120.2(10) ? C223 C222 H222 . . . 121.0(14) ? C222 C223 C224 . . . 124.1(15) ? C222 C223 H223 . . . 116.9(11) ? C224 C223 H223 . . . 118.9(13) ? C223 C224 C225 . . . 117.4(12) ? C223 C224 H224 . . . 121.4(17) ? C225 C224 H224 . . . 121.0(13) ? C224 C225 C226 . . . 122.1(11) ? C224 C225 H225 . . . 119.1(13) ? C226 C225 H225 . . . 118.8(17) ? C221 C226 C225 . . . 120.4(14) ? C221 C226 H226 . . . 119.0(11) ? C225 C226 H226 . . . 120.7(11) ? C26 C261 C262 . . . 120.6(11) ? C26 C261 C266 . . . 123.5(13) ? C262 C261 C266 . . . 115.9(12) ? C261 C262 C263 . . . 122.0(15) ? C261 C262 H262 . . . 117.6(15) ? C263 C262 H262 . . . 120(2) ? C262 C263 C264 . . . 121(2) ? C262 C263 H263 . . . 119.2(18) ? C264 C263 H263 . . . 120(2) ? C263 C264 C265 . . . 116.6(15) ? C263 C264 H264 . . . 122(2) ? C265 C264 H264 . . . 121.7(16) ? C264 C265 C266 . . . 123.8(13) ? C264 C265 H265 . . . 118.4(14) ? C266 C265 H265 . . . 117.8(16) ? C261 C266 C265 . . . 120.6(15) ? C261 C266 H266 . . . 118.5(13) ? C265 C266 H266 . . . 121.0(12) ? Y O3 C31 . . . 167.7(8) ? O3 C31 C32 . . . 119.2(9) ? O3 C31 C36 . . . 120.1(12) ? C32 C31 C36 . . . 120.7(9) ? C31 C32 C33 . . . 119.2(10) ? C31 C32 C321 . . . 122.6(9) ? C33 C32 C321 . . . 118.1(13) ? C32 C33 C34 . . . 120.1(14) ? C32 C33 H33 . . . 119.1(11) ? C34 C33 H33 . . . 120.9(11) ? C33 C34 C35 . . . 120.7(10) ? C33 C34 H34 . . . 120.1(16) ? C35 C34 H34 . . . 119.1(13) ? C34 C35 C36 . . . 121.1(10) ? C34 C35 H35 . . . 119.2(10) ? C36 C35 H35 . . . 119.7(14) ? C31 C36 C35 . . . 118.1(13) ? C31 C36 C361 . . . 121.5(9) ? C35 C36 C361 . . . 120.4(10) ? C32 C321 C322 . . . 120.9(12) ? C32 C321 C326 . . . 120.5(10) ? C322 C321 C326 . . . 118.6(11) ? C321 C322 C323 . . . 119.9(13) ? C321 C322 H322 . . . 119.3(11) ? C323 C322 H322 . . . 120.8(11) ? C322 C323 C324 . . . 120.5(11) ? C322 C323 H323 . . . 119.5(17) ? C324 C323 H323 . . . 120.0(14) ? C323 C324 C325 . . . 121.7(13) ? C323 C324 H324 . . . 119.2(13) ? C325 C324 H324 . . . 119.1(17) ? C324 C325 C326 . . . 117.9(16) ? C324 C325 H325 . . . 119.9(15) ? C326 C325 H325 . . . 122.2(14) ? C321 C326 C325 . . . 121.3(12) ? C321 C326 H326 . . . 119.6(13) ? C325 C326 H326 . . . 119.0(16) ? C36 C361 C362 . . . 122.1(12) ? C36 C361 C366 . . . 119.4(11) ? C362 C361 C366 . . . 118.5(15) ? C361 C362 C363 . . . 121.0(14) ? C361 C362 H362 . . . 119.8(17) ? C363 C362 H362 . . . 119.2(14) ? C362 C363 C364 . . . 119.0(17) ? C362 C363 H363 . . . 122(2) ? C364 C363 H363 . . . 119(2) ? C363 C364 C365 . . . 120(2) ? C363 C364 H364 . . . 123(2) ? C365 C364 H364 . . . 116(2) ? C364 C365 C366 . . . 120.3(19) ? C364 C365 H365 . . . 122(3) ? C366 C365 H365 . . . 118.0(19) ? C361 C366 C365 . . . 120.8(13) ? C361 C366 H366 . . . 118.9(17) ? C365 C366 H366 . . . 120.4(15) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Y C11 3.257(12) . . ? Y C12 3.554(11) . . ? Y C121 2.845(11) . . ? Y C122 2.899(10) . . ? Y C123 3.041(14) . . ? Y C124 3.134(16) . . ? Y C125 3.053(16) . . ? Y C126 2.906(12) . . ? Y C21 3.316(10) . . ? Y C22 3.853(11) . . ? Y C221 3.434(11) . . ? Y C222 2.913(13) . . ? Y C223 3.385(16) . . ? Y C31 3.391(9) . . ? Y C321 4.007(13) . . ? Y C322 3.509(15) . . ? Y C362 3.990(13) . . ? Y H122 3.4207(11) . . ? Y H123 3.6172(14) . . ? Y H124 3.7704(15) . . ? Y H125 3.6441(13) . . ? Y H126 3.4294(13) . . ? Y H222 2.7737(13) . . ? Y H223 3.6015(15) . . ? Y H322 3.1548(14) . . ? Y H362 3.4294(11) . . ? O1 C12 2.357(13) . . ? O1 C16 2.395(15) . . ? O1 C121 2.685(15) . . ? O1 C161 2.90(2) . . ? C11 C13 2.407(17) . . ? C11 C14 2.794(16) . . ? C11 C15 2.37(2) . . ? C11 C121 2.47(2) . . ? C11 C161 2.49(2) . . ? C12 C14 2.42(2) . . ? C12 C15 2.75(2) . . ? C12 C16 2.44(2) . . ? C12 C122 2.526(19) . . ? C12 C126 2.47(2) . . ? C12 H13 2.041(10) . . ? C12 H126 2.625(10) . . ? C13 C15 2.36(2) . . ? C13 C16 2.79(2) . . ? C13 C121 2.53(2) . . ? C13 H14 2.082(16) . . ? C14 C16 2.446(17) . . ? C14 H13 2.059(18) . . ? C14 H15 2.022(17) . . ? C15 C161 2.486(19) . . ? C15 H14 2.038(13) . . ? C16 C162 2.48(2) . . ? C16 C166 2.47(2) . . ? C16 H15 2.049(12) . . ? C16 H162 2.661(11) . . ? C16 H166 2.637(11) . . ? C121 C123 2.40(2) . . ? C121 C124 2.79(2) . . ? C121 C125 2.44(2) . . ? C121 H122 2.059(9) . . ? C121 H126 2.065(8) . . ? C122 C124 2.37(2) . . ? C122 C125 2.786(15) . . ? C122 C126 2.403(13) . . ? C122 H123 2.025(14) . . ? C123 C125 2.400(14) . . ? C123 C126 2.757(17) . . ? C123 H122 2.036(15) . . ? C123 H124 2.021(15) . . ? C124 C126 2.42(2) . . ? C124 H123 1.996(10) . . ? C124 H125 2.100(10) . . ? C125 H124 2.086(16) . . ? C125 H126 2.070(18) . . ? C126 H125 2.085(15) . . ? C161 C163 2.38(3) . . ? C161 C164 2.76(4) . . ? C161 C165 2.40(3) . . ? C161 H15 2.622(13) . . ? C161 H162 2.038(13) . . ? C161 H166 2.074(14) . . ? C162 C164 2.38(4) . . ? C162 C165 2.71(3) . . ? C162 C166 2.37(2) . . ? C162 H163 2.063(18) . . ? C163 C165 2.34(4) . . ? C163 C166 2.74(3) . . ? C163 H162 2.03(3) . . ? C163 H164 2.13(3) . . ? C164 C166 2.35(4) . . ? C164 H163 2.07(4) . . ? C164 H165 1.99(4) . . ? C165 H164 1.92(3) . . ? C165 H166 2.09(3) . . ? C166 H165 2.02(2) . . ? O2 C22 2.368(14) . . ? O2 C26 2.399(12) . . ? O2 C221 2.804(13) . . ? O2 C222 2.935(16) . . ? O2 C261 2.851(13) . . ? O2 H222 2.663(9) . . ? C21 C23 2.401(17) . . ? C21 C24 2.782(16) . . ? C21 C25 2.432(15) . . ? C21 C221 2.472(15) . . ? C21 C261 2.534(16) . . ? C22 C24 2.397(16) . . ? C22 C25 2.790(17) . . ? C22 C26 2.441(17) . . ? C22 C222 2.552(19) . . ? C22 C226 2.498(14) . . ? C22 H23 2.062(12) . . ? C22 H226 2.659(10) . . ? C23 C25 2.388(19) . . ? C23 C26 2.790(18) . . ? C23 C221 2.502(16) . . ? C23 H24 2.016(13) . . ? C24 C26 2.427(17) . . ? C24 H23 2.021(14) . . ? C24 H25 2.069(14) . . ? C25 C261 2.498(17) . . ? C25 H24 2.068(13) . . ? C26 C262 2.51(2) . . ? C26 C266 2.528(16) . . ? C26 H25 2.055(10) . . ? C26 H262 2.650(14) . . ? C221 C223 2.42(2) . . ? C221 C224 2.823(17) . . ? C221 C225 2.407(14) . . ? C221 H23 2.662(11) . . ? C221 H222 2.114(12) . . ? C221 H226 2.043(11) . . ? C222 C224 2.397(14) . . ? C222 C225 2.752(16) . . ? C222 C226 2.421(19) . . ? C222 H223 2.011(13) . . ? C223 C225 2.33(2) . . ? C223 C226 2.74(2) . . ? C223 H222 2.046(11) . . ? C223 H224 2.037(11) . . ? C224 C226 2.42(2) . . ? C224 H223 2.016(16) . . ? C224 H225 2.047(17) . . ? C225 H224 2.064(18) . . ? C225 H226 2.059(17) . . ? C226 H225 2.048(10) . . ? C261 C263 2.42(3) . . ? C261 C264 2.82(2) . . ? C261 C265 2.386(17) . . ? C261 H25 2.665(11) . . ? C261 H262 2.058(14) . . ? C261 H266 2.050(13) . . ? C262 C264 2.39(2) . . ? C262 C265 2.70(2) . . ? C262 C266 2.38(2) . . ? C262 H263 2.021(18) . . ? C263 C265 2.34(3) . . ? C263 C266 2.74(3) . . ? C263 H262 2.040(19) . . ? C263 H264 2.074(18) . . ? C264 C266 2.40(2) . . ? C264 H263 2.050(19) . . ? C264 H265 2.03(2) . . ? C265 H264 2.055(17) . . ? C265 H266 2.038(16) . . ? C266 H265 2.011(12) . . ? O3 C32 2.388(16) . . ? O3 C36 2.397(10) . . ? O3 C321 2.879(18) . . ? O3 C322 2.935(17) . . ? O3 C361 2.869(14) . . ? O3 C362 2.951(18) . . ? O3 H322 2.567(9) . . ? O3 H362 2.579(9) . . ? C31 C33 2.434(19) . . ? C31 C34 2.784(14) . . ? C31 C35 2.408(12) . . ? C31 C321 2.55(2) . . ? C31 C361 2.53(2) . . ? C32 C34 2.406(13) . . ? C32 C35 2.788(16) . . ? C32 C36 2.45(2) . . ? C32 C322 2.514(13) . . ? C32 C326 2.49(2) . . ? C32 H33 2.075(13) . . ? C32 H322 2.672(10) . . ? C32 H326 2.658(14) . . ? C33 C35 2.40(2) . . ? C33 C36 2.82(2) . . ? C33 C321 2.489(13) . . ? C33 H34 2.049(10) . . ? C34 C36 2.43(2) . . ? C34 H33 2.055(16) . . ? C34 H35 2.055(17) . . ? C35 C361 2.50(2) . . ? C35 H34 2.065(14) . . ? C36 C362 2.49(2) . . ? C36 C366 2.48(2) . . ? C36 H35 2.061(8) . . ? C36 H362 2.672(12) . . ? C36 H366 2.626(13) . . ? C321 C323 2.396(15) . . ? C321 C324 2.764(18) . . ? C321 C325 2.43(2) . . ? C321 H33 2.631(9) . . ? C321 H322 2.051(13) . . ? C321 H326 2.052(13) . . ? C322 C324 2.38(2) . . ? C322 C325 2.78(2) . . ? C322 C326 2.39(2) . . ? C322 H323 2.043(10) . . ? C323 C325 2.39(2) . . ? C323 C326 2.741(17) . . ? C323 H322 2.043(17) . . ? C323 H324 2.032(17) . . ? C324 C326 2.372(17) . . ? C324 H323 2.050(16) . . ? C324 H325 2.020(16) . . ? C325 H324 2.019(13) . . ? C325 H326 2.071(14) . . ? C326 H325 2.088(16) . . ? C361 C363 2.41(2) . . ? C361 C364 2.77(3) . . ? C361 C365 2.40(3) . . ? C361 H35 2.668(11) . . ? C361 H362 2.046(10) . . ? C361 H366 2.052(11) . . ? C362 C364 2.39(3) . . ? C362 C365 2.73(2) . . ? C362 C366 2.354(18) . . ? C362 H363 2.107(17) . . ? C363 C365 2.36(2) . . ? C363 C366 2.75(2) . . ? C363 H362 2.10(2) . . ? C363 H364 2.06(2) . . ? C364 C366 2.38(3) . . ? C364 H363 2.03(2) . . ? C364 H365 2.06(2) . . ? C365 H364 2.00(2) . . ? C365 H366 2.06(3) . . ? C366 H365 2.032(18) . . ? H13 H14 2.3844(4) . . ? H14 H15 2.3258(4) . . ? H122 H123 2.3307(4) . . ? H123 H124 2.2939(4) . . ? H125 H126 2.3930(4) . . ? H126 H35 2.3504(3) . 2 ? H162 H163 2.3646(4) . . ? H164 H165 2.2122(3) . . ? H165 H166 2.3362(4) . . ? H23 H24 2.3151(3) . . ? H24 H25 2.3767(4) . . ? H222 H223 2.3135(3) . . ? H223 H224 2.3353(4) . . ? H224 H225 2.3641(3) . . ? H225 H226 2.3543(3) . . ? H226 H226 2.3628(3) . '2 655' ? H262 H263 2.3334(4) . . ? H263 H264 2.3842(4) . . ? H264 H265 2.3486(4) . . ? H265 H266 2.3165(4) . . ? H266 H266 2.2074(4) . '2 666' ? H33 H34 2.3690(3) . . ? H34 H35 2.3523(4) . . ? H322 H323 2.3504(4) . . ? H323 H324 2.3390(3) . . ? H324 H325 2.3123(3) . . ? H325 H326 2.3998(4) . . ? H363 H364 2.3711(4) . . ? H364 H365 2.3147(4) . . ? H365 H366 2.3366(3) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 852 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 18 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min -12 _reflns_limit_l_max 12 _reflns_number_observed ? _reflns_d_resolution_high .847 _reflns_d_resolution_low 15.215 _diffrn_reflns_av_sigmaI/netI .152 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .122 _refine_ls_wR_factor_all .128 _refine_ls_goodness_of_fit_all 2.995 _refine_ls_shift/su_mean .013 data_prodpp _audit_creation_date 98-05-05 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum C54_O3_H39_Pr1 #ActaC _chemical_formula_weight 876.81 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-NONIUS software' #ActaC _computing_cell_refinement 'Enraf-NONIUS software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 15.827(6) #ActaC _cell_length_b 13.506(5) #ActaC _cell_length_c 11.012(3) #ActaC _cell_angle_alpha 116.39(3) #ActaC _cell_angle_beta 92.77(3) #ActaC _cell_angle_gamma 101.30(2) #ActaC _cell_volume 2043.0(14) #ActaC _cell_formula_units_Z 2 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used ? #ActaC _cell_measurement_theta_min ? #ActaC _cell_measurement_theta_max ? #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description needle #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max 0.62 #ActaC _exptl_crystal_size_mid 0.16 #ActaC _exptl_crystal_size_min 0.10 #ActaC _exptl_crystal_density_diffrn 1.425 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 892 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 1.24 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.826 #ActaC _exptl_absorpt_correction_T_max 0.885 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/theta #ActaC _diffrn_standards_number ? #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number .132680+05 #ActaC _diffrn_reflns_av_R_equivalents .032 #ActaC _diffrn_reflns_av_sigmaI/netI .069 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 18 #ActaC _diffrn_reflns_limit_k_min -16 #ActaC _diffrn_reflns_limit_k_max 15 #ActaC _diffrn_reflns_limit_l_min -13 #ActaC _diffrn_reflns_limit_l_max 13 #ActaC _diffrn_reflns_theta_min 1.33 #ActaC _diffrn_reflns_theta_max 24.97 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 108 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 6 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 78 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Pr ? 