# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Arindam Banerjee' _publ_contact_author_address ; Department of Biological Chemistry Indian Association for the Cultivation of Science Jadavpur Kolkata 700032 INDIA ; _publ_contact_author_email BCAB@MAHENDRA.IACS.RES.IN _publ_section_title ; X-ray crystallographic signature of supramolecular triple helix formation from a water soluble synthetic tetrapeptide ; loop_ _publ_author_name 'Arindam Banerjee' 'Apurba Kumar Das' 'Debasish Haldar' 'Raghurama P. Hegde' 'N. Shamala' data_yuyv _database_code_depnum_ccdc_archive 'CCDC 235556' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tyrosyl-alpha-aminoisobutyryl-tyrosyl-valine dihydrate ; _chemical_name_common 'Tyrosyl-alpha-aminoisobutyryl-tyrosyl-valine dihydrate' _chemical_melting_point ? _chemical_formula_moiety 'C27 H36 N4 O7, 2(H2 O1)' _chemical_formula_sum 'C27 H40 N4 O9' _chemical_formula_weight 564.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 65' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z+2/3' 'y, -x+y, z+1/6' '-x+y, -x, z+1/3' 'x-y, x, z+5/6' _cell_length_a 8.807(3) _cell_length_b 8.807(3) _cell_length_c 64.67(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4344(3) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'clear diamond shaped' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1812 _exptl_absorpt_coefficient_mu 0.098 _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 32470 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -75 _diffrn_reflns_limit_l_max 77 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.03 _reflns_number_total 5738 _reflns_number_gt 5080 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement ? _computing_data_reduction 'SAINT (Bruker AXS Inc.,1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1053P)^2^+4.5690P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1(2) _refine_ls_number_reflns 5738 _refine_ls_number_parameters 385 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.2307 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.001 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 N1 N -0.0469(6) -0.0383(7) 0.12827(8) 0.0680(13) Uani 1 1 d . . . H1A H -0.0636 -0.1463 0.1293 0.102 Uiso 1 1 calc R . . H1B H -0.1493 -0.0418 0.1295 0.102 Uiso 1 1 calc R . . H1C H 0.0249 0.0284 0.1383 0.102 Uiso 1 1 calc R . . C1A C 0.0308(7) 