# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name N.Shamala _publ_contact_author_email saravind@physics.iisc.ernet.in loop_ _publ_author_name S.Chandrappa S.Aravinda S.Ragothama R.Sonti R.Raj 'Veldore Harini' N.Shamala P.Balaram data_acv8 _database_code_depnum_ccdc_archive 'CCDC 850189' #TrackingRef 'acv8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-Butyloxycarbonyl-leucyl-valyl-valyl-(1-aminocyclohexan-1-oyl)-valyl- leucyl-valyl-valyl-methyl ester hemihydrate ; _chemical_name_common Boc-Leu-Val-Val-Ac6c-Leu-Val-Val-OMe _chemical_melting_point ? _chemical_formula_moiety 'C50 H90 N8 O11 *0.5(H2O)' _chemical_formula_sum 'C50 H90 N8 O11.50' _chemical_formula_weight 987.30 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.516(3) _cell_length_b 27.593(4) _cell_length_c 21.050(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.919(3) _cell_angle_gamma 90.00 _cell_volume 6050(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'color less' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none _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 'BRUKER AXS SMART APEX CCD with Mo source' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71594 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.06 _reflns_number_total 14733 _reflns_number_gt 8010 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement ? _computing_data_reduction SAINT _computing_structure_solution 'SnB (Weeks and Miller, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1000P)^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 'riding over the heavy atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(10) _refine_ls_number_reflns 14733 _refine_ls_number_parameters 1252 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1814 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 3.079 _refine_ls_shift/su_mean 0.185 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 C11 C 0.6603(7) 0.02527(19) 0.3714(3) 0.0848(17) Uani 1 1 d . . . C12 C 0.7802(8) 0.0322(3) 0.4189(5) 0.138(3) Uani 1 1 d . . . H12A H 0.7905 0.0052 0.4479 0.207 Uiso 1 1 calc R . . H12B H 0.7730 0.0616 0.4426 0.207 Uiso 1 1 calc R . . H12C H 0.8534 0.0343 0.3963 0.207 Uiso 1 1 calc R . . C13 C 0.6638(10) -0.0229(2) 0.3367(4) 0.142(3) Uani 1 1 d . . . H13A H 0.6753 -0.0487 0.3675 0.212 Uiso 1 1 calc R . . H13B H 0.7339 -0.0229 0.3119 0.212 Uiso 1 1 calc R . . H13C H 0.5845 -0.0275 0.3088 0.212 Uiso 1 1 calc R . . C14 C 0.6367(11) 0.0667(3) 0.3253(3) 0.145(4) Uani 1 1 d . . . H14A H 0.5601 0.0606 0.2959 0.217 Uiso 1 1 calc R . . H14B H 0.7083 0.0699 0.3018 0.217 Uiso 1 1 calc R . . H14C H 0.6265 0.0960 0.3485 0.217 Uiso 1 1 calc R . . O1 O 0.5532(4) 0.01838(11) 0.40813(16) 0.0770(10) Uani 1 1 d . . . C10' C 0.5162(5) 0.05223(16) 0.4458(2) 0.0566(11) Uani 1 1 d . . . O10 O 0.5517(3) 0.09427(10) 0.44754(15) 0.0621(8) Uani 1 1 d . . . N11 N 0.4320(4) 0.03367(12) 0.48160(17) 0.0569(9) Uani 1 1 d . . . H11 H 0.4177 0.0030 0.4804 0.068 Uiso 1 1 calc R . . C11A C 0.3636(4) 0.06409(14) 0.5226(2) 0.0541(10) Uani 1 1 d . . . H11A H 0.2966 0.0820 0.4953 0.065 Uiso 1 1 calc R . . C11B C 0.2985(5) 0.03084(16) 0.5673(2) 0.0647(12) Uani 1 1 d . . . H11B H 0.3647 0.0134 0.5948 0.078 Uiso 1 1 calc R . . H11C H 0.2469 0.0071 0.5413 0.078 Uiso 1 1 calc R . . C11C C 0.2124(6) 0.0572(2) 0.6098(3) 0.0867(18) Uani 1 1 d . . . H11D H 0.2577 0.0859 0.6287 0.104 Uiso 1 1 calc R . . C11D C 0.0897(9) 0.0721(4) 0.5751(6) 0.176(4) Uani 1 1 d . . . H11E H 0.0412 0.0889 0.6037 0.263 Uiso 1 1 calc R . . H11F H 0.0429 0.0440 0.5582 0.263 Uiso 1 1 calc R . . H11G H 0.1038 0.0932 0.5405 0.263 Uiso 1 1 calc R . . C11E C 0.1867(11) 0.0224(3) 0.6644(5) 0.174(4) Uani 1 1 d . . . H11H H 0.2668 0.0134 0.6892 0.261 Uiso 1 1 calc R . . H11I H 0.1439 -0.0061 0.6463 0.261 Uiso 1 1 calc R . . H11J H 0.1336 0.0383 0.6917 0.261 Uiso 1 1 calc R . . C11' C 0.4483(4) 0.09996(14) 0.56205(19) 0.0469(10) Uani 1 1 d . . . O11 O 0.4108(3) 0.14184(9) 0.56845(14) 0.0553(7) Uani 1 1 d . . . N12 N 0.5610(3) 0.08436(11) 0.59268(15) 0.0493(8) Uani 1 1 d . . . H12 H 0.5855 0.0551 0.5874 0.059 Uiso 1 1 calc R . . C12A C 0.6416(4) 0.11673(15) 0.6346(2) 0.0529(10) Uani 1 1 d . . . H12D H 0.5922 0.1271 0.6684 0.063 Uiso 1 1 calc R . . C12B C 0.7598(5) 0.08907(19) 0.6669(2) 0.0720(14) Uani 1 1 d . . . H12E H 0.7970 0.0716 0.6334 0.086 Uiso 1 1 calc R . . C12C C 0.8632(6) 0.1235(3) 0.7002(3) 0.103(2) Uani 1 1 d . . . H12F H 0.9362 0.1049 0.7189 0.154 Uiso 1 1 calc R . . H12G H 0.8290 0.1412 0.7333 0.154 Uiso 1 1 calc R . . H12H H 0.8890 0.1457 0.6693 0.154 Uiso 1 1 calc R . . C12D C 0.7189(8) 0.0519(2) 0.7132(3) 0.105(2) Uani 1 1 d . . . H12I H 0.7927 0.0342 0.7325 0.157 Uiso 1 1 calc R . . H12J H 0.6583 0.0299 0.6903 0.157 Uiso 1 1 calc R . . H12K H 0.6798 0.0681 0.7459 0.157 Uiso 1 1 calc R . . C12' C 0.6773(4) 0.16241(16) 0.5993(2) 0.0548(11) Uani 1 1 d . . . O12 O 0.6833(4) 0.20169(13) 0.62612(17) 0.0855(11) Uani 1 1 d . . . N13 N 0.7057(3) 0.15662(12) 0.53981(17) 0.0544(9) Uani 1 1 d . . . H13 H 0.7099 0.1280 0.5241 0.065 Uiso 1 1 calc R . . C13A C 0.7297(4) 0.19878(16) 0.5014(2) 0.0568(11) Uani 1 1 d . . . H13D H 0.7893 0.2200 0.5283 0.068 Uiso 1 1 calc R . . C13B C 0.7942(5) 0.18409(19) 0.4430(3) 0.0737(14) Uani 1 1 d . . . H13E H 0.7384 0.1603 0.4183 0.088 Uiso 1 1 calc R . . C13C C 0.9210(6) 0.1606(3) 0.4627(4) 0.108(2) Uani 1 1 d . . . H13F H 0.9109 0.1342 0.4914 0.162 Uiso 1 1 calc R . . H13G H 0.9798 0.1839 0.4840 0.162 Uiso 1 1 calc R . . H13H H 0.9539 0.1484 0.4254 0.162 Uiso 1 1 calc R . . C13D C 0.8064(8) 0.2277(3) 0.3996(4) 0.116(2) Uani 1 1 d . . . H13I H 0.7237 0.2424 0.3882 0.173 Uiso 1 1 calc R . . H13J H 0.8390 0.2172 0.3614 0.173 Uiso 1 1 calc R . . H13K H 0.8643 0.2509 0.4218 0.173 Uiso 1 1 calc R . . C13' C 0.6062(4) 0.22747(15) 0.4813(2) 0.0492(10) Uani 1 1 d . . . O13 O 0.6052(3) 0.27177(10) 0.48628(15) 0.0607(8) Uani 1 1 d . . . N14 N 0.5026(3) 0.20213(12) 0.45676(16) 0.0504(8) Uani 1 1 d . . . H14 H 0.5063 0.1710 0.4564 0.060 Uiso 1 1 calc R . . C14A C 0.3824(4) 0.22633(14) 0.43039(18) 0.0477(9) Uani 1 1 d . . . C14B C 0.3977(5) 0.25132(17) 0.3662(2) 0.0653(12) Uani 1 1 d . . . H14D H 0.3220 0.2706 0.3521 0.078 Uiso 1 1 calc R . . H14E H 0.4712 0.2728 0.3724 0.078 Uiso 1 1 calc R . . C14C C 0.2743(5) 0.18863(16) 0.4186(2) 0.0626(12) Uani 1 1 d . . . H14F H 0.2720 0.1704 0.4578 0.075 Uiso 1 1 calc R . . H14G H 0.1931 0.2056 0.4091 0.075 Uiso 1 1 calc R . . C14D C 0.2858(6) 0.1534(2) 0.3651(3) 0.0829(16) Uani 1 1 d . . . H14H H 0.3584 0.1321 0.3775 0.100 Uiso 1 1 calc R . . H14I H 0.2090 0.1336 0.3577 0.100 Uiso 1 1 calc R . . C14E C 0.3037(8) 0.1792(2) 0.3043(3) 0.104(2) Uani 1 1 d . . . H14J H 0.2262 0.1969 0.2885 0.124 Uiso 1 1 calc R . . H14K H 0.3187 0.1556 0.2719 0.124 Uiso 1 1 calc R . . C14F C 0.4159(7) 0.2140(2) 0.3150(2) 0.0881(18) Uani 1 1 d . . . H14L H 0.4245 0.2304 0.2751 0.106 Uiso 1 1 calc R . . H14M H 0.4943 0.1959 0.3281 0.106 Uiso 1 1 calc R . . C14' C 0.3465(4) 0.26378(14) 0.47925(19) 0.0464(9) Uani 1 1 d . . . O14 O 0.3091(3) 0.30448(10) 0.46286(13) 0.0575(7) Uani 1 1 d . . . N15 N 0.3501(3) 0.24825(12) 0.53990(15) 0.0466(8) Uani 1 1 d . . . H15 H 0.3821 0.2203 0.5507 0.056 Uiso 1 1 calc R . . C15A C 0.3001(4) 0.27862(15) 0.58770(19) 0.0482(9) Uani 1 1 d . . . H15A H 0.2202 0.2929 0.5662 0.058 Uiso 1 1 calc R . . C15B C 0.2634(5) 0.24951(17) 0.6442(2) 0.0639(12) Uani 1 1 d . . . H15B H 0.2272 0.2727 0.6720 0.077 Uiso 1 1 calc R . . C15C C 0.3740(6) 0.22627(19) 0.6841(2) 0.0747(14) Uani 1 1 d . . . H15C H 0.4386 0.2502 0.6971 0.112 Uiso 1 1 calc R . . H15D H 0.4091 0.2015 0.6596 0.112 Uiso 1 1 calc R . . H15E H 0.3458 0.2121 0.7214 0.112 Uiso 1 1 calc R . . C15D C 0.1577(7) 0.2128(2) 0.6230(3) 0.101(2) Uani 1 1 d . . . H15F H 0.0868 0.2288 0.5979 0.151 Uiso 1 1 calc R . . H15G H 0.1292 0.1984 0.6601 0.151 Uiso 1 1 calc R . . H15H H 0.1904 0.1880 0.5977 0.151 Uiso 1 1 calc R . . C15' C 0.3863(4) 0.32070(14) 0.61083(18) 0.0474(9) Uani 1 1 d . . . O15 O 0.3446(3) 0.35244(11) 0.64281(17) 0.0719(9) Uani 1 1 d . . . N16 N 0.5056(3) 0.32115(11) 0.59583(15) 0.0465(8) Uani 1 1 d . . . H16 H 0.5327 0.2960 0.5777 0.056 Uiso 1 1 calc R . . C16A C 0.5921(4) 0.36232(14) 0.60875(18) 0.0489(10) Uani 1 1 d . . . H16A H 0.5661 0.3798 0.6453 0.059 Uiso 1 1 calc R . . C16B C 0.7301(4) 0.34595(18) 0.6280(2) 0.0624(12) Uani 1 1 d . . . H16B H 0.7534 0.3245 0.5949 0.075 Uiso 1 1 calc R . . H16C H 0.7854 0.3742 0.6293 0.075 Uiso 1 1 calc R . . C16C C 0.7573(6) 0.3201(2) 0.6919(3) 0.0882(18) Uani 1 1 d . . . H16D H 0.6929 0.2946 0.6930 0.106 Uiso 1 1 calc R . . C16D C 0.7480(11) 0.3534(4) 0.7450(3) 0.159(4) Uani 1 1 d . . . H16E H 0.6653 0.3687 0.7391 0.239 Uiso 1 1 calc R . . H16F H 0.8138 0.3776 0.7461 0.239 Uiso 1 1 calc R . . H16G H 0.7589 0.3357 0.7846 0.239 Uiso 1 1 calc R . . C16E C 0.8878(8) 0.2968(4) 0.6985(5) 0.157(4) Uani 1 1 d . . . H16H H 0.8926 0.2756 0.6627 0.235 Uiso 1 1 calc R . . H16I H 0.9016 0.2784 0.7376 0.235 Uiso 1 1 calc R . . H16J H 0.9524 0.3215 0.6994 0.235 Uiso 1 1 calc R . . C16' C 0.5824(4) 0.39772(14) 0.5526(2) 0.0492(10) Uani 1 1 d . . . O16 O 0.6424(3) 0.43569(11) 0.55877(16) 0.0712(9) Uani 