# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Bharadwaj, Parimal K.' 'Das, Puspendu K.' 'Krishnan, Anu' 'Mukhopadhyay, Pritam' 'Savitha, G.' _publ_contact_author_name 'Dr Parimal K Bharadwaj' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Kanpur 208016 INDIA ; _publ_contact_author_email 'PKB@IITK.AC.IN' _publ_section_title ; A new class of three dimensional D-pi-A trigonal cryptand derivatives for second-order nonlinear optics ; data_L1 _database_code_CSD 172621 _audit_creation_date 25-01-02 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source synthesized _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical 'C51 H51 N11 O15' _chemical_formula_moiety 'C51 H51 N11 O15 1/3(C5 H5 N)' _chemical_formula_structural 'C56 H56 N12 O15' _chemical_formula_sum 'C158 H158 N34 O45' _chemical_formula_weight ? _chemical_melting_point '215 Celcius' _computing_data_collection 'CAD4 Express (Enraf Nonius,1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius,1994)' _computing_data_reduction 'XCAD4(Harms and Wocadlo,1995)' _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 16.63(5) _cell_length_b 16.63(6) _cell_length_c 16.00(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3832(14) _cell_formula_units_Z 3 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 14.3 _cell_special_details ; ? ; _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3 _symmetry_space_group_name_Hall P3 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -y,+x-y,+z -x+y,-x,+z _exptl_crystal_description triangular _exptl_crystal_preparation 'evaporation from pyridine solution' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas 1.43 _exptl_crystal_density_method floatation _exptl_crystal_F_000 1704 _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 0.11/ _exptl_absorpt_correction_type 'Not done' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK-alpha _diffrn_radiation_source 'fine focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'proportional counter' _diffrn_measurement_device 'Enraf Nonius Turbo CAD4' _diffrn_measurement_method theta-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every hour' _diffrn_standards_decay_% 'less than 0.3%' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1, 4, -2 0 -4 1 0 -4 0 loop_ _diffrn_attenuator_code ? _diffrn_attenuator_scale 13.648 _diffrn_reflns_number 3753 _diffrn_reflns_av_R_equivalents .034 _diffrn_reflns_av_sigmaI/netI .092 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 22.47 _diffrn_reflns_reduction_process No_monochr_Lp_applied 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 ? 0 158 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 158 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 34 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 45 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom O1a .5342(8) .3134(8) -.063(1) .098(8) Uani ? ? O2a .4357(8) .2090(8) .019(1) .075(7) Uani ? ? O3a .586(1) .097(1) -.239(1) .11(1) Uani ? ? O4a .466(1) -.026(1) -.290(2) .14(1) Uani ? ? O5a .1429(7) .1885(6) .066(1) .058(6) Uani ? ? N1a .00000 .00000 -.136(2) .034(8) Uani ? ? N2a .2602(7) .1486(7) -.099(1) .041(6) Uani ? ? N3a .4661(9) .238(1) -.051(1) .059(8) Uani ? ? N4a .503(1) .050(1) -.253(2) .09(1) Uani ? ? N5a .00000 .00000 .152(2) .044(9) Uani ? ? C1a .0953(9) .0696(9) -.157(1) .046(4) Uiso ? ? C2a .1605(9) .0740(9) -.091(1) .042(3) Uiso ? ? C3a .3238(9) .1306(9) -.138(1) .042(3) Uiso ? ? C4a .4193(9) .1752(9) -.122(1) .041(3) Uiso ? ? C5a .480(1) .153(1) -.162(1) .050(4) Uiso ? ? C6a .444(1) .083(1) -.217(1) .062(4) Uiso ? ? C7a .350(1) .035(1) -.236(1) .061(4) Uiso ? ? C8a .292(1) .059(1) -.198(1) .051(4) Uiso ? ? C9a .2880(9) .2302(9) -.046(1) .042(3) Uiso ? ? C10a .2275(9) .2735(9) -.052(1) .040(3) Uiso ? ? C11a .242(1) .334(1) -.115(1) .063(4) Uiso ? ? C12a .194(1) .383(1) -.122(1) .068(5) Uiso ? ? C13a .238(1) -.122(1) -.062(2) .065(5) Uiso ? ? C14a .1071(9) .298(1) .005(1) .048(4) Uiso ? ? C15a .1576(9) .252(1) .009(1) .044(4) Uiso ? ? C16a .074(1) .169(1) .129(1) .054(4) Uiso ? ? C17a .068(1) .092(1) .185(1) .061(4) Uiso ? ? O1b .2688(8) .0004(7) .526(1) .092(8) Uani ? ? O2b .1586(9) .0113(9) .464(1) .102(9) Uani ? ? O3b .1106(8) -.0576(8) -.344(1) .092(8) Uani ? ? O4b .1507(9) -.1570(9) -.310(1) .12(1) Uani ? ? O5b .6194(6) .4540(6) .315(1) .054(5) Uani ? ? N1b .66666 .33333 .625(2) .06(1) Uani ? ? N2b .4304(7) .1985(7) .523(1) .050(6) Uani ? ? N3b .2287(9) .0422(9) .508(1) .069(8) Uani ? ? N4b .136(1) .233(1) .661(1) .070(9) Uani ? ? N5b .66666 .33333 .210(2) .05(1) Uani ? ? C1b .5680(9) .269(1) .624(1) .045(4) Uiso ? ? C2b .527(1) .2753(9) .539(1) .050(4) Uiso ? ? C3b .3570(9) .1997(9) .559(1) .040(3) Uiso ? ? C4b .2606(9) .1324(9) .548(1) .046(4) Uiso ? ? C5b .191(1) .145(1) .579(1) .055(4) Uiso ? ? C6b .212(1) .222(1) .627(1) .054(4) Uiso ? ? C7b .303(1) .286(1) .645(1) .053(4) Uiso ? ? C8b .371(1) .272(1) .613(1) .050(4) Uiso ? ? C9b .427(1) .156(1) .441(1) .054(4) Uiso ? ? C10b .4773(9) .1012(9) .445(1) .040(3) Uiso ? ? C11b .465(1) .047(1) .511(1) .051(4) Uiso ? ? C12b .480(1) .482(1) .515(1) .058(4) Uiso ? ? C13b .433(1) .426(1) .454(1) .062(4) Uiso ? ? C14b .587(1) .062(1) .385(1) .051(4) Uiso ? ? C15b .572(1) .463(1) .381(1) .050(4) Uiso ? ? C16b .606(1) .172(1) .244(1) .055(4) Uiso ? ? C17b .604(1) .237(1) .186(1) .061(4) Uiso ? ? O1c .4341(7) .4112(7) .046(1) .066(6) Uani ? ? O2c .4778(8) .012(1) -.033(1) .098(9) Uani ? ? O3c -.115(1) .1953(8) .159(1) .102(9) Uani ? ? O4c .7808(8) .7195(9) .283(1) .090(8) Uani ? ? O5c .5096(6) .7430(6) .370(1) .056(6) Uani ? ? N1c .33333 .66667 .052(2) .04(1) Uani ? ? N2c .3720(7) .5277(7) .146(1) .042(6) Uani ? ? N3c .4956(8) .4930(9) .033(1) .050(7) Uani ? ? N4c -.0678(9) .2477(9) .214(2) .062(8) Uani ? ? N5c .33333 .66667 .450(2) .05(1) Uani ? ? C1c .359(1) .603(1) .019(2) .093(6) Uiso ? ? C2c .336(1) .517(1) .063(1) .050(4) Uiso ? ? C3c .4622(9) .5544(9) .163(1) .040(3) Uiso ? ? C4c .5249(9) .5527(9) .107(1) .039(3) Uiso ? ? C5c .6206(9) .5969(9) .121(1) .041(3) Uiso ? ? C6c .653(1) .639(1) .195(1) .052(4) Uiso ? ? C7c .593(1) .6341(9) .259(1) .048(4) Uiso ? ? C8c .5021(9) .5926(9) .241(1) .044(3) Uiso ? ? C9c .309(1) .513(1) .214(1) .054(4) Uiso ? ? C10c .277(1) .425(1) .263(1) .050(4) Uiso ? ? C11c .2867(9) .3526(9) .230(1) .047(4) Uiso ? ? C12c .256(1) .271(1) .278(1) .063(5) Uiso ? ? C13c .211(1) .262(1) .349(1) .062(4) Uiso ? ? C14c .200(1) .331(1) .385(1) .054(4) Uiso ? ? C15c .585(1) .821(1) .338(1) .050(4) Uiso ? ? C16c .221(1) .498(1) .458(1) .059(4) Uiso ? ? C17c .241(1) .593(1) .477(1) .068(5) Uiso ? ? C1PY .337(3) -.251(2) -.272(2) .16(1) Uiso ? ? C2PY .334(3) -.416(2) -.271(2) .16(1) Uiso ? ? H011a .11287 .05576 -.21186 .05000 Uiso ? ? H012a .10054 .13005 -.16407 .05000 Uiso ? ? H021a .13858 .08244 -.04025 .05000 Uiso ? ? H022a .15799 .01502 -.09190 .05000 Uiso ? ? H05a .54489 .18682 -.15180 .05000 Uiso ? ? H07a .32593 -.01617 -.27922 .05000 Uiso ? ? H08a .22753 .02729 -.21699 .05000 Uiso ? ? H091a .28876 .21198 .00867 .05000 Uiso ? ? H092a .35053 .27609 -.06286 .05000 Uiso ? ? H11a .28687 .34393 -.15763 .05000 Uiso ? ? H12a .17056 .42703 -.12731 .05000 Uiso ? ? H13a .24745 -.17437 -.06173 .05000 Uiso ? ? H14a .08118 .33939 .00337 .05000 Uiso ? ? H161a .08941 .22378 .15890 .05000 Uiso ? ? H162a .01393 .14861 .10171 .05000 Uiso ? ? H171a .12938 .09913 .18407 .05000 Uiso ? ? H172a .05224 .10014 .23779 .05000 Uiso ? ? H011b .55501 .20721 .63170 .05000 Uiso ? ? H012b .53823 .28453 .66687 .05000 Uiso ? ? H021b .52820 .33378 .53504 .05000 Uiso ? ? H022b .56791 .27626 .49438 .05000 Uiso ? ? H05b .12629 .09957 .56582 .05000 Uiso ? ? H07b .31782 .33863 .67730 .05000 Uiso ? ? H08b .43537 .31527 .62797 .05000 Uiso ? ? H091b .36337 .11534 .42261 .05000 Uiso ? ? H092b .45494 .20291 .39577 .05000 Uiso ? ? H11b .45842 -.00956 .53498 .05000 Uiso ? ? H12b .50438 .54328 .53708 .05000 Uiso ? ? H13b .38213 .42820 .42005 .05000 Uiso ? ? H14b .59888 .00986 .37923 .05000 Uiso ? ? H161b .65881 .16285 .24941 .05000 Uiso ? ? H162b .55136 .11160 .25565 .05000 Uiso ? ? H171b .62180 .22627 .12686 .05000 Uiso ? ? H172b .54160 .22661 .17607 .05000 Uiso ? ? H011c .34245 .59188 -.04131 .05000 Uiso ? ? H012c .43026 .63897 .01474 .05000 Uiso ? ? H021c .26690 .48368 .06376 .05000 Uiso ? ? H022c .35103 .47898 .02766 .05000 Uiso ? ? H05c .66161 .59535 .07711 .05000 Uiso ? ? H07c .61779 .65983 .31138 .05000 Uiso ? ? H08c .45966 .58864 .28287 .05000 Uiso ? ? H091c .33928 .56656 .24915 .05000 Uiso ? ? H092c .25498 .51388 .18980 .05000 Uiso ? ? H11c .31382 .35984 .17348 .05000 Uiso ? ? H12c .26755 .22405 .25720 .05000 Uiso ? ? H13c .18737 .20160 .37595 .05000 Uiso ? ? H14c .14432 .31718 .41187 .05000 Uiso ? ? H161c .17402 .46176 .41262 .05000 Uiso ? ? H162c .21684 .45733 .49744 .05000 Uiso ? ? H171c .19565 .60471 .44589 .05000 Uiso ? ? H172c .23425 .59854 .53245 .05000 Uiso ? ? H1PY .28680 -.23481 -.27243 .05000 Uiso ? ? 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 O1a .044(7) .055(8) .15(1) -.009(6) .007(8) -.018(8) O2a .090(9) .068(8) .083(9) .053(7) -.023(8) -.006(7) O3a .07(1) .16(1) .14(1) .08(1) .030(9) -.00(1) O4a .13(1) .14(2) .16(2) .09(1) .01(1) -.05(1) O5a .053(7) .045(6) .089(8) .033(5) .011(6) .006(6) N1a .016(6) .016(6) .07(1) .008(3) .00000 .00000 N2a .021(6) .027(6) .067(8) .006(5) .004(5) -.010(6) N3a .036(8) .06(1) .08(1) .025(8) .001(8) .014(8) N4a .07(1) .12(2) .10(1) .07(1) .03(1) .03(1) N5a .040(7) .040(7) .05(1) .020(4) .00000 .00000 O1b .058(8) .041(7) .18(1) .027(6) .003(8) -.001(8) O2b .075(9) .09(1) .13(1) .034(8) -.024(8) -.058(9) O3b .09(1) .037(7) .11(1) -.000(7) -.008(8) -.012(7) O4b .064(9) .09(1) .16(1) .012(8) -.060(9) .027(9) O5b .043(6) .042(6) .071(7) .018(5) -.017(5) -.010(5) N1b .028(7) .028(7) .14(2) .014(4) .00000 .00000 N2b .030(7) .039(7) .070(9) .010(6) .000(6) -.014(6) N3b .049(9) .060(9) .09(1) .020(8) -.002(8) -.025(8) N4b .05(1) .09(1) .07(1) .045(9) .006(8) -.009(9) N5b .041(7) .041(7) .07(1) .021(4) .00000 .00000 O1c .044(6) .045(7) .105(9) .019(6) .001(6) -.012(6) O2c .061(8) .15(1) .073(9) .044(9) .003(7) .038(9) O3c .10(1) .044(8) .14(1) .019(7) -.03(1) -.011(8) O4c .060(8) .090(9) .11(1) .030(7) -.035(8) -.009(9) O5c .050(6) .048(6) .073(8) .027(5) -.006(5) -.000(5) N1c .025(6) .025(6) .08(2) .012(3) .00000 .00000 N2c .025(6) .037(6) .067(9) .019(5) .006(6) .009(6) N3c .034(7) .050(9) .067(9) .023(7) .000(7) -.007(7) N4c .053(9) .038(8) .09(1) .020(7) .016(8) .015(9) N5c .029(7) .029(7) .09(2) .015(3) .00000 .00000 _atom_sites_solution_primary 'all O, N and most C atoms' _atom_sites_solution_secondary 'rest of the C atoms' _atom_sites_solution_hydrogens 'calculated positions' _refine_special_details 'sfls:_F_counting statistical weight_full_matrix' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'counting statistical' _refine_ls_hydrogen_treatment 'no refinement' _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 1991 _refine_ls_number_parameters 447 _refine_ls_number_restraints 'all C atoms isotropic' _refine_ls_number_constraints 0 _refine_ls_R_factor_all .113 _refine_ls_R_factor_obs .066 _refine_ls_wR_factor_all .109 _refine_ls_wR_factor_obs .065 _refine_ls_goodness_of_fit_all 2.903 _refine_ls_goodness_of_fit_obs 2.321 _refine_ls_shift/esd_max 0.0005 _refine_ls_shift/esd_mean 0.0003 _refine_diff_density_min -.488 _refine_diff_density_max .705 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1b N3b 1.22(3) 3_665 3_665 ? O2b N3b 1.23(2) 3_665 3_665 ? O3b N4b 1.21(3) 1_666 3_665 ? O4b N4b 1.20(4) 1_666 3_665 ? O5b C15b 1.37(3) . . ? O5b C16b 1.48(3) . 