Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'John Ripmeester' _publ_contact_author_address ; Steacie Institute for Molecular Sciences National Research Council Ottawa Ontario K1A 0R6 CANADA ; _publ_contact_author_email JOHN.RIPMEESTER@NRC.CA _publ_section_title ; The ability of lower peptides to form co-crystals: Inclusion compounds of Leu-Leu-Leu tripeptide with pyridine and picolines ; loop_ _publ_author_name 'John Ripmeester' 'Tara Burchell' 'Gary D. Enright' 'Dmitriy V. Soldatov' data_1 _database_code_depnum_ccdc_archive 'CCDC 642087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_formula_sum 'C23 H40 N4 O4' _chemical_formula_weight 436.59 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5399(9) _cell_length_b 12.0328(11) _cell_length_c 12.2882(12) _cell_angle_alpha 101.156(4) _cell_angle_beta 100.498(4) _cell_angle_gamma 99.211(4) _cell_volume 1332.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7972 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9779 _exptl_absorpt_correction_T_max 0.9970 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6760 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6760 _reflns_number_gt 5386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1173P)^2^+0.4624P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details rm _refine_ls_number_reflns 6760 _refine_ls_number_parameters 1061 _refine_ls_number_restraints 2892 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2169 _refine_ls_wR_factor_gt 0.1945 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _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 O1 O 0.3991(8) 0.5852(6) 0.8118(5) 0.0346(15) Uani 0.589(4) 1 d PU A 1 O2 O -0.0327(6) 0.2943(5) 0.7828(4) 0.0350(13) Uani 0.589(4) 1 d PU A 1 O3 O 0.2896(6) 0.0321(4) 0.7666(4) 0.0509(14) Uani 0.589(4) 1 d PU A 1 O4 O 0.0722(5) -0.0792(4) 0.7603(4) 0.0568(13) Uani 0.589(4) 1 d PU A 1 N1 N 0.2985(10) 0.7870(7) 0.7991(6) 0.0421(18) Uani 0.589(4) 1 d PDU A 1 H1A H 0.2627 0.8424 0.7683 0.063 Uiso 0.589(4) 1 calc PR A 1 H1B H 0.3917 0.7887 0.7910 0.063 Uiso 0.589(4) 1 calc PR A 1 H1C H 0.2969 0.8005 0.8743 0.063 Uiso 0.589(4) 1 calc PR A 1 N2 N 0.1688(8) 0.5060(6) 0.8194(5) 0.0295(14) Uani 0.589(4) 1 d PU A 1 H2A H 0.0782 0.5152 0.8131 0.035 Uiso 0.589(4) 1 calc PR A 1 N3 N 0.1604(9) 0.2092(7) 0.7589(5) 0.0228(13) Uani 0.589(4) 1 d PU A 1 H3A H 0.2557 0.2182 0.7704 0.027 Uiso 0.589(4) 1 calc PR A 1 C1 C 0.2075(12) 0.6716(9) 0.7400(7) 0.040(2) Uani 0.589(4) 1 d PDU A 1 H1D H 0.1067 0.6701 0.7528 0.048 Uiso 0.589(4) 1 calc PR A 1 C2 C 0.2663(12) 0.5833(9) 0.7900(6) 0.0292(18) Uani 0.589(4) 1 d PU A 1 C3 C 0.2100(14) 0.4096(13) 0.8606(7) 0.0298(18) Uani 0.589(4) 1 d PDU A 1 H3B H 0.3107 0.4036 0.8514 0.036 Uiso 0.589(4) 1 calc PR A 1 C4 C 0.1047(12) 0.3017(9) 0.7944(6) 0.0296(17) Uani 0.589(4) 1 d PU A 1 C5 C 0.0722(9) 0.0928(6) 0.7019(5) 0.0328(14) Uani 0.589(4) 1 d PDU A 1 H5A H -0.0196 0.0861 0.7307 0.039 Uiso 0.589(4) 1 calc PR A 1 C6 C 0.1495(10) 0.0006(8) 0.7390(6) 0.0283(16) Uani 0.589(4) 1 d PU A 1 C7 C 0.2003(12) 0.6553(9) 0.6121(7) 0.049(2) Uani 0.589(4) 1 d PDU A 1 H7A H 0.1628 0.7203 0.5868 0.058 Uiso 0.589(4) 1 calc PR A 1 H7B H 0.3007 0.6604 0.5997 0.058 Uiso 0.589(4) 1 calc PR A 1 C8 C 0.1065(13) 0.5421(9) 0.5366(11) 0.057(2) Uani 0.589(4) 1 d PDU A 1 H8A H 0.0216 0.5193 0.5704 0.068 Uiso 0.589(4) 1 calc PR A 1 C9 C 0.1921(13) 0.4450(10) 0.5278(12) 0.069(3) Uani 0.589(4) 1 d PDU A 1 H9A H 0.1304 0.3746 0.4765 0.103 Uiso 0.589(4) 1 calc PR A 1 H9B H 0.2228 0.4302 0.6033 0.103 Uiso 0.589(4) 1 calc PR A 1 H9C H 0.2782 0.4678 0.4979 0.103 Uiso 0.589(4) 1 calc PR A 1 C10 C 0.0497(15) 0.5574(13) 0.4176(12) 0.084(3) Uani 0.589(4) 1 d PDU A 1 H10A H -0.0007 0.6225 0.4225 0.126 Uiso 0.589(4) 1 calc PR A 1 H10B H -0.0183 0.4866 0.3728 0.126 Uiso 0.589(4) 1 calc PR A 1 H10C H 0.1314 0.5729 0.3809 0.126 Uiso 0.589(4) 1 calc PR A 1 C11 C 0.2060(11) 0.4322(7) 0.9839(6) 0.0452(18) Uani 0.589(4) 1 d PDU A 1 H11A H 0.1103 0.4510 0.9910 0.054 Uiso 0.589(4) 1 calc PR A 1 H11B H 0.2810 0.5021 1.0238 0.054 Uiso 0.589(4) 1 calc PR A 1 C12 C 0.2293(5) 0.3378(5) 1.0464(4) 0.0524(14) Uani 0.589(4) 1 d PDU A 1 H12A H 0.1559 0.2657 1.0064 0.063 Uiso 0.589(4) 1 calc PR A 1 C13 C 0.2096(6) 0.3751(7) 1.1667(5) 0.082(2) Uani 0.589(4) 1 d PDU A 1 H13A H 0.1108 0.3888 1.1646 0.124 Uiso 0.589(4) 1 calc PR A 1 H13B H 0.2804 0.4464 1.2058 0.124 Uiso 0.589(4) 1 calc PR A 1 H13C H 0.2251 0.3141 1.2074 0.124 Uiso 0.589(4) 1 calc PR A 1 C14 C 0.3813(5) 0.3131(5) 1.0505(5) 0.0620(16) Uani 0.589(4) 1 d PDU A 1 H14A H 0.3952 0.2897 0.9729 0.093 Uiso 0.589(4) 1 calc PR A 1 H14B H 0.3931 0.2506 1.0900 0.093 Uiso 0.589(4) 1 calc PR A 1 H14C H 0.4538 0.3829 1.0914 0.093 Uiso 0.589(4) 1 calc PR A 1 C15 C 0.0272(10) 0.0783(6) 0.5741(5) 0.096(2) Uani 0.589(4) 1 d PDU A 1 H15A H -0.0551 0.1182 0.5604 0.116 Uiso 0.589(4) 1 calc PR A 1 H15B H 0.1092 0.1222 0.5508 0.116 Uiso 0.589(4) 1 calc PR A 1 C16 C -0.0165(10) -0.0371(8) 0.4933(7) 0.122(3) Uani 0.589(4) 1 d PDU A 1 H16A H -0.0612 -0.0936 0.5334 0.147 Uiso 0.589(4) 1 calc PR A 1 C17 C -0.1297(13) -0.0325(12) 0.3944(9) 0.177(5) Uani 0.589(4) 1 d PDU A 1 H17A H -0.1484 -0.1048 0.3363 0.266 Uiso 0.589(4) 1 calc PR A 1 H17B H -0.0956 0.0327 0.3624 0.266 Uiso 0.589(4) 1 calc PR A 1 H17C H -0.2197 -0.0224 0.4193 0.266 Uiso 0.589(4) 1 calc PR A 1 C18 C 0.1126(11) -0.0771(9) 0.4597(9) 0.141(3) Uani 0.589(4) 1 d PDU A 1 H18A H 0.0830 -0.1568 0.4141 0.211 Uiso 0.589(4) 1 calc PR A 1 H18B H 0.1858 -0.0740 0.5281 0.211 Uiso 0.589(4) 1 calc PR A 1 H18C H 0.1541 -0.0268 0.4148 0.211 Uiso 0.589(4) 1 calc PR A 1 O1A O 0.3830(11) 0.5708(8) 0.7685(6) 0.0244(18) Uani 0.411(4) 1 d PU A 2 O2A O -0.0389(9) 0.2870(7) 0.7317(5) 0.0320(18) Uani 0.411(4) 1 d PU A 2 O3A O 0.2730(10) 0.0001(7) 0.7153(7) 0.057(2) Uani 0.411(4) 1 d PU A 2 O4A O 0.0819(8) -0.0963(6) 0.6941(7) 0.068(2) Uani 0.411(4) 1 d PU A 2 N1A N 0.2777(13) 0.7764(9) 0.7573(7) 0.033(2) Uani 0.411(4) 1 d PDU A 2 H1A1 H 0.2819 0.7913 0.8334 0.049 Uiso 0.411(4) 1 calc PR A 2 H1A2 H 0.2379 0.8306 0.7271 0.049 Uiso 0.411(4) 1 calc PR A 2 H1A3 H 0.3691 0.7787 0.7448 0.049 Uiso 0.411(4) 1 calc PR A 2 N2A N 0.1603(13) 0.4982(10) 0.7882(7) 0.0218(18) Uani 0.411(4) 1 d PU A 2 H2AA H 0.0694 0.5069 0.7771 0.026 Uiso 0.411(4) 1 calc PR A 2 N3A N 0.1514(15) 0.1994(12) 0.7229(8) 0.032(2) Uani 0.411(4) 1 d PU A 2 H3AA H 0.2467 0.2082 0.7415 0.039 Uiso 0.411(4) 1 calc PR A 2 C1A C 0.1886(16) 0.6625(11) 0.7039(10) 0.033(2) Uani 0.411(4) 1 d PDU A 2 H1AC H 0.0883 0.6626 0.7174 0.039 Uiso 0.411(4) 1 calc PR A 2 C2A C 0.2485(17) 0.5715(15) 0.7584(10) 0.032(2) Uani 0.411(4) 1 d PU A 2 C3A C 0.191(2) 0.3986(19) 0.8396(11) 0.029(2) Uani 0.411(4) 1 d PDU A 2 H3AB H 0.2941 0.3930 0.8389 0.035 Uiso 0.411(4) 1 calc PR A 2 C4A C 0.0938(16) 0.2886(13) 0.7597(9) 0.028(2) Uani 0.411(4) 1 d PU A 2 C5A C 0.0714(16) 0.0908(11) 0.6560(8) 0.048(2) Uani 0.411(4) 1 d PDU A 2 H5AA H -0.0331 0.0761 0.6610 0.058 Uiso 0.411(4) 1 calc PR A 2 C6A C 0.1524(19) 0.0040(14) 0.6961(10) 0.051(3) Uani 0.411(4) 1 d PU A 2 C7A C 0.1768(17) 0.6311(13) 0.5760(10) 0.045(2) Uani 0.411(4) 1 d PDU A 2 H7AA H 0.1412 0.6928 0.5428 0.054 Uiso 0.411(4) 1 calc PR A 2 H7AB H 0.2752 0.6289 0.5616 0.054 Uiso 0.411(4) 1 calc PR A 2 C8A C 0.076(2) 0.5159(13) 0.5155(16) 0.058(3) Uani 0.411(4) 1 d PDU A 2 H8AA H -0.0029 0.5021 0.5574 0.070 Uiso 0.411(4) 1 calc PR A 2 C9A C 0.151(2) 0.4125(14) 0.506(2) 0.077(4) Uani 0.411(4) 1 d PDU A 2 H9AA H 0.1925 0.4044 0.5826 0.115 Uiso 0.411(4) 1 calc PR A 2 H9AB H 0.2284 0.4244 0.4648 0.115 Uiso 0.411(4) 1 calc PR A 2 H9AC H 0.0792 0.3421 0.4653 0.115 Uiso 0.411(4) 1 calc PR A 2 C10A C 0.007(2) 0.5223(18) 0.3952(15) 0.078(4) Uani 0.411(4) 1 d PDU A 2 H10D H -0.0312 0.5933 0.3981 0.118 Uiso 0.411(4) 1 calc PR A 2 H10E H -0.0720 0.4550 0.3612 0.118 Uiso 0.411(4) 1 calc PR A 2 H10F H 0.0810 0.5226 0.3491 0.118 Uiso 0.411(4) 1 calc PR A 2 C11A C 0.1731(16) 0.4064(10) 0.9602(9) 0.041(2) Uani 0.411(4) 1 d PDU A 2 H11C H 0.2045 0.3390 0.9848 0.049 Uiso 0.411(4) 1 calc PR A 2 H11D H 0.0678 0.3978 0.9590 0.049 Uiso 0.411(4) 1 calc PR A 2 C12A C 0.2519(7) 0.5138(8) 1.0509(6) 0.068(2) Uani 0.411(4) 1 d PDU A 2 H12B H 0.2184 0.5819 1.0271 0.082 Uiso 0.411(4) 1 calc PR A 2 C13A C 0.2106(9) 0.5072(9) 1.1643(6) 0.083(3) Uani 0.411(4) 1 d PDU A 2 H13D H 0.2582 0.5786 1.2211 0.124 Uiso 0.411(4) 1 calc PR A 2 H13E H 0.2424 0.4411 1.1898 0.124 Uiso 0.411(4) 1 calc PR A 2 H13F H 0.1048 0.4975 1.1547 0.124 Uiso 0.411(4) 1 calc PR A 2 C14A C 0.4127(8) 0.5332(9) 1.0633(8) 0.085(3) Uani 0.411(4) 1 d PDU A 2 H14D H 0.4368 0.5420 0.9908 0.128 Uiso 0.411(4) 1 calc PR A 2 H14E H 0.4483 0.4669 1.0851 0.128 Uiso 0.411(4) 1 calc PR A 2 H14F H 0.4588 0.6035 1.1222 0.128 Uiso 0.411(4) 1 calc PR A 2 C15A C 0.0921(8) 0.0755(6) 0.5331(6) 0.0463(18) Uani 0.411(4) 1 d PDU A 2 H15C H 0.0470 0.1317 0.4969 0.056 Uiso 0.411(4) 1 calc PR A 2 H15D H 0.1973 0.0913 0.5336 0.056 Uiso 0.411(4) 1 calc PR A 2 C16A C 0.0242(8) -0.0447(9) 0.4659(9) 0.085(3) Uani 0.411(4) 1 d PDU A 2 H16B H 0.0422 -0.0969 0.5188 0.102 Uiso 0.411(4) 1 calc PR A 2 C17A C -0.1382(7) -0.0569(7) 0.4331(8) 0.047(2) Uani 0.411(4) 1 d PDU A 2 H17D H -0.1858 -0.1198 0.4622 0.070 Uiso 0.411(4) 1 calc PR A 2 H17E H -0.1695 -0.0744 0.3501 0.070 Uiso 0.411(4) 1 calc PR A 2 H17F H -0.1650 0.0156 0.4657 0.070 Uiso 0.411(4) 1 calc PR A 2 C18A C 0.0899(15) -0.0833(11) 0.3702(11) 0.141(3) Uani 0.411(4) 1 d PDU A 2 H18D H 0.0161 -0.1381 0.3092 0.211 Uiso 0.411(4) 1 calc PR A 2 H18E H 0.1695 -0.1211 0.3954 0.211 Uiso 0.411(4) 1 calc PR A 2 H18F H 0.1280 -0.0164 0.3420 0.211 Uiso 0.411(4) 1 calc PR A 2 N21 N 0.5765(7) 0.0819(5) 0.7552(4) 0.0323(12) Uani 0.710(5) 1 d PDU B 1 H21A H 0.5891 0.0143 0.7137 0.048 Uiso 0.710(5) 1 calc PR B 1 H21B H 0.4811 0.0762 0.7581 0.048 Uiso 0.710(5) 1 calc PR B 1 H21C H 0.6318 0.0963 0.8269 0.048 Uiso 0.710(5) 1 calc PR B 1 N22 N 0.7102(7) 0.3781(5) 0.8020(4) 0.0331(12) Uani 0.710(5) 1 d PU B 1 H22A H 0.7952 0.3660 0.7898 0.040 Uiso 0.710(5) 1 calc PR B 1 N23 N 0.6897(7) 0.6472(5) 0.7539(4) 0.0281(12) Uani 0.710(5) 1 d PU B 1 H23A H 0.6003 0.6424 0.7644 0.034 Uiso 0.710(5) 1 calc PR B 1 O21 O 0.4781(6) 0.2952(4) 0.7950(4) 0.0348(11) Uani 0.710(5) 1 d PU B 1 O22 O 0.8920(6) 0.5749(5) 0.7772(4) 0.0322(11) Uani 0.710(5) 1 d PU B 1 O23 O 0.5810(6) 0.8341(4) 0.7791(4) 0.0404(12) Uani 0.710(5) 1 d PU B 1 O24 O 0.7051(5) 0.9162(4) 0.6686(4) 0.0513(12) Uani 0.710(5) 1 d PU B 1 C21 C 0.6216(10) 0.1783(6) 0.7006(5) 0.0295(14) Uani 0.710(5) 1 d PDU B 1 H21D H 0.7274 0.1854 0.7004 0.035 Uiso 0.710(5) 1 calc PR B 1 C22 C 0.5997(7) 0.2900(6) 0.7709(4) 0.0237(13) Uani 0.710(5) 1 d PU B 1 C23 C 0.7005(10) 0.4934(7) 0.8549(5) 0.0298(14) Uani 0.710(5) 1 d PDU B 1 H23B H 0.5961 0.4987 0.8507 0.036 Uiso 0.710(5) 1 calc PR B 1 C24 C 0.7685(9) 0.5740(7) 0.7910(5) 0.0277(14) Uani 0.710(5) 1 d PU B 1 C25 C 0.7462(8) 0.7351(6) 0.6965(4) 0.0326(14) Uani 0.710(5) 1 d PDU B 1 H25A H 0.8509 0.7657 0.7352 0.039 Uiso 0.710(5) 1 calc PR B 1 C26 C 0.6683(9) 0.8367(7) 0.7137(5) 0.0367(16) Uani 0.710(5) 1 d PU B 1 C27 C 0.5355(12) 0.1523(8) 0.5780(5) 0.0446(16) Uani 0.710(5) 1 d PDU B 1 H27A H 0.4310 0.1410 0.5801 0.053 Uiso 0.710(5) 1 calc PR B 1 H27B H 0.5521 0.0772 0.5387 0.053 Uiso 0.710(5) 1 calc PR B 1 C28 C 0.5628(9) 0.2390(6) 0.5022(7) 0.0582(19) Uani 0.710(5) 1 d PDU B 1 H28A H 0.5576 0.3173 0.5450 0.070 Uiso 0.710(5) 1 calc PR B 1 C29 C 0.4478(14) 0.2083(8) 0.3886(9) 0.080(3) Uani 0.710(5) 1 d PDU B 1 H29A H 0.4732 0.2625 0.3418 0.121 Uiso 0.710(5) 1 calc PR B 1 H29B H 0.3517 0.2136 0.4043 0.121 Uiso 0.710(5) 1 calc PR B 1 H29C H 0.4457 0.1293 0.3478 0.121 Uiso 0.710(5) 1 calc PR B 1 C30 C 0.7169(12) 0.2455(8) 0.4767(9) 0.083(3) Uani 0.710(5) 1 d PDU B 1 H30A H 0.7292 0.2958 0.4238 0.124 Uiso 0.710(5) 1 calc PR B 1 H30B H 0.7284 0.1678 0.4425 0.124 Uiso 0.710(5) 1 calc PR B 1 H30C H 0.7905 0.2770 0.5476 0.124 Uiso 0.710(5) 1 calc PR B 1 C31 C 0.7837(14) 0.5278(9) 0.9777(6) 0.0496(17) Uani 0.710(5) 1 d PDU B 1 H31A H 0.7421 0.4715 1.0182 0.060 Uiso 0.710(5) 1 calc PR B 1 H31B H 0.8857 0.5200 0.9791 0.060 Uiso 0.710(5) 1 calc PR B 1 C32 C 0.7858(9) 0.6462(7) 1.0433(7) 0.0751(18) Uani 0.710(5) 1 d PDU B 1 H32A H 0.8193 0.7038 1.0000 0.090 Uiso 0.710(5) 1 calc PR B 1 C33 C 0.8904(10) 0.6695(8) 1.1554(8) 0.116(3) Uani 0.710(5) 1 d PDU B 1 H33A H 0.8955 0.7485 1.1976 0.174 Uiso 0.710(5) 1 calc PR B 1 H33B H 0.9871 0.6609 1.1430 0.174 Uiso 0.710(5) 1 calc PR B 1 H33C H 0.8573 0.6145 1.1992 0.174 Uiso 0.710(5) 1 calc PR B 1 C34 C 0.6343(8) 0.6543(7) 1.0565(6) 0.123(3) Uani 0.710(5) 1 d PDU B 1 H34A H 0.5675 0.6302 0.9817 0.185 Uiso 0.710(5) 1 calc PR B 1 H34B H 0.6322 0.7343 1.0912 0.185 Uiso 0.710(5) 1 calc PR B 1 H34C H 0.6043 0.6037 1.1053 0.185 Uiso 0.710(5) 1 calc PR B 1 C35 C 0.7422(11) 0.6846(10) 0.5707(5) 0.0430(17) Uani 0.710(5) 1 d PDU B 1 H35A H 0.8063 0.6276 0.5678 0.052 Uiso 0.710(5) 1 calc PR B 1 H35B H 0.7853 0.7481 0.5388 0.052 Uiso 0.710(5) 1 calc PR B 1 C36 C 0.5927(9) 0.6252(6) 0.4915(6) 0.0616(17) Uani 0.710(5) 1 d PDU B 1 H36A H 0.5364 0.5746 0.5310 0.074 Uiso 0.710(5) 1 calc PR B 1 C37 C 0.4956(9) 0.7048(8) 0.4437(8) 0.084(2) Uani 0.710(5) 1 d PDU B 1 H37A H 0.4689 0.7544 0.5066 0.126 Uiso 0.710(5) 1 calc PR B 1 H37B H 0.4071 0.6570 0.3913 0.126 Uiso 0.710(5) 1 calc PR B 1 H37C H 0.5495 0.7530 0.4031 0.126 Uiso 0.710(5) 1 calc PR B 1 C38 C 0.6137(6) 0.5508(5) 0.3803(5) 0.095(2) Uani 0.710(5) 1 d PDU B 1 H38A H 0.5186 0.5179 