1 1 d . . . N17 N 0.5067(4) 0.38548(12) 0.49946(17) 0.0546(9) Uani 1 1 d . . . H17 H 0.4661 0.3584 0.4988 0.066 Uiso 1 1 calc R . . C17A C 0.4886(5) 0.41581(15) 0.4416(2) 0.0535(11) Uani 1 1 d . . . H17A H 0.5513 0.4422 0.4485 0.064 Uiso 1 1 calc R . . C17B C 0.5210(5) 0.38625(17) 0.3835(2) 0.0649(12) Uani 1 1 d . . . H17B H 0.4647 0.3578 0.3783 0.078 Uiso 1 1 calc R . . C17C C 0.6575(6) 0.3691(2) 0.3939(3) 0.0906(17) Uani 1 1 d . . . H17C H 0.6720 0.3501 0.4324 0.136 Uiso 1 1 calc R . . H17D H 0.7141 0.3965 0.3980 0.136 Uiso 1 1 calc R . . H17E H 0.6739 0.3497 0.3581 0.136 Uiso 1 1 calc R . . C17D C 0.4951(7) 0.4171(2) 0.3225(2) 0.0917(18) Uani 1 1 d . . . H17F H 0.4074 0.4278 0.3168 0.138 Uiso 1 1 calc R . . H17G H 0.5106 0.3980 0.2862 0.138 Uiso 1 1 calc R . . H17H H 0.5511 0.4447 0.3264 0.138 Uiso 1 1 calc R . . C17' C 0.3580(4) 0.43872(15) 0.4301(2) 0.0545(11) Uani 1 1 d . . . O17 O 0.3443(3) 0.48134(11) 0.41503(18) 0.0775(10) Uani 1 1 d . . . N18 N 0.2586(4) 0.41020(14) 0.4357(2) 0.0658(10) Uani 1 1 d . . . H18 H 0.2733 0.3805 0.4469 0.079 Uiso 1 1 calc R . . C18A C 0.1268(5) 0.42644(19) 0.4238(3) 0.0818(16) Uani 1 1 d . . . H18A H 0.1305 0.4612 0.4145 0.098 Uiso 1 1 calc R . . C18B C 0.0493(6) 0.4027(2) 0.3629(4) 0.108(2) Uani 1 1 d . . . H18B H -0.0385 0.4154 0.3587 0.129 Uiso 1 1 calc R . . C18C C 0.1054(11) 0.4181(5) 0.3060(4) 0.183(5) Uani 1 1 d . . . H18C H 0.1080 0.4529 0.3044 0.274 Uiso 1 1 calc R . . H18D H 0.0538 0.4061 0.2681 0.274 Uiso 1 1 calc R . . H18E H 0.1909 0.4055 0.3082 0.274 Uiso 1 1 calc R . . C18D C 0.0418(9) 0.3496(3) 0.3664(6) 0.166(4) Uani 1 1 d . . . H18F H 0.0018 0.3405 0.4030 0.249 Uiso 1 1 calc R . . H18G H 0.1268 0.3362 0.3705 0.249 Uiso 1 1 calc R . . H18H H -0.0080 0.3374 0.3281 0.249 Uiso 1 1 calc R . . C18' C 0.0585(6) 0.4222(3) 0.4811(4) 0.104(2) Uani 1 1 d . . . O18 O -0.0446(6) 0.4408(3) 0.4827(4) 0.178(3) Uani 1 1 d . . . C1TM C 0.0538(10) 0.3941(5) 0.5876(5) 0.186(5) Uani 1 1 d . . . H1T1 H 0.1067 0.3753 0.6194 0.279 Uiso 1 1 calc R . . H1T2 H -0.0284 0.3787 0.5775 0.279 Uiso 1 1 calc R . . H1T3 H 0.0426 0.4260 0.6040 0.279 Uiso 1 1 calc R . . O1TM O 0.1172(4) 0.3975(2) 0.5282(3) 0.1222(17) Uani 1 1 d . . . C21 C 0.3315(9) 0.3656(2) -0.1566(3) 0.106(2) Uani 1 1 d . . . C22 C 0.2097(11) 0.3527(4) -0.1292(6) 0.182(5) Uani 1 1 d . . . H22A H 0.1880 0.3785 -0.1021 0.273 Uiso 1 1 calc R . . H22B H 0.2231 0.3234 -0.1045 0.273 Uiso 1 1 calc R . . H22C H 0.1408 0.3480 -0.1636 0.273 Uiso 1 1 calc R . . C23 C 0.3231(14) 0.4157(3) -0.1887(5) 0.208(7) Uani 1 1 d . . . H23A H 0.3011 0.4396 -0.1589 0.312 Uiso 1 1 calc R . . H23B H 0.2585 0.4152 -0.2256 0.312 Uiso 1 1 calc R . . H23C H 0.4046 0.4238 -0.2017 0.312 Uiso 1 1 calc R . . C24 C 0.3736(15) 0.3270(4) -0.1997(4) 0.207(6) Uani 1 1 d . . . H24A H 0.4518 0.3368 -0.2147 0.311 Uiso 1 1 calc R . . H24B H 0.3081 0.3223 -0.2357 0.311 Uiso 1 1 calc R . . H24C H 0.3875 0.2972 -0.1763 0.311 Uiso 1 1 calc R . . O2 O 0.4216(5) 0.37438(12) -0.10248(18) 0.0962(13) Uani 1 1 d . . . C20' C 0.4722(5) 0.34076(17) -0.0617(2) 0.0647(13) Uani 1 1 d . . . O20 O 0.4442(3) 0.29719(11) -0.06622(16) 0.0672(9) Uani 1 1 d . . . N21 N 0.5533(4) 0.35973(13) -0.0148(2) 0.0649(10) Uani 1 1 d . . . H21 H 0.5603 0.3907 -0.0122 0.078 Uiso 1 1 calc R . . C21A C 0.6299(5) 0.33038(17) 0.0316(3) 0.0672(13) Uani 1 1 d . . . H21A H 0.6934 0.3133 0.0099 0.081 Uiso 1 1 calc R . . C21B C 0.7006(7) 0.3641(2) 0.0806(4) 0.110(2) Uani 1 1 d . . . H21B H 0.7499 0.3867 0.0584 0.132 Uiso 1 1 calc R . . H21C H 0.6376 0.3829 0.0997 0.132 Uiso 1 1 calc R . . C21C C 0.7876(11) 0.3414(4) 0.1324(7) 0.200(6) Uani 1 1 d D . . H21D H 0.8259 0.3121 0.1169 0.240 Uiso 1 1 calc R . . C21D C 0.8908(17) 0.3776(7) 0.1568(11) 0.418(16) Uani 1 1 d . . . H21E H 0.9512 0.3626 0.1894 0.627 Uiso 1 1 calc R . . H21F H 0.8524 0.4051 0.1746 0.627 Uiso 1 1 calc R . . H21G H 0.9345 0.3879 0.1221 0.627 Uiso 1 1 calc R . . C21E C 0.7256(14) 0.3302(8) 0.1935(7) 0.258(8) Uani 1 1 d D . . H21H H 0.7868 0.3138 0.2242 0.387 Uiso 1 1 calc R . . H21I H 0.6518 0.3099 0.1824 0.387 Uiso 1 1 calc R . . H21J H 0.7000 0.3599 0.2117 0.387 Uiso 1 1 calc R . . C21' C 0.5537(5) 0.29305(15) 0.0629(2) 0.0556(11) Uani 1 1 d . . . O21 O 0.5984(3) 0.25245(11) 0.07412(16) 0.0684(9) Uani 1 1 d . . . N22 N 0.4411(4) 0.30640(13) 0.07890(17) 0.0587(9) Uani 1 1 d . . . H22 H 0.4113 0.3350 0.0700 0.070 Uiso 1 1 calc R . . C22A C 0.3688(5) 0.27158(18) 0.1119(2) 0.0694(13) Uani 1 1 d . . . H22D H 0.4237 0.2621 0.1514 0.083 Uiso 1 1 calc R . . C22B C 0.2492(6) 0.2966(2) 0.1319(3) 0.0884(17) Uani 1 1 d . . . H22E H 0.2005 0.3127 0.0948 0.106 Uiso 1 1 calc R . . C22C C 0.1669(9) 0.2587(3) 0.1580(5) 0.153(4) Uani 1 1 d . . . H22F H 0.1371 0.2360 0.1247 0.229 Uiso 1 1 calc R . . H22G H 0.0946 0.2740 0.1729 0.229 Uiso 1 1 calc R . . H22H H 0.2166 0.2419 0.1929 0.229 Uiso 1 1 calc R . . C22D C 0.2906(9) 0.3338(3) 0.1847(4) 0.125(3) Uani 1 1 d . . . H22I H 0.2161 0.3501 0.1960 0.188 Uiso 1 1 calc R . . H22J H 0.3471 0.3571 0.1695 0.188 Uiso 1 1 calc R . . H22K H 0.3343 0.3175 0.2218 0.188 Uiso 1 1 calc R . . C22' C 0.3376(5) 0.22613(19) 0.0735(3) 0.0714(14) Uani 1 1 d . . . O22 O 0.3397(5) 0.18681(14) 0.0989(2) 0.1025(14) Uani 1 1 d . . . N23 N 0.3051(3) 0.23156(14) 0.0089(2) 0.0610(10) Uani 1 1 d . . . H23 H 0.2974 0.2600 -0.0077 0.073 Uiso 1 1 calc R . . C23A C 0.2835(4) 0.18885(17) -0.0315(2) 0.0603(12) Uani 1 1 d . . . H23D H 0.2261 0.1671 -0.0120 0.072 Uiso 1 1 calc R . . C23B C 0.2172(5) 0.2027(2) -0.0976(3) 0.0789(15) Uani 1 1 d . . . H23E H 0.2688 0.2279 -0.1147 0.095 Uiso 1 1 calc R . . C23C C 0.2082(7) 0.1595(3) -0.1435(3) 0.115(2) Uani 1 1 d . . . H23F H 0.1684 0.1696 -0.1852 0.173 Uiso 1 1 calc R . . H23G H 0.1576 0.1344 -0.1277 0.173 Uiso 1 1 calc R . . H23H H 0.2928 0.1474 -0.1464 0.173 Uiso 1 1 calc R . . C23D C 0.0821(6) 0.2249(3) -0.0912(4) 0.122(3) Uani 1 1 d . . . H23I H 0.0923 0.2519 -0.0623 0.183 Uiso 1 1 calc R . . H23J H 0.0294 0.2007 -0.0750 0.183 Uiso 1 1 calc R . . H23K H 0.0420 0.2356 -0.1326 0.183 Uiso 1 1 calc R . . C23' C 0.4091(4) 0.16136(16) -0.0356(2) 0.0499(10) Uani 1 1 d . . . O23 O 0.4130(3) 0.11755(11) -0.02972(15) 0.0622(8) Uani 1 1 d . . . N24 N 0.5105(3) 0.18795(12) -0.04588(16) 0.0478(8) Uani 1 1 d . . . H24 H 0.5041 0.2190 -0.0469 0.057 Uiso 1 1 calc R . . C24A C 0.6323(4) 0.16517(15) -0.0554(2) 0.0490(10) Uani 1 1 d . . . C24B C 0.6189(5) 0.13920(17) -0.1204(2) 0.0633(12) Uani 1 1 d . . . H24D H 0.5476 0.1166 -0.1235 0.076 Uiso 1 1 calc R . . H24E H 0.6964 0.1209 -0.1237 0.076 Uiso 1 1 calc R . . C24C C 0.5961(6) 0.1759(2) -0.1759(2) 0.0808(16) Uani 1 1 d . . . H24F H 0.5889 0.1588 -0.2164 0.097 Uiso 1 1 calc R . . H24G H 0.5158 0.1928 -0.1740 0.097 Uiso 1 1 calc R . . C24D C 0.7055(6) 0.2130(2) -0.1727(3) 0.0858(17) Uani 1 1 d . . . H24H H 0.6877 0.2359 -0.2077 0.103 Uiso 1 1 calc R . . H24I H 0.7852 0.1964 -0.1772 0.103 Uiso 1 1 calc R . . C24E C 0.7191(5) 0.23964(18) -0.1095(3) 0.0701(13) Uani 1 1 d . . . H24J H 0.7919 0.2615 -0.1069 0.084 Uiso 1 1 calc R . . H24K H 0.6427 0.2589 -0.1073 0.084 Uiso 1 1 calc R . . C24F C 0.7384(4) 0.20438(16) -0.0524(2) 0.0561(11) Uani 1 1 d . . . H24L H 0.7400 0.2227 -0.0130 0.067 Uiso 1 1 calc R . . H24M H 0.8211 0.1886 -0.0513 0.067 Uiso 1 1 calc R . . C24' C 0.6745(4) 0.12946(14) -0.00129(19) 0.0458(9) Uani 1 1 d . . . O24 O 0.7141(3) 0.08842(10) -0.01161(13) 0.0564(7) Uani 1 1 d . . . N25 N 0.6706(3) 0.14521(11) 0.05838(15) 0.0459(8) Uani 1 1 d . . . H25 H 0.6368 0.1729 0.0645 0.055 Uiso 1 1 calc R . . C25A C 0.7233(4) 0.11559(15) 0.1137(2) 0.0515(10) Uani 1 1 d . . . H25A H 0.8046 0.1022 0.1037 0.062 Uiso 1 1 calc R . . C25B C 0.7564(5) 0.14675(17) 0.1750(2) 0.0688(13) Uani 1 1 d . . . H25B H 0.7975 0.1248 0.2083 0.083 Uiso 1 1 calc R . . C25C C 0.6409(6) 0.1669(2) 0.1998(2) 0.0787(15) Uani 1 1 d . . . H25C H 0.5811 0.1412 0.2041 0.118 Uiso 1 1 calc R . . H25D H 0.6010 0.1907 0.1704 0.118 Uiso 1 1 calc R . . H25E H 0.6663 0.1816 0.2409 0.118 Uiso 1 1 calc R . . C25D C 0.8575(6) 0.1849(2) 0.1647(3) 0.099(2) Uani 1 1 d . . . H25F H 0.8788 0.2035 0.2033 0.149 Uiso 1 1 calc R . . H25G H 0.8239 0.2060 0.1302 0.149 Uiso 1 1 calc R . . H25H H 0.9332 0.1690 0.1543 0.149 Uiso 1 1 calc R . . C25' C 0.6402(4) 0.07291(15) 0.12609(19) 0.0507(10) Uani 1 1 d . . . O25 O 0.6838(4) 0.04133(12) 0.16380(17) 0.0751(10) Uani 1 1 d . . . N26 N 0.5221(3) 0.07113(12) 0.09437(15) 0.0482(8) Uani 1 1 d . . . H26 H 0.4946 0.0958 0.0715 0.058 Uiso 1 1 calc R . . C26A C 0.4376(4) 0.03036(15) 0.0960(2) 0.0537(10) Uani 1 1 d . . . H26A H 0.4654 0.0129 0.1361 0.064 Uiso 1 1 calc R . . C26B C 0.3009(5) 0.04618(18) 0.0977(3) 0.0657(12) Uani 1 1 d . . . H26B H 0.2771 0.0689 0.0629 0.079 Uiso 1 1 calc R . . H26C H 0.2455 0.0181 0.0898 0.079 Uiso 1 1 calc R . . C26C C 0.2753(6) 0.0700(2) 0.1606(3) 0.094(2) Uani 1 1 d . . . H26D H 0.3407 0.0949 0.1719 0.113 Uiso 1 1 calc R . . C26D C 0.2836(10) 0.0345(4) 0.2149(4) 0.154(4) Uani 1 1 d . . . H26E H 0.3671 0.0197 0.2209 0.231 Uiso 1 1 calc R . . H26F H 0.2193 0.0099 0.2052 0.231 Uiso 1 1 calc R . . H26G H 0.2699 0.0511 0.2535 0.231 Uiso 1 1 calc R . . C26E C 0.1474(7) 0.0939(3) 