0 2 -.53 2.845 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Pr .279549(17) .20494(2) .22620(3) .04171(13) Uani ? ? O1 .2248(2) .3361(3) .2046(3) .0524(16) Uani ? ? C11 .1821(3) .4144(4) .2761(5) .044(2) Uani ? ? C12 .1587(3) .4218(4) .4002(5) .044(2) Uani ? ? C13 .1156(4) .5037(4) .4783(6) .058(3) Uani ? ? C14 .0945(4) .5771(5) .4319(7) .067(3) Uani ? ? C15 .1157(4) .5680(4) .3089(6) .060(3) Uani ? ? C16 .1594(3) .4885(4) .2296(5) .049(2) Uani ? ? C121 .1806(3) .3378(4) .4390(5) .047(2) Uani ? ? C122 .2599(3) .3573(4) .5161(5) .053(2) Uani ? ? C123 .2827(3) .2707(5) .5363(6) .059(3) Uani ? ? C124 .2275(4) .1636(5) .4798(6) .062(3) Uani ? ? C125 .1487(4) .1410(5) .4011(7) .065(3) Uani ? ? C126 .1252(3) .2274(5) .3817(6) .059(3) Uani ? ? C161 .1815(4) .4807(5) .0967(6) .059(3) Uani ? ? C162 .1163(6) .4391(6) -.0165(8) .099(4) Uani ? ? C163 .1367(10) .4331(8) -.1387(11) .144(8) Uani ? ? C164 .2222(12) .4723(11) -.1459(12) .168(11) Uani ? ? C165 .2861(8) .5170(12) -.0371(14) .161(8) Uani ? ? C166 .2661(5) .5187(8) .0858(8) .107(5) Uani ? ? O2 .4175(2) .2673(3) .3168(3) .0492(15) Uani ? ? C21 .5009(3) .2752(4) .3019(5) .045(2) Uani ? ? C22 .5242(3) .2426(4) .1709(5) .050(2) Uani ? ? C23 .6112(4) .2472(5) .1548(6) .063(3) Uani ? ? C24 .6752(4) .2849(5) .2671(7) .071(3) Uani ? ? C25 .6516(3) .3147(5) .3936(6) .063(3) Uani ? ? C26 .5654(3) .3117(4) .4162(5) .047(2) Uani ? ? C221 .4541(3) .1975(4) .0484(5) .051(2) Uani ? ? C222 .3939(3) .2590(4) .0455(5) .053(2) Uani ? ? C223 .3274(4) .2140(5) -.0658(6) .064(3) Uani ? ? C224 .3211(4) .1086(6) -.1729(6) .077(3) Uani ? ? C225 .3804(5) .0472(6) -.1727(6) .083(3) Uani ? ? C226 .4475(4) .0907(5) -.0632(6) .066(3) Uani ? ? C261 .5401(3) .3383(4) .5531(5) .047(2) Uani ? ? C262 .5467(5) .2670(5) .6122(7) .078(3) Uani ? ? C263 .5204(5) .2878(7) .7368(8) .096(4) Uani ? ? C264 .4882(5) .3804(6) .8068(6) .080(3) Uani ? ? C265 .4814(4) .4526(5) .7527(6) .066(3) Uani ? ? C266 .5068(4) .4305(5) .6269(6) .058(3) Uani ? ? O3 .2120(2) .0346(3) .0787(3) .0528(16) Uani ? ? C31 .1756(3) -.0775(4) .0118(5) .045(2) Uani ? ? C32 .1932(3) -.1495(4) .0653(5) .048(2) Uani ? ? C33 .1520(4) -.2649(4) -.0030(6) .056(2) Uani ? ? C34 .0951(4) -.3098(4) -.1243(6) .062(3) Uani ? ? C35 .0795(3) -.2398(4) -.1784(5) .051(2) Uani ? ? C36 .1177(3) -.1236(4) -.1130(5) .047(2) Uani ? ? C321 .2553(3) -.1037(4) .1939(5) .052(2) Uani ? ? C322 .3362(4) -.0304(5) .2165(6) .060(3) Uani ? ? C323 .3947(4) .0129(5) .3363(6) .066(3) Uani ? ? C324 .3731(4) -.0182(5) .4364(7) .075(3) Uani ? ? C325 .2942(5) -.0936(5) .4155(6) .073(3) Uani ? ? C326 .2354(4) -.1350(5) .2947(6) .064(3) Uani ? ? C361 .1001(3) -.0509(4) -.1752(5) .049(2) Uani ? ? C362 .0749(4) .0506(5) -.0997(6) .063(3) Uani ? ? C363 .0586(5) .1172(6) -.1602(8) .084(4) Uani ? ? C364 .0666(5) .0852(7) -.2938(9) .089(4) Uani ? ? C365 .0905(4) -.0150(6) -.3707(7) .077(3) Uani ? ? C366 .1068(4) -.0830(5) -.3129(6) .064(3) Uani ? ? H13 .10114 .50852 .56655 .07200 Uiso ? ? H14 .06447 .63578 .48727 .08300 Uiso ? ? H15 .09922 .61763 .27324 .07600 Uiso ? ? H122 .29985 .43236 .55454 .06400 Uiso ? ? H123 .33820 .28674 .59162 .07300 Uiso ? ? H124 .24358 .10296 .49355 .07700 Uiso ? ? H125 .10919 .06475 .35964 .08300 Uiso ? ? H126 .06929 .21145 .32396 .07300 Uiso ? ? H162 .05364 .41485 -.00779 .12900 Uiso ? ? H163 .09332 .40270 -.22416 .16800 Uiso ? ? H164 .23901 .46377 -.23223 .18700 Uiso ? ? H165 .34794 .55519 -.04107 .18500 Uiso ? ? H166 .31227 .54860 .16742 .13000 Uiso ? ? H23 .62713 .22362 .06158 .07900 Uiso ? ? H24 .73710 .29020 .25329 .08500 Uiso ? ? H25 .69712 .33861 .47240 .08000 Uiso ? ? H222 .39794 .33441 .12189 .06500 Uiso ? ? H223 .28538 .25786 -.06827 .07800 Uiso ? ? H224 .27506 .07526 -.25158 .09600 Uiso ? ? H225 .37722 -.02741 -.25004 .10000 Uiso ? ? H226 .49036 .04605 -.06443 .08200 Uiso ? ? H262 .57164 .19979 .56280 .09700 Uiso ? ? H263 .52631 .23755 .77586 .12000 Uiso ? ? H264 .46887 .39574 .89540 .09900 Uiso ? ? H265 .45776 .51928 .80321 .08200 Uiso ? ? H266 .50211 .48239 .58942 .07200 Uiso ? ? H33 .16267 -.31444 .03654 .06900 Uiso ? ? H34 .06523 -.39053 -.16994 .07500 Uiso ? ? H35 .04089 -.27245 -.26618 .06300 Uiso ? ? H322 .35338 -.00900 .14555 .07700 Uiso ? ? H323 .45081 .06516 .34970 .08300 Uiso ? ? H324 .41411 .01297 .52260 .09200 Uiso ? ? H325 .28030 -.11737 .48535 .09400 Uiso ? ? H326 .17892 -.18829 .28140 .08100 Uiso ? ? H362 .06779 .07227 -.00437 .07700 Uiso ? ? H363 .04023 .18860 -.10633 .10500 Uiso ? ? H364 .05680 .13314 -.33492 .10800 Uiso ? ? H365 .09544 -.03915 -.46861 .09800 Uiso ? ? H366 .12322 -.15490 -.36754 .08100 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Pr .03675(15) .03985(15) .04299(17) .00649(10) .00345(11) .01582(12) O1 .060(2) .053(2) .053(2) .0238(17) .0214(18) .0267(18) C11 .048(3) .041(3) .041(3) .008(2) .007(2) .016(2) C12 .041(3) .047(3) .046(3) .006(2) .012(2) .024(2) C13 .064(3) .051(3) .056(4) .011(3) .022(3) .021(3) C14 .068(4) .054(3) .081(4) .028(3) .032(3) .026(3) C15 .066(4) .051(3) .074(4) .023(3) .021(3) .034(3) C16 .047(3) .048(3) .056(3) .008(2) .009(2) .030(3) C121 .048(3) .051(3) .043(3) .014(2) .021(2) .021(2) C122 .059(3) .054(3) .038(3) .009(3) .009(2) .017(2) C123 .052(3) .081(4) .048(3) .012(3) .002(3) .036(3) C124 .058(4) .074(4) .073(4) .022(3) .023(3) .049(3) C125 .050(3) .063(4) .091(5) .004(3) .015(3) .047(3) C126 .041(3) .065(4) .078(4) .009(3) .010(3) .041(3) C161 .080(4) .052(3) .059(4) .030(3) .020(3) .030(3) C162 .158(8) .060(4) .070(5) .006(4) -.009(5) .032(4) C163 .273(16) .079(6) .074(7) .036(8) -.009(9) .037(5) C164 .34(2) .162(12) .069(7) .163(15) .095(12) .069(8) C165 .180(11) .271(15) .171(11) .151(11) .135(10) .174(12) C166 .105(6) .185(9) .105(6) .076(6) .059(5) .111(7) O2 .0350(18) .066(2) .045(2) .0087(16) .0074(15) .0267(17) C21 .039(3) .044(3) .050(3) .007(2) .006(2) .022(2) C22 .048(3) .048(3) .049(3) .009(2) .009(2) .020(2) C23 .050(3) .068(4) .063(4) .014(3) .017(3) .021(3) C24 .041(3) .086(4) .083(5) .017(3) .016(3) .035(4) C25 .043(3) .068(4) .072(4) .008(3) -.004(3) .030(3) C26 .042(3) .042(3) .053(3) .006(2) .003(2) .021(2) C221 .053(3) .057(3) .044(3) .005(3) .010(2) .027(3) C222 .053(3) .059(3) .048(3) .008(3) .013(3) .027(3) C223 .052(3) .082(4) .053(4) .009(3) .003(3) .032(3) C224 .067(4) .105(5) .047(4) -.002(4) .003(3) .035(4) C225 .105(6) .076(4) .040(4) -.001(4) .000(4) .013(3) C226 .087(4) .062(4) .048(4) .020(3) .015(3) .022(3) C261 .038(3) .047(3) .049(3) -.000(2) -.006(2) .021(2) C262 .104(5) .069(4) .076(5) .027(4) .002(4) .046(4) C263 .136(7) .101(6) .079(5) .024(5) .006(5) .068(5) C264 .089(5) .090(5) .049(4) -.007(4) .004(3) .035(4) C265 .072(4) .066(4) .049(4) .004(3) .008(3) .023(3) C266 .071(4) .054(3) .050(3) .007(3) .008(3) .028(3) O3 .070(2) .0408(19) .040(2) .0005(17) -.0012(17) .0185(16) C31 .045(3) .041(3) .044(3) .005(2) .007(2) .017(2) C32 .048(3) .054(3) .045(3) .009(2) .007(2) .026(2) C33 .062(3) .041(3) .063(4) .010(2) .006(3) .025(3) C34 .061(3) .044(3) .069(4) .004(3) -.000(3) .022(3) C35 .050(3) .045(3) .046(3) .003(2) -.004(2) .014(2) C36 .042(3) .046(3) .050(3) .008(2) .007(2) .021(2) C321 .059(3) .047(3) .051(3) .016(3) .007(3) .023(3) C322 .061(4) .061(3) .057(4) .020(3) .005(3) .024(3) C323 .062(4) .066(4) .067(4) .019(3) -.000(3) .027(3) C324 .077(4) .071(4) .075(5) .025(4) -.011(4) .031(4) C325 .110(5) .069(4) .056(4) .036(4) .008(4) .037(3) C326 .072(4) .059(4) .063(4) .010(3) .007(3) .032(3) C361 .042(3) .052(3) .051(3) .001(2) .002(2) .026(3) C362 .063(4) .059(3) .064(4) .011(3) .001(3) .028(3) C363 .085(5) .073(4) .100(6) .016(4) -.002(4) .048(4) C364 .080(5) .096(6) .111(7) -.001(4) -.011(4) .076(5) C365 .070(4) .091(5) .070(4) -.012(4) -.009(3) .051(4) C366 .053(3) .072(4) .062(4) .000(3) .003(3) .034(3) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme calc #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 5447 #ActaC _refine_ls_number_parameters 523 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .059 #ActaC _refine_ls_R_factor_obs .039 #ActaC _refine_ls_wR_factor_all .052 #ActaC _refine_ls_wR_factor_obs .046 #ActaC _refine_ls_goodness_of_fit_all 1.159 #ActaC _refine_ls_goodness_of_fit_obs 1.18 #ActaC _refine_ls_shift/esd_max .081 #ActaC _refine_ls_shift/esd_mean .003 #ActaC _refine_diff_density_min -1.212 #ActaC _refine_diff_density_max .651 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Pr O1 2.214(4) . . ? Pr C121 2.980(5) . . ? Pr C122 3.005(5) . . ? Pr C123 3.118(6) . . ? Pr C124 3.197(8) . . ? Pr C125 3.148(7) . . ? Pr C126 3.037(6) . . ? Pr O2 2.189(3) . . ? data_xvcb _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris(2,6-diphenylphenolato)cerium(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H39 Ce O3' _chemical_formula_weight 875.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P(-1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.5685(4) _cell_length_b 13.3666(3) _cell_length_c 10.9262(1) _cell_angle_alpha 116.029(1) _cell_angle_beta 92.403(1) _cell_angle_gamma 100.750(1) _cell_volume 1987.