3_665 ? N1b C1b 1.44(2) . 3_665 ? N1b C1b 1.44(1) . . ? N1b C1b 1.44(5) . 2_655 ? N2b C2b 1.50(2) 3_665 3_665 ? N2b C3b 1.36(2) 3_665 3_665 ? N2b C9b 1.47(3) 3_665 3_665 ? N3b C4b 1.46(4) 3_665 3_665 ? N4b C6b 1.46(3) 3_665 3_665 ? N5b C17b 1.46(3) . 3_665 ? N5b C17b 1.46(4) . . ? N5b C17b 1.46(5) . 2_655 ? C1b C2b 1.54(3) 3_665 3_665 ? C1b H011b .95(3) 3_665 3_665 ? C1b H012b .95(2) 3_665 3_665 ? C2b H021b .97(3) 3_665 3_665 ? C2b H022b .97(2) 3_665 3_665 ? C3b C4b 1.44(2) 3_665 3_665 ? C3b C8b 1.40(4) 3_665 3_665 ? C4b C5b 1.37(3) 3_665 3_665 ? C5b C6b 1.38(4) 3_665 3_665 ? C5b H05b .98(2) 3_665 3_665 ? C6b C7b 1.38(3) 3_665 3_665 ? C7b C8b 1.36(3) 3_665 3_665 ? C7b H07b .94(3) 3_665 3_665 ? C8b H08b .97(2) 3_665 3_665 ? C9b C10b 1.52(4) 3_665 3_665 ? C9b H091b .97(2) 3_665 3_665 ? C9b H092b 1.00(3) 3_665 3_665 ? C10b C11b 1.35(4) 3_665 3_665 ? C10b C15b 1.38(3) 3_665 . ? C11b C12b 1.46(3) 3_665 . ? C11b H11b .97(3) 3_665 3_665 ? C12b C13b 1.31(3) . . ? C12b H11b .99(1) . 3_665 ? C12b H12b .96(2) . . ? C13b C14b 1.38(4) . 3_665 ? C13b H13b 1.02(2) . . ? C13b H14b 1.25(2) . 3_665 ? C14b C15b 1.39(3) 3_665 . ? C14b H14b .99(3) 3_665 3_665 ? C16b C17b 1.45(4) 3_665 3_665 ? C16b H161b .96(2) 3_665 3_665 ? C16b H162b .98(3) 3_665 3_665 ? C17b H171b 1.03(2) 3_665 3_665 ? C17b H172b .98(2) 3_665 3_665 ? H11b H12b .476(1) 3_665 . ? O1c N3c 1.24(3) . . ? O2c N3c 1.21(3) 3_665 . ? O3c N4c 1.21(4) 2_665 2_665 ? O4c N4c 1.22(3) . 2_665 ? O5c C15c 1.38(2) 3_565 3_565 ? O5c C16c 1.44(3) 3_565 . ? O5c H161c 1.09(1) 3_565 . ? N1c C1c 1.43(5) . . ? N1c C1c 1.43(5) . 2_665 ? N1c C1c 1.43(6) . 3_565 ? N2c C2c 1.42(3) . . ? N2c C3c 1.36(2) . . ? N2c C9c 1.46(3) . . ? N3c C4c 1.46(3) . . ? N4c C6c 1.47(3) 2_665 . ? N5c C17c 1.47(2) . . ? N5c C17c 1.47(5) . 2_665 ? N5c C17c 1.47(3) . 3_565 ? C1c C2c 1.46(5) . . ? C1c H011c .99(3) . . ? C1c H012c 1.02(2) . . ? C2c H021c .99(1) . . ? C2c H022c .98(3) . . ? C3c C4c 1.38(3) . . ? C3c C8c 1.41(3) . . ? C4c C5c 1.40(2) . . ? C5c C6c 1.35(3) . . ? C5c H05c .99(2) . . ? C6c C7c 1.40(3) . . ? C7c C8c 1.35(2) . . ? C7c H07c .94(2) . . ? C8c H08c .95(2) . . ? C9c C10c 1.50(4) . . ? C9c H091c .95(3) . . ? C9c H092c .98(2) . . ? C10c C11c 1.40(5) . . ? C10c C15c 1.35(3) . 3_565 ? C11c C12c 1.42(4) . . ? C11c H11c .99(2) . . ? C12c C13c 1.31(3) . . ? C12c H12c .95(4) . . ? C13c C14c 1.39(5) . . ? C13c H13c .98(3) . . ? C14c C15c 1.42(3) . 3_565 ? C14c H14c .93(2) . . ? C16c C17c 1.48(5) . . ? C16c H161c 1.01(2) . . ? C16c H162c .90(3) . . ? C17c H171c 1.00(3) . . ? C17c H172c .91(2) . . ? O1a N3a 1.21(3) 3_666 3_666 ? O2a N3a 1.22(3) 3_666 3_666 ? O3a N4a 1.22(3) 3_666 3_666 ? O4a N4a 1.25(5) 3_666 3_666 ? O5a C15a 1.32(4) 3_666 3_666 ? O5a C16a 1.43(3) 3_666 3_666 ? N1a C1a 1.46(2) 1_666 3_666 ? N1a C1a 1.46(2) 1_666 1_666 ? N1a C1a 1.46(5) 1_666 2_666 ? N2a C2a 1.50(2) 3_666 3_666 ? N2a C3a 1.38(3) 3_666 3_666 ? N2a C9a 1.46(4) 3_666 3_666 ? N3a C4a 1.49(3) 3_666 3_666 ? N4a C6a 1.46(4) 3_666 3_666 ? N5a C17a 1.47(3) 1_666 3_666 ? N5a C17a 1.47(4) 1_666 1_666 ? N5a C17a 1.47(5) 1_666 2_666 ? C1a C2a 1.49(3) 3_666 3_666 ? C1a H011a .98(2) 3_666 3_666 ? C1a H012a .97(3) 3_666 3_666 ? C2a H021a .93(2) 3_666 3_666 ? C2a H022a .96(3) 3_666 3_666 ? C3a C4a 1.40(2) 3_666 3_666 ? C3a C8a 1.42(4) 3_666 3_666 ? C4a C5a 1.38(3) 3_666 3_666 ? C5a C6a 1.34(4) 3_666 3_666 ? C5a H05a .95(2) 3_666 3_666 ? C6a C7a 1.39(2) 3_666 3_666 ? C7a C8a 1.36(4) 3_666 3_666 ? C7a H07a 1.00(3) 3_666 3_666 ? C8a H08a .98(2) 3_666 3_666 ? C9a C10a 1.50(3) 3_666 3_666 ? C9a H091a .93(2) 3_666 3_666 ? C9a H092a .97(2) 3_666 3_666 ? C10a C11a 1.36(4) 3_666 3_666 ? C10a C15a 1.42(3) 3_666 3_666 ? C11a C12a 1.40(5) 3_666 3_666 ? C11a H11a .96(2) 3_666 3_666 ? C12a C13a 1.43(3) 3_666 1_666 ? C12a H12a .99(4) 3_666 3_666 ? C12a H13a 1.29(3) 3_666 1_666 ? C13a C14a 1.42(4) 1_666 3_666 ? C13a H13a .95(2) 1_666 1_666 ? C13a H14a 1.20(2) 1_666 3_666 ? C14a C15a 1.38(4) 3_666 3_666 ? C14a H14a .98(3) 3_666 3_666 ? C16a C17a 1.51(5) 3_666 3_666 ? C16a H161a .94(3) 3_666 3_666 ? C16a H162a .99(2) 3_666 3_666 ? C17a H171a .97(2) 3_666 3_666 ? C17a H172a .92(2) 3_666 3_666 ? C1PY C2PY 1.31(4) 3_666 1_566 ? C1PY H1PY .99(3) 3_666 3_666 ? C1PY C2PY 1.4(1) 3_666 2_556 ? 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 ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15b O5b C16b 118(2) . . 3_665 ? C1b N1b C1b 120(2) 3_665 . . ? C1b N1b C1b 120(2) 3_665 . 2_655 ? C1b N1b C1b 120(2) . . 2_655 ? C2b N2b C3b 120(2) 3_665 3_665 3_665 ? C2b N2b C9b 109(1) 3_665 3_665 3_665 ? C3b N2b C9b 124(1) 3_665 3_665 3_665 ? O1b N3b O2b 125(3) 3_665 3_665 3_665 ? O1b N3b C4b 117(2) 3_665 3_665 3_665 ? O2b N3b C4b 117(3) 3_665 3_665 3_665 ? O3b N4b O4b 125(2) 1_666 3_665 1_666 ? O3b N4b C6b 118(3) 1_666 3_665 3_665 ? O4b N4b C6b 117(2) 1_666 3_665 3_665 ? C17b N5b C17b 114(2) 3_665 . . ? C17b N5b C17b 113(2) 3_665 . 2_655 ? C17b N5b C17b 114(2) . . 2_655 ? N1b C1b C2b 110(2) . 3_665 3_665 ? N1b C1b H011b 111(2) . 3_665 3_665 ? N1b C1b H012b 110(2) . 3_665 3_665 ? C2b C1b H011b 108(2) 3_665 3_665 3_665 ? C2b C1b H012b 109(2) 3_665 3_665 3_665 ? H011b C1b H012b 109(2) 3_665 3_665 3_665 ? N2b C2b C1b 115(2) 3_665 3_665 3_665 ? N2b C2b H021b 108(2) 3_665 3_665 3_665 ? N2b C2b H022b 109(2) 3_665 3_665 3_665 ? C1b C2b H021b 109(2) 3_665 3_665 3_665 ? C1b C2b H022b 109(2) 3_665 3_665 3_665 ? H021b C2b H022b 106(2) 3_665 3_665 3_665 ? N2b C3b C4b 126(2) 3_665 3_665 3_665 ? N2b C3b C8b 121(2) 3_665 3_665 3_665 ? C4b C3b C8b 113(2) 3_665 3_665 3_665 ? N3b C4b C3b 123(2) 3_665 3_665 3_665 ? N3b C4b C5b 114(2) 3_665 3_665 3_665 ? C3b C4b C5b 122(3) 3_665 3_665 3_665 ? C4b C5b C6b 120(2) 3_665 3_665 3_665 ? C4b C5b H05b 119(3) 3_665 3_665 3_665 ? C6b C5b H05b 120(2) 3_665 3_665 3_665 ? N4b C6b C5b 119(2) 3_665 3_665 3_665 ? N4b C6b C7b 121(3) 3_665 3_665 3_665 ? C5b C6b C7b 120(2) 3_665 3_665 3_665 ? C6b C7b C8b 119(3) 3_665 3_665 3_665 ? C6b C7b H07b 120(2) 3_665 3_665 3_665 ? C8b C7b H07b 121(2) 3_665 3_665 3_665 ? C3b C8b C7b 125(2) 3_665 3_665 3_665 ? C3b C8b H08b 116(2) 3_665 3_665 3_665 ? C7b C8b H08b 119(3) 3_665 3_665 3_665 ? N2b C9b C10b 111(2) 3_665 3_665 3_665 ? N2b C9b H091b 112(2) 3_665 3_665 3_665 ? N2b C9b H092b 112(3) 3_665 3_665 3_665 ? C10b C9b H091b 109(3) 3_665 3_665 3_665 ? C10b C9b H092b 108(2) 3_665 3_665 3_665 ? H091b C9b H092b 104(2) 3_665 3_665 3_665 ? C9b C10b C11b 119(2) 3_665 3_665 3_665 ? C9b C10b C15b 121(2) 3_665 3_665 . ? C11b C10b C15b 120(2) 3_665 3_665 . ? C10b C11b C12b 118(2) 3_665 3_665 . ? C10b C11b H11b 150(3) 3_665 3_665 3_665 ? C12b C11b H11b 42(1) . 3_665 3_665 ? C11b C12b C13b 120(2) 3_665 . . ? C11b C12b H11b 41(1) 3_665 . 3_665 ? C11b C12b H12b 68(1) 3_665 . . ? C13b C12b H11b 151(2) . . 3_665 ? C13b C12b H12b 145(2) . . . ? H11b C12b H12b 28.2(5) 3_665 . . ? C12b C13b C14b 122(2) . . 3_665 ? C12b C13b H13b 126(2) . . . ? C12b C13b H14b 157(2) . . 3_665 ? C14b C13b H13b 95(2) 3_665 . . ? C14b C13b H14b 44(1) 3_665 . 3_665 ? H13b C13b H14b 53(1) . . 3_665 ? C13b C14b C15b 118(2) . 3_665 . ? C13b C14b H14b 61(2) . 3_665 3_665 ? C15b C14b H14b 157(2) . 3_665 3_665 ? O5b C15b C10b 117(2) . . 3_665 ? O5b C15b C14b 122(2) . . 3_665 ? C10b C15b C14b 121(2) 3_665 . 3_665 ? O5b C16b C17b 106(2) . 3_665 3_665 ? O5b C16b H161b 124(2) . 3_665 3_665 ? O5b C16b H162b 62(1) . 3_665 3_665 ? C17b C16b H161b 122(2) 3_665 3_665 3_665 ? C17b C16b H162b 121(2) 3_665 3_665 3_665 ? H161b C16b H162b 107(3) 3_665 3_665 3_665 ? N5b C17b C16b 113(2) . 3_665 3_665 ? N5b C17b H171b 108(2) . 3_665 3_665 ? N5b C17b H172b 110(3) . 3_665 3_665 ? C16b C17b H171b 111(3) 3_665 3_665 3_665 ? C16b C17b H172b 114(2) 3_665 3_665 3_665 ? H171b C17b H172b 101(2) 3_665 3_665 3_665 ? C11b H11b C12b 97(2) 3_665 3_665 . ? C11b H11b H12b 161(1) 3_665 3_665 . ? C12b H11b H12b 72(1) . 3_665 . ? C12b H12b H11b 79(1) . . 3_665 ? C13b H14b C14b 75(2) . 3_665 3_665 ? C15c O5c C16c 121(2) 3_565 3_565 . ? C15c O5c H161c 105(1) 3_565 3_565 . ? C16c O5c H161c 44.4(9) . 3_565 . ? C1c N1c C1c 107(3) . . 2_665 ? C1c N1c C1c 107(2) . . 3_565 ? C1c N1c C1c 107(2) 2_665 . 3_565 ? C2c N2c C3c 124(2) . . . ? C2c N2c C9c 117(1) . . . ? C3c N2c C9c 119(2) . . . ? O1c N3c O2c 124(2) . . 3_665 ? O1c N3c C4c 115(2) . . . ? O2c N3c C4c 121(2) 3_665 . . ? O3c N4c O4c 122(3) 2_665 2_665 . ? O3c N4c C6c 118(2) 2_665 2_665 . ? O4c N4c C6c 120(2) . 2_665 . ? C17c N5c C17c 112(2) . . 2_665 ? C17c N5c C17c 112(3) . . 3_565 ? C17c N5c C17c 112(3) 2_665 . 3_565 ? N1c C1c C2c 121(2) . . . ? N1c C1c H011c 110(4) . . . ? N1c C1c H012c 106(3) . . . ? C2c C1c H011c 112(3) . . . ? C2c C1c H012c 105(3) . . . ? H011c C1c H012c 101(2) . . . ? N2c C2c C1c 116(2) . . . ? N2c C2c H021c 111(2) . . . ? N2c C2c H022c 113(3) . . . ? C1c C2c H021c 103(2) . . . ? C1c C2c H022c 109(2) . . . ? H021c C2c H022c 104(2) . . . ? N2c C3c C4c 126(2) . . . ? N2c C3c C8c 121(2) . . . ? C4c C3c C8c 113(1) . . . ? N3c C4c C3c 123(1) . . . ? N3c C4c C5c 113(2) . . . ? C3c C4c C5c 124(2) . . . ? C4c C5c C6c 118(2) . . . ? C4c C5c H05c 120(2) . . . ? C6c C5c H05c 123(1) . . . ? N4c C6c C5c 120(2) 2_665 . . ? N4c C6c C7c 117(2) 2_665 . . ? C5c C6c C7c 122(1) . . . ? C6c C7c C8c 117(2) . . . ? C6c C7c H07c 120(1) . . . ? C8c C7c H07c 123(2) . . . ? C3c C8c C7c 125(2) . . . ? C3c C8c H08c 115(1) . . . ? C7c C8c H08c 120(2) . . . ? N2c C9c C10c 115(3) . . . ? N2c C9c H091c 106(1) . . . ? N2c C9c H092c 106(2) . . . ? C10c C9c H091c 112(2) . . . ? C10c C9c H092c 110(2) . . . ? H091c C9c H092c 107(3) . . . ? C9c C10c C11c 121(2) . . . ? C9c C10c C15c 120(3) . . 3_565 ? C11c C10c C15c 119(2) . . 3_565 ? C10c C11c C12c 119(2) . . . ? C10c C11c H11c 119(3) . . . ? C12c C11c H11c 123(3) . . . ? C11c C12c C13c 119(3) . . . ? C11c C12c H12c 117(2) . . . ? C13c C12c H12c 123(3) . . . ? C12c C13c C14c 125(3) . . . ? C12c C13c H13c 115(3) . . . ? C14c C13c H13c 121(2) . . . ? C13c C14c C15c 115(2) . . 3_565 ? C13c C14c H14c 121(2) . . . ? C15c C14c H14c 111(3) 3_565 . . ? O5c C15c C10c 117(2) 3_565 3_565 . ? O5c C15c C14c 120(2) 3_565 3_565 . ? C10c C15c C14c 123(2) . 