# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Fernando Formaggio' 'Alberto Bianco' 'Marco Crisma' 'Piero Geotti Bianchini' 'Cristina Peggion' _publ_contact_author_name 'Fernando Formaggio' _publ_contact_author_email FERNANDO.FORMAGGIO@UNIPD.IT _publ_section_title ; Conformationally controlled, thymine-based alpha-nucleopeptides ; # Attachment 'mc110.cif' data_mc110 _database_code_depnum_ccdc_archive 'CCDC 714103' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Benzyloxycarbonyl-/a-aminoisobutyryl-(D,L)- alanylthymine-/a-aminoisobutyric acid tert-butyl ester ; _chemical_name_common Z-Aib-(D,L)-AlaT-Aib-OtBu _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H39 N5 O8' _chemical_formula_weight 573.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.341(3) _cell_length_b 17.198(4) _cell_length_c 14.434(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.36(6) _cell_angle_gamma 90.00 _cell_volume 3058.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 12 _cell_measurement_theta_max 21 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.764 _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 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW1100 diffractometer' _diffrn_measurement_method '\q-2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 5075 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 60.05 _reflns_number_total 4537 _reflns_number_gt 3678 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _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^)+(0.0925P)^2^+1.1497P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0038(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4537 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1756 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 C01 C 0.08486(13) 0.20650(12) 0.62148(14) 0.0630(7) Uani 1 1 d G . . C02 C 0.0830(2) 0.13497(13) 0.66619(16) 0.0902(10) Uani 1 1 d G . . H02 H 0.0173 0.1137 0.6818 0.108 Uiso 1 1 calc R . . C03 C 0.1794(3) 0.09531(12) 0.68756(17) 0.1077(14) Uani 1 1 d G . . H03 H 0.1781 0.0475 0.7175 0.129 Uiso 1 1 calc R . . C04 C 0.2776(2) 0.12718(17) 0.66420(19) 0.1104(15) Uani 1 1 d G . . H04 H 0.3421 0.1006 0.6785 0.132 Uiso 1 1 calc R . . C05 C 0.27949(13) 0.19871(18) 0.61949(19) 0.1062(14) Uani 1 1 d G . . H05 H 0.3452 0.2200 0.6039 0.127 Uiso 1 1 calc R . . C06 C 0.18311(17) 0.23837(12) 0.59813(15) 0.0799(9) Uani 1 1 d G . . H06 H 0.1844 0.2862 0.5682 0.096 Uiso 1 1 calc R . . C07 C -0.0182(2) 0.2495(2) 