0.0356(6) 0.10817(9) 0.0529(12) Uani 1 1 d . . . H1A1 H 0.139(7) 0.044(6) 0.1087(8) 0.043(13) Uiso 1 1 d . . . C1' C 0.0574(7) 0.2186(7) 0.10724(8) 0.0525(12) Uani 1 1 d . . . O1 O -0.0521(6) 0.2484(6) 0.11438(8) 0.0767(12) Uani 1 1 d . . . C1B C -0.0900(8) -0.0780(7) 0.09091(10) 0.0725(18) Uani 1 1 d . . . H1B1 H -0.1210 -0.1987 0.0934 0.087 Uiso 1 1 calc R . . H1B2 H -0.1973 -0.0725 0.0914 0.087 Uiso 1 1 calc R . . C1G C -0.0134(9) -0.0267(7) 0.06961(10) 0.0680(16) Uani 1 1 d . . . C1D1 C 0.1162(14) -0.0562(11) 0.06312(12) 0.099(3) Uani 1 1 d . . . H1D1 H 0.1615 -0.1053 0.0722 0.119 Uiso 1 1 calc R . . C1D2 C -0.0731(9) 0.0512(10) 0.05619(11) 0.0761(18) Uani 1 1 d . . . H1D2 H -0.1575 0.0785 0.0604 0.091 Uiso 1 1 calc R . . C1E1 C 0.1800(13) -0.0157(12) 0.04381(13) 0.095(2) Uani 1 1 d . . . H1E1 H 0.2676 -0.0397 0.0400 0.114 Uiso 1 1 calc R . . C1E2 C -0.0064(10) 0.0903(10) 0.03588(11) 0.082(2) Uani 1 1 d . . . H1E2 H -0.0520 0.1384 0.0267 0.098 Uiso 1 1 calc R . . C1Z C 0.1227(10) 0.0596(9) 0.02937(10) 0.0749(17) Uani 1 1 d . . . O1N O 0.1882(9) 0.0964(7) 0.00985(8) 0.1003(17) Uani 1 1 d . . . H1N H 0.1403 0.1408 0.0033 0.150 Uiso 1 1 calc R . . N2 N 0.2045(5) 0.3418(5) 0.09761(6) 0.0443(8) Uani 1 1 d . . . H2 H 0.2818 0.3149 0.0939 0.053 Uiso 1 1 calc R . . C2A C 0.2370(6) 0.5185(6) 0.09338(7) 0.0489(11) Uani 1 1 d . . . C2' C 0.2482(6) 0.6164(7) 0.11324(8) 0.0489(11) Uani 1 1 d . . . O2 O 0.2139(7) 0.7339(6) 0.11350(7) 0.0724(12) Uani 1 1 d . . . C2B1 C 0.0989(11) 0.5122(10) 0.07902(10) 0.0782(19) Uani 1 1 d . . . H2B1 H -0.0138 0.4500 0.0856 0.117 Uiso 1 1 calc R . . H2B2 H 0.0973 0.4532 0.0665 0.117 Uiso 1 1 calc R . . H2B3 H 0.1254 0.6295 0.0759 0.117 Uiso 1 1 calc R . . C2B2 C 0.4133(8) 0.6170(8) 0.08259(10) 0.0674(15) Uani 1 1 d . . . H2B4 H 0.5028 0.6209 0.0914 0.101 Uiso 1 1 calc R . . H2B5 H 0.4392 0.7343 0.0796 0.101 Uiso 1 1 calc R . . H2B6 H 0.4095 0.5581 0.0699 0.101 Uiso 1 1 calc R . . N3 N 0.3155(5) 0.5791(5) 0.12972(6) 0.0454(9) Uani 1 1 d . . . H3 H 0.3414 0.4972 0.1289 0.054 Uiso 1 1 calc R . . C3A C 0.3455(6) 0.6762(6) 0.14898(7) 0.0424(9) Uani 1 1 d . . . H3A H 0.236(6) 0.670(5) 0.1525(7) 0.027(10) Uiso 1 1 d . . . C3' C 0.4807(6) 0.8702(6) 0.14520(8) 0.0469(10) Uani 1 1 d . . . O3 O 0.6062(5) 0.9073(5) 0.13473(7) 0.0667(11) Uani 1 1 d . . . C3B C 0.4068(9) 0.5948(7) 0.16543(8) 0.0591(14) Uani 1 