0.3287 0.142 Uiso 0.710(5) 1 calc PR B 1 H38B H 0.6615 0.4881 0.3979 0.142 Uiso 0.710(5) 1 calc PR B 1 H38C H 0.6743 0.5992 0.3440 0.142 Uiso 0.710(5) 1 calc PR B 1 N21A N 0.5611(19) 0.0805(15) 0.7144(10) 0.036(3) Uani 0.290(5) 1 d PDU B 2 H21G H 0.5760 0.0129 0.6748 0.055 Uiso 0.290(5) 1 calc PR B 2 H21E H 0.4640 0.0766 0.7091 0.055 Uiso 0.290(5) 1 calc PR B 2 H21F H 0.6069 0.0928 0.7887 0.055 Uiso 0.290(5) 1 calc PR B 2 N22A N 0.695(2) 0.3684(15) 0.7654(11) 0.029(2) Uani 0.290(5) 1 d PU B 2 H22B H 0.7788 0.3538 0.7529 0.035 Uiso 0.290(5) 1 calc PR B 2 N23A N 0.6791(18) 0.6391(14) 0.7160(10) 0.025(2) Uani 0.290(5) 1 d PU B 2 H23C H 0.5886 0.6326 0.7241 0.030 Uiso 0.290(5) 1 calc PR B 2 O21A O 0.4613(14) 0.2868(11) 0.7487(8) 0.027(2) Uani 0.290(5) 1 d PU B 2 O22A O 0.8878(15) 0.5639(12) 0.7340(8) 0.023(2) Uani 0.290(5) 1 d PU B 2 O23A O 0.5560(16) 0.8173(12) 0.7361(10) 0.040(3) Uani 0.290(5) 1 d PU B 2 O24A O 0.6659(12) 0.8977(10) 0.6208(8) 0.041(3) Uani 0.290(5) 1 d PU B 2 C21A C 0.621(3) 0.1771(18) 0.6664(15) 0.038(3) Uani 0.290(5) 1 d PDU B 2 H21Z H 0.7269 0.1848 0.6679 0.045 Uiso 0.290(5) 1 calc PR B 2 C22A C 0.584(2) 0.2804(16) 0.7336(12) 0.028(2) Uani 0.290(5) 1 d PU B 2 C23A C 0.695(3) 0.495(2) 0.8227(14) 0.028(2) Uani 0.290(5) 1 d PDU B 2 H23D H 0.5928 0.5049 0.8228 0.034 Uiso 0.290(5) 1 calc PR B 2 C24A C 0.759(2) 0.570(2) 0.7583(13) 0.026(2) Uani 0.290(5) 1 d PU B 2 C25A C 0.733(2) 0.724(2) 0.6582(16) 0.038(2) Uani 0.290(5) 1 d PDU B 2 H25B H 0.8344 0.7591 0.7024 0.046 Uiso 0.290(5) 1 calc PR B 2 C26A C 0.649(2) 0.822(2) 0.6730(15) 0.040(3) Uani 0.290(5) 1 d PDU B 2 C27A C 0.526(3) 0.150(2) 0.5465(18) 0.051(3) Uani 0.290(5) 1 d PDU B 2 H27D H 0.4206 0.1288 0.5449 0.061 Uiso 0.290(5) 1 calc PR B 2 H27C H 0.5546 0.0895 0.4930 0.061 Uiso 0.290(5) 1 calc PR B 2 C28A C 0.570(2) 0.2714(15) 0.527(2) 0.054(3) Uani 0.290(5) 1 d PDU B 2 H28B H 0.5531 0.3336 0.5871 0.065 Uiso 0.290(5) 1 calc PR B 2 C29A C 0.460(3) 0.2486(19) 0.414(2) 0.067(5) Uani 0.290(5) 1 d PDU B 2 H29D H 0.4736 0.3165 0.3807 0.100 Uiso 0.290(5) 1 calc PR B 2 H29E H 0.3610 0.2336 0.4266 0.100 Uiso 0.290(5) 1 calc PR B 2 H29F H 0.4748 0.1813 0.3612 0.100 Uiso 0.290(5) 1 calc PR B 2 C30A C 0.729(2) 0.2897(15) 0.5134(16) 0.049(4) Uani 0.290(5) 1 d PDU B 2 H30D H 0.7950 0.3076 0.5883 0.074 Uiso 0.290(5) 1 calc PR B 2 H30E H 0.7478 0.3541 0.4764 0.074 Uiso 0.290(5) 1 calc PR B 2 H30F H 0.7450 0.2191 0.4665 0.074 Uiso 0.290(5) 1 calc PR B 2 C31A C 0.784(4) 0.510(2) 0.9519(15) 0.045(3) Uani 0.290(5) 1 d PDU B 2 H31C H 0.7353 0.4506 0.9860 0.054 Uiso 0.290(5) 1 calc PR B 2 H31D H 0.8837 0.4975 0.9512 0.054 Uiso 0.290(5) 1 calc PR B 2 C32A C 0.792(2) 0.6366(16) 1.0285(17) 0.070(3) Uani 0.290(5) 1 d PDU B 2 H32B H 0.6923 0.6536 1.0087 0.084 Uiso 0.290(5) 1 calc PR B 2 C33A C 0.9028(12) 0.7450(10) 1.0112(10) 0.062(3) Uani 0.290(5) 1 d PDU B 2 H33D H 0.8751 0.7544 0.9332 0.093 Uiso 0.290(5) 1 calc PR B 2 H33E H 1.0021 0.7308 1.0251 0.093 Uiso 0.290(5) 1 calc PR B 2 H33F H 0.8985 0.8155 1.0648 0.093 Uiso 0.290(5) 1 calc PR B 2 C34A C 0.818(3) 0.630(2) 1.1607(17) 0.101(5) Uani 0.290(5) 1 d PDU B 2 H34D H 0.7482 0.5650 1.1692 0.152 Uiso 0.290(5) 1 calc PR B 2 H34E H 0.8041 0.7023 1.2065 0.152 Uiso 0.290(5) 1 calc PR B 2 H34F H 0.9173 0.6196 1.1865 0.152 Uiso 0.290(5) 1 calc PR B 2 C35A C 0.747(3) 0.682(3) 0.5413(16) 0.052(3) Uani 0.290(5) 1 d PDU B 2 H35Z H 0.7960 0.6159 0.5359 0.062 Uiso 0.290(5) 1 calc PR B 2 H35C H 0.8037 0.7446 0.5155 0.062 Uiso 0.290(5) 1 calc PR B 2 C36A C 0.598(2) 0.6478(14) 0.472(2) 0.066(3) Uani 0.290(5) 1 d PDU B 2 H36B H 0.6094 0.6373 0.3918 0.080 Uiso 0.290(5) 1 calc PR B 2 C37A C 0.518(3) 0.743(2) 0.488(2) 0.092(5) Uani 0.290(5) 1 d PDU B 2 H37D H 0.4149 0.7133 0.4524 0.139 Uiso 0.290(5) 1 calc PR B 2 H37E H 0.5580 0.8038 0.4535 0.139 Uiso 0.290(5) 1 calc PR B 2 H37F H 0.5287 0.7740 0.5698 0.139 Uiso 0.290(5) 1 calc PR B 2 C38A C 0.5512(17) 0.5304(15) 0.4862(16) 0.106(4) Uani 0.290(5) 1 d PDU B 2 H38D H 0.6176 0.5174 0.5512 0.160 Uiso 0.290(5) 1 calc PR B 2 H38E H 0.5526 0.4743 0.4172 0.160 Uiso 0.290(5) 1 calc PR B 2 H38F H 0.4522 0.5210 0.4995 0.160 Uiso 0.290(5) 1 calc PR B 2 N1P N 0.3599(5) 0.8375(4) 0.0210(4) 0.1151(13) Uani 1 1 d DU . . C5P C 0.2985(7) 0.8112(5) 0.0987(6) 0.149(2) Uani 1 1 d DU . . H5PA H 0.2034 0.7643 0.0771 0.179 Uiso 1 1 calc R . . C4P C 0.3610(10) 0.8462(7) 0.2087(7) 0.188(3) Uani 1 1 d DU . . H4PA H 0.3071 0.8281 0.2630 0.225 Uiso 1 1 calc R . . C3P C 0.5071(11) 0.9101(6) 0.2473(6) 0.190(3) Uani 1 1 d DU . . H3PA H 0.5544 0.9326 0.3255 0.227 Uiso 1 1 calc R . . C2P C 0.5729(10) 0.9363(6) 0.1654(7) 0.228(3) Uani 1 1 d DU . . H2PA H 0.6698 0.9798 0.1849 0.274 Uiso 1 1 calc R . . C1P C 0.5004(8) 0.9004(5) 0.0528(5) 0.173(3) Uani 1 1 d DU . . H1PB H 0.5486 0.9196 -0.0042 0.207 Uiso 1 1 calc R . . N11P N 0.6675(15) 0.1754(10) -0.0248(10) 0.131(3) Uani 0.326(5) 1 d PDU C 1 C11P C 0.5585(14) 0.2101(11) 0.0239(11) 0.128(4) Uani 0.326(5) 1 d PDU C 1 H11F H 0.4630 0.1954 -0.0220 0.153 Uiso 0.326(5) 1 calc PR C 1 C12P C 0.5820(17) 0.2661(12) 0.1379(12) 0.151(4) Uani 0.326(5) 1 d PDU C 1 H12C H 0.5039 0.2891 0.1685 0.181 Uiso 0.326(5) 1 calc PR C 1 C13P C 0.7162(19) 0.2872(12) 0.2041(12) 0.152(4) Uani 0.326(5) 1 d PDU C 1 H13G H 0.7328 0.3255 0.2819 0.182 Uiso 0.326(5) 1 calc PR C 1 C14P C 0.8268(16) 0.2549(14) 0.1616(11) 0.161(4) Uani 0.326(5) 1 d PDU C 1 H14G H 0.9218 0.2673 0.2078 0.194 Uiso 0.326(5) 1 calc PR C 1 C15P C 0.7947(16) 0.2010(13) 0.0437(13) 0.139(3) Uani 0.326(5) 1 d PDU C 1 H15E H 0.8740 0.1819 0.0121 0.167 Uiso 0.326(5) 1 calc PR C 1 N21P N 0.7841(8) 0.1194(6) -0.0401(5) 0.126(2) Uani 0.674(5) 1 d PDU C 2 C21P C 0.8887(8) 0.0566(6) -0.0638(6) 0.147(3) Uani 0.674(5) 1 d PDU C 2 H21H H 0.8730 0.0126 -0.1396 0.176 Uiso 0.674(5) 1 calc PR C 2 C22P C 1.0081(10) 0.0510(8) 0.0073(8) 0.202(4) Uani 0.674(5) 1 d PDU C 2 H22C H 1.0717 0.0053 -0.0212 0.242 Uiso 0.674(5) 1 calc PR C 2 C23P C 1.0451(15) 0.1074(10) 0.1193(9) 0.237(4) Uani 0.674(5) 1 d PDU C 2 H23P H 1.1294 0.1020 0.1712 0.284 Uiso 0.674(5) 1 calc PR C 2 C24P C 0.9419(13) 0.1758(10) 0.1496(7) 0.216(4) Uani 0.674(5) 1 d PDU C 2 H24A H 0.9568 0.2187 0.2257 0.259 Uiso 0.674(5) 1 calc PR C 2 C25P C 0.8203(12) 0.1805(8) 0.0697(8) 0.182(3) Uani 0.674(5) 1 d PDU C 2 H25P H 0.7582 0.2300 0.0938 0.218 Uiso 0.674(5) 1 calc PR C 2 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 O1 0.021(2) 0.035(2) 0.043(3) 0.002(3) 0.000(3) 0.0073(17) O2 0.019(2) 0.037(2) 0.046(3) 0.001(2) 0.004(2) 0.0112(15) O3 0.030(2) 0.052(3) 0.077(3) 0.021(2) 0.012(2) 0.018(2) O4 0.050(2) 0.040(2) 0.080(3) 0.031(2) 0.001(2) 0.0030(19) N1 0.049(3) 0.040(3) 0.052(4) 0.021(3) 0.023(3) 0.027(2) N2 0.020(2) 0.034(2) 0.034(3) 0.004(2) 0.003(3) 0.0108(16) N3 0.016(2) 0.021(2) 0.026(3) 0.003(2) -0.002(2) 0.0031(17) C1 0.027(4) 0.047(3) 0.055(5) 0.018(3) 0.016(3) 0.013(3) C2 0.025(3) 0.027(3) 0.033(4) 0.001(3) -0.001(3) 0.012(2) C3 0.019(4) 0.028(3) 0.046(4) 0.011(3) 0.005(3) 0.013(3) C4 0.025(3) 0.028(3) 0.037(3) 0.005(3) 0.006(3) 0.014(2) C5 0.024(2) 0.023(2) 0.041(3) -0.002(3) -0.011(3) 0.0087(19) C6 0.024(3) 0.026(3) 0.039(4) 0.007(3) 0.009(3) 0.017(2) C7 0.034(3) 0.059(4) 0.058(6) 0.021(4) 0.004(4) 0.020(3) C8 0.036(5) 0.066(5) 0.066(5) 0.015(4) 0.008(4) 0.007(4) C9 0.067(6) 0.061(6) 0.068(6) -0.002(5) 0.024(5) -0.006(4) C10 0.049(7) 0.099(8) 0.100(7) 0.021(6) 0.013(5) 0.007(6) C11 0.028(4) 0.060(4) 0.050(4) 0.004(3) 0.012(3) 0.020(3) C12 0.028(3) 0.067(3) 0.064(3) 0.025(3) 0.009(2) 0.005(2) C13 0.051(4) 0.130(6) 0.065(4) 0.022(4) 0.007(3) 0.021(4) C14 0.042(3) 0.078(4) 0.070(4) 0.030(3) -0.001(3) 0.022(3) C15 0.122(4) 0.058(3) 0.076(4) -0.011(3) -0.030(4) 0.016(3) C16 0.111(5) 0.116(4) 0.109(5) -0.006(4) -0.005(4) 0.004(4) C17 0.156(8) 0.188(9) 0.135(9) -0.018(7) -0.021(7) 0.009(8) C18 0.158(6) 0.136(6) 0.154(8) 0.027(7) 0.078(7) 0.065(5) O1A 0.021(3) 0.025(3) 0.027(4) 0.009(3) 0.000(3) 0.008(2) O2A 0.021(3) 0.029(3) 0.043(4) -0.008(3) 0.007(3) 0.0165(19) O3A 0.035(3) 0.063(4) 0.071(4) 0.005(3) 0.006(3) 0.023(3) O4A 0.057(3) 0.044(3) 0.095(4) 0.010(3) -0.001(3) 0.016(3) N1A 0.029(3) 0.031(3) 0.041(4) 0.013(3) 0.003(3) 0.013(3) N2A 0.0205(19) 0.0221(19) 0.023(2) 0.0045(11) 0.0042(10) 0.0066(10) N3A 0.025(3) 0.033(3) 0.036(4) 0.002(3) 0.002(3) 0.012(2) C1A 0.017(4) 0.041(4) 0.046(6) 0.020(4) -0.002(4) 0.021(3) C2A 0.018(4) 0.042(4) 0.039(5) 0.013(4) 0.001(4) 0.013(3) C3A 0.013(4) 0.029(4) 0.045(4) 0.007(4) 0.000(3) 0.011(3) C4A 0.011(3) 0.022(4) 0.040(5) -0.004(4) -0.002(4) -0.005(3) C5A 0.045(3) 0.035(3) 0.053(4) 0.003(4) -0.009(4) 0.007(3) C6A 0.033(4) 0.041(4) 0.068(5) 0.003(5) -0.011(5) 0.010(3) C7A 0.033(5) 0.057(5) 0.050(6) 0.012(4) 0.011(5) 0.020(4) C8A 0.049(6) 0.063(6) 0.058(6) 0.012(5) 0.006(5) 0.007(5) C9A 0.079(10) 0.053(8) 0.092(9) -0.002(7) 0.016(7) 0.020(7) C10A 0.063(11) 0.099(10) 0.077(8) 0.033(7) 0.026(7) -0.002(7) C11A 0.017(4) 0.052(4) 0.055(4) 0.013(3) 0.003(3) 0.013(3) C12A 0.044(4) 0.084(5) 0.061(4) -0.005(4) 0.006(4) -0.001(4) C13A 0.061(5) 0.116(7) 0.060(5) -0.013(5) 0.027(4) 0.011(5) C14A 0.064(6) 0.087(6) 0.081(6) -0.024(5) 0.014(5) -0.002(5) C15A 0.043(2) 0.046(2) 0.049(2) 0.0078(11) 0.0112(10) 0.0098(10) C16A 0.051(4) 0.112(5) 0.091(5) -0.018(4) 0.052(4) 0.022(4) C17A 0.039(4) 0.054(4) 0.052(5) 0.021(4) 0.020(4) 0.002(3) C18A 0.158(6) 0.136(6) 0.154(8) 0.027(7) 0.078(7) 0.065(5) N21 0.022(2) 0.031(2) 0.054(3) 0.024(2) 0.013(2) 0.0119(15) N22 0.022(2) 0.0277(19) 0.053(3) 0.009(2) 0.008(2) 0.0144(16) N23 0.0218(18) 0.0261(19) 0.037(3) 0.005(2) 0.007(2) 0.0073(14) O21 0.024(2) 0.0307(17) 0.054(3) 0.012(2) 0.012(2) 0.0109(14) O22 0.0244(19) 0.0339(19) 0.043(3) 0.007(2) 0.014(2) 0.0137(14) O23 0.040(2) 0.031(2) 0.057(3) 0.009(2) 0.021(2) 0.0173(16) O24 0.053(3) 0.035(2) 0.079(3) 0.020(2) 0.030(2) 0.0184(18) C21 0.021(2) 0.024(2) 0.055(4) 0.026(3) 0.015(3) 0.0083(17) C22 0.017(2) 0.021(2) 0.039(3) 0.012(2) 0.010(2) 0.0113(17) C23 0.029(2) 0.028(2) 0.038(4) 0.008(3) 0.010(3) 0.0182(17) C24 0.020(2) 0.0204(19) 0.040(3) 0.000(3) 0.002(3) 0.0103(17) C25 0.022(2) 0.025(2) 0.053(3) 0.005(3) 0.015(3) 0.0097(18) C26 0.036(3) 0.021(3) 0.058(4) 0.011(3) 0.018(3) 0.010(2) C27 0.041(3) 0.037(2) 0.061(4) 0.017(3) 0.010(3) 0.016(2) C28 0.049(3) 0.045(4) 0.078(4) 0.017(3) 0.003(3) 0.013(3) C29 0.091(5) 0.065(6) 0.077(5) 0.010(4) -0.009(4) 0.030(5) C30 0.072(4) 0.082(6) 0.099(6) 0.029(4) 0.019(4) 0.016(5) C31 0.043(2) 0.051(4) 0.064(4) 0.012(3) 0.021(3) 0.027(3) C32 0.094(4) 0.064(3) 0.074(4) 0.013(3) 0.024(3) 0.033(3) C33 0.127(7) 0.112(7) 0.082(5) -0.010(4) 0.006(5) 0.004(5) C34 0.121(5) 0.135(5) 0.111(5) -0.018(4) 0.018(4) 0.086(5) C35 0.043(2) 0.035(2) 0.065(4) 0.020(3) 0.022(3) 0.024(2) C36 0.058(3) 0.049(3) 0.090(4) 0.044(3) 0.015(3) 0.011(3) C37 0.053(4) 0.099(6) 0.106(6) 0.037(4) 0.015(4) 0.019(4) C38 0.078(4) 0.088(4) 0.091(4) -0.011(3) -0.020(3) 0.020(3) N21A 0.029(4) 0.040(4) 0.041(5) 0.006(4) 0.006(4) 0.017(3) N22A 0.026(3) 0.029(3) 0.033(4) 0.002(3) 0.007(3) 0.014(3) N23A 0.019(3) 0.026(3) 0.034(4) 0.003(3) 0.006(3) 0.017(3) O21A 0.020(4) 0.030(3) 0.033(5) 0.006(4) 0.002(4) 0.013(3) O22A 0.013(3) 0.034(4) 0.021(4) -0.007(4) 0.009(4) 0.010(3) O23A 0.037(4) 0.034(4) 0.048(5) 0.010(4) 0.009(4) 0.008(3) O24A 0.045(4) 0.035(4) 0.047(5) 0.016(3) 0.011(3) 0.015(3) C21A 0.029(4) 0.034(4) 0.050(6) 0.014(4) 0.001(5) 0.007(4) C22A 0.023(3) 0.027(3) 0.037(4) 0.011(3) 0.005(3) 0.008(3) C23A 0.028(3) 0.022(3) 0.036(4) 0.005(3) 0.008(3) 0.013(3) C24A 0.025(4) 0.025(3) 0.028(4) 0.006(3) 0.006(3) 0.009(3) C25A 0.030(4) 0.034(4) 0.055(5) 0.008(4) 0.016(4) 0.015(3) C26A 0.038(5) 0.030(5) 0.056(6) 0.011(5) 0.016(5) 0.009(4) C27A 0.040(5) 0.042(5) 0.070(6) 0.015(5) 0.010(5) 0.005(4) C28A 0.048(4) 0.041(5) 0.074(6) 0.022(5) 0.007(5) 0.007(5) C29A 0.052(7) 0.059(10) 0.082(9) 0.010(8) 0.010(7) 0.003(8) C30A 0.032(6) 0.052(8) 0.072(9) 0.047(7) 0.008(6) -0.003(7) C31A 0.042(4) 0.042(5) 0.052(5) 0.001(5) 0.019(5) 0.014(4) C32A 0.078(5) 0.065(5) 0.066(5) 0.007(5) 0.017(5) 0.019(5) C33A 0.058(7) 0.068(6) 0.056(6) 0.009(5) 0.011(5) 0.008(5) C34A 0.135(11) 0.095(10) 0.058(7) 0.009(7) 0.007(9) 0.009(9) C35A 0.046(4) 0.043(4) 0.077(6) 0.021(5) 0.029(5) 0.013(4) C36A 0.056(5) 0.065(5) 0.088(5) 0.033(5) 0.020(5) 0.016(5) C37A 0.069(9) 0.094(9) 0.109(11) 0.030(9) -0.005(9) 0.021(8) C38A 0.070(8) 0.095(8) 0.150(10) 0.042(8) 0.019(8) -0.007(7) N1P 0.136(3) 0.102(3) 0.125(3) 0.042(2) 0.040(2) 0.045(2) C5P 0.185(5) 0.170(5) 0.139(4) 0.048(4) 0.080(4) 0.105(4) C4P 0.251(7) 0.202(6) 0.156(5) 0.054(5) 0.067(5) 0.138(5) C3P 0.300(8) 0.168(5) 0.105(4) 0.022(4) 0.033(5) 0.086(6) C2P 0.300(7) 0.203(6) 0.139(5) 0.045(5) -0.005(5) -0.014(6) C1P 0.200(6) 0.165(5) 0.125(4) 0.058(4) -0.009(4) -0.028(5) N11P 0.147(4) 0.135(4) 0.118(4) 0.028(3) 0.044(3) 0.032(4) C11P 0.179(8) 0.135(7) 0.101(7) 0.047(6) 0.063(6) 0.061(7) C12P 0.200(9) 0.139(8) 0.117(8) 0.025(7) 0.033(7) 0.053(8) C13P 0.194(9) 0.146(8) 0.104(7) 0.011(7) 0.021(7) 0.041(8) C14P 0.188(7) 0.172(6) 0.089(6) -0.024(6) 0.015(6) 0.019(6) C15P 0.176(6) 0.135(6) 0.100(5) 0.010(5) 0.034(5) 0.028(5) N21P 0.145(4) 0.125(3) 0.102(3) 0.004(3) 0.032(3) 0.034(3) C21P 0.147(6) 0.157(6) 0.113(5) 0.011(4) -0.032(4) 0.057(5) C22P 0.185(7) 0.232(8) 0.144(6) 0.009(6) -0.044(6) 0.048(6) C23P 0.241(8) 0.255(8) 0.137(6) -0.049(6) -0.021(6) 0.017(7) C24P 0.220(7) 0.231(7) 0.123(5) -0.052(6) -0.019(5) 0.016(6) C25P 0.201(5) 0.181(5) 0.130(5) -0.022(4) 0.040(4) 0.009(5) _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 