0.6009(3) 0.0889(11) Uani 1 1 d . . . H07A H -0.0630 0.2465 0.6538 0.107 Uiso 1 1 calc R . . H07B H -0.0026 0.3038 0.5895 0.107 Uiso 1 1 calc R . . OU O -0.07617(14) 0.21623(13) 0.51999(13) 0.0715(6) Uani 1 1 d . . . C0 C -0.1857(2) 0.21143(15) 0.52309(18) 0.0530(6) Uani 1 1 d . . . O0 O -0.23427(15) 0.22821(11) 0.59085(12) 0.0620(5) Uani 1 1 d . . . N1 N -0.22982(16) 0.18473(13) 0.44250(13) 0.0525(5) Uani 1 1 d . . . H1 H -0.1879 0.1712 0.3997 0.063 Uiso 1 1 calc R . . C1A C -0.3484(2) 0.17780(16) 0.42483(16) 0.0530(6) Uani 1 1 d . . . C1B1 C -0.3661(2) 0.13285(19) 0.33338(18) 0.0668(8) Uani 1 1 d . . . H1B1 H -0.3356 0.1617 0.2842 0.100 Uiso 1 1 calc R . . H1B2 H -0.4425 0.1257 0.3194 0.100 Uiso 1 1 calc R . . H1B3 H -0.3313 0.0830 0.3392 0.100 Uiso 1 1 calc R . . C1B2 C -0.4014(2) 0.25744(18) 0.4172(2) 0.0703(8) Uani 1 1 d . . . H1B4 H -0.3865 0.2856 0.4740 0.105 Uiso 1 1 calc R . . H1B5 H -0.4785 0.2514 0.4063 0.105 Uiso 1 1 calc R . . H1B6 H -0.3729 0.2856 0.3667 0.105 Uiso 1 1 calc R . . C1 C -0.39692(18) 0.12916(15) 0.50069(16) 0.0499(6) Uani 1 1 d . . . O1 O -0.48992(14) 0.14079(12) 0.52479(13) 0.0676(5) Uani 1 1 d . . . N2 N -0.33644(16) 0.07039(12) 0.53561(13) 0.0519(5) Uani 1 1 d . . . H2 H -0.2706 0.0666 0.5197 0.062 Uiso 1 1 calc R . . C2A C -0.3753(2) 0.01315(15) 0.59838(16) 0.0523(6) Uani 1 1 d . . . H2A H -0.4517 0.0039 0.5792 0.063 Uiso 1 1 calc R . . C2B C -0.31722(19) -0.06396(15) 0.58861(18) 0.0534(6) Uani 1 1 d . . . H2B1 H -0.3588 -0.1040 0.6179 0.064 Uiso 1 1 calc R . . H2B2 H -0.3167 -0.0765 0.5231 0.064 Uiso 1 1 calc R . . N1T N -0.20449(16) -0.06683(12) 0.62873(14) 0.0512(5) Uani 1 1 d . . . C2T C -0.1218(2) -0.04058(16) 0.57763(17) 0.0540(6) Uani 1 1 d . . . O2T O -0.13816(14) -0.00200(12) 0.50608(12) 0.0650(5) Uani 1 1 d . . . N3T N -0.01978(17) -0.05936(14) 0.61075(15) 0.0589(6) Uani 1 1 d . . . H3T H 0.0325 -0.0431 0.5790 0.071 Uiso 1 1 calc R . . C4T C 0.0094(2) -0.10188(16) 0.69006(18) 0.0556(6) Uani 1 1 d . . . O4T O 0.10439(15) -0.11832(13) 0.70824(13) 0.0723(6) Uani 1 1 d . . . C5T C -0.0806(2) -0.12209(15) 0.74544(17) 0.0537(6) Uani 1 1 d . . . C6T C -0.1809(2) -0.10434(14) 0.71217(17) 0.0527(6) Uani 1 1 d . . . H6T H -0.2386 -0.1181 0.7475 0.063 Uiso 1 1 calc R . . C7T C -0.0573(3) -0.1613(2) 0.8369(2) 0.0724(8) Uani 1 1 d . . . H7T1 H -0.0303 -0.1237 0.8817 0.109 Uiso 1 1 calc R . . H7T2 H -0.0038 -0.2011 0.8304 0.109 Uiso 1 1 calc R . . H7T3 H -0.1228 -0.1841 0.8573 0.109 Uiso 