0.1532(5) 0.140(3) Uani 1 1 d . . . H26H H 0.1413 0.1165 0.1183 0.210 Uiso 1 1 calc R . . H26I H 0.1369 0.1107 0.1921 0.210 Uiso 1 1 calc R . . H26J H 0.0813 0.0698 0.1444 0.210 Uiso 1 1 calc R . . C26' C 0.4459(4) -0.00524(15) 0.0413(2) 0.0540(11) Uani 1 1 d . . . O26 O 0.3780(4) -0.04161(12) 0.0367(2) 0.0825(11) Uani 1 1 d . . . N27 N 0.5277(3) 0.00497(12) 0.00039(17) 0.0545(9) Uani 1 1 d . . . H27 H 0.5740 0.0307 0.0069 0.065 Uiso 1 1 calc R . . C27A C 0.5430(4) -0.02491(15) -0.0547(2) 0.0558(11) Uani 1 1 d . . . H27A H 0.4802 -0.0512 -0.0555 0.067 Uiso 1 1 calc R . . C27B C 0.5098(5) 0.00341(18) -0.1174(2) 0.0697(13) Uani 1 1 d . . . H27B H 0.5641 0.0324 -0.1151 0.084 Uiso 1 1 calc R . . C27C C 0.3707(7) 0.0197(3) -0.1247(3) 0.104(2) Uani 1 1 d . . . H27C H 0.3510 0.0379 -0.1636 0.155 Uiso 1 1 calc R . . H27D H 0.3573 0.0396 -0.0888 0.155 Uiso 1 1 calc R . . H27E H 0.3158 -0.0082 -0.1263 0.155 Uiso 1 1 calc R . . C27D C 0.5369(7) -0.0271(2) -0.1757(3) 0.098(2) Uani 1 1 d . . . H27F H 0.6252 -0.0371 -0.1697 0.147 Uiso 1 1 calc R . . H27G H 0.5200 -0.0079 -0.2140 0.147 Uiso 1 1 calc R . . H27H H 0.4824 -0.0551 -0.1796 0.147 Uiso 1 1 calc R . . C27' C 0.6742(5) -0.04836(16) -0.0485(2) 0.0589(12) Uani 1 1 d . . . O27 O 0.6852(4) -0.09210(12) -0.0590(2) 0.0839(11) Uani 1 1 d . . . N28 N 0.7762(4) -0.01966(14) -0.0360(2) 0.0698(11) Uani 1 1 d . . . H28 H 0.7648 0.0105 -0.0284 0.084 Uiso 1 1 calc R . . C28A C 0.9046(5) -0.0375(2) -0.0348(2) 0.0720(14) Uani 1 1 d . . . H28A H 0.8994 -0.0676 -0.0597 0.086 Uiso 1 1 calc R . . C28B C 0.9912(7) -0.0020(3) -0.0662(3) 0.101(2) Uani 1 1 d . . . H28B H 1.0764 -0.0169 -0.0630 0.121 Uiso 1 1 calc R . . C28C C 1.0072(8) 0.0451(3) -0.0336(4) 0.122(3) Uani 1 1 d . . . H28C H 1.0388 0.0402 0.0109 0.183 Uiso 1 1 calc R . . H28D H 0.9260 0.0615 -0.0375 0.183 Uiso 1 1 calc R . . H28E H 1.0674 0.0644 -0.0529 0.183 Uiso 1 1 calc R . . C28D C 0.9424(9) 0.0037(5) -0.1371(4) 0.165(4) Uani 1 1 d . . . H28F H 0.9383 -0.0275 -0.1575 0.247 Uiso 1 1 calc R . . H28G H 0.9997 0.0243 -0.1566 0.247 Uiso 1 1 calc R . . H28H H 0.8583 0.0179 -0.1422 0.247 Uiso 1 1 calc R . . C28' C 0.9673(6) -0.0492(2) 0.0305(3) 0.0916(18) Uani 1 1 d D . . O28 O 0.9407(6) -0.0291(3) 0.0779(3) 0.150(2) Uani 1 1 d D . . O2TM O 1.0581(5) -0.0822(2) 0.0332(3) 0.1197(16) Uani 1 1 d . . . C2TM C 1.1277(8) -0.0964(4) 0.0902(5) 0.162(4) Uani 1 1 d . . . H2T1 H 1.1888 -0.1207 0.0822 0.243 Uiso 1 1 calc R . . H2T2 H 1.0707 -0.1095 0.1178 0.243 Uiso 1 1 calc R . . H2T3 H 1.1721 -0.0689 0.1106 0.243 Uiso 1 1 calc R . . O1W O 0.9234(8) 0.0116(5) 0.2199(6) 0.254(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 C11 0.128(5) 0.059(3) 0.077(3) -0.016(3) 0.046(4) -0.002(3) C12 0.117(6) 0.113(6) 0.197(9) -0.027(6) 0.067(7) 0.010(5) C13 0.233(9) 0.077(4) 0.138(6) -0.045(4) 0.106(7) -0.006(5) C14 0.282(11) 0.091(5) 0.075(4) -0.001(4) 0.075(6) -0.014(6) O1 0.121(3) 0.0461(18) 0.072(2) -0.0193(16) 0.041(2) -0.0034(18) C10' 0.083(3) 0.041(2) 0.046(2) -0.0022(19) 0.007(2) 0.003(2) O10 0.093(2) 0.0349(16) 0.0610(18) -0.0056(13) 0.0180(16) -0.0029(15) N11 0.080(3) 0.0326(17) 0.060(2) -0.0043(16) 0.0156(19) 0.0003(17) C11A 0.062(3) 0.036(2) 0.064(3) -0.0045(19) 0.007(2) 0.0055(19) C11B 0.072(3) 0.044(2) 0.082(3) -0.013(2) 0.024(3) -0.007(2) C11C 0.084(4) 0.062(3) 0.124(5) -0.012(3) 0.049(4) -0.009(3) C11D 0.112(6) 0.198(10) 0.219(11) -0.038(9) 0.032(7) 0.060(7) C11E 0.247(11) 0.119(7) 0.191(9) 0.004(6) 0.153(9) -0.001(7) C11' 0.061(3) 0.033(2) 0.048(2) -0.0031(17) 0.016(2) 0.0043(18) O11 0.0675(18) 0.0326(15) 0.0674(19) -0.0032(13) 0.0153(15) 0.0061(13) N12 0.068(2) 0.0311(17) 0.0491(19) -0.0028(14) 0.0109(17) 0.0040(16) C12A 0.066(3) 0.045(2) 0.047(2) -0.0109(19) 0.008(2) -0.001(2) C12B 0.087(4) 0.067(3) 0.058(3) -0.017(2) -0.003(2) 0.011(3) C12C 0.085(4) 0.119(5) 0.096(4) -0.029(4) -0.013(3) 0.005(4) C12D 0.172(7) 0.073(4) 0.061(3) 0.007(3) -0.016(4) 0.021(4) C12' 0.065(3) 0.044(2) 0.056(3) -0.014(2) 0.010(2) -0.002(2) O12 0.127(3) 0.057(2) 0.077(2) -0.0218(18) 0.031(2) -0.024(2) N13 0.064(2) 0.0358(18) 0.064(2) -0.0023(16) 0.0125(18) 0.0044(16) C13A 0.063(3) 0.046(2) 0.064(3) -0.003(2) 0.017(2) -0.012(2) C13B 0.074(3) 0.064(3) 0.091(4) -0.010(3) 0.038(3) -0.007(3) C13C 0.067(4) 0.132(6) 0.133(6) -0.012(5) 0.037(4) 0.007(4) C13D 0.141(6) 0.104(5) 0.120(5) 0.012(4) 0.084(5) -0.004(4) C13' 0.065(3) 0.040(2) 0.047(2) -0.0029(18) 0.022(2) -0.006(2) O13 0.076(2) 0.0358(16) 0.073(2) -0.0033(14) 0.0222(16) -0.0082(14) N14 0.069(2) 0.0300(16) 0.054(2) -0.0031(15) 0.0171(17) -0.0006(16) C14A 0.065(3) 0.038(2) 0.040(2) 0.0023(17) 0.0077(18) -0.0023(19) C14B 0.093(4) 0.051(3) 0.053(3) 0.002(2) 0.014(2) 0.008(2) C14C 0.075(3) 0.043(2) 0.066(3) -0.003(2) -0.005(2) -0.001(2) C14D 0.111(4) 0.062(3) 0.071(3) -0.016(3) -0.007(3) -0.010(3) C14E 0.160(6) 0.080(4) 0.063(4) -0.028(3) -0.011(4) 0.005(4) C14F 0.135(5) 0.083(4) 0.048(3) -0.007(3) 0.017(3) 0.014(4) C14' 0.058(3) 0.034(2) 0.047(2) 0.0022(17) 0.0073(18) -0.0016(18) O14 0.085(2) 0.0337(15) 0.0527(17) 0.0032(13) 0.0068(15) 0.0066(14) N15 0.059(2) 0.0347(17) 0.0462(19) 0.0028(14) 0.0093(15) 0.0063(15) C15A 0.052(2) 0.046(2) 0.048(2) 0.0024(18) 0.0094(18) 0.0074(18) C15B 0.081(3) 0.055(3) 0.062(3) -0.002(2) 0.031(2) -0.010(2) C15C 0.113(4) 0.059(3) 0.055(3) 0.015(2) 0.021(3) 0.012(3) C15D 0.112(5) 0.086(4) 0.111(5) -0.010(4) 0.036(4) -0.036(4) C15' 0.066(3) 0.039(2) 0.038(2) 0.0056(17) 0.0085(18) -0.0010(19) O15 0.093(2) 0.0494(18) 0.080(2) -0.0180(17) 0.0346(19) 0.0000(17) N16 0.061(2) 0.0364(17) 0.0436(18) -0.0026(14) 0.0115(16) 0.0018(15) C16A 0.065(3) 0.041(2) 0.039(2) -0.0031(17) 0.0011(18) -0.0016(19) C16B 0.065(3) 0.057(3) 0.062(3) 0.013(2) -0.004(2) -0.005(2) C16C 0.093(4) 0.083(4) 0.079(4) 0.031(3) -0.022(3) -0.021(3) C16D 0.223(10) 0.184(9) 0.059(4) 0.012(5) -0.021(5) -0.007(8) C16E 0.115(6) 0.155(8) 0.180(8) 0.087(7) -0.053(6) 0.006(5) C16' 0.059(3) 0.035(2) 0.052(2) -0.0002(18) 0.003(2) 0.0019(19) O16 0.095(2) 0.0387(17) 0.072(2) 0.0073(15) -0.0151(18) -0.0115(17) N17 0.067(2) 0.0442(19) 0.0499(19) 0.0116(16) -0.0010(16) -0.0145(17) C17A 0.071(3) 0.037(2) 0.051(2) 0.0130(18) 0.005(2) -0.011(2) C17B 0.088(4) 0.054(3) 0.055(3) 0.007(2) 0.018(2) -0.010(2) C17C 0.098(4) 0.085(4) 0.095(4) 0.014(3) 0.034(3) 0.005(3) C17D 0.143(5) 0.084(4) 0.050(3) 0.014(3) 0.018(3) -0.003(4) C17' 0.075(3) 0.038(2) 0.047(2) 0.0059(18) -0.002(2) -0.012(2) O17 0.094(2) 0.0376(17) 0.093(2) 0.0200(16) -0.0153(19) -0.0085(16) N18 0.063(2) 0.045(2) 0.087(3) 0.0187(19) 0.000(2) -0.0007(18) C18A 0.068(3) 0.055(3) 0.121(5) 0.025(3) 0.009(3) 0.007(3) C18B 0.082(4) 0.087(4) 0.140(6) 0.007(4) -0.031(4) -0.006(3) C18C 0.173(9) 0.262(14) 0.103(6) -0.020(8) -0.012(6) -0.068(10) C18D 0.132(7) 0.086(5) 0.252(11) -0.013(6) -0.074(7) -0.008(5) C18' 0.066(4) 0.088(4) 0.157(7) 0.026(4) 0.008(4) 0.011(3) O18 0.114(4) 0.215(7) 0.212(7) 0.057(6) 0.052(4) 0.074(5) C1TM 0.149(8) 0.258(13) 0.173(9) 0.069(9) 0.103(7) 0.037(9) O1TM 0.088(3) 0.140(4) 0.146(4) 0.046(4) 0.043(3) 0.026(3) C21 0.176(7) 0.064(4) 0.069(4) 0.016(3) -0.016(4) 0.002(4) C22 0.173(10) 0.113(7) 0.237(13) 0.023(8) -0.054(10) 0.019(7) C23 0.372(18) 0.084(5) 0.132(7) 0.053(5) -0.093(9) -0.023(8) C24 0.42(2) 0.137(8) 0.068(5) -0.026(5) 0.028(7) 0.036(10) O2 0.165(4) 0.049(2) 0.071(2) 0.0150(18) 0.001(3) 0.001(2) C20' 0.100(4) 0.038(3) 0.063(3) 0.009(2) 0.038(3) 0.011(2) O20 0.091(2) 0.0413(18) 0.072(2) 0.0057(15) 0.0221(17) 0.0027(16) N21 0.093(3) 0.0318(18) 0.073(3) -0.0001(18) 0.021(2) 0.0016(19) C21A 0.066(3) 0.045(3) 0.092(4) 0.006(2) 0.016(3) 0.006(2) C21B 0.093(4) 0.068(4) 0.156(6) 0.028(4) -0.035(4) -0.016(3) C21C 0.169(10) 0.122(7) 0.276(16) 0.046(9) -0.083(11) -0.049(7) C21D 0.34(2) 0.273(18) 0.53(3) 0.15(2) -0.32(2) -0.164(16) C21E 0.209(15) 0.33(2) 0.219(14) 0.041(16) -0.036(12) 0.050(16) C21' 0.068(3) 0.038(2) 0.059(3) -0.0019(19) 0.004(2) 0.010(2) O21 0.082(2) 0.0428(17) 0.078(2) 0.0077(16) 0.0046(17) 0.0118(16) N22 0.075(3) 0.0412(19) 0.063(2) 0.0080(17) 0.0209(19) 0.0097(18) C22A 0.091(4) 0.056(3) 0.064(3) 0.011(2) 0.024(3) 0.009(3) C22B 0.102(4) 0.082(4) 0.091(4) 0.008(3) 0.048(3) 0.005(3) C22C 0.137(7) 0.147(7) 0.195(9) 0.023(7) 0.098(7) -0.002(6) C22D 0.159(7) 0.111(5) 0.117(6) -0.002(5) 0.061(5) 0.017(5) C22' 0.081(3) 0.057(3) 0.079(4) 0.015(3) 0.024(3) -0.001(3) O22 0.160(4) 0.055(2) 0.092(3) 0.027(2) 0.015(3) -0.016(2) N23 0.058(2) 0.048(2) 0.080(3) 0.0177(19) 0.0174(19) 0.0060(17) C23A 0.051(3) 0.056(3) 0.074(3) 0.012(2) 0.007(2) -0.006(2) C23B 0.064(3) 0.076(3) 0.091(4) 0.016(3) -0.009(3) -0.007(3) C23C 0.126(6) 0.103(5) 0.103(5) 0.010(4) -0.033(4) -0.012(4) C23D 0.064(4) 0.143(6) 0.153(7) 0.025(5) -0.010(4) 0.019(4) C23' 0.056(3) 0.045(2) 0.047(2) 0.0042(18) 0.0019(19) -0.004(2) O23 0.0686(19) 0.0434(18) 0.073(2) 0.0072(15) 0.0027(15) -0.0066(14) N24 0.054(2) 0.0334(17) 0.057(2) 0.0056(15) 0.0104(16) 0.0029(15) C24A 0.058(3) 0.041(2) 0.051(2) -0.0002(18) 0.0180(19) 0.0034(19) C24B 0.085(3) 0.054(3) 0.051(3) 0.002(2) 0.010(2) 0.010(2) C24C 0.112(4) 0.079(4) 0.052(3) 0.011(3) 0.016(3) 0.013(3) C24D 0.107(4) 0.086(4) 0.071(4) 0.028(3) 0.034(3) 0.012(3) C24E 0.078(3) 0.055(3) 0.084(4) 