O1 C2 1.242(14) . ? O2 C4 1.279(13) . ? O3 C6 1.292(10) . ? O4 C6 1.214(10) . ? N1 C1 1.484(9) . ? N2 C2 1.355(12) . ? N2 C3 1.434(17) . ? N3 C4 1.341(13) . ? N3 C5 1.479(10) . ? C1 C2 1.462(15) . ? C1 C7 1.534(6) . ? C3 C4 1.494(14) . ? C3 C11 1.496(6) . ? C5 C15 1.518(6) . ? C5 C6 1.522(10) . ? C7 C8 1.528(6) . ? C8 C10 1.520(7) . ? C8 C9 1.529(6) . ? C11 C12 1.512(7) . ? C12 C13 1.514(6) . ? C12 C14 1.521(5) . ? C15 C16 1.489(7) . ? C16 C17 1.488(7) . ? C16 C18 1.489(7) . ? O1A C2A 1.27(2) . ? O2A C4A 1.246(17) . ? O3A C6A 1.142(17) . ? O4A C6A 1.277(18) . ? N1A C1A 1.451(11) . ? N2A C2A 1.273(18) . ? N2A C3A 1.50(2) . ? N3A C4A 1.32(2) . ? N3A C5A 1.415(16) . ? C1A C7A 1.522(7) . ? C1A C2A 1.52(2) . ? C3A C11A 1.508(7) . ? C3A C4A 1.531(19) . ? C5A C6A 1.499(19) . ? C5A C15A 1.538(8) . ? C7A C8A 1.520(7) . ? C8A C9A 1.525(7) . ? C8A C10A 1.526(7) . ? C11A C12A 1.518(7) . ? C12A C14A 1.490(7) . ? C12A C13A 1.529(7) . ? C15A C16A 1.495(7) . ? C16A C18A 1.463(7) . ? C16A C17A 1.503(7) . ? N21 C21 1.492(6) . ? N22 C22 1.312(8) . ? N22 C23 1.439(10) . ? N23 C24 1.339(10) . ? N23 C25 1.467(9) . ? O21 C22 1.257(8) . ? O22 C24 1.220(10) . ? O23 C26 1.259(10) . ? O24 C26 1.231(9) . ? C21 C22 1.518(10) . ? C21 C27 1.526(6) . ? C23 C24 1.502(11) . ? C23 C31 1.515(6) . ? C25 C26 1.530(10) . ? C25 C35 1.538(6) . ? C27 C28 1.549(7) . ? C28 C29 1.550(7) . ? C28 C30 1.551(8) . ? C31 C32 1.490(6) . ? C32 C33 1.494(7) . ? C32 C34 1.499(7) . ? C35 C36 1.546(6) . ? C36 C38 1.546(7) . ? C36 C37 1.557(7) . ? N21A C21A 1.482(14) . ? N22A C22A 1.31(2) . ? N22A C23A 1.55(3) . ? N23A C24A 1.33(3) . ? N23A C25A 1.43(2) . ? O21A C22A 1.23(2) . ? O22A C24A 1.33(3) . ? O23A C26A 1.28(3) . ? O24A C26A 1.22(2) . ? C21A C22A 1.48(3) . ? C21A C27A 1.526(16) . ? C23A C24A 1.44(3) . ? C23A C31A 1.620(13) . ? C25A C35A 1.464(15) . ? C25A C26A 1.52(3) . ? C27A C28A 1.533(16) . ? C28A C29A 1.535(16) . ? C28A C30A 1.538(15) . ? C31A C32A 1.610(13) . ? C32A C34A 1.617(13) . ? C32A C33A 1.617(13) . ? C35A C36A 1.465(15) . ? C36A C38A 1.464(14) . ? C36A C37A 1.471(15) . ? N1P C5P 1.271(6) . ? N1P C1P 1.376(7) . ? C5P C4P 1.329(8) . ? C4P C3P 1.426(9) . ? C3P C2P 1.340(9) . ? C2P C1P 1.380(8) . ? N11P C15P 1.298(12) . ? N11P C11P 1.372(12) . ? C11P C12P 1.392(13) . ? C12P C13P 1.342(12) . ? C13P C14P 1.338(12) . ? C14P C15P 1.424(13) . ? N21P C25P 1.359(9) . ? N21P C21P 1.383(8) . ? C21P C22P 1.323(9) . ? C22P C23P 1.366(10) . ? C23P C24P 1.436(12) . ? C24P C25P 1.392(11) . ? 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 C2 N2 C3 121.4(9) . . ? C4 N3 C5 124.3(7) . . ? C2 C1 N1 109.0(7) . . ? C2 C1 C7 114.3(8) . . ? N1 C1 C7 108.5(6) . . ? O1 C2 N2 122.4(9) . . ? O1 C2 C1 121.4(9) . . ? N2 C2 C1 115.9(9) . . ? N2 C3 C4 108.8(8) . . ? N2 C3 C11 106.8(9) . . ? C4 C3 C11 111.4(8) . . ? O2 C4 N3 121.2(8) . . ? O2 C4 C3 121.2(9) . . ? N3 C4 C3 117.1(9) . . ? N3 C5 C15 112.0(6) . . ? N3 C5 C6 109.9(6) . . ? C15 C5 C6 114.8(6) . . ? O4 C6 O3 128.9(7) . . ? O4 C6 C5 115.3(7) . . ? O3 C6 C5 113.9(7) . . ? C8 C7 C1 115.9(7) . . ? C10 C8 C7 110.6(7) . . ? C10 C8 C9 108.7(10) . . ? C7 C8 C9 111.4(7) . . ? C3 C11 C12 118.1(8) . . ? C11 C12 C13 109.3(5) . . ? C11 C12 C14 111.0(5) . . ? C13 C12 C14 109.0(4) . . ? C16 C15 C5 122.7(7) . . ? C17 C16 C18 113.0(8) . . ? C17 C16 C15 109.5(6) . . ? C18 C16 C15 111.0(7) . . ? C2A N2A C3A 128.6(13) . . ? C4A N3A C5A 125.0(12) . . ? N1A C1A C7A 112.5(9) . . ? N1A C1A C2A 110.2(9) . . ? C7A C1A C2A 110.0(11) . . ? O1A C2A N2A 123.5(15) . . ? O1A C2A C1A 118.1(13) . . ? N2A C2A C1A 118.4(13) . . ? N2A C3A C11A 116.5(14) . . ? N2A C3A C4A 107.0(11) . . ? C11A C3A C4A 111.0(12) . . ? O2A C4A N3A 122.2(10) . . ? O2A C4A C3A 117.7(14) . . ? N3A C4A C3A 120.1(13) . . ? N3A C5A C6A 104.9(10) . . ? N3A C5A C15A 110.4(9) . . ? C6A C5A C15A 100.9(9) . . ? O3A C6A O4A 106.6(14) . . ? O3A C6A C5A 133.0(14) . . ? O4A C6A C5A 119.4(12) . . ? C8A C7A C1A 114.3(11) . . ? C7A C8A C9A 114.6(11) . . ? C7A C8A C10A 109.1(11) . . ? C9A C8A C10A 107.8(15) . . ? C3A C11A C12A 119.0(11) . . ? C14A C12A C11A 112.3(9) . . ? C14A C12A C13A 111.0(7) . . ? C11A C12A C13A 110.2(9) . . ? C16A C15A C5A 110.7(8) . . ? C18A C16A C15A 113.9(7) . . ? C18A C16A C17A 113.7(8) . . ? C15A C16A C17A 109.7(6) . . ? C22 N22 C23 123.8(6) . . ? C24 N23 C25 122.7(6) . . ? N21 C21 C22 108.7(5) . . ? N21 C21 C27 110.1(5) . . ? C22 C21 C27 111.9(6) . . ? O21 C22 N22 123.0(6) . . ? O21 C22 C21 119.6(6) . . ? N22 C22 C21 117.4(6) . . ? N22 C23 C24 107.3(6) . . ? N22 C23 C31 111.1(6) . . ? C24 C23 C31 108.4(7) . . ? O22 C24 N23 121.8(7) . . ? O22 C24 C23 121.1(7) . . ? N23 C24 C23 117.1(7) . . ? N23 C25 C26 110.1(5) . . ? N23 C25 C35 112.6(6) . . ? C26 C25 C35 113.1(6) . . ? O24 C26 O23 126.7(7) . . ? O24 C26 C25 116.5(6) . . ? O23 C26 C25 116.6(6) . . ? C21 C27 C28 120.3(7) . . ? C27 C28 C29 112.6(7) . . ? C27 C28 C30 110.7(8) . . ? C29 C28 C30 109.3(8) . . ? C32 C31 C23 117.4(8) . . ? C31 C32 C33 109.0(7) . . ? C31 C32 C34 108.8(7) . . ? C33 C32 C34 112.1(7) . . ? C25 C35 C36 117.9(7) . . ? C38 C36 C35 110.2(6) . . ? C38 C36 C37 101.1(6) . . ? C35 C36 C37 117.3(7) . . ? C22A N22A C23A 127.5(17) . . ? C24A N23A C25A 123.6(16) . . ? C22A C21A N21A 104.4(16) . . ? C22A C21A C27A 108.1(19) . . ? N21A C21A C27A 103.3(15) . . ? O21A C22A N22A 123.6(17) . . ? O21A C22A C21A 124.1(17) . . ? N22A C22A C21A 111.9(17) . . ? C24A C23A N22A 108.1(15) . . ? C24A C23A C31A 116.0(19) . . ? N22A C23A C31A 103.3(15) . . ? O22A C24A N23A 120.3(17) . . ? O22A C24A C23A 121.8(19) . . ? N23A C24A C23A 117.6(19) . . ? N23A C25A C35A 117.3(19) . . ? N23A C25A C26A 108.7(16) . . ? C35A C25A C26A 114.1(19) . . ? O24A C26A O23A 122(2) . . ? O24A C26A C25A 120.2(18) . . ? O23A C26A C25A 118.0(18) . . ? C21A C27A C28A 94.8(19) . . ? C27A C28A C29A 94.7(17) . . ? C27A C28A C30A 109(2) . . ? C29A C28A C30A 112.7(18) . . ? C32A C31A C23A 111(2) . . ? C31A C32A C34A 108.8(15) . . ? C31A C32A C33A 118.5(18) . . ? C34A C32A C33A 111.0(15) . . ? C25A C35A C36A 106(2) . . ? C38A C36A C35A 103.0(18) . . ? C38A C36A C37A 126(2) . . ? C35A C36A C37A 111(2) . . ? C5P N1P C1P 118.0(6) . . ? N1P C5P C4P 123.1(7) . . ? C5P C4P C3P 121.6(7) . . ? C2P C3P C4P 115.3(7) . . ? C3P C2P C1P 120.3(8) . . ? N1P C1P C2P 121.6(6) . . ? C15P N11P C11P 114.4(12) . . ? N11P C11P C12P 122.8(10) . . ? C13P C12P C11P 119.4(10) . . ? C14P C13P C12P 120.6(12) . . ? C13P C14P C15P 116.6(10) . . ? N11P C15P C14P 126.1(11) . . ? C25P N21P C21P 110.8(8) . . ? C22P C21P N21P 127.3(6) . . ? C21P C22P C23P 123.6(9) . . ? C22P C23P C24P 112.1(10) . . ? C25P C24P C23P 121.3(7) . . ? N21P C25P C24P 124.8(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 N1 C1 C2 N2 130.7(8) . . . . ? N2 C3 C4 N3 135.7(9) . . . . ? N3 C5 C6 O3 -28.8(8) . . . . ? N3 C5 C6 O4 136.7(7) . . . . ? C2 N2 C3 C4 -129.4(8) . . . . ? C4 N3 C5 C6 -143.9(7) . . . . ? C1 C2 N2 C3 174.8(6) . . . . ? C3 C4 N3 C5 174.1(7) . . . . ? N1A C1A C2A N2A 131.9(13) . . . . ? N2A C3A C4A N3A 128.0(14) . . . . ? N3A C5A C6A O3A -45.3(18) . . . . ? N3A C5A C6A O4A 148.0(12) . . . . ? C2A N2A C3A C4A -121.5(13) . . . . ? C4A N3A C5A C6A -144.6(12) . . . . ? C1A C2A N2A C3A 177.9(10) . . . . ? C3A C4A N3A C5A 175.1(12) . . . . ? N21 C21 C22 N22 128.3(6) . . . . ? N22 C23 C24 N23 128.0(6) . . . . ? N23 C25 C26 O23 5.6(7) . . . . ? N23 C25 C26 O24 -179.4(5) . . . . ? C22 N22 C23 C24 -130.1(6) . . . . ? C24 N23 C25 C26 -153.7(5) . . . . ? C21 C22 N22 C23 171.1(5) . . . . ? C23 C24 N23 C25 176.2(5) . . . . ? N21A C21A C22A N22A 134.9(16) . . . . ? N22A C23A C24A N23A 122.5(17) . . . . ? N23A C25A C26A O23A 3.9(19) . . . . ? N23A C25A C26A O24A -172.2(15) . . . . ? C22A N22A C23A C24A -127.8(19) . . . . ? C24A N23A C25A C26A -152.7(14) . . . . ? C21A C22A N22A C23A 171.3(14) . . . . ? C23A C24A N23A C25A 174.8(15) . . . . ? 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 N1 H1B O23 0.91 1.84 2.729(10) 164.6 . N1A H1A3 O23A 0.91 1.80 2.691(19) 166.9 . N3 H3A O21 0.88 2.12 2.964(10) 161.4 . N3A H3AA O21A 0.88 2.09 2.912(19) 154.9 . N21 H21B O3 0.91 1.85 2.742(8) 167.5 . N23 H23A O1 0.88 2.15 3.002(10) 161.7 . N21A H21E O3A 0.91 1.93 2.77(2) 152.6 . N23A H23C O1A 0.88 2.19 3.03(2) 161.3 . N1 H1A O4 0.91 2.17 2.919(10) 138.6 1_565 N1 H1A O3 0.91 2.26 3.064(10) 147.0 1_565 N1A H1A2 O4A 0.91 1.87 2.699(14) 150.8 1_565 N1A H1A2 O3A 0.91 2.05 2.843(14) 144.7 1_565 N1 H1C N1P 0.91 1.74 2.609(8) 159.6 1_556 N1A H1A1 N1P 0.91 2.22 3.102(10) 163.6 1_556 N21 H21C N11P 0.91 1.83 2.643(13) 147.8 1_556 N21A H21F N21P 0.91 2.38 3.262(15) 163.8 1_556 N2 H2A O22 0.88 2.03 2.880(10) 162.8 1_455 N2A H2AA O22A 0.88 1.98 2.839(19) 163.4 1_455 N21 H21A O24 0.91 1.82 2.654(8) 151.3 1_545 N21 H21A O23 0.91 2.45 3.057(8) 124.5 1_545 N21A H21G O24A 0.91 1.82 2.70(2) 161.4 1_545 N21A H21G O23A 0.91 2.60 3.22(2) 126.7 1_545 N22 H22A O2 0.88 1.98 2.828(9) 161.2 1_655 N22A H22B O2A 0.88 2.07 2.93(2) 168.0 1_655 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.427 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.055 _chemical_name_common 'L-leucyl-L-leucyl-L-leucine - pyridine clathrate (1:1)' #===END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 642088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_sum 'C24 H42.24 N4 O4.12' _chemical_formula_weight 452.87 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5544(5) _cell_length_b 12.1536(7) _cell_length_c 12.3690(7) _cell_angle_alpha 102.810(3) _cell_angle_beta 105.373(2) _cell_angle_gamma 97.475(2) _cell_volume 1322.91(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9153 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 30.20 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 495 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9404 _exptl_absorpt_correction_T_max 0.9816 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30188 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10356 _reflns_number_gt 9301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0691P)^2^+0.9481P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details rm _refine_ls_number_reflns 30188 _refine_ls_number_parameters 595 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _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 O1 O 1.10074(14) 1.21479(10) 0.24628(12) 0.0293(3) Uani 1 1 d . . . O2 O 0.69316(13) 0.95087(9) 0.24691(10) 0.0214(3) Uani 1 1 d . . . O3 O 1.02126(15) 0.68914(12) 0.25540(14) 0.0446(4) Uani 1 1 d . . . O4 O 0.80507(13) 0.57213(10) 0.21571(11) 0.0249(3) Uani 1 1 d . . . N1 N 0.98710(15) 1.42810(11) 0.26535(12) 0.0190(3) Uani 1 1 d . . . H1A H 0.9926 1.4362 0.3414 0.028 Uiso 1 1 calc R . . H1B H 0.9413 1.4826 0.2394 0.028 Uiso 1 1 calc R . . H1C H 1.0801 1.4369 0.2585 0.028 Uiso 1 1 calc R . . N2 N 0.89070(15) 1.15979(11) 0.29040(12) 0.0183(3) Uani 1 1 d . . . H2A H 0.8024 1.1743 0.2888 0.022 Uiso 1 1 calc R . . N3 N 0.88781(15) 0.86776(10) 0.23265(11) 0.0164(3) Uani 1 1 d . . . H3A H 0.9848 0.8798 0.2482 0.020 Uiso 1 1 calc R . . C1 C 0.90106(18) 1.31156(13) 0.19477(14) 0.0171(4) Uani 1 1 d . . . H1D H 0.7983 1.3042 0.2012 0.021 Uiso 1 1 calc R . . C2 C 0.97359(18) 1.22328(13) 0.24596(15) 0.0177(4) Uani 1 1 d . . . C3 C 0.93643(18) 1.06821(13) 0.34126(14) 0.0169(4) Uani 1 1 d . . . H3B H 1.0397 1.0623 0.3409 0.020 Uiso 1 1 calc R . . C4 C 0.82854(19) 0.95549(13) 0.26784(13) 0.0151(3) Uani 1 1 d . . . C5 C 0.80350(19) 0.75189(13) 0.16951(15) 0.0195(4) Uani 1 1 d . . . H5A H 0.7019 0.7432 0.1784 0.023 Uiso 1 1 calc R . . C6 C 0.88345(19) 0.66481(14) 0.21813(15) 0.0207(4) Uani 1 1 d . . . C7 C 0.8920(2) 1.29847(16) 0.06858(16) 0.0292(4) Uani 1 1 d . . . H7A H 0.9921 1.2951 0.0611 0.035 Uiso 1 1 calc R . . H7B H 0.8650 1.3687 0.0479 0.035 Uiso 1 1 calc R . . C8 C 0.7835(3) 1.1943(2) -0.0204(2) 0.0494(6) Uani 1 1 d . . . H8A H 0.6872 1.1887 -0.0024 0.059 Uiso 1 1 calc R . . C9 C 0.7568(4) 1.2147(3) -0.1425(2) 0.0877(12) Uani 1 1 d . . . H9A H 0.6872 1.1482 -0.2006 0.132 Uiso 1 1 calc R . . H9B H 0.8509 1.2246 -0.1602 0.132 Uiso 1 1 calc R . . H9C H 0.7152 1.2841 -0.1441 0.132 Uiso 1 1 calc R . . C10 C 0.8337(3) 1.0815(2) -0.0205(2) 0.0579(7) Uani 1 1 d . . . H10A H 0.8489 1.0682 0.0567 0.087 Uiso 1 1 calc R . . H10B H 0.9269 1.0844 -0.0399 0.087 Uiso 1 1 calc R . . H10C H 0.7579 1.0186 -0.0785 0.087 Uiso 1 1 calc R . . C11 C 0.9282(2) 1.09373(14) 0.46622(15) 0.0232(4) Uani 1 1 d . . . H11A H 1.0037 1.1638 0.5129 0.028 Uiso 1 1 calc R . . H11B H 0.8300 1.1125 0.4648 0.028 Uiso 1 1 calc R . . C12 C 0.9502(2) 1.00042(16) 0.53003(15) 0.0258(4) Uani 1 1 d . . . H12B H 0.8731 0.9299 0.4839 0.031 Uiso 1 1 calc R . . C13 C 0.9258(3) 1.04109(19) 0.64876(17) 0.0393(5) Uani 1 1 d . . . H13B H 0.8280 1.0614 0.6379 0.059 Uiso 1 1 calc R . . H13C H 1.0025 1.1087 0.6966 0.059 Uiso 1 1 calc R . . H13D H 0.9313 0.9792 0.6878 0.059 Uiso 1 1 calc R . . C14 C 1.1014(2) 0.96846(19) 0.54471(18) 0.0380(5) Uani 1 1 d . . . H14B H 1.1157 0.9432 0.4681 0.057 Uiso 1 1 calc R . . H14C H 1.1074 0.9059 0.5829 0.057 Uiso 1 1 calc R . . H14D H 1.1787 1.0357 0.5926 0.057 Uiso 1 1 calc R . . C15 C 0.7924(2) 0.73101(17) 0.03773(17) 0.0356(5) Uani 1 1 d . . . H15A H 0.7435 0.7899 0.0079 0.043 Uiso 1 1 calc R . . H15B H 0.8940 0.7427 0.0312 0.043 Uiso 1 1 calc R . . C16 C 0.7082(3) 0.61246(19) -0.03981(17) 0.0433(6) Uani 1 1 d . . . H16D H 0.7349 0.5552 0.0051 0.052 Uiso 1 1 calc R . . C17 C 0.5442(3) 0.6050(3) -0.0665(3) 0.0810(10) Uani 1 1 d . . . H17A H 0.4922 0.5282 -0.1163 0.121 Uiso 