3_565 . ? O5c C16c C17c 109(2) 3_565 . . ? O5c C16c H161c 50(1) 3_565 . . ? O5c C16c H162c 126(3) 3_565 . . ? C17c C16c H161c 119(3) . . . ? C17c C16c H162c 123(2) . . . ? H161c C16c H162c 108(3) . . . ? N5c C17c C16c 115(2) . . . ? N5c C17c H171c 106(2) . . . ? N5c C17c H172c 110(2) . . . ? C16c C17c H171c 108(2) . . . ? C16c C17c H172c 109(3) . . . ? H171c C17c H172c 109(3) . . . ? O5c H161c C16c 86(1) 3_565 . . ? C15a O5a C16a 118(2) 3_666 3_666 3_666 ? C1a N1a C1a 114(2) 3_666 1_666 1_666 ? C1a N1a C1a 114(2) 3_666 1_666 2_666 ? C1a N1a C1a 114(2) 1_666 1_666 2_666 ? C2a N2a C3a 121(2) 3_666 3_666 3_666 ? C2a N2a C9a 115(2) 3_666 3_666 3_666 ? C3a N2a C9a 122(1) 3_666 3_666 3_666 ? O1a N3a O2a 123(2) 3_666 3_666 3_666 ? O1a N3a C4a 120(2) 3_666 3_666 3_666 ? O2a N3a C4a 117(2) 3_666 3_666 3_666 ? O3a N4a O4a 124(3) 3_666 3_666 3_666 ? O3a N4a C6a 116(3) 3_666 3_666 3_666 ? O4a N4a C6a 119(2) 3_666 3_666 3_666 ? C17a N5a C17a 108(2) 3_666 1_666 1_666 ? C17a N5a C17a 108(2) 3_666 1_666 2_666 ? C17a N5a C17a 108(2) 1_666 1_666 2_666 ? N1a C1a C2a 110(2) 1_666 3_666 3_666 ? N1a C1a H011a 111(2) 1_666 3_666 3_666 ? N1a C1a H012a 110(1) 1_666 3_666 3_666 ? C2a C1a H011a 110(2) 3_666 3_666 3_666 ? C2a C1a H012a 110(2) 3_666 3_666 3_666 ? H011a C1a H012a 105(2) 3_666 3_666 3_666 ? N2a C2a C1a 117(2) 3_666 3_666 3_666 ? N2a C2a H021a 108(2) 3_666 3_666 3_666 ? N2a C2a H022a 108(2) 3_666 3_666 3_666 ? C1a C2a H021a 107(2) 3_666 3_666 3_666 ? C1a C2a H022a 106(2) 3_666 3_666 3_666 ? H021a C2a H022a 110(2) 3_666 3_666 3_666 ? N2a C3a C4a 127(2) 3_666 3_666 3_666 ? N2a C3a C8a 119(1) 3_666 3_666 3_666 ? C4a C3a C8a 114(2) 3_666 3_666 3_666 ? N3a C4a C3a 124(2) 3_666 3_666 3_666 ? N3a C4a C5a 110(1) 3_666 3_666 3_666 ? C3a C4a C5a 124(2) 3_666 3_666 3_666 ? C4a C5a C6a 118(2) 3_666 3_666 3_666 ? C4a C5a H05a 122(3) 3_666 3_666 3_666 ? C6a C5a H05a 120(2) 3_666 3_666 3_666 ? N4a C6a C5a 120(2) 3_666 3_666 3_666 ? N4a C6a C7a 118(3) 3_666 3_666 3_666 ? C5a C6a C7a 122(2) 3_666 3_666 3_666 ? C6a C7a C8a 119(3) 3_666 3_666 3_666 ? C6a C7a H07a 120(2) 3_666 3_666 3_666 ? C8a C7a H07a 121(2) 3_666 3_666 3_666 ? C3a C8a C7a 122(2) 3_666 3_666 3_666 ? C3a C8a H08a 121(2) 3_666 3_666 3_666 ? C7a C8a H08a 117(3) 3_666 3_666 3_666 ? N2a C9a C10a 116(2) 3_666 3_666 3_666 ? N2a C9a H091a 107(3) 3_666 3_666 3_666 ? N2a C9a H092a 107(2) 3_666 3_666 3_666 ? C10a C9a H091a 109(2) 3_666 3_666 3_666 ? C10a C9a H092a 109(3) 3_666 3_666 3_666 ? H091a C9a H092a 109(2) 3_666 3_666 3_666 ? C9a C10a C11a 119(2) 3_666 3_666 3_666 ? C9a C10a C15a 120(2) 3_666 3_666 3_666 ? C11a C10a C15a 121(2) 3_666 3_666 3_666 ? C10a C11a C12a 123(2) 3_666 3_666 3_666 ? C10a C11a H11a 119(3) 3_666 3_666 3_666 ? C12a C11a H11a 118(3) 3_666 3_666 3_666 ? C11a C12a C13a 116(3) 3_666 3_666 1_666 ? C11a C12a H12a 170(3) 3_666 3_666 3_666 ? C11a C12a H13a 126(2) 3_666 3_666 1_666 ? C13a C12a H12a 71(2) 1_666 3_666 3_666 ? C13a C12a H13a 41(1) 1_666 3_666 1_666 ? H12a C12a H13a 53(2) 3_666 3_666 1_666 ? C12a C13a C14a 121(2) 3_666 1_666 3_666 ? C12a C13a H13a 62(2) 3_666 1_666 1_666 ? C12a C13a H14a 160(2) 3_666 1_666 3_666 ? C14a C13a H13a 121(2) 3_666 1_666 1_666 ? C14a C13a H14a 43(1) 3_666 1_666 3_666 ? H13a C13a H14a 113(2) 1_666 1_666 3_666 ? C13a C14a C15a 120(2) 1_666 3_666 3_666 ? C13a C14a H14a 56(2) 1_666 3_666 3_666 ? C15a C14a H14a 170(2) 3_666 3_666 3_666 ? O5a C15a C10a 118(2) 3_666 3_666 3_666 ? O5a C15a C14a 124(2) 3_666 3_666 3_666 ? C10a C15a C14a 118(2) 3_666 3_666 3_666 ? O5a C16a C17a 108(2) 3_666 3_666 3_666 ? O5a C16a H161a 110(2) 3_666 3_666 3_666 ? O5a C16a H162a 108(2) 3_666 3_666 3_666 ? C17a C16a H161a 113(2) 3_666 3_666 3_666 ? C17a C16a H162a 110(2) 3_666 3_666 3_666 ? H161a C16a H162a 107(3) 3_666 3_666 3_666 ? N5a C17a C16a 111(2) 1_666 3_666 3_666 ? N5a C17a H171a 110(3) 1_666 3_666 3_666 ? N5a C17a H172a 110(2) 1_666 3_666 3_666 ? C16a C17a H171a 106(2) 3_666 3_666 3_666 ? C16a C17a H172a 109(3) 3_666 3_666 3_666 ? H171a C17a H172a 111(2) 3_666 3_666 3_666 ? C12a H13a C13a 77(2) 3_666 1_666 1_666 ? C13a H14a C14a 81(2) 1_666 3_666 3_666 ? C2PY C1PY H1PY 167(6) 1_566 3_666 3_666 ? C2PY C1PY C2PY 122(5) 1_566 3_666 2_556 ? H1PY C1PY C2PY 71(3) 3_666 3_666 2_556 ? C1PY C2PY C1PY 118(4) 3_666 1_566 2_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16b O5b C15b C10b -177(2) 3_665 . . 3_665 ? C16b O5b C15b C14b 4(3) 3_665 . . 3_665 ? C15b O5b C16b C17b -179(2) . . 3_665 3_665 ? C15b O5b C16b H161b -29(4) . . 3_665 3_665 ? C15b O5b C16b H162b 63(2) . . 3_665 3_665 ? C1b N1b C1b C2b -110(3) . . 3_665 3_665 ? C1b N1b C1b H011b 10(4) . . 3_665 3_665 ? C1b N1b C1b H012b 130(3) . . 3_665 3_665 ? C1b N1b C1b C2b 67(3) 2_655 . 3_665 3_665 ? C1b N1b C1b H011b -173(2) 2_655 . 3_665 3_665 ? C1b N1b C1b H012b -52(4) 2_655 . 3_665 3_665 ? C3b N2b C2b C1b 78(3) 3_665 3_665 3_665 3_665 ? C3b N2b C2b H021b -44(3) 3_665 3_665 3_665 3_665 ? C3b N2b C2b H022b -160(2) 3_665 3_665 3_665 3_665 ? C9b N2b C2b C1b -128(2) 3_665 3_665 3_665 3_665 ? C9b N2b C2b H021b 110(2) 3_665 3_665 3_665 3_665 ? C9b N2b C2b H022b -5(3) 3_665 3_665 3_665 3_665 ? C2b N2b C3b C4b 178(2) 3_665 3_665 3_665 3_665 ? C2b N2b C3b C8b -1(4) 3_665 3_665 3_665 3_665 ? C9b N2b C3b C4b 28(4) 3_665 3_665 3_665 3_665 ? C9b N2b C3b C8b -151(3) 3_665 3_665 3_665 3_665 ? C2b N2b C9b C10b 70(3) 3_665 3_665 3_665 3_665 ? C2b N2b C9b H091b -167(3) 3_665 3_665 3_665 3_665 ? C2b N2b C9b H092b -51(3) 3_665 3_665 3_665 3_665 ? C3b N2b C9b C10b -137(2) 3_665 3_665 3_665 3_665 ? C3b N2b C9b H091b -15(4) 3_665 3_665 3_665 3_665 ? C3b N2b C9b H092b 102(3) 3_665 3_665 3_665 3_665 ? O1b N3b C4b C3b 42(3) 3_665 3_665 3_665 3_665 ? O1b N3b C4b C5b -133(2) 3_665 3_665 3_665 3_665 ? O2b N3b C4b C3b -144(2) 3_665 3_665 3_665 3_665 ? O2b N3b C4b C5b 41(3) 3_665 3_665 3_665 3_665 ? O3b N4b C6b C5b 11(4) 1_666 3_665 3_665 3_665 ? O3b N4b C6b C7b -167(3) 1_666 3_665 3_665 3_665 ? O4b N4b C6b C5b -168(3) 1_666 3_665 3_665 3_665 ? O4b N4b C6b C7b 14(4) 1_666 3_665 3_665 3_665 ? C17b N5b C17b C16b 81(2) . . 3_665 3_665 ? C17b N5b C17b H171b -42(3) . . 3_665 3_665 ? C17b N5b C17b H172b -151(2) . . 3_665 3_665 ? C17b N5b C17b C16b -147(2) 2_655 . 3_665 3_665 ? C17b N5b C17b H171b 90(2) 2_655 . 3_665 3_665 ? C17b N5b C17b H172b -20(3) 2_655 . 3_665 3_665 ? N1b C1b C2b N2b 167(2) . 3_665 3_665 3_665 ? N1b C1b C2b H021b -71(2) . 3_665 3_665 3_665 ? N1b C1b C2b H022b 45(3) . 3_665 3_665 3_665 ? H011b C1b C2b N2b 46(3) 3_665 3_665 3_665 3_665 ? H011b C1b C2b H021b 168(1) 3_665 3_665 3_665 3_665 ? H011b C1b C2b H022b -76(3) 3_665 3_665 3_665 3_665 ? H012b C1b C2b N2b -72(3) 3_665 3_665 3_665 3_665 ? H012b C1b C2b H021b 50(3) 3_665 3_665 3_665 3_665 ? H012b C1b C2b H022b 165(3) 3_665 3_665 3_665 3_665 ? N2b C3b C4b N3b 13(4) 3_665 3_665 3_665 3_665 ? N2b C3b C4b C5b -172(3) 3_665 3_665 3_665 3_665 ? C8b C3b C4b N3b -168(2) 3_665 3_665 3_665 3_665 ? C8b C3b C4b C5b 7(4) 3_665 3_665 3_665 3_665 ? N2b C3b C8b C7b 172(3) 3_665 3_665 3_665 3_665 ? N2b C3b C8b H08b -8(4) 3_665 3_665 3_665 3_665 ? C4b C3b C8b C7b -7(4) 3_665 3_665 3_665 3_665 ? C4b C3b C8b H08b 173(2) 3_665 3_665 3_665 3_665 ? N3b C4b C5b C6b 172(2) 3_665 3_665 3_665 3_665 ? N3b C4b C5b H05b -10(4) 3_665 3_665 3_665 3_665 ? C3b C4b C5b C6b -3(4) 3_665 3_665 3_665 3_665 ? C3b C4b C5b H05b 175(2) 3_665 3_665 3_665 3_665 ? C4b C5b C6b N4b -179(3) 3_665 3_665 3_665 3_665 ? C4b C5b C6b C7b -1(4) 3_665 3_665 3_665 3_665 ? H05b C5b C6b N4b 2(4) 3_665 3_665 3_665 3_665 ? H05b C5b C6b C7b -180(3) 3_665 3_665 3_665 3_665 ? N4b C6b C7b C8b 180(3) 3_665 3_665 3_665 3_665 ? N4b C6b C7b H07b -3(4) 3_665 3_665 3_665 3_665 ? C5b C6b C7b C8b 2(4) 3_665 3_665 3_665 3_665 ? C5b C6b C7b H07b 179(3) 3_665 3_665 3_665 3_665 ? C6b C7b C8b C3b 3(4) 3_665 3_665 3_665 3_665 ? C6b C7b C8b H08b -177(3) 3_665 3_665 3_665 3_665 ? H07b C7b C8b C3b -174(3) 3_665 3_665 3_665 3_665 ? H07b C7b C8b H08b 6(5) 3_665 3_665 3_665 3_665 ? N2b C9b C10b C11b 43(3) 3_665 3_665 3_665 3_665 ? N2b C9b C10b C15b -135(2) 3_665 3_665 3_665 . ? H091b C9b C10b C11b -81(3) 3_665 3_665 3_665 3_665 ? H091b C9b C10b C15b 101(2) 3_665 3_665 3_665 . ? H092b C9b C10b C11b 166(2) 3_665 3_665 3_665 3_665 ? H092b C9b C10b C15b -12(3) 3_665 3_665 3_665 . ? C9b C10b C11b C12b -178(2) 3_665 3_665 3_665 . ? C9b C10b C11b H11b 142(3) 3_665 3_665 3_665 3_665 ? C15b C10b C11b C12b 1(3) . 3_665 3_665 . ? C15b C10b C11b H11b -39(4) . 3_665 3_665 3_665 ? C9b C10b C15b O5b -1(3) 3_665 3_665 . . ? C9b C10b C15b C14b 177(2) 3_665 3_665 . 3_665 ? C11b C10b C15b O5b -180(2) 3_665 3_665 . . ? C11b C10b C15b C14b -2(3) 3_665 3_665 . 3_665 ? C10b C11b C12b C13b 0(3) 3_665 3_665 . . ? C10b C11b C12b H11b -152(3) 3_665 3_665 . 3_665 ? C10b C11b C12b H12b -143(2) 3_665 3_665 . . ? H11b C11b C12b C13b 151(3) 3_665 3_665 . . ? H11b C11b C12b H11b -.0001(2) 3_665 3_665 . 3_665 ? H11b C11b C12b H12b 8.4(7) 3_665 3_665 . . ? C10b C11b H11b C12b 58(3) 3_665 3_665 3_665 . ? C10b C11b H11b H12b 3(5) 3_665 3_665 3_665 . ? C12b C11b H11b C12b 0(2) . 3_665 3_665 . ? C12b C11b H11b H12b -55(3) . 3_665 3_665 . ? C11b C12b C13b C14b 0(3) 3_665 . . 3_665 ? C11b C12b C13b H13b -124(2) 3_665 . . . ? C11b C12b C13b H14b -46(6) 3_665 . . 3_665 ? H11b C12b C13b C14b 42(6) 3_665 . . 3_665 ? H11b C12b C13b H13b -83(5) 3_665 . . . ? H11b C12b C13b H14b -5(9) 3_665 . . 3_665 ? H12b C12b C13b C14b 96(4) . . . 3_665 ? H12b C12b C13b H13b -29(5) . . . . ? H12b C12b C13b H14b 49(7) . . . 3_665 ? C11b C12b H11b C11b 0(2) 3_665 . 3_665 3_665 ? C11b C12b H11b H12b 163(1) 3_665 . 3_665 . ? C13b C12b H11b C11b -60(5) . . 3_665 3_665 ? C13b C12b H11b H12b 103(5) . . 3_665 . ? H12b C12b H11b C11b -163(1) . . 3_665 3_665 ? H12b C12b H11b H12b -.00006 . . 3_665 . ? C11b C12b H12b H11b -12(1) 3_665 . . 3_665 ? C13b C12b H12b H11b -124(3) . . . 3_665 ? H11b C12b H12b H11b -.00006 3_665 . . 3_665 ? C12b C13b C14b C15b -1(3) . . 3_665 . ? C12b C13b C14b H14b -155(2) . . 3_665 3_665 ? H13b C13b C14b C15b 137(2) . . 3_665 . ? H13b C13b C14b H14b -16.8(9) . . 3_665 3_665 ? H14b C13b C14b C15b 154(3) 3_665 . 3_665 . ? H14b C13b C14b H14b -.0001(1) 3_665 . 3_665 3_665 ? C12b C13b H14b C14b 63(5) . . 3_665 3_665 ? C14b C13b H14b C14b 0(1) 3_665 . 3_665 3_665 ? H13b C13b H14b C14b 159(1) . . 3_665 3_665 ? C13b C14b C15b O5b 180(2) . 3_665 . . ? C13b C14b C15b C10b 2(3) . 3_665 . 3_665 ? H14b C14b C15b O5b -98(6) 3_665 3_665 . . ? H14b C14b C15b C10b 84(6) 3_665 3_665 . 3_665 ? C13b C14b H14b C13b 0(1) . 3_665 3_665 . ? C15b C14b H14b C13b -95(6) . 3_665 3_665 . ? O5b C16b C17b N5b 81(2) . 3_665 3_665 . ? O5b C16b C17b H171b -158(2) . 3_665 3_665 3_665 ? O5b C16b C17b H172b -45(3) . 3_665 3_665 3_665 ? H161b C16b C17b N5b -71(4) 3_665 3_665 3_665 . ? H161b C16b C17b H171b 51(4) 3_665 3_665 3_665 3_665 ? H161b C16b C17b H172b 164(3) 3_665 3_665 3_665 3_665 ? H162b C16b C17b N5b 147(2) 3_665 3_665 3_665 . ? H162b C16b C17b H171b -91(3) 3_665 3_665 3_665 3_665 ? H162b C16b C17b H172b 22(4) 3_665 3_665 3_665 3_665 ? C11b H11b H12b C12b 59(3) 3_665 3_665 . . ? C12b H11b H12b C12b 0(2) . 3_665 . . ? C16c O5c C15c C10c -159(1) . 3_565 3_565 . ? C16c O5c C15c C14c 18(2) . 3_565 3_565 . ? H161c O5c C15c C10c 155(2) . 3_565 3_565 . ? H161c O5c C15c C14c -27(2) . 3_565 3_565 . ? C15c O5c C16c C17c 168(1) 3_565 3_565 . . ? C15c O5c C16c H161c -80(2) 3_565 3_565 . . ? C15c O5c C16c H162c 4(2) 3_565 3_565 . . ? H161c O5c C16c C17c -112(2) . 3_565 . . ? H161c O5c C16c H161c -.0001(1) . 3_565 . . ? H161c O5c C16c H162c 84(2) . 3_565 . . ? C15c O5c H161c C16c 119(2) 3_565 3_565 . . ? C16c O5c H161c C16c 0(3) . 3_565 . . ? C1c N1c C1c C2c 155(2) 2_665 . . . ? C1c N1c C1c H011c -73(2) 2_665 . . . ? C1c N1c C1c H012c 35(3) 2_665 . . . ? C1c N1c C1c C2c -90(3) 3_565 . . . ? C1c N1c C1c H011c 42(3) 3_565 . . . ? C1c N1c C1c H012c 150(2) 3_565 . . . ? C3c N2c C2c C1c -76(4) . . . . ? C3c N2c C2c H021c 167(3) . . . . ? C3c N2c C2c H022c 50(3) . . . . ? C9c N2c C2c C1c 100(3) . . . . ? C9c N2c C2c H021c -17(4) . . . . ? C9c N2c C2c H022c -133(2) . . . . ? C2c N2c C3c C4c -17(4) . . . . ? C2c N2c C3c C8c 159(3) . . . . ? C9c N2c C3c C4c 166(3) . . . . ? C9c N2c C3c C8c -17(4) . . . . ? C2c N2c C9c C10c 108(2) . . . . ? C2c N2c C9c H091c -128(3) . . . . ? C2c N2c C9c H092c -14(4) . . . . ? C3c N2c C9c C10c -75(3) . . . . ? C3c N2c C9c H091c 49(4) . . . . ? C3c N2c C9c H092c 163(2) . . . . ? O1c N3c C4c C3c -47(4) . . . . ? O1c N3c C4c C5c 125(2) . . . . ? O2c N3c C4c C3c 138(3) 3_665 . . . ? O2c N3c C4c C5c -50(4) 3_665 . . . ? O3c N4c C6c C5c 6(4) 2_665 2_665 . . ? O3c N4c C6c C7c -180(3) 2_665 2_665 . . ? O4c N4c C6c C5c -177(3) . 