1 d . . . H3B1 H 0.5273 0.6272 0.1625 0.071 Uiso 1 1 calc R . . H3B2 H 0.3363 0.4682 0.1644 0.071 Uiso 1 1 calc R . . C3G C 0.3964(8) 0.6488(7) 0.18745(8) 0.0554(12) Uani 1 1 d . . . C3D1 C 0.2417(9) 0.5718(9) 0.19727(11) 0.089(2) Uani 1 1 d . . . H3D1 H 0.1427 0.4887 0.1902 0.107 Uiso 1 1 calc R . . C3D2 C 0.5391(8) 0.7695(9) 0.19846(9) 0.0655(15) Uani 1 1 d . . . H3D2 H 0.6487 0.8246 0.1922 0.079 Uiso 1 1 calc R . . C3E1 C 0.2237(10) 0.6117(10) 0.21773(10) 0.086(2) Uani 1 1 d . . . H3E1 H 0.1149 0.5563 0.2242 0.103 Uiso 1 1 calc R . . C3E2 C 0.5241(9) 0.8114(9) 0.21868(10) 0.0705(16) Uani 1 1 d . . . H3E2 H 0.6228 0.8942 0.2258 0.085 Uiso 1 1 calc R . . C3Z C 0.3687(8) 0.7332(8) 0.22792(8) 0.0599(14) Uani 1 1 d . . . O3N O 0.3553(7) 0.7842(7) 0.24803(7) 0.0871(15) Uani 1 1 d . . . H3N H 0.2535 0.7268 0.2520 0.131 Uiso 1 1 calc R . . N4 N 0.4478(6) 0.9834(5) 0.15444(6) 0.0496(9) Uani 1 1 d . . . H4 H 0.3630 0.9442 0.1632 0.060 Uiso 1 1 calc R . . C4A C 0.5474(7) 1.1727(6) 0.15065(8) 0.0481(10) Uani 1 1 d . . . H4A H 0.6259 1.1909 0.1390 0.058 Uiso 1 1 calc R . . C4' C 0.4228(7) 1.2374(6) 0.14362(8) 0.0492(11) Uani 1 1 d . . . O4 O 0.2680(5) 1.1625(5) 0.14990(6) 0.0633(10) Uani 1 1 d . . . C4B C 0.6628(9) 1.2802(8) 0.16858(10) 0.0725(18) Uani 1 1 d . . . H4B H 0.7203 1.4043 0.1647 0.087 Uiso 1 1 calc R . . C4G1 C 0.5561(13) 1.2553(12) 0.18779(11) 0.097(3) Uani 1 1 d . . . H4G1 H 0.6323 1.3249 0.1988 0.146 Uiso 1 1 calc R . . H4G2 H 0.4966 1.1339 0.1917 0.146 Uiso 1 1 calc R . . H4G3 H 0.4715 1.2912 0.1851 0.146 Uiso 1 1 calc R . . C4G2 C 0.8068(12) 1.2328(13) 0.17285(16) 0.112(3) Uani 1 1 d . . . H4G4 H 0.8749 1.2513 0.1605 0.167 Uiso 1 1 calc R . . H4G5 H 0.7532 1.1120 0.1769 0.167 Uiso 1 1 calc R . . H4G6 H 0.8817 1.3057 0.1838 0.167 Uiso 1 1 calc R . . O5 O 0.4908(6) 1.3701(5) 0.13222(7) 0.0700(11) Uani 1 1 d . . . O1W O 0.8438(8) 1.6111(8) 0.12740(12) 0.1067(19) Uani 1 1 d D . . H1W1 H 0.931(5) 1.577(7) 0.1288(14) 0.10(3) Uiso 1 1 d D . . H1W2 H 0.734(3) 1.503(4) 0.1280(12) 0.08(2) Uiso 1 1 d D . . O2W O 0.0609(9) 0.5269(11) 0.26517(9) 0.126(3) Uani 1 1 d D . . H2W1 H -0.05(2) 0.47(2) 0.258(5) 1.7(15) Uiso 1 1 d D . . H2W2 H 0.08(2) 0.432(14) 0.268(3) 0.20(8) Uiso 1 1 d 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 N1 0.051(2) 0.066(3) 0.060(3) 0.010(2) -0.005(2) 0.009(2) C1A 0.040(2) 0.040(2) 0.067(3) 