1 1 calc R . . H17B H 0.5149 0.6632 -0.1069 0.121 Uiso 1 1 calc R . . H17C H 0.5182 0.6189 0.0062 0.121 Uiso 1 1 calc R . . C18 C 0.7535(5) 0.5810(3) -0.1475(3) 0.1104(14) Uani 1 1 d . . . H18A H 0.6969 0.5047 -0.1954 0.166 Uiso 1 1 calc R . . H18B H 0.8595 0.5798 -0.1261 0.166 Uiso 1 1 calc R . . H18C H 0.7337 0.6380 -0.1917 0.166 Uiso 1 1 calc R . . O21 O 0.21612(13) -0.04585(10) 0.29624(11) 0.0257(3) Uani 1 1 d . . . O22 O 0.62718(13) 0.24536(10) 0.29631(11) 0.0266(3) Uani 1 1 d . . . O23 O 0.27402(14) 0.47324(11) 0.25284(12) 0.0300(3) Uani 1 1 d . . . O24 O 0.38669(15) 0.55533(10) 0.14508(11) 0.0271(3) Uani 1 1 d . . . N21 N 0.31311(16) -0.25579(11) 0.25339(12) 0.0201(3) Uani 1 1 d . . . H21A H 0.3752 -0.2397 0.3272 0.030 Uiso 1 1 calc R . . H21B H 0.3222 -0.3244 0.2109 0.030 Uiso 1 1 calc R . . H21C H 0.2180 -0.2599 0.2552 0.030 Uiso 1 1 calc R . . N22 N 0.44200(16) 0.04022(11) 0.29750(13) 0.0206(3) Uani 1 1 d . . . H22B H 0.5252 0.0300 0.2826 0.025 Uiso 1 1 calc R . . N23 N 0.40694(15) 0.29731(11) 0.23956(12) 0.0170(3) Uani 1 1 d . B . H23B H 0.3125 0.2832 0.2349 0.020 Uiso 1 1 calc R . . C21 C 0.35201(18) -0.16355(13) 0.19929(14) 0.0165(4) Uani 1 1 d . . . H21D H 0.4568 -0.1576 0.1978 0.020 Uiso 1 1 calc R . . C22 C 0.33258(19) -0.05040(14) 0.27048(15) 0.0194(4) Uani 1 1 d . . . C23 C 0.42735(19) 0.15667(14) 0.35150(15) 0.0200(4) Uani 1 1 d . . . H23C H 0.3199 0.1590 0.3373 0.024 Uiso 1 1 calc R . . C24 C 0.49440(19) 0.23733(13) 0.29166(14) 0.0175(4) Uani 1 1 d . . . C25 C 0.45920(18) 0.38636(14) 0.18903(14) 0.0178(4) Uani 1 1 d . . . H25A H 0.5619 0.4248 0.2400 0.021 Uiso 1 1 calc R A 1 C26 C 0.36274(19) 0.47863(14) 0.19530(15) 0.0198(4) Uani 1 1 d . B . C27 C 0.2468(2) -0.19266(15) 0.07559(16) 0.0257(4) Uani 1 1 d . . . H27A H 0.1439 -0.2061 0.0791 0.031 Uiso 1 1 calc R . . H27B H 0.2623 -0.2659 0.0307 0.031 Uiso 1 1 calc R . . C28 C 0.2624(2) -0.10210(17) 0.00877(17) 0.0317(5) Uani 1 1 d . . . H28A H 0.2564 -0.0266 0.0579 0.038 Uiso 1 1 calc R . . C29 C 0.1340(3) -0.1336(2) -0.10385(18) 0.0451(6) Uani 1 1 d . . . H29A H 0.1441 -0.0752 -0.1462 0.068 Uiso 1 1 calc R . . H29B H 0.0401 -0.1367 -0.0855 0.068 Uiso 1 1 calc R . . H29C H 0.1353 -0.2089 -0.1522 0.068 Uiso 1 1 calc R . . C30 C 0.4092(3) -0.0878(2) -0.0170(2) 0.0458(6) Uani 1 1 d . . . H30A H 0.4141 -0.0288 -0.0593 0.069 Uiso 1 1 calc R . . H30B H 0.4178 -0.1611 -0.0646 0.069 Uiso 1 1 calc R . . H30C H 0.4905 -0.0641 0.0563 0.069 Uiso 1 1 calc R . . C31 C 0.5064(2) 0.19105(15) 0.48464(16) 0.0247(4) Uani 1 1 d . . . H31A H 0.4752 0.1266 0.5155 0.030 Uiso 1 1 calc R . . H31B H 0.6143 0.1989 0.4969 0.030 Uiso 1 1 calc R . . C32 C 0.4804(2) 0.30198(16) 0.55776(19) 0.0375(5) Uani 1 1 d . . . H32A H 0.5345 0.3077 0.6406 0.045 Uiso 1 1 calc R . . C33 C 0.3167(3) 0.2920(2) 0.5501(2) 0.0510(6) Uani 1 1 d . . . H33A H 0.3023 0.3638 0.5966 0.077 Uiso 1 1 calc R . . H33B H 0.2856 0.2278 0.5800 0.077 Uiso 1 1 calc R . . H33C H 0.2572 0.2782 0.4688 0.077 Uiso 1 1 calc R . . C34 C 0.5342(3) 0.41271(18) 0.5364(2) 0.0484(6) Uani 1 1 d . . . H34A H 0.6394 0.4201 0.5417 0.073 Uiso 1 1 calc R . . H34B H 0.5216 0.4766 0.5947 0.073 Uiso 1 1 calc R . . H34C H 0.4773 0.4147 0.4585 0.073 Uiso 1 1 calc R . . C35 C 0.4693(2) 0.33915(15) 0.06696(16) 0.0251(4) Uani 0.819(5) 1 d PD B 1 H35A H 0.5347 0.3990 0.0503 0.030 Uiso 0.819(5) 1 calc PR B 1 H35B H 0.5185 0.2724 0.0674 0.030 Uiso 0.819(5) 1 calc PR B 1 C36 C 0.3255(3) 0.3013(3) -0.0330(2) 0.0325(8) Uani 0.819(5) 1 d PD B 1 H36 H 0.2702 0.3658 -0.0313 0.039 Uiso 0.819(5) 1 calc PR B 1 C37 C 0.2273(3) 0.1951(3) -0.0281(2) 0.0551(10) Uani 0.819(5) 1 d PD B 1 H37A H 0.1361 0.1747 -0.0938 0.083 Uiso 0.819(5) 1 calc PR B 1 H37B H 0.2026 0.2110 0.0451 0.083 Uiso 0.819(5) 1 calc PR B 1 H37C H 0.2799 0.1309 -0.0325 0.083 Uiso 0.819(5) 1 calc PR B 1 C38 C 0.3622(5) 0.2715(3) -0.1495(3) 0.0785(14) Uani 0.819(5) 1 d PD B 1 H38A H 0.2700 0.2482 -0.2145 0.118 Uiso 0.819(5) 1 calc PR B 1 H38B H 0.4163 0.2083 -0.1515 0.118 Uiso 0.819(5) 1 calc PR B 1 H38C H 0.4236 0.3394 -0.1563 0.118 Uiso 0.819(5) 1 calc PR B 1 C35A C 0.4693(2) 0.33915(15) 0.06696(16) 0.0251(4) Uani 0.181(5) 1 d PD B 2 H35C H 0.5483 0.2936 0.0715 0.030 Uiso 0.181(5) 1 calc PR B 2 H35D H 0.4975 0.4044 0.0361 0.030 Uiso 0.181(5) 1 calc PR B 2 C36A C 0.3206(13) 0.2616(11) -0.0191(10) 0.033(5) Uiso 0.181(5) 1 d PD B 2 H36A H 0.2738 0.2083 0.0182 0.039 Uiso 0.181(5) 1 calc PR B 2 C37A C 0.2144(13) 0.3380(10) -0.0653(10) 0.038(3) Uiso 0.181(5) 1 d PD B 2 H37D H 0.1225 0.2889 -0.1207 0.057 Uiso 0.181(5) 1 calc PR B 2 H37E H 0.2617 0.3868 -0.1043 0.057 Uiso 0.181(5) 1 calc PR B 2 H37F H 0.1918 0.3867 -0.0001 0.057 Uiso 0.181(5) 1 calc PR B 2 C38A C 0.3579(16) 0.1933(13) -0.1279(11) 0.054(4) Uiso 0.181(5) 1 d PD B 2 H38D H 0.4192 0.1386 -0.1051 0.081 Uiso 0.181(5) 1 calc PR B 2 H38E H 0.4121 0.2473 -0.1580 0.081 Uiso 0.181(5) 1 calc PR B 2 H38F H 0.2658 0.1512 -0.1884 0.081 Uiso 0.181(5) 1 calc PR B 2 N11P N 0.02767(18) 0.46911(13) 0.51360(13) 0.0293(4) Uani 1 1 d . . . C11P C -0.0554(3) 0.40589(17) 0.55664(18) 0.0372(5) Uani 1 1 d . . . H11P H -0.1378 0.3495 0.5041 0.045 Uiso 1 1 calc R . . C12P C -0.0278(4) 0.4181(3) 0.6735(2) 0.0669(9) Uani 1 1 d . . . H12P H -0.0897 0.3719 0.7020 0.080 Uiso 1 1 calc R . . C13P C 0.0952(5) 0.5011(3) 0.7498(2) 0.0846(11) Uani 1 1 d . . . H13P H 0.1201 0.5115 0.8315 0.101 Uiso 1 1 calc R . . C14P C 0.1784(4) 0.5670(3) 0.7036(3) 0.0713(9) Uani 1 1 d . . . H14P H 0.2607 0.6249 0.7536 0.086 Uiso 1 1 calc R . . C15P C 0.1430(2) 0.54954(18) 0.5848(2) 0.0433(6) Uani 1 1 d . . . C16P C 0.2305(3) 0.6188(2) 0.5293(3) 0.0695(8) Uani 1 1 d . . . H16A H 0.1868 0.5929 0.4446 0.104 Uiso 1 1 calc R . . H16B H 0.3332 0.6081 0.5505 0.104 Uiso 1 1 calc R . . H16C H 0.2285 0.7005 0.5568 0.104 Uiso 1 1 calc R . . N21P N 0.56198(18) 0.76420(13) 0.45549(14) 0.0307(4) Uani 1 1 d . . . C21P C 0.6455(2) 0.69370(16) 0.41328(18) 0.0304(4) Uani 1 1 d . . . H21P H 0.6205 0.6630 0.3314 0.036 Uiso 1 1 calc R . . C22P C 0.7635(2) 0.66490(17) 0.48309(18) 0.0347(5) Uani 1 1 d . . . H22P H 0.8181 0.6140 0.4506 0.042 Uiso 1 1 calc R . . C23P C 0.8015(3) 0.71083(19) 0.60073(19) 0.0453(6) Uani 1 1 d . . . H23P H 0.8841 0.6931 0.6513 0.054 Uiso 1 1 calc R . . C24P C 0.7191(3) 0.78285(19) 0.64511(18) 0.0426(5) Uani 1 1 d . . . H24P H 0.7428 0.8142 0.7268 0.051 Uiso 1 1 calc R . . C25P C 0.6018(2) 0.80926(17) 0.57023(18) 0.0344(5) Uani 1 1 d . . . C26P C 0.5092(3) 0.89130(18) 0.6141(2) 0.0507(6) Uani 1 1 d . . . H26A H 0.4317 0.8992 0.5478 0.076 Uiso 1 1 calc R . . H26B H 0.5729 0.9669 0.6564 0.076 Uiso 1 1 calc R . . H26C H 0.4633 0.8607 0.6662 0.076 Uiso 1 1 calc R . . O1W O 0.0725(7) 0.5365(5) 0.0173(5) 0.0446(15) Uiso 0.25 1 d P . . 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 O1 0.0148(7) 0.0232(7) 0.0607(9) 0.0207(6) 0.0191(6) 0.0091(5) O2 0.0112(6) 0.0159(6) 0.0376(7) 0.0065(5) 0.0079(5) 0.0048(5) O3 0.0125(8) 0.0251(7) 0.0995(12) 0.0295(8) 0.0107(7) 0.0066(6) O4 0.0186(7) 0.0151(6) 0.0439(8) 0.0116(5) 0.0108(5) 0.0048(5) N1 0.0186(8) 0.0113(7) 0.0324(8) 0.0098(6) 0.0117(6) 0.0066(6) N2 0.0131(8) 0.0116(7) 0.0348(8) 0.0079(6) 0.0109(6) 0.0078(6) N3 0.0111(7) 0.0083(7) 0.0283(8) 0.0031(6) 0.0051(6) 0.0018(6) C1 0.0140(9) 0.0108(8) 0.0309(9) 0.0089(7) 0.0105(7) 0.0040(7) C2 0.0121(9) 0.0116(8) 0.0303(9) 0.0043(7) 0.0088(7) 0.0035(7) C3 0.0110(8) 0.0089(8) 0.0301(9) 0.0057(7) 0.0043(7) 0.0026(6) C4 0.0178(9) 0.0123(8) 0.0179(8) 0.0069(6) 0.0068(6) 0.0039(7) C5 0.0120(9) 0.0107(8) 0.0322(10) 0.0022(7) 0.0037(7) 0.0020(7) C6 0.0157(10) 0.0121(9) 0.0334(10) 0.0046(7) 0.0060(7) 0.0050(7) C7 0.0345(12) 0.0243(10) 0.0329(11) 0.0090(8) 0.0122(8) 0.0139(9) C8 0.0301(13) 0.0571(15) 0.0463(13) -0.0146(11) 0.0108(10) 0.0088(11) C9 0.110(3) 0.086(2) 0.0382(15) -0.0168(14) -0.0135(15) 0.055(2) C10 0.074(2) 0.0356(13) 0.0517(15) -0.0103(11) 0.0242(13) -0.0056(12) C11 0.0201(10) 0.0170(9) 0.0305(10) 0.0011(8) 0.0077(7) 0.0060(7) C12 0.0264(11) 0.0237(10) 0.0237(9) 0.0044(8) 0.0038(7) 0.0036(8) C13 0.0440(14) 0.0440(13) 0.0299(11) 0.0106(10) 0.0102(9) 0.0102(10) C14 0.0381(13) 0.0394(12) 0.0359(12) 0.0099(10) 0.0058(9) 0.0171(10) C15 0.0352(12) 0.0298(11) 0.0376(11) 0.0123(9) 0.0069(9) -0.0046(9) C16 0.0500(15) 0.0446(13) 0.0251(11) 0.0082(10) 0.0009(9) -0.0020(11) C17 0.048(2) 0.0671(19) 0.095(2) -0.0054(17) 0.0029(15) -0.0161(15) C18 0.106(3) 0.106(3) 0.085(2) -0.035(2) 0.042(2) -0.017(2) O21 0.0172(7) 0.0154(6) 0.0512(8) 0.0102(6) 0.0190(6) 0.0067(5) O22 0.0160(7) 0.0232(7) 0.0507(8) 0.0198(6) 0.0157(6) 0.0101(5) O23 0.0231(7) 0.0219(7) 0.0546(8) 0.0130(6) 0.0229(6) 0.0104(6) O24 0.0371(8) 0.0155(6) 0.0373(7) 0.0128(6) 0.0177(6) 0.0125(6) N21 0.0175(8) 0.0142(7) 0.0295(8) 0.0065(6) 0.0076(6) 0.0047(6) N22 0.0132(8) 0.0118(7) 0.0427(9) 0.0099(6) 0.0131(6) 0.0087(6) N23 0.0098(7) 0.0124(7) 0.0302(8) 0.0063(6) 0.0072(6) 0.0042(6) C21 0.0126(9) 0.0132(8) 0.0281(9) 0.0095(7) 0.0083(7) 0.0066(7) C22 0.0161(9) 0.0143(9) 0.0294(9) 0.0092(7) 0.0052(7) 0.0065(7) C23 0.0148(9) 0.0122(8) 0.0361(10) 0.0062(7) 0.0114(7) 0.0054(7) C24 0.0171(9) 0.0092(8) 0.0273(9) 0.0025(7) 0.0102(7) 0.0039(7) C25 0.0114(8) 0.0136(8) 0.0282(9) 0.0052(7) 0.0056(7) 0.0036(7) C26 0.0159(9) 0.0129(8) 0.0291(9) 0.0012(8) 0.0082(7) 0.0028(7) C27 0.0234(10) 0.0215(9) 0.0307(10) 0.0068(8) 0.0044(7) 0.0074(8) C28 0.0280(11) 0.0310(11) 0.0369(11) 0.0122(9) 0.0067(8) 0.0094(9) C29 0.0485(15) 0.0461(13) 0.0364(12) 0.0137(10) -0.0004(10) 0.0177(11) C30 0.0401(14) 0.0667(16) 0.0436(13) 0.0302(12) 0.0189(10) 0.0157(12) C31 0.0238(10) 0.0201(9) 0.0333(10) 0.0097(8) 0.0110(8) 0.0060(8) C32 0.0350(13) 0.0230(10) 0.0435(12) 0.0017(9) 0.0016(9) 0.0013(9) C33 0.0443(15) 0.0469(14) 0.0524(14) -0.0083(11) 0.0118(11) 0.0202(12) C34 0.0497(16) 0.0332(12) 0.0524(14) -0.0027(10) 0.0127(11) 0.0040(11) C35 0.0279(11) 0.0175(9) 0.0363(10) 0.0086(8) 0.0171(8) 0.0084(8) C36 0.0467(19) 0.0292(17) 0.0242(14) 0.0054(13) 0.0111(11) 0.0186(13) C37 0.0321(18) 0.084(2) 0.0400(17) 0.0199(16) 0.0022(12) -0.0071(16) C38 0.109(3) 0.074(3) 0.0326(17) -0.0001(16) 0.0270(18) -0.036(2) C35A 0.0279(11) 0.0175(9) 0.0363(10) 0.0086(8) 0.0171(8) 0.0084(8) N11P 0.0279(9) 0.0204(8) 0.0358(9) 0.0011(7) 0.0054(7) 0.0118(7) C11P 0.0509(15) 0.0265(11) 0.0413(13) 0.0056(9) 0.0247(10) 0.0162(10) C12P 0.105(3) 0.0640(17) 0.0625(19) 0.0238(15) 0.0570(18) 0.0449(18) C13P 0.130(3) 0.095(2) 0.0280(14) 0.0029(16) 0.0138(17) 0.065(2) C14P 0.067(2) 0.0589(18) 0.0567(19) -0.0193(15) -0.0119(14) 0.0286(16) C15P 0.0319(13) 0.0311(12) 0.0526(14) -0.0045(10) -0.0008(10) 0.0131(10) C16P 0.0372(16) 0.0434(15) 0.106(2) 0.0045(15) 0.0070(14) -0.0090(12) N21P 0.0245(9) 0.0242(8) 0.0402(10) 0.0069(7) 0.0078(7) 0.0005(7) C21P 0.0269(11) 0.0250(10) 0.0401(11) 0.0086(9) 0.0113(8) 0.0062(9) C22P 0.0324(12) 0.0276(11) 0.0426(12) 0.0088(9) 0.0073(9) 0.0100(9) C23P 0.0381(14) 0.0441(13) 0.0459(13) 0.0105(11) -0.0017(10) 0.0138(11) C24P 0.0466(14) 0.0408(13) 0.0326(11) 0.0046(10) 0.0029(10) 0.0095(11) C25P 0.0344(12) 0.0260(10) 0.0399(12) 0.0051(9) 0.0114(9) 0.0018(9) C26P 0.0488(16) 0.0292(12) 0.0711(17) -0.0003(11) 0.0253(12) 0.0068(11) _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 O1 C2 1.232(2) . ? O2 C4 1.2411(19) . ? O3 C6 1.245(2) . ? O4 C6 1.259(2) . ? N1 C1 1.487(2) . ? N2 C2 1.336(2) . ? N2 C3 1.455(2) . ? N3 C4 1.315(2) . ? N3 C5 1.458(2) . ? C1 C7 1.511(2) . ? C1 C2 1.515(2) . ? C3 C4 1.533(2) . ? C3 C11 1.533(2) . ? C5 C6 1.521(2) . ? C5 C15 1.565(3) . ? C7 C8 1.524(3) . ? C8 C10 1.511(4) . ? C8 C9 1.544(4) . ? C11 C12 1.525(3) . ? C12 C14 1.520(3) . ? C12 C13 1.531(3) . ? C15 C16 1.523(3) . ? C16 C18 1.494(4) . ? C16 C17 1.500(4) . ? O21 C22 1.240(2) . ? O22 C24 1.245(2) . ? O23 C26 1.247(2) . ? O24 C26 1.258(2) . ? N21 C21 1.483(2) . ? N22 C22 1.330(2) . ? N22 C23 1.466(2) . ? N23 C24 1.314(2) . ? N23 C25 1.462(2) . ? C21 C22 1.522(2) . ? C21 C27 1.526(2) . ? C23 C24 1.526(2) . ? C23 C31 1.553(3) . ? C25 C35 1.525(2) . ? C25 C26 1.543(2) . ? C27 C28 1.531(3) . ? C28 C30 1.515(3) . ? C28 C29 1.525(3) . ? C31 C32 1.537(3) . ? C32 C34 1.482(3) . ? C32 C33 1.529(3) . ? C35 C36 1.520(3) . ? C36 C37 1.516(4) . ? C36 C38 1.550(4) . ? C36A C37A 1.546(12) . ? C36A C38A 1.569(12) . ? N11P C11P 1.323(3) . ? N11P C15P 1.330(3) . ? C11P C12P 1.369(3) . ? C12P C13P 1.404(5) . ? C13P C14P 1.370(5) . ? C14P C15P 1.377(4) . ? C15P C16P 1.501(4) . ? N21P C25P 1.332(3) . ? N21P C21P 1.358(3) . ? C21P C22P 1.364(3) . ? C22P C23P 1.367(3) . ? C23P C24P 1.372(3) . ? C24P C25P 1.375(3) . ? C25P C26P 1.522(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N2 C3 124.45(14) . . ? C4 N3 C5 124.33(14) . . ? N1 C1 C7 109.36(14) . . ? N1 C1 C2 108.09(13) . . ? C7 C1 C2 113.78(14) . . ? O1 C2 N2 124.51(16) . . ? O1 C2 C1 120.42(15) . . ? N2 C2 C1 115.06(14) . . ? N2 C3 C4 107.65(13) . . ? N2 C3 C11 109.26(13) . . ? C4 C3 C11 109.50(13) . . ? O2 C4 N3 123.99(14) . . ? O2 C4 C3 119.45(14) . . ? N3 C4 C3 116.55(14) . . ? N3 C5 C6 109.10(13) . . ? N3 C5 C15 109.11(14) . . ? C6 C5 C15 109.22(15) . . ? O3 C6 O4 124.70(16) . . ? O3 C6 C5 117.94(15) . . ? O4 C6 C5 117.34(15) . . ? C1 C7 C8 116.89(17) . . ? C10 C8 C7 114.1(2) . . ? C10 C8 C9 109.7(2) . . ? C7 C8 C9 108.6(2) . . ? C12 C11 C3 117.96(14) . . ? C14 C12 C11 113.22(16) . . ? C14 C12 C13 110.41(16) . . ? C11 C12 C13 108.76(15) . . ? C16 C15 C5 115.30(16) . . ? C18 C16 C17 112.2(2) . . ? C18 C16 C15 111.7(2) . . ? C17 C16 C15 110.8(2) . . ? C22 N22 C23 121.61(14) . . ? C24 N23 C25 123.05(14) . . ? N21 C21 C22 108.32(13) . . ? N21 C21 C27 108.50(13) . . ? C22 C21 C27 109.66(14) . . ? O21 C22 N22 123.70(15) . . ? O21 C22 C21 119.54(15) . . ? N22 C22 C21 116.70(14) . . ? N22 C23 C24 106.87(13) . . ? N22 C23 C31 110.65(14) . . ? C24 C23 C31 111.73(14) . . ? O22 C24 N23 123.46(15) . . ? O22 C24 C23 119.61(15) . . ? N23 C24 C23 116.90(15) . . ? N23 C25 C35 113.62(13) . . ? N23 C25 C26 109.03(13) . . ? C35 C25 C26 112.96(14) . . ? O23 C26 O24 126.40(16) . . ? O23 C26 C25 117.69(15) . . ? O24 C26 C25 115.84(15) . . ? C21 C27 C28 116.04(15) . . ? C30 C28 C29 110.37(18) . . ? C30 C28 C27 112.52(17) . . ? C29 C28 C27 109.71(17) . . ? C32 C31 C23 117.38(16) . . ? C34 C32 C33 108.9(2) . . ? C34 C32 C31 118.00(19) . . ? C33 C32 C31 110.72(16) . . ? C36 C35 C25 117.52(17) . . ? C37 C36 C35 112.7(3) . . ? C37 C36 C38 107.5(2) . . ? C35 C36 C38 109.0(2) . . ? C37A C36A C38A 105.6(10) . . ? C11P N11P C15P 120.05(19) . . ? N11P C11P C12P 122.9(2) . . ? C11P C12P C13P 117.8(3) . . ? C14P C13P C12P 118.4(3) . . ? C13P C14P C15P 120.3(3) . . ? N11P C15P C14P 120.6(2) . . ? N11P C15P C16P 116.8(2) . . ? C14P C15P C16P 122.6(2) . . ? C25P N21P C21P 117.51(17) . . ? N21P C21P C22P 122.97(19) . . ? C21P C22P C23P 118.6(2) . . ? C22P C23P C24P 119.3(2) . . ? C23P C24P C25P 119.4(2) . . ? N21P C25P C24P 122.16(19) . . ? N21P C25P C26P 116.07(19) . . ? C24P C25P C26P 121.8(2) . . ? 