2_665 . . ? O4c N4c C6c C7c -3(4) . 2_665 . . ? C17c N5c C17c C16c -49(3) 2_665 . . . ? C17c N5c C17c H171c -168(3) 2_665 . . . ? C17c N5c C17c H172c 75(4) 2_665 . . . ? C17c N5c C17c C16c -175(2) 3_565 . . . ? C17c N5c C17c H171c 65(3) 3_565 . . . ? C17c N5c C17c H172c -52(4) 3_565 . . . ? N1c C1c C2c N2c -60(3) . . . . ? N1c C1c C2c H021c 62(3) . . . . ? N1c C1c C2c H022c 172(2) . . . . ? H011c C1c C2c N2c 169(2) . . . . ? H011c C1c C2c H021c -69(3) . . . . ? H011c C1c C2c H022c 41(3) . . . . ? H012c C1c C2c N2c 61(3) . . . . ? H012c C1c C2c H021c -178(2) . . . . ? H012c C1c C2c H022c -68(3) . . . . ? N2c C3c C4c N3c -22(5) . . . . ? N2c C3c C4c C5c 167(3) . . . . ? C8c C3c C4c N3c 161(3) . . . . ? C8c C3c C4c C5c -10(4) . . . . ? N2c C3c C8c C7c -169(3) . . . . ? N2c C3c C8c H08c 10(4) . . . . ? C4c C3c C8c C7c 8(4) . . . . ? C4c C3c C8c H08c -173(3) . . . . ? N3c C4c C5c C6c -168(3) . . . . ? N3c C4c C5c H05c 11(4) . . . . ? C3c C4c C5c C6c 4(5) . . . . ? C3c C4c C5c H05c -177(3) . . . . ? C4c C5c C6c N4c 178(3) . . . 2_665 ? C4c C5c C6c C7c 5(5) . . . . ? H05c C5c C6c N4c 0(5) . . . 2_665 ? H05c C5c C6c C7c -174(3) . . . . ? N4c C6c C7c C8c 180(3) 2_665 . . . ? N4c C6c C7c H07c 0(5) 2_665 . . . ? C5c C6c C7c C8c -6(5) . . . . ? C5c C6c C7c H07c 175(3) . . . . ? C6c C7c C8c C3c 0(5) . . . . ? C6c C7c C8c H08c -179(3) . . . . ? H07c C7c C8c C3c 179(3) . . . . ? H07c C7c C8c H08c 0(5) . . . . ? N2c C9c C10c C11c -17(2) . . . . ? N2c C9c C10c C15c 165(2) . . . 3_565 ? H091c C9c C10c C11c -138(2) . . . . ? H091c C9c C10c C15c 44(3) . . . 3_565 ? H092c C9c C10c C11c 103(3) . . . . ? H092c C9c C10c C15c -75(3) . . . 3_565 ? C9c C10c C11c C12c -180(2) . . . . ? C9c C10c C11c H11c 0(2) . . . . ? C15c C10c C11c C12c -2(2) 3_565 . . . ? C15c C10c C11c H11c 177(2) 3_565 . . . ? C9c C10c C15c O5c -6(2) . . 3_565 3_565 ? C9c C10c C15c C14c 176(2) . . 3_565 . ? C11c C10c C15c O5c 176(1) . . 3_565 3_565 ? C11c C10c C15c C14c -1(3) . . 3_565 . ? C10c C11c C12c C13c 6(3) . . . . ? C10c C11c C12c H12c -175(2) . . . . ? H11c C11c C12c C13c -173(2) . . . . ? H11c C11c C12c H12c 6(3) . . . . ? C11c C12c C13c C14c -7(3) . . . . ? C11c C12c C13c H13c 175(2) . . . . ? H12c C12c C13c C14c 174(2) . . . . ? H12c C12c C13c H13c -4(3) . . . . ? C12c C13c C14c C15c 3(3) . . . 3_565 ? C12c C13c C14c H14c 142(2) . . . . ? H13c C13c C14c C15c -179(2) . . . 3_565 ? H13c C13c C14c H14c -40(4) . . . . ? C13c C14c C15c O5c -176(2) . . 3_565 3_565 ? C13c C14c C15c C10c 0(3) . . 3_565 . ? H14c C14c C15c O5c 41(3) . . 3_565 3_565 ? H14c C14c C15c C10c -142(2) . . 3_565 . ? O5c C16c C17c N5c -55(2) 3_565 . . . ? O5c C16c C17c H171c 63(2) 3_565 . . . ? O5c C16c C17c H172c -179(2) 3_565 . . . ? H161c C16c C17c N5c -109(2) . . . . ? H161c C16c C17c H171c 9(3) . . . . ? H161c C16c C17c H172c 127(2) . . . . ? H162c C16c C17c N5c 109(2) . . . . ? H162c C16c C17c H171c -133(2) . . . . ? H162c C16c C17c H172c -15(3) . . . . ? O5c C16c H161c O5c -.0(9) 3_565 . . 3_565 ? C17c C16c H161c O5c 91(2) . . . 3_565 ? H162c C16c H161c O5c -122(2) . . . 3_565 ? C16a O5a C15a C10a 178(2) 3_666 3_666 3_666 3_666 ? C16a O5a C15a C14a -4(3) 3_666 3_666 3_666 3_666 ? C15a O5a C16a C17a 178(2) 3_666 3_666 3_666 3_666 ? C15a O5a C16a H161a -57(3) 3_666 3_666 3_666 3_666 ? C15a O5a C16a H162a 59(4) 3_666 3_666 3_666 3_666 ? C1a N1a C1a C2a 142(2) 1_666 1_666 3_666 3_666 ? C1a N1a C1a H011a -95(3) 1_666 1_666 3_666 3_666 ? C1a N1a C1a H012a 21(3) 1_666 1_666 3_666 3_666 ? C1a N1a C1a C2a -83(3) 2_666 1_666 3_666 3_666 ? C1a N1a C1a H011a 40(3) 2_666 1_666 3_666 3_666 ? C1a N1a C1a H012a 156(2) 2_666 1_666 3_666 3_666 ? C3a N2a C2a C1a -94(3) 3_666 3_666 3_666 3_666 ? C3a N2a C2a H021a 144(2) 3_666 3_666 3_666 3_666 ? C3a N2a C2a H022a 25(3) 3_666 3_666 3_666 3_666 ? C9a N2a C2a C1a 101(3) 3_666 3_666 3_666 3_666 ? C9a N2a C2a H021a -20(3) 3_666 3_666 3_666 3_666 ? C9a N2a C2a H022a -139(2) 3_666 3_666 3_666 3_666 ? C2a N2a C3a C4a -153(3) 3_666 3_666 3_666 3_666 ? C2a N2a C3a C8a 26(3) 3_666 3_666 3_666 3_666 ? C9a N2a C3a C4a 11(4) 3_666 3_666 3_666 3_666 ? C9a N2a C3a C8a -170(2) 3_666 3_666 3_666 3_666 ? C2a N2a C9a C10a -51(3) 3_666 3_666 3_666 3_666 ? C2a N2a C9a H091a 71(2) 3_666 3_666 3_666 3_666 ? C2a N2a C9a H092a -172(2) 3_666 3_666 3_666 3_666 ? C3a N2a C9a C10a 144(2) 3_666 3_666 3_666 3_666 ? C3a N2a C9a H091a -94(2) 3_666 3_666 3_666 3_666 ? C3a N2a C9a H092a 23(3) 3_666 3_666 3_666 3_666 ? O1a N3a C4a C3a -131(3) 3_666 3_666 3_666 3_666 ? O1a N3a C4a C5a 61(4) 3_666 3_666 3_666 3_666 ? O2a N3a C4a C3a 53(4) 3_666 3_666 3_666 3_666 ? O2a N3a C4a C5a -115(3) 3_666 3_666 3_666 3_666 ? O3a N4a C6a C5a -10(5) 3_666 3_666 3_666 3_666 ? O3a N4a C6a C7a 175(3) 3_666 3_666 3_666 3_666 ? O4a N4a C6a C5a 165(3) 3_666 3_666 3_666 3_666 ? O4a N4a C6a C7a -10(4) 3_666 3_666 3_666 3_666 ? C17a N5a C17a C16a -86(2) 1_666 1_666 3_666 3_666 ? C17a N5a C17a H171a 157(2) 1_666 1_666 3_666 3_666 ? C17a N5a C17a H172a 35(3) 1_666 1_666 3_666 3_666 ? C17a N5a C17a C16a 157(2) 2_666 1_666 3_666 3_666 ? C17a N5a C17a H171a 40(3) 2_666 1_666 3_666 3_666 ? C17a N5a C17a H172a -82(3) 2_666 1_666 3_666 3_666 ? N1a C1a C2a N2a -174(2) 1_666 3_666 3_666 3_666 ? N1a C1a C2a H021a -53(3) 1_666 3_666 3_666 3_666 ? N1a C1a C2a H022a 65(2) 1_666 3_666 3_666 3_666 ? H011a C1a C2a N2a 63(3) 3_666 3_666 3_666 3_666 ? H011a C1a C2a H021a -176(3) 3_666 3_666 3_666 3_666 ? H011a C1a C2a H022a -58(3) 3_666 3_666 3_666 3_666 ? H012a C1a C2a N2a -52(3) 3_666 3_666 3_666 3_666 ? H012a C1a C2a H021a 69(3) 3_666 3_666 3_666 3_666 ? H012a C1a C2a H022a -173(2) 3_666 3_666 3_666 3_666 ? N2a C3a C4a N3a 12(5) 3_666 3_666 3_666 3_666 ? N2a C3a C4a C5a 179(3) 3_666 3_666 3_666 3_666 ? C8a C3a C4a N3a -167(3) 3_666 3_666 3_666 3_666 ? C8a C3a C4a C5a 0(4) 3_666 3_666 3_666 3_666 ? N2a C3a C8a C7a -177(3) 3_666 3_666 3_666 3_666 ? N2a C3a C8a H08a 6(4) 3_666 3_666 3_666 3_666 ? C4a C3a C8a C7a 2(4) 3_666 3_666 3_666 3_666 ? C4a C3a C8a H08a -175(3) 3_666 3_666 3_666 3_666 ? N3a C4a C5a C6a 167(3) 3_666 3_666 3_666 3_666 ? N3a C4a C5a H05a -15(4) 3_666 3_666 3_666 3_666 ? C3a C4a C5a C6a -1(4) 3_666 3_666 3_666 3_666 ? C3a C4a C5a H05a 177(3) 3_666 3_666 3_666 3_666 ? C4a C5a C6a N4a -173(3) 3_666 3_666 3_666 3_666 ? C4a C5a C6a C7a 2(5) 3_666 3_666 3_666 3_666 ? H05a C5a C6a N4a 9(5) 3_666 3_666 3_666 3_666 ? H05a C5a C6a C7a -176(3) 3_666 3_666 3_666 3_666 ? N4a C6a C7a C8a 174(3) 3_666 3_666 3_666 3_666 ? N4a C6a C7a H07a -7(5) 3_666 3_666 3_666 3_666 ? C5a C6a C7a C8a 0(5) 3_666 3_666 3_666 3_666 ? C5a C6a C7a H07a 178(3) 3_666 3_666 3_666 3_666 ? C6a C7a C8a C3a -1(4) 3_666 3_666 3_666 3_666 ? C6a C7a C8a H08a 175(3) 3_666 3_666 3_666 3_666 ? H07a C7a C8a C3a -180(3) 3_666 3_666 3_666 3_666 ? H07a C7a C8a H08a -4(5) 3_666 3_666 3_666 3_666 ? N2a C9a C10a C11a -83(3) 3_666 3_666 3_666 3_666 ? N2a C9a C10a C15a 98(2) 3_666 3_666 3_666 3_666 ? H091a C9a C10a C11a 157(2) 3_666 3_666 3_666 3_666 ? H091a C9a C10a C15a -23(3) 3_666 3_666 3_666 3_666 ? H092a C9a C10a C11a 37(3) 3_666 3_666 3_666 3_666 ? H092a C9a C10a C15a -142(2) 3_666 3_666 3_666 3_666 ? C9a C10a C11a C12a -175(2) 3_666 3_666 3_666 3_666 ? C9a C10a C11a H11a 4(4) 3_666 3_666 3_666 3_666 ? C15a C10a C11a C12a 4(4) 3_666 3_666 3_666 3_666 ? C15a C10a C11a H11a -176(2) 3_666 3_666 3_666 3_666 ? C9a C10a C15a O5a -5(3) 3_666 3_666 3_666 3_666 ? C9a C10a C15a C14a 176(2) 3_666 3_666 3_666 3_666 ? C11a C10a C15a O5a 175(2) 3_666 3_666 3_666 3_666 ? C11a C10a C15a C14a -3(3) 3_666 3_666 3_666 3_666 ? C10a C11a C12a C13a -5(4) 3_666 3_666 3_666 1_666 ? C10a C11a C12a H12a 126(14) 3_666 3_666 3_666 3_666 ? C10a C11a C12a H13a 41(4) 3_666 3_666 3_666 1_666 ? H11a C11a C12a C13a 175(2) 3_666 3_666 3_666 1_666 ? H11a C11a C12a H12a -53(16) 3_666 3_666 3_666 3_666 ? H11a C11a C12a H13a -138(2) 3_666 3_666 3_666 1_666 ? C11a C12a C13a C14a 5(4) 3_666 3_666 1_666 3_666 ? C11a C12a C13a H13a 116(2) 3_666 3_666 1_666 1_666 ? C11a C12a C13a H14a 37(8) 3_666 3_666 1_666 3_666 ? H12a C12a C13a C14a -167(2) 3_666 3_666 1_666 3_666 ? H12a C12a C13a H13a -56(2) 3_666 3_666 1_666 1_666 ? H12a C12a C13a H14a -135(7) 3_666 3_666 1_666 3_666 ? H13a C12a C13a C14a -111(3) 1_666 3_666 1_666 3_666 ? H13a C12a C13a H13a -.0001(2) 1_666 3_666 1_666 1_666 ? H13a C12a C13a H14a -79(7) 1_666 3_666 1_666 3_666 ? C11a C12a H13a C13a -89(3) 3_666 3_666 1_666 1_666 ? C13a C12a H13a C13a 0(2) 1_666 3_666 1_666 1_666 ? H12a C12a H13a C13a 103(1) 3_666 3_666 1_666 1_666 ? C12a C13a C14a C15a -4(4) 3_666 1_666 3_666 3_666 ? C12a C13a C14a H14a 165(3) 3_666 1_666 3_666 3_666 ? H13a C13a C14a C15a -78(3) 1_666 1_666 3_666 3_666 ? H13a C13a C14a H14a 91(2) 1_666 1_666 3_666 3_666 ? H14a C13a C14a C15a -169(3) 3_666 1_666 3_666 3_666 ? H14a C13a C14a H14a -.0001(1) 3_666 1_666 3_666 3_666 ? C12a C13a H13a C12a 0(2) 3_666 1_666 1_666 3_666 ? C14a C13a H13a C12a 111(2) 3_666 1_666 1_666 3_666 ? H14a C13a H13a C12a 159(2) 3_666 1_666 1_666 3_666 ? C12a C13a H14a C14a -42(7) 3_666 1_666 3_666 3_666 ? C14a C13a H14a C14a 0(2) 3_666 1_666 3_666 3_666 ? H13a C13a H14a C14a -112(2) 1_666 1_666 3_666 3_666 ? C13a C14a C15a O5a -175(2) 1_666 3_666 3_666 3_666 ? C13a C14a C15a C10a 3(3) 1_666 3_666 3_666 3_666 ? H14a C14a C15a O5a 118(13) 3_666 3_666 3_666 3_666 ? H14a C14a C15a C10a -64(14) 3_666 3_666 3_666 3_666 ? C13a C14a H14a C13a 0(1) 1_666 3_666 3_666 1_666 ? C15a C14a H14a C13a 73(14) 3_666 3_666 3_666 1_666 ? O5a C16a C17a N5a -89(2) 3_666 3_666 3_666 1_666 ? O5a C16a C17a H171a 30(3) 3_666 3_666 3_666 3_666 ? O5a C16a C17a H172a 149(2) 3_666 3_666 3_666 3_666 ? H161a C16a C17a N5a 149(2) 3_666 3_666 3_666 1_666 ? H161a C16a C17a H171a -92(3) 3_666 3_666 3_666 3_666 ? H161a C16a C17a H172a 27(2) 3_666 3_666 3_666 3_666 ? H162a C16a C17a N5a 30(3) 3_666 3_666 3_666 1_666 ? H162a C16a C17a H171a 149(2) 3_666 3_666 3_666 3_666 ? H162a C16a C17a H172a -92(3) 3_666 3_666 3_666 3_666 ? H1PY C1PY C2PY C1PY -178(15) 3_666 3_666 1_566 2_556 ? C2PY C1PY C2PY C1PY 2(5) 2_556 3_666 1_566 2_556 ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min -17 _reflns_limit_l_max 17 _reflns_number_total 3332 _reflns_number_observed 1991 _reflns_observed_criterion 'refl_observed_if_Fobs >2.000_sigma(Fobs)' _reflns_d_resolution_high .93 _reflns_d_resolution_low 15.949 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 3.5493 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_observed_status _refln_scale_group_code ? ? ? ? ? ? ? ? #===END #CIF File for L3 data_L3 _database_code_CSD 172622 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point '230 Celcius' _chemical_formula_moiety 'C53 H57 N9 O9' _chemical_formula_sum 'C53 H57 N9 O9' _chemical_formula_weight 964.