1 1 calc R . . C2 C -0.3723(2) 0.03696(16) 0.70043(17) 0.0547(6) Uani 1 1 d . . . O2 O -0.41175(17) -0.00634(12) 0.75624(13) 0.0706(6) Uani 1 1 d . . . N3 N -0.32055(18) 0.10294(13) 0.72408(14) 0.0586(6) Uani 1 1 d . . . H3 H -0.2907 0.1295 0.6820 0.070 Uiso 1 1 calc R . . C3A C -0.3136(3) 0.13104(17) 0.82014(18) 0.0631(7) Uani 1 1 d . . . C3B1 C -0.2270(3) 0.1943(2) 0.8271(2) 0.0858(10) Uani 1 1 d . . . H3B1 H -0.1579 0.1723 0.8144 0.129 Uiso 1 1 calc R . . H3B2 H -0.2232 0.2159 0.8886 0.129 Uiso 1 1 calc R . . H3B3 H -0.2453 0.2345 0.7828 0.129 Uiso 1 1 calc R . . C3B2 C -0.4233(3) 0.1610(2) 0.8459(2) 0.0814(9) Uani 1 1 d . . . H3B4 H -0.4472 0.2012 0.8033 0.122 Uiso 1 1 calc R . . H3B5 H -0.4174 0.1817 0.9077 0.122 Uiso 1 1 calc R . . H3B6 H -0.4749 0.1191 0.8429 0.122 Uiso 1 1 calc R . . C3 C -0.2689(3) 0.06421(17) 0.88195(18) 0.0651(7) Uani 1 1 d . . . O3 O -0.1957(2) 0.02285(15) 0.86049(14) 0.0860(7) Uani 1 1 d . . . OT O -0.31541(18) 0.06220(11) 0.96267(12) 0.0678(6) Uani 1 1 d . . . CT1 C -0.2846(3) 0.00303(18) 1.03387(19) 0.0714(8) Uani 1 1 d . . . CT2 C -0.3124(4) -0.0766(2) 0.9954(3) 0.0998(12) Uani 1 1 d . . . HT2A H -0.3840 -0.0756 0.9656 0.150 Uiso 1 1 calc R . . HT2B H -0.3100 -0.1138 1.0451 0.150 Uiso 1 1 calc R . . HT2C H -0.2610 -0.0910 0.9511 0.150 Uiso 1 1 calc R . . CT3 C -0.1661(4) 0.0108(3) 1.0640(3) 0.1193(16) Uani 1 1 d . . . HT3A H -0.1228 -0.0013 1.0128 0.179 Uiso 1 1 calc R . . HT3B H -0.1485 -0.0246 1.1141 0.179 Uiso 1 1 calc R . . HT3C H -0.1514 0.0631 1.0842 0.179 Uiso 1 1 calc R . . CT4 C -0.3572(4) 0.0230(3) 1.1107(2) 0.1069(13) Uani 1 1 d . . . HT4A H -0.3429 0.0753 1.1311 0.160 Uiso 1 1 calc R . . HT4B H -0.3432 -0.0122 1.1617 0.160 Uiso 1 1 calc R . . HT4C H -0.4317 0.0185 1.0883 0.160 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 C01 0.0592(16) 0.0749(19) 0.0539(15) -0.0124(14) -0.0067(12) -0.0078(14) C02 0.104(3) 0.091(3) 0.076(2) -0.0052(19) 0.0043(19) -0.018(2) C03 0.140(4) 0.102(3) 0.077(2) 0.004(2) -0.024(2) 0.023(3) C04 0.104(3) 0.127(4) 0.095(3) -0.029(3) -0.039(2) 0.036(3) C05 0.060(2) 0.140(4) 0.117(3) -0.039(3) -0.0064(19) -0.004(2) C06 0.070(2) 0.090(2) 0.079(2) -0.0016(17) -0.0049(16) -0.0121(17) C07 0.0536(17) 0.107(3) 0.103(2) -0.038(2) -0.0219(16) 0.0031(17) OU 0.0447(10) 0.1011(15) 0.0676(12) -0.0170(11) -0.0065(8) -0.0048(10) C0 0.0511(14) 0.0563(15) 0.0505(15) 0.0020(12) -0.0062(11) -0.0007(11) O0 0.0648(11) 0.0716(12) 0.0489(10) -0.0082(9) -0.0014(9) 0.0002(9) N1 