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 C23 C24 N23 C25 173.57(14) . . . . ? C21 C22 N22 C23 171.44(15) . . . . ? C24 N23 C25 C26 -150.18(14) . . . . ? C22 N22 C23 C24 -137.75(16) . . . . ? N23 C25 C26 O24 -173.72(14) . . . . ? N23 C25 C26 O23 9.2(2) . . . . ? N22 C23 C24 N23 121.15(15) . . . . ? N21 C21 C22 N22 133.34(15) . . . . ? C3 C4 N3 C5 175.35(14) . . . . ? C1 C2 N2 C3 178.39(14) . . . . ? C4 N3 C5 C6 -137.56(16) . . . . ? C2 N2 C3 C4 -117.78(16) . . . . ? N3 C5 C6 O4 148.69(15) . . . . ? N3 C5 C6 O3 -32.6(2) . . . . ? N2 C3 C4 N3 129.67(15) . . . . ? N1 C1 C2 N2 115.41(15) . . . . ? 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 N23 H23B O1 0.88 2.14 2.9956(18) 164.7 1_445 N21 H21C O3 0.91 1.90 2.790(2) 164.6 1_445 N21 H21B O23 0.91 2.63 3.2641(18) 127.3 1_545 N21 H21B O24 0.91 1.78 2.6673(18) 166.0 1_545 N21 H21A N21P 0.91 2.04 2.897(2) 157.2 1_545 N1 H1B O3 0.91 2.48 3.1799(18) 134.5 1_565 N1 H1B O4 0.91 1.81 2.6774(18) 158.8 1_565 N3 H3A O21 0.88 2.15 3.0049(18) 165.4 1_665 N1 H1C O23 0.91 1.87 2.7769(19) 173.3 1_665 N1 H1A N11P 0.91 2.00 2.910(2) 172.8 1_665 N22 H22B O2 0.88 2.07 2.9159(18) 160.9 1_545 N2 H2A O22 0.88 2.00 2.8586(18) 166.7 1_565 _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.404 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.065 _chemical_name_common ;L-leucyl-L-leucyl-L-leucine - 2-methylpyridine clathrate (1:1:0.12) ; #===END data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 642089' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_sum 'C24 H42 N4 O4' _chemical_formula_weight 450.61 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5671(14) _cell_length_b 12.091(2) _cell_length_c 12.440(2) _cell_angle_alpha 102.069(8) _cell_angle_beta 101.335(7) _cell_angle_gamma 99.598(7) _cell_volume 1346.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3093 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9595 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22690 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_sigmaI/netI 0.1637 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 21.96 _reflns_number_total 5970 _reflns_number_gt 3805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details rm _refine_ls_number_reflns 5970 _refine_ls_number_parameters 756 _refine_ls_number_restraints 3003 _refine_ls_R_factor_all 0.1744 _refine_ls_R_factor_gt 0.1291 _refine_ls_wR_factor_ref 0.3669 _refine_ls_wR_factor_gt 0.3111 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.227 _refine_ls_shift/su_max 0.002 _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 O1 O 0.1189(7) 0.7912(6) 0.1671(6) 0.0377(19) Uani 0.730(7) 1 d PDU A 1 O2 O 0.5354(6) 1.0692(5) 0.1563(6) 0.0329(18) Uani 0.730(7) 1 d PDU A 1 O3 O 0.2134(7) 1.3246(6) 0.1557(7) 0.041(2) Uani 0.730(7) 1 d PDU A 1 O4 O 0.3211(8) 1.4005(6) 0.0411(7) 0.055(2) Uani 0.730(7) 1 d PDU A 1 N1 N 0.2118(9) 0.5765(7) 0.1315(7) 0.040(2) Uani 0.730(7) 1 d PDU A 1 H1A H 0.2666 0.5897 0.2034 0.059 Uiso 0.730(7) 1 calc PR A 1 H1B H 0.2220 0.5086 0.0889 0.059 Uiso 0.730(7) 1 calc PR A 1 H1C H 0.1163 0.5721 0.1327 0.059 Uiso 0.730(7) 1 calc PR A 1 N2 N 0.3479(7) 0.8731(6) 0.1748(6) 0.0281(17) Uani 0.730(7) 1 d PDU A 1 H2A H 0.4302 0.8609 0.1583 0.034 Uiso 0.730(7) 1 calc PR A 1 N3 N 0.3339(8) 1.1455(6) 0.1366(5) 0.0321(18) Uani 0.730(7) 1 d PDU A 1 H3A H 0.2432 1.1383 0.1435 0.038 Uiso 0.730(7) 1 calc PR A 1 C1 C 0.2617(10) 0.6727(6) 0.0815(6) 0.034(2) Uani 0.730(7) 1 d PDU A 1 H1S H 0.3671 0.6798 0.0805 0.040 Uiso 0.730(7) 1 calc PR A 1 C2 C 0.2365(9) 0.7855(7) 0.1470(7) 0.032(2) Uani 0.730(7) 1 d PDU A 1 C3 C 0.3427(9) 0.9924(7) 0.2331(6) 0.0315(18) Uani 0.730(7) 1 d PDU A 1 H3B H 0.2393 0.9997 0.2288 0.038 Uiso 0.730(7) 1 calc PR A 1 C4 C 0.4144(9) 1.0716(7) 0.1751(7) 0.032(2) Uani 0.730(7) 1 d PDU A 1 C5 C 0.3906(9) 1.2346(7) 0.0852(7) 0.0304(18) Uani 0.730(7) 1 d PDU A 1 H5 H 0.4916 1.2722 0.1318 0.036 Uiso 0.730(7) 1 calc PR A 1 C6 C 0.3000(10) 1.3262(8) 0.0967(8) 0.036(2) Uani 0.730(7) 1 d PDU A 1 C7 C 0.1670(11) 0.6407(8) -0.0376(7) 0.048(2) Uani 0.730(7) 1 d PDU A 1 H7A H 0.0630 0.6255 -0.0350 0.058 Uiso 0.730(7) 1 calc PR A 1 H7B H 0.1863 0.5686 -0.0810 0.058 Uiso 0.730(7) 1 calc PR A 1 C8 C 0.1960(11) 0.7364(9) -0.0980(8) 0.056(2) Uani 0.730(7) 1 d PDU A 1 H8A H 0.1851 0.8108 -0.0509 0.067 Uiso 0.730(7) 1 calc PR A 1 C9 C 0.3470(13) 0.7526(12) -0.1219(11) 0.074(3) Uani 0.730(7) 1 d PDU A 1 H9A H 0.3609 0.8161 -0.1591 0.111 Uiso 0.730(7) 1 calc PR A 1 H9B H 0.3561 0.6810 -0.1715 0.111 Uiso 0.730(7) 1 calc PR A 1 H9C H 0.4213 0.7711 -0.0505 0.111 Uiso 0.730(7) 1 calc PR A 1 C10 C 0.0756(13) 0.6990(11) -0.2085(10) 0.080(4) Uani 0.730(7) 1 d PDU A 1 H10A H 0.0875 0.7569 -0.2524 0.119 Uiso 0.730(7) 1 calc PR A 1 H10B H -0.0202 0.6922 -0.1905 0.119 Uiso 0.730(7) 1 calc PR A 1 H10C H 0.0828 0.6239 -0.2529 0.119 Uiso 0.730(7) 1 calc PR A 1 C11 C 0.4294(11) 1.0202(8) 0.3583(7) 0.040(2) Uani 0.730(7) 1 d PDU A 1 H11A H 0.5295 1.0080 0.3595 0.049 Uiso 0.730(7) 1 calc PR A 1 H11B H 0.3826 0.9641 0.3952 0.049 Uiso 0.730(7) 1 calc PR A 1 C12 C 0.4411(9) 1.1453(7) 0.4306(7) 0.044(2) Uani 0.730(7) 1 d PDU A 1 H12A H 0.4809 1.2033 0.3914 0.053 Uiso 0.730(7) 1 calc PR A 1 C13 C 0.5422(14) 1.1639(13) 0.5464(10) 0.102(4) Uani 0.730(7) 1 d PDU A 1 H13A H 0.5532 1.2435 0.5903 0.152 Uiso 0.730(7) 1 calc PR A 1 H13B H 0.6380 1.1505 0.5374 0.152 Uiso 0.730(7) 1 calc PR A 1 H13C H 0.5007 1.1096 0.5862 0.152 Uiso 0.730(7) 1 calc PR A 1 C14 C 0.2955(11) 1.1646(11) 0.4506(9) 0.086(3) Uani 0.730(7) 1 d PDU A 1 H14A H 0.3082 1.2429 0.4982 0.128 Uiso 0.730(7) 1 calc PR A 1 H14B H 0.2566 1.1075 0.4888 0.128 Uiso 0.730(7) 1 calc PR A 1 H14C H 0.2273 1.1558 0.3779 0.128 Uiso 0.730(7) 1 calc PR A 1 C15 C 0.4034(9) 1.1896(8) -0.0349(7) 0.050(2) Uani 0.730(7) 1 d PDU A 1 H15A H 0.4581 1.1268 -0.0361 0.060 Uiso 0.730(7) 1 calc PR A 1 H15B H 0.4612 1.2530 -0.0573 0.060 Uiso 0.730(7) 1 calc PR A 1 C16 C 0.2585(11) 1.1435(10) -0.1221(9) 0.067(3) Uani 0.730(7) 1 d PDU A 1 H16A H 0.1926 1.1987 -0.1100 0.080 Uiso 0.730(7) 1 calc PR A 1 C17 C 0.187(2) 1.0293(11) -0.1165(13) 0.115(5) Uani 0.730(7) 1 d PDU A 1 H17A H 0.1681 1.0338 -0.0414 0.173 Uiso 0.730(7) 1 calc PR A 1 H17B H 0.2514 0.9751 -0.1299 0.173 Uiso 0.730(7) 1 calc PR A 1 H17C H 0.0952 1.0021 -0.1743 0.173 Uiso 0.730(7) 1 calc PR A 1 C18 C 0.2821(19) 1.1275(16) -0.2439(11) 0.132(5) Uani 0.730(7) 1 d PDU A 1 H18A H 0.3409 1.1993 -0.2503 0.198 Uiso 0.730(7) 1 calc PR A 1 H18B H 0.1873 1.1088 -0.2985 0.198 Uiso 0.730(7) 1 calc PR A 1 H18C H 0.3330 1.0642 -0.2599 0.198 Uiso 0.730(7) 1 calc PR A 1 O1A O 0.1429(19) 0.8049(17) 0.2166(15) 0.030(5) Uiso 0.270(7) 1 d PDU A 2 O2A O 0.5632(16) 1.0951(15) 0.2036(15) 0.027(4) Uiso 0.270(7) 1 d PDU A 2 O3A O 0.2462(18) 1.3443(16) 0.2025(14) 0.021(5) Uiso 0.270(7) 1 d PDU A 2 O4A O 0.3664(19) 1.4293(16) 0.0907(15) 0.035(5) Uiso 0.270(7) 1 d PDU A 2 N1A N 0.239(2) 0.5974(17) 0.1736(18) 0.021(5) Uiso 0.270(7) 1 d PDU A 2 H1A1 H 0.2531 0.5294 0.1342 0.032 Uiso 0.270(7) 1 calc PR A 2 H1A2 H 0.1424 0.5914 0.1712 0.032 Uiso 0.270(7) 1 calc PR A 2 H1A3 H 0.2904 0.6132 0.2469 0.032 Uiso 0.270(7) 1 calc PR A 2 N2A N 0.380(2) 0.8909(14) 0.2214(16) 0.025(3) Uiso 0.270(7) 1 d PDU A 2 H2AA H 0.4632 0.8763 0.2094 0.030 Uiso 0.270(7) 1 calc PR A 2 N3A N 0.359(2) 1.1628(16) 0.1775(16) 0.031(3) Uiso 0.270(7) 1 d PDU A 2 H3AA H 0.2673 1.1536 0.1809 0.037 Uiso 0.270(7) 1 calc PR A 2 C1A C 0.291(3) 0.6937(17) 0.1215(17) 0.038(4) Uiso 0.270(7) 1 d PDU A 2 H1AC H 0.3991 0.7041 0.1313 0.046 Uiso 0.270(7) 1 calc PR A 2 C2A C 0.260(2) 0.8042(18) 0.188(2) 0.031(4) Uiso 0.270(7) 1 d PDU A 2 C3A C 0.373(3) 1.0077(16) 0.2764(18) 0.031(3) Uiso 0.270(7) 1 d PDU A 2 H3AB H 0.2696 1.0126 0.2738 0.037 Uiso 0.270(7) 1 calc PR A 2 C4A C 0.439(2) 1.090(2) 0.215(2) 0.034(3) Uiso 0.270(7) 1 d PDU A 2 C5A C 0.421(3) 1.2564(17) 0.1315(18) 0.032(3) Uiso 0.270(7) 1 d PDU A 2 H5A H 0.5229 1.2904 0.1790 0.039 Uiso 0.270(7) 1 calc PR A 2 C6A C 0.331(3) 1.359(2) 0.144(2) 0.040(4) Uiso 0.270(7) 1 d PDU A 2 C7A C 0.220(3) 0.674(2) -0.0053(19) 0.049(4) Uiso 0.270(7) 1 d PDU A 2 H7A1 H 0.2577 0.6110 -0.0469 0.058 Uiso 0.270(7) 1 calc PR A 2 H7A2 H 0.1138 0.6434 -0.0158 0.058 Uiso 0.270(7) 1 calc PR A 2 C8A C 0.234(3) 0.772(3) -0.065(2) 0.063(5) Uiso 0.270(7) 1 d PDU A 2 H8AA H 0.2181 0.8446 -0.0182 0.076 Uiso 0.270(7) 1 calc PR A 2 C9A C 0.390(3) 0.790(4) -0.082(3) 0.072(9) Uiso 0.270(7) 1 d PDU A 2 H9AA H 0.4089 0.8555 -0.1156 0.108 Uiso 0.270(7) 1 calc PR A 2 H9AB H 0.4014 0.7195 -0.1329 0.108 Uiso 0.270(7) 1 calc PR A 2 H9AC H 0.4600 0.8049 -0.0089 0.108 Uiso 0.270(7) 1 calc PR A 2 C10A C 0.142(4) 0.745(4) -0.187(3) 0.089(8) Uiso 0.270(7) 1 d PDU A 2 H10D H 0.0382 0.7356 -0.1859 0.134 Uiso 0.270(7) 1 calc PR A 2 H10E H 0.1576 0.6727 -0.2309 0.134 Uiso 0.270(7) 1 calc PR A 2 H10F H 0.1699 0.8083 -0.2211 0.134 Uiso 0.270(7) 1 calc PR A 2 C11A C 0.462(3) 1.045(3) 0.3986(19) 0.044(4) Uiso 0.270(7) 1 d PDU A 2 H11C H 0.4298 0.9812 0.4331 0.053 Uiso 0.270(7) 1 calc PR A 2 H11D H 0.5641 1.0428 0.3947 0.053 Uiso 0.270(7) 1 calc PR A 2 C12A C 0.471(3) 1.155(2) 0.485(2) 0.069(5) Uiso 0.270(7) 1 d PDU A 2 H12B H 0.3724 1.1631 0.4964 0.082 Uiso 0.270(7) 1 calc PR A 2 C13A C 0.526(3) 1.239(2) 0.420(2) 0.064(6) Uiso 0.270(7) 1 d PDU A 2 H13D H 0.4617 1.2205 0.3446 0.096 Uiso 0.270(7) 1 calc PR A 2 H13E H 0.6255 1.2327 0.4141 0.096 Uiso 0.270(7) 1 calc PR A 2 H13F H 0.5279 1.3183 0.4606 0.096 Uiso 0.270(7) 1 calc PR A 2 C14A C 0.583(5) 1.188(4) 0.599(3) 0.108(9) Uiso 0.270(7) 1 d PDU A 2 H14D H 0.5475 1.1442 0.6495 0.162 Uiso 0.270(7) 1 calc PR A 2 H14E H 0.5991 1.2710 0.6325 0.162 Uiso 0.270(7) 1 calc PR A 2 H14F H 0.6759 1.1688 0.5867 0.162 Uiso 0.270(7) 1 calc PR A 2 C15A C 0.433(3) 1.217(2) 0.0101(16) 0.042(4) Uiso 0.270(7) 1 d PDU A 2 H15C H 0.4994 1.2830 -0.0016 0.050 Uiso 0.270(7) 1 calc PR A 2 H15D H 0.4901 1.1553 0.0119 0.050 Uiso 0.270(7) 1 calc PR A 2 C16A C 0.321(3) 1.173(3) -0.0982(19) 0.063(4) Uiso 0.270(7) 1 d PDU A 2 H16B H 0.2717 1.2396 -0.0882 0.076 Uiso 0.270(7) 1 calc PR A 2 C17A C 0.189(4) 1.082(4) -0.110(3) 0.082(7) Uiso 0.270(7) 1 d PDU A 2 H17D H 0.1915 1.0622 -0.0369 0.123 Uiso 0.270(7) 1 calc PR A 2 H17E H 0.1887 1.0126 -0.1672 0.123 Uiso 0.270(7) 1 calc PR A 2 H17F H 0.1013 1.1110 -0.1323 0.123 Uiso 0.270(7) 1 calc PR A 2 C18A C 0.340(4) 1.175(4) -0.216(2) 0.082(7) Uiso 0.270(7) 1 d PDU A 2 H18D H 0.2479 1.1361 -0.2722 0.124 Uiso 0.270(7) 1 calc PR A 2 H18E H 0.4169 1.1343 -0.2325 0.124 Uiso 0.270(7) 1 calc PR A 2 H18F H 0.3669 1.2553 -0.2208 0.124 Uiso 0.270(7) 1 calc PR A 2 O21 O 0.0467(7) 1.0840(6) 0.1930(7) 0.047(2) Uani 0.719(5) 1 d PDU B 1 O22 O -0.3768(6) 0.7996(5) 0.1871(7) 0.0455(18) Uani 0.719(5) 1 d PDU B 1 O23 O -0.0628(7) 0.5388(5) 0.1735(6) 0.0512(18) Uani 0.719(5) 1 d PDU B 1 O24 O -0.2707(7) 0.4101(6) 0.1451(8) 0.061(2) Uani 0.719(5) 1 d PDU B 1 N21 N -0.0598(8) 1.2872(7) 0.1913(7) 0.045(2) Uani 0.719(5) 1 d PDU B 1 H21A H -0.0943 1.3427 0.1613 0.067 Uiso 0.719(5) 1 calc PR B 1 H21B H 0.0349 1.2911 0.1876 0.067 Uiso 0.719(5) 1 calc PR B 1 H21C H -0.0654 1.2990 0.2648 0.067 Uiso 0.719(5) 1 calc PR B 1 N22 N -0.1801(8) 1.0091(6) 0.2101(6) 0.0307(17) Uani 0.719(5) 1 d PDU B 1 H22A H -0.2714 1.0162 0.2010 0.037 Uiso 0.719(5) 1 calc PR B 1 N23 N -0.1919(7) 0.7112(5) 0.1592(6) 0.0275(17) Uani 0.719(5) 1 d PDU B 1 H23A H -0.0989 0.7189 0.1588 0.033 Uiso 0.719(5) 1 calc PR B 1 C21 C -0.1486(11) 1.1716(7) 0.1263(7) 0.041(2) Uani 0.719(5) 1 d PDU B 1 H21G H -0.2513 1.1674 0.1341 0.049 Uiso 0.719(5) 1 calc PR B 1 C22 C -0.0862(9) 1.0832(8) 0.1817(7) 0.037(2) Uani 0.719(5) 1 d PDU B 1 C23 C -0.1360(9) 0.9139(7) 0.2571(7) 0.0331(19) Uani 0.719(5) 1 d PDU B 1 H23B H -0.0372 0.9053 0.2462 0.040 Uiso 0.719(5) 1 calc PR B 1 C24 C -0.2445(8) 0.8073(7) 0.1975(7) 0.0312(19) Uani 0.719(5) 1 d PDU B 1 C26 C -0.1968(9) 0.5055(8) 0.1471(9) 0.048(2) Uani 0.719(5) 1 d PDU B 1 C27 C -0.1491(11) 1.1520(8) 0.0012(7) 0.051(2) Uani 0.719(5) 1 d PDU B 1 H27A H -0.0487 1.1494 -0.0067 0.061 Uiso 0.719(5) 1 calc PR B 1 H27B H -0.1749 1.2197 -0.0246 0.061 Uiso 