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.473(4) _cell_length_b 21.974(5) _cell_length_c 36.982(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10136(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.9 _cell_measurement_theta_max 15.3 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 1.25 _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_method Floatation _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 0.09/mm _exptl_absorpt_correction_type 'not done' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK-alpha _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'theta-2theta scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every hour' _diffrn_standards_decay_% 'less than 0.5%' _diffrn_reflns_number 7346 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.2206 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 22.47 _reflns_number_total 6604 _reflns_number_gt 2231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0706P)^2^+4.6194P] 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 SHELXL _refine_ls_extinction_coef 0.00051(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6510 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2868 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2110 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.0006 _refine_ls_shift/su_mean 0.0004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9741(6) 0.1204(3) 0.03036(18) 0.065(2) Uani 1 1 d . . . H1A H 0.9806 0.1030 0.0064 0.078 Uiso 1 1 calc R . . H1B H 1.0433 0.1373 0.0369 0.078 Uiso 1 1 calc R . . C2 C 0.8919(6) 0.1720(4) 0.02914(19) 0.072(2) Uani 1 1 d . . . H2A H 0.9019 0.1950 0.0070 0.087 Uiso 1 1 calc R . . H2B H 0.8204 0.1546 0.0286 0.087 Uiso 1 1 calc R . . C3 C 0.9739(6) 0.2588(3) 0.0608(2) 0.0566(19) Uani 1 1 d . . . C4 C 1.0505(7) 0.2650(4) 0.0334(2) 0.072(2) Uani 1 1 d . . . H4 H 1.0514 0.2377 0.0142 0.086 Uiso 1 1 calc R . . C5 C 1.1237(8) 0.3109(5) 0.0349(2) 0.091(3) Uani 1 1 d . . . H5 H 1.1737 0.3149 0.0164 0.109 Uiso 1 1 calc R . . C6 C 1.1247(7) 0.3512(4) 0.0632(2) 0.083(3) Uani 1 1 d . . . C7 C 1.0496(7) 0.3467(4) 0.0901(2) 0.094(3) Uani 1 1 d . . . H7 H 1.0497 0.3743 0.1092 0.113 Uiso 1 1 calc R . . C8 C 0.9748(7) 0.3015(4) 0.0888(2) 0.078(2) Uani 1 1 d . . . H8 H 0.9233 0.2991 0.1069 0.094 Uiso 1 1 calc R . . C9 C 0.8172(5) 0.2074(3) 0.08743(19) 0.059(2) Uani 1 1 d . . . H9A H 0.8489 0.2127 0.1112 0.071 Uiso 1 1 calc R . . H9B H 0.7878 0.1666 0.0862 0.071 Uiso 1 1 calc R . . C10 C 0.7274(6) 0.2526(3) 0.0829(2) 0.0532(18) Uani 1 1 d . . . C42 C 1.0217(6) 0.0466(4) 0.1871(2) 0.076(2) Uani 1 1 d . . . H42 H 1.0111 0.0869 0.1940 0.091 Uiso 1 1 calc R . . C11 C 0.7144(6) 0.2894(4) 0.0526(2) 0.071(2) Uani 1 1 d . . . H11 H 0.7632 0.2861 0.0337 0.085 Uiso 1 1 calc R . . C12 C 0.6315(8) 0.3305(4) 0.0498(3) 0.086(3) Uani 1 1 d . . . H12 H 0.6263 0.3554 0.0295 0.103 Uiso 1 1 calc R . . C13 C 0.5573(8) 0.3346(4) 0.0766(3) 0.097(3) Uani 1 1 d . . . H13 H 0.5000 0.3614 0.0744 0.117 Uiso 1 1 calc R . . C14 C 0.5671(7) 0.2994(4) 0.1066(3) 0.093(3) Uani 1 1 d . . . H14 H 0.5169 0.3031 0.1250 0.112 Uiso 1 1 calc R . . C15 C 0.6496(7) 0.2586(4) 0.1102(2) 0.066(2) Uani 1 1 d . . . C16 C 0.6133(7) 0.2365(4) 0.1727(2) 0.094(3) Uani 1 1 d . . . H16A H 0.5363 0.2325 0.1698 0.112 Uiso 1 1 calc R . . H16B H 0.6290 0.2783 0.1791 0.112 Uiso 1 1 calc R . . C17 C 0.6510(9) 0.1953(4) 0.2018(2) 0.099(3) Uani 1 1 d . . . H17A H 0.6186 0.2083 0.2243 0.119 Uiso 1 1 calc R . . H17B H 0.6247 0.1546 0.1966 0.119 Uiso 1 1 calc R . . C34 C 0.7909(9) 0.1509(4) 0.2359(2) 0.110(3) Uani 1 1 d . . . H34A H 0.7670 0.1688 0.2585 0.132 Uiso 1 1 calc R . . H34B H 0.8684 0.1475 0.2371 0.132 Uiso 1 1 calc R . . C33 C 0.7449(9) 0.0885(4) 0.2331(2) 0.105(3) Uani 1 1 d . . . H33A H 0.7771 0.0620 0.2511 0.125 Uiso 1 1 calc R . . H33B H 0.6682 0.0896 0.2372 0.125 Uiso 1 1 calc R . . C32 C 0.7312(6) 0.0103(4) 0.1886(2) 0.065(2) Uani 1 1 d . . . C31 C 0.7022(7) -0.0329(4) 0.2136(2) 0.084(3) Uani 1 1 d . . . H31 H 0.7054 -0.0246 0.2383 0.101 Uiso 1 1 calc R . . C30 C 0.6687(8) -0.0883(5) 0.2013(3) 0.104(3) Uani 1 1 d . . . H30 H 0.6502 -0.1182 0.2180 0.125 Uiso 1 1 calc R . . C29 C 0.6617(8) -0.1011(4) 0.1657(3) 0.111(3) Uani 1 1 d . . . H29 H 0.6369 -0.1388 0.1578 0.133 Uiso 1 1 calc R . . C28 C 0.6918(7) -0.0575(4) 0.1414(2) 0.090(3) Uani 1 1 d . . . H28 H 0.6887 -0.0664 0.1168 0.108 Uiso 1 1 calc R . . C27 C 0.7265(6) -0.0010(4) 0.1521(2) 0.062(2) Uani 1 1 d . . . C26 C 0.7636(6) 0.0471(3) 0.12617(17) 0.066(2) Uani 1 1 d . . . H26A H 0.7362 0.0862 0.1342 0.079 Uiso 1 1 calc R . . H26B H 0.8412 0.0491 0.1270 0.079 Uiso 1 1 calc R . . C20 C 0.6352(7) 0.0598(4) 0.0753(2) 0.064(2) Uani 1 1 d . . . C24 C 0.6037(8) 0.0462(4) 0.0402(2) 0.083(3) Uani 1 1 d . . . H24 H 0.6472 0.0216 0.0259 0.099 Uiso 1 1 calc R . . C23 C 0.5097(9) 0.0682(5) 0.0262(2) 0.094(3) Uani 1 1 d . . . H23 H 0.4895 0.0593 0.0026 0.113 Uiso 1 1 calc R . . C22 C 0.4454(8) 0.1041(5) 0.0481(3) 0.086(3) Uani 1 1 d . . . C21 C 0.4758(8) 0.1179(4) 0.0819(3) 0.094(3) Uani 1 1 d . . . H21 H 0.4338 0.1441 0.0956 0.112 Uiso 1 1 calc R . . C25 C 0.5658(8) 0.0946(4) 0.0962(2) 0.080(3) Uani 1 1 d . . . H25 H 0.5819 0.1017 0.1204 0.097 Uiso 1 1 calc R . . C19 C 0.7992(6) -0.0011(3) 0.0675(2) 0.068(2) Uani 1 1 d . . . H19A H 0.7552 -0.0310 0.0551 0.081 Uiso 1 1 calc R . . H19B H 0.8474 -0.0229 0.0835 0.081 Uiso 1 1 calc R . . C18 C 0.8653(6) 0.0326(3) 0.03958(18) 0.065(2) Uani 1 1 d . . . H18A H 0.8999 0.0034 0.0238 0.078 Uiso 1 1 calc R . . H18B H 0.8181 0.0575 0.0249 0.078 Uiso 1 1 calc R . . C35 C 1.0411(6) 0.0359(3) 0.0653(2) 0.066(2) Uani 1 1 d . . . H35A H 1.0794 0.0266 0.0432 0.079 Uiso 1 1 calc R . . H35B H 1.0173 -0.0023 0.0756 0.079 Uiso 1 1 calc R . . C36 C 1.1186(6) 0.0649(4) 0.0913(2) 0.075(2) Uani 1 1 d . . . H36A H 1.1796 0.0381 0.0943 0.091 Uiso 1 1 calc R . . H36B H 1.1446 0.1026 0.0808 0.091 Uiso 1 1 calc R . . C37 C 1.0618(6) 0.0329(4) 0.1525(2) 0.064(2) Uani 1 1 d . . . C38 C 1.0898(6) -0.0274(5) 0.1446(2) 0.077(2) Uani 1 1 d . . . H38 H 1.1231 -0.0367 0.1228 0.093 Uiso 1 1 calc R . . C39 C 1.0679(7) -0.0729(4) 0.1692(3) 0.089(3) Uani 1 1 d . . . H39 H 1.0859 -0.1130 0.1640 0.107 Uiso 1 1 calc R . . C40 C 1.0187(7) -0.0584(5) 0.2017(3) 0.080(3) Uani 1 1 d . . . C41 C 0.9983(7) 0.0005(5) 0.2106(2) 0.088(3) Uani 1 1 d . . . H41 H 0.9680 0.0095 0.2329 0.106 Uiso 1 1 calc R . . C43 C 1.0324(5) 0.1395(3) 0.1335(2) 0.067(2) Uani 1 1 d . . . H43A H 0.9686 0.1366 0.1484 0.081 Uiso 1 1 calc R . . H43B H 1.0116 0.1573 0.1106 0.081 Uiso 1 1 calc R . . C44 C 1.1115(7) 0.1809(4) 0.1518(2) 0.069(2) Uani 1 1 d . . . C45 C 1.2202(9) 0.1763(6) 0.1467(3) 0.133(4) Uani 1 1 d . . . H45 H 1.2472 0.1441 0.1332 0.160 Uiso 1 1 calc R . . C46 C 1.2912(10) 0.2188(8) 0.1613(4) 0.163(6) Uani 1 1 d . . . H46 H 1.3642 0.2155 0.1567 0.196 Uiso 1 1 calc R . . C47 C 1.2547(13) 0.2637(7) 0.1816(3) 0.147(6) Uani 1 1 d . . . H47 H 1.3026 0.2916 0.1915 0.177 Uiso 1 1 calc R . . C48 C 1.1478(10) 0.2697(5) 0.1883(2) 0.106(3) Uani 1 1 d . . . H48 H 1.1224 0.3012 0.2027 0.127 Uiso 1 1 calc R . . C49 C 1.0775(8) 0.2280(4) 0.1732(2) 0.072(2) Uani 1 1 d . . . C50 C 0.9331(8) 0.2522(4) 0.2119(2) 0.094(3) Uani 1 1 d . . . H50A H 0.9592 0.2931 0.2161 0.112 Uiso 1 1 calc R . . H50B H 0.9605 0.2260 0.2309 0.112 Uiso 1 1 calc R . . C51 C 0.8125(8) 0.2515(4) 0.2121(2) 0.092(3) Uani 1 1 d . . . H51A H 0.7878 0.2681 0.2349 0.110 Uiso 1 1 calc R . . H51B H 0.7872 0.2783 0.1930 0.110 Uiso 1 1 calc R . . N1 N 0.9471(5) 0.0715(3) 0.05603(14) 0.0577(15) Uani 1 1 d . . . N2 N 0.9004(5) 0.2135(3) 0.06028(15) 0.0588(16) Uani 1 1 d . . . N3 N 1.2021(8) 0.3987(5) 0.0644(3) 0.130(3) Uani 1 1 d . . . N4 N 0.7637(6) 0.1917(3) 0.20700(16) 0.0734(18) Uani 1 1 d . . . N5 N 0.7306(5) 0.0374(3) 0.08898(15) 0.0627(16) Uani 1 1 d . . . N6 N 0.3449(8) 0.1260(5) 0.0331(4) 0.124(3) Uani 1 1 d . . . N7 N 1.0738(4) 0.0783(3) 0.12702(17) 0.0641(16) Uani 1 1 d . . . N8 N 0.9886(8) -0.1070(5) 0.2256(3) 0.100(3) Uani 1 1 d . . . O1 O 1.2735(6) 0.4017(3) 0.0407(2) 0.148(3) Uani 1 1 d . . . O2 O 1.1985(7) 0.4367(5) 0.0884(3) 0.200(5) Uani 1 1 d . . . O3 O 0.6655(4) 0.2214(2) 0.13931(14) 0.0736(15) Uani 1 1 d . . . O4 O 0.7669(4) 0.0663(2) 0.19788(13) 0.0764(15) Uani 1 1 d . . . O5 O 0.2963(7) 0.1647(5) 0.0489(3) 0.169(4) Uani 1 1 d . . . O6 O 0.3126(7) 0.1037(5) 0.0050(3) 0.181(4) Uani 1 1 d . . . O7 O 1.0162(7) -0.1599(4) 0.21804(19) 0.130(3) Uani 1 1 d . . . O8 O 0.9381(6) -0.0948(3) 0.2533(2) 0.132(3) Uani 1 1 d . . . O9 O 0.9678(5) 0.2311(3) 0.17787(15) 0.0930(18) Uani 1 1 d . . . C1S C 0.4240(11) 0.0378(9) 0.1815(4) 0.132(6) Uani 1 1 d . . . C2S C 0.3905(12) -0.0156(8) 0.1659(4) 0.200(7) Uani 1 1 d . . . H2S1 H 0.3476 -0.0067 0.1450 0.299 Uiso 1 1 calc R . . H2S2 H 0.3487 -0.0384 0.1830 0.299 Uiso 1 1 calc R . . H2S3 H 0.4518 -0.0391 0.1588 0.299 Uiso 1 1 calc R . . N1S N 0.4509(11) 0.0790(7) 0.1965(4) 0.178(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.080(6) 0.069(5) 0.046(4) -0.006(4) 0.013(4) -0.001(5) C2 0.091(6) 0.075(6) 0.051(5) 0.002(4) 0.000(4) 0.004(5) C3 0.061(5) 0.058(5) 0.050(5) 0.003(4) -0.001(4) -0.002(5) C4 0.086(6) 0.076(6) 0.053(5) -0.005(4) 0.020(5) -0.017(5) C5 0.093(7) 0.105(8) 0.076(7) -0.014(6) 0.026(5) -0.014(6) C6 0.068(6) 0.113(8) 0.069(6) -0.007(6) 0.016(5) -0.039(6) C7 0.092(7) 0.110(8) 0.080(6) -0.018(5) 0.010(6) -0.041(6) C8 0.076(6) 0.095(7) 0.063(5) -0.019(5) 0.021(4) -0.018(6) C9 0.045(5) 0.068(5) 0.065(5) 0.012(4) -0.004(4) 0.002(4) C10 0.052(5) 0.054(5) 0.054(5) 0.005(4) -0.011(4) -0.004(4) C42 0.077(6) 0.073(6) 0.077(6) -0.007(6) -0.007(5) -0.003(5) C11 0.069(6) 0.072(6) 0.071(6) -0.002(5) -0.021(4) 0.008(5) C12 0.087(7) 0.075(7) 0.095(7) 0.018(5) -0.024(6) 0.019(6) C13 0.079(7) 0.088(8) 0.125(9) 0.011(7) -0.028(7) 0.030(6) C14 0.079(7) 0.089(7) 0.111(8) 0.011(6) 0.001(6) 0.030(6) C15 0.063(6) 0.066(6) 0.067(6) 0.008(5) -0.005(5) 0.001(5) C16 0.078(6) 0.113(8) 0.089(7) 0.012(6) 0.020(6) 0.009(5) C17 0.109(9) 0.112(8) 0.077(6) 0.003(6) 0.041(6) 0.013(7) C34 0.203(11) 0.069(6) 0.056(5) -0.010(5) -0.015(6) 0.007(7) C33 0.196(10) 0.066(6) 0.051(5) 0.002(5) 0.006(6) 0.006(6) C32 0.074(6) 0.052(6) 0.071(6) 0.000(5) 0.001(5) -0.004(4) C31 0.121(7) 0.061(6) 0.071(6) 0.007(5) 0.004(5) -0.008(6) C30 0.143(9) 0.077(8) 0.093(8) 0.028(6) 0.014(6) -0.013(6) C29 0.174(10) 0.091(7) 0.068(6) 0.001(6) -0.007(7) -0.058(7) C28 0.123(8) 0.081(7) 0.067(6) 0.013(6) -0.003(5) -0.036(6) C27 0.064(5) 0.064(6) 0.059(5) 0.014(5) -0.010(4) -0.014(4) C26 0.067(5) 0.076(5) 0.054(5) 0.004(4) -0.005(4) -0.013(4) C20 0.061(6) 0.072(6) 0.060(6) 0.004(5) -0.003(5) -0.012(5) C24 0.091(7) 0.100(7) 0.058(6) -0.008(5) -0.013(5) 0.001(6) C23 0.088(7) 0.123(8) 0.071(6) 0.013(6) -0.020(6) -0.013(6) C22 0.056(7) 0.121(9) 0.082(7) 0.015(6) -0.008(6) 0.001(6) C21 0.081(7) 0.114(8) 0.086(8) -0.013(6) 0.005(6) 0.011(6) C25 0.070(6) 0.114(8) 0.057(5) -0.008(5) 0.009(5) 0.003(6) C19 0.068(5) 0.072(5) 0.063(5) -0.008(5) -0.013(4) -0.010(5) C18 0.084(6) 0.062(5) 0.049(5) -0.012(4) 0.002(4) 0.004(5) C35 0.071(5) 0.057(5) 0.069(5) -0.001(4) 0.004(4) 0.016(5) C36 0.061(5) 0.087(6) 0.078(6) 0.011(5) 0.021(5) 0.012(5) C37 0.050(5) 0.085(7) 0.057(6) 0.000(5) -0.011(4) 0.005(5) C38 0.074(6) 0.074(7) 0.084(6) 0.007(6) 0.001(5) 0.023(5) C39 0.099(7) 0.077(7) 0.091(7) -0.003(6) -0.019(6) 0.015(6) C40 0.074(6) 0.094(9) 0.072(7) 0.027(7) -0.012(5) -0.006(6) C41 0.099(7) 0.076(7) 0.090(6) 0.014(6) 0.001(5) 0.001(6) C43 0.050(5) 0.063(6) 0.088(6) -0.001(5) -0.012(4) -0.002(5) C44 0.063(6) 0.090(7) 0.053(5) 0.002(5) 0.000(4) -0.014(6) C45 0.067(8) 0.209(13) 0.125(9) -0.045(8) 0.009(6) -0.031(8) C46 0.087(9) 0.281(19) 0.122(11) -0.045(11) 0.003(8) -0.094(11) C47 0.143(13) 0.213(16) 0.087(8) 0.010(8) -0.027(9) -0.119(12) C48 0.121(9) 0.107(8) 0.090(7) -0.015(6) -0.025(7) -0.064(8) C49 0.064(7) 0.086(7) 0.065(6) 0.012(5) -0.011(5) -0.016(6) C50 0.108(8) 0.091(7) 0.081(7) -0.012(5) -0.013(6) -0.002(6) C51 0.129(9) 0.072(7) 0.075(6) -0.014(5) 0.005(6) 0.004(6) N1 0.065(4) 