0.0426(11) 0.0698(13) 0.0446(11) 0.0000(10) -0.0004(8) -0.0005(9) C1A 0.0489(13) 0.0668(16) 0.0423(13) 0.0010(11) -0.0060(10) 0.0022(12) C1B1 0.0589(16) 0.096(2) 0.0447(14) -0.0039(14) -0.0059(12) -0.0086(15) C1B2 0.0654(17) 0.0768(19) 0.0674(18) 0.0111(15) -0.0075(14) 0.0103(15) C1 0.0369(12) 0.0659(16) 0.0457(13) -0.0056(11) -0.0070(10) -0.0003(11) O1 0.0494(10) 0.0839(14) 0.0692(12) 0.0046(10) 0.0005(9) 0.0049(9) N2 0.0455(11) 0.0647(13) 0.0450(11) 0.0035(10) -0.0017(9) 0.0003(10) C2A 0.0470(13) 0.0627(15) 0.0464(13) -0.0013(11) -0.0030(10) -0.0041(11) C2B 0.0466(13) 0.0605(15) 0.0525(14) -0.0055(12) -0.0023(11) -0.0096(11) N1T 0.0492(11) 0.0555(12) 0.0490(11) 0.0021(9) 0.0041(9) -0.0040(9) C2T 0.0559(15) 0.0596(15) 0.0470(14) 0.0026(12) 0.0069(11) 0.0017(12) O2T 0.0534(11) 0.0866(14) 0.0559(11) 0.0181(10) 0.0105(8) 0.0077(9) N3T 0.0473(12) 0.0750(15) 0.0549(13) 0.0132(11) 0.0080(9) 0.0037(10) C4T 0.0545(16) 0.0631(16) 0.0493(14) -0.0001(12) 0.0042(11) 0.0024(12) O4T 0.0508(11) 0.1032(16) 0.0626(12) 0.0121(11) 0.0017(9) 0.0128(10) C5T 0.0552(15) 0.0566(15) 0.0496(14) 0.0020(11) 0.0052(11) -0.0012(12) C6T 0.0562(15) 0.0519(14) 0.0507(14) 0.0016(11) 0.0093(11) -0.0049(11) C7T 0.0725(19) 0.085(2) 0.0595(17) 0.0172(15) 0.0020(14) -0.0016(16) C2 0.0545(14) 0.0616(16) 0.0481(14) 0.0012(12) 0.0029(11) 0.0011(12) O2 0.0867(14) 0.0721(13) 0.0542(11) 0.0035(10) 0.0133(10) -0.0148(10) N3 0.0713(14) 0.0616(13) 0.0428(11) 0.0008(10) 0.0023(10) -0.0100(11) C3A 0.0829(19) 0.0609(16) 0.0452(14) -0.0018(12) 0.0023(13) -0.0009(14) C3B1 0.122(3) 0.075(2) 0.0596(18) -0.0095(15) -0.0038(17) -0.0238(19) C3B2 0.104(3) 0.079(2) 0.0620(18) 0.0041(16) 0.0100(17) 0.0225(18) C3 0.086(2) 0.0625(17) 0.0462(15) -0.0076(13) -0.0042(14) 0.0009(15) O3 0.0995(17) 0.0978(17) 0.0603(12) -0.0021(12) 0.0016(11) 0.0259(14) OT 0.0971(15) 0.0618(11) 0.0442(10) 0.0007(8) 0.0018(9) 0.0052(10) CT1 0.094(2) 0.0684(18) 0.0503(15) 0.0064(13) -0.0092(14) 0.0021(16) CT2 0.126(3) 0.066(2) 0.105(3) 0.0096(19) -0.010(2) 0.003(2) CT3 0.105(3) 0.167(5) 0.081(2) 0.023(3) -0.032(2) -0.020(3) CT4 0.154(4) 0.108(3) 0.061(2) 0.020(2) 0.022(2) 0.016(3) _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 C01 C02 1.3900 . ? C01 C06 1.3900 . ? C01 C07 1.486(4) . ? C02 C03 1.3900 . ? C03 C04 1.3900 . ? C04 C05 1.3900 . ? C05 C06 1.3900 . ? C07 OU 1.451(4) . ? OU C0 1.358(3) . ? C0 O0 1.212(3) . ? C0 N1 1.337(3) . ? N1 C1A 1.475(3) . ? C1A C1B2 1.519(4) . ? C1A C1 1.528(4) . ? C1A