0.719(5) 1 calc PR B 1 C28 C -0.2537(13) 1.0413(9) -0.0787(11) 0.065(3) Uani 0.719(5) 1 d PDU B 1 H28A H -0.3450 1.0280 -0.0512 0.079 Uiso 0.719(5) 1 calc PR B 1 C29 C -0.2928(19) 1.0572(15) -0.1954(13) 0.109(5) Uani 0.719(5) 1 d PDU B 1 H29A H -0.3599 0.9870 -0.2454 0.164 Uiso 0.719(5) 1 calc PR B 1 H29B H -0.2041 1.0720 -0.2231 0.164 Uiso 0.719(5) 1 calc PR B 1 H29C H -0.3401 1.1232 -0.1946 0.164 Uiso 0.719(5) 1 calc PR B 1 C30 C -0.1817(18) 0.9345(11) -0.0755(13) 0.088(4) Uani 0.719(5) 1 d PDU B 1 H30A H -0.2486 0.8646 -0.1264 0.132 Uiso 0.719(5) 1 calc PR B 1 H30B H -0.1612 0.9247 0.0019 0.132 Uiso 0.719(5) 1 calc PR B 1 H30C H -0.0904 0.9472 -0.1000 0.132 Uiso 0.719(5) 1 calc PR B 1 C31 C -0.1325(12) 0.9449(10) 0.3783(8) 0.054(2) Uani 0.719(5) 1 d PDU B 1 H31A H -0.2293 0.9595 0.3861 0.064 Uiso 0.719(5) 1 calc PR B 1 H31B H -0.0602 1.0188 0.4136 0.064 Uiso 0.719(5) 1 calc PR B 1 C32 C -0.0965(10) 0.8595(9) 0.4442(8) 0.060(2) Uani 0.719(5) 1 d PDU B 1 H32A H -0.1728 0.7865 0.4091 0.072 Uiso 0.719(5) 1 calc PR B 1 C33 C -0.1097(14) 0.9006(12) 0.5613(9) 0.095(4) Uani 0.719(5) 1 d PDU B 1 H33A H -0.2054 0.9199 0.5601 0.143 Uiso 0.719(5) 1 calc PR B 1 H33B H -0.0326 0.9697 0.6003 0.143 Uiso 0.719(5) 1 calc PR B 1 H33C H -0.0997 0.8396 0.6014 0.143 Uiso 0.719(5) 1 calc PR B 1 C34 C 0.0498(11) 0.8284(10) 0.4412(9) 0.077(3) Uani 0.719(5) 1 d PDU B 1 H34A H 0.0532 0.7984 0.3625 0.115 Uiso 0.719(5) 1 calc PR B 1 H34B H 0.0629 0.7691 0.4830 0.115 Uiso 0.719(5) 1 calc PR B 1 H34C H 0.1280 0.8976 0.4763 0.115 Uiso 0.719(5) 1 calc PR B 1 C25 C -0.2891(10) 0.5960(7) 0.1190(8) 0.048(2) Uani 0.719(5) 1 d PDU B 1 H25B H -0.3637 0.5947 0.1652 0.057 Uiso 0.719(5) 1 calc PR B 1 C35 C -0.3740(12) 0.5591(10) -0.0079(8) 0.074(3) Uani 0.719(5) 1 d PDU B 1 H35A H -0.4423 0.4841 -0.0198 0.089 Uiso 0.719(5) 1 calc PR B 1 H35B H -0.4343 0.6165 -0.0199 0.089 Uiso 0.719(5) 1 calc PR B 1 C36 C -0.2935(14) 0.5460(12) -0.0989(10) 0.088(3) Uani 0.719(5) 1 d PDU B 1 H36A H -0.2146 0.6173 -0.0813 0.106 Uiso 0.719(5) 1 calc PR B 1 C37 C -0.2221(17) 0.4421(12) -0.1104(13) 0.122(4) Uani 0.719(5) 1 d PDU B 1 H37A H -0.1421 0.4542 -0.0436 0.183 Uiso 0.719(5) 1 calc PR B 1 H37B H -0.1835 0.4332 -0.1784 0.183 Uiso 0.719(5) 1 calc PR B 1 H37C H -0.2946 0.3721 -0.1167 0.183 Uiso 0.719(5) 1 calc PR B 1 C38 C -0.3881(16) 0.5344(17) -0.2131(12) 0.153(6) Uani 0.719(5) 1 d PDU B 1 H38A H -0.4397 0.5981 -0.2100 0.229 Uiso 0.719(5) 1 calc PR B 1 H38B H -0.4592 0.4603 -0.2365 0.229 Uiso 0.719(5) 1 calc PR B 1 H38C H -0.3274 0.5372 -0.2678 0.229 Uiso 0.719(5) 1 calc PR B 1 C25A C -0.293(3) 0.5837(19) 0.057(2) 0.060(4) Uiso 0.281(5) 1 d PDU B 2 H25A H -0.3978 0.5684 0.0596 0.072 Uiso 0.281(5) 1 calc PR B 2 C35A C -0.258(3) 0.592(3) -0.053(2) 0.085(4) Uiso 0.281(5) 1 d PDU B 2 H35C H -0.2561 0.6745 -0.0482 0.102 Uiso 0.281(5) 1 calc PR B 2 H35D H -0.3532 0.5508 -0.1052 0.102 Uiso 0.281(5) 1 calc PR B 2 C36A C -0.158(3) 0.570(3) -0.131(2) 0.123(5) Uiso 0.281(5) 1 d PDU B 2 H36B H -0.0696 0.5483 -0.0919 0.148 Uiso 0.281(5) 1 calc PR B 2 C37A C -0.243(5) 0.471(3) -0.237(3) 0.140(9) Uiso 0.281(5) 1 d PDU B 2 H37D H -0.1916 0.4072 -0.2439 0.210 Uiso 0.281(5) 1 calc PR B 2 H37E H -0.2502 0.5001 -0.3054 0.210 Uiso 0.281(5) 1 calc PR B 2 H37F H -0.3417 0.4426 -0.2287 0.210 Uiso 0.281(5) 1 calc PR B 2 C38A C -0.114(6) 0.672(3) -0.179(3) 0.228(18) Uiso 0.281(5) 1 d PDU B 2 H38D H -0.0621 0.7397 -0.1168 0.342 Uiso 0.281(5) 1 calc PR B 2 H38E H -0.2010 0.6900 -0.2220 0.342 Uiso 0.281(5) 1 calc PR B 2 H38F H -0.0494 0.6531 -0.2292 0.342 Uiso 0.281(5) 1 calc PR B 2 O21A O 0.0255(18) 1.0597(17) 0.1472(15) 0.029(5) Uiso 0.281(5) 1 d PDU B 2 O22A O -0.3931(14) 0.7877(12) 0.1248(13) 0.020(4) Uiso 0.281(5) 1 d PDU B 2 O23A O -0.0747(19) 0.5152(16) 0.1003(16) 0.056(5) Uiso 0.281(5) 1 d PDU B 2 O24A O -0.2801(19) 0.3981(16) 0.0781(16) 0.052(5) Uiso 0.281(5) 1 d PDU B 2 N21A N -0.0867(19) 1.2652(14) 0.1427(15) 0.020(4) Uiso 0.281(5) 1 d PDU B 2 H21D H -0.0726 1.2782 0.2192 0.030 Uiso 0.281(5) 1 calc PR B 2 H21E H -0.1346 1.3177 0.1182 0.030 Uiso 0.281(5) 1 calc PR B 2 H21F H 0.0013 1.2725 0.1243 0.030 Uiso 0.281(5) 1 calc PR B 2 N22A N -0.201(2) 0.9846(15) 0.1659(16) 0.033(3) Uiso 0.281(5) 1 d PDU B 2 H22B H -0.2933 0.9898 0.1524 0.039 Uiso 0.281(5) 1 calc PR B 2 N23A N -0.209(2) 0.6977(14) 0.1046(16) 0.035(3) Uiso 0.281(5) 1 d PDU B 2 H23D H -0.1148 0.7118 0.1072 0.043 Uiso 0.281(5) 1 calc PR B 2 C21A C -0.175(3) 1.1466(16) 0.0880(18) 0.042(3) Uiso 0.281(5) 1 d PDU B 2 H21H H -0.2754 1.1416 0.1010 0.050 Uiso 0.281(5) 1 calc PR B 2 C22A C -0.104(2) 1.061(2) 0.140(2) 0.036(3) Uiso 0.281(5) 1 d PDU B 2 C23A C -0.159(2) 0.8909(16) 0.2161(15) 0.030(3) Uiso 0.281(5) 1 d PDU B 2 H23E H -0.0582 0.8830 0.2089 0.036 Uiso 0.281(5) 1 calc PR B 2 C24A C -0.2687(17) 0.7849(15) 0.1458(19) 0.031(3) Uiso 0.281(5) 1 d PDU B 2 C26A C -0.208(2) 0.4939(18) 0.0777(17) 0.050(3) Uiso 0.281(5) 1 d PDU B 2 C27A C -0.184(3) 1.123(3) -0.0378(19) 0.057(4) Uiso 0.281(5) 1 d PDU B 2 H27C H -0.0878 1.1164 -0.0527 0.069 Uiso 0.281(5) 1 calc PR B 2 H27D H -0.2152 1.1874 -0.0673 0.069 Uiso 0.281(5) 1 calc PR B 2 C28A C -0.295(4) 1.011(2) -0.095(3) 0.074(5) Uiso 0.281(5) 1 d PDU B 2 H28B H -0.3795 1.0013 -0.0589 0.089 Uiso 0.281(5) 1 calc PR B 2 C29A C -0.342(5) 1.019(4) -0.215(3) 0.082(7) Uiso 0.281(5) 1 d PDU B 2 H29D H -0.3960 1.0810 -0.2170 0.124 Uiso 0.281(5) 1 calc PR B 2 H29E H -0.4049 0.9453 -0.2615 0.124 Uiso 0.281(5) 1 calc PR B 2 H29F H -0.2556 1.0365 -0.2448 0.124 Uiso 0.281(5) 1 calc PR B 2 C30A C -0.233(4) 0.901(3) -0.114(3) 0.069(9) Uiso 0.281(5) 1 d PDU B 2 H30D H -0.3133 0.8326 -0.1408 0.104 Uiso 0.281(5) 1 calc PR B 2 H30E H -0.1703 0.8982 -0.0429 0.104 Uiso 0.281(5) 1 calc PR B 2 H30F H -0.1755 0.9029 -0.1713 0.104 Uiso 0.281(5) 1 calc PR B 2 C31A C -0.169(3) 0.904(2) 0.3391(16) 0.052(3) Uiso 0.281(5) 1 d PDU B 2 H31C H -0.1446 0.8333 0.3593 0.063 Uiso 0.281(5) 1 calc PR B 2 H31D H -0.2738 0.8984 0.3375 0.063 Uiso 0.281(5) 1 calc PR B 2 C32A C -0.087(3) 1.005(2) 0.4412(17) 0.061(5) Uiso 0.281(5) 1 d PDU B 2 H32B H -0.0711 1.0819 0.4226 0.073 Uiso 0.281(5) 1 calc PR B 2 C33A C -0.128(4) 1.008(3) 0.555(2) 0.095(8) Uiso 0.281(5) 1 d PDU B 2 H33D H -0.2340 0.9872 0.5421 0.142 Uiso 0.281(5) 1 calc PR B 2 H33E H -0.0911 1.0866 0.6046 0.142 Uiso 0.281(5) 1 calc PR B 2 H33F H -0.0837 0.9533 0.5907 0.142 Uiso 0.281(5) 1 calc PR B 2 C34A C 0.054(3) 0.960(3) 0.468(3) 0.102(7) Uiso 0.281(5) 1 d PDU B 2 H34D H 0.1026 0.9593 0.4057 0.153 Uiso 0.281(5) 1 calc PR B 2 H34E H 0.0303 0.8817 0.4783 0.153 Uiso 0.281(5) 1 calc PR B 2 H34F H 0.1196 1.0116 0.5380 0.153 Uiso 0.281(5) 1 calc PR B 2 N1P N 0.0192(10) 1.3361(7) 0.4229(7) 0.100(3) Uani 1 1 d G . . C1P C -0.0305(8) 1.2985(7) 0.5096(10) 0.133(4) Uani 1 1 d GD . . H1PB H -0.1188 1.2420 0.4927 0.160 Uiso 1 1 calc R . . C2P C 0.0490(13) 1.3437(9) 0.6212(8) 0.138(5) Uani 1 1 d GD . . C3P C 0.1782(12) 1.4265(9) 0.6459(7) 0.138(5) Uani 1 1 d GD . . H3PA H 0.2326 1.4574 0.7222 0.165 Uiso 1 1 calc R . . C4P C 0.2278(9) 1.4640(7) 0.5591(11) 0.205(9) Uani 1 1 d G . . H4PA H 0.3161 1.5206 0.5761 0.246 Uiso 1 1 calc R . . C5P C 0.1483(12) 1.4188(8) 0.4476(9) 0.134(4) Uani 1 1 d G . . H5PA H 0.1822 1.4445 0.3883 0.161 Uiso 1 1 calc R . . C6P C -0.004(2) 1.2986(19) 0.7154(13) 0.233(9) Uani 1 1 d D . . H6PA H 0.0656 1.3368 0.7882 0.350 Uiso 1 1 calc R . . H6PB H -0.0110 1.2147 0.7003 0.350 Uiso 1 1 calc R . . H6PC H -0.1000 1.3154 0.7182 0.350 Uiso 1 1 calc R . . N21P N -0.5849(5) 0.6313(6) -0.6339(7) 0.111(3) Uani 1 1 d G . . C21P C -0.4787(7) 0.5661(6) -0.6402(6) 0.108(3) Uani 1 1 d GD . . H21P H -0.4859 0.5095 -0.7078 0.129 Uiso 1 1 calc R . . C22P C -0.3621(7) 0.5837(8) -0.5475(7) 0.120(4) Uani 1 1 d GD . . C23P C -0.3517(10) 0.6666(9) -0.4485(6) 0.173(7) Uani 1 1 d GD . . H23C H -0.2720 0.6786 -0.3851 0.208 Uiso 1 1 calc R . . C24P C -0.4579(12) 0.7318(8) -0.4422(7) 0.208(8) Uani 1 1 d G . . H24A H -0.4508 0.7884 -0.3745 0.249 Uiso 1 1 calc R . . C25P C -0.5745(9) 0.7142(7) -0.5349(9) 0.163(6) Uani 1 1 d G . . H25P H -0.6471 0.7587 -0.5306 0.195 Uiso 1 1 calc R . . C26P C -0.2441(14) 0.5144(13) -0.5568(12) 0.193(7) Uani 1 1 d D . . H26A H -0.1698 0.5372 -0.4850 0.289 Uiso 1 1 calc R . . H26B H -0.1987 0.5298 -0.6178 0.289 Uiso 1 1 calc R . . H26C H -0.2878 0.4316 -0.5735 0.289 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 O1 0.035(3) 0.028(3) 0.055(4) 0.007(3) 0.006(3) 0.029(2) O2 0.033(2) 0.029(2) 0.038(2) 0.0069(18) 0.0021(17) 0.0187(16) O3 0.042(3) 0.027(3) 0.057(4) 0.010(3) 0.006(3) 0.029(3) O4 0.061(4) 0.035(3) 0.081(4) 0.017(3) 0.017(3) 0.044(3) N1 0.039(3) 0.037(3) 0.044(3) 0.007(2) 0.004(2) 0.0235(19) N2 0.027(2) 0.026(2) 0.034(3) 0.0036(18) 0.0049(18) 0.0208(17) N3 0.029(2) 0.030(2) 0.038(3) 0.0049(18) 0.0040(18) 0.0199(17) C1 0.045(3) 0.026(3) 0.038(4) 0.007(3) 0.009(3) 0.030(3) C2 0.032(3) 0.027(3) 0.039(4) 0.001(3) 0.005(3) 0.026(3) C3 0.031(2) 0.027(2) 0.037(2) 0.0023(18) 0.0062(18) 0.0189(18) C4 0.032(3) 0.029(3) 0.039(3) 0.004(3) 0.003(3) 0.025(3) C5 0.030(2) 0.030(2) 0.034(3) 0.0060(18) 0.0058(18) 0.0193(18) C6 0.039(3) 0.031(3) 0.044(4) 0.008(3) 0.011(3) 0.025(3) C7 0.050(4) 0.039(4) 0.056(4) 0.005(3) 0.008(3) 0.028(3) C8 0.067(5) 0.046(5) 0.061(5) 0.017(4) 0.008(4) 0.033(4) C9 0.098(7) 0.056(7) 0.080(8) 0.029(6) 0.017(7) 0.039(6) C10 0.082(8) 0.064(8) 0.097(7) 0.033(6) 0.005(6) 0.031(7) C11 0.047(4) 0.032(4) 0.048(5) 0.004(4) 0.010(4) 0.032(4) C12 0.066(4) 0.039(4) 0.036(4) 0.012(4) 0.013(4) 0.034(4) C13 0.115(8) 0.112(8) 0.056(7) -0.011(7) -0.019(7) 0.053(7) C14 0.090(7) 0.097(8) 0.084(7) 0.005(6) 0.028(6) 0.072(6) C15 0.057(4) 0.037(4) 0.050(4) 0.004(4) -0.012(4) 0.036(4) C16 0.061(5) 0.054(5) 0.085(5) 0.013(5) 0.006(5) 0.032(5) C17 0.141(10) 0.061(8) 0.128(9) 0.008(8) 0.018(8) 0.014(8) C18 0.144(11) 0.136(12) 0.102(8) 0.008(9) 0.007(8) 0.045(10) O21 0.050(4) 0.032(4) 0.068(4) 0.013(3) 0.010(3) 0.035(3) O22 0.046(3) 0.043(3) 0.057(4) 0.016(3) 0.012(3) 0.030(3) O23 0.054(3) 0.049(3) 0.062(4) 0.020(3) 0.010(3) 0.037(3) O24 0.060(4) 0.050(3) 0.081(4) 0.018(3) 0.013(3) 0.038(3) N21 0.046(3) 0.038(3) 0.053(3) 0.012(2) 0.005(2) 0.026(2) N22 0.028(2) 0.029(2) 0.037(2) 0.0039(18) 0.0030(18) 0.0237(17) N23 0.030(2) 0.025(2) 0.034(2) 0.0083(18) 0.0064(18) 0.0233(17) C21 0.037(3) 0.036(3) 0.054(4) 0.013(3) 0.003(3) 0.029(3) C22 0.036(3) 0.032(3) 0.048(4) 0.008(3) 0.006(3) 0.028(3) C23 0.034(2) 0.032(2) 0.037(3) 0.0096(18) 0.0046(18) 0.0208(18) C24 0.032(2) 0.030(2) 0.035(3) 0.0085(18) 0.0076(18) 0.0184(18) C26 0.043(4) 0.042(4) 0.065(4) 0.007(3) 0.012(3) 0.034(3) C27 0.052(4) 0.046(4) 0.062(4) 0.015(3) 0.010(3) 0.032(3) C28 0.060(5) 0.057(5) 0.084(5) 0.010(4) 0.014(4) 0.039(4) C29 0.102(10) 0.095(10) 0.114(8) 0.002(7) 0.004(7) 0.035(8) C30 0.099(9) 0.062(7) 0.107(9) 0.008(7) 0.020(7) 0.049(7) C31 0.050(4) 0.055(5) 0.056(5) 0.005(4) 0.006(4) 0.033(4) C32 0.062(5) 0.060(5) 0.071(5) 0.025(4) 0.015(4) 0.038(4) C33 0.095(8) 0.115(9) 0.091(7) 0.036(7) 0.025(6) 0.049(7) C34 0.077(4) 0.075(4) 0.079(4) 0.020(2) 0.016(2) 0.026(2) C25 0.048(3) 0.038(3) 0.061(3) 0.010(3) 0.007(3) 0.031(3) C35 0.073(5) 0.068(5) 0.087(5) 0.020(4) 0.010(4) 0.037(4) C36 0.081(5) 0.105(6) 0.103(5) 0.036(5) 0.041(5) 0.052(5) C37 0.124(9) 0.107(8) 0.154(9) 0.031(8) 0.047(7) 0.064(7) C38 0.093(10) 0.210(15) 0.142(10) -0.014(11) 0.022(8) 0.079(10) N1P 0.099(7) 0.077(6) 0.156(8) 0.040(6) 0.042(6) 0.076(5) C1P 0.093(9) 0.121(10) 0.227(15) 0.059(12) 0.066(11) 0.086(8) C2P 0.137(13) 0.112(11) 0.187(15) 0.010(11) 0.068(11) 0.087(10) C3P 0.158(14) 0.133(12) 0.134(11) 0.004(9) 0.028(9) 0.107(11) C4P 0.32(3) 0.223(19) 0.171(16) 0.089(16) 0.126(19) 0.195(18) C5P 0.149(12) 0.135(12) 0.126(11) 0.039(9) 0.031(9) 0.050(10) C6P 0.222(18) 0.33(3) 0.214(18) 0.151(19) 0.082(14) 0.098(17) N21P 0.076(5) 0.118(7) 0.190(9) 0.092(7) 0.051(5) 0.075(5) C21P 0.098(8) 0.084(7) 0.138(9) 0.021(6) 0.003(7) 0.051(6) C22P 0.081(7) 0.143(11) 0.148(10) 0.047(8) 0.008(7) 0.069(7) C23P 0.217(16) 0.165(13) 0.123(11) 0.002(9) -0.027(10) 0.128(12) C24P 0.175(16) 0.177(16) 0.231(19) -0.009(13) -0.014(13) 0.079(14) C25P 0.231(18) 0.068(8) 0.246(17) 0.050(10) 0.121(15) 0.097(10) C26P 0.139(11) 0.202(15) 0.293(18) 0.105(14) 0.039(11) 0.150(11) _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 O1 C2 1.210(8) . ? O2 C4 1.229(8) . ? O3 C6 1.211(8) . ? O4 C6 1.258(8) . ? N1 C1 1.484(9) . ? N2 C2 1.305(9) . ? N2 C3 1.486(9) . ? N3 C4 1.373(8) . ? N3 C5 1.446(9) . ? C1 C7 1.511(10) . ? C1 C2 1.517(9) . ? C3 C4 1.474(9) . ? C3 C11 1.552(10) . ? C5 C15 1.516(10) . ? C5 C6 1.516(12) . ? C7 C8 1.523(10) . ? C8 C9 1.520(11) . ? C8 C10 1.537(11) . ? C11 C12 1.564(10) . ? C12 C14 1.509(10) . ? C12 C13 1.519(11) . ? C15 C16 1.519(11) . ? C16 C17 1.456(12) . ? C16 C18 1.553(11) . ? O1A C2A 1.236(15) . ? O2A C4A 1.218(14) . ? O3A C6A 1.207(15) . ? O4A C6A 1.224(14) . ? N1A C1A 1.507(16) . ? N2A C2A 1.349(15) . ? N2A C3A 1.452(15) . ? N3A C4A 1.349(15) . ? N3A C5A 1.463(15) . ? C1A C2A 1.527(15) . ? C1A C7A 1.542(15) . ? C3A C4A 1.507(14) . ? C3A C11A 1.520(15) . ? C5A C15A 1.518(14) . ? C5A C6A 1.63(3) . ? C7A C8A 1.531(15) . ? C8A C10A 1.531(15) . ? C8A C9A 1.534(15) . ? C11A C12A 1.510(15) . ? C12A C13A 1.512(15) . ? C12A C14A 1.524(15) . ? C15A C16A 1.481(15) . ? C16A C17A 1.489(15) . ? C16A C18A 1.522(15) . ? O21 C22 1.249(8) . ? O22 C24 1.232(8) . ? O23 C26 1.232(9) . ? O24 C26 1.241(9) . ? N21 C21 1.480(10) . ? N22 C22 1.312(9) . ? N22 C23 1.480(9) . ? N23 C24 1.373(9) . ? N23 C25 1.466(9) . ? C21 C27 1.523(10) . ? C21 C22 1.528(9) . ? C23 C24 1.463(10) . ? C23 C31 1.467(10) . ? C26 C25 1.569(12) . ? C27 C28 1.544(11) . ? C28 C29 1.488(11) . ? C28 C30 1.566(11) . ? C31 C32 1.490(10) . ? C32 C33 1.475(11) . ? C32 C34 1.514(10) . ? C25 C35 1.560(11) . ? C35 C36 1.485(11) . ? C36 C38 1.492(12) . ? C36 C37 1.521(12) . ? C25A N23A 1.414(16) . ? C25A C35A 1.487(14) . ? C25A C26A 1.49(4) . ? C35A C36A 1.508(15) . ? C36A C38A 1.509(15) . ? C36A C37A 1.559(15) . ? O21A C22A 1.228(15) . ? O22A C24A 1.175(14) . ? O23A C26A 1.223(14) . ? O24A C26A 1.246(14) . ? N21A C21A 1.481(16) . ? N22A C22A 1.333(15) . ? N22A C23A 1.480(15) . ? N23A C24A 1.339(15) . ? C21A C27A 1.512(15) . ? C21A C22A 1.513(15) . ? C23A C24A 1.495(15) . ? C23A C31A 1.530(15) . ? C27A C28A 1.518(15) . ? C28A C29A 1.497(15) . ? C28A C30A 1.532(15) . ? C31A C32A 1.537(15) . ? C32A C34A 1.534(15) . ? C32A C33A 1.535(15) . ? N1P C1P 1.3900 . ? N1P C5P 1.3900 . ? C1P C2P 1.3900 . ? C2P C3P 1.3900 . ? C2P C6P 1.528(13) . ? C3P C4P 1.3900 . ? C4P C5P 1.3900 . ? N21P C21P 1.3900 . ? N21P C25P 1.3900 . ? C21P C22P 1.3900 . ? C22P C23P 1.3900 . ? C22P C26P 1.522(10) . ? C23P C24P 1.3900 . ? C24P C25P 1.3900 . ? 