0.014(3) 0.033(3) 0.002(2) C24F 0.055(3) 0.051(2) 0.065(3) 0.005(2) 0.022(2) 0.001(2) C24' 0.046(2) 0.041(2) 0.052(2) -0.0006(18) 0.0108(18) -0.0013(18) O24 0.0717(19) 0.0443(16) 0.0539(17) 0.0007(13) 0.0113(14) 0.0101(14) N25 0.055(2) 0.0341(17) 0.0474(19) -0.0016(14) 0.0046(15) 0.0042(15) C25A 0.056(2) 0.045(2) 0.053(2) -0.0011(19) 0.0047(19) 0.0031(19) C25B 0.084(3) 0.055(3) 0.062(3) -0.002(2) -0.013(3) -0.005(2) C25C 0.116(4) 0.062(3) 0.057(3) -0.014(2) 0.010(3) 0.007(3) C25D 0.108(5) 0.068(4) 0.112(5) -0.016(3) -0.016(4) -0.019(3) C25' 0.071(3) 0.038(2) 0.043(2) -0.0017(18) 0.008(2) 0.004(2) O25 0.088(2) 0.0566(19) 0.074(2) 0.0220(17) -0.0106(18) -0.0024(17) N26 0.061(2) 0.0375(18) 0.0462(18) 0.0036(15) 0.0085(17) 0.0023(16) C26A 0.067(3) 0.044(2) 0.053(2) 0.0071(19) 0.019(2) -0.001(2) C26B 0.065(3) 0.059(3) 0.077(3) -0.012(2) 0.023(2) -0.007(2) C26C 0.080(4) 0.101(4) 0.110(5) -0.042(4) 0.043(3) -0.019(3) C26D 0.179(9) 0.202(10) 0.092(5) -0.002(6) 0.063(5) 0.009(8) C26E 0.107(5) 0.135(7) 0.192(8) -0.053(6) 0.076(6) 0.008(5) C26' 0.068(3) 0.034(2) 0.062(3) 0.0013(19) 0.019(2) 0.001(2) O26 0.095(3) 0.0431(18) 0.119(3) -0.0175(19) 0.051(2) -0.0128(18) N27 0.065(2) 0.0440(19) 0.056(2) -0.0121(16) 0.0138(18) -0.0118(17) C27A 0.067(3) 0.042(2) 0.061(3) -0.013(2) 0.014(2) -0.013(2) C27B 0.090(4) 0.054(3) 0.063(3) -0.011(2) 0.001(3) -0.010(3) C27C 0.117(6) 0.090(4) 0.094(4) -0.020(4) -0.019(4) 0.019(4) C27D 0.153(6) 0.084(4) 0.057(3) -0.015(3) 0.014(3) -0.003(4) C27' 0.084(3) 0.043(3) 0.054(3) -0.007(2) 0.024(2) -0.005(2) O27 0.101(3) 0.046(2) 0.112(3) -0.0144(19) 0.040(2) -0.0021(18) N28 0.070(3) 0.048(2) 0.091(3) -0.019(2) 0.009(2) -0.003(2) C28A 0.075(3) 0.070(3) 0.070(3) -0.007(3) 0.008(3) 0.004(3) C28B 0.089(4) 0.127(6) 0.088(4) 0.019(4) 0.019(3) 0.001(4) C28C 0.105(5) 0.102(5) 0.163(8) 0.030(5) 0.030(5) -0.012(4) C28D 0.156(7) 0.252(12) 0.086(5) 0.050(7) 0.017(5) 0.011(8) C28' 0.087(4) 0.099(5) 0.093(5) 0.019(4) 0.028(4) -0.012(4) O28 0.153(5) 0.203(6) 0.093(3) 0.033(4) 0.014(3) 0.040(5) O2TM 0.096(3) 0.127(4) 0.135(4) 0.047(3) 0.009(3) 0.024(3) C2TM 0.102(5) 0.208(10) 0.173(8) 0.125(8) 0.005(5) 0.029(6) O1W 0.147(6) 0.292(12) 0.309(12) 0.046(10) -0.016(7) -0.010(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C14 1.498(9) . ? C11 O1 1.465(7) . ? C11 C12 1.509(11) . ? C11 C13 1.520(8) . ? O1 C10' 1.317(5) . ? C10' O10 1.217(5) . ? C10' N11 1.342(6) . ? N11 C11A 1.462(5) . ? C11A C11' 1.503(6) . ? C11A C11B 1.540(6) . ? C11B C11C 1.542(7) . ? C11C C11D 1.451(11) . ? C11C C11E 1.550(11) . ? C11' O11 1.235(4) . ? C11' N12 1.340(5) . ? N12 C12A 1.445(5) . ? C12A C12' 1.536(6) . ? C12A C12B 1.535(7) . ? C12B C12C 1.538(8) . ? C12B C12D 1.516(9) . ? C12' O12 1.220(5) . ? C12' N13 1.336(6) . ? N13 C13A 1.458(5) . ? C13A C13' 1.530(6) . ? C13A C13B 1.539(7) . ? C13B C13C 1.490(8) . ? C13B C13D 1.527(9) . ? C13' O13 1.227(5) . ? C13' N14 1.337(5) . ? N14 C14A 1.469(5) . ? C14A C14' 1.542(6) . ? C14A C14C 1.536(6) . ? C14A C14B 1.544(6) . ? C14B C14F 1.523(7) . ? C14C C14D 1.506(7) . ? C14D C14E 1.499(9) . ? C14E C14F 1.513(9) . ? C14' O14 1.224(5) . ? C14' N15 1.342(5) . ? N15 C15A 1.462(5) . ? C15A C15' 1.512(6) . ? C15A C15B 1.528(6) . ? C15B C15D 1.525(8) . ? C15B C15C 1.484(7) . ? C15' O15 1.222(5) . ? C15' N16 1.335(5) . ? N16 C16A 1.457(5) . ? C16A C16' 1.526(6) . ? C16A C16B 1.521(6) . ? C16B C16C 1.514(7) . ? C16C C16E 1.505(11) . ? C16C C16D 1.460(11) . ? C16' O16 1.221(5) . ? C16' N17 1.324(5) . ? N17 C17A 1.469(5) . ? C17A C17' 1.501(7) . ? C17A C17B 1.546(7) . ? C17B C17C 1.499(8) . ? C17B C17D 1.533(7) . ? C17' O17 1.222(5) . ? C17' N18 1.326(6) . ? N18 C18A 1.445(7) . ? C18A C18' 1.491(10) . ? C18A C18B 1.566(9) . ? C18B C18D 1.470(10) . ? C18B C18C 1.469(12) . ? C18' O18 1.205(8) . ? C18' O1TM 1.289(8) . ? C1TM O1TM 1.498(9) . ? C21 O2 1.398(8) . ? C21 C24 1.506(11) . ? C21 C22 1.519(14) . ? C21 C23 1.536(9) . ? O2 C20' 1.325(6) . ? C20' O20 1.238(6) . ? C20' N21 1.320(7) . ? N21 C21A 1.429(6) . ? C21A C21' 1.511(7) . ? C21A C21B 1.509(8) . ? C21B C21C 1.463(12) . ? C21C C21D 1.511(16) . ? C21C C21E 1.5516(11) . ? C21' O21 1.225(5) . ? C21' N22 1.327(6) . ? N22 C22A 1.459(6) . ? C22A C22' 1.504(8) . ? C22A C22B 1.544(8) . ? C22B C22D 1.531(10) . ? C22B C22C 1.508(10) . ? C22' O22 1.208(6) . ? C22' N23 1.363(7) . ? N23 C23A 1.453(6) . ? C23A C23B 1.517(7) . ? C23A C23' 1.536(6) . ? C23B C23C 1.530(9) . ? C23B C23D 1.569(9) . ? C23' O23 1.216(5) . ? C23' N24 1.336(5) . ? N24 C24A 1.465(5) . ? C24A C24' 1.525(6) . ? C24A C24B 1.534(6) . ? C24A C24F 1.550(6) . ? C24B C24C 1.540(7) . ? C24C C24D 1.533(8) . ? C24D C24E 1.511(8) . ? C24E C24F 1.537(6) . ? C24' O24 1.236(5) . ? C24' N25 1.335(5) . ? N25 C25A 1.467(5) . ? C25A C25' 1.511(6) . ? C25A C25B 1.551(6) . ? C25B C25D 1.532(8) . ? C25B C25C 1.494(8) . ? C25' O25 1.224(5) . ? C25' N26 1.327(6) . ? N26 C26A 1.437(5) . ? C26A C26' 1.525(6) . ? C26A C26B 1.508(7) . ? C26B C26C 1.535(7) . ? C26C C26E 1.487(10) . ? C26C C26D 1.499(11) . ? C26' O26 1.227(5) . ? C26' N27 1.329(6) . ? N27 C27A 1.449(5) . ? C27A C27' 1.513(7) . ? C27A C27B 1.533(7) . ? C27B C27C 1.517(9) . ? C27B C27D 1.546(7) . ? C27' O27 1.235(5) . ? C27' N28 1.330(6) . ? N28 C28A 1.434(6) . ? C28A C28' 1.475(8) . ? C28A C28B 1.546(9) . ? C28B C28C 1.469(11) . ? C28B C28D 1.518(10) . ? C28' O28 1.2096(10) . ? C28' O2TM 1.314(7) . ? O2TM C2TM 1.374(9) . ? 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 C14 C11 O1 111.7(6) . . ? C14 C11 C12 112.4(7) . . ? O1 C11 C12 107.5(5) . . ? C14 C11 C13 111.6(6) . . ? O1 C11 C13 102.2(5) . . ? C12 C11 C13 110.9(7) . . ? C10' O1 C11 122.5(4) . . ? O10 C10' N11 124.7(4) . . ? O10 C10' O1 125.4(4) . . ? N11 C10' O1 109.9(4) . . ? C10' N11 C11A 122.0(3) . . ? N11 C11A C11' 113.7(4) . . ? N11 C11A C11B 108.3(3) . . ? C11' C11A C11B 109.5(4) . . ? C11A C11B C11C 114.8(4) . . ? C11D C11C C11B 113.2(6) . . ? C11D C11C C11E 108.4(7) . . ? C11B C11C C11E 108.3(5) . . ? O11 C11' N12 121.6(4) . . ? O11 C11' C11A 120.2(4) . . ? N12 C11' C11A 118.2(3) . . ? C11' N12 C12A 120.0(3) . . ? N12 C12A C12' 112.0(3) . . ? N12 C12A C12B 109.5(3) . . ? C12' C12A C12B 112.7(4) . . ? C12A C12B C12C 111.9(4) . . ? C12A C12B C12D 109.7(5) . . ? C12C C12B C12D 111.7(5) . . ? O12 C12' N13 122.4(4) . . ? O12 C12' C12A 120.4(4) . . ? N13 C12' C12A 117.2(4) . . ? C12' N13 C13A 120.1(4) . . ? N13 C13A C13' 111.2(3) . . ? N13 C13A C13B 111.2(4) . . ? C13' C13A C13B 111.4(4) . . ? C13C C13B C13D 111.4(5) . . ? C13C C13B C13A 111.6(5) . . ? C13D C13B C13A 110.7(4) . . ? O13 C13' N14 122.5(4) . . ? O13 C13' C13A 120.6(4) . . ? N14 C13' C13A 116.9(4) . . ? C13' N14 C14A 121.4(3) . . ? N14 C14A C14' 109.3(3) . . ? N14 C14A C14C 109.4(3) . . ? C14' C14A C14C 108.5(3) . . ? N14 C14A C14B 110.3(4) . . ? C14' C14A C14B 110.4(3) . . ? C14C C14A C14B 108.9(4) . . ? C14F C14B C14A 110.8(4) . . ? C14D C14C C14A 115.1(4) . . ? C14E C14D C14C 111.4(4) . . ? C14D C14E C14F 111.1(5) . . ? C14E C14F C14B 111.4(5) . . ? O14 C14' N15 121.8(4) . . ? O14 C14' C14A 121.7(3) . . ? N15 C14' C14A 116.3(3) . . ? C14' N15 C15A 120.4(3) . . ? N15 C15A C15' 113.9(3) . . ? N15 C15A C15B 112.8(3) . . ? C15' C15A C15B 111.0(3) . . ? C15D C15B C15C 111.2(5) . . ? C15D C15B C15A 112.0(4) . . ? C15C C15B C15A 113.9(4) . . ? O15 C15' N16 123.0(4) . . ? O15 C15' C15A 118.9(4) . . ? N16 C15' C15A 118.2(4) . . ? C15' N16 C16A 123.1(3) . . ? N16 C16A C16' 112.4(3) . . ? N16 C16A C16B 111.5(3) . . ? C16' C16A C16B 110.9(4) . . ? C16C C16B C16A 115.6(4) . . ? C16E C16C C16D 110.7(7) . . ? C16E C16C C16B 109.9(6) . . ? C16D C16C C16B 111.1(6) . . ? O16 C16' N17 123.4(4) . . ? O16 C16' C16A 119.3(4) . . ? N17 C16' C16A 117.4(4) . . ? C16' N17 C17A 123.3(3) . . ? C17' C17A N17 112.6(4) . . ? C17' C17A C17B 113.1(4) . . ? N17 C17A C17B 109.7(3) . . ? C17C C17B C17D 110.7(5) . . ? C17C C17B C17A 111.2(4) . . ? C17D C17B C17A 109.6(4) . . ? O17 C17' N18 121.9(4) . . ? O17 C17' C17A 121.3(4) . . ? N18 C17' C17A 116.8(4) . . ? C17' N18 C18A 123.3(4) . . ? N18 C18A C18' 113.2(5) . . ? N18 C18A C18B 113.0(5) . . ? C18' C18A C18B 112.0(5) . . ? C18D C18B C18C 111.1(10) . . ? C18D C18B C18A 113.6(6) . . ? C18C C18B C18A 109.0(6) . . ? O18 C18' O1TM 122.8(8) . . ? O18 C18' C18A 121.7(7) . . ? O1TM C18' C18A 115.5(6) . . ? C18' O1TM C1TM 117.0(7) . . ? O2 C21 C24 113.0(8) . . ? O2 C21 C22 104.1(6) . . ? C24 C21 C22 113.3(8) . . ? O2 C21 C23 101.2(6) . . ? C24 C21 C23 112.1(8) . . ? C22 C21 C23 112.2(9) . . ? C20' O2 C21 125.0(4) . . ? O20 C20' N21 124.4(4) . . ? O20 C20' O2 124.0(5) . . ? N21 C20' O2 111.5(4) . . ? C20' N21 C21A 122.1(4) . . ? N21 C21A C21' 113.7(4) . . ? N21 C21A C21B 107.2(4) . . ? C21' C21A C21B 111.3(5) . . ? C21C C21B C21A 116.4(7) . . ? C21B C21C C21D 108.5(10) . . ? C21B C21C C21E 114.3(11) . . ? C21D C21C C21E 102.3(15) . . ? O21 C21' N22 122.5(4) . . ? O21 C21' C21A 119.7(4) . . ? N22 C21' C21A 117.8(4) . . ? C21' N22 C22A 118.7(4) . . ? N22 C22A C22' 112.4(4) . . ? N22 C22A C22B 109.4(4) . . ? C22' C22A C22B 113.2(5) . . ? C22D C22B C22A 109.7(6) . . ? C22D C22B C22C 108.7(6) . . ? C22A C22B C22C 108.6(5) . . ? O22 C22' N23 121.7(5) . . ? O22 