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_process_details 'face indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CCD' _diffrn_measurement_method '180 x 1 deg phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number N/A _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17742 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 30.03 _reflns_number_total 10596 _reflns_number_gt 9570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski and Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Siemans, 1993)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+1.9874P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef N/A _refine_ls_number_reflns 10596 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce -0.721710(8) -0.795528(11) -1.768772(13) 0.01523(5) Uani 1 1 d . . . O1 O -0.77493(13) -0.65941(15) -1.79074(19) 0.0219(4) Uani 1 1 d . . . O2 O -0.58074(11) -0.73078(16) -1.67967(18) 0.0207(4) Uani 1 1 d . . . O3 O -0.79393(12) -0.96569(15) -1.92054(19) 0.0223(4) Uani 1 1 d . . . C11 C -0.81871(16) -0.5801(2) -1.7203(3) 0.0179(5) Uani 1 1 d . . . C12 C -0.84295(16) -0.5706(2) -1.5935(3) 0.0197(5) Uani 1 1 d . . . C121 C -0.81997(17) -0.6564(2) -1.5537(3) 0.0192(5) Uani 1 1 d . . . C122 C -0.73832(17) -0.6372(2) -1.4789(3) 0.0215(5) Uani 1 1 d . . . H122 H -0.6989 -0.5643 -1.4426 0.026 Uiso 1 1 calc R . . C123 C -0.71424(18) -0.7242(2) -1.4571(3) 0.0250(5) Uani 1 1 d . . . H123 H -0.6588 -0.7098 -1.4054 0.030 Uiso 1 1 calc R . . C124 C -0.77085(19) -0.8317(2) -1.5104(3) 0.0253(5) Uani 1 1 d . . . H124 H -0.7541 -0.8909 -1.4959 0.030 Uiso 1 1 calc R . . C125 C -0.85219(18) -0.8521(2) -1.5850(3) 0.0271(6) Uani 1 1 d . . . H125 H -0.8911 -0.9255 -1.6219 0.033 Uiso 1 1 calc R . . C126 C -0.87685(17) -0.7652(2) -1.6058(3) 0.0235(5) Uani 1 1 d . . . H126 H -0.9329 -0.7797 -1.6560 0.028 Uiso 1 1 calc R . . C13 C -0.88751(18) -0.4887(2) -1.5156(3) 0.0249(5) Uani 1 1 d . . . H13 H -0.9023 -0.4825 -1.4295 0.030 Uiso 1 1 calc R . . C14 C -0.91059(19) -0.4154(2) -1.5643(3) 0.0280(6) Uani 1 1 d . . . H14 H -0.9414 -0.3591 -1.5120 0.034 Uiso 1 1 calc R . . C15 C -0.88794(18) -0.4258(2) -1.6904(3) 0.0261(6) Uani 1 1 d . . . H15 H -0.9046 -0.3767 -1.7242 0.031 Uiso 1 1 calc R . . C16 C -0.84164(17) -0.5060(2) -1.7685(3) 0.0205(5) Uani 1 1 d . . . C161 C -0.8147(2) -0.5116(2) -1.9001(3) 0.0248(5) Uani 1 1 d . . . C162 C -0.8745(3) -0.5583(3) -2.0186(3) 0.0423(8) Uani 1 1 d . . . H162 H -0.9344 -0.5897 -2.0186 0.051 Uiso 1 1 calc R . . C163 C -0.8458(4) -0.5591(3) -2.1397(4) 0.0564(12) Uani 1 1 d . . . H163 H -0.8860 -0.5938 -2.2227 0.068 Uiso 1 1 calc R . . C164 C -0.7596(3) -0.5094(3) -2.1373(4) 0.0545(11) Uani 1 1 d . . . H164 H -0.7412 -0.5068 -2.2179 0.065 Uiso 1 1 calc R . . C165 C -0.7005(3) -0.4638(4) -2.0205(4) 0.0508(10) Uani 1 1 d . . . H165 H -0.6409 -0.4306 -2.0203 0.061 Uiso 1 1 calc R . . C166 C -0.7273(2) -0.4658(3) -1.9026(4) 0.0393(8) Uani 1 1 d . . . H166 H -0.6855 -0.4355 -1.8221 0.047 Uiso 1 1 calc R . . C21 C -0.49620(15) -0.7254(2) -1.6973(3) 0.0167(4) Uani 1 1 d . . . C22 C -0.47225(16) -0.7594(2) -1.8311(3) 0.0192(5) Uani 1 1 d . . . C221 C -0.54275(17) -0.8033(2) -1.9506(3) 0.0204(5) Uani 1 1 d . . . C222 C -0.60599(17) -0.7417(2) -1.9534(3) 0.0218(5) Uani 1 1 d . . . H222 H -0.6026 -0.6685 -1.8786 0.026 Uiso 1 1 calc R . . C223 C -0.67343(19) -0.7850(3) -2.0631(3) 0.0271(6) Uani 1 1 d . . . H223 H -0.7152 -0.7415 -2.0632 0.033 Uiso 1 1 calc R . . C224 C -0.6795(2) -0.8920(3) -2.1724(3) 0.0319(6) Uani 1 1 d . . . H224 H -0.7263 -0.9228 -2.2466 0.038 Uiso 1 1 calc R . . C225 C -0.6173(2) -0.9539(3) -2.1732(3) 0.0339(7) Uani 1 1 d . . . H225 H -0.6211 -1.0269 -2.2485 0.041 Uiso 1 1 calc R . . C226 C -0.5491(2) -0.9096(2) -2.0639(3) 0.0278(6) Uani 1 1 d . . . H226 H -0.5063 -0.9523 -2.0664 0.033 Uiso 1 1 calc R . . C23 C -0.38384(18) -0.7567(2) -1.8485(3) 0.0264(6) Uani 1 1 d . . . H23 H -0.3675 -0.7798 -1.9380 0.032 Uiso 1 1 calc R . . C24 C -0.31926(18) -0.7208(3) -1.7369(3) 0.0290(6) Uani 1 1 d . . . H24 H -0.2591 -0.7183 -1.7501 0.035 Uiso 1 1 calc R . . C25 C -0.34286(17) -0.6886(2) -1.6061(3) 0.0246(5) Uani 1 1 d . . . H25 H -0.2986 -0.6651 -1.5302 0.030 Uiso 1 1 calc R . . C26 C -0.43096(16) -0.6904(2) -1.5846(3) 0.0190(5) Uani 1 1 d . . . C261 C -0.45804(16) -0.6622(2) -1.4459(3) 0.0194(5) Uani 1 1 d . . . C262 C -0.4572(2) -0.7375(2) -1.3896(3) 0.0291(6) Uani 1 1 d . . . H262 H -0.4358 -0.8045 -1.4377 0.035 Uiso 1 1 calc R . . C263 C -0.4873(2) -0.7164(3) -1.2640(3) 0.0360(7) Uani 1 1 d . . . H263 H -0.4872 -0.7696 -1.2282 0.043 Uiso 1 1 calc R . . C264 C -0.5172(2) -0.6189(3) -1.1916(3) 0.0314(6) Uani 1 1 d . . . H264 H -0.5375 -0.6042 -1.1059 0.038 Uiso 1 1 calc R . . C265 C -0.51714(19) -0.5423(2) -1.2455(3) 0.0258(5) Uani 1 1 d . . . H265 H -0.5374 -0.4746 -1.1961 0.031 Uiso 1 1 calc R . . C266 C -0.48790(18) -0.5636(2) -1.3704(3) 0.0214(5) Uani 1 1 d . . . H266 H -0.4882 -0.5099 -1.4055 0.026 Uiso 1 1 calc R . . C31 C -0.82894(16) -1.0779(2) -1.9853(2) 0.0178(5) Uani 1 1 d . . . C32 C -0.80997(17) -1.1493(2) -1.9292(3) 0.0196(5) Uani 1 1 d . . . C321 C -0.74660(18) -1.1021(2) -1.8007(3) 0.0211(5) Uani 1 1 d . . . C322 C -0.66511(17) -1.0280(2) -1.7813(3) 0.0219(5) Uani 1 1 d . . . H322 H -0.6500 -1.0071 -1.8515 0.026 Uiso 1 1 calc R . . C323 C -0.60586(19) -0.9846(2) -1.6620(3) 0.0269(6) Uani 1 1 d . . . H323 H -0.5512 -0.9338 -1.6508 0.032 Uiso 1 1 calc R . . C324 C -0.6266(2) -1.0155(2) -1.5588(3) 0.0288(6) Uani 1 1 d . . . H324 H -0.5866 -0.9852 -1.4763 0.035 Uiso 1 1 calc R . . C325 C -0.7061(2) -1.0911(2) -1.5775(3) 0.0284(6) Uani 1 1 d . . . H325 H -0.7200 -1.1138 -1.5083 0.034 Uiso 1 1 calc R . . C326 C -0.7655(2) -1.1335(2) -1.6967(3) 0.0261(5) Uani 1 1 d . . . H326 H -0.8198 -1.1848 -1.7078 0.031 Uiso 1 1 calc R . . C33 C -0.85105(18) -1.2658(2) -1.9948(3) 0.0227(5) Uani 1 1 d . . . H33 H -0.8394 -1.3136 -1.9555 0.027 Uiso 1 1 calc R . . C34 C -0.90842(18) -1.3123(2) -2.1163(3) 0.0246(5) Uani 1 1 d . . . H34 H -0.9367 -1.3913 -2.1595 0.030 Uiso 1 1 calc R . . C35 C -0.92428(17) -1.2424(2) -2.1745(3) 0.0220(5) Uani 1 1 d . . . H35 H -0.9623 -1.2749 -2.2593 0.026 Uiso 1 1 calc R . . C36 C -0.88567(16) -1.1255(2) -2.1114(3) 0.0184(5) Uani 1 1 d . . . C361 C -0.90317(16) -1.0528(2) -2.1761(3) 0.0200(5) Uani 1 1 d . . . C362 C -0.92929(18) -0.9504(2) -2.1026(3) 0.0255(5) Uani 1 1 d . . . H362 H -0.9365 -0.9263 -2.0087 0.031 Uiso 1 1 calc R . . C363 C -0.9450(2) -0.8834(3) -2.1654(4) 0.0333(7) Uani 1 1 d . . . H363 H -0.9633 -0.8145 -2.1144 0.040 Uiso 1 1 calc R . . C364 C -0.9339(2) -0.9169(3) -2.3017(4) 0.0345(7) Uani 1 1 d . . . H364 H -0.9435 -0.8704 -2.3439 0.041 Uiso 1 1 calc R . . C365 C -0.9088(2) -1.0188(3) -2.3765(3) 0.0318(6) Uani 1 1 d . . . H365 H -0.9021 -1.0426 -2.4706 0.038 Uiso 1 1 calc R . . C366 C -0.89343(18) -1.0863(2) -2.3147(3) 0.0244(5) Uani 1 1 d . . . H366 H -0.8761 -1.1558 -2.3668 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01530(7) 0.01276(7) 0.01581(7) 0.00472(5) 0.00199(4) 0.00365(4) O1 0.0302(10) 0.0202(8) 0.0215(9) 0.0121(8) 0.0090(7) 0.0123(7) O2 0.0173(8) 0.0274(9) 0.0183(8) 0.0112(8) 0.0039(7) 0.0049(7) O3 0.0289(10) 0.0146(8) 0.0191(9) 0.0061(7) -0.0013(7) 0.0004(7) C11 0.0175(11) 0.0153(10) 0.0213(11) 0.0087(9) 0.0022(9) 0.0039(8) C12 0.0196(11) 0.0157(10) 0.0232(12) 0.0076(10) 0.0064(9) 0.0050(9) C121 0.0214(12) 0.0204(11) 0.0200(11) 0.0116(10) 0.0083(9) 0.0067(9) C122 0.0252(12) 0.0209(11) 0.0151(11) 0.0057(10) 0.0041(9) 0.0040(10) C123 0.0250(13) 0.0317(14) 0.0190(12) 0.0117(11) 0.0031(10) 0.0076(11) C124 0.0284(14) 0.0270(13) 0.0301(14) 0.0191(12) 0.0096(11) 0.0109(11) C125 0.0223(13) 0.0244(13) 0.0388(16) 0.0194(12) 0.0078(11) 0.0010(10) C126 0.0164(11) 0.0261(13) 0.0318(14) 0.0167(12) 0.0052(10) 0.0040(9) C13 0.0262(13) 0.0201(12) 0.0282(13) 0.0090(11) 0.0134(11) 0.0079(10) C14 0.0303(14) 0.0195(12) 0.0364(15) 0.0110(12) 0.0168(12) 0.0120(11) C15 0.0277(13) 0.0189(12) 0.0358(15) 0.0141(11) 0.0090(11) 0.0095(10) C16 0.0212(12) 0.0163(11) 0.0244(12) 0.0094(10) 0.0050(10) 0.0043(9) C161 0.0383(15) 0.0198(12) 0.0234(13) 0.0126(11) 0.0084(11) 0.0146(11) C162 0.067(2) 0.0200(13) 0.0326(17) 0.0104(13) -0.0083(16) 0.0000(14) C163 0.114(4) 0.0207(14) 0.0239(16) 0.0049(13) -0.0127(19) 0.0100(19) C164 0.101(4) 0.045(2) 0.0306(18) 0.0192(16) 0.031(2) 0.037(2) C165 0.059(2) 0.073(3) 0.048(2) 0.042(2) 0.0322(19) 0.036(2) C166 0.0382(17) 0.062(2) 0.0373(17) 0.0336(17) 0.0167(14) 0.0242(16) C21 0.0160(10) 0.0154(10) 0.0184(11) 0.0077(9) 0.0019(9) 0.0028(8) C22 0.0209(12) 0.0174(11) 0.0193(11) 0.0080(10) 0.0049(9) 0.0045(9) C221 0.0213(12) 0.0224(12) 0.0174(11) 0.0099(10) 0.0057(9) 0.0023(9) C222 0.0238(12) 0.0242(12) 0.0173(11) 0.0104(10) 0.0056(9) 0.0023(10) C223 0.0252(13) 0.0367(15) 0.0228(13) 0.0176(12) 0.0042(10) 0.0039(11) C224 0.0293(14) 0.0396(16) 0.0206(13) 0.0137(12) -0.0009(11) -0.0051(12) C225 0.0478(18) 0.0272(14) 0.0171(12) 0.0051(11) 0.0020(12) 0.0000(13) C226 0.0369(15) 0.0261(13) 0.0197(12) 0.0092(11) 0.0076(11) 0.0077(11) C23 0.0244(13) 0.0287(13) 0.0254(13) 0.0103(11) 0.0118(11) 0.0079(11) C24 0.0158(12) 0.0343(15) 0.0351(15) 0.0137(13) 0.0074(11) 0.0062(10) C25 0.0181(12) 0.0242(12) 0.0294(14) 0.0109(11) 0.0006(10) 0.0040(10) C26 0.0186(11) 0.0168(11) 0.0217(12) 0.0087(10) 0.0027(9) 0.0041(9) C261 0.0200(11) 0.0164(10) 0.0188(11) 0.0071(9) -0.0024(9) 0.0008(9) C262 0.0367(16) 0.0233(13) 0.0302(14) 0.0142(12) -0.0003(12) 0.0091(11) C263 0.0493(19) 0.0331(15) 0.0327(16) 0.0246(14) 0.0009(14) 0.0018(14) C264 0.0367(16) 0.0349(15) 0.0196(13) 0.0146(12) 0.0032(11) -0.0039(12) C265 0.0289(14) 0.0241(12) 0.0208(12) 0.0087(11) 0.0039(10) 0.0015(10) C266 0.0278(13) 0.0179(11) 0.0194(12) 0.0099(10) 0.0029(10) 0.0040(10) C31 0.0203(11) 0.0134(10) 0.0164(11) 0.0040(9) 0.0036(9) 0.0032(8) C32 0.0225(12) 0.0170(11) 0.0180(11) 0.0070(9) 0.0034(9) 0.0042(9) C321 0.0275(13) 0.0179(11) 0.0177(11) 0.0073(10) 0.0020(10) 0.0076(10) C322 0.0237(12) 0.0221(12) 0.0223(12) 0.0109(10) 0.0057(10) 0.0082(10) C323 0.0235(13) 0.0246(13) 0.0284(14) 0.0078(11) 0.0007(11) 0.0075(10) C324 0.0334(15) 0.0275(13) 0.0242(13) 0.0090(11) -0.0027(11) 0.0130(11) C325 0.0416(16) 0.0255(13) 0.0234(13) 0.0140(11) 0.0042(12) 0.0124(12) C326 0.0327(14) 0.0224(12) 0.0246(13) 0.0123(11) 0.0029(11) 0.0057(11) C33 0.0254(13) 0.0184(11) 0.0253(13) 0.0110(10) 0.0025(10) 0.0052(10) C34 0.0256(13) 0.0148(11) 0.0290(14) 0.0077(10) 0.0000(11) 0.0009(9) C35 0.0214(12) 0.0184(11) 0.0213(12) 0.0052(10) -0.0007(9) 0.0037(9) C36 0.0179(11) 0.0169(11) 0.0194(11) 0.0068(9) 0.0033(9) 0.0055(9) C361 0.0193(11) 0.0172(11) 0.0224(12) 0.0095(10) 0.0002(9) 0.0008(9) C362 0.0268(13) 0.0247(13) 0.0271(13) 0.0132(11) 0.0038(11) 0.0071(10) C363 0.0348(16) 0.0267(14) 0.0422(17) 0.0182(14) 0.0030(13) 0.0097(12) C364 0.0323(15) 0.0376(16) 0.0430(18) 0.0298(15) -0.0016(13) 0.0014(13) C365 0.0294(15) 0.0396(16) 0.0260(14) 0.0192(13) -0.0022(11) -0.0028(12) C366 0.0232(12) 0.0232(12) 0.0227(12) 0.0088(11) 0.0009(10) 0.0007(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O3 2.183(2) . ? Ce1 O2 2.2105(19) . ? Ce1 O1 2.2323(18) . ? Ce1 C121 2.975(3) . ? Ce1 C222 2.989(3) . ? Ce1 C122 2.995(3) . ? Ce1 C126 3.043(3) . ? Ce1 C123 3.098(3) . ? Ce1 C125 3.135(3) . ? Ce1 C124 3.167(3) . ? O1 C11 1.333(3) . ? O2 C21 1.331(3) . ? O3 C31 1.334(3) . ? C11 C16 1.401(3) . ? C11 C12 1.409(4) . ? C12 C13 1.385(3) . ? C12 C121 1.487(3) . ? C121 C122 1.399(4) . ? C121 C126 1.405(4) . ? C122 C123 1.395(4) . ? C123 C124 1.390(4) . ? C124 C125 1.390(4) . ? C125 C126 1.392(4) . ? C13 C14 1.395(4) . ? C14 C15 1.390(4) . ? C15 C16 1.390(4) . ? C16 C161 1.489(4) . ? C161 C162 1.380(4) . ? C161 C166 1.391(5) . ? C162 C163 1.410(6) . ? C163 C164 1.375(7) . ? C164 C165 1.363(6) . ? C165 C166 1.381(5) . ? C21 C26 1.407(3) . ? C21 C22 1.417(3) . ? C22 C23 1.393(4) . ? C22 C221 1.490(4) . ? C221 C226 1.398(4) . ? C221 C222 1.405(4) . ? C222 C223 1.390(4) . ? C223 C224 1.386(4) . ? C224 C225 1.385(5) . ? C225 C226 1.393(4) . ? C23 C24 1.390(4) . ? C24 C25 1.388(4) . ? C25 C26 1.399(4) . ? C26 C261 1.493(4) . ? C261 C262 1.392(4) . ? C261 C266 1.393(4) . ? C262 C263 1.396(5) . ? C263 C264 1.375(5) . ? C264 C265 1.387(4) . ? C265 C266 1.382(4) . ? C31 C32 1.406(3) . ? C31 C36 1.415(3) . ? C32 C33 1.399(4) . ? C32 C321 1.488(4) . ? C321 C326 1.398(4) . ? C321 C322 1.400(4) . ? C322 C323 1.386(4) . ? C323 C324 1.391(4) . ? C324 C325 1.388(4) . ? C325 C326 1.389(4) . ? C33 C34 1.384(4) . ? C34 C35 1.391(4) . ? C35 C36 1.395(3) . ? C36 C361 1.484(3) . ? C361 C362 1.397(4) . ? C361 C366 1.403(4) . ? C362 C363 1.392(4) . ? C363 C364 1.384(5) . ? C364 C365 1.387(5) . ? C365 C366 1.389(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ce1 O2 130.55(8) . . ? O3 