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 C2 N2 C3 123.3(7) . . ? C4 N3 C5 123.3(7) . . ? N1 C1 C7 105.1(7) . . ? N1 C1 C2 110.2(7) . . ? C7 C1 C2 109.5(7) . . ? O1 C2 N2 124.2(7) . . ? O1 C2 C1 120.7(8) . . ? N2 C2 C1 115.0(7) . . ? C4 C3 N2 106.9(6) . . ? C4 C3 C11 109.4(7) . . ? N2 C3 C11 109.0(6) . . ? O2 C4 N3 120.9(8) . . ? O2 C4 C3 123.2(7) . . ? N3 C4 C3 115.8(7) . . ? N3 C5 C15 114.3(7) . . ? N3 C5 C6 108.0(6) . . ? C15 C5 C6 113.6(6) . . ? O3 C6 O4 123.9(8) . . ? O3 C6 C5 120.5(8) . . ? O4 C6 C5 115.6(7) . . ? C1 C7 C8 111.7(7) . . ? C9 C8 C7 112.7(9) . . ? C9 C8 C10 111.3(10) . . ? C7 C8 C10 104.8(8) . . ? C3 C11 C12 115.6(7) . . ? C14 C12 C13 106.6(8) . . ? C14 C12 C11 112.0(8) . . ? C13 C12 C11 109.5(8) . . ? C5 C15 C16 114.7(8) . . ? C17 C16 C15 111.8(10) . . ? C17 C16 C18 105.4(10) . . ? C15 C16 C18 110.6(10) . . ? C2A N2A C3A 121.1(18) . . ? C4A N3A C5A 122.1(19) . . ? N1A C1A C2A 107.0(18) . . ? N1A C1A C7A 114.8(18) . . ? C2A C1A C7A 109(2) . . ? O1A C2A N2A 127(2) . . ? O1A C2A C1A 121.7(19) . . ? N2A C2A C1A 110.8(16) . . ? N2A C3A C4A 108.7(17) . . ? N2A C3A C11A 111.7(19) . . ? C4A C3A C11A 107(2) . . ? O2A C4A N3A 120.5(19) . . ? O2A C4A C3A 120.9(19) . . ? N3A C4A C3A 118.5(17) . . ? N3A C5A C15A 114.0(15) . . ? N3A C5A C6A 110.7(16) . . ? C15A C5A C6A 111(2) . . ? O3A C6A O4A 138(3) . . ? O3A C6A C5A 110.7(18) . . ? O4A C6A C5A 111.4(18) . . ? C8A C7A C1A 122(2) . . ? C7A C8A C10A 116(3) . . ? C7A C8A C9A 105(3) . . ? C10A C8A C9A 102(3) . . ? C12A C11A C3A 127(2) . . ? C11A C12A C13A 97(2) . . ? C11A C12A C14A 120(3) . . ? C13A C12A C14A 105.0(15) . . ? C16A C15A C5A 132(2) . . ? C15A C16A C17A 121(2) . . ? C15A C16A C18A 128(2) . . ? C17A C16A C18A 108.1(14) . . ? C22 N22 C23 121.6(7) . . ? C24 N23 C25 120.7(7) . . ? N21 C21 C27 110.8(8) . . ? N21 C21 C22 106.7(6) . . ? C27 C21 C22 113.6(7) . . ? O21 C22 N22 125.4(8) . . ? O21 C22 C21 118.5(8) . . ? N22 C22 C21 116.1(7) . . ? C24 C23 C31 111.5(8) . . ? C24 C23 N22 107.9(6) . . ? C31 C23 N22 106.9(7) . . ? O22 C24 N23 120.2(7) . . ? O22 C24 C23 123.0(7) . . ? N23 C24 C23 116.7(7) . . ? O23 C26 O24 128.5(9) . . ? O23 C26 C25 117.1(8) . . ? O24 C26 C25 114.3(8) . . ? C21 C27 C28 116.2(9) . . ? C29 C28 C27 110.0(10) . . ? C29 C28 C30 111.7(12) . . ? C27 C28 C30 109.9(9) . . ? C23 C31 C32 117.1(8) . . ? C33 C32 C31 109.6(9) . . ? C33 C32 C34 111.6(8) . . ? C31 C32 C34 114.5(8) . . ? N23 C25 C35 116.8(8) . . ? N23 C25 C26 107.8(7) . . ? C35 C25 C26 110.6(7) . . ? C36 C35 C25 120.3(10) . . ? C35 C36 C38 112.9(11) . . ? C35 C36 C37 114.5(11) . . ? C38 C36 C37 105.9(10) . . ? N23A C25A C35A 88.4(19) . . ? N23A C25A C26A 113(2) . . ? C35A C25A C26A 97(2) . . ? C25A C35A C36A 148(3) . . ? C35A C36A C38A 113(2) . . ? C35A C36A C37A 109(2) . . ? C38A C36A C37A 104.6(14) . . ? C22A N22A C23A 121.9(18) . . ? C24A N23A C25A 122(2) . . ? N21A C21A C27A 108.4(18) . . ? N21A C21A C22A 108.9(18) . . ? C27A C21A C22A 112(2) . . ? O21A C22A N22A 126(2) . . ? O21A C22A C21A 122(2) . . ? N22A C22A C21A 111.8(17) . . ? N22A C23A C24A 103.7(14) . . ? N22A C23A C31A 114.5(19) . . ? C24A C23A C31A 107.6(17) . . ? O22A C24A N23A 126.7(19) . . ? O22A C24A C23A 119.6(17) . . ? N23A C24A C23A 113.4(16) . . ? O23A C26A O24A 121(2) . . ? O23A C26A C25A 122(2) . . ? O24A C26A C25A 116.6(19) . . ? C21A C27A C28A 108(2) . . ? C29A C28A C27A 104(2) . . ? C29A C28A C30A 100(3) . . ? C27A C28A C30A 116(3) . . ? C23A C31A C32A 126.9(19) . . ? C34A C32A C33A 98(2) . . ? C34A C32A C31A 97(2) . . ? C33A C32A C31A 118(2) . . ? C1P N1P C5P 120.0 . . ? N1P C1P C2P 120.0 . . ? C3P C2P C1P 120.0 . . ? C3P C2P C6P 120.5(8) . . ? C1P C2P C6P 119.5(8) . . ? C2P C3P C4P 120.0 . . ? C5P C4P C3P 120.0 . . ? C4P C5P N1P 120.0 . . ? C21P N21P C25P 120.0 . . ? N21P C21P C22P 120.0 . . ? C21P C22P C23P 120.0 . . ? C21P C22P C26P 119.4(6) . . ? C23P C22P C26P 120.5(6) . . ? C24P C23P C22P 120.0 . . ? C23P C24P C25P 120.0 . . ? C24P C25P N21P 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 132.1(8) . . . . ? N2 C3 C4 N3 125.8(7) . . . . ? N3 C5 C6 O3 9.9(12) . . . . ? N3 C5 C6 O4 -169.5(8) . . . . ? C2 N2 C3 C4 -135.2(8) . . . . ? C4 N3 C5 C6 -157.6(7) . . . . ? C1 C2 N2 C3 176.3(6) . . . . ? C3 C4 N3 C5 175.4(7) . . . . ? N1A C1A C2A N2A 129(2) . . . . ? N2A C3A C4A N3A 126(2) . . . . ? N3A C5A C6A O3A 10(3) . . . . ? N3A C5A C6A O4A -170(2) . . . . ? C2A N2A C3A C4A -128(2) . . . . ? C4A N3A C5A C6A -156(2) . . . . ? C1A C2A N2A C3A 173.8(18) . . . . ? C3A C4A N3A C5A 171.3(19) . . . . ? N21 C21 C22 N22 127.5(8) . . . . ? N22 C23 C24 N23 133.0(7) . . . . ? N23 C25 C26 O23 -14.3(12) . . . . ? N23 C25 C26 O24 162.2(9) . . . . ? C22 N22 C23 C24 -133.2(8) . . . . ? C24 N23 C25 C26 -148.3(8) . . . . ? C21 C22 N22 C23 175.7(7) . . . . ? C23 C24 N23 C25 167.8(7) . . . . ? N21A C21A C22A N22A 134(2) . . . . ? N22A C23A C24A N23A 128.0(19) . . . . ? N23A C25A C26A O23A -21(3) . . . . ? N23A C25A C26A O24A 154.2(19) . . . . ? C22A N22A C23A C24A -132(2) . . . . ? C24A N23A C25A C26A -147(2) . . . . ? C21A C22A N22A C23A 178.8(17) . . . . ? C23A C24A N23A C25A 166.4(19) . . . . ? 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 N1 H1C O23 0.91 1.89 2.762(10) 161.1 . N3 H3A O21 0.88 2.13 2.981(10) 161.2 . N1A H1A2 O23A 0.91 2.06 2.89(3) 152.1 . N3A H3AA O21A 0.88 2.32 3.15(3) 157.7 . N21 H21C N1P 0.91 1.90 2.739(12) 152.7 . N21 H21B O3 0.91 1.83 2.715(10) 164.6 . N23 H23A O1 0.88 2.10 2.946(9) 162.2 . N21A H21D N1P 0.91 2.42 3.31(2) 167.0 . N21A H21F O3A 0.91 2.29 3.06(2) 141.7 . N23A H23D O1A 0.88 2.51 3.30(3) 149.4 . N1 H1A N21P 0.91 2.14 3.045(11) 173.5 1_656 N1A H1A3 N21P 0.91 1.66 2.55(2) 166.1 1_656 N1 H1B O4 0.91 1.81 2.661(10) 155.2 1_545 N1 H1B O3 0.91 2.53 3.125(10) 123.7 1_545 N1A H1A1 O4A 0.91 1.82 2.67(3) 153.3 1_545 N1A H1A1 O3A 0.91 2.55 3.17(3) 125.3 1_545 N2 H2A O22 0.88 2.10 2.903(9) 152.1 1_655 N2A H2AA O22A 0.88 2.18 3.01(2) 156.8 1_655 N21 H21A O24 0.91 1.99 2.740(10) 139.1 1_565 N21 H21A O23 0.91 2.31 3.100(9) 145.3 1_565 N21A H21E O24A 0.91 1.87 2.76(3) 162.6 1_565 N21A H21E O23A 0.91 2.43 3.16(2) 137.9 1_565 N22 H22A O2 0.88 2.07 2.921(9) 163.2 1_455 N22A H22B O2A 0.88 2.12 2.87(3) 142.8 1_455 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 21.96 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.575 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.102 _chemical_name_common 'L-leucyl-L-leucyl-L-leucine - 3-methylpyridine clathrate (1:1)' #===END data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 642090' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_sum 'C24 H42.28 N4 O4.14' _chemical_formula_weight 453.22 _chemical_absolute_configuration rm 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 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 9.5358(6) _cell_length_b 23.6420(17) _cell_length_c 12.0899(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.904(3) _cell_angle_gamma 90.00 _cell_volume 2692.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9888 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 26.74 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9627 _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62643 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11005 _reflns_number_gt 8581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0555P)^2^+0.5986P] 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 0.0055(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details rm _refine_ls_number_reflns 11005 _refine_ls_number_parameters 982 _refine_ls_number_restraints 1031 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.004 _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 N1 N 0.6909(4) 0.81261(15) 1.3528(3) 0.0197(6) Uani 0.543(3) 1 d PDU A 1 H1A H 0.6671 0.8324 1.4117 0.030 Uiso 0.543(3) 1 calc PR A 1 H1B H 0.7871 0.8103 1.3593 0.030 Uiso 0.543(3) 1 calc PR A 1 H1C H 0.6537 0.7772 1.3524 0.030 Uiso 0.543(3) 1 calc PR A 1 N2 N 0.5718(7) 0.7982(2) 1.0664(6) 0.0167(6) Uani 0.543(3) 1 d PDU A 1 H2B H 0.4832 0.8074 1.0699 0.020 Uiso 0.543(3) 1 calc PR A 1 N3 N 0.5914(5) 0.83079(16) 0.7868(4) 0.0169(6) Uani 0.543(3) 1 d PDU A 1 H3A H 0.6839 0.8259 0.7947 0.020 Uiso 0.543(3) 1 calc PR A 1 O1 O 0.808(4) 0.7915(15) 1.1431(16) 0.0246(17) Uani 0.543(3) 1 d PDU A 1 O2 O 0.3969(9) 0.8123(2) 0.8753(8) 0.0305(16) Uani 0.543(3) 1 d PU A 1 O3 O 0.7196(8) 0.8251(3) 0.6053(7) 0.0370(16) Uani 0.543(3) 1 d PU A 1 O4 O 0.5251(6) 0.8520(2) 0.4968(5) 0.0358(14) Uani 0.543(3) 1 d PU A 1 C1 C 0.6344(6) 0.84152(18) 1.2481(4) 0.0173(6) Uani 0.543(3) 1 d PDU A 1 H1AA H 0.5286 0.8440 1.2402 0.021 Uiso 0.543(3) 1 calc PR A 1 C2 C 0.6767(8) 0.8074(3) 1.1511(6) 0.0176(7) Uani 0.543(3) 1 d PDU A 1 C3 C 0.6143(18) 0.7716(6) 0.9665(7) 0.0190(12) Uani 0.543(3) 1 d PDU A 1 H3B H 0.7184 0.7748 0.9644 0.023 Uiso 0.543(3) 1 calc PR A 1 C4 C 0.5242(5) 0.80236(18) 0.8697(4) 0.0163(6) Uani 0.543(3) 1 d PDU A 1 C5 C 0.5341(5) 0.86630(18) 0.6920(3) 0.0262(11) Uani 0.543(3) 1 d PDU A 1 H5A H 0.4285 0.8623 0.6766 0.031 Uiso 0.543(3) 1 calc PR A 1 C6 C 0.5986(6) 0.8458(2) 0.5895(5) 0.0252(13) Uani 0.543(3) 1 d PDU A 1 C7 C 0.6980(11) 0.9008(3) 1.2497(6) 0.0260(12) Uani 0.543(3) 1 d PDU A 1 H7B H 0.8028 0.8975 1.2636 0.031 Uiso 0.543(3) 1 calc PR A 1 H7C H 0.6694 0.9220 1.3133 0.031 Uiso 0.543(3) 1 calc PR A 1 C8 C 0.6549(7) 0.9356(2) 1.1421(5) 0.0367(10) Uani 0.543(3) 1 d PDU A 1 H8D H 0.5526 0.9286 1.1123 0.044 Uiso 0.543(3) 1 calc PR A 1 C9 C 0.7456(6) 0.9225(3) 1.0506(5) 0.0452(13) Uani 0.543(3) 1 d PDU A 1 H9A H 0.7124 0.9454 0.9841 0.068 Uiso 0.543(3) 1 calc PR A 1 H9B H 0.7371 0.8823 1.0311 0.068 Uiso 0.543(3) 1 calc PR A 1 H9C H 0.8451 0.9316 1.0784 0.068 Uiso 0.543(3) 1 calc PR A 1 C10 C 0.6758(8) 0.9982(2) 1.1767(6) 0.0542(13) Uani 0.543(3) 1 d PDU A 1 H10A H 0.6510 1.0223 1.1107 0.081 Uiso 0.543(3) 1 calc PR A 1 H10B H 0.7752 1.0046 1.2092 0.081 Uiso 0.543(3) 1 calc PR A 1 H10C H 0.6145 1.0074 1.2322 0.081 Uiso 0.543(3) 1 calc PR A 1 C11 C 0.554(4) 0.7125(7) 0.931(3) 0.0409(14) Uani 0.543(3) 1 d PDU A 1 H11A H 0.4523 0.7104 0.9383 0.049 Uiso 0.543(3) 1 calc PR A 1 H11C H 0.5644 0.7047 0.8523 0.049 Uiso 0.543(3) 1 calc PR A 1 C12 C 0.6401(12) 0.6695(5) 1.0096(14) 0.0594(17) Uani 0.543(3) 1 d PDU A 1 H12B H 0.6219 0.6819 1.0852 0.071 Uiso 0.543(3) 1 calc PR A 1 C13 C 0.5456(12) 0.6161(4) 0.9873(10) 0.075(3) Uani 0.543(3) 1 d PDU A 1 H13A H 0.4454 0.6272 0.9756 0.113 Uiso 0.543(3) 1 calc PR A 1 H13B H 0.5643 0.5906 1.0518 0.113 Uiso 0.543(3) 1 calc PR A 1 H13C H 0.5673 0.5966 0.9204 0.113 Uiso 0.543(3) 1 calc PR A 1 C14 C 0.8028(11) 0.6625(5) 1.0271(7) 0.069(2) Uani 0.543(3) 1 d PDU A 1 H14B H 0.8303 0.6310 1.0785 0.103 Uiso 0.543(3) 1 calc PR A 1 H14C H 0.8478 0.6974 1.0588 0.103 Uiso 0.543(3) 1 calc PR A 1 H14D H 0.8338 0.6547 0.9550 0.103 Uiso 0.543(3) 1 calc PR A 1 C15 C 0.5738(6) 0.92871(16) 0.7214(4) 0.0276(12) Uani 0.543(3) 1 d PDU A 1 H15A H 0.5274 0.9397 0.7859 0.033 Uiso 0.543(3) 1 calc PR A 1 H15B H 0.6776 0.9305 0.7464 0.033 Uiso 0.543(3) 1 calc PR A 1 C16 C 0.5359(4) 0.97296(15) 0.6298(3) 0.0338(9) Uani 0.543(3) 1 d PDU A 1 H16A H 0.5937 0.9655 0.5690 0.041 Uiso 0.543(3) 1 calc PR A 1 C17 C 0.3791(4) 0.9710(2) 0.5792(4) 0.0408(11) Uani 0.543(3) 1 d PDU A 1 H17A H 0.3561 0.9337 0.5461 0.061 Uiso 0.543(3) 1 calc PR A 1 H17B H 0.3595 1.0001 0.5210 0.061 Uiso 0.543(3) 1 calc PR A 1 H17C H 0.3210 0.9781 0.6379 0.061 Uiso 0.543(3) 1 calc PR A 1 C18 C 0.5776(5) 1.03097(18) 0.6812(4) 0.0494(12) Uani 0.543(3) 1 d PDU A 1 H18A H 0.5536 1.0604 0.6243 0.074 Uiso 0.543(3) 1 calc PR A 1 H18B H 0.6799 1.0317 0.7082 0.074 Uiso 0.543(3) 1 calc PR A 1 H18C H 0.5259 1.0379 0.7439 0.074 Uiso 0.543(3) 1 calc PR A 1 N1A N 0.7113(5) 0.79375(19) 1.3558(4) 0.0197(6) Uani 0.457(3) 1 d PDU A 2 H1A1 H 0.6868 0.8087 1.4195 0.030 Uiso 0.457(3) 1 calc PR A 2 H1A2 H 0.8071 0.7956 1.3590 0.030 Uiso 0.457(3) 1 calc PR A 2 H1A3 H 0.6828 0.7570 1.3492 0.030 Uiso 0.457(3) 1 calc PR A 2 N2A N 0.5800(9) 0.7871(3) 1.0697(7) 0.0167(6) Uani 0.457(3) 1 d PDU A 2 H2XY H 0.4939 0.7864 1.0873 0.020 Uiso 0.457(3) 1 calc PR A 2 N3A N 0.5846(6) 0.8149(2) 0.7820(5) 0.0169(6) Uani 0.457(3) 1 d PDU A 2 H3ZZ H 0.6701 0.8003 0.7852 0.020 Uiso 0.457(3) 1 calc PR A 2 O1A O 0.802(4) 0.7894(19) 1.162(2) 0.0246(17) Uani 