0.006(2) -0.004(2) 0.012(2) C1' 0.049(3) 0.052(3) 0.040(3) -0.003(2) -0.004(2) 0.014(2) O1 0.063(2) 0.079(3) 0.087(3) 0.014(2) 0.021(2) 0.035(2) C1B 0.064(3) 0.045(3) 0.070(4) 0.014(3) -0.011(3) -0.002(3) C1G 0.071(4) 0.040(3) 0.066(4) -0.001(2) -0.013(3) 0.007(3) C1D1 0.165(9) 0.084(5) 0.067(5) 0.026(4) 0.019(5) 0.076(6) C1D2 0.062(4) 0.089(5) 0.062(4) 0.006(3) -0.006(3) 0.027(3) C1E1 0.130(7) 0.107(6) 0.077(5) 0.016(4) 0.010(5) 0.081(5) C1E2 0.091(5) 0.085(5) 0.058(4) 0.004(3) -0.021(4) 0.035(4) C1Z 0.089(5) 0.075(4) 0.051(3) 0.005(3) 0.006(3) 0.033(4) O1N 0.133(5) 0.086(3) 0.073(3) 0.009(3) -0.003(3) 0.048(3) N2 0.046(2) 0.043(2) 0.037(2) -0.0013(15) 0.0000(16) 0.0177(17) C2A 0.049(3) 0.049(3) 0.035(2) -0.0038(19) 0.0004(19) 0.015(2) C2' 0.049(2) 0.048(3) 0.054(3) 0.000(2) 0.003(2) 0.028(2) O2 0.107(3) 0.087(3) 0.058(2) 0.000(2) -0.001(2) 0.075(3) C2B1 0.107(5) 0.075(4) 0.057(4) -0.004(3) -0.026(3) 0.048(4) C2B2 0.068(4) 0.055(3) 0.062(3) 0.019(3) 0.018(3) 0.018(3) N3 0.059(2) 0.044(2) 0.037(2) -0.0029(16) -0.0024(16) 0.0282(18) C3A 0.056(3) 0.039(2) 0.038(2) 0.0043(17) 0.008(2) 0.028(2) C3' 0.053(3) 0.044(2) 0.048(3) 0.007(2) 0.001(2) 0.027(2) O3 0.053(2) 0.060(2) 0.082(3) 0.008(2) 0.027(2) 0.0243(18) C3B 0.087(4) 0.046(3) 0.048(3) 0.007(2) -0.007(3) 0.036(3) C3G 0.075(3) 0.050(3) 0.043(3) 0.003(2) -0.002(2) 0.032(3) C3D1 0.062(4) 0.077(4) 0.063(4) -0.017(3) -0.001(3) -0.015(3) C3D2 0.064(3) 0.082(4) 0.046(3) 0.006(3) -0.001(2) 0.033(3) C3E1 0.072(4) 0.082(4) 0.057(4) -0.006(3) 0.011(3) 0.003(3) C3E2 0.071(4) 0.077(4) 0.055(3) -0.009(3) -0.004(3) 0.030(3) C3Z 0.071(3) 0.061(3) 0.034(3) 0.007(2) 0.003(2) 0.023(3) O3N 0.089(3) 0.089(3) 0.048(2) -0.013(2) 0.007(2) 0.018(3) N4 0.059(2) 0.044(2) 0.047(2) 0.0024(17) 0.0017(18) 0.0275(19) C4A 0.054(3) 0.039(2) 0.051(3) 0.0037(19) 0.000(2) 0.023(2) C4' 0.061(3) 0.047(3) 0.038(2) -0.011(2) -0.008(2) 0.026(2) O4 0.057(2) 0.069(2) 0.063(2) -0.0049(19) -0.0075(18) 0.0311(19) C4B 0.074(4) 0.050(3) 0.071(4) -0.011(3) -0.032(3) 0.014(3) C4G1 0.127(7) 0.103(6) 0.049(4) -0.017(4) -0.021(4) 0.048(5) C4G2 0.084(5) 0.113(6) 0.123(8) -0.027(6) -0.051(5) 0.039(5) O5 0.099(3) 0.063(2) 0.067(2) 0.015(2) 0.011(2) 0.054(2) O1W 0.088(3) 0.093(4) 0.142(5) 0.032(4) 0.034(4) 0.047(3) O2W 0.097(4) 0.127(6) 0.065(3) 0.010(3) 0.006(3) -0.011(4) _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 N1 