Ce1 O1 111.21(7) . . ? O2 Ce1 O1 110.38(8) . . ? O3 Ce1 C121 117.14(8) . . ? O2 Ce1 C121 106.03(8) . . ? O1 Ce1 C121 60.41(7) . . ? O3 Ce1 C222 97.59(8) . . ? O2 Ce1 C222 66.84(7) . . ? O1 Ce1 C222 77.56(8) . . ? C121 Ce1 C222 132.28(7) . . ? O3 Ce1 C122 134.81(8) . . ? O2 Ce1 C122 80.13(8) . . ? O1 Ce1 C122 76.86(7) . . ? C121 Ce1 C122 27.11(7) . . ? C222 Ce1 C122 127.10(8) . . ? O3 Ce1 C126 90.95(8) . . ? O2 Ce1 C126 125.51(7) . . ? O1 Ce1 C126 74.18(7) . . ? C121 Ce1 C126 26.97(7) . . ? C222 Ce1 C126 151.69(7) . . ? C122 Ce1 C126 46.98(8) . . ? O3 Ce1 C123 120.54(8) . . ? O2 Ce1 C123 73.30(8) . . ? O1 Ce1 C123 103.12(8) . . ? C121 Ce1 C123 47.08(7) . . ? C222 Ce1 C123 137.18(8) . . ? C122 Ce1 C123 26.40(7) . . ? C126 Ce1 C123 53.74(8) . . ? O3 Ce1 C125 81.08(8) . . ? O2 Ce1 C125 116.22(7) . . ? O1 Ce1 C125 100.17(7) . . ? C121 Ce1 C125 46.85(7) . . ? C222 Ce1 C125 176.81(7) . . ? C122 Ce1 C125 53.93(8) . . ? C126 Ce1 C125 25.99(7) . . ? C123 Ce1 C125 45.33(8) . . ? O3 Ce1 C124 94.99(8) . . ? O2 Ce1 C124 91.00(7) . . ? O1 Ce1 C124 114.70(7) . . ? C121 Ce1 C124 54.40(7) . . ? C222 Ce1 C124 157.68(7) . . ? C122 Ce1 C124 46.08(7) . . ? C126 Ce1 C124 45.66(7) . . ? C123 Ce1 C124 25.61(8) . . ? C125 Ce1 C124 25.48(7) . . ? C11 O1 Ce1 138.23(16) . . ? C21 O2 Ce1 149.19(16) . . ? C31 O3 Ce1 162.89(17) . . ? O1 C11 C16 122.1(2) . . ? O1 C11 C12 119.1(2) . . ? C16 C11 C12 118.8(2) . . ? C13 C12 C11 121.4(2) . . ? C13 C12 C121 123.4(2) . . ? C11 C12 C121 115.2(2) . . ? C122 C121 C126 118.2(2) . . ? C122 C121 C12 121.9(2) . . ? C126 C121 C12 119.4(2) . . ? C122 C121 Ce1 77.23(15) . . ? C126 C121 Ce1 79.22(15) . . ? C12 C121 Ce1 106.93(16) . . ? C123 C122 C121 120.7(2) . . ? C123 C122 Ce1 80.94(16) . . ? C121 C122 Ce1 75.66(15) . . ? C124 C123 C122 120.4(3) . . ? C124 C123 Ce1 79.98(17) . . ? C122 C123 Ce1 72.66(15) . . ? C123 C124 C125 119.6(3) . . ? C123 C124 Ce1 74.41(16) . . ? C125 C124 Ce1 75.99(17) . . ? C124 C125 C126 120.2(3) . . ? C124 C125 Ce1 78.54(16) . . ? C126 C125 Ce1 73.29(16) . . ? C125 C126 C121 120.9(2) . . ? C125 C126 Ce1 80.72(17) . . ? C121 C126 Ce1 73.81(15) . . ? C12 C13 C14 119.7(3) . . ? C15 C14 C13 119.1(2) . . ? C14 C15 C16 122.0(3) . . ? C15 C16 C11 119.1(3) . . ? C15 C16 C161 120.8(2) . . ? C11 C16 C161 120.1(2) . . ? C162 C161 C166 119.1(3) . . ? C162 C161 C16 121.9(3) . . ? C166 C161 C16 119.0(3) . . ? C161 C162 C163 119.6(4) . . ? C164 C163 C162 119.8(4) . . ? C165 C164 C163 120.7(4) . . ? C164 C165 C166 119.9(4) . . ? C165 C166 C161 120.9(3) . . ? O2 C21 C26 120.3(2) . . ? O2 C21 C22 119.8(2) . . ? C26 C21 C22 119.8(2) . . ? C23 C22 C21 119.2(2) . . ? C23 C22 C221 121.6(2) . . ? C21 C22 C221 119.2(2) . . ? C226 C221 C222 117.4(2) . . ? C226 C221 C22 120.6(2) . . ? C222 C221 C22 122.0(2) . . ? C223 C222 C221 121.6(3) . . ? C223 C222 Ce1 94.31(17) . . ? C221 C222 Ce1 98.26(16) . . ? C224 C223 C222 119.8(3) . . ? C225 C224 C223 119.8(3) . . ? C224 C225 C226 120.3(3) . . ? C225 C226 C221 121.1(3) . . ? C24 C23 C22 121.0(3) . . ? C25 C24 C23 119.8(2) . . ? C24 C25 C26 120.8(3) . . ? C25 C26 C21 119.4(2) . . ? C25 C26 C261 121.4(2) . . ? C21 C26 C261 119.1(2) . . ? C262 C261 C266 117.5(3) . . ? C262 C261 C26 120.2(2) . . ? C266 C261 C26 122.2(2) . . ? C261 C262 C263 121.2(3) . . ? C264 C263 C262 120.3(3) . . ? C263 C264 C265 119.1(3) . . ? C266 C265 C264 120.6(3) . . ? C265 C266 C261 121.2(2) . . ? O3 C31 C32 120.5(2) . . ? O3 C31 C36 119.7(2) . . ? C32 C31 C36 119.8(2) . . ? C33 C32 C31 119.6(2) . . ? C33 C32 C321 119.8(2) . . ? C31 C32 C321 120.6(2) . . ? C326 C321 C322 117.6(2) . . ? C326 C321 C32 120.8(2) . . ? C322 C321 C32 121.6(2) . . ? C323 C322 C321 121.6(3) . . ? C322 C323 C324 119.9(3) . . ? C325 C324 C323 119.5(3) . . ? C324 C325 C326 120.4(3) . . ? C325 C326 C321 121.1(3) . . ? C34 C33 C32 120.9(2) . . ? C33 C34 C35 119.4(2) . . ? C34 C35 C36 121.6(2) . . ? C35 C36 C31 118.7(2) . . ? C35 C36 C361 120.6(2) . . ? C31 C36 C361 120.7(2) . . ? C362 C361 C366 118.2(2) . . ? C362 C361 C36 121.9(2) . . ? C366 C361 C36 119.9(2) . . ? C363 C362 C361 120.9(3) . . ? C364 C363 C362 120.2(3) . . ? C363 C364 C365 119.7(3) . . ? C364 C365 C366 120.4(3) . . ? C365 C366 C361 120.7(3) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 1.597 _refine_diff_density_min -1.458 _refine_diff_density_rms 0.109 data_ladpp2 _audit_creation_date 98-11-20 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum C54_H39_O3_La1 #ActaC _chemical_formula_weight 874.81 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf NONIUS software' #ActaC _computing_cell_refinement 'Enraf NONIUS software' #ActaC _computing_data_reduction xtal_DIFDAT_SORTRF_ADDREF_ABSORB #ActaC _computing_structure_smlution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA]CIFIO #ActaC _cell_length_a 15.703(6) #ActaC _cell_length_b 13.537(5) #ActaC _cell_length_c 10.391(3) #ActaC _cell_angle_alpha 95.79(3) #ActaC _cell_angle_beta 104.77(3) #ActaC _cell_angle_gamma 102.13(3) #ActaC _cell_volume 2060.1(13) #ActaC _cell_formula_units_Z 2 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used ? #ActaC _cell_measurement_theta_min ? #ActaC _cell_measurement_theta_max ? #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M ? #ActaC _symmetry_space_group_name_Hall -P_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description prism #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max 0.40 #ActaC _exptl_crystal_size_mid 0.20 #ActaC _exptl_crystal_size_min 0.20 #ActaC _exptl_crystal_density_diffrn 1.41 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 887.87 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 1.08 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.786 #ActaC _exptl_absorpt_correction_T_max 0.843 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/theta #ActaC _diffrn_standards_number ? #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time ? #ActaC _diffrn_standards_decay_% ? #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 7232 #ActaC _diffrn_reflns_av_R_equivalents ? #ActaC _diffrn_reflns_av_sigmaI/netI 0 #ActaC _diffrn_reflns_limit_h_min -18 #ActaC _diffrn_reflns_limit_h_max 17 #ActaC _diffrn_reflns_limit_k_min -16 #ActaC _diffrn_reflns_limit_k_max 15 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 12 #ActaC _diffrn_reflns_theta_min 1.38 #ActaC _diffrn_reflns_theta_max 24.98 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 108 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 78 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 6 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 La ? 0 2 -.588 2.452 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC La .78674(3) .69576(3) .52781(5) .0450(2) Uani ? ? O1 .6975(3) .5376(3) .4986(4) .057(2) Uani ? ? C11 .6663(4) .4669(5) .5675(7) .046(3) Uani ? ? C12 .7005(4) .4836(5) .7079(7) .048(3) Uani ? ? C121 .7713(4) .5806(5) .7681(6) .046(3) Uani ? ? C122 .7492(4) .6700(6) .8086(7) .057(4) Uani ? ? C123 .8138(5) .7613(6) .8478(7) .064(4) Uani ? ? C124 .9017(5) .7664(6) .8464(7) .061(4) Uani ? ? C125 .9256(4) .6797(6) .8062(7) .061(4) Uani ? ? C126 .8621(5) .5866(5) .7685(7) .057(4) Uani ? ? C13 .6683(5) .4127(5) .7810(7) .058(4) Uani ? ? C14 .6039(5) .3233(6) .7184(8) .065(4) Uani ? ? C15 .5707(4) .3079(5) .5789(8) .060(4) Uani ? ? C16 .6014(4) .3749(5) .5004(7) .048(3) Uani ? ? C161 .5685(5) .3577(5) .3517(8) .052(4) Uani ? ? C162 .5959(6) .2876(6) .2758(9) .081(5) Uani ? ? C163 .5684(7) .2736(7) .1357(11) .100(6) Uani ? ? C164 .5134(6) .3259(8) .0720(9) .091(6) Uani ? ? C165 .4838(5) .3943(8) .1412(11) .085(6) Uani ? ? C166 .5109(5) .4096(6) .2830(9) .068(4) Uani ? ? O2 .7158(3) .8207(3) .5484(4) .050(2) Uani ? ? C21 .6701(4) .8804(5) .4795(7) .042(3) Uani ? ? C22 .6509(4) .8635(5) .3366(7) .042(3) Uani ? ? C221 .6853(4) .7827(5) .2757(6) .043(3) Uani ? ? C222 .6440(5) .6801(6) .2599(7) .056(4) Uani ? ? C223 .6796(5) .6061(5) .2090(7) .058(4) Uani ? ? C224 .7585(5) .6337(6) .1701(7) .061(4) Uani ? ? C225 .8001(5) .7338(7) .1860(8) .069(5) Uani ? ? C226 .7651(5) .8096(5) .2361(7) .062(4) Uani ? ? C23 .6048(4) .9238(5) .2626(7) .056(4) Uani ? ? C24 .5774(5) 1.0026(6) .3208(8) .062(4) Uani ? ? C25 .5983(5) 1.0190(5) .4607(8) .059(4) Uani ? ? C26 .6423(4) .9601(5) .5417(7) .043(3) Uani ? ? C261 .6593(4) .9801(5) .6917(7) .052(4) Uani ? ? C262 .6864(6) 1.0784(6) .7599(9) .081(5) Uani ? ? C263 .6986(7) 1.0985(7) .8965(11) .106(6) Uani ? ? C264 .6781(6) 1.0239(8) .9654(8) .090(5) Uani ? ? C265 .6506(5) .9239(7) .9005(9) .074(5) Uani ? ? C266 .6404(5) .9040(6) .7624(8) .060(4) Uani ? ? O3 .9199(3) .7058(3) .4904(4) .054(2) Uani ? ? C31 1.0048(4) .7305(5) .4796(7) .051(4) Uani ? ? C32 1.0664(5) .8198(5) .5585(7) .053(4) Uani ? ? C321 1.0386(5) .8910(5) .6474(8) .059(4) Uani ? ? C322 .9605(6) .9252(6) .6030(7) .069(4) Uani ? ? C323 .9363(7) .9966(7) .6832(11) .089(6) Uani ? ? C324 .9940(9) 1.0322(7) .8147(13) .106(7) Uani ? ? C325 1.0693(8) 1.0002(8) .8609(10) .098(6) Uani ? ? C326 1.0923(5) .9300(6) .7791(9) .079(5) Uani ? ? C33 1.1559(5) .8395(6) .5501(7) .063(4) Uani ? ? C34 1.1814(5) .7766(6) .4639(9) .068(4) Uani ? ? C35 1.1199(5) .6929(6) .3827(8) .064(4) Uani ? ? C36 1.0305(4) .6660(5) .3898(7) .050(4) Uani ? ? C361 .9663(4) .5725(5) .3037(7) .052(4) Uani ? ? C362 .9135(5) .5013(6) .3560(7) .060(4) Uani ? ? C363 .8558(5) .4126(6) .2734(10) .075(5) Uani ? ? C364 .8478(6) .3954(7) .1388(10) .088(5) Uani ? ? C365 .8997(6) .4660(8) .0870(8) .079(5) Uani ? ? C366 .9581(5) .5542(6) .1663(8) .062(4) Uani ? ? H122 .68446 .66044 .80093 .04428 Uiso ? ? H123 .79611 .82909 .85973 .05986 Uiso ? ? H124 .94267 .82905 .86228 .04809 Uiso ? ? H125 .98097 .67609 .80320 .07217 Uiso ? ? H126 .87881 .52129 .73151 .06513 Uiso ? ? H13 .69399 .42284 .87290 .02791 Uiso ? ? H14 .58173 .27651 .76673 .05101 Uiso ? ? H15 .53520 .25267 .53001 .05085 Uiso ? ? H162 .64335 .24874 .32854 .06135 Uiso ? ? H163 .59649 .23249 .10738 .07674 Uiso ? ? H164 .48961 .31703 -.02486 .10952 Uiso ? ? H165 .44553 .42840 .10791 .05748 Uiso ? ? H166 .49414 .46286 .31926 .07725 Uiso ? ? H222 .59745 .66454 .28385 .05817 Uiso ? ? H223 .65243 .53457 .19574 .04145 Uiso ? ? H224 .78893 .57679 .14675 .07162 Uiso ? ? H225 .85246 .75235 .17335 .07229 Uiso ? ? H226 .79596 .88475 .25175 .04512 Uiso ? ? H23 .58450 .90972 .17609 .05366 Uiso ? ? H24 .54470 1.05146 .27562 .05652 Uiso ? ? H25 .58522 1.06813 .50245 .02706 Uiso ? ? H262 .69871 1.13487 .71193 .07491 Uiso ? ? H263 .71149 1.17316 .93613 .11958 Uiso ? ? H264 .68264 1.03148 1.06151 .07592 Uiso ? ? H265 .63784 .87666 .94206 .05716 Uiso ? ? H266 .61934 .83388 .71148 .02506 Uiso ? ? H322 .92964 .90146 .51935 .04432 Uiso ? ? H323 .87595 1.02010 .64802 .07417 Uiso ? ? H324 .97756 1.07869 .85640 .07099 Uiso ? ? H325 1.09673 1.02723 .94217 .12580 Uiso ? ? H326 1.14236 .90087 .82128 .06891 Uiso ? ? H33 1.19174 .90198 .59667 .07423 Uiso ? ? H34 1.24270 .79048 .46393 .06128 Uiso ? ? H35 1.13896 .64305 .33015 .04084 Uiso ? ? H362 .92537 .51871 .46479 .07813 Uiso ? ? H363 .82906 .36831 .31721 .07246 Uiso ? ? H364 .81290 .33630 .06884 .13274 Uiso ? ? H365 .90152 .46010 -.00616 .09090 Uiso ? ? H366 .98670 .60653 .13339 .06910 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC La .0358(2) .0418(2) .0569(3) .00708(16) .01435(18) .00810(19) O1 .064(3) .055(3) .040(3) -.006(2) .008(2) .008(2) C11 .041(4) .046(4) .053(5) .014(3) .011(4) .010(4) C12 .046(4) .044(4) .054(5) .012(3) .012(4) .017(4) C121 .048(4) .041(4) .043(4) .007(3) .004(3) .007(3) C122 .043(4) .062(5) .061(5) .008(4) .014(4) .002(4) C123 .061(5) .064(5) .058(5) .003(4) .018(4) -.013(4) C124 .062(5) .053(5) .053(5) -.002(4) .007(4) .001(4) C125 .037(4) .066(5) .070(6) .003(4) .008(4) .012(4) C126 .046(5) .052(5) .069(5) .013(4) .008(4) .010(4) C13 .065(5) .060(5) .040(4) .008(4) .006(4) .011(4) C14 .069(5) .057(5) .063(6) -.000(4) .016(5) .017(4) C15 .046(4) .043(4) .079(6) -.005(3) .012(4) .009(4) C16 .042(4) .037(4) .063(5) .004(3) .013(4) .007(4) C161 .040(4) .052(5) .055(5) -.005(4) .009(4) .003(4) C162 .084(6) .078(6) .074(7) .024(5) .012(5) -.005(5) C163 .099(8) .112(8) .079(8) .025(6) .020(6) -.023(6) C164 .066(6) .122(9) .065(7) .000(6) .004(5) .012(6) C165 .049(5) .114(8) .087(8) .018(5) .006(5) .031(6) C166 .056(5) .079(6) .063(6) .009(4) .014(4) .009(5) O2 .059(3) .059(3) .036(3) .023(2) .012(2) .009(2) C21 .037(4) .043(4) .043(5) .005(3) .009(3) .015(4) C22 .038(4) .042(4) .045(5) .009(3) .010(3) .008(3) C221 .047(4) .047(4) .033(4) .007(4) .008(3) .007(3) C222 .054(5) .064(5) .052(5) .016(4) .019(4) .006(4) C223 .064(5) .048(5) .057(5) .009(4) .010(4) .007(4) C224 .064(5) .075(6) .042(5) .024(5) .015(4) -.007(4) C225 .069(6) .077(6) .071(6) .014(5) .041(5) .007(5) C226 .063(5) .055(5) .071(6) .006(4) .032(4) .011(4) C23 .051(4) .070(5) .046(5) .017(4) .010(4) .014(4) C24 .062(5) .071(5) .065(6) .032(4) .022(4) .023(5) C25 .062(5) .046(4) .082(6) .020(4) .038(5) .014(4) C26 .038(4) .044(4) .052(5) .009(3) .023(3) .010(4) C261 .048(4) .054(5) .061(5) .011(4) .030(4) .009(4) C262 .122(7) .049(5) .067(6) -.001(5) .042(5) -.007(4) C263 .142(9) .065(6) .094(8) -.020(6) .051(7) -.017(6) C264 .091(7) .103(8) .065(6) -.001(6) .030(5) -.009(6) C265 .069(6) .095(7) .070(6) .023(5) .033(5) .025(5) C266 .061(5) .054(5) .061(6) .012(4) .021(4) -.008(4) O3 .039(3) .077(3) .042(3) .007(2) .014(2) .001(2) C31 .037(4) .066(5) .051(5) .014(4) .013(4) .016(4) C32 .050(5) .053(5) .052(5) -.000(4) .015(4) .013(4) C321 .064(5) .048(5) .061(6) -.000(4) .024(5) .007(4) C322 .085(6) .070(6) .053(5) .018(5) .024(5) .011(4) C323 .120(8) .074(6) .093(8) .034(6) .056(7) .020(6) C324 .157(12) .055(6) .126(11) .011(7) .093(10) .005(6) C325 .120(9) .083(8) .067(7) -.035(6) .047(7) -.019(6) C326 .076(6) .075(6) .068(6) -.016(5) .020(5) .006(5) C33 .052(5) .062(5) .067(6) -.004(4) .016(4) .013(4) C34 .038(5) .077(6) .098(7) .013(4) .032(5) .025(5) C35 .048(5) .069(5) .074(6) .001(4) .029(4) .008(4) C36 .044(4) .053(5) .053(5) .011(4) .016(4) .008(4) C361 .050(4) .064(5) .048(5) .018(4) .020(4) .009(4) C362 .064(5) .056(5) .059(5) .011(4) .016(4) .016(4) C363 .065(6) .063(6) .086(7) .007(4) .009(5) .014(5) C364 .077(7) .083(7) .085(8) .016(5) -.000(6) -.007(6) C365 .071(6) .109(8) .064(6) .041(6) .025(5) -.003(6) C366 .058(5) .082(6) .055(6) .022(4) .026(4) .013(5) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment ? #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 4192 #ActaC _refine_ls_number_parameters 523 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .094 #ActaC _refine_ls_R_factor_obs .044 #ActaC _refine_ls_wR_factor_all .048 #ActaC _refine_ls_wR_factor_obs .039 #ActaC _refine_ls_goodness_of_fit_all 1.186 #ActaC _refine_ls_goodness_of_fit_obs 1.282 #ActaC _refine_ls_shift/esd_max .023 #ActaC _refine_ls_shift/esd_mean . #ActaC _refine_diff_density_min -.548 #ActaC _refine_diff_density_max .844 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC La O1 2.242(4) . . ? La O2 2.234(5) . . ? La O3 2.201(5) . . ? O1 C11 1.338(9) . . ? C11 C12 1.397(10) . . ? C11 C16 1.417(8) . . ? C12 C121 1.490(8) . . ? C12 C13 1.376(10) . . ? C121 C122 1.382(11) . . ? C121 C126 1.409(10) . . ? C122 C123 1.373(9) . . ? C122 H122 .979(7) . . ? C123 C124 1.372(12) . . ? C123 H123 1.017(8) . . ? C124 C125 1.364(12) . . ? C124 H124 .921(7) . . ? C125 C126 1.382(9) . . ? C125 H125 .889(8) . . ? C126 H126 1.038(8) . . ? C13 C14 1.379(9) . . ? C13 H13 .920(6) . . ? C14 C15 1.387(11) . . ? C14 H14 .914(8) . . ? C15 C16 1.373(11) . . ? C15 H15 .856(6) . . ? C16 C161 1.476(10) . . ? C161 C162 1.378(13) . . ? C161 C166 1.364(11) . . ? C162 C163 1.390(14) . . ? C162 H162 1.071(9) . . ? C163 C164 1.320(16) . . ? C163 H163 .853(12) . . ? C164 C165 1.345(16) . . ? C164 H164 .965(9) . . ? C165 C166 1.405(14) . . ? C165 H165 .859(10) . . ? C166 H166 .898(9) . . ? O2 C21 1.333(8) . . ? C21 C22 1.422(9) . . ? C21 C26 1.405(10) . . ? C22 C221 1.473(10) . . ? C22 C23 1.369(10) . . ? C221 C222 1.378(10) . . ? C221 C226 1.405(11) . . ? C222 C223 1.368(12) . . ? C222 H222 .825(8) . . ? C223 C224 1.389(12) . . ? C223 H223 .953(7) . . ? C224 C225 1.347(12) . . ? C224 H224 1.029(9) . . ? C225 C226 1.379(13) . . ? C225 H225 .856(9) . . ? C226 H226 1.007(7) . . ? C23 C24 1.373(11) . . ? C23 H23 .860(6) . . ? C24 C25 1.390(12) . . ? C24 H24 1.002(8) . . ? C25 C26 1.376(10) . . ? C25 H25 .846(8) . . ? C26 C261 1.499(10) . . ? C261 C262 1.368(10) . . ? C261 C266 1.351(11) . . ? C262 C263 1.374(14) . . ? C262 H262 .966(9) . . ? C263 C264 1.327(15) . . ? C263 H263 1.009(9) . . ? C264 C265 1.377(13) . . ? C264 H264 .976(9) . . ? C265 C266 1.393(13) . . ? C265 H265 .826(10) . . ? C266 H266 .984(7) . . ? O3 C31 1.342(8) . . ? C31 C32 1.406(8) . . ? C31 C36 1.404(11) . . ? C32 C321 1.476(12) . . ? C32 C33 1.401(11) . . ? C321 C322 1.386(12) . . ? C321 C326 1.393(11) . . ? C322 C323 1.389(14) . . ? C322 H322 .870(7) . . ? C323 C324 1.405(15) . . ? C323 H323 1.052(11) . . ? C324 C325 1.336(18) . . ? C324 H324 .849(13) . . ? C325 C326 1.377(15) . . ? C325 H325 .848(9) . . ? C326 H326 .976(9) . . ? C33 C34 1.364(12) . . ? C33 H33 .919(6) . . ? C34 C35 1.363(9) . . ? C34 H34 .941(7) . . ? C35 C36 1.397(10) . . ? C35 H35 .968(8) . . ? C36 C361 1.482(8) . . ? C361 C362 1.382(11) . . ? C361 C366 1.392(11) . . ? C362 C363 1.392(9) . . ? C362 H362 1.090(7) . . ? C363 C364 1.363(15) . . ? C363 H363 .889(9) . . ? C364 C365 1.367(14) . . ? C364 H364 .982(8) . . ? C365 C366 1.379(11) . . ? C365 H365 .972(9) . . ? C366 H366 .902(8) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC La C11 3.396(7) . . ? La C121 3.107(7) . . ? La C122 3.159(8) . . ? La C123 3.248(8) . . ? La C124 3.274(7) . . ? La C125 3.206(7) . . ? La C126 3.132(7) . . ? La C21 3.400(7) . . ? La C221 3.173(7) . . ? La C222 3.052(6) . . ? La C223 3.282(7) . . ? La C224 3.618(7) . . ? La C225 3.691(9) . . ? La C226 3.510(8) . . ? La C31 3.528(7) . . ? La C322 3.544(7) . . ? La H222 3.2945(11) . . ? La H322 3.2126(10) . . ? O1 C12 2.356(9) . . ? O1 C121 2.694(7) . . ? O1 C16 2.400(7) . . ? O1 C161 2.823(7) . . ? C11 C121 2.443(8) . . ? C11 C13 2.401(10) . . ? C11 C14 2.792(11) . . ? C11 C15 2.384(9) . . ? C11 C161 2.489(9) . . ? C12 C122 2.509(9) . . ? C12 C126 2.510(9) . . ? C12 C14 2.402(10) . . ? C12 C15 2.745(8) . . ? C12 C16 2.434(8) . . ? C12 H122 2.577(7) . . ? C12 H126 2.680(7) . . ? C12 H13 1.991(7) . . ? C121 C123 2.396(10) . . ? C121 C124 2.785(9) . . ? C121 C125 2.421(9) . . ? C121 C13 2.536(9) . . ? C121 H122 1.982(8) . . ? C121 H126 2.115(8) . . ? C121 H13 2.698(7) . . ? C122 C124 2.387(10) . . ? C122 C125 2.752(10) . . ? C122 C126 2.390(11) . . ? C122 H123 2.090(7) . . ? C123 C125 2.366(12) . . ? C123 C126 2.744(12) . . ? C123 H122 2.103(7) . . ? C123 H124 1.999(8) . . ? C124 C126 2.383(10) . . ? C124 H123 2.043(9) . . ? C124 H125 2.015(9) . . ? C125 H124 1.988(8) . . ? C125 H126 2.110(8) . . ? C126 H125 1.924(7) . . ? C13 C15 2.370(9) . . ? C13 C16 2.789(10) . . ? C13 H14 2.014(7) . . ? C14 C16 2.430(12) . . ? C14 H13 2.000(6) . . ? C14 H15 2.005(7) . . ? C15 C161 2.514(12) . . ? C15 H14 2.011(9) . . ? C16 C162 2.479(12) . . ? C16 C166 2.490(11) . . ? C16 H15 1.859(6) . . ? C16 H162 2.645(7) . . ? C161 C163 2.411(14) . . ? C161 C164 2.773(12) . . ? C161 C165 2.410(12) . . ? C161 H15 2.538(8) . . ? C161 H162 2.101(8) . . ? C161 H166 2.025(8) . . ? C162 C164 2.353(13) . . ? C162 C165 2.713(14) . . ? C162 C166 2.338(13) . . ? C162 H163 1.835(10) . . ? C163 C165 2.317(15) . . ? C163 C166 2.716(15) . . ? C163 H162 2.148(10) . . ? C163 H164 2.027(11) . . ? C164 C166 2.378(13) . . ? C164 H163 1.995(12) . . ? C164 H165 1.980(12) . . ? C165 H164 1.959(11) . . ? C165 H166 1.936(11) . . ? C166 H165 1.918(8) . . ? O2 C22 2.362(8) . . ? O2 C221 2.727(7) . . ? O2 C26 2.408(8) . . ? O2 C261 2.913(9) . . ? O2 H266 2.561(5) . . ? C21 C221 2.473(10) . . ? C21 C23 2.412(10) . . ? C21 C24 2.813(10) . . ? C21 C25 2.384(10) . . ? C21 C261 2.530(10) . . ? C22 C222 2.501(10) . . ? C22 C226 2.487(11) . . ? C22 C24 2.405(11) . . ? C22 C25 2.740(11) . . ? C22 C26 2.435(10) . . ? C22 H222 2.603(6) . . ? C22 H226 2.616(7) . . ? C22 H23 1.965(6) . . ? C221 C223 2.397(10) . . ? C221 C224 2.786(12) . . ? C221 C225 2.406(12) . . ? C221 C23 2.498(11) . . ? C221 H222 1.905(6) . . ? C221 H226 2.067(7) . . ? C221 H23 2.683(7) . . ? C222 C224 2.388(12) . . ? C222 C225 2.729(12) . . ? C222 C226 2.383(10) . . ? C222 H223 2.057(8) . . ? C223 C225 2.359(11) . . ? C223 C226 2.752(10) . . ? C223 H222 1.926(9) . . ? C223 H224 2.080(9) . . ? C224 C226 2.384(11) . . ? C224 H223 2.001(8) . . ? C224 H225 1.930(8) . . ? C225 H224 2.085(9) . . ? C225 H226 2.108(9) . . ? C226 H225 1.926(9) . . ? C23 C25 2.354(11) . . ? C23 C26 2.779(10) . . ? C23 H24 2.145(8) . . ? C24 C26 2.441(10) . . ? C24 H23 1.902(8) . . ? C24 H25 1.966(8) . . ? C25 C261 2.500(11) . . ? C25 H24 2.025(8) . . ? C26 C262 2.487(10) . . ? C26 C266 2.494(11) . . ? C26 H25 1.895(7) . . ? C26 H262 2.643(6) . . ? C26 H266 2.615(7) . . ? C261 C263 2.389(12) . . ? C261 C264 2.772(12) . . ? C261 C265 2.397(13) . . ? C261 H25 2.555(8) . . ? C261 H262 2.029(7) . . ? C261 H266 1.995(7) . . ? C262 C264 2.354(13) . . ? C262 C265 2.714(13) . . ? C262 C266 2.325(11) . . ? C262 H263 2.025(8) . . ? C263 C265 2.333(13) . . ? C263 C266 2.704(11) . . ? C263 H262 2.028(11) . . ? C263 H264 2.065(11) . . ? C264 C266 2.388(12) . . ? C264 H263 2.051(11) . . ? C264 H265 1.931(11) . . ? C265 H264 1.986(9) . . ? C265 H266 2.087(9) . . ? C266 H265 1.948(9) . . ? O3 C32 2.374(7) . . ? O3 C321 2.844(7) . . ? O3 C322 2.953(9) . . ? O3 C36 2.368(9) . . ? O3 C361 2.850(9) . . ? O3 C362 2.942(9) . . ? O3 H322 2.603(5) . . ? O3 H362 2.541(5) . . ? C31 C321 2.516(10) . . ? C31 C33 2.402(9) . . ? C31 C34 2.762(10) . . ? C31 C35 2.398(12) . . ? C31 C361 2.527(10) . . ? C32 C322 2.503(12) . . ? C32 C326 2.494(11) . . ? C32 C34 2.409(12) . . ? C32 C35 2.784(11) . . ? C32 C36 2.448(9) . . ? C32 H322 2.577(8) . . ? C32 H326 2.696(6) . . ? C32 H33 1.965(6) . . ? C321 C323 2.433(14) . . ? C321 C324 2.770(16) . . ? C321 C325 2.414(12) . . ? C321 C33 2.501(13) . . ? C321 H322 1.922(8) . . ? C321 H326 2.073(7) . . ? C321 H33 2.569(9) . . ? C322 C324 2.380(14) . . ? C322 C325 2.742(11) . . ? C322 C326 2.372(11) . . ? C322 H323 2.132(9) . . ? C323 C325 2.398(14) . . ? C323 C326 2.771(14) . . ? C323 H322 1.995(11) . . ? C323 H324 1.896(10) . . ? C324 C326 2.350(17) . . ? C324 H323 2.154(12) . . ? C324 H325 1.826(13) . . ? C325 H324 1.956(13) . . ? C325 H326 2.017(13) . . ? C326 H325 2.015(9) . . ? C33 C35 2.369(10) . . ? C33 C36 2.786(8) . . ? C33 H34 1.995(9) . . ? C34 C36 2.407(9) . . ? C34 H33 2.027(9) . . ? C34 H35 2.039(8) . . ? C35 C361 2.494(9) . . ? C35 H34 2.012(6) . . ? C36 C362 2.502(9) . . ? C36 C366 2.490(9) . . ? C36 H35 2.025(8) . . ? C36 H362 2.626(7) . . ? C36 H366 2.573(7) . . ? C361 C363 2.408(10) . . ? C361 C364 2.796(10) . . ? C361 C365 2.398(10) . . ? C361 H35 2.611(7) . . ? C361 H362 2.084(8) . . ? C361 H366 1.959(8) . . ? C362 C364 2.399(11) . . ? C362 C365 2.732(12) . . ? C362 C366 2.381(12) . . ? C362 H363 1.934(7) . . ? C363 C365 2.346(14) . . ? C363 C366 2.746(12) . . ? C363 H362 2.206(8) . . ? C363 H364 2.139(9) . . ? C364 C366 2.401(11) . . ? C364 H363 2.007(11) . . ? C364 H365 2.086(11) . . ? C365 H224 2.668(11) . . ? C365 H364 1.943(9) . . ? C365 H366 2.026(9) . . ? C366 H224 2.696(8) . . ? C366 H365 1.969(7) . . ? H123 H124 2.2949(9) . . ? H124 H125 2.3412(7) . . ? H125 H126 2.2765(7) . . ? H126 H35 2.1904(8) . 