0.061(4) 0.047(4) 0.003(3) 0.009(3) 0.003(4) N2 0.053(4) 0.072(5) 0.052(4) -0.002(4) 0.010(3) -0.001(4) N3 0.129(8) 0.163(9) 0.097(7) -0.014(6) 0.018(6) -0.082(8) N4 0.092(6) 0.059(5) 0.070(5) -0.002(4) -0.006(4) 0.011(4) N5 0.071(5) 0.075(5) 0.043(4) -0.010(3) 0.004(4) -0.008(4) N6 0.089(9) 0.138(10) 0.145(10) 0.018(8) -0.029(8) -0.006(7) N7 0.054(4) 0.075(5) 0.063(4) 0.006(4) -0.001(3) 0.007(4) N8 0.117(7) 0.108(8) 0.073(6) 0.022(7) -0.029(6) -0.013(7) O1 0.140(6) 0.175(7) 0.128(6) -0.014(5) 0.043(5) -0.087(5) O2 0.188(8) 0.240(10) 0.171(8) -0.107(7) 0.051(6) -0.146(7) O3 0.073(4) 0.079(4) 0.069(4) -0.001(3) 0.021(3) 0.014(3) O4 0.106(4) 0.069(4) 0.054(3) -0.006(3) 0.003(3) -0.006(3) O5 0.124(7) 0.181(9) 0.203(10) 0.019(7) 0.007(6) 0.064(6) O6 0.133(7) 0.224(10) 0.186(9) -0.012(8) -0.082(7) 0.024(6) O7 0.182(8) 0.086(5) 0.123(6) 0.028(5) -0.025(5) -0.018(6) O8 0.152(7) 0.155(7) 0.091(5) 0.043(5) 0.008(5) -0.016(5) O9 0.091(5) 0.116(5) 0.072(4) -0.039(3) -0.010(3) 0.000(4) C1S 0.118(11) 0.190(19) 0.087(10) -0.020(10) -0.014(7) 0.012(12) C2S 0.190(14) 0.248(18) 0.161(13) -0.061(13) -0.046(10) -0.040(12) N1S 0.169(12) 0.205(15) 0.160(12) -0.026(9) 0.026(9) -0.008(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 C1 N1 1.474(8) . ? C1 C2 1.529(9) . ? C2 N2 1.474(8) . ? C3 N2 1.353(8) . ? C3 C8 1.396(10) . ? C3 C4 1.399(9) . ? C4 C5 1.361(10) . ? C5 C6 1.370(10) . ? C6 C7 1.372(10) . ? C6 N3 1.423(11) . ? C7 C8 1.363(10) . ? C9 N2 1.450(8) . ? C9 C10 1.506(9) . ? C10 C11 1.391(9) . ? C10 C15 1.405(9) . ? C42 C41 1.366(10) . ? C42 C37 1.407(10) . ? C11 C12 1.377(10) . ? C12 C13 1.361(11) . ? C13 C14 1.355(11) . ? C14 C15 1.371(10) . ? C15 O3 1.367(8) . ? C16 O3 1.433(8) . ? C16 C17 1.484(10) . ? C17 N4 1.420(10) . ? C34 N4 1.438(9) . ? C34 C33 1.490(10) . ? C33 O4 1.418(8) . ? C32 O4 1.352(8) . ? C32 C27 1.373(9) . ? C32 C31 1.375(10) . ? C31 C30 1.366(11) . ? C30 C29 1.351(11) . ? C29 C28 1.364(10) . ? C28 C27 1.373(10) . ? C27 C26 1.501(9) . ? C26 N5 1.452(8) . ? C20 N5 1.384(9) . ? C20 C24 1.387(9) . ? C20 C25 1.391(10) . ? C24 C23 1.370(11) . ? C23 C22 1.386(11) . ? C22 C21 1.339(11) . ? C22 N6 1.454(12) . ? C21 C25 1.344(10) . ? C19 N5 1.443(8) . ? C19 C18 1.514(9) . ? C18 N1 1.463(8) . ? C35 N1 1.450(8) . ? C35 C36 1.505(9) . ? C36 N7 1.464(9) . ? C37 N7 1.380(9) . ? C37 C38 1.402(10) . ? C38 C39 1.379(10) . ? C39 C40 1.389(11) . ? C40 C41 1.358(11) . ? C40 N8 1.435(12) . ? C43 N7 1.459(8) . ? C43 C44 1.503(10) . ? C44 C49 1.371(10) . ? C44 C45 1.372(11) . ? C45 C46 1.395(14) . ? C46 C47 1.321(16) . ? C47 C48 1.363(15) . ? C48 C49 1.384(11) . ? C49 O9 1.380(9) . ? C50 O9 1.410(9) . ? C50 C51 1.505(10) . ? C51 N4 1.460(9) . ? N3 O2 1.221(10) . ? N3 O1 1.251(9) . ? N6 O5 1.197(11) . ? N6 O6 1.219(11) . ? N8 O8 1.232(9) . ? N8 O7 1.245(9) . ? C1S N1S 1.112(16) . ? C1S C2S 1.373(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 114.0(6) . . ? N2 C2 C1 112.8(6) . . ? N2 C3 C8 120.7(7) . . ? N2 C3 C4 121.5(7) . . ? C8 C3 C4 117.8(8) . . ? C5 C4 C3 120.1(8) . . ? C4 C5 C6 121.0(8) . . ? C5 C6 C7 120.1(8) . . ? C5 C6 N3 120.3(9) . . ? C7 C6 N3 119.5(9) . . ? C8 C7 C6 119.6(8) . . ? C7 C8 C3 121.4(8) . . ? N2 C9 C10 113.2(6) . . ? C11 C10 C15 116.3(7) . . ? C11 C10 C9 123.9(7) . . ? C15 C10 C9 119.8(7) . . ? C41 C42 C37 119.8(8) . . ? C12 C11 C10 122.1(8) . . ? C13 C12 C11 119.8(9) . . ? C14 C13 C12 119.8(9) . . ? C13 C14 C15 121.3(9) . . ? O3 C15 C14 125.3(8) . . ? O3 C15 C10 114.1(7) . . ? C14 C15 C10 120.6(8) . . ? O3 C16 C17 109.8(7) . . ? N4 C17 C16 116.5(7) . . ? N4 C34 C33 115.6(7) . . ? O4 C33 C34 107.9(6) . . ? O4 C32 C27 115.4(7) . . ? O4 C32 C31 122.9(8) . . ? C27 C32 C31 121.7(8) . . ? C30 C31 C32 118.1(8) . . ? C29 C30 C31 122.1(8) . . ? C30 C29 C28 118.5(8) . . ? C29 C28 C27 122.1(8) . . ? C32 C27 C28 117.5(7) . . ? C32 C27 C26 119.1(7) . . ? C28 C27 C26 123.3(7) . . ? N5 C26 C27 114.5(6) . . ? N5 C20 C24 120.7(8) . . ? N5 C20 C25 121.7(8) . . ? C24 C20 C25 117.6(8) . . ? C23 C24 C20 121.4(8) . . ? C24 C23 C22 118.3(9) . . ? C21 C22 C23 120.7(9) . . ? C21 C22 N6 121.7(12) . . ? C23 C22 N6 117.6(11) . . ? C22 C21 C25 121.2(9) . . ? C21 C25 C20 120.6(8) . . ? N5 C19 C18 114.3(6) . . ? N1 C18 C19 112.5(5) . . ? N1 C35 C36 116.2(6) . . ? N7 C36 C35 114.6(6) . . ? N7 C37 C38 121.0(8) . . ? N7 C37 C42 120.4(8) . . ? C38 C37 C42 118.7(8) . . ? C39 C38 C37 120.0(8) . . ? C38 C39 C40 119.5(9) . . ? C41 C40 C39 120.7(9) . . ? C41 C40 N8 120.8(11) . . ? C39 C40 N8 118.5(11) . . ? C40 C41 C42 120.9(9) . . ? N7 C43 C44 113.6(6) . . ? C49 C44 C45 116.1(9) . . ? C49 C44 C43 120.9(8) . . ? C45 C44 C43 122.9(9) . . ? C44 C45 C46 121.7(11) . . ? C47 C46 C45 120.1(13) . . ? C46 C47 C48 120.7(12) . . ? C47 C48 C49 119.0(11) . . ? C44 C49 O9 114.6(8) . . ? C44 C49 C48 122.4(10) . . ? O9 C49 C48 123.0(10) . . ? O9 C50 C51 107.9(7) . . ? N4 C51 C50 115.1(8) . . ? C35 N1 C18 110.3(6) . . ? C35 N1 C1 111.1(6) . . ? C18 N1 C1 108.5(6) . . ? C3 N2 C9 122.9(6) . . ? C3 N2 C2 121.1(6) . . ? C9 N2 C2 115.6(6) . . ? O2 N3 O1 120.1(9) . . ? O2 N3 C6 120.0(10) . . ? O1 N3 C6 119.9(10) . . ? C17 N4 C34 111.6(8) . . ? C17 N4 C51 112.4(7) . . ? C34 N4 C51 111.6(7) . . ? C20 N5 C19 121.1(6) . . ? C20 N5 C26 122.6(6) . . ? C19 N5 C26 116.2(6) . . ? O5 N6 O6 122.4(12) . . ? O5 N6 C22 119.0(12) . . ? O6 N6 C22 118.6(12) . . ? C37 N7 C43 121.0(6) . . ? C37 N7 C36 120.8(7) . . ? C43 N7 C36 117.9(6) . . ? O8 N8 O7 122.1(10) . . ? O8 N8 C40 118.9(11) . . ? O7 N8 C40 119.0(11) . . ? C15 O3 C16 118.3(6) . . ? C32 O4 C33 118.8(6) . . ? C49 O9 C50 115.6(7) . . ? N1S C1S C2S 175.1(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 76.8(8) . . . . ? N2 C3 C4 C5 -179.6(7) . . . . ? C8 C3 C4 C5 1.0(11) . . . . ? C3 C4 C5 C6 0.8(13) . . . . ? C4 C5 C6 C7 -1.7(13) . . . . ? C4 C5 C6 N3 179.7(8) . . . . ? C5 C6 C7 C8 0.8(13) . . . . ? N3 C6 C7 C8 179.4(8) . . . . ? C6 C7 C8 C3 1.1(13) . . . . ? N2 C3 C8 C7 178.7(7) . . . . ? C4 C3 C8 C7 -1.9(11) . . . . ? N2 C9 C10 C11 10.8(9) . . . . ? N2 C9 C10 C15 -170.3(6) . . . . ? C15 C10 C11 C12 1.6(10) . . . . ? C9 C10 C11 C12 -179.5(7) . . . . ? C10 C11 C12 C13 -2.1(12) . . . . ? C11 C12 C13 C14 1.9(13) . . . . ? C12 C13 C14 C15 -1.3(14) . . . . ? C13 C14 C15 O3 -179.9(8) . . . . ? C13 C14 C15 C10 0.8(13) . . . . ? C11 C10 C15 O3 179.7(6) . . . . ? C9 C10 C15 O3 0.7(9) . . . . ? C11 C10 C15 C14 -0.9(10) . . . . ? C9 C10 C15 C14 -179.8(7) . . . . ? O3 C16 C17 N4 53.9(10) . . . . ? N4 C34 C33 O4 49.6(11) . . . . ? O4 C32 C31 C30 -179.0(7) . . . . ? C27 C32 C31 C30 0.3(12) . . . . ? C32 C31 C30 C29 -1.2(14) . . . . ? C31 C30 C29 C28 1.7(15) . . . . ? C30 C29 C28 C27 -1.5(15) . . . . ? O4 C32 C27 C28 179.3(7) . . . . ? C31 C32 C27 C28 -0.1(12) . . . . ? O4 C32 C27 C26 2.0(10) . . . . ? C31 C32 C27 C26 -177.5(7) . . . . ? C29 C28 C27 C32 0.7(13) . . . . ? C29 C28 C27 C26 177.9(8) . . . . ? C32 C27 C26 N5 -165.1(7) . . . . ? C28 C27 C26 N5 17.8(11) . . . . ? N5 C20 C24 C23 -179.8(7) . . . . ? C25 C20 C24 C23 2.6(12) . . . . ? C20 C24 C23 C22 -0.8(12) . . . . ? C24 C23 C22 C21 1.4(13) . . . . ? C24 C23 C22 N6 -178.7(8) . . . . ? C23 C22 C21 C25 -4.0(14) . . . . ? N6 C22 C21 C25 176.1(8) . . . . ? C22 C21 C25 C20 6.0(13) . . . . ? N5 C20 C25 C21 177.2(7) . . . . ? C24 C20 C25 C21 -5.2(12) . . . . ? N5 C19 C18 N1 68.0(8) . . . . ? N1 C35 C36 N7 61.6(8) . . . . ? C41 C42 C37 N7 172.3(7) . . . . ? C41 C42 C37 C38 -8.1(11) . . . . ? N7 C37 C38 C39 -173.9(7) . . . . ? C42 C37 C38 C39 6.5(11) . . . . ? C37 C38 C39 C40 -0.4(12) . . . . ? C38 C39 C40 C41 -4.2(12) . . . . ? C38 C39 C40 N8 174.9(7) . . . . ? C39 C40 C41 C42 2.6(13) . . . . ? N8 C40 C41 C42 -176.5(8) . . . . ? C37 C42 C41 C40 3.6(12) . . . . ? N7 C43 C44 C49 -152.1(7) . . . . ? N7 C43 C44 C45 31.5(11) . . . . ? C49 C44 C45 C46 -2.6(14) . . . . ? C43 C44 C45 C46 174.0(10) . . . . ? C44 C45 C46 C47 2(2) . . . . ? C45 C46 C47 C48 -1(2) . . . . ? C46 C47 C48 C49 -0.4(18) . . . . ? C45 C44 C49 O9 -179.6(7) . . . . ? C43 C44 C49 O9 3.7(10) . . . . ? C45 C44 C49 C48 1.4(12) . . . . ? C43 C44 C49 C48 -175.2(7) . . . . ? C47 C48 C49 C44 0.0(13) . . . . ? C47 C48 C49 O9 -178.8(9) . . . . ? O9 C50 C51 N4 61.4(9) . . . . ? C36 C35 N1 C18 -163.7(6) . . . . ? C36 C35 N1 C1 75.9(7) . . . . ? C19 C18 N1 C35 82.2(7) . . . . ? C19 C18 N1 C1 -155.8(6) . . . . ? C2 C1 N1 C35 -160.3(6) . . . . ? C2 C1 N1 C18 78.3(7) . . . . ? C8 C3 N2 C9 2.0(10) . . . . ? C4 C3 N2 C9 -177.3(6) . . . . ? C8 C3 N2 C2 173.9(7) . . . . ? C4 C3 N2 C2 -5.4(10) . . . . ? C10 C9 N2 C3 75.5(8) . . . . ? C10 C9 N2 C2 -96.9(7) . . . . ? C1 C2 N2 C3 82.0(8) . . . . ? C1 C2 N2 C9 -105.6(7) . . . . ? C5 C6 N3 O2 175.4(11) . . . . ? C7 C6 N3 O2 -3.2(15) . . . . ? C5 C6 N3 O1 -4.2(14) . . . . ? C7 C6 N3 O1 177.2(9) . . . . ? C16 C17 N4 C34 179.7(7) . . . . ? C16 C17 N4 C51 53.4(10) . . . . ? C33 C34 N4 C17 53.5(10) . . . . ? C33 C34 N4 C51 -179.8(8) . . . . ? C50 C51 N4 C17 -170.8(7) . . . . ? C50 C51 N4 C34 62.9(10) . . . . ? C24 C20 N5 C19 -0.6(10) . . . . ? C25 C20 N5 C19 176.9(7) . . . . ? C24 C20 N5 C26 -175.9(7) . . . . ? C25 C20 N5 C26 1.6(10) . . . . ? C18 C19 N5 C20 77.6(8) . . . . ? C18 C19 N5 C26 -106.9(7) . . . . ? C27 C26 N5 C20 89.7(8) . . . . ? C27 C26 N5 C19 -85.8(8) . . . . ? C21 C22 N6 O5 12.0(15) . . . . ? C23 C22 N6 O5 -168.0(11) . . . . ? C21 C22 N6 O6 -167.3(11) . . . . ? C23 C22 N6 O6 12.7(14) . . . . ? C38 C37 N7 C43 172.2(6) . . . . ? C42 C37 N7 C43 -8.2(9) . . . . ? C38 C37 N7 C36 -1.5(10) . . . . ? C42 C37 N7 C36 178.1(6) . . . . ? C44 C43 N7 C37 89.8(8) . . . . ? C44 C43 N7 C36 -96.3(8) . . . . ? C35 C36 N7 C37 78.7(8) . . . . ? C35 C36 N7 C43 -95.2(8) . . . . ? C41 C40 N8 O8 4.3(13) . . . . ? C39 C40 N8 O8 -174.9(8) . . . . ? C41 C40 N8 O7 -174.3(8) . . . . ? C39 C40 N8 O7 6.5(12) . . . . ? C14 C15 O3 C16 -18.7(11) . . . . ? C10 C15 O3 C16 160.7(6) . . . . ? C17 C16 O3 C15 -173.1(7) . . . . ? C27 C32 O4 C33 161.4(7) . . . . ? C31 C32 O4 C33 -19.1(11) . . . . ? C34 C33 O4 C32 -178.9(7) . . . . ? C44 C49 O9 C50 145.9(7) . . . . ? C48 C49 O9 C50 -35.1(10) . . . . ? C51 C50 O9 C49 -179.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 22.47 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.202 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.044 #===END #CIF File for L4 data_L4 _database_code_CSD 172623 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '160 celcius' _chemical_formula_moiety 'C53 H54 N12 O15' _chemical_formula_sum 'C53 H54 N12 O15' _chemical_formula_weight 1099.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.798(2) _cell_length_b 12.137(7) _cell_length_c 19.707(6) _cell_angle_alpha 89.51(6) _cell_angle_beta 79.11(2) _cell_angle_gamma 75.62(4) _cell_volume 2682.