C22' C22A 121.4(5) . . ? N23 C22' C22A 116.8(4) . . ? C22' N23 C23A 119.5(4) . . ? N23 C23A C23B 110.3(4) . . ? N23 C23A C23' 111.6(4) . . ? C23B C23A C23' 111.2(4) . . ? C23C C23B C23A 111.3(5) . . ? C23C C23B C23D 112.3(5) . . ? C23A C23B C23D 109.1(5) . . ? O23 C23' N24 123.1(4) . . ? O23 C23' C23A 120.1(4) . . ? N24 C23' C23A 116.7(4) . . ? C23' N24 C24A 121.2(3) . . ? N24 C24A C24' 110.2(3) . . ? N24 C24A C24B 110.4(4) . . ? C24' C24A C24B 110.2(3) . . ? N24 C24A C24F 109.5(3) . . ? C24' C24A C24F 106.7(3) . . ? C24B C24A C24F 109.8(4) . . ? C24A C24B C24C 110.8(4) . . ? C24D C24C C24B 111.6(5) . . ? C24C C24D C24E 110.0(4) . . ? C24F C24E C24D 111.5(4) . . ? C24E C24F C24A 113.2(4) . . ? O24 C24' N25 121.2(4) . . ? O24 C24' C24A 122.1(4) . . ? N25 C24' C24A 116.6(3) . . ? C24' N25 C25A 120.5(3) . . ? N25 C25A C25' 114.0(3) . . ? N25 C25A C25B 111.6(3) . . ? C25' C25A C25B 110.9(4) . . ? C25D C25B C25A 110.1(4) . . ? C25D C25B C25C 114.1(5) . . ? C25A C25B C25C 113.4(4) . . ? O25 C25' N26 122.7(4) . . ? O25 C25' C25A 119.5(4) . . ? N26 C25' C25A 117.7(4) . . ? C25' N26 C26A 123.7(3) . . ? N26 C26A C26' 112.8(3) . . ? N26 C26A C26B 111.6(4) . . ? C26' C26A C26B 110.9(4) . . ? C26C C26B C26A 115.2(5) . . ? C26E C26C C26D 109.1(6) . . ? C26E C26C C26B 111.3(6) . . ? C26D C26C C26B 112.3(6) . . ? O26 C26' N27 122.9(4) . . ? O26 C26' C26A 119.6(4) . . ? N27 C26' C26A 117.5(4) . . ? C26' N27 C27A 123.4(4) . . ? C27' C27A N27 112.0(4) . . ? C27' C27A C27B 112.9(4) . . ? N27 C27A C27B 111.2(4) . . ? C27C C27B C27A 109.9(5) . . ? C27C C27B C27D 111.2(5) . . ? C27A C27B C27D 111.2(4) . . ? O27 C27' N28 121.6(5) . . ? O27 C27' C27A 120.6(4) . . ? N28 C27' C27A 117.6(4) . . ? C27' N28 C28A 122.1(4) . . ? N28 C28A C28' 113.0(5) . . ? N28 C28A C28B 112.6(5) . . ? C28' C28A C28B 108.9(5) . . ? C28C C28B C28D 111.7(8) . . ? C28C C28B C28A 113.3(6) . . ? C28D C28B C28A 110.4(6) . . ? O28 C28' O2TM 122.1(7) . . ? O28 C28' C28A 122.9(6) . . ? O2TM C28' C28A 114.9(6) . . ? C28' O2TM C2TM 122.1(7) . . ? 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 C14 C11 O1 C10' -60.5(7) . . . . ? C12 C11 O1 C10' 63.3(7) . . . . ? C13 C11 O1 C10' -179.9(6) . . . . ? C11 O1 C10' O10 11.3(8) . . . . ? C11 O1 C10' N11 -169.5(5) . . . . ? O10 C10' N11 C11A 6.3(7) . . . . ? O1 C10' N11 C11A -172.9(4) . . . . ? C10' N11 C11A C11' -45.9(5) . . . . ? C10' N11 C11A C11B -167.9(4) . . . . ? N11 C11A C11B C11C -175.0(4) . . . . ? C11' C11A C11B C11C 60.5(6) . . . . ? C11A C11B C11C C11D 76.0(8) . . . . ? C11A C11B C11C C11E -163.8(6) . . . . ? N11 C11A C11' O11 138.2(4) . . . . ? C11B C11A C11' O11 -100.4(5) . . . . ? N11 C11A C11' N12 -45.6(5) . . . . ? C11B C11A C11' N12 75.7(5) . . . . ? O11 C11' N12 C12A 0.3(6) . . . . ? C11A C11' N12 C12A -175.8(4) . . . . ? C11' N12 C12A C12' -58.1(5) . . . . ? C11' N12 C12A C12B 176.2(4) . . . . ? N12 C12A C12B C12C 167.4(4) . . . . ? C12' C12A C12B C12C 42.1(6) . . . . ? N12 C12A C12B C12D -68.0(5) . . . . ? C12' C12A C12B C12D 166.7(4) . . . . ? N12 C12A C12' O12 142.1(5) . . . . ? C12B C12A C12' O12 -93.9(5) . . . . ? N12 C12A C12' N13 -40.4(5) . . . . ? C12B C12A C12' N13 83.6(5) . . . . ? O12 C12' N13 C13A -7.8(7) . . . . ? C12A C12' N13 C13A 174.7(4) . . . . ? C12' N13 C13A C13' -70.1(5) . . . . ? C12' N13 C13A C13B 165.1(4) . . . . ? N13 C13A C13B C13C -61.1(6) . . . . ? C13' C13A C13B C13C 174.2(4) . . . . ? N13 C13A C13B C13D 174.3(5) . . . . ? C13' C13A C13B C13D 49.6(6) . . . . ? N13 C13A C13' O13 134.1(4) . . . . ? C13B C13A C13' O13 -101.2(5) . . . . ? N13 C13A C13' N14 -47.6(5) . . . . ? C13B C13A C13' N14 77.1(5) . . . . ? O13 C13' N14 C14A 4.0(6) . . . . ? C13A C13' N14 C14A -174.3(3) . . . . ? C13' N14 C14A C14' -50.0(5) . . . . ? C13' N14 C14A C14C -168.7(4) . . . . ? C13' N14 C14A C14B 71.5(5) . . . . ? N14 C14A C14B C14F 66.6(5) . . . . ? C14' C14A C14B C14F -172.6(4) . . . . ? C14C C14A C14B C14F -53.5(6) . . . . ? N14 C14A C14C C14D -69.0(5) . . . . ? C14' C14A C14C C14D 171.8(4) . . . . ? C14B C14A C14C C14D 51.6(5) . . . . ? C14A C14C C14D C14E -52.3(7) . . . . ? C14C C14D C14E C14F 53.9(7) . . . . ? C14D C14E C14F C14B -58.3(7) . . . . ? C14A C14B C14F C14E 58.6(6) . . . . ? N14 C14A C14' O14 135.9(4) . . . . ? C14C C14A C14' O14 -104.9(4) . . . . ? C14B C14A C14' O14 14.4(6) . . . . ? N14 C14A C14' N15 -48.4(5) . . . . ? C14C C14A C14' N15 70.8(5) . . . . ? C14B C14A C14' N15 -169.9(4) . . . . ? O14 C14' N15 C15A 4.6(6) . . . . ? C14A C14' N15 C15A -171.1(4) . . . . ? C14' N15 C15A C15' -74.8(5) . . . . ? C14' N15 C15A C15B 157.5(4) . . . . ? N15 C15A C15B C15D -61.3(5) . . . . ? C15' C15A C15B C15D 169.5(4) . . . . ? N15 C15A C15B C15C 65.9(5) . . . . ? C15' C15A C15B C15C -63.3(5) . . . . ? N15 C15A C15' O15 168.5(4) . . . . ? C15B C15A C15' O15 -62.9(5) . . . . ? N15 C15A C15' N16 -12.2(5) . . . . ? C15B C15A C15' N16 116.4(4) . . . . ? O15 C15' N16 C16A -8.3(6) . . . . ? C15A C15' N16 C16A 172.5(3) . . . . ? C15' N16 C16A C16' -91.2(4) . . . . ? C15' N16 C16A C16B 143.6(4) . . . . ? N16 C16A C16B C16C -67.3(5) . . . . ? C16' C16A C16B C16C 166.6(4) . . . . ? C16A C16B C16C C16E 168.0(6) . . . . ? C16A C16B C16C C16D -69.1(7) . . . . ? N16 C16A C16' O16 174.5(4) . . . . ? C16B C16A C16' O16 -60.0(5) . . . . ? N16 C16A C16' N17 -4.7(5) . . . . ? C16B C16A C16' N17 120.9(4) . . . . ? O16 C16' N17 C17A 1.2(7) . . . . ? C16A C16' N17 C17A -179.6(4) . . . . ? C16' N17 C17A C17' -108.7(5) . . . . ? C16' N17 C17A C17B 124.5(5) . . . . ? C17' C17A C17B C17C 173.2(4) . . . . ? N17 C17A C17B C17C -60.2(5) . . . . ? C17' C17A C17B C17D 50.4(5) . . . . ? N17 C17A C17B C17D 176.9(4) . . . . ? N17 C17A C17' O17 135.4(4) . . . . ? C17B C17A C17' O17 -99.5(5) . . . . ? N17 C17A C17' N18 -46.2(5) . . . . ? C17B C17A C17' N18 78.9(5) . . . . ? O17 C17' N18 C18A 0.7(7) . . . . ? C17A C17' N18 C18A -177.6(5) . . . . ? C17' N18 C18A C18' -119.3(6) . . . . ? C17' N18 C18A C18B 112.1(6) . . . . ? N18 C18A C18B C18D 60.3(9) . . . . ? C18' C18A C18B C18D -68.9(9) . . . . ? N18 C18A C18B C18C -64.1(8) . . . . ? C18' C18A C18B C18C 166.6(8) . . . . ? N18 C18A C18' O18 168.3(7) . . . . ? C18B C18A C18' O18 -62.5(9) . . . . ? N18 C18A C18' O1TM -11.5(8) . . . . ? C18B C18A C18' O1TM 117.7(6) . . . . ? O18 C18' O1TM C1TM -2.2(12) . . . . ? C18A C18' O1TM C1TM 177.6(8) . . . . ? C24 C21 O2 C20' -52.9(10) . . . . ? C22 C21 O2 C20' 70.4(8) . . . . ? C23 C21 O2 C20' -173.0(8) . . . . ? C21 O2 C20' O20 -0.9(9) . . . . ? C21 O2 C20' N21 -179.3(6) . . . . ? O20 C20' N21 C21A 8.1(8) . . . . ? O2 C20' N21 C21A -173.6(4) . . . . ? C20' N21 C21A C21' -51.3(6) . . . . ? C20' N21 C21A C21B -174.8(5) . . . . ? N21 C21A C21B C21C -178.8(9) . . . . ? C21' C21A C21B C21C 56.3(10) . . . . ? C21A C21B C21C C21D 153.9(13) . . . . ? C21A C21B C21C C21E -92.6(15) . . . . ? N21 C21A C21' O21 140.8(4) . . . . ? C21B C21A C21' O21 -98.0(6) . . . . ? N21 C21A C21' N22 -41.1(6) . . . . ? C21B C21A C21' N22 80.1(6) . . . . ? O21 C21' N22 C22A 0.9(7) . . . . ? C21A C21' N22 C22A -177.2(4) . . . . ? C21' N22 C22A C22' -59.2(6) . . . . ? C21' N22 C22A C22B 174.0(5) . . . . ? N22 C22A C22B C22D -68.7(6) . . . . ? C22' C22A C22B C22D 165.0(5) . . . . ? N22 C22A C22B C22C 172.6(6) . . . . ? C22' C22A C22B C22C 46.3(8) . . . . ? N22 C22A C22' O22 142.3(5) . . . . ? C22B C22A C22' O22 -93.0(7) . . . . ? N22 C22A C22' N23 -38.7(6) . . . . ? C22B C22A C22' N23 86.0(6) . . . . ? O22 C22' N23 C23A -5.7(7) . . . . ? C22A C22' N23 C23A 175.3(4) . . . . ? C22' N23 C23A C23B 165.9(4) . . . . ? C22' N23 C23A C23' -69.9(5) . . . . ? N23 C23A C23B C23C 173.0(5) . . . . ? C23' C23A C23B C23C 48.7(6) . . . . ? N23 C23A C23B C23D -62.5(6) . . . . ? C23' C23A C23B C23D 173.1(5) . . . . ? N23 C23A C23' O23 134.3(4) . . . . ? C23B C23A C23' O23 -102.0(5) . . . . ? N23 C23A C23' N24 -45.7(5) . . . . ? C23B C23A C23' N24 78.0(5) . . . . ? O23 C23' N24 C24A 4.6(6) . . . . ? C23A C23' N24 C24A -175.4(4) . . . . ? C23' N24 C24A C24' -51.7(5) . . . . ? C23' N24 C24A C24B 70.3(5) . . . . ? C23' N24 C24A C24F -168.7(4) . . . . ? N24 C24A C24B C24C 66.5(5) . . . . ? C24' C24A C24B C24C -171.6(4) . . . . ? C24F C24A C24B C24C -54.3(5) . . . . ? C24A C24B C24C C24D 58.4(6) . . . . ? C24B C24C C24D C24E -58.3(6) . . . . ? C24C C24D C24E C24F 55.5(6) . . . . ? C24D C24E C24F C24A -54.2(5) . . . . ? N24 C24A C24F C24E -68.4(5) . . . . ? C24' C24A C24F C24E 172.4(4) . . . . ? C24B C24A C24F C24E 53.0(5) . . . . ? N24 C24A C24' O24 134.3(4) . . . . ? C24B C24A C24' O24 12.2(6) . . . . ? C24F C24A C24' O24 -106.9(4) . . . . ? N24 C24A C24' N25 -47.7(5) . . . . ? C24B C24A C24' N25 -169.8(4) . . . . ? C24F C24A C24' N25 71.0(4) . . . . ? O24 C24' N25 C25A 5.1(6) . . . . ? C24A C24' N25 C25A -172.8(3) . . . . ? C24' N25 C25A C25' -75.0(5) . . . . ? C24' N25 C25A C25B 158.3(4) . . . . ? N25 C25A C25B C25D -60.7(5) . . . . ? C25' C25A C25B C25D 171.0(4) . . . . ? N25 C25A C25B C25C 68.5(5) . . . . ? C25' C25A C25B C25C -59.9(5) . . . . ? N25 C25A C25' O25 167.9(4) . . . . ? C25B C25A C25' O25 -65.1(5) . . . . ? N25 C25A C25' N26 -11.2(5) . . . . ? C25B C25A C25' N26 115.9(4) . . . . ? O25 C25' N26 C26A -6.1(6) . . . . ? C25A C25' N26 C26A 172.9(3) . . . . ? C25' N26 C26A C26' -93.2(5) . . . . ? C25' N26 C26A C26B 141.1(4) . . . . ? N26 C26A C26B C26C -70.0(6) . . . . ? C26' C26A C26B C26C 163.3(4) . . . . ? C26A C26B C26C C26E 167.5(6) . . . . ? C26A C26B C26C C26D -69.8(7) . . . . ? N26 C26A C26' O26 -179.5(4) . . . . ? C26B C26A C26' O26 -53.4(6) . . . . ? N26 C26A C26' N27 0.5(6) . . . . ? C26B C26A C26' N27 126.6(4) . . . . ? O26 C26' N27 C27A 1.7(7) . . . . ? C26A C26' N27 C27A -178.3(4) . . . . ? C26' N27 C27A C27' -113.7(5) . . . . ? C26' N27 C27A C27B 118.9(5) . . . . ? C27' C27A C27B C27C 171.9(4) . . . . ? N27 C27A C27B C27C -61.2(5) . . . . ? C27' C27A C27B C27D 48.4(6) . . . . ? N27 C27A C27B C27D 175.2(4) . . . . ? N27 C27A C27' O27 131.8(4) . . . . ? C27B C27A C27' O27 -101.7(5) . . . . ? N27 C27A C27' N28 -52.9(5) . . . . ? C27B C27A C27' N28 73.5(5) . . . . ? O27 C27' N28 C28A 0.8(7) . . . . ? C27A C27' N28 C28A -174.4(4) . . . . ? C27' N28 C28A C28' -96.7(6) . . . . ? C27' N28 C28A C28B 139.4(5) . . . . ? N28 C28A C28B C28C 61.8(7) . . . . ? C28' C28A C28B C28C -64.3(7) . . . . ? N28 C28A C28B C28D -64.2(8) . . . . ? C28' C28A C28B C28D 169.7(7) . . . . ? N28 C28A C28' O28 -28.3(8) . . . . ? C28B C28A C28' O28 97.6(8) . . . . ? N28 C28A C28' O2TM 154.0(5) . . . . ? C28B C28A C28' O2TM -80.2(7) . . . . ? O28 C28' O2TM C2TM 0.9(10) . . . . ? C28A C28' O2TM C2TM 178.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.635 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.049 # Attachment 'fac8.cif' data_fac8 _database_code_depnum_ccdc_archive 'CCDC 850190' #TrackingRef 'fac8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-Butyloxycarbonyl-leucyl-phenylalanyl-valyl-(1-aminocyclohexan-1-oyl)-valyl- leucyl-phenylalanyl-valyl-methyl ester ; _chemical_name_common Boc-Leu-Phe-Val-Ac6c-Val-Leu-Phe-Val-OMe _chemical_melting_point ? _chemical_formula_moiety 'C58 H90 N8 O11' _chemical_formula_sum 'C58 H90 N8 O11' _chemical_formula_weight 1075.38 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.312(4) _cell_length_b 19.868(6) _cell_length_c 28.099(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6315(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour 'color less' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.078 _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 'BRUKER AXS SMART APEX CCD with Mo source' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62458 _diffrn_reflns_av_R_equivalents 0.1495 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 26.89 _reflns_number_total 7153 _reflns_number_gt 4488 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement ? _computing_data_reduction SAINT _computing_structure_solution 'SHELXD (Schneider and Sheldrick, 2002)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1000P)^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 'riding over the heavy atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(10) _refine_ls_number_reflns 7153 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1279 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.1855 _refine_ls_wR_factor_gt 0.1619 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.363 _refine_ls_shift/su_mean 0.044 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 0.6545(6) 0.1642(3) -0.21063(18) 0.0758(17) Uani 1 1 d . . . C2 C 0.5549(7) 0.1859(4) -0.1790(3) 0.107(2) Uani 1 1 d . . . H2A H 0.4819 0.1680 -0.1909 0.160 Uiso 1 1 calc R . . H2B H 0.5507 0.2342 -0.1785 0.160 Uiso 1 1 calc R . . H2C H 0.5684 0.1696 -0.1473 0.160 Uiso 1 1 calc R . . C3 C 0.7722(8) 0.1912(4) -0.1946(3) 0.113(2) Uani 1 1 d . . . H3A H 0.8327 0.1765 -0.2161 0.169 Uiso 1 1 calc R . . H3B H 0.7893 0.1749 -0.1632 0.169 Uiso 1 1 calc R . . H3C H 0.7697 0.2395 -0.1942 0.169 Uiso 1 1 calc R . . C4 C 0.6344(9) 0.1820(4) -0.2632(2) 0.123(3) Uani 1 1 d . . . H4A H 0.5589 0.1651 -0.2732 0.184 Uiso 1 1 calc R . . H4B H 0.6956 0.1620 -0.2822 0.184 Uiso 1 1 calc R . . H4C H 0.6362 0.2300 -0.2670 0.184 Uiso 1 1 calc R . . O O 0.6602(3) 0.09091(18) -0.21344(11) 0.0702(10) Uani 1 1 d . . . C0' C 0.6887(4) 0.0529(3) -0.17661(14) 0.0509(11) Uani 1 1 d . . . O0 O 0.7008(3) 0.07287(15) -0.13562(9) 0.0520(8) Uani 1 1 d . . . N1 N 0.7061(3) -0.0104(2) -0.19008(11) 0.0499(9) Uani 1 1 d . . . H1 H 0.7025 -0.0203 -0.2198 0.060 Uiso 1 1 calc R . . C1A C 0.7309(4) -0.0628(2) -0.15599(13) 0.0477(11) Uani 1 1 d . . . H1A H 0.6646 -0.0647 -0.1336 0.057 Uiso 1 1 calc R . . C1' C 0.8422(4) -0.0495(2) -0.12771(13) 0.0437(10) Uani 1 1 d . . . O1 O 0.8504(3) -0.07152(16) -0.08725(10) 0.0581(8) Uani 1 1 d . . . C1B C 0.7390(5) -0.1303(3) -0.18087(17) 0.0637(13) Uani 1 1 d . . . H1B1 H 0.7888 -0.1255 -0.2088 0.076 Uiso 1 1 calc R . . H1B2 H 0.7771 -0.1621 -0.1597 0.076 Uiso 1 1 calc R . . C1G C 0.6220(6) -0.1589(4) -0.1961(2) 0.100(2) Uani 1 1 d . . . H1G H 0.5749 -0.1211 -0.2079 0.120 Uiso 1 1 calc R . . C1D1 C 0.5570(11) -0.1874(6) -0.1550(3) 0.193(6) Uani 1 1 d . . . H1D1 H 0.4809 -0.2030 -0.1654 0.289 Uiso 1 1 calc R . . H1D2 H 0.5469 -0.1533 -0.1312 0.289 Uiso 1 1 calc R . . H1D3 H 0.6009 -0.2243 -0.1419 0.289 Uiso 1 1 calc R . . C1D2 C 0.6371(9) -0.2070(5) -0.2374(3) 0.158(4) Uani 1 1 d . . . H1D4 H 0.6770 -0.1845 -0.2630 0.237 Uiso 1 1 calc R . . H1D5 H 0.5608 -0.2220 -0.2480 0.237 Uiso 1 1 calc R . . H1D6 H 0.6830 -0.2451 -0.2274 0.237 Uiso 1 1 calc R . . N2 N 0.9288(3) -0.01390(19) -0.14787(11) 0.0443(8) Uani 1 1 d . . . H2 H 0.9213 0.0001 -0.1767 0.053 Uiso 1 1 calc R . . C2A C 1.0348(4) 0.0011(3) -0.12155(14) 0.0522(12) Uani 1 1 d . . . H2A1 H 1.0691 -0.0419 -0.1115 0.063 Uiso 1 1 calc R . . C2' C 1.0078(4) 0.0418(3) -0.07608(14) 0.0551(12) Uani 1 1 d . . . O2 O 1.0736(3) 0.0374(2) -0.04172(12) 0.0903(14) Uani 1 1 d . . . C2B C 1.1252(4) 0.0364(3) -0.15048(17) 0.0625(13) Uani 1 1 d . . . H2B1 H 1.1785 0.0595 -0.1289 0.075 Uiso 1 1 calc R . . H2B2 H 1.0856 0.0705 -0.1693 0.075 Uiso 1 1 calc R . . C2G C 1.1983(4) -0.0061(3) -0.18354(16) 0.0635(14) Uani 1 1 d . . . C2D1 C 1.1633(5) -0.0691(3) -0.2005(2) 0.0778(16) Uani 1 1 d . . . H2D1 H 1.0929 -0.0883 -0.1901 0.093 Uiso 1 1 calc R . . C2D2 C 1.3041(5) 0.0177(4) -0.1980(2) 0.0904(18) Uani 1 1 d . . . H2D2 H 1.3301 0.0585 -0.1856 0.109 Uiso 1 1 calc R . . C2E1 C 1.2337(6) -0.1025(4) -0.2326(2) 0.091(2) Uani 1 1 d . . . H2E1 H 1.2104 -0.1442 -0.2444 0.109 Uiso 1 1 calc R . . C2E2 C 1.3729(6) -0.0140(5) -0.2290(3) 0.107(2) Uani 1 1 d . . . H2E2 H 1.4446 0.0047 -0.2382 0.129 Uiso 1 1 calc R . . C2Z C 1.3376(7) -0.0745(5) -0.2472(2) 0.108(3) Uani 1 1 d . . . H2Z H 1.3844 -0.0965 -0.2695 0.129 Uiso 1 1 calc R . . N3 N 0.9142(3) 0.08263(18) -0.07735(11) 0.0451(9) Uani 1 1 d . . . H3 H 0.8763 0.0878 -0.1036 0.054 Uiso 1 1 calc R . . C3A C 0.8746(4) 0.1189(2) -0.03487(14) 0.0465(11) Uani 1 1 d . . . H3A1 H 0.9446 0.1259 -0.0150 0.056 Uiso 1 1 calc R . . C3' C 0.7889(4) 0.0771(2) -0.00589(13) 0.0414(10) Uani 1 1 d . . . O3 O 0.7969(3) 0.07658(15) 0.03774(9) 0.0499(7) Uani 1 1 d . . . C3B C 0.8270(5) 0.1884(2) -0.04740(17) 0.0605(13) Uani 1 1 d . . . H3B1 H 0.7629 0.1828 -0.0705 0.073 Uiso 1 1 calc R . . C3G1 C 0.9231(7) 0.2314(3) -0.0701(2) 0.095(2) Uani 1 1 d . . . H3G1 H 0.8911 0.2746 -0.0783 0.143 Uiso 1 1 calc R . . H3G2 H 0.9519 0.2096 -0.0983 0.143 Uiso 1 1 calc R . . H3G3 H 0.9870 0.2371 -0.0480 0.143 Uiso 1 1 calc R . . C3G2 C 0.7768(7) 0.2221(3) -0.0035(2) 0.091(2) Uani 1 1 d . . . H3G4 H 0.7454 0.2654 -0.0119 0.137 Uiso 1 1 calc R . . H3G5 H 0.8383 0.2277 0.0197 0.137 Uiso 1 1 calc R . . H3G6 H 0.7150 0.1947 0.0096 0.137 Uiso 1 1 calc R . . N4 N 0.7045(3) 0.04195(18) -0.02845(11) 0.0454(9) Uani 1 1 d . . . H4 H 0.7029 0.0421 -0.0591 0.054 Uiso 1 1 calc R . . C4A C 0.6157(4) 0.0037(2) -0.00262(13) 0.0487(11) Uani 1 1 d . . . C4' C 0.6755(4) -0.0425(2) 0.03380(14) 0.0487(11) Uani 1 1 d . . . O4 O 0.6327(3) -0.05197(18) 0.07324(10) 0.0647(9) Uani 1 1 d . . . C4B1 C 0.5286(4) 0.0509(3) 0.02241(17) 0.0698(15) Uani 1 1 d . . . H4B1 H 0.5720 0.0822 0.0423 0.084 Uiso 1 1 calc R . . H4B2 H 0.4770 0.0247 0.0429 0.084 Uiso 1 1 calc R . . C4B2 C 0.5476(5) -0.0414(3) -0.03803(17) 0.0699(15) Uani 1 1 d . . . H4B3 H 0.6042 -0.0677 -0.0561 0.084 Uiso 1 1 calc R . . H4B4 H 0.4988 -0.0726 -0.0202 0.084 Uiso 1 1 calc R . . C4G1 C 0.4548(5) 0.0897(4) -0.0129(2) 0.094(2) Uani 1 1 d . . . H4G1 H 0.5062 0.1181 -0.0319 0.113 Uiso 1 1 calc R . . H4G2 H 0.4004 0.1187 0.0042 0.113 Uiso 1 1 calc R . . C4G2 C 0.4708(5) -0.0033(4) -0.07196(19) 0.093(2) Uani 1 1 d . . . H4G3 H 0.5200 0.0229 -0.0933 0.111 Uiso 1 1 calc R . . H4G4 H 0.4254 -0.0348 -0.0910 0.111 Uiso 1 1 calc R . . C4D C 0.3858(5) 0.0440(5) -0.0453(3) 0.120(3) Uani 1 1 d . . . H4D1 H 0.3302 0.0177 -0.0268 0.144 Uiso 1 1 calc R . . H4D2 H 0.3414 0.0707 -0.0680 0.144 Uiso 1 1 calc R . . N5 N 0.7734(4) -0.07405(19) 0.01979(12) 0.0537(10) Uani 1 1 d . . . H5 H 0.8032 -0.0647 -0.0076 0.064 Uiso 1 1 calc R . . C5A C 0.8314(6) -0.1241(3) 0.04986(17) 0.0676(14) Uani 1 1 d . . . H5A H 0.7696 -0.1546 0.0613 0.081 Uiso 1 1 calc R . . C5' C 0.8907(5) -0.0947(3) 0.09329(17) 0.0667(15) Uani 1 1 d . . . O5 O 0.9259(5) -0.1323(2) 0.12478(13) 0.0965(14) Uani 1 1 d . . . C5B C 