2_766 ? H13 H14 2.3127(6) . . ? H14 H15 2.3479(7) . . ? H162 H163 2.1997(6) . . ? H164 H165 2.2718(5) . . ? H165 H166 2.1005(6) . . ? H222 H223 2.3228(6) . . ? H223 H224 2.2979(8) . . ? H224 H225 2.3346(8) . . ? H225 H226 2.3249(6) . . ? H23 H24 2.3611(6) . . ? H24 H25 2.2536(7) . . ? H25 H262 2.3831(6) . . ? H262 H263 2.2827(7) . . ? H264 H265 2.1996(7) . . ? H265 H266 2.3356(7) . . ? H323 H324 2.2855(6) . . ? H324 H325 2.1457(6) . . ? H325 H326 2.3575(5) . . ? H33 H34 2.3391(5) . . ? H34 H35 2.3427(6) . . ? H362 H363 2.3828(6) . . ? H364 H365 2.2779(5) . . ? H365 H366 2.2667(6) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC O1 La O2 114.03(17) . . . ? O1 La O3 116.17(17) . . . ? O2 La O3 128.43(16) . . . ? La O1 C11 141.8(4) . . . ? O1 C11 C12 119.0(5) . . . ? O1 C11 C16 121.2(6) . . . ? C12 C11 C16 119.8(6) . . . ? C11 C12 C121 115.6(6) . . . ? C11 C12 C13 120.0(5) . . . ? C121 C12 C13 124.4(6) . . . ? C12 C121 C122 121.7(6) . . . ? C12 C121 C126 119.9(6) . . . ? C122 C121 C126 117.8(6) . . . ? C121 C122 C123 120.8(7) . . . ? C121 C122 H122 113.1(6) . . . ? C123 C122 H122 126.0(8) . . . ? C122 C123 C124 120.8(8) . . . ? C122 C123 H123 121.2(8) . . . ? C124 C123 H123 116.7(7) . . . ? C123 C124 C125 119.7(6) . . . ? C123 C124 H124 120.1(8) . . . ? C125 C124 H124 119.8(8) . . . ? C124 C125 C126 120.4(7) . . . ? C124 C125 H125 125.5(7) . . . ? C126 C125 H125 114.0(8) . . . ? C121 C126 C125 120.3(7) . . . ? C121 C126 H126 118.7(6) . . . ? C125 C126 H126 120.7(7) . . . ? C12 C13 C14 121.4(6) . . . ? C12 C13 H13 118.9(6) . . . ? C14 C13 H13 119.5(8) . . . ? C13 C14 C15 117.9(7) . . . ? C13 C14 H14 121.6(8) . . . ? C15 C14 H14 120.5(6) . . . ? C14 C15 C16 123.4(6) . . . ? C14 C15 H15 125.1(8) . . . ? C16 C15 H15 110.9(8) . . . ? C11 C16 C15 117.4(6) . . . ? C11 C16 C161 118.7(6) . . . ? C15 C16 C161 123.8(5) . . . ? C16 C161 C162 120.5(7) . . . ? C16 C161 C166 122.5(7) . . . ? C162 C161 C166 117.0(7) . . . ? C161 C162 C163 121.1(9) . . . ? C161 C162 H162 117.6(8) . . . ? C163 C162 H162 121.1(9) . . . ? C162 C163 C164 120.5(10) . . . ? C162 C163 H163 107.4(10) . . . ? C164 C163 H163 132.0(12) . . . ? C163 C164 C165 120.7(9) . . . ? C163 C164 H164 124.2(12) . . . ? C165 C164 H164 115.0(11) . . . ? C164 C165 C166 119.7(9) . . . ? C164 C165 H165 126.6(11) . . . ? C166 C165 H165 113.6(11) . . . ? C161 C166 C165 121.0(8) . . . ? C161 C166 H166 125.7(8) . . . ? C165 C166 H166 112.5(9) . . . ? La O2 C21 143.6(4) . . . ? O2 C21 C22 118.0(6) . . . ? O2 C21 C26 123.1(6) . . . ? C22 C21 C26 118.9(6) . . . ? C21 C22 C221 117.3(6) . . . ? C21 C22 C23 119.6(6) . . . ? C221 C22 C23 123.0(6) . . . ? C22 C221 C222 122.6(7) . . . ? C22 C221 C226 119.5(6) . . . ? C222 C221 C226 117.8(7) . . . ? C221 C222 C223 121.6(7) . . . ? C221 C222 H222 117.5(8) . . . ? C223 C222 H222 120.9(8) . . . ? C222 C223 C224 120.0(7) . . . ? C222 C223 H223 123.8(8) . . . ? C224 C223 H223 116.2(8) . . . ? C223 C224 C225 119.1(8) . . . ? C223 C224 H224 117.9(7) . . . ? C225 C224 H224 122.1(8) . . . ? C224 C225 C226 121.9(8) . . . ? C224 C225 H225 120.7(10) . . . ? C226 C225 H225 117.1(8) . . . ? C221 C226 C225 119.6(7) . . . ? C221 C226 H226 117.0(7) . . . ? C225 C226 H226 123.4(8) . . . ? C22 C23 C24 122.6(7) . . . ? C22 C23 H23 122.0(8) . . . ? C24 C23 H23 114.9(8) . . . ? C23 C24 C25 116.9(7) . . . ? C23 C24 H24 128.4(8) . . . ? C25 C24 H24 114.7(8) . . . ? C24 C25 C26 123.9(7) . . . ? C24 C25 H25 121.1(8) . . . ? C26 C25 H25 115.0(8) . . . ? C21 C26 C25 118.0(7) . . . ? C21 C26 C261 121.1(6) . . . ? C25 C26 C261 120.8(7) . . . ? C26 C261 C262 120.3(7) . . . ? C26 C261 C266 122.0(6) . . . ? C262 C261 C266 117.4(7) . . . ? C261 C262 C263 121.2(8) . . . ? C261 C262 H262 119.7(8) . . . ? C263 C262 H262 119.1(7) . . . ? C262 C263 C264 121.2(8) . . . ? C262 C263 H263 115.5(9) . . . ? C264 C263 H263 122.2(11) . . . ? C263 C264 C265 119.2(9) . . . ? C263 C264 H264 126.7(10) . . . ? C265 C264 H264 114.0(10) . . . ? C264 C265 C266 119.1(9) . . . ? C264 C265 H265 120.4(10) . . . ? C266 C265 H265 120.5(9) . . . ? C261 C266 C265 121.7(7) . . . ? C261 C266 H266 116.5(8) . . . ? C265 C266 H266 121.9(8) . . . ? La O3 C31 169.0(4) . . . ? O3 C31 C32 119.5(7) . . . ? O3 C31 C36 119.2(5) . . . ? C32 C31 C36 121.3(6) . . . ? C31 C32 C321 121.6(7) . . . ? C31 C32 C33 117.7(7) . . . ? C321 C32 C33 120.7(6) . . . ? C32 C321 C322 122.0(6) . . . ? C32 C321 C326 120.8(7) . . . ? C322 C321 C326 117.2(8) . . . ? C321 C322 C323 122.5(7) . . . ? C321 C322 H322 115.0(9) . . . ? C323 C322 H322 122.4(9) . . . ? C322 C323 C324 116.8(10) . . . ? C322 C323 H323 121.2(8) . . . ? C324 C323 H323 121.9(11) . . . ? C323 C324 C325 122.1(12) . . . ? C323 C324 H324 112.1(13) . . . ? C325 C324 H324 125.6(12) . . . ? C324 C325 C326 120.1(9) . . . ? C324 C325 H325 111.6(13) . . . ? C326 C325 H325 128.3(12) . . . ? C321 C326 C325 121.3(8) . . . ? C321 C326 H326 121.0(9) . . . ? C325 C326 H326 117.0(8) . . . ? C32 C33 C34 121.2(6) . . . ? C32 C33 H33 114.1(8) . . . ? C34 C33 H33 124.0(8) . . . ? C33 C34 C35 120.6(7) . . . ? C33 C34 H34 118.8(7) . . . ? C35 C34 H34 120.6(9) . . . ? C34 C35 C36 121.4(8) . . . ? C34 C35 H35 121.1(8) . . . ? C36 C35 H35 116.6(6) . . . ? C31 C36 C35 117.8(6) . . . ? C31 C36 C361 122.2(6) . . . ? C35 C36 C361 120.0(7) . . . ? C36 C361 C362 121.7(7) . . . ? C36 C361 C366 120.0(7) . . . ? C362 C361 C366 118.2(6) . . . ? C361 C362 C363 120.4(7) . . . ? C361 C362 H362 114.4(6) . . . ? C363 C362 H362 125.0(8) . . . ? C362 C363 C364 121.0(8) . . . ? C362 C363 H363 114.2(9) . . . ? C364 C363 H363 124.6(8) . . . ? C363 C364 C365 118.4(7) . . . ? C363 C364 H364 130.9(10) . . . ? C365 C364 H364 110.5(10) . . . ? C364 C365 C366 122.0(8) . . . ? C364 C365 H365 125.4(9) . . . ? C366 C365 H365 112.6(9) . . . ? C361 C366 C365 119.9(8) . . . ? C361 C366 H366 115.7(7) . . . ? C365 C366 H366 124.0(8) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min -16 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _reflns_number_total 7232 #ActaC _reflns_number_observed 4192 #ActaC _reflns_observed_criterion refl_observed_if_I____>3.000_sigma(I___) _reflns_d_resolution_high .842 _reflns_d_resolution_low 14.721 data_luodpp _audit_creation_date 98-05-06 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical C54_H39_Lu_O3 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum C54_H39_Lu_O3 #ActaC _chemical_formula_weight 910.87 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-Nonius software' #ActaC _computing_cell_refinement 'Enraf-Nonius software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 15.888(6) #ActaC _cell_length_b 13.524(3) #ActaC _cell_length_c 10.939(4) #ActaC _cell_angle_alpha 116.49(2) #ActaC _cell_angle_beta 92.86(3) #ActaC _cell_angle_gamma 103.63(2) #ActaC _cell_volume 2011.7(13) #ActaC _cell_formula_units_Z 2 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used ? #ActaC _cell_measurement_theta_min ? #ActaC _cell_measurement_theta_max ? #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description plate #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max 0.50 #ActaC _exptl_crystal_size_mid 0.25 #ActaC _exptl_crystal_size_min 0.08 #ActaC _exptl_crystal_density_diffrn 1.504 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 916 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 2.50 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.555 #ActaC _exptl_absorpt_correction_T_max 0.870 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/theta #ActaC _diffrn_standards_number ? #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number .114700+05 #ActaC _diffrn_reflns_av_R_equivalents .048 #ActaC _diffrn_reflns_av_sigmaI/netI .104 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 18 #ActaC _diffrn_reflns_limit_k_min -16 #ActaC _diffrn_reflns_limit_k_max 15 #ActaC _diffrn_reflns_limit_l_min -12 #ActaC _diffrn_reflns_limit_l_max 12 #ActaC _diffrn_reflns_theta_min 1.34 #ActaC _diffrn_reflns_theta_max 25.01 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 108 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 6 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 78 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Lu ? 0 2 -.988 5.858 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Lu .27925(2) .20774(3) .22658(4) .03678(16) Uani ? ? O1 .2299(3) .3277(4) .1980(5) .042(2) Uani ? ? C11 .1871(5) .4048(6) .2732(8) .036(3) Uani ? ? C12 .1657(5) .4084(6) .3967(8) .038(3) Uani ? ? C13 .1241(6) .4881(7) .4779(9) .053(4) Uani ? ? C14 .1034(6) .5622(7) .4363(10) .053(4) Uani ? ? C15 .1224(6) .5562(7) .3134(10) .052(4) Uani ? ? C16 .1626(5) .4769(6) .2279(9) .041(4) Uani ? ? C121 .1858(5) .3193(7) .4283(8) .040(3) Uani ? ? C122 .2637(5) .3429(7) .5130(8) .047(4) Uani ? ? C123 .2857(6) .2536(8) .5266(9) .051(4) Uani ? ? C124 .2321(6) .1445(8) .4581(10) .055(4) Uani ? ? C125 .1530(6) .1177(7) .3746(10) .058(4) Uani ? ? C126 .1304(5) .2053(8) .3582(10) .052(4) Uani ? ? C161 .1785(6) .4703(7) .0925(10) .052(4) Uani ? ? C162 .1081(7) .4415(8) -.0091(11) .071(5) Uani ? ? C163 .1238(13) .4366(9) -.1359(13) .107(9) Uani ? ? C164 .2083(17) .4647(17) -.1589(17) .149(13) Uani ? ? C165 .2737(13) .4897(18) -.064(2) .159(13) Uani ? ? C166 .2619(8) .4934(13) .0621(15) .105(8) Uani ? ? O2 .4095(3) .2653(4) .3158(5) .038(2) Uani ? ? C21 .4935(5) .2741(6) .3010(8) .039(3) Uani ? ? C22 .5163(5) .2393(6) .1702(8) .041(3) Uani ? ? C23 .6036(5) .2457(7) .1576(10) .054(4) Uani ? ? C24 .6679(6) .2860(9) .2716(11) .063(5) Uani ? ? C25 .6455(5) .3184(7) .4007(10) .050(4) Uani ? ? C26 .5589(5) .3140(6) .4183(8) .039(3) Uani ? ? C221 .4480(5) .1917(6) .0467(8) .039(3) Uani ? ? C222 .3869(5) .2491(6) .0408(8) .040(3) Uani ? ? C223 .3222(6) .2036(8) -.0761(10) .057(4) Uani ? ? C224 .3173(7) .1005(9) -.1878(9) .065(5) Uani ? ? C225 .3765(8) .0418(8) -.1839(10) .072(5) Uani ? ? C226 .4411(6) .0875(7) -.0671(9) .055(4) Uani ? ? C261 .5350(5) .3421(6) .5574(8) .041(3) Uani ? ? C262 .5436(6) .2754(8) .6211(11) .062(5) Uani ? ? C263 .5186(8) .2958(9) .7476(12) .082(6) Uani ? ? C264 .4862(7) .3864(9) .8162(10) .068(5) Uani ? ? C265 .4781(6) .4551(7) .7596(10) .054(4) Uani ? ? C266 .5023(5) .4339(7) .6310(9) .048(4) Uani ? ? O3 .2218(3) .0428(4) .0812(5) .044(2) Uani ? ? C31 .1807(5) -.0705(6) .0088(8) .041(3) Uani ? ? C32 .1980(5) -.1471(6) .0554(8) .043(3) Uani ? ? C33 .1535(6) -.2650(7) -.0197(9) .053(4) Uani ? ? C34 .0954(6) -.3077(7) -.1402(10) .057(4) Uani ? ? C35 .0794(5) -.2335(7) -.1879(8) .046(4) Uani ? ? C36 .1223(5) -.1140(6) -.1148(8) .039(3) Uani ? ? C321 .2598(6) -.1066(7) .1852(9) .047(4) Uani ? ? C322 .3434(6) -.0287(7) .2147(9) .047(4) Uani ? ? C323 .4003(6) .0096(8) .3374(10) .060(4) Uani ? ? C324 .3779(7) -.0283(8) .4274(11) .065(5) Uani ? ? C325 .2978(8) -.1064(9) .3996(11) .069(5) Uani ? ? C326 .2384(6) -.1458(7) .2782(10) .056(4) Uani ? ? C361 .1019(5) -.0398(7) -.1720(9) .045(4) Uani ? ? C362 .0796(6) .0609(8) -.0905(10) .060(4) Uani ? ? C363 .0622(8) .1286(10) -.1433(15) .086(6) Uani ? ? C364 .0666(8) .0997(13) -.279(2) .106(8) Uani ? ? C365 .0854(8) -.0006(13) -.3617(14) .093(7) Uani ? ? C366 .1030(6) -.0704(9) -.3113(10) .065(5) Uani ? ? H13 .10752 .48960 .56334 .06900 Uiso ? ? H14 .07772 .62128 .49526 .06800 Uiso ? ? H15 .10643 .60821 .28265 .06500 Uiso ? ? H122 .30296 .42160 .56320 .05700 Uiso ? ? H123 .34128 .26982 .58230 .06300 Uiso ? ? H124 .24790 .08370 .46992 .06700 Uiso ? ? H125 .11386 .03922 .32836 .07300 Uiso ? ? H126 .07458 .18705 .29782 .06600 Uiso ? ? H23 .62004 .22122 .06519 .06800 Uiso ? ? H24 .72888 .29269 .25988 .07500 Uiso ? ? H25 .69008 .34394 .48054 .05900 Uiso ? ? H222 .38971 .32219 .12054 .05100 Uiso ? ? H223 .27988 .24561 -.07600 .06800 Uiso ? ? H224 .27231 .06967 -.26977 .08100 Uiso ? ? H225 .37314 -.03146 -.26304 .09100 Uiso ? ? H226 .48309 .04606 -.06730 .06900 Uiso ? ? H262 .56748 .21151 .57579 .07900 Uiso ? ? H263 .52449 .24714 .78906 .10300 Uiso ? ? H264 .46551 .39985 .90352 .08400 Uiso ? ? H265 .45508 .51968 .80897 .06800 Uiso ? ? H266 .49532 .48456 .59224 .06000 Uiso ? ? H33 .16341 -.31705 .01448 .06600 Uiso ? ? H34 .06607 -.38961 -.19138 .07000 Uiso ? ? H35 .03671 -.26308 -.27249 .05700 Uiso ? ? H322 .36052 -.00177 .14756 .05700 Uiso ? ? H323 .45819 .06551 .35632 .07600 Uiso ? ? H324 .41766 -.00027 .51213 .08000 Uiso ? ? H325 .28315 -.13538 .46543 .08600 Uiso ? ? H326 .18024 -.20236 .25952 .07300 Uiso ? ? H362 .07412 .08012 .00580 .07700 Uiso ? ? H363 .04619 .19949 -.08334 .10900 Uiso ? ? H364 .05722 .15223 -.31305 .12900 Uiso ? ? H365 .08506 -.02205 -.45969 .11900 Uiso ? ? H366 .11672 -.14259 -.37202 .08900 Uiso ? ? H162 .04592 .42362 .00858 .09200 Uiso ? ? H163 .07159 .41379 -.20793 .13700 Uiso ? ? H164 .21571 .45818 -.24851 .18700 Uiso ? ? H165 .33349 .50958 -.08123 .18700 Uiso ? ? H166 .31311 .51362 .13171 .12500 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Lu .02998(19) .03195(18) .0411(2) .00741(12) .00271(14) .01211(14) O1 .048(3) .044(3) .045(3) .024(3) .020(3) .024(3) C11 .032(4) .036(4) .037(5) .004(3) .009(4) .017(4) C12 .048(5) .035(4) .023(4) .017(4) .007(4) .005(3) C13 .058(6) .052(5) .043(5) .016(4) .019(5) .018(4) C14 .056(6) .046(5) .054(6) .019(4) .019(5) .016(4) C15 .054(6) .053(5) .058(6) .025(4) .013(5) .029(5) C16 .042(5) .034(4) .046(5) .013(4) .008(4) .019(4) C121 .040(5) .050(5) .040(5) .018(4) .014(4) .027(4) C122 .046(5) .053(5) .032(5) .007(4) -.002(4) .017(4) C123 .051(5) .060(6) .038(5) .019(5) .001(4) .020(4) C124 .062(6) .059(6) .057(6) .024(5) .019(5) .035(5) C125 .054(6) .043(5) .073(7) -.001(4) .011(5) .032(5) C126 .030(5) .066(6) .058(6) .005(4) .009(4) .031(5) C161 .068(6) .038(5) .053(6) .021(4) .011(5) .023(4) C162 .084(8) .060(6) .066(7) .014(5) -.006(6) .032(5) C163 .218(18) .062(7) .049(8) .055(9) .009(10) .025(6) C164 .29(3) .199(17) .085(11) .20(2) .123(16) .106(12) C165 .190(18) .29(2) .193(18) .186(18) .155(16) .22(2) C166 .088(9) .187(14) .129(12) .087(9) .057(9) .123(11) O2 .032(3) .045(3) .036(3) .006(2) .006(2) .019(2) C21 .036(5) .036(4) .041(5) .004(3) .011(4) .018(4) C22 .032(4) .043(4) .041(5) .008(3) .008(4) .015(4) C23 .038(5) .059(5) .057(6) .013(4) .016(5) .021(5) C24 .033(5) .087(7) .066(7) .021(5) .012(5) .030(6) C25 .026(4) .058(5) .055(6) .006(4) -.007(4) .021(5) C26 .040(5) .033(4) .039(5) .010(3) .003(4) .014(4) C221 .030(4) .046(5) .038(5) .003(4) .009(4) .020(4) C222 .040(5) .037(4) .037(5) .002(4) .012(4) .016(4) C223 .044(5) .073(6) .052(6) .010(5) -.000(5) .032(5) C224 .062(7) .085(7) .033(6) -.000(5) -.003(5) .028(5) C225 .087(8) .067(6) .038(6) .007(6) .002(6) .012(5) C226 .071(6) .052(5) .038(5) .015(5) .008(5) .018(4) C261 .037(5) .044(4) .038(5) .007(4) -.006(4) .018(4) C262 .062(6) .061(6) .062(7) .026(5) -.003(5) .027(5) C263 .125(10) .074(7) .056(7) .024(7) .001(7) .042(6) C264 .091(8) .072(7) .036(6) .004(6) .002(5) .032(5) C265 .055(6) .046(5) .042(6) .001(4) .008(5) .011(4) C266 .048(5) .041(5) .052(6) .005(4) .003(4) .025(4) O3 .050(3) .034(3) .038(3) .000(2) -.001(3) .016(2) C31 .044(5) .034(4) .034(5) .004(4) .003(4) .012(4) C32 .043(5) .040(4) .039(5) .006(4) .005(4) .016(4) C33 .062(6) .037(4) .051(6) .002(4) .001(5) .019(4) C34 .063(6) .029(4) .065(7) .008(4) .004(5) .012(4) C35 .042(5) .049(5) .034(5) .006(4) .001(4) .013(4) C36 .039(5) .036(4) .029(5) .002(3) .008(4) .008(4) C321 .056(6) .039(4) .048(6) .014(4) .008(4) .022(4) C322 .052(5) .057(5) .042(5) .016(4) .011(4) .031(4) C323 .057(6) .059(6) .053(7) .015(5) -.002(5) .019(5) C324 .068(7) .068(7) .064(7) .026(6) -.007(6) .035(6) C325 .100(9) .066(6) .066(7) .032(6) .018(7) .048(6) C326 .076(7) .049(5) .050(6) .014(5) .000(5) .033(5) C361 .041(5) .051(5) .039(5) -.001(4) -.008(4) .026(4) C362 .062(6) .053(5) .063(7) .008(5) -.015(5) .033(5) C363 .080(8) .075(7) .098(10) .011(6) -.021(7) .046(7) C364 .068(8) .096(10) .168(16) -.019(7) -.038(9) .101(11) C365 .069(8) .125(11) .095(10) -.016(8) -.011(7) .084(10) C366 .054(6) .080(7) .053(7) -.012(5) -.015(5) .041(6) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme calc #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 4705 #ActaC _refine_ls_number_parameters 523 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .082 #ActaC _refine_ls_R_factor_obs .041 #ActaC _refine_ls_wR_factor_all .059 #ActaC _refine_ls_wR_factor_obs .048 #ActaC _refine_ls_goodness_of_fit_all 1.124 #ActaC _refine_ls_goodness_of_fit_obs 1.136 #ActaC _refine_ls_shift/esd_max .093 #ActaC _refine_ls_shift/esd_mean .002 #ActaC _refine_diff_density_min -.621 #ActaC _refine_diff_density_max 1.184 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Lu O1 2.090(7) . . ? Lu C11 3.196(9) . . ? Lu C121 2.787(8) . . ? Lu C122 2.898(8) . . ? Lu C123 3.048(10) . . ? Lu C124 3.087(12) . . ? Lu C125 3.009(11) . . ? Lu C126 2.831(9) . . ? Lu O2 2.049(5) . . ? Lu C222 2.877(9) . . ? Lu O3 2.017(4) . . ? O1 C11 1.362(9) . . ? C11 C12 1.393(13) . . ? C11 C16 1.392(14) . . ? C12 C13 1.389(12) . . ? C12 C121 1.487(14) . . ? C13 C14 1.366(17) . . ? C13 H13 .977(10) . . ? C14 C15 1.363(16) . . ? C14 H14 .970(9) . . ? C15 C16 1.385(12) . . ? C15 H15 .980(12) . . ? C16 C161 1.482(15) . . ? C121 C122 1.390(12) . . ? C121 C126 1.407(10) . . ? C122 C123 1.399(16) . . ? C122 H122 .977(7) . . ? C123 C124 1.350(11) . . ? C123 H123 .967(9) . . ? C124 C125 1.386(14) . . ? C124 H124 .971(12) . . ? C125 C126 1.396(17) . . ? C125 H125 .974(8) . . ? C126 H126 .988(9) . . ? C161 C162 1.387(15) . . ? C161 C166 1.379(17) . . ? C162 C163 1.40(2) . . ? C162 H162 1.010(11) . . ? C163 C164 1.37(3) . . ? C163 H163 1.001(17) . . ? C164 C165 1.30(3) . . ? C164 H164 .96(2) . . ? C165 C166 1.38(3) . . ? C165 H165 .97(2) . . ? C166 H166 .982(14) . . ? O2 C21 1.337(10) . . ? C21 C22 1.390(12) . . ? C21 C26 1.415(11) . . ? C22 C23 1.387(12) . . ? C22 C221 1.471(11) . . ? C23 C24 1.378(14) . . ? C23 H23 .984(10) . . ? C24 C25 1.373(15) . . ? C24 H24 .972(9) . . ? C25 C26 1.390(12) . . ? C25 H25 .968(9) . . ? C26 C261 1.488(13) . . ? C221 C222 1.393(13) . . ? C221 C226 1.377(10) . . ? C222 C223 1.393(12) . . ? C222 H222 .973(7) . . ? C223 C224 1.365(12) . . ? C223 H223 .977(11) . . ? C224 C225 1.377(19) . . ? C224 H224 .974(10) . . ? C225 C226 1.391(14) . . ? C225 H225 .969(9) . . ? C226 H226 .967(11) . . ? C261 C262 1.388(17) . . ? C261 C266 1.384(12) . . ? C262 C263 1.384(18) . . ? C262 H262 .963(10) . . ? C263 C264 1.358(17) . . ? C263 H263 .969(16) . . ? C264 C265 1.352(18) . . ? C264 H264 .978(11) . . ? C265 C266 1.398(15) . . ? C265 H265 .968(9) . . ? C266 H266 .975(11) . . ? O3 C31 1.340(8) . . ? C31 C32 1.415(15) . . ? C31 C36 1.394(11) . . ? C32 C33 1.399(10) . . ? C32 C321 1.482(12) . . ? C33 C34 1.369(14) . . ? C33 H33 .970(12) . . ? C34 C35 1.384(16) . . ? C34 H34 .967(7) . . ? C35 C36 1.411(10) . . ? C35 H35 .978(8) . . ? C36 C361 1.481(15) . . ? C321 C322 1.405(11) . . ? C321 C326 1.365(16) . . ? C322 C323 1.388(14) . . ? C322 H322 .978(11) . . ? C323 C324 1.326(19) . . ? C323 H323 .987(9) . . ? C324 C325 1.367(15) . . ? C324 H324 .958(11) . . ? C325 C326 1.394(15) . . ? C325 H325 .976(14) . . ? C326 H326 .995(9) . . ? C361 C362 1.397(13) . . ? C361 C366 1.392(15) . . ? C362 C363 1.35(2) . . ? C362 H362 .980(11) . . ? C363 C364 1.37(3) . . ? C363 H363 .993(12) . . ? C364 C365 1.37(2) . . ? C364 H364 .97(2) . . ? C365 C366 1.36(2) . . ? C365 H365 .976(15) . . ? C366 H366 .989(10) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Lu C12 3.496(8) . . ? Lu C21 3.269(8) . . ? Lu C22 3.802(8) . . ? Lu C221 3.395(8) . . ? Lu C223 3.393(12) . . ? Lu C31 3.338(6) . . ? Lu C32 4.127(8) . . ? Lu C321 4.003(10) . . ? Lu C322 3.529(11) . . ? Lu C323 4.177(13) . . ? Lu C362 3.978(9) . . ? Lu H122 3.4516(10) . . ? Lu H123 3.6236(14) . . ? Lu H125 3.6155(8) . . ? Lu H126 3.3583(12) . . ? Lu H222 2.7103(7) . . ? Lu H223 3.5681(13) . . ? Lu H322 3.1770(8) . . ? Lu H362 3.5041(11) . . ? O1 C12 2.364(10) . . ? O1 C16 2.406(11) . . ? O1 C121 2.691(12) . . ? O1 C161 2.891(14) . . ? C11 C13 2.406(12) . . ? C11 C14 2.768(12) . . ? C11 C15 2.381(14) . . ? C11 C121 2.441(15) . . ? C11 C161 2.510(16) . . ? C12 C14 2.389(14) . . ? C12 C15 2.740(15) . . ? C12 C16 2.410(15) . . ? C12 C122 2.508(14) . . ? C12 C126 2.500(13) . . ? C12 H13 2.060(8) . . ? C13 C15 2.360(17) . . ? C13 C16 2.778(14) . . ? C13 C121 2.544(14) . . ? C13 H14 2.038(11) . . ? C14 C16 2.406(13) . . ? C14 H13 2.035(12) . . ? C14 H15 2.034(12) . . ? C15 C161 2.486(14) . . ? C15 H14 2.028(10) . . ? C16 C162 2.484(16) . . ? C16 C166 2.512(19) . . ? C16 H15 2.039(9) . . ? C121 C123 2.412(15) . . ? C121 C124 2.780(16) . . ? C121 C125 2.433(13) . . ? C121 H122 2.061(7) . . ? C121 H126 2.083(6) . . ? C122 C124 2.389(14) . . ? C122 C125 2.784(10) . . ? C122 C126 2.406(10) . . ? C122 H123 2.053(11) . . ? C123 C125 2.384(11) . . ? C123 C126 2.761(13) . . ? C123 H122 2.070(11) . . ? C123 H124 2.016(10) . . ? C124 C126 2.395(17) . . ? C124 H123 2.013(8) . . ? C124 H125 2.059(8) . . ? C125 H124 2.042(12) . . ? C125 H126 2.070(12) . . ? C126 H125 2.069(11) . . ? C161 C163 2.406(18) . . ? C161 C164 2.78(2) . . ? C161 C165 2.40(3) . . ? C161 H162 2.084(10) . . ? C161 H166 2.047(10) . . ? C162 C164 2.41(3) . . ? C162 C165 2.72(2) . . ? C162 C166 2.363(17) . . ? C162 H163 2.062(13) . . ? C163 C165 2.30(3) . . ? C163 C166 2.71(2) . . ? C163 H162 2.098(17) . . ? C163 H164 2.008(18) . . ? C164 C166 2.35(3) . . ? C164 H163 2.08(3) . . ? C164 H165 1.96(3) . . ? C165 