C1A 1.462(7) . ? C1A C1' 1.509(8) . ? C1A C1B 1.521(8) . ? C1' O1 1.210(7) . ? C1' N2 1.356(6) . ? C1B C1G 1.501(9) . ? C1G C1D1 1.357(12) . ? C1G C1D2 1.364(10) . ? C1D1 C1E1 1.342(11) . ? C1D2 C1E2 1.409(10) . ? C1E1 C1Z 1.379(11) . ? C1E2 C1Z 1.361(11) . ? C1Z O1N 1.358(9) . ? N2 C2A 1.461(7) . ? C2A C2B1 1.509(8) . ? C2A C2B2 1.518(8) . ? C2A C2' 1.522(7) . ? C2' O2 1.214(6) . ? C2' N3 1.338(6) . ? N3 C3A 1.458(6) . ? C3A C3B 1.525(7) . ? C3A C3' 1.537(7) . ? C3' O3 1.194(6) . ? C3' N4 1.313(6) . ? C3B C3G 1.518(8) . ? C3G C3D1 1.340(9) . ? C3G C3D2 1.371(8) . ? C3D1 C3E1 1.398(9) . ? C3D2 C3E2 1.383(9) . ? C3E1 C3Z 1.358(9) . ? C3E2 C3Z 1.328(9) . ? C3Z O3N 1.400(7) . ? N4 C4A 1.465(6) . ? C4A C4B 1.520(7) . ? C4A C4' 1.537(7) . ? C4' O4 1.249(7) . ? C4' O5 1.252(7) . ? C4B C4G1 1.506(11) . ? C4B C4G2 1.546(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1A C1' 107.4(5) . . ? N1 C1A C1B 110.0(4) . . ? C1' C1A C1B 110.9(5) . . ? O1 C1' N2 123.2(5) . . ? O1 C1' C1A 120.1(5) . . ? N2 C1' C1A 116.7(5) . . ? C1G C1B C1A 114.4(5) . . ? C1D1 C1G C1D2 118.1(7) . . ? C1D1 C1G C1B 121.4(6) . . ? C1D2 C1G C1B 120.4(7) . . ? C1E1 C1D1 C1G 121.2(8) . . ? C1G C1D2 C1E2 119.8(8) . . ? C1D1 C1E1 C1Z 123.5(8) . . ? C1Z C1E2 C1D2 121.8(7) . . ? C1E2 C1Z O1N 122.5(7) . . ? C1E2 C1Z C1E1 115.4(7) . . ? O1N C1Z C1E1 122.1(8) . . ? C1' N2 C2A 122.6(4) . . ? N2 C2A C2B1 110.6(4) . . ? N2 C2A C2B2 107.1(5) . . ? C2B1 C2A C2B2 108.3(5) . . ? N2 C2A C2' 111.6(4) . . ? C2B1 C2A C2' 111.3(5) . . ? C2B2 C2A C2' 107.8(4) . . ? O2 C2' N3 121.8(5) . . ? O2 C2' C2A 121.4(5) . . ? N3 C2' C2A 116.4(4) . . ? C2' N3 C3A 120.6(4) . . ? N3 C3A C3B 108.9(4) . . ? N3 C3A C3' 109.1(4) . . ? C3B C3A C3' 112.0(4) . . ? O3 C3' N4 125.2(5) . . ? O3 C3' C3A 119.4(4) . . ? N4 C3' C3A 115.4(4) . . ? C3A C3B C3G 114.6(5) . . ? C3D1 C3G C3D2 116.9(5) . . ? C3D1 C3G C3B 119.4(5) . . ? C3D2 C3G C3B 123.6(5) . . ? C3G C3D1 C3E1 122.4(6) . . ? C3G C3D2 C3E2 121.7(6) . . ? C3Z C3E1 C3D1 118.5(6) . . ? C3Z C3E2 C3D2 119.9(6) . . ? C3E2 C3Z C3E1 120.6(6) . . ? C3E2 C3Z O3N 118.8(5) . . ? C3E1 C3Z O3N 120.5(6) . . ? C3' N4 C4A 123.6(4) . . ? N4 C4A C4B 114.5(4) . . ? N4 C4A C4' 109.8(4) . . ? C4B C4A C4' 111.9(4) . . ? O4 C4' O5 124.8(5) . . ? O4 C4' C4A 120.1(5) . . ? O5 C4' C4A 115.0(5) . . ? C4G1 C4B C4A 111.4(5) . . ? C4G1 C4B C4G2 110.5(7) . . ? C4A C4B C4G2 