0.9198(9) -0.1669(4) 0.0219(3) 0.117(3) Uani 1 1 d . . . H5B H 0.9500 -0.1986 0.0456 0.140 Uiso 1 1 calc R . . C5G1 C 1.0281(8) -0.1308(5) 0.0053(3) 0.129(3) Uani 1 1 d . . . H5G1 H 1.0615 -0.1059 0.0313 0.194 Uiso 1 1 calc R . . H5G2 H 1.0075 -0.1005 -0.0200 0.194 Uiso 1 1 calc R . . H5G3 H 1.0848 -0.1629 -0.0061 0.194 Uiso 1 1 calc R . . C5G2 C 0.8537(16) -0.2113(5) -0.0127(4) 0.218(7) Uani 1 1 d . . . H5G4 H 0.7865 -0.2308 0.0029 0.327 Uiso 1 1 calc R . . H5G5 H 0.9050 -0.2464 -0.0238 0.327 Uiso 1 1 calc R . . H5G6 H 0.8275 -0.1848 -0.0393 0.327 Uiso 1 1 calc R . . N6 N 0.9011(3) -0.0281(2) 0.09607(12) 0.0535(10) Uani 1 1 d . . . H6 H 0.8810 -0.0045 0.0717 0.064 Uiso 1 1 calc R . . C6A C 0.9448(4) 0.0070(3) 0.13799(14) 0.0558(12) Uani 1 1 d . . . H6A H 1.0064 -0.0209 0.1525 0.067 Uiso 1 1 calc R . . C6' C 0.8458(4) 0.0175(2) 0.17547(14) 0.0495(11) Uani 1 1 d . . . O6 O 0.8736(3) 0.0376(2) 0.21488(10) 0.0717(11) Uani 1 1 d . . . C6B C 0.9986(5) 0.0730(3) 0.12554(16) 0.0673(14) Uani 1 1 d . . . H6B1 H 0.9359 0.1024 0.1144 0.081 Uiso 1 1 calc R . . H6B2 H 1.0299 0.0926 0.1545 0.081 Uiso 1 1 calc R . . C6G C 1.0940(7) 0.0735(5) 0.0893(3) 0.120(3) Uani 1 1 d . . . H6G H 1.0591 0.0564 0.0598 0.144 Uiso 1 1 calc R . . C6D1 C 1.1894(8) 0.0283(7) 0.1014(5) 0.217(7) Uani 1 1 d . . . H6D1 H 1.2492 0.0303 0.0772 0.326 Uiso 1 1 calc R . . H6D2 H 1.1595 -0.0169 0.1036 0.326 Uiso 1 1 calc R . . H6D3 H 1.2228 0.0413 0.1315 0.326 Uiso 1 1 calc R . . C6D2 C 1.1350(11) 0.1440(6) 0.0791(5) 0.216(7) Uani 1 1 d . . . H6D4 H 1.1966 0.1429 0.0556 0.324 Uiso 1 1 calc R . . H6D5 H 1.1647 0.1641 0.1077 0.324 Uiso 1 1 calc R . . H6D6 H 1.0698 0.1701 0.0673 0.324 Uiso 1 1 calc R . . N7 N 0.7360(3) 0.00585(19) 0.16206(11) 0.0462(9) Uani 1 1 d . . . H7 H 0.7238 -0.0094 0.1338 0.055 Uiso 1 1 calc R . . C7A C 0.6348(4) 0.0176(2) 0.19264(14) 0.0499(11) Uani 1 1 d . . . H7A H 0.6644 0.0403 0.2212 0.060 Uiso 1 1 calc R . . C7' C 0.5760(4) -0.0460(3) 0.20883(14) 0.0531(12) Uani 1 1 d . . . O7 O 0.5451(3) -0.0529(2) 0.25029(10) 0.0692(10) Uani 1 1 d . . . C7B C 0.5461(4) 0.0657(3) 0.16891(16) 0.0565(12) Uani 1 1 d . . . H7B1 H 0.5283 0.0494 0.1372 0.068 Uiso 1 1 calc R . . H7B2 H 0.4732 0.0656 0.1871 0.068 Uiso 1 1 calc R . . C7G C 0.5910(4) 0.1360(3) 0.16553(15) 0.0557(12) Uani 1 1 d . . . C7D1 C 0.5577(6) 0.1839(4) 0.1982(2) 0.0897(19) Uani 1 1 d . . . H7D1 H 0.5044 0.1724 0.2220 0.108 Uiso 1 1 calc R . . C7D2 C 0.6697(5) 0.1561(3) 0.13103(16) 0.0666(14) Uani 1 1 d . . . H7D2 H 0.6926 0.1251 0.1080 0.080 Uiso 1 1 calc R . . C7E1 C 0.6015(8) 0.2486(4) 0.1966(3) 0.112(3) Uani 1 1 d . . . H7E1 H 0.5767 0.2803 0.2188 0.134 Uiso 1 1 calc R . . C7E2 C 0.7153(6) 0.2195(3) 0.12930(19) 0.0800(17) Uani 1 1 d . . . H7E2 H 0.7695 0.2311 0.1058 0.096 Uiso 1 1 calc R . . C7Z C 0.6804(7) 0.2662(3) 0.1627(2) 0.095(2) Uani 1 1 d . . . H7Z H 0.7111 0.3096 0.1620 0.113 Uiso 1 1 calc R . . N8 N 0.5531(4) -0.0929(2) 0.17551(13) 0.0643(11) Uani 1 1 d . . . H8 H 0.5766 -0.0856 0.1469 0.077 Uiso 1 1 calc R . . C8A C 0.4917(5) -0.1541(3) 0.18530(19) 0.0728(15) Uani 1 1 d . . . H8A H 0.4818 -0.1562 0.2199 0.087 Uiso 1 1 calc R . . C8' C 0.5575(6) -0.2169(3) 0.1713(2) 0.0811(17) Uani 1 1 d . . . O8 O 0.5296(5) -0.2705(2) 0.1854(2) 0.131(2) Uani 1 1 d . . . C8B C 0.3675(6) -0.1554(3) 0.1640(2) 0.0904(18) Uani 1 1 d . . . H8B H 0.3350 -0.2001 0.1709 0.108 Uiso 1 1 calc R . . C8G1 C 0.2880(7) -0.1062(4) 0.1876(3) 0.129(3) Uani 1 1 d . . . H8G1 H 0.2108 -0.1087 0.1735 0.193 Uiso 1 1 calc R . . H8G2 H 0.3191 -0.0616 0.1835 0.193 Uiso 1 1 calc R . . H8G3 H 0.2827 -0.1163 0.2209 0.193 Uiso 1 1 calc R . . C8G2 C 0.3678(8) -0.1481(5) 0.1106(3) 0.133(3) Uani 1 1 d . . . H8G4 H 0.4185 -0.1816 0.0969 0.200 Uiso 1 1 calc R . . H8G5 H 0.3962 -0.1041 0.1022 0.200 Uiso 1 1 calc R . . H8G6 H 0.2889 -0.1538 0.0987 0.200 Uiso 1 1 calc R . . O0M O 0.6441(4) -0.2067(2) 0.14195(16) 0.0974(14) Uani 1 1 d . . . C0M C 0.7079(9) -0.2654(4) 0.1268(3) 0.131(3) Uani 1 1 d . . . H0M1 H 0.7690 -0.2524 0.1049 0.197 Uiso 1 1 calc R . . H0M2 H 0.6547 -0.2961 0.1113 0.197 Uiso 1 1 calc R . . H0M3 H 0.7429 -0.2870 0.1539 0.197 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 C1 0.095(4) 0.086(4) 0.047(3) 0.012(3) -0.008(3) 0.018(4) C2 0.113(5) 0.107(5) 0.101(5) 0.012(4) 0.001(4) 0.046(5) C3 0.141(7) 0.095(5) 0.103(5) 0.017(4) 0.005(5) -0.021(5) C4 0.193(9) 0.108(5) 0.066(4) 0.031(4) -0.015(5) 0.048(6) O 0.097(3) 0.075(2) 0.0389(16) 0.0032(16) -0.0163(18) 0.019(2) C0' 0.048(3) 0.072(3) 0.032(2) 0.005(2) -0.0072(19) 0.010(2) O0 0.0579(18) 0.0679(19) 0.0300(14) -0.0033(14) -0.0066(13) 0.0064(17) N1 0.058(2) 0.069(3) 0.0227(16) -0.0028(17) -0.0053(16) 0.000(2) C1A 0.050(2) 0.063(3) 0.030(2) -0.005(2) 0.0046(18) -0.006(2) C1' 0.051(2) 0.054(2) 0.026(2) -0.0016(18) 0.0013(18) 0.005(2) O1 0.067(2) 0.074(2) 0.0330(15) 0.0053(15) -0.0022(14) -0.0023(18) C1B 0.072(3) 0.071(3) 0.049(3) -0.005(2) 0.003(2) -0.007(3) C1G 0.099(5) 0.111(5) 0.091(4) -0.042(4) 0.016(4) -0.042(4) C1D1 0.203(10) 0.218(11) 0.157(9) -0.068(8) 0.071(9) -0.138(10) C1D2 0.162(9) 0.175(8) 0.137(7) -0.079(7) -0.007(7) -0.049(8) N2 0.0403(19) 0.068(2) 0.0250(15) -0.0053(16) 0.0028(15) 0.0007(19) C2A 0.038(2) 0.080(3) 0.039(2) -0.010(2) 0.0023(19) 0.006(2) C2' 0.046(3) 0.084(4) 0.035(2) -0.010(2) 0.001(2) 0.004(3) O2 0.068(2) 0.151(4) 0.052(2) -0.036(2) -0.0234(19) 0.038(3) C2B 0.056(3) 0.074(3) 0.058(3) -0.002(2) 0.000(2) -0.005(3) C2G 0.043(3) 0.099(4) 0.049(3) -0.009(3) 0.004(2) 0.000(3) C2D1 0.056(3) 0.106(5) 0.072(3) -0.009(3) 0.015(3) 0.006(3) C2D2 0.050(3) 0.115(5) 0.106(5) -0.008(4) 0.018(3) 0.001(3) C2E1 0.088(5) 0.109(5) 0.076(4) -0.025(4) 0.007(4) 0.033(4) C2E2 0.066(4) 0.147(7) 0.108(6) 0.021(5) 0.033(4) 0.009(5) C2Z 0.088(5) 0.173(8) 0.062(4) -0.007(5) 0.031(4) 0.043(6) N3 0.050(2) 0.059(2) 0.0254(16) -0.0027(15) -0.0004(15) 0.0010(19) C3A 0.053(3) 0.055(3) 0.031(2) -0.0049(19) -0.0012(19) 0.000(2) C3' 0.048(2) 0.047(2) 0.030(2) -0.0073(18) -0.0021(18) 0.013(2) O3 0.0655(19) 0.0601(18) 0.0241(13) -0.0038(12) -0.0024(13) 0.0040(16) C3B 0.075(3) 0.058(3) 0.049(3) 0.002(2) 0.006(2) 0.004(3) C3G1 0.125(5) 0.080(4) 0.081(4) 0.007(3) 0.023(4) -0.022(4) C3G2 0.146(6) 0.052(3) 0.075(4) 0.002(3) 0.028(4) 0.029(4) N4 0.049(2) 0.066(2) 0.0213(15) -0.0022(15) -0.0006(15) -0.0001(19) C4A 0.044(2) 0.074(3) 0.029(2) -0.006(2) 0.0062(18) -0.008(2) C4' 0.055(3) 0.062(3) 0.029(2) -0.0067(19) 0.006(2) -0.015(2) O4 0.070(2) 0.092(2) 0.0322(16) 0.0034(16) 0.0078(15) -0.0138(19) C4B1 0.055(3) 0.111(4) 0.043(2) -0.006(3) 0.005(2) 0.008(3) C4B2 0.058(3) 0.108(4) 0.045(2) -0.010(3) 0.003(2) -0.027(3) C4G1 0.066(4) 0.150(6) 0.068(4) 0.004(4) 0.004(3) 0.039(4) C4G2 0.056(3) 0.169(7) 0.052(3) -0.007(4) -0.009(3) -0.014(4) C4D 0.054(4) 0.223(10) 0.083(4) 0.001(5) -0.013(4) 0.020(5) N5 0.070(3) 0.058(2) 0.0328(17) 0.0023(17) 0.0085(18) 0.000(2) C5A 0.092(4) 0.057(3) 0.055(3) 0.007(2) 0.003(3) 0.006(3) C5' 0.084(4) 0.074(4) 0.042(3) 0.011(3) 0.015(3) 0.025(3) O5 0.148(4) 0.086(3) 0.056(2) 0.023(2) -0.004(2) 0.031(3) C5B 0.178(8) 0.082(5) 0.090(5) -0.023(4) -0.008(6) 0.056(5) C5G1 0.137(7) 0.164(8) 0.087(5) 0.003(5) 0.037(5) 0.071(7) C5G2 0.37(2) 0.135(8) 0.145(8) -0.052(7) 0.028(12) 0.034(12) N6 0.059(2) 0.072(3) 0.0300(18) 0.0142(18) 0.0015(16) 0.008(2) C6A 0.051(3) 0.085(3) 0.032(2) 0.016(2) 0.001(2) 0.008(3) C6' 0.046(3) 0.071(3) 0.031(2) 0.015(2) 0.0047(19) 0.002(2) O6 0.057(2) 0.133(3) 0.0246(15) 0.0029(17) -0.0021(14) -0.010(2) C6B 0.059(3) 0.103(4) 0.040(2) 0.008(3) -0.003(2) -0.014(3) C6G 0.100(5) 0.148(7) 0.112(6) 0.022(5) 0.034(5) -0.025(6) C6D1 0.078(5) 0.295(16) 0.278(14) 0.148(13) 0.064(7) 0.037(8) C6D2 0.217(13) 0.178(10) 0.252(13) -0.003(10) 0.131(11) -0.092(10) N7 0.045(2) 0.067(2) 0.0269(16) -0.0050(16) 0.0013(15) 0.0037(18) C7A 0.047(3) 0.072(3) 0.0300(19) -0.006(2) -0.0013(19) 0.003(2) C7' 0.050(3) 0.077(3) 0.032(2) 0.002(2) 0.005(2) 0.005(3) O7 0.074(2) 0.101(3) 0.0330(16) 0.0033(16) 0.0122(16) -0.007(2) C7B 0.045(2) 0.078(3) 0.047(2) -0.006(2) 0.002(2) 0.005(3) C7G 0.055(3) 0.074(3) 0.039(2) -0.010(2) 0.002(2) 0.017(3) C7D1 0.094(4) 0.102(5) 0.073(4) -0.025(3) 0.028(4) 0.008(4) C7D2 0.093(4) 0.067(3) 0.039(2) -0.008(2) 0.001(3) 0.017(3) C7E1 0.143(7) 0.090(5) 0.103(5) -0.047(4) 0.029(5) 0.019(5) C7E2 0.105(5) 0.076(4) 0.059(3) 0.001(3) 0.010(3) 0.009(4) C7Z 0.121(6) 0.073(4) 0.090(5) -0.013(4) -0.002(5) 0.006(4) N8 0.083(3) 0.073(3) 0.0373(19) 0.000(2) 0.011(2) -0.009(2) C8A 0.082(4) 0.077(4) 0.059(3) 0.004(3) 0.017(3) -0.018(3) C8' 0.095(5) 0.077(4) 0.071(4) 0.011(3) 0.010(4) -0.006(4) O8 0.142(4) 0.080(3) 0.170(5) 0.026(3) 0.063(4) -0.005(3) C8B 0.082(4) 0.086(4) 0.103(5) -0.003(4) 0.004(4) -0.014(4) C8G1 0.095(5) 0.123(6) 0.168(8) -0.004(6) 0.013(6) 0.021(5) C8G2 0.128(7) 0.175(8) 0.097(5) -0.016(5) -0.030(5) -0.014(6) O0M 0.119(3) 0.078(3) 0.095(3) 0.020(2) 0.046(3) 0.009(3) C0M 0.162(8) 0.102(5) 0.129(6) 0.028(5) 0.069(6) 0.037(6) _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 O 1.460(7) . ? C1 C3 1.505(10) . ? C1 C2 1.499(9) . ? C1 C4 1.534(8) . ? O C0' 1.320(5) . ? C0' O0 1.226(5) . ? C0' N1 1.328(6) . ? N1 C1A 1.442(6) . ? C1A C1' 1.512(6) . ? C1A C1B 1.516(7) . ? C1' O1 