C1B1 1.534(4) . ? C1 O1 1.235(3) . ? C1 N2 1.337(3) . ? N2 C2A 1.439(3) . ? C2A C2B 1.518(4) . ? C2A C2 1.527(4) . ? C2B N1T 1.476(3) . ? N1T C2T 1.370(3) . ? N1T C6T 1.382(3) . ? C2T O2T 1.234(3) . ? C2T N3T 1.359(3) . ? N3T C4T 1.388(3) . ? C4T O4T 1.219(3) . ? C4T C5T 1.449(4) . ? C5T C6T 1.337(4) . ? C5T C7T 1.495(4) . ? C2 O2 1.219(3) . ? C2 N3 1.337(3) . ? N3 C3A 1.466(3) . ? C3A C3B2 1.515(4) . ? C3A C3B1 1.524(4) . ? C3A C3 1.537(4) . ? C3 O3 1.204(4) . ? C3 OT 1.329(3) . ? OT CT1 1.480(3) . ? CT1 CT4 1.506(5) . ? CT1 CT3 1.507(5) . ? CT1 CT2 1.509(5) . ? 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 C02 C01 C06 120.0 . . ? C02 C01 C07 119.7(2) . . ? C06 C01 C07 120.3(2) . . ? C01 C02 C03 120.0 . . ? C02 C03 C04 120.0 . . ? C05 C04 C03 120.0 . . ? C06 C05 C04 120.0 . . ? C05 C06 C01 120.0 . . ? OU C07 C01 109.9(3) . . ? C0 OU C07 116.2(2) . . ? O0 C0 N1 126.1(2) . . ? O0 C0 OU 123.6(2) . . ? N1 C0 OU 110.4(2) . . ? C0 N1 C1A 121.8(2) . . ? N1 C1A C1B2 111.0(2) . . ? N1 C1A C1 110.30(19) . . ? C1B2 C1A C1 111.1(2) . . ? N1 C1A C1B1 106.2(2) . . ? C1B2 C1A C1B1 110.7(2) . . ? C1 C1A C1B1 107.4(2) . . ? O1 C1 N2 121.6(2) . . ? O1 C1 C1A 121.5(2) . . ? N2 C1 C1A 116.8(2) . . ? C1 N2 C2A 123.7(2) . . ? N2 C2A C2B 111.3(2) . . ? N2 C2A C2 115.7(2) . . ? C2B C2A C2 109.8(2) . . ? N1T C2B C2A 115.6(2) . . ? C2T N1T C6T 119.8(2) . . ? C2T N1T C2B 119.5(2) . . ? C6T N1T C2B 120.2(2) . . ? O2T C2T N3T 121.6(2) . . ? O2T C2T N1T 122.5(2) . . ? N3T C2T N1T 115.9(2) . . ? C2T N3T C4T 127.3(2) . . ? O4T C4T N3T 120.0(2) . . ? O4T C4T C5T 125.8(2) . . ? N3T C4T C5T 114.3(2) . . ? C6T C5T C4T 118.1(2) . . ? C6T C5T C7T 123.1(2) . . ? C4T C5T C7T 118.8(2) . . ? C5T C6T N1T 124.3(2) . . ? O2 C2 N3 123.6(2) . . ? O2 C2 C2A 119.0(2) . . ? N3 C2 C2A 117.3(2) . . ? C2 N3 C3A 121.5(2) . . ? N3 C3A C3B2 109.9(3) . . ? N3 C3A C3B1 107.4(2) . . ? C3B2 C3A C3B1 112.0(3) . . ? N3 C3A C3 107.5(2) . . ? C3B2 C3A C3 114.0(2) . . ? C3B1 C3A C3 105.6(3) . . ? O3 C3 OT 125.4(3) . . ? O3 C3 C3A 122.8(3) . . ? OT C3 C3A 111.7(3) . . ? C3 OT CT1 121.3(2) . . ? OT CT1 CT4 102.4(3) . . ? OT CT1 CT3 110.2(3) . . ? CT4 CT1 CT3 112.1(3) . . ? OT CT1 CT2 108.9(2) . . ? CT4 CT1 CT2 110.2(3) . . ? CT3 CT1 CT2 112.5(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 C06 C01 C02 C03 0.0 . . . . ? C07 C01 C02 C03 -178.5(2) . . . . ? C01 C02 C03 C04 0.0 . . . . ? C02 C03 C04 C05 0.0 . . . . ? C03 C04 C05 C06 0.0 . . . . ? C04 C05 C06 C01 0.0 . . . . ? C02 C01 C06 C05 0.0 . . . . ? C07 C01 C06 C05 178.5(2) . . . . ? C02 C01 C07 OU -78.4(3) . . . . y C06 C01 C07 OU 103.1(3) . . . . y C01 C07 OU C0 140.9(3) . . . . y C07 OU C0 O0 -5.1(4) . . . . ? C07 OU C0 N1 175.9(3) . . . . y O0 C0 N1 C1A 4.5(4) . . . . ? OU C0 N1 C1A -176.6(2) . . . . y C0 N1 C1A C1B2 69.0(3) . . . . ? C0 N1 C1A C1 -54.6(3) . . . . y C0 N1 C1A C1B1 -170.6(2) . . . . ? N1 C1A C1 O1 149.0(2) . . . . ? C1B2 C1A C1 O1 25.5(3) . . . . ? C1B1 C1A C1 O1 -95.6(3) . . . . ? N1 C1A C1 N2 -35.0(3) . . . . y C1B2 C1A C1 N2 -158.5(2) . . . . ? C1B1 C1A C1 N2 80.4(3) . . . . ? O1 C1 N2 C2A 4.3(4) . . . . ? C1A C1 N2 C2A -171.7(2) . . . . y C1 N2 C2A C2B 151.3(2) . . . . ? C1 N2 C2A C2 -82.4(3) . . . . y N2 C2A C2B N1T 74.3(3) . . . . y C2 C2A C2B N1T -55.2(3) . . . . ? C2A C2B N1T C2T -84.2(3) . . . . y C2A C2B N1T C6T 103.8(3) . . . . y C6T N1T C2T O2T -174.8(2) . . . . ? C2B N1T C2T O2T 13.1(4) . . . . ? C6T N1T C2T N3T 5.0(3) . . . . ? C2B N1T C2T N3T -167.1(2) . . . . ? O2T C2T N3T C4T 179.7(3) . . . . ? N1T C2T N3T C4T 0.0(4) . . . . ? C2T N3T C4T O4T 175.5(3) . . . . ? C2T N3T C4T C5T -5.2(4) . . . . ? O4T C4T C5T C6T -175.3(3) . . . . ? N3T C4T C5T C6T 5.4(4) . . . . ? O4T C4T C5T C7T 5.0(4) . . . . ? N3T C4T C5T C7T -174.3(3) . . . . ? C4T C5T C6T N1T -1.0(4) . . . . ? C7T C5T C6T N1T 178.7(3) . . . . ? C2T N1T C6T C5T -4.6(4) . . . . ? C2B N1T C6T C5T 167.4(2) . . . . ? N2 C2A C2 O2 174.4(2) . . . . ? C2B C2A C2 O2 -58.6(3) . . . . ? N2 C2A C2 N3 -9.3(3) . . . . y C2B C2A C2 N3 117.7(3) . . . . ? O2 C2 N3 C3A -4.1(4) . . . . ? C2A C2 N3 C3A 179.7(2) . . . . y C2 N3 C3A C3B2 -72.1(3) . . . . ? C2 N3 C3A C3B1 165.8(3) . . . . ? C2 N3 C3A C3 52.6(3) . . . . y N3 C3A C3 O3 41.8(4) . . . . ? C3B2 C3A C3 O3 163.9(3) . . . . ? C3B1 C3A C3 O3 -72.7(4) . . . . ? N3 C3A C3 OT -142.7(2) . . . . y C3B2 C3A C3 OT -20.6(4) . . . . ? C3B1 C3A C3 OT 102.8(3) . . . . ? O3 C3 OT CT1 -4.1(5) . . . . ? C3A C3 OT CT1 -179.5(2) . . . . y C3 OT CT1 CT4 -179.7(3) . . . . y C3 OT CT1 CT3 60.8(4) . . . . y C3 OT CT1 CT2 -63.0(4) . . . . y loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O0 0.86 2.28 3.117(3) 163.8 . N2 H2 O2T 0.86 2.03 2.800(3) 147.9 . N1 H1 O4T 0.86 2.12 2.971(3) 168.8 3_556 N3T H3T O2T 0.86 2.00 2.853(3) 172.0 3_556 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 60.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.201 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.045 #===END===