110.6(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1A C1' O1 -39.3(7) . . . . ? C1B C1A C1' O1 80.9(7) . . . . ? N1 C1A C1' N2 142.6(4) . . . . y C1B C1A C1' N2 -97.1(6) . . . . ? N1 C1A C1B C1G -172.8(6) . . . . y C1' C1A C1B C1G 68.5(7) . . . . ? C1A C1B C1G C1D1 71.9(9) . . . . y C1A C1B C1G C1D2 -108.2(7) . . . . y C1D2 C1G C1D1 C1E1 -2.3(12) . . . . ? C1B C1G C1D1 C1E1 177.6(7) . . . . ? C1D1 C1G C1D2 C1E2 3.2(10) . . . . ? C1B C1G C1D2 C1E2 -176.7(6) . . . . ? C1G C1D1 C1E1 C1Z 0.9(15) . . . . ? C1G C1D2 C1E2 C1Z -3.0(11) . . . . ? C1D2 C1E2 C1Z O1N 179.9(7) . . . . ? C1D2 C1E2 C1Z C1E1 1.5(11) . . . . ? C1D1 C1E1 C1Z C1E2 -0.5(13) . . . . ? C1D1 C1E1 C1Z O1N -178.9(8) . . . . ? O1 C1' N2 C2A -5.5(8) . . . . ? C1A C1' N2 C2A 172.5(4) . . . . y C1' N2 C2A C2B1 -62.3(6) . . . . ? C1' N2 C2A C2B2 179.9(5) . . . . ? C1' N2 C2A C2' 62.1(6) . . . . y N2 C2A C2' O2 -154.1(5) . . . . ? C2B1 C2A C2' O2 -30.1(7) . . . . ? C2B2 C2A C2' O2 88.5(6) . . . . ? N2 C2A C2' N3 32.9(6) . . . . y C2B1 C2A C2' N3 156.9(5) . . . . ? C2B2 C2A C2' N3 -84.5(6) . . . . ? O2 C2' N3 C3A 1.9(8) . . . . ? C2A C2' N3 C3A 174.9(4) . . . . y C2' N3 C3A C3B 175.0(5) . . . . ? C2' N3 C3A C3' -62.6(6) . . . . y N3 C3A C3' O3 -41.8(6) . . . . ? C3B C3A C3' O3 78.8(6) . . . . ? N3 C3A C3' N4 139.5(4) . . . . y C3B C3A C3' N4 -99.9(5) . . . . ? N3 C3A C3B C3G -164.3(4) . . . . y C3' C3A C3B C3G 74.9(6) . . . . ? C3A C3B C3G C3D1 79.4(7) . . . . y C3A C3B C3G C3D2 -103.0(7) . . . . y C3D2 C3G C3D1 C3E1 0.5(12) . . . . ? C3B C3G C3D1 C3E1 178.2(7) . . . . ? C3D1 C3G C3D2 C3E2 -0.7(10) . . . . ? C3B C3G C3D2 C3E2 -178.3(6) . . . . ? C3G C3D1 C3E1 C3Z 0.1(13) . . . . ? C3G C3D2 C3E2 C3Z 0.4(10) . . . . ? C3D2 C3E2 C3Z C3E1 0.2(11) . . . . ? C3D2 C3E2 C3Z O3N -176.8(6) . . . . ? C3D1 C3E1 C3Z C3E2 -0.4(12) . . . . ? C3D1 C3E1 C3Z O3N 176.5(7) . . . . ? O3 C3' N4 C4A 9.7(8) . . . . ? C3A C3' N4 C4A -171.7(4) . . . . y C3' N4 C4A C4B -109.9(6) . . . . ? C3' N4 C4A C4' 123.2(5) . . . . y N4 C4A C4' O4 30.7(6) . . . . ? C4B C4A C4' O4 -97.7(6) . . . . ? N4 C4A C4' O5 -151.9(4) . . . . y C4B C4A C4' O5 79.8(6) . . . . ? N4 C4A C4B C4G1 -59.5(7) . . . . y C4' C4A C4B C4G1 66.3(7) . . . . ? N4 C4A C4B C4G2 63.7(8) . . . . y C4' C4A C4B C4G2 -170.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.240 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.054