1.222(5) . ? C1' N2 1.334(5) . ? C1B C1G 1.501(8) . ? C1G C1D1 1.480(10) . ? C1G C1D2 1.514(10) . ? N2 C2A 1.440(5) . ? C2A C2B 1.483(7) . ? C2A C2' 1.543(6) . ? C2' O2 1.223(5) . ? C2' N3 1.335(6) . ? C2B C2G 1.503(7) . ? C2G C2D2 1.349(8) . ? C2G C2D1 1.396(8) . ? C2D1 C2E1 1.375(8) . ? C2D2 C2E2 1.326(10) . ? C2E1 C2Z 1.363(11) . ? C2E2 C2Z 1.365(11) . ? N3 C3A 1.464(5) . ? C3A C3' 1.514(6) . ? C3A C3B 1.523(6) . ? C3' O3 1.229(4) . ? C3' N4 1.342(5) . ? C3B C3G2 1.515(7) . ? C3B C3G1 1.523(8) . ? N4 C4A 1.454(5) . ? C4A C4' 1.533(6) . ? C4A C4B1 1.532(7) . ? C4A C4B2 1.545(6) . ? C4' O4 1.224(5) . ? C4' N5 1.332(6) . ? C4B1 C4G1 1.509(8) . ? C4B2 C4G2 1.496(8) . ? C4G1 C4D 1.505(10) . ? C4G2 C4D 1.539(10) . ? N5 C5A 1.460(6) . ? C5A C5' 1.511(8) . ? C5A C5B 1.531(9) . ? C5' O5 1.225(6) . ? C5' N6 1.330(7) . ? C5B C5G1 1.494(12) . ? C5B C5G2 1.511(14) . ? N6 C6A 1.456(6) . ? C6A C6B 1.486(7) . ? C6A C6' 1.551(6) . ? C6' O6 1.218(5) . ? C6' N7 1.319(6) . ? C6B C6G 1.483(8) . ? C6G C6D1 1.444(12) . ? C6G C6D2 1.504(12) . ? N7 C7A 1.450(5) . ? C7A C7' 1.499(7) . ? C7A C7B 1.539(6) . ? C7' O7 1.224(5) . ? C7' N8 1.346(6) . ? C7B C7G 1.489(7) . ? C7G C7D1 1.376(7) . ? C7G C7D2 1.375(7) . ? C7D1 C7E1 1.378(10) . ? C7D2 C7E2 1.362(8) . ? C7E1 C7Z 1.350(10) . ? C7E2 C7Z 1.378(8) . ? N8 C8A 1.427(7) . ? C8A C8B 1.528(9) . ? C8A C8' 1.504(9) . ? C8' O8 1.180(7) . ? C8' O0M 1.296(7) . ? C8B C8G1 1.484(10) . ? C8B C8G2 1.510(10) . ? O0M C0M 1.437(8) . ? 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 O C1 C3 109.4(5) . . ? O C1 C2 110.7(5) . . ? C3 C1 C2 112.6(5) . . ? O C1 C4 100.6(5) . . ? C3 C1 C4 109.7(6) . . ? C2 C1 C4 113.1(6) . . ? C0' O C1 122.6(4) . . ? O0 C0' N1 123.9(4) . . ? O0 C0' O 125.4(5) . . ? N1 C0' O 110.7(4) . . ? C0' N1 C1A 121.5(3) . . ? N1 C1A C1' 112.6(4) . . ? N1 C1A C1B 110.1(3) . . ? C1' C1A C1B 110.3(4) . . ? O1 C1' N2 122.0(4) . . ? O1 C1' C1A 119.3(4) . . ? N2 C1' C1A 118.8(3) . . ? C1G C1B C1A 114.4(5) . . ? C1D1 C1G C1B 111.2(6) . . ? C1D1 C1G C1D2 114.4(7) . . ? C1B C1G C1D2 111.0(6) . . ? C1' N2 C2A 120.2(3) . . ? N2 C2A C2B 113.0(4) . . ? N2 C2A C2' 111.6(3) . . ? C2B C2A C2' 110.1(4) . . ? O2 C2' N3 123.2(4) . . ? O2 C2' C2A 119.8(4) . . ? N3 C2' C2A 117.0(4) . . ? C2A C2B C2G 116.9(4) . . ? C2D2 C2G C2D1 117.6(5) . . ? C2D2 C2G C2B 118.5(5) . . ? C2D1 C2G C2B 123.9(4) . . ? C2G C2D1 C2E1 119.5(6) . . ? C2E2 C2D2 C2G 123.4(7) . . ? C2D1 C2E1 C2Z 119.9(7) . . ? C2D2 C2E2 C2Z 119.5(7) . . ? C2E2 C2Z C2E1 120.0(6) . . ? C2' N3 C3A 121.3(3) . . ? N3 C3A C3' 111.4(3) . . ? N3 C3A C3B 111.5(3) . . ? C3' C3A C3B 113.3(4) . . ? O3 C3' N4 121.3(4) . . ? O3 C3' C3A 119.6(4) . . ? N4 C3' C3A 119.1(3) . . ? C3A C3B C3G2 110.2(4) . . ? C3A C3B C3G1 110.7(5) . . ? C3G2 C3B C3G1 111.1(5) . . ? C3' N4 C4A 121.8(3) . . ? N4 C4A C4' 110.0(3) . . ? N4 C4A C4B1 110.7(4) . . ? C4' C4A C4B1 110.1(3) . . ? N4 C4A C4B2 109.0(3) . . ? C4' C4A C4B2 107.6(4) . . ? C4B1 C4A C4B2 109.3(4) . . ? O4 C4' N5 121.6(4) . . ? O4 C4' C4A 121.5(4) . . ? N5 C4' C4A 116.8(3) . . ? C4A C4B1 C4G1 111.5(4) . . ? C4G2 C4B2 C4A 114.0(5) . . ? C4B1 C4G1 C4D 112.1(6) . . ? C4D C4G2 C4B2 111.2(5) . . ? C4G2 C4D C4G1 109.8(5) . . ? C4' N5 C5A 121.5(4) . . ? N5 C5A C5' 113.8(4) . . ? N5 C5A C5B 112.0(4) . . ? C5' C5A C5B 109.9(5) . . ? O5 C5' N6 122.3(5) . . ? O5 C5' C5A 119.5(5) . . ? N6 C5' C5A 118.2(4) . . ? C5G1 C5B C5G2 119.1(8) . . ? C5G1 C5B C5A 115.5(6) . . ? C5G2 C5B C5A 109.4(9) . . ? C5' N6 C6A 123.7(4) . . ? N6 C6A C6B 111.8(3) . . ? N6 C6A C6' 111.7(4) . . ? C6B C6A C6' 109.7(4) . . ? O6 C6' N7 124.1(4) . . ? O6 C6' C6A 118.3(4) . . ? N7 C6' C6A 117.5(4) . . ? C6G C6B C6A 117.7(6) . . ? C6B C6G C6D1 112.2(7) . . ? C6B C6G C6D2 111.2(7) . . ? C6D1 C6G C6D2 113.3(9) . . ? C6' N7 C7A 123.1(3) . . ? N7 C7A C7' 113.3(4) . . ? N7 C7A C7B 111.0(3) . . ? C7' C7A C7B 111.5(4) . . ? O7 C7' N8 122.0(5) . . ? O7 C7' C7A 120.7(4) . . ? N8 C7' C7A 117.2(4) . . ? C7G C7B C7A 112.8(4) . . ? C7D1 C7G C7D2 116.6(5) . . ? C7D1 C7G C7B 120.9(5) . . ? C7D2 C7G C7B 122.5(4) . . ? C7G C7D1 C7E1 121.7(6) . . ? C7E2 C7D2 C7G 122.6(5) . . ? C7Z C7E1 C7D1 120.2(6) . . ? C7D2 C7E2 C7Z 119.3(6) . . ? C7E1 C7Z C7E2 119.7(7) . . ? C7' N8 C8A 123.3(4) . . ? N8 C8A C8B 112.7(5) . . ? N8 C8A C8' 114.5(5) . . ? C8B C8A C8' 109.9(5) . . ? O8 C8' O0M 123.9(6) . . ? O8 C8' C8A 121.9(6) . . ? O0M C8' C8A 114.2(5) . . ? C8G1 C8B C8A 111.9(6) . . ? C8G1 C8B C8G2 112.4(7) . . ? C8A C8B C8G2 112.7(6) . . ? C8' O0M C0M 116.2(5) . . ? 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 C3 C1 O C0' 57.6(7) . . . . ? C2 C1 O C0' -67.1(7) . . . . ? C4 C1 O C0' 173.1(5) . . . . ? C1 O C0' O0 8.2(8) . . . . ? C1 O C0' N1 -170.0(5) . . . . ? O0 C0' N1 C1A 5.8(7) . . . . ? O C0' N1 C1A -176.1(4) . . . . ? C0' N1 C1A C1' -60.0(5) . . . . ? C0' N1 C1A C1B 176.3(4) . . . . ? N1 C1A C1' O1 150.9(4) . . . . ? C1B C1A C1' O1 -85.6(5) . . . . ? N1 C1A C1' N2 -29.2(5) . . . . ? C1B C1A C1' N2 94.3(5) . . . . ? N1 C1A C1B C1G -74.4(6) . . . . ? C1' C1A C1B C1G 160.6(5) . . . . ? C1A C1B C1G C1D1 -76.3(9) . . . . ? C1A C1B C1G C1D2 155.1(6) . . . . ? O1 C1' N2 C2A -1.6(6) . . . . ? C1A C1' N2 C2A 178.5(4) . . . . ? C1' N2 C2A C2B 175.6(4) . . . . ? C1' N2 C2A C2' -59.7(5) . . . . ? N2 C2A C2' O2 152.5(5) . . . . ? C2B C2A C2' O2 -81.2(6) . . . . ? N2 C2A C2' N3 -30.2(6) . . . . ? C2B C2A C2' N3 96.1(5) . . . . ? N2 C2A C2B C2G -79.3(5) . . . . ? C2' C2A C2B C2G 155.1(4) . . . . ? C2A C2B C2G C2D2 -158.1(5) . . . . ? C2A C2B C2G C2D1 22.2(7) . . . . ? C2D2 C2G C2D1 C2E1 -3.2(8) . . . . ? C2B C2G C2D1 C2E1 176.6(5) . . . . ? C2D1 C2G C2D2 C2E2 3.3(10) . . . . ? C2B C2G C2D2 C2E2 -176.5(6) . . . . ? C2G C2D1 C2E1 C2Z 0.9(9) . . . . ? C2G C2D2 C2E2 C2Z -0.9(11) . . . . ? C2D2 C2E2 C2Z C2E1 -1.6(12) . . . . ? C2D1 C2E1 C2Z C2E2 1.5(10) . . . . ? O2 C2' N3 C3A -8.3(7) . . . . ? C2A C2' N3 C3A 174.5(4) . . . . ? C2' N3 C3A C3' -87.9(5) . . . . ? C2' N3 C3A C3B 144.6(4) . . . . ? N3 C3A C3' O3 138.5(4) . . . . ? C3B C3A C3' O3 -95.0(5) . . . . ? N3 C3A C3' N4 -42.4(5) . . . . ? C3B C3A C3' N4 84.2(5) . . . . ? N3 C3A C3B C3G2 175.0(5) . . . . ? C3' C3A C3B C3G2 48.5(6) . . . . ? N3 C3A C3B C3G1 -61.8(5) . . . . ? C3' C3A C3B C3G1 171.7(4) . . . . ? O3 C3' N4 C4A 2.4(6) . . . . ? C3A C3' N4 C4A -176.7(4) . . . . ? C3' N4 C4A C4' -51.4(5) . . . . ? C3' N4 C4A C4B1 70.6(5) . . . . ? C3' N4 C4A C4B2 -169.2(4) . . . . ? N4 C4A C4' O4 141.5(4) . . . . ? C4B1 C4A C4' O4 19.1(6) . . . . ? C4B2 C4A C4' O4 -99.9(5) . . . . ? N4 C4A C4' N5 -41.2(5) . . . . ? C4B1 C4A C4' N5 -163.5(4) . . . . ? C4B2 C4A C4' N5 77.4(5) . . . . ? N4 C4A C4B1 C4G1 66.7(6) . . . . ? C4' C4A C4B1 C4G1 -171.4(5) . . . . ? C4B2 C4A C4B1 C4G1 -53.4(6) . . . . ? N4 C4A C4B2 C4G2 -68.7(5) . . . . ? C4' C4A C4B2 C4G2 172.0(4) . . . . ? C4B1 C4A C4B2 C4G2 52.5(5) . . . . ? C4A C4B1 C4G1 C4D 58.4(6) . . . . ? C4A C4B2 C4G2 C4D -53.8(7) . . . . ? C4B2 C4G2 C4D C4G1 54.9(8) . . . . ? C4B1 C4G1 C4D C4G2 -57.8(8) . . . . ? O4 C4' N5 C5A 3.2(6) . . . . ? C4A C4' N5 C5A -174.1(4) . . . . ? C4' N5 C5A C5' -70.4(6) . . . . ? C4' N5 C5A C5B 164.3(5) . . . . ? N5 C5A C5' O5 168.7(5) . . . . ? C5B C5A C5' O5 -64.9(7) . . . . ? N5 C5A C5' N6 -10.4(7) . . . . ? C5B C5A C5' N6 116.0(6) . . . . ? N5 C5A C5B C5G1 69.0(8) . . . . ? C5' C5A C5B C5G1 -58.4(7) . . . . ? N5 C5A C5B C5G2 -68.5(8) . . . . ? C5' C5A C5B C5G2 164.0(7) . . . . ? O5 C5' N6 C6A -5.9(8) . . . . ? C5A C5' N6 C6A 173.2(4) . . . . ? C5' N6 C6A C6B 153.8(5) . . . . ? C5' N6 C6A C6' -82.9(6) . . . . ? N6 C6A C6' O6 169.7(4) . . . . ? C6B C6A C6' O6 -65.7(5) . . . . ? N6 C6A C6' N7 -12.2(6) . . . . ? C6B C6A C6' N7 112.4(5) . . . . ? N6 C6A C6B C6G -54.5(6) . . . . ? C6' C6A C6B C6G -178.9(5) . . . . ? C6A C6B C6G C6D1 -54.6(10) . . . . ? C6A C6B C6G C6D2 177.3(8) . . . . ? O6 C6' N7 C7A 1.8(7) . . . . ? C6A C6' N7 C7A -176.1(4) . . . . ? C6' N7 C7A C7' -110.1(5) . . . . ? C6' N7 C7A C7B 123.7(5) . . . . ? N7 C7A C7' O7 136.1(4) . . . . ? C7B C7A C7' O7 -97.9(5) . . . . ? N7 C7A C7' N8 -47.4(6) . . . . ? C7B C7A C7' N8 78.6(5) . . . . ? N7 C7A C7B C7G -69.9(5) . . . . ? C7' C7A C7B C7G 162.8(4) . . . . ? C7A C7B C7G C7D1 -98.8(6) . . . . ? C7A C7B C7G C7D2 79.2(6) . . . . ? C7D2 C7G C7D1 C7E1 -0.3(9) . . . . ? C7B C7G C7D1 C7E1 177.8(6) . . . . ? C7D1 C7G C7D2 C7E2 1.4(8) . . . . ? C7B C7G C7D2 C7E2 -176.7(5) . . . . ? C7G C7D1 C7E1 C7Z -1.0(12) . . . . ? C7G C7D2 C7E2 C7Z -1.2(9) . . . . ? C7D1 C7E1 C7Z C7E2 1.2(12) . . . . ? C7D2 C7E2 C7Z C7E1 -0.2(10) . . . . ? O7 C7' N8 C8A -0.1(8) . . . . ? C7A C7' N8 C8A -176.5(5) . . . . ? C7' N8 C8A C8B 108.8(6) . . . . ? C7' N8 C8A C8' -124.6(6) . . . . ? N8 C8A C8' O8 164.7(7) . . . . ? C8B C8A C8' O8 -67.2(8) . . . . ? N8 C8A C8' O0M -16.9(7) . . . . ? C8B C8A C8' O0M 111.1(6) . . . . ? N8 C8A C8B C8G1 -67.6(7) . . . . ? C8' C8A C8B C8G1 163.3(6) . . . . ? N8 C8A C8B C8G2 60.1(8) . . . . ? C8' C8A C8B C8G2 -68.9(8) . . . . ? O8 C8' O0M C0M -0.4(11) . . . . ? C8A C8' O0M C0M -178.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 26.89 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.393 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.051