H164 1.99(2) . . ? C165 H166 2.06(2) . . ? C166 H165 2.041(17) . . ? O2 C22 2.365(10) . . ? O2 C26 2.380(9) . . ? O2 C221 2.808(10) . . ? O2 C222 2.914(11) . . ? O2 C261 2.844(10) . . ? C21 C23 2.391(13) . . ? C21 C24 2.781(12) . . ? C21 C25 2.419(11) . . ? C21 C221 2.481(12) . . ? C21 C261 2.525(12) . . ? C22 C24 2.414(12) . . ? C22 C25 2.786(12) . . ? C22 C26 2.428(12) . . ? C22 C222 2.499(13) . . ? C22 C226 2.482(10) . . ? C22 H23 2.056(8) . . ? C23 C25 2.380(14) . . ? C23 C26 2.766(13) . . ? C23 C221 2.485(11) . . ? C23 H24 2.041(9) . . ? C24 C26 2.401(14) . . ? C24 H23 2.048(11) . . ? C24 H25 2.038(12) . . ? C25 C261 2.490(13) . . ? C25 H24 2.047(9) . . ? C26 C262 2.505(17) . . ? C26 C266 2.526(12) . . ? C26 H25 2.046(8) . . ? C221 C223 2.429(14) . . ? C221 C224 2.803(12) . . ? C221 C225 2.415(10) . . ? C221 H222 2.048(9) . . ? C221 H226 2.035(8) . . ? C222 C224 2.390(10) . . ? C222 C225 2.742(11) . . ? C222 C226 2.365(13) . . ? C222 H223 2.054(9) . . ? C223 C225 2.369(16) . . ? C223 C226 2.749(16) . . ? C223 H222 2.057(8) . . ? C223 H224 2.032(8) . . ? C224 C226 2.399(16) . . ? C224 H223 2.045(11) . . ? C224 H225 2.039(12) . . ? C225 H224 2.054(13) . . ? C225 H226 2.043(12) . . ? C226 H225 2.055(7) . . ? C261 C263 2.435(18) . . ? C261 C264 2.811(14) . . ? C261 C265 2.425(12) . . ? C261 H262 2.040(10) . . ? C261 H266 2.048(9) . . ? C262 C264 2.371(14) . . ? C262 C265 2.712(14) . . ? C262 C266 2.346(16) . . ? C262 H263 2.060(13) . . ? C263 C265 2.342(18) . . ? C263 C266 2.74(2) . . ? C263 H262 2.022(12) . . ? C263 H264 2.040(12) . . ? C264 C266 2.392(17) . . ? C264 H263 2.016(13) . . ? C264 H265 2.011(14) . . ? C265 H264 2.022(12) . . ? C265 H266 2.058(12) . . ? C266 H265 2.058(9) . . ? O3 C32 2.388(11) . . ? O3 C36 2.371(7) . . ? O3 C321 2.880(13) . . ? O3 C322 2.942(13) . . ? O3 C361 2.874(10) . . ? O3 C362 2.990(13) . . ? C31 C33 2.434(13) . . ? C31 C34 2.802(10) . . ? C31 C35 2.414(9) . . ? C31 C321 2.536(15) . . ? C31 C361 2.526(14) . . ? C32 C34 2.406(9) . . ? C32 C35 2.772(12) . . ? C32 C36 2.427(14) . . ? C32 C322 2.511(10) . . ? C32 C326 2.480(15) . . ? C32 H33 2.060(9) . . ? C33 C35 2.381(15) . . ? C33 C36 2.797(15) . . ? C33 C321 2.470(10) . . ? C33 C326 2.981(13) . . ? C33 H34 2.028(7) . . ? C34 C36 2.436(13) . . ? C34 H33 2.030(12) . . ? C34 H35 2.058(12) . . ? C35 C361 2.484(14) . . ? C35 H34 2.054(10) . . ? C36 C362 2.517(15) . . ? C36 C366 2.492(17) . . ? C36 H35 2.064(6) . . ? C321 C323 2.422(11) . . ? C321 C324 2.779(14) . . ? C321 C325 2.390(17) . . ? C321 H322 2.063(9) . . ? C321 H326 2.051(10) . . ? C322 C324 2.362(17) . . ? C322 C325 2.721(18) . . ? C322 C326 2.373(15) . . ? C322 H323 2.052(8) . . ? C323 C325 2.331(17) . . ? C323 C326 2.743(12) . . ? C323 H322 2.068(12) . . ? C323 H324 1.985(13) . . ? C324 C326 2.401(12) . . ? C324 H323 2.015(13) . . ? C324 H325 2.027(12) . . ? C325 H324 2.026(10) . . ? C325 H326 2.078(10) . . ? C326 H325 2.066(11) . . ? C361 C363 2.396(18) . . ? C361 C364 2.76(3) . . ? C361 C365 2.38(2) . . ? C361 H362 2.053(8) . . ? C361 H366 2.066(8) . . ? C362 C364 2.35(3) . . ? C362 C365 2.714(18) . . ? C362 C366 2.388(13) . . ? C362 H363 2.035(12) . . ? C363 C365 2.359(18) . . ? C363 C366 2.751(16) . . ? C363 H362 2.027(18) . . ? C363 H364 2.021(18) . . ? C364 C366 2.38(2) . . ? C364 H363 2.051(18) . . ? C364 H365 2.021(16) . . ? C365 H364 2.057(18) . . ? C365 H366 2.052(19) . . ? C366 H365 2.033(14) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC O1 Lu C11 17.7(2) . . . ? O1 Lu C121 65.2(3) . . . ? O1 Lu C122 83.2(3) . . . ? O1 Lu C123 110.0(2) . . . ? O1 Lu C124 121.0(3) . . . ? O1 Lu C125 105.4(3) . . . ? O1 Lu C126 78.1(3) . . . ? O1 Lu O2 115.4(2) . . . ? O1 Lu C222 79.0(2) . . . ? O1 Lu O3 113.9(2) . . . ? C11 Lu C121 47.6(3) . . . ? C11 Lu C122 66.4(3) . . . ? C11 Lu C123 92.8(3) . . . ? C11 Lu C124 103.7(3) . . . ? C11 Lu C125 90.7(3) . . . ? C11 Lu C126 63.4(3) . . . ? C11 Lu O2 115.38(18) . . . ? C11 Lu C222 95.2(2) . . . ? C11 Lu O3 120.9(2) . . . ? C121 Lu C122 28.2(2) . . . ? C121 Lu C123 48.6(3) . . . ? C121 Lu C124 56.2(3) . . . ? C121 Lu C125 49.5(3) . . . ? C121 Lu C126 29.0(2) . . . ? C121 Lu O2 108.2(2) . . . ? C121 Lu C222 139.7(3) . . . ? C121 Lu O3 119.0(2) . . . ? C122 Lu C123 27.1(3) . . . ? C122 Lu C124 46.9(3) . . . ? C122 Lu C125 56.2(2) . . . ? C122 Lu C126 49.7(2) . . . ? C122 Lu O2 81.0(2) . . . ? C122 Lu C222 134.9(2) . . . ? C122 Lu O3 133.6(2) . . . ? C123 Lu C124 25.4(2) . . . ? C123 Lu C125 46.3(2) . . . ? C123 Lu C126 55.9(3) . . . ? C123 Lu O2 73.0(2) . . . ? C123 Lu C222 142.3(2) . . . ? C123 Lu O3 115.5(3) . . . ? C124 Lu C125 26.2(3) . . . ? C124 Lu C126 47.5(3) . . . ? C124 Lu O2 89.3(3) . . . ? C124 Lu C222 156.8(3) . . . ? C124 Lu O3 90.4(2) . . . ? C125 Lu C126 27.4(3) . . . ? C125 Lu O2 115.5(3) . . . ? C125 Lu C222 168.84(18) . . . ? C125 Lu O3 77.5(2) . . . ? C126 Lu O2 128.1(2) . . . ? C126 Lu C222 155.6(3) . . . ? C126 Lu O3 90.2(2) . . . ? O2 Lu C222 70.2(2) . . . ? O2 Lu O3 122.0(2) . . . ? C222 Lu O3 91.4(2) . . . ? Lu O1 C11 134.5(6) . . . ? Lu C11 O1 27.8(4) . . . ? Lu C11 C12 90.4(6) . . . ? Lu C11 C16 149.6(6) . . . ? O1 C11 C12 118.2(9) . . . ? O1 C11 C16 121.8(8) . . . ? C12 C11 C16 119.9(7) . . . ? C11 C12 C13 119.8(9) . . . ? C11 C12 C121 115.9(7) . . . ? C13 C12 C121 124.3(9) . . . ? C12 C13 C14 120.2(9) . . . ? C12 C13 H13 120.1(11) . . . ? C14 C13 H13 119.7(9) . . . ? C13 C14 C15 119.7(9) . . . ? C13 C14 H14 120.6(11) . . . ? C15 C14 H14 119.7(11) . . . ? C14 C15 C16 122.2(11) . . . ? C14 C15 H15 119.6(9) . . . ? C16 C15 H15 118.2(10) . . . ? C11 C16 C15 118.1(9) . . . ? C11 C16 C161 121.7(8) . . . ? C15 C16 C161 120.2(10) . . . ? Lu C121 C12 105.7(6) . . . ? Lu C121 C122 80.3(5) . . . ? Lu C121 C126 77.2(5) . . . ? C12 C121 C122 121.3(7) . . . ? C12 C121 C126 119.5(8) . . . ? C122 C121 C126 118.8(9) . . . ? Lu C122 C121 71.4(5) . . . ? Lu C122 C123 82.5(5) . . . ? Lu C122 H122 116.9(7) . . . ? C121 C122 C123 119.8(7) . . . ? C121 C122 H122 120.1(10) . . . ? C123 C122 H122 120.1(8) . . . ? Lu C123 C122 70.5(5) . . . ? Lu C123 C124 78.9(6) . . . ? Lu C123 H123 119.5(7) . . . ? C122 C123 C124 120.8(9) . . . ? C122 C123 H123 119.3(8) . . . ? C124 C123 H123 119.8(11) . . . ? Lu C124 C123 75.7(7) . . . ? Lu C124 C125 73.7(7) . . . ? Lu C124 H124 124.5(7) . . . ? C123 C124 C125 121.2(11) . . . ? C123 C124 H124 119.7(10) . . . ? C125 C124 H124 119.0(8) . . . ? Lu C125 C124 80.0(7) . . . ? Lu C125 C126 69.1(6) . . . ? Lu C125 H125 121.6(7) . . . ? C124 C125 C126 118.9(8) . . . ? C124 C125 H125 120.5(11) . . . ? C126 C125 H125 120.6(10) . . . ? Lu C126 C121 73.8(5) . . . ? Lu C126 C125 83.4(6) . . . ? Lu C126 H126 114.2(7) . . . ? C121 C126 C125 120.5(8) . . . ? C121 C126 H126 119.9(11) . . . ? C125 C126 H126 119.6(8) . . . ? C16 C161 C162 119.9(9) . . . ? C16 C161 C166 122.7(10) . . . ? C162 C161 C166 117.4(12) . . . ? C161 C162 C163 119.6(12) . . . ? C161 C162 H162 120.0(12) . . . ? C163 C162 H162 120.4(13) . . . ? C162 C163 C164 120.7(15) . . . ? C162 C163 H163 117.6(17) . . . ? C164 C163 H163 121.6(16) . . . ? C163 C164 C165 119(2) . . . ? C163 C164 H164 118(2) . . . ? C165 C164 H164 123(3) . . . ? C164 C165 C166 122(2) . . . ? C164 C165 H165 119(2) . . . ? C166 C165 H165 119(2) . . . ? C161 C166 C165 120.6(14) . . . ? C161 C166 H166 119.3(16) . . . ? C165 C166 H166 120.1(15) . . . ? Lu O2 C21 149.1(5) . . . ? O2 C21 C22 120.3(7) . . . ? O2 C21 C26 119.7(8) . . . ? C22 C21 C26 119.9(7) . . . ? C21 C22 C23 118.9(8) . . . ? C21 C22 C221 120.3(7) . . . ? C23 C22 C221 120.8(8) . . . ? C22 C23 C24 121.6(9) . . . ? C22 C23 H23 119.2(9) . . . ? C24 C23 H23 119.2(9) . . . ? C23 C24 C25 119.8(8) . . . ? C23 C24 H24 119.6(11) . . . ? C25 C24 H24 120.7(10) . . . ? C24 C25 C26 120.7(8) . . . ? C24 C25 H25 120.1(8) . . . ? C26 C25 H25 119.3(9) . . . ? C21 C26 C25 119.2(8) . . . ? C21 C26 C261 120.9(7) . . . ? C25 C26 C261 119.8(8) . . . ? C22 C221 C222 121.5(6) . . . ? C22 C221 C226 121.2(9) . . . ? C222 C221 C226 117.3(8) . . . ? Lu C222 C221 99.4(6) . . . ? Lu C222 C223 99.3(6) . . . ? Lu C222 H222 70.4(5) . . . ? C221 C222 C223 121.4(7) . . . ? C221 C222 H222 118.9(8) . . . ? C223 C222 H222 119.7(9) . . . ? C222 C223 C224 120.1(10) . . . ? C222 C223 H223 119.1(8) . . . ? C224 C223 H223 120.8(9) . . . ? C223 C224 C225 119.6(9) . . . ? C223 C224 H224 119.7(12) . . . ? C225 C224 H224 120.8(9) . . . ? C224 C225 C226 120.2(8) . . . ? C224 C225 H225 119.8(10) . . . ? C226 C225 H225 120.0(12) . . . ? C221 C226 C225 121.5(10) . . . ? C221 C226 H226 119.5(8) . . . ? C225 C226 H226 119.0(8) . . . ? C26 C261 C262 121.2(8) . . . ? C26 C261 C266 123.2(10) . . . ? C262 C261 C266 115.6(9) . . . ? C261 C262 C263 122.9(10) . . . ? C261 C262 H262 119.3(11) . . . ? C263 C262 H262 117.8(13) . . . ? C262 C263 C264 119.7(13) . . . ? C262 C263 H263 121.2(12) . . . ? C264 C263 H263 119.1(12) . . . ? C263 C264 C265 119.6(11) . . . ? C263 C264 H264 120.8(14) . . . ? C265 C264 H264 119.5(11) . . . ? C264 C265 C266 120.8(9) . . . ? C264 C265 H265 119.3(10) . . . ? C266 C265 H265 119.8(11) . . . ? C261 C266 C265 121.3(10) . . . ? C261 C266 H266 119.5(10) . . . ? C265 C266 H266 119.2(9) . . . ? Lu O3 C31 167.4(6) . . . ? O3 C31 C32 120.2(7) . . . ? O3 C31 C36 120.2(9) . . . ? C32 C31 C36 119.6(6) . . . ? C31 C32 C33 119.7(8) . . . ? C31 C32 C321 122.2(6) . . . ? C33 C32 C321 118.0(9) . . . ? C32 C33 C34 120.8(10) . . . ? C32 C33 H33 119.8(9) . . . ? C34 C33 H33 119.5(7) . . . ? C33 C34 C35 119.8(7) . . . ? C33 C34 H34 119.5(11) . . . ? C35 C34 H34 120.7(9) . . . ? C34 C35 C36 121.3(8) . . . ? C34 C35 H35 120.3(7) . . . ? C36 C35 H35 118.4(10) . . . ? C31 C36 C35 118.8(9) . . . ? C31 C36 C361 122.9(6) . . . ? C35 C36 C361 118.3(7) . . . ? C32 C321 C322 120.9(9) . . . ? C32 C321 C326 121.2(7) . . . ? C322 C321 C326 117.9(9) . . . ? C321 C322 C323 120.3(10) . . . ? C321 C322 H322 118.9(9) . . . ? C323 C322 H322 120.9(8) . . . ? C322 C323 C324 120.9(9) . . . ? C322 C323 H323 118.6(12) . . . ? C324 C323 H323 120.5(10) . . . ? C323 C324 C325 119.9(10) . . . ? C323 C324 H324 119.8(10) . . . ? C325 C324 H324 120.3(13) . . . ? C324 C325 C326 120.9(12) . . . ? C324 C325 H325 118.8(11) . . . ? C326 C325 H325 120.3(10) . . . ? C321 C326 C325 120.1(9) . . . ? C321 C326 H326 119.9(9) . . . ? C325 C326 H326 120.0(12) . . . ? C36 C361 C362 122.0(9) . . . ? C36 C361 C366 120.2(8) . . . ? C362 C361 C366 117.8(11) . . . ? C361 C362 C363 121.4(11) . . . ? C361 C362 H362 118.5(12) . . . ? C363 C362 H362 120.0(10) . . . ? C362 C363 C364 120.2(12) . . . ? C362 C363 H363 119.9(15) . . . ? C364 C363 H363 120.0(17) . . . ? C363 C364 C365 119(2) . . . ? C363 C364 H364 118.5(14) . . . ? C365 C364 H364 122(2) . . . ? C364 C365 C366 121.7(15) . . . ? C364 C365 H365 118(2) . . . ? C366 C365 H365 120.1(14) . . . ? C361 C366 C365 119.5(10) . . . ? C361 C366 H366 119.5(13) . . . ? C365 C366 H366 121.0(11) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min -16 _reflns_limit_k_max 15 _reflns_limit_l_min -12 _reflns_limit_l_max 12 _reflns_number_total 7068 #ActaC _reflns_number_observed 4705 #ActaC _reflns_observed_criterion refl_observed_if_I____>4.000_sigma(I___) _reflns_d_resolution_high .841 _reflns_d_resolution_low 15.147