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.7 _cell_measurement_theta_max 14.6 _exptl_crystal_description 'rectangular parallelopiped' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 1.38 _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method floatation _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Turbo CAD4' _diffrn_measurement_method 'theta-2theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every hour' _diffrn_standards_decay_% 'less than 0.7%' _diffrn_reflns_number 7391 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.3072 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 22.48 _reflns_number_total 6980 _reflns_number_gt 1941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms and Wocadlo, 1995)' _computing_structure_solution 'xtal' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3' _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^)+(0.1664P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0054(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6980 _refine_ls_number_parameters 638 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3104 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.3421 _refine_ls_wR_factor_gt 0.2234 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0406(10) 0.0810(10) 0.6608(6) 0.047(3) Uiso 1 1 d . . . H1A H 0.0102 0.0417 0.6284 0.056 Uiso 1 1 calc R . . H1B H 0.0698 0.1414 0.6365 0.056 Uiso 1 1 calc R . . C2 C -0.0602(10) 0.1333(10) 0.7194(6) 0.045(3) Uiso 1 1 d . . . H2A H -0.1349 0.1445 0.7032 0.054 Uiso 1 1 calc R . . H2B H -0.0614 0.0799 0.7563 0.054 Uiso 1 1 calc R . . C3 C -0.1420(10) 0.3408(11) 0.7495(6) 0.042(3) Uani 1 1 d . . . C4 C -0.2206(12) 0.3653(10) 0.7042(6) 0.040(3) Uani 1 1 d . . . C5 C -0.3205(12) 0.4537(13) 0.7133(7) 0.061(4) Uani 1 1 d . . . H5 H -0.3761 0.4606 0.6847 0.073 Uiso 1 1 calc R . . C6 C -0.3360(12) 0.5348(11) 0.7683(7) 0.049(3) Uani 1 1 d . . . C7 C -0.2525(12) 0.5188(11) 0.8092(6) 0.051(4) Uani 1 1 d . . . H7 H -0.2604 0.5735 0.8437 0.061 Uiso 1 1 calc R . . C8 C -0.1577(11) 0.4254(11) 0.8015(6) 0.049(4) Uani 1 1 d . . . H8 H -0.1031 0.4177 0.8308 0.059 Uiso 1 1 calc R . . C9 C 0.0304(10) 0.2299(10) 0.7956(6) 0.049(3) Uiso 1 1 d . . . H9A H 0.0722 0.1503 0.7956 0.059 Uiso 1 1 calc R . . H9B H -0.0153 0.2516 0.8420 0.059 Uiso 1 1 calc R . . C10 C 0.1231(10) 0.3000(10) 0.7796(6) 0.042(3) Uani 1 1 d . . . C11 C 0.1382(11) 0.3572(10) 0.7185(6) 0.047(3) Uani 1 1 d . . . H11 H 0.0897 0.3577 0.6863 0.056 Uiso 1 1 calc R . . C12 C 0.2292(12) 0.4137(10) 0.7074(7) 0.056(4) Uani 1 1 d . . . H12 H 0.2386 0.4558 0.6681 0.067 Uiso 1 1 calc R . . C13 C 0.3051(11) 0.4092(11) 0.7527(7) 0.057(4) Uani 1 1 d . . . H13 H 0.3692 0.4422 0.7423 0.068 Uiso 1 1 calc R . . C14 C 0.2849(10) 0.3547(11) 0.8140(6) 0.045(3) Uani 1 1 d . . . C15 C 0.1942(10) 0.2984(9) 0.8256(6) 0.039(3) Uani 1 1 d . . . H15 H 0.1825 0.2588 0.8659 0.047 Uiso 1 1 calc R . . C16 C 0.4514(11) 0.3973(11) 0.8526(6) 0.055(4) Uiso 1 1 d . . . H16A H 0.4272 0.4771 0.8424 0.066 Uiso 1 1 calc R . . H16B H 0.5102 0.3578 0.8136 0.066 Uiso 1 1 calc R . . C17 C 0.5041(11) 0.3843(11) 0.9182(6) 0.054(4) Uiso 1 1 d . . . H17A H 0.5662 0.4248 0.9137 0.065 Uiso 1 1 calc R . . H17B H 0.4423 0.4187 0.9572 0.065 Uiso 1 1 calc R . . C18 C 0.1104(10) -0.1108(10) 0.6914(6) 0.046(3) Uiso 1 1 d . . . H18A H 0.1134 -0.1426 0.6459 0.055 Uiso 1 1 calc R . . H18B H 0.0291 -0.0986 0.7167 0.055 Uiso 1 1 calc R . . C19 C 0.1918(10) -0.1980(10) 0.7287(6) 0.042(3) Uiso 1 1 d . . . H19A H 0.1689 -0.2693 0.7275 0.050 Uiso 1 1 calc R . . H19B H 0.2726 -0.2109 0.7026 0.050 Uiso 1 1 calc R . . C20 C 0.1826(11) -0.2509(10) 0.8491(7) 0.046(3) Uani 1 1 d . . . C21 C 0.0946(11) -0.3131(10) 0.8518(6) 0.049(3) Uani 1 1 d . . . C22 C 0.0912(11) -0.4036(11) 0.8962(7) 0.053(4) Uani 1 1 d . . . H22 H 0.0377 -0.4479 0.8947 0.064 Uiso 1 1 calc R . . C23 C 0.1666(12) -0.4254(10) 0.9410(7) 0.047(3) Uani 1 1 d . . . C24 C 0.2468(12) -0.3624(12) 0.9442(6) 0.057(4) Uani 1 1 d . . . H24 H 0.2960 -0.3778 0.9767 0.069 Uiso 1 1 calc R . . C25 C 0.2547(10) -0.2763(10) 0.8992(6) 0.047(3) Uani 1 1 d . . . H25 H 0.3092 -0.2336 0.9019 0.057 Uiso 1 1 calc R . . C26 C 0.2751(10) -0.0994(10) 0.8065(6) 0.048(3) Uiso 1 1 d . . . H26A H 0.2766 -0.0493 0.7679 0.058 Uiso 1 1 calc R . . H26B H 0.3547 -0.1487 0.8028 0.058 Uiso 1 1 calc R . . C27 C 0.2455(12) -0.0296(10) 0.8712(6) 0.044(3) Uani 1 1 d . . . C28 C 0.1326(12) 0.0129(10) 0.9103(7) 0.046(3) Uani 1 1 d . . . H28 H 0.0687 -0.0075 0.8971 0.055 Uiso 1 1 calc R . . C29 C 0.1104(12) 0.0844(11) 0.9679(7) 0.059(4) Uani 1 1 d . . . H29 H 0.0334 0.1101 0.9934 0.070 Uiso 1 1 calc R . . C30 C 0.2031(13) 0.1167(10) 0.9869(6) 0.052(4) Uani 1 1 d . . . H30 H 0.1886 0.1666 1.0250 0.062 Uiso 1 1 calc R . . C31 C 0.3187(12) 0.0763(10) 0.9505(7) 0.042(3) Uani 1 1 d . . . C32 C 0.3378(11) 0.0069(9) 0.8936(7) 0.045(3) Uani 1 1 d . . . H32 H 0.4150 -0.0178 0.8682 0.054 Uiso 1 1 calc R . . C33 C 0.3981(11) 0.2002(11) 1.0118(7) 0.060(4) Uiso 1 1 d . . . H33A H 0.3751 0.1816 1.0595 0.072 Uiso 1 1 calc R . . H33B H 0.3364 0.2629 1.0006 0.072 Uiso 1 1 calc R . . C34 C 0.5174(10) 0.2315(10) 1.0003(6) 0.046(3) Uiso 1 1 d . . . H34A H 0.5116 0.2936 1.0325 0.055 Uiso 1 1 calc R . . H34B H 0.5778 0.1667 1.0106 0.055 Uiso 1 1 calc R . . C35 C 0.2496(10) -0.0090(10) 0.6319(6) 0.044(3) Uiso 1 1 d . . . H35A H 0.2311 -0.0029 0.5859 0.053 Uiso 1 1 calc R . . H35B H 0.3030 -0.0833 0.6344 0.053 Uiso 1 1 calc R . . C36 C 0.3111(10) 0.0822(10) 0.6441(6) 0.040(3) Uiso 1 1 d . . . H36A H 0.2580 0.1562 0.6404 0.048 Uiso 1 1 calc R . . H36B H 0.3265 0.0776 0.6909 0.048 Uiso 1 1 calc R . . C37 C 0.4515(11) 0.1636(10) 0.5574(6) 0.040(3) Uani 1 1 d . . . C38 C 0.3701(12) 0.2471(11) 0.5292(6) 0.046(3) Uani 1 1 d . . . C39 C 0.4037(12) 0.3310(11) 0.4889(6) 0.051(4) Uani 1 1 d . . . H39 H 0.3467 0.3875 0.4732 0.062 Uiso 1 1 calc R . . C40 C 0.5218(13) 0.3305(12) 0.4722(6) 0.055(4) Uani 1 1 d . . . C41 C 0.6067(13) 0.2488(12) 0.4980(6) 0.056(4) Uani 1 1 d . . . H41 H 0.6866 0.2500 0.4874 0.067 Uiso 1 1 calc R . . C42 C 0.5719(11) 0.1662(11) 0.5394(6) 0.049(3) Uani 1 1 d . . . H42 H 0.6294 0.1110 0.5557 0.058 Uiso 1 1 calc R . . C43 C 0.5162(10) -0.0264(10) 0.6006(6) 0.044(3) Uiso 1 1 d . . . H43A H 0.5776 -0.0322 0.5595 0.053 Uiso 1 1 calc R . . H43B H 0.4829 -0.0915 0.5987 0.053 Uiso 1 1 calc R . . C44 C 0.5763(11) -0.0389(12) 0.6615(6) 0.048(3) Uani 1 1 d . . . C45 C 0.6411(13) -0.1453(12) 0.6724(7) 0.068(4) Uani 1 1 d . . . H45 H 0.6430 -0.2059 0.6432 0.081 Uiso 1 1 calc R . . C46 C 0.7041(13) -0.1654(14) 0.7259(8) 0.080(5) Uani 1 1 d . . . H46 H 0.7478 -0.2388 0.7317 0.096 Uiso 1 1 calc R . . C47 C 0.7029(13) -0.0786(14) 0.7702(7) 0.071(4) Uani 1 1 d . . . H47 H 0.7460 -0.0914 0.8057 0.085 Uiso 1 1 calc R . . C48 C 0.6358(11) 0.0276(12) 0.7605(7) 0.050(3) Uani 1 1 d . . . C49 C 0.5744(10) 0.0488(10) 0.7071(6) 0.039(3) Uani 1 1 d . . . H49 H 0.5311 0.1224 0.7014 0.046 Uiso 1 1 calc R . . C50 C 0.6858(12) 0.1028(11) 0.8593(7) 0.062(4) Uiso 1 1 d . . . H50A H 0.7696 0.0648 0.8445 0.075 Uiso 1 1 calc R . . H50B H 0.6489 0.0539 0.8904 0.075 Uiso 1 1 calc R . . C51 C 0.6739(11) 0.2127(11) 0.8960(7) 0.060(4) Uiso 1 1 d . . . H51A H 0.7268 0.2000 0.9291 0.071 Uiso 1 1 calc R . . H51B H 0.6995 0.2652 0.8627 0.071 Uiso 1 1 calc R . . N1 N 0.1396(8) 0.0013(7) 0.6830(5) 0.043(3) Uani 1 1 d . . . N2 N -0.0537(8) 0.2416(8) 0.7477(5) 0.042(3) Uani 1 1 d . . . N3 N -0.1956(14) 0.3040(11) 0.6379(7) 0.076(4) Uani 1 1 d . . . N4 N -0.4407(11) 0.6279(10) 0.7773(7) 0.061(3) Uani 1 1 d . . . N5 N 0.1927(8) -0.1700(8) 0.8005(5) 0.039(3) Uani 1 1 d . . . N6 N -0.0068(11) -0.2772(14) 0.8174(6) 0.067(4) Uani 1 1 d . . . N7 N 0.1639(12) -0.5171(10) 0.9889(7) 0.064(4) Uani 1 1 d . . . N8 N 0.4239(8) 0.0732(8) 0.5955(5) 0.044(3) Uani 1 1 d . . . N9 N 0.2455(10) 0.2458(13) 0.5326(6) 0.060(3) Uani 1 1 d . . . N10 N 0.5607(15) 0.4185(12) 0.4265(6) 0.067(4) Uani 1 1 d . . . N11 N 0.5544(9) 0.2643(9) 0.9319(5) 0.053(3) Uani 1 1 d . . . O1 O -0.0966(11) 0.2808(9) 0.6043(5) 0.083(4) Uani 1 1 d . . . O2 O -0.2827(11) 0.2796(11) 0.6208(7) 0.137(6) Uani 1 1 d . . . O3 O -0.5103(9) 0.6417(9) 0.7381(6) 0.093(4) Uani 1 1 d . . . O4 O -0.4550(9) 0.6935(10) 0.8279(6) 0.086(3) Uani 1 1 d . . . O5 O 0.3502(7) 0.3493(7) 0.8645(4) 0.055(2) Uani 1 1 d . . . O6 O -0.0558(9) -0.1781(11) 0.8223(6) 0.096(4) Uani 1 1 d . . . O7 O -0.0339(12) -0.3494(12) 0.7876(7) 0.134(6) Uani 1 1 d . . . O8 O 0.1079(8) -0.5866(8) 0.9775(5) 0.066(3) Uani 1 1 d . . . O9 O 0.2155(10) -0.5236(9) 1.0367(5) 0.091(4) Uani 1 1 d . . . O10 O 0.4157(8) 0.1032(7) 0.9665(4) 0.059(3) Uani 1 1 d . . . O11 O 0.1687(9) 0.3315(9) 0.5506(5) 0.083(3) Uani 1 1 d . . . O12 O 0.2280(8) 0.1545(9) 0.5142(5) 0.071(3) Uani 1 1 d . . . O13 O 0.4809(11) 0.4953(9) 0.4140(5) 0.085(4) Uani 1 1 d . . . O14 O 0.6673(12) 0.4015(10) 0.4070(6) 0.106(4) Uani 1 1 d . . . O15 O 0.6303(7) 0.1220(7) 0.8008(4) 0.056(2) Uani 1 1 d . . . N1S N 0.1666(17) 0.4249(15) 0.4022(9) 0.142(7) Uani 1 1 d . . . C2S C 0.078(2) 0.4021(19) 0.4076(11) 0.123(8) Uiso 1 1 d . . . C1S C -0.034(2) 0.372(2) 0.4232(12) 0.180(10) Uiso 1 1 d . . . H1SA H -0.0631 0.3672 0.3812 0.271 Uiso 1 1 calc R . . H1SB H -0.0906 0.4288 0.4542 0.271 Uiso 1 1 calc R . . H1SC H -0.0234 0.2996 0.4444 0.271 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 C3 0.034(8) 0.034(8) 0.059(9) -0.003(7) -0.001(7) -0.018(7) C4 0.052(9) 0.034(8) 0.048(9) 0.012(7) -0.029(7) -0.021(7) C5 0.041(9) 0.072(11) 0.067(10) 0.015(9) -0.011(8) -0.007(8) C6 0.050(9) 0.041(9) 0.055(9) -0.001(7) -0.006(8) -0.012(8) C7 0.051(9) 0.053(10) 0.056(9) 0.004(7) -0.013(8) -0.025(8) C8 0.035(8) 0.056(10) 0.057(9) 0.008(8) -0.022(7) -0.005(8) C10 0.036(8) 0.043(8) 0.054(9) 0.012(7) -0.019(7) -0.016(6) C11 0.060(9) 0.051(9) 0.035(8) -0.001(7) -0.023(7) -0.012(7) C12 0.069(10) 0.042(9) 0.062(10) 0.019(7) -0.019(8) -0.021(8) C13 0.049(9) 0.071(11) 0.066(10) 0.019(8) -0.013(8) -0.041(8) C14 0.042(8) 0.058(9) 0.044(8) 0.007(7) -0.025(7) -0.015(7) C15 0.042(8) 0.026(7) 0.052(8) 0.010(6) -0.005(7) -0.017(6) C20 0.045(8) 0.038(8) 0.059(9) 0.001(7) -0.014(7) -0.017(7) C21 0.051(9) 0.040(9) 0.059(9) 0.019(7) -0.015(7) -0.014(7) C22 0.055(9) 0.043(9) 0.069(10) 0.020(8) -0.017(8) -0.021(7) C23 0.061(9) 0.028(8) 0.060(9) 0.020(7) -0.018(8) -0.022(7) C24 0.068(10) 0.061(10) 0.041(8) -0.001(8) -0.028(7) 0.001(8) C25 0.053(9) 0.046(9) 0.057(8) 0.014(7) -0.037(7) -0.018(7) C27 0.062(10) 0.028(8) 0.051(8) 0.010(6) -0.012(8) -0.027(7) C28 0.052(9) 0.032(8) 0.061(9) 0.010(7) -0.008(8) -0.027(7) C29 0.061(10) 0.042(9) 0.075(11) -0.002(8) 0.005(8) -0.031(8) C30 0.082(11) 0.042(9) 0.040(8) 0.008(7) 0.000(8) -0.040(9) C31 0.049(9) 0.027(8) 0.056(9) 0.007(7) -0.012(8) -0.019(7) C32 0.053(9) 0.017(7) 0.068(10) 0.002(7) -0.011(7) -0.014(6) C37 0.048(9) 0.030(8) 0.033(7) -0.009(6) 0.001(6) -0.002(7) C38 0.054(9) 0.039(9) 0.043(8) 0.012(7) -0.014(7) -0.008(7) C39 0.060(10) 0.057(10) 0.032(8) -0.002(7) -0.007(7) -0.008(8) C40 0.064(11) 0.063(11) 0.041(8) -0.005(8) -0.007(8) -0.021(9) C41 0.064(10) 0.059(10) 0.052(9) 0.009(8) -0.013(8) -0.032(9) C42 0.051(9) 0.054(10) 0.043(8) -0.001(7) -0.011(7) -0.015(7) C44 0.044(8) 0.052(10) 0.044(8) 0.003(7) -0.010(7) -0.007(7) C45 0.087(12) 0.042(10) 0.074(11) -0.002(8) -0.029(9) -0.002(9) C46 0.084(12) 0.060(12) 0.098(13) 0.010(10) -0.048(11) 0.002(9) C47 0.074(11) 0.067(12) 0.062(10) -0.001(9) -0.030(9) 0.015(9) C48 0.052(9) 0.049(10) 0.050(9) -0.004(8) -0.013(7) -0.010(8) C49 0.042(8) 0.028(8) 0.042(8) 0.006(6) -0.009(7) -0.003(6) N1 0.046(6) 0.024(6) 0.062(7) 0.010(5) -0.009(5) -0.016(5) N2 0.044(7) 0.045(7) 0.042(6) -0.002(5) -0.018(5) -0.013(6) N3 0.073(10) 0.074(10) 0.079(11) -0.003(8) -0.049(9) 0.009(9) N4 0.055(9) 0.041(8) 0.077(10) -0.005(7) 0.006(7) -0.006(7) N5 0.049(7) 0.033(6) 0.043(6) 0.013(5) -0.005(5) -0.029(5) N6 0.062(9) 0.078(11) 0.076(9) 0.030(9) -0.029(7) -0.038(9) N7 0.079(10) 0.040(9) 0.060(9) 0.003(7) 0.015(7) -0.012(7) N8 0.042(6) 0.035(7) 0.056(7) 0.019(5) -0.015(5) -0.009(5) N9 0.045(8) 0.070(10) 0.050(8) 0.032(7) -0.009(6) 0.011(8) N10 0.096(12) 0.063(10) 0.051(8) 0.020(7) -0.001(8) -0.048(10) N11 0.047(7) 0.065(8) 0.048(7) -0.004(6) -0.008(5) -0.019(6) O1 0.093(9) 0.079(8) 0.057(7) -0.004(6) -0.015(6) 0.018(7) O2 0.100(10) 0.158(13) 0.156(12) -0.076(10) -0.077(9) 0.002(9) O3 0.075(8) 0.083(9) 0.130(10) 0.012(7) -0.057(8) -0.011(6) O4 0.075(8) 0.084(9) 0.083(8) -0.018(7) -0.014(6) 0.011(6) O5 0.062(6) 0.052(6) 0.061(6) 0.028(5) -0.020(5) -0.031(5) O6 0.064(8) 0.074(9) 0.156(11) 0.052(8) -0.041(7) -0.015(7) O7 0.153(12) 0.119(11) 0.189(14) 0.041(10) -0.119(11) -0.079(10) O8 0.075(7) 0.033(6) 0.074(7) 0.021(5) 0.007(5) -0.001(5) O9 0.146(11) 0.077(8) 0.052(7) 0.028(6) -0.041(7) -0.013(7) O10 0.061(6) 0.040(6) 0.085(7) -0.012(5) -0.025(5) -0.019(5) O11 0.059(7) 0.076(8) 0.096(8) 0.023(6) -0.011(6) 0.012(6) O12 0.068(7) 0.071(8) 0.092(8) 0.028(6) -0.030(6) -0.040(6) O13 0.129(10) 0.053(8) 0.086(8) 0.025(6) -0.038(7) -0.033(7) O14 0.098(10) 0.108(10) 0.116(10) 0.027(7) 0.013(8) -0.061(9) O15 0.071(6) 0.051(6) 0.049(5) -0.004(5) -0.030(5) -0.006(5) N1S 0.137(16) 0.143(17) 0.166(17) 0.055(12) -0.053(13) -0.054(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.456(13) . ? C1 C2 1.507(14) . ? C2 N2 1.458(13) . ? C3 N2 1.378(14) . ? C3 C4 1.384(15) . ? C3 C8 1.411(16) . ? C4 C5 1.366(16) . ? C4 N3 1.453(16) . ? C5 C6 1.425(17) . ? C6 C7 1.365(16) . ? C6 N4 1.435(16) . ? C7 C8 1.366(16) . ? C9 N2 1.476(13) . ? C9 C10 1.532(15) . ? C10 C15 1.342(14) . ? C10 C11 1.390(15) . ? C11 C12 1.394(16) . ? C12 C13 1.370(15) . ? C13 C14 1.383(16) . ? C14 O5 1.362(12) . ? C14 C15 1.390(15) . ? C16 O5 1.435(13) . ? C16 C17 1.527(15) . ? C17 N11 1.473(14) . ? C18 N1 1.484(13) . ? C18 C19 1.527(14) . ? C19 N5 1.461(13) . ? C20 N5 1.376(14) . ? C20 C25 1.404(15) . ? C20 C21 1.421(16) . ? C21 C22 1.401(15) . ? C21 N6 1.458(16) . ? C22 C23 1.348(15) . ? C23 C24 1.366(16) . ? C23 N7 1.456(16) . ? C24 C25 1.375(16) . ? C26 N5 1.467(13) . ? C26 C27 1.473(15) . ? C27 C28 1.383(15) . ? C27 C32 1.414(15) . ? C28 C29 1.379(16) . ? C29 C30 1.365(16) . ? C30 C31 1.386(16) . ? C31 O10 1.357(13) . ? C31 C32 1.357(15) . ? C33 O10 1.432(13) . ? C33 C34 1.522(15) . ? C34 N11 1.422(13) . ? C35 N1 1.463(13) . ? C35 C36 1.510(14) . ? C36 N8 1.465(13) . ? C37 N8 1.395(14) . ? C37 C38 1.402(15) . ? C37 C42 1.406(15) . ? C38 C39 1.375(15) . ? C38 N9 1.463(15) . ? C39 C40 1.368(16) . ? C40 C41 1.391(17) . ? C40 N10 1.495(17) . ? C41 C42 1.380(16) . ? C43 N8 1.429(13) . ? C43 C44 1.492(15) . ? C44 C45 1.367(16) . ? C44 C49 1.392(15) . ? C45 C46 1.388(17) . ? C46 C47 1.370(18) . ? C47 C48 1.368(17) . ? C48 C49 1.375(15) . ? C48 O15 1.381(14) . ? C50 O15 1.420(13) . ? C50 C51 1.486(16) . ? C51 N11 1.440(14) . ? N3 O1 1.195(14) . ? N3 O2 1.242(14) . ? N4 O3 1.213(13) . ? N4 O4 1.241(13) . ? N6 O6 1.194(14) . ? N6 O7 1.197(14) . ? N7 O9 1.207(14) . ? N7 O8 1.239(13) . ? N9 O11 1.202(13) . ? N9 O12 1.245(14) . ? N10 O13 1.209(15) . ? N10 O14 1.209(14) . ? N1S C2S 1.13(2) . ? C2S C1S 1.44(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 113.6(10) . . ? N2 C2 C1 114.7(10) . . ? N2 C3 C4 125.1(12) . . ? N2 C3 C8 119.4(12) . . ? C4 C3 C8 115.4(12) . . ? C5 C4 C3 124.8(13) . . ? C5 C4 N3 113.6(12) . . ? C3 C4 N3 121.3(13) . . ? C4 C5 C6 117.2(13) . . ? C7 C6 C5 118.6(13) . . ? C7 C6 N4 124.3(14) . . ? C5 C6 N4 117.1(13) . . ? C6 C7 C8 122.6(13) . . ? C7 C8 C3 120.5(12) . . ? N2 C9 C10 115.7(10) . . ? C15 C10 C11 121.2(11) . . ? C15 C10 C9 116.9(10) . . ? C11 C10 C9 121.8(11) . . ? C10 C11 C12 117.2(11) . . ? C13 C12 C11 122.2(12) . . ? C12 C13 C14 118.9(11) . . ? O5 C14 C13 124.4(11) . . ? O5 C14 C15 116.4(11) . . ? C13 C14 C15 119.2(11) . . ? C10 C15 C14 121.2(11) . . ? O5 C16 C17 107.5(10) . . ? N11 C17 C16 112.5(10) . . ? N1 C18 C19 115.3(9) . . ? N5 C19 C18 117.1(9) . . ? N5 C20 C25 123.6(11) . . ? N5 C20 C21 120.6(11) . . ? C25 C20 C21 115.8(12) . . ? C22 C21 C20 121.2(12) . . ? C22 C21 N6 115.6(12) . . ? C20 C21 N6 122.5(11) . . ? C23 C22 C21 119.0(12) . . ? C22 C23 C24 122.0(12) . . ? C22 C23 N7 120.6(13) . . ? C24 C23 N7 117.4(13) . . ? C23 C24 C25 119.7(12) . . ? C24 C25 C20 121.9(12) . . ? N5 C26 C27 114.7(10) . . ? C28 C27 C32 115.3(11) . . ? C28 C27 C26 126.1(12) . . ? C32 C27 C26 118.3(12) . . ? C29 C28 C27 123.0(12) . . ? C30 C29 C28 119.0(13) . . ? C29 C30 C31 121.0(12) . . ? O10 C31 C32 116.7(12) . . ? O10 C31 C30 124.5(12) . . ? C32 C31 C30 118.7(12) . . ? C31 C32 C27 123.0(12) . . ? O10 C33 C34 105.8(10) . . ? N11 C34 C33 113.6(10) . . ? N1 C35 C36 111.4(9) . . ? N8 C36 C35 113.4(9) . . ? N8 C37 C38 125.2(12) . . ? N8 C37 C42 118.2(11) . . ? C38 C37 C42 116.3(12) . . ? C39 C38 C37 122.6(13) . . ? C39 C38 N9 113.4(11) . . ? C37 C38 N9 123.6(12) . . ? C40 C39 C38 119.4(13) . . ? C39 C40 C41 120.4(13) . . ? C39 C40 N10 120.3(14) . . ? C41 C40 N10 119.3(13) . . ? C42 C41 C40 119.7(13) . . ? C41 C42 C37 121.4(13) . . ? N8 C43 C44 120.1(10) . . ? C45 C44 C49 117.2(12) . . ? C45 C44 C43 117.1(12) . . ? C49 C44 C43 125.8(12) . . ? C44 C45 C46 121.6(14) . . ? C47 C46 C45 120.9(14) . . ? C48 C47 C46 117.6(14) . . ? C47 C48 C49 121.9(13) . . ? C47 C48 O15 122.7(13) . . ? C49 C48 O15 115.2(12) . . ? C48 C49 C44 120.7(12) . . ? O15 C50 C51 110.2(11) . . ? N11 C51 C50 113.6(11) . . ? C1 N1 C35 110.4(9) . . ? C1 N1 C18 108.2(9) . . ? C35 N1 C18 110.3(9) . . ? C3 N2 C2 123.3(9) . . ? C3 N2 C9 119.7(10) . . ? C2 N2 C9 113.7(10) . . ? O1 N3 O2 124.9(15) . . ? O1 N3 C4 119.9(13) . . ? O2 N3 C4 115.2(14) . . ? O3 N4 O4 122.2(13) . . ? O3 N4 C6 122.3(13) . . ? O4 N4 C6 115.5(13) . . ? C20 N5 C19 118.8(9) . . ? C20 N5 C26 117.3(10) . . ? C19 N5 C26 112.7(9) . . ? O6 N6 O7 126.2(15) . . ? O6 N6 C21 116.5(13) . . ? O7 N6 C21 117.3(15) . . ? O9 N7 O8 122.9(13) . . ? O9 N7 C23 120.2(14) . . ? O8 N7 C23 116.9(13) . . ? C37 N8 C43 119.7(10) . . ? C37 N8 C36 123.6(10) . . ? C43 N8 C36 115.3(9) . . ? O11 N9 O12 124.8(13) . . ? O11 N9 C38 119.1(14) . . ? O12 N9 C38 116.1(12) . . ? O13 N10 O14 129.8(13) . . ? O13 N10 C40 115.2(14) . . ? O14 N10 C40 115.0(14) . . ? C34 N11 C51 118.6(10) . . ? C34 N11 C17 115.3(10) . . ? C51 N11 C17 116.8(10) . . ? C14 O5 C16 118.6(9) . . ? C31 O10 C33 118.7(10) . . ? C48 O15 C50 117.0(10) . . ? N1S C2S C1S 173(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 92.9(12) . . . . ? N2 C3 C4 C5 167.8(12) . . . . ? C8 C3 C4 C5 -11.3(18) . . . . ? N2 C3 C4 N3 -18.8(19) . . . . ? C8 C3 C4 N3 162.2(12) . . . . ? C3 C4 C5 C6 8.8(19) . . . . ? N3 C4 C5 C6 -165.1(12) . . . . ? C4 C5 C6 C7 -1.3(18) . . . . ? C4 C5 C6 N4 179.6(11) . . . . ? C5 C6 C7 C8 -3.0(19) . . . . ? N4 C6 C7 C8 176.0(12) . . . . ? C6 C7 C8 C3 0.4(19) . . . . ? N2 C3 C8 C7 -172.8(11) . . . . ? C4 C3 C8 C7 6.3(17) . . . . ? N2 C9 C10 C15 174.6(11) . . . . ? N2 C9 C10 C11 -9.2(17) . . . . ? C15 C10 C11 C12 -0.8(19) . . . . ? C9 C10 C11 C12 -176.8(11) . . . . ? C10 C11 C12 C13 3(2) . . . . ? C11 C12 C13 C14 -5(2) . . . . ? C12 C13 C14 O5 -176.6(12) . . . . ? C12 C13 C14 C15 5(2) . . . . ? C11 C10 C15 C14 0.6(19) . . . . ? C9 C10 C15 C14 176.8(11) . . . . ? O5 C14 C15 C10 178.8(11) . . . . ? C13 C14 C15 C10 -2.8(19) . . . . ? O5 C16 C17 N11 66.1(13) . . . . ? N1 C18 C19 N5 62.9(13) . . . . ? N5 C20 C21 C22 173.3(11) . . . . ? C25 C20 C21 C22 -7.7(19) . . . . ? N5 C20 C21 N6 -16(2) . . . . ? C25 C20 C21 N6 162.9(12) . . . . ? C20 C21 C22 C23 6(2) . . . . ? N6 C21 C22 C23 -165.6(13) . . . . ? C21 C22 C23 C24 0(2) . . . . ? C21 C22 C23 N7 178.6(12) . . . . ? C22 C23 C24 C25 -2(2) . . . . ? N7 C23 C24 C25 178.7(11) . . . . ? C23 C24 C25 C20 0(2) . . . . ? N5 C20 C25 C24 -176.0(12) . . . . ? C21 C20 C25 C24 5.2(19) . . . . ? N5 C26 C27 C28 -29.0(17) . . . . ? N5 C26 C27 C32 156.9(10) . . . . ? C32 C27 C28 C29 -1.2(17) . . . . ? C26 C27 C28 C29 -175.4(12) . . . . ? C27 C28 C29 C30 1.3(19) . . . . ? C28 C29 C30 C31 -1.8(18) . . . . ? C29 C30 C31 O10 -179.2(11) . . . . ? C29 C30 C31 C32 2.4(18) . . . . ? O10 C31 C32 C27 179.0(10) . . . . ? C30 C31 C32 C27 -2.5(18) . . . . ? C28 C27 C32 C31 1.8(17) . . . . ? C26 C27 C32 C31 176.5(11) . . . . ? O10 C33 C34 N11 62.7(13) . . . . ? N1 C35 C36 N8 178.1(9) . . . . ? N8 C37 C38 C39 -176.5(11) . . . . ? C42 C37 C38 C39 -3.1(17) . . . . ? N8 C37 C38 N9 -4.2(19) . . . . ? C42 C37 C38 N9 169.2(11) . . . . ? C37 C38 C39 C40 3.5(18) . . . . ? N9 C38 C39 C40 -169.5(11) . . . . ? C38 C39 C40 C41 -2.6(19) . . . . ? C38 C39 C40 N10 177.9(11) . . . . ? C39 C40 C41 C42 1.5(19) . . . . ? N10 C40 C41 C42 -179.0(11) . . . . ? C40 C41 C42 C37 -1.2(18) . . . . ? N8 C37 C42 C41 175.8(11) . . . . ? C38 C37 C42 C41 1.9(17) . . . . ? N8 C43 C44 C45 164.1(11) . . . . ? N8 C43 C44 C49 -17.5(19) . . . . ? C49 C44 C45 C46 -1(2) . . . . ? C43 C44 C45 C46 177.5(13) . . . . ? C44 C45 C46 C47 0(2) . . . . ? C45 C46 C47 C48 1(2) . . . . ? C46 C47 C48 C49 -2(2) . . . . ? C46 C47 C48 O15 -178.2(13) . . . . ? C47 C48 C49 C44 1.5(19) . . . . ? O15 C48 C49 C44 177.9(10) . . . . ? C45 C44 C49 C48 0.1(18) . . . . ? C43 C44 C49 C48 -178.3(12) . . . . ? O15 C50 C51 N11 71.2(14) . . . . ? C2 C1 N1 C35 -156.3(9) . . . . ? C2 C1 N1 C18 82.9(11) . . . . ? C36 C35 N1 C1 86.0(11) . . . . ? C36 C35 N1 C18 -154.5(9) . . . . ? C19 C18 N1 C1 -167.8(10) . . . . ? C19 C18 N1 C35 71.4(12) . . . . ? C4 C3 N2 C2 -26.8(18) . . . . ? C8 C3 N2 C2 152.2(10) . . . . ? C4 C3 N2 C9 175.1(11) . . . . ? C8 C3 N2 C9 -5.9(16) . . . . ? C1 C2 N2 C3 121.6(12) . . . . ? C1 C2 N2 C9 -79.2(12) . . . . ? C10 C9 N2 C3 -72.4(14) . . . . ? C10 C9 N2 C2 127.5(11) . . . . ? C5 C4 N3 O1 133.8(14) . . . . ? C3 C4 N3 O1 -40.4(19) . . . . ? C5 C4 N3 O2 -46.3(17) . . . . ? C3 C4 N3 O2 139.5(13) . . . . ? C7 C6 N4 O3 176.9(13) . . . . ? C5 C6 N4 O3 -4.0(18) . . . . ? C7 C6 N4 O4 -2.9(18) . . . . ? C5 C6 N4 O4 176.2(12) . . . . ? C25 C20 N5 C19 134.7(12) . . . . ? C21 C20 N5 C19 -46.5(16) . . . . ? C25 C20 N5 C26 -6.4(17) . . . . ? C21 C20 N5 C26 172.4(11) . . . . ? C18 C19 N5 C20 132.5(11) . . . . ? C18 C19 N5 C26 -84.7(12) . . . . ? C27 C26 N5 C20 -61.3(14) . . . . ? C27 C26 N5 C19 155.3(10) . . . . ? C22 C21 N6 O6 128.1(14) . . . . ? C20 C21 N6 O6 -43.0(19) . . . . ? C22 C21 N6 O7 -51.2(18) . . . . ? C20 C21 N6 O7 137.8(15) . . . . ? C22 C23 N7 O9 -166.7(13) . . . . ? C24 C23 N7 O9 12.4(19) . . . . ? C22 C23 N7 O8 13.9(19) . . . . ? C24 C23 N7 O8 -167.0(12) . . . . ? C38 C37 N8 C43 157.9(11) . . . . ? C42 C37 N8 C43 -15.4(15) . . . . ? C38 C37 N8 C36 -36.4(17) . . . . ? C42 C37 N8 C36 150.3(10) . . . . ? C44 C43 N8 C37 95.7(13) . . . . ? C44 C43 N8 C36 -71.1(14) . . . . ? C35 C36 N8 C37 128.4(11) . . . . ? C35 C36 N8 C43 -65.4(13) . . . . ? C39 C38 N9 O11 -54.6(15) . . . . ? C37 C38 N9 O11 132.4(13) . . . . ? C39 C38 N9 O12 123.3(12) . . . . ? C37 C38 N9 O12 -49.7(16) . . . . ? C39 C40 N10 O13 9.3(18) . . . . ? C41 C40 N10 O13 -170.2(12) . . . . ? C39 C40 N10 O14 -170.1(13) . . . . ? C41 C40 N10 O14 10.4(18) . . . . ? C33 C34 N11 C51 -130.7(11) . . . . ? C33 C34 N11 C17 83.7(13) . . . . ? C50 C51 N11 C34 86.3(14) . . . . ? C50 C51 N11 C17 -128.7(11) . . . . ? C16 C17 N11 C34 -130.6(10) . . . . ? C16 C17 N11 C51 83.2(13) . . . . ? C13 C14 O5 C16 -3.7(18) . . . . ? C15 C14 O5 C16 174.6(11) . . . . ? C17 C16 O5 C14 177.5(10) . . . . ? C32 C31 O10 C33 161.5(11) . . . . ? C30 C31 O10 C33 -16.9(17) . . . . ? C34 C33 O10 C31 -161.2(10) . . . . ? C47 C48 O15 C50 -7.7(18) . . . . ? C49 C48 O15 C50 175.9(11) . . . . ? C51 C50 O15 C48 178.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.425 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.087 #===END