0.457(3) 1 d PU A 2 O2A O 0.3986(9) 0.8350(3) 0.8732(8) 0.0243(16) Uani 0.457(3) 1 d PU A 2 O3A O 0.7062(11) 0.8016(3) 0.6057(9) 0.0365(19) Uani 0.457(3) 1 d PU A 2 O4A O 0.5132(8) 0.8280(3) 0.4842(6) 0.0363(17) Uani 0.457(3) 1 d PU A 2 C1A C 0.6403(7) 0.8267(2) 1.2563(5) 0.0173(6) Uani 0.457(3) 1 d PDU A 2 H1ZZ H 0.5348 0.8239 1.2514 0.021 Uiso 0.457(3) 1 calc PR A 2 C2A C 0.6864(10) 0.7992(4) 1.1531(7) 0.0176(7) Uani 0.457(3) 1 d PDU A 2 C3A C 0.592(2) 0.7748(7) 0.9513(9) 0.0190(12) Uani 0.457(3) 1 d PDU A 2 H3ZQ H 0.6954 0.7791 0.9468 0.023 Uiso 0.457(3) 1 calc PR A 2 C4A C 0.5179(7) 0.8189(2) 0.8692(5) 0.0163(6) Uani 0.457(3) 1 d PDU A 2 C5A C 0.5015(5) 0.83736(19) 0.6789(4) 0.0194(11) Uani 0.457(3) 1 d PDU A 2 H5ZZ H 0.4091 0.8166 0.6672 0.023 Uiso 0.457(3) 1 calc PR A 2 C6A C 0.5808(8) 0.8204(3) 0.5819(6) 0.0292(17) Uani 0.457(3) 1 d PDU A 2 C7A C 0.6862(13) 0.8888(3) 1.2719(8) 0.0260(12) Uani 0.457(3) 1 d PDU A 2 H7X H 0.7908 0.8899 1.2772 0.031 Uiso 0.457(3) 1 calc PR A 2 H7Y H 0.6635 0.9014 1.3452 0.031 Uiso 0.457(3) 1 calc PR A 2 C8A C 0.6248(9) 0.9333(3) 1.1841(6) 0.0367(10) Uani 0.457(3) 1 d PDU A 2 H8E H 0.5197 0.9277 1.1666 0.044 Uiso 0.457(3) 1 calc PR A 2 C9A C 0.6870(9) 0.9285(3) 1.0745(6) 0.0452(13) Uani 0.457(3) 1 d PDU A 2 H9D H 0.6731 0.8899 1.0451 0.068 Uiso 0.457(3) 1 calc PR A 2 H9E H 0.7887 0.9371 1.0890 0.068 Uiso 0.457(3) 1 calc PR A 2 H9F H 0.6389 0.9553 1.0195 0.068 Uiso 0.457(3) 1 calc PR A 2 C10A C 0.6537(10) 0.9934(3) 1.2320(7) 0.0542(13) Uani 0.457(3) 1 d PDU A 2 H10D H 0.6148 1.0214 1.1756 0.081 Uiso 0.457(3) 1 calc PR A 2 H10E H 0.7562 0.9992 1.2520 0.081 Uiso 0.457(3) 1 calc PR A 2 H10F H 0.6082 0.9979 1.2988 0.081 Uiso 0.457(3) 1 calc PR A 2 C11A C 0.565(5) 0.7104(8) 0.944(4) 0.0409(14) Uani 0.457(3) 1 d PDU A 2 H11D H 0.4618 0.7053 0.9447 0.049 Uiso 0.457(3) 1 calc PR A 2 H11E H 0.5825 0.6985 0.8691 0.049 Uiso 0.457(3) 1 calc PR A 2 C12A C 0.6401(15) 0.6666(6) 1.0271(17) 0.0594(17) Uani 0.457(3) 1 d PDU A 2 H12C H 0.6557 0.6802 1.1064 0.071 Uiso 0.457(3) 1 calc PR A 2 C13A C 0.5902(9) 0.6043(5) 1.0148(9) 0.038(2) Uani 0.457(3) 1 d PDU A 2 H13D H 0.6453 0.5814 1.0737 0.058 Uiso 0.457(3) 1 calc PR A 2 H13E H 0.6046 0.5899 0.9413 0.058 Uiso 0.457(3) 1 calc PR A 2 H13F H 0.4893 0.6021 1.0214 0.058 Uiso 0.457(3) 1 calc PR A 2 C14A C 0.7774(15) 0.6643(6) 0.9750(9) 0.069(2) Uani 0.457(3) 1 d PDU A 2 H14E H 0.8468 0.6399 1.0205 0.103 Uiso 0.457(3) 1 calc PR A 2 H14F H 0.8166 0.7025 0.9724 0.103 Uiso 0.457(3) 1 calc PR A 2 H14G H 0.7563 0.6490 0.8989 0.103 Uiso 0.457(3) 1 calc PR A 2 C15A C 0.4660(4) 0.90081(16) 0.6831(3) 0.0206(9) Uani 0.457(3) 1 d PDU A 2 H15X H 0.4061 0.9111 0.6115 0.025 Uiso 0.457(3) 1 calc PR A 2 H15Y H 0.4080 0.9066 0.7433 0.025 Uiso 0.457(3) 1 calc PR A 2 C16A C 0.5915(7) 0.9422(2) 0.7027(6) 0.0338(9) Uani 0.457(3) 1 d PDU A 2 H16J H 0.6628 0.9266 0.7645 0.041 Uiso 0.457(3) 1 calc PR A 2 C17A C 0.6657(5) 0.9500(2) 0.6002(4) 0.0339(12) Uani 0.457(3) 1 d PDU A 2 H17X H 0.7449 0.9765 0.6183 0.051 Uiso 0.457(3) 1 calc PR A 2 H17Y H 0.5979 0.9650 0.5379 0.051 Uiso 0.457(3) 1 calc PR A 2 H17Z H 0.7017 0.9134 0.5787 0.051 Uiso 0.457(3) 1 calc PR A 2 C18A C 0.5406(6) 0.9990(2) 0.7421(6) 0.0499(16) Uani 0.457(3) 1 d PDU A 2 H18D H 0.6211 1.0252 0.7569 0.075 Uiso 0.457(3) 1 calc PR A 2 H18E H 0.4997 0.9935 0.8109 0.075 Uiso 0.457(3) 1 calc PR A 2 H18F H 0.4684 1.0149 0.6839 0.075 Uiso 0.457(3) 1 calc PR A 2 N21 N 0.004(2) 0.8364(6) -0.3340(17) 0.0148(17) Uani 0.506(3) 1 d PU B 3 H21A H 0.0292 0.8608 -0.3857 0.022 Uiso 0.506(3) 1 calc PR B 3 H21B H -0.0922 0.8363 -0.3384 0.022 Uiso 0.506(3) 1 calc PR B 3 H21C H 0.0345 0.8010 -0.3476 0.022 Uiso 0.506(3) 1 calc PR B 3 N22 N 0.132(2) 0.8101(13) -0.0473(13) 0.023(2) Uani 0.506(3) 1 d PDU B 3 H22U H 0.2182 0.8201 -0.0580 0.028 Uiso 0.506(3) 1 calc PR B 3 N23 N 0.098(2) 0.8423(15) 0.223(2) 0.0265(6) Uani 0.506(3) 1 d PDU B 3 H23U H 0.0156 0.8249 0.2187 0.032 Uiso 0.506(3) 1 calc PR B 3 O21 O -0.094(3) 0.8018(9) -0.1390(16) 0.0193(16) Uani 0.506(3) 1 d PDU B 3 O22 O 0.312(2) 0.8464(10) 0.152(2) 0.022(2) Uani 0.506(3) 1 d PDU B 3 O23 O -0.0127(12) 0.8272(6) 0.4077(11) 0.0239(19) Uani 0.506(3) 1 d PDU B 3 O24 O 0.1060(17) 0.8920(8) 0.5065(11) 0.040(3) Uani 0.506(3) 1 d PDU B 3 C21 C 0.067(2) 0.8539(4) -0.2249(12) 0.0218(5) Uani 0.506(3) 1 d PDU B 3 H21D H 0.1727 0.8560 -0.2196 0.026 Uiso 0.506(3) 1 calc PR B 3 C22 C 0.0257(12) 0.8152(4) -0.1331(9) 0.0159(7) Uani 0.506(3) 1 d PDU B 3 C23 C 0.1145(8) 0.7893(2) 0.0599(5) 0.0164(6) Uani 0.506(3) 1 d PDU B 3 H23B H 0.0114 0.7852 0.0650 0.020 Uiso 0.506(3) 1 calc PR B 3 C24 C 0.1844(7) 0.8316(2) 0.1471(5) 0.0155(6) Uani 0.506(3) 1 d PDU B 3 C25 C 0.1418(9) 0.8832(3) 0.3130(7) 0.0203(6) Uani 0.506(3) 1 d PDU B 3 H25B H 0.2474 0.8809 0.3329 0.024 Uiso 0.506(3) 1 calc PR B 3 C26 C 0.0774(10) 0.8657(3) 0.4169(7) 0.0178(7) Uani 0.506(3) 1 d PDU B 3 C27 C 0.0023(6) 0.9138(3) -0.2302(5) 0.0253(7) Uani 0.506(3) 1 d PDU B 3 H27A H 0.0256 0.9334 -0.2974 0.030 Uiso 0.506(3) 1 calc PR B 3 H27B H -0.1023 0.9105 -0.2384 0.030 Uiso 0.506(3) 1 calc PR B 3 C28 C 0.0550(7) 0.9498(3) -0.1265(5) 0.0253(16) Uani 0.506(3) 1 d PDU B 3 H28A H 0.0346 0.9281 -0.0599 0.030 Uiso 0.506(3) 1 calc PR B 3 C29 C 0.2154(6) 0.9608(3) -0.1092(5) 0.0316(15) Uani 0.506(3) 1 d PDU B 3 H29A H 0.2660 0.9246 -0.1070 0.047 Uiso 0.506(3) 1 calc PR B 3 H29B H 0.2434 0.9810 -0.0384 0.047 Uiso 0.506(3) 1 calc PR B 3 H29C H 0.2391 0.9838 -0.1711 0.047 Uiso 0.506(3) 1 calc PR B 3 C30 C -0.0325(8) 1.0047(3) -0.1313(7) 0.0403(14) Uani 0.506(3) 1 d PDU B 3 H30A H -0.1338 0.9954 -0.1435 0.060 Uiso 0.506(3) 1 calc PR B 3 H30B H -0.0108 1.0284 -0.1930 0.060 Uiso 0.506(3) 1 calc PR B 3 H30C H -0.0085 1.0252 -0.0605 0.060 Uiso 0.506(3) 1 calc PR B 3 C31 C 0.188(2) 0.7313(4) 0.0695(11) 0.0212(12) Uani 0.506(3) 1 d PDU B 3 H31A H 0.2894 0.7364 0.0637 0.025 Uiso 0.506(3) 1 calc PR B 3 H31B H 0.1451 0.7074 0.0059 0.025 Uiso 0.506(3) 1 calc PR B 3 C32 C 0.1761(8) 0.7002(2) 0.1797(7) 0.0250(19) Uani 0.506(3) 1 d PDU B 3 H32A H 0.0802 0.7081 0.1999 0.030 Uiso 0.506(3) 1 calc PR B 3 C33 C 0.1895(6) 0.63636(18) 0.1643(4) 0.0433(13) Uani 0.506(3) 1 d PDU B 3 H33A H 0.1149 0.6234 0.1046 0.065 Uiso 0.506(3) 1 calc PR B 3 H33B H 0.1793 0.6170 0.2343 0.065 Uiso 0.506(3) 1 calc PR B 3 H33C H 0.2827 0.6277 0.1440 0.065 Uiso 0.506(3) 1 calc PR B 3 C34 C 0.2885(5) 0.7197(2) 0.2771(4) 0.0427(12) Uani 0.506(3) 1 d PDU B 3 H34A H 0.2755 0.6993 0.3453 0.064 Uiso 0.506(3) 1 calc PR B 3 H34B H 0.2781 0.7604 0.2889 0.064 Uiso 0.506(3) 1 calc PR B 3 H34C H 0.3834 0.7119 0.2593 0.064 Uiso 0.506(3) 1 calc PR B 3 C35 C 0.1017(8) 0.9459(2) 0.2989(5) 0.0249(15) Uani 0.506(3) 1 d PDU B 3 H35A H -0.0031 0.9490 0.2843 0.030 Uiso 0.506(3) 1 calc PR B 3 H35B H 0.1353 0.9658 0.3702 0.030 Uiso 0.506(3) 1 calc PR B 3 C36 C 0.1619(4) 0.97576(15) 0.2052(3) 0.0317(10) Uani 0.506(3) 1 d PDU B 3 H36A H 0.1369 0.9535 0.1345 0.038 Uiso 0.506(3) 1 calc PR B 3 C37 C 0.3232(4) 0.9807(2) 0.2325(4) 0.0428(12) Uani 0.506(3) 1 d PDU B 3 H37A H 0.3651 0.9428 0.2421 0.064 Uiso 0.506(3) 1 calc PR B 3 H37B H 0.3487 1.0023 0.3018 0.064 Uiso 0.506(3) 1 calc PR B 3 H37C H 0.3594 1.0002 0.1711 0.064 Uiso 0.506(3) 1 calc PR B 3 C38 C 0.0933(6) 1.03439(17) 0.1886(4) 0.0477(13) Uani 0.506(3) 1 d PDU B 3 H38A H -0.0099 1.0303 0.1698 0.072 Uiso 0.506(3) 1 calc PR B 3 H38B H 0.1298 1.0541 0.1277 0.072 Uiso 0.506(3) 1 calc PR B 3 H38C H 0.1162 1.0563 0.2579 0.072 Uiso 0.506(3) 1 calc PR B 3 N21A N 0.005(2) 0.8229(6) -0.3377(18) 0.0148(17) Uani 0.494(3) 1 d PU B 4 H21L H 0.0322 0.8398 -0.3985 0.022 Uiso 0.494(3) 1 calc PR B 4 H21E H -0.0915 0.8241 -0.3438 0.022 Uiso 0.494(3) 1 calc PR B 4 H21F H 0.0342 0.7863 -0.3340 0.022 Uiso 0.494(3) 1 calc PR B 4 N22A N 0.133(2) 0.8035(13) -0.0534(13) 0.023(2) Uani 0.494(3) 1 d PDU B 4 H22E H 0.2201 0.8063 -0.0686 0.028 Uiso 0.494(3) 1 calc PR B 4 N23A N 0.105(2) 0.8418(15) 0.219(2) 0.0265(6) Uani 0.494(3) 1 d PDU B 4 H23V H 0.0132 0.8361 0.2049 0.032 Uiso 0.494(3) 1 calc PR B 4 O21A O -0.104(3) 0.8120(10) -0.1239(16) 0.0193(16) Uani 0.494(3) 1 d PDU B 4 O22A O 0.300(3) 0.8347(10) 0.140(2) 0.022(2) Uani 0.494(3) 1 d PDU B 4 O23A O -0.0053(14) 0.8159(6) 0.3944(12) 0.030(3) Uani 0.494(3) 1 d PDU B 4 O24A O 0.1189(14) 0.8839(8) 0.5032(10) 0.027(2) Uani 0.494(3) 1 d PDU B 4 C21A C 0.072(2) 0.8547(4) -0.2295(13) 0.0218(5) Uani 0.494(3) 1 d PDU B 4 H21Q H 0.1780 0.8521 -0.2231 0.026 Uiso 0.494(3) 1 calc PR B 4 C22A C 0.0264(13) 0.8233(4) -0.1305(10) 0.0159(7) Uani 0.494(3) 1 d PDU B 4 C23A C 0.1133(8) 0.7772(2) 0.0562(5) 0.0164(6) Uani 0.494(3) 1 d PDU B 4 H23C H 0.0097 0.7737 0.0603 0.020 Uiso 0.494(3) 1 calc PR B 4 C24A C 0.1823(8) 0.8183(2) 0.1463(6) 0.0155(6) Uani 0.494(3) 1 d PDU B 4 C25A C 0.1571(9) 0.8751(3) 0.3172(7) 0.0203(6) Uani 0.494(3) 1 d PDU B 4 H25D H 0.2619 0.8701 0.3387 0.024 Uiso 0.494(3) 1 calc PR B 4 C26A C 0.0793(10) 0.8561(3) 0.4138(7) 0.0178(7) Uani 0.494(3) 1 d PDU B 4 C27A C 0.0324(6) 0.9165(3) -0.2097(5) 0.0253(7) Uani 0.494(3) 1 d PDU B 4 H27C H 0.0704 0.9402 -0.2658 0.030 Uiso 0.494(3) 1 calc PR B 4 H27D H -0.0723 0.9195 -0.2252 0.030 Uiso 0.494(3) 1 calc PR B 4 C28A C 0.0823(7) 0.9424(3) -0.0937(5) 0.0257(17) Uani 0.494(3) 1 d PDU B 4 H28B H 0.0472 0.9185 -0.0355 0.031 Uiso 0.494(3) 1 calc PR B 4 C29A C 0.2442(6) 0.9468(3) -0.0671(6) 0.0362(16) Uani 0.494(3) 1 d PDU B 4 H29D H 0.2711 0.9639 0.0070 0.054 Uiso 0.494(3) 1 calc PR B 4 H29E H 0.2792 0.9704 -0.1236 0.054 Uiso 0.494(3) 1 calc PR B 4 H29F H 0.2858 0.9090 -0.0676 0.054 Uiso 0.494(3) 1 calc PR B 4 C30A C 0.0156(8) 1.0017(3) -0.0931(7) 0.0403(14) Uani 0.494(3) 1 d PDU B 4 H30D H 0.0463 1.0197 -0.0204 0.060 Uiso 0.494(3) 1 calc PR B 4 H30E H -0.0881 0.9983 -0.1061 0.060 Uiso 0.494(3) 1 calc PR B 4 H30F H 0.0460 1.0247 -0.1524 0.060 Uiso 0.494(3) 1 calc PR B 4 C31A C 0.186(2) 0.7195(5) 0.0796(10) 0.0212(12) Uani 0.494(3) 1 d PDU B 4 H31C H 0.2811 0.7216 0.0573 0.025 Uiso 0.494(3) 1 calc PR B 4 H31D H 0.1305 0.6911 0.0306 0.025 Uiso 0.494(3) 1 calc PR B 4 C32A C 0.2026(6) 0.6976(3) 0.2009(9) 0.031(2) Uani 0.494(3) 1 d PDU B 4 H32B H 0.2484 0.7280 0.2516 0.037 Uiso 0.494(3) 1 calc PR B 4 C33A C 0.0591(5) 0.6829(2) 0.2363(4) 0.0380(11) Uani 0.494(3) 1 d PDU B 4 H33D H 0.0743 0.6703 0.3145 0.057 Uiso 0.494(3) 1 calc PR B 4 H33E H 0.0135 0.6526 0.1884 0.057 Uiso 0.494(3) 1 calc PR B 4 H33F H -0.0020 0.7164 0.2288 0.057 Uiso 0.494(3) 1 calc PR B 4 C34A C 0.3001(6) 0.6460(2) 0.2127(4) 0.0463(13) Uani 0.494(3) 1 d PDU B 4 H34D H 0.3913 0.6561 0.1901 0.069 Uiso 0.494(3) 1 calc PR B 4 H34E H 0.2559 0.6154 0.1647 0.069 Uiso 0.494(3) 1 calc PR B 4 H34F H 0.3158 0.6334 0.2908 0.069 Uiso 0.494(3) 1 calc PR B 4 C35A C 0.1233(8) 0.9357(2) 0.2710(5) 0.0269(16) Uani 0.494(3) 1 d PDU B 4 H35C H 0.1621 0.9393 0.2000 0.032 Uiso 0.494(3) 1 calc PR B 4 H35D H 0.0189 0.9394 0.2526 0.032 Uiso 0.494(3) 1 calc PR B 4 C36A C 0.1788(4) 0.98552(17) 0.3464(4) 0.0390(12) Uani 0.494(3) 1 d PDU B 4 H36B H 0.1360 0.9828 0.4167 0.047 Uiso 0.494(3) 1 calc PR B 4 C37A C 0.3400(5) 0.9833(3) 0.3787(6) 0.073(2) Uani 0.494(3) 1 d PDU B 4 H37D H 0.3676 0.9466 0.4130 0.110 Uiso 0.494(3) 1 calc PR B 4 H37E H 0.3711 1.0135 0.4323 0.110 Uiso 0.494(3) 1 calc PR B 4 H37F H 0.3847 0.9882 0.3116 0.110 Uiso 0.494(3) 1 calc PR B 4 C38A C 0.1346(6) 1.04236(19) 0.2910(5) 0.0561(16) Uani 0.494(3) 1 d PDU B 4 H38D H 0.0311 1.0434 0.2701 0.084 Uiso 0.494(3) 1 calc PR B 4 H38E H 0.1793 1.0469 0.2238 0.084 Uiso 0.494(3) 1 calc PR B 4 H38F H 0.1650 1.0731 0.3437 0.084 Uiso 0.494(3) 1 calc PR B 4 N1P N 0.8287(13) 0.2259(6) 0.3575(9) 0.025(3) Uani 0.376(7) 1 d PDU C 5 C1P C 0.7701(15) 0.1913(6) 0.2756(13) 0.046(3) Uani 0.376(7) 1 d PDU C 5 H1PB H 0.8056 0.1874 0.2068 0.055 Uiso 0.376(7) 1 calc PR C 5 C2P C 0.6543(15) 0.1619(5) 0.2994(11) 0.052(3) Uani 0.376(7) 1 d PDU C 5 H2PA H 0.6072 0.1366 0.2450 0.062 Uiso 0.376(7) 1 calc PR C 5 C3P C 0.6041(16) 0.1680(5) 0.3997(11) 0.043(4) Uani 0.376(7) 1 d PDU C 5 C4P C 0.6710(7) 0.2041(2) 0.4785(6) 0.0353(17) Uani 0.376(7) 1 d PDU C 5 H4PA H 0.6382 0.2084 0.5483 0.042 Uiso 0.376(7) 1 calc PR C 5 C5P C 0.7870(7) 0.2345(3) 0.4561(6) 0.0297(15) Uani 0.376(7) 1 d PDU C 5 H5PA H 0.8350 0.2604 0.5089 0.036 Uiso 0.376(7) 1 calc PR C 5 C6P C 0.4707(14) 0.1337(5) 0.4236(9) 0.0697(15) Uani 0.376(7) 1 d PDU C 5 H6PA H 0.4368 0.1094 0.3593 0.105 Uiso 0.376(7) 1 calc PR C 5 H6PB H 0.3954 0.1601 0.4360 0.105 Uiso 0.376(7) 1 calc PR C 5 H6PC H 0.4969 0.1102 0.4904 0.105 Uiso 0.376(7) 1 calc PR C 5 N01P N 0.8252(10) 0.2364(5) 0.3476(6) 0.038(2) Uani 0.624(7) 1 d PDU C 6 C01P C 0.8068(9) 0.1850(4) 0.3009(7) 0.0468(19) Uani 0.624(7) 1 d PDU C 6 H01B H 0.8771 0.1738 0.2576 0.056 Uiso 0.624(7) 1 calc PR C 6 C02P C 0.7010(7) 0.1459(3) 0.3066(6) 0.0463(16) Uani 0.624(7) 1 d PDU C 6 H02A H 0.7010 0.1106 0.2688 0.056 Uiso 0.624(7) 1 calc PR C 6 C03P C 0.5959(10) 0.1588(4) 0.3676(6) 0.0416(19) Uani 0.624(7) 1 d PDU C 6 C04P C 0.6055(6) 0.2110(3) 0.4182(5) 0.0499(14) Uani 0.624(7) 1 d PDU C 6 H04A H 0.5355 0.2228 0.4613 0.060 Uiso 0.624(7) 1 calc PR C 6 C05P C 0.7171(6) 0.24625(19) 0.4061(4) 0.0477(14) Uani 0.624(7) 1 d PDU C 6 H05A H 0.7186 0.2817 0.4432 0.057 Uiso 0.624(7) 1 calc PR C 6 C06P C 0.4799(8) 0.1192(3) 0.3777(5) 0.0697(15) Uani 0.624(7) 1 d PDU C 6 H06A H 0.4936 0.0844 0.3368 0.105 Uiso 0.624(7) 1 calc PR C 6 H06B H 0.3891 0.1365 0.3461 0.105 Uiso 0.624(7) 1 calc PR C 6 H06C H 0.4795 0.1104 0.4568 0.105 Uiso 0.624(7) 1 calc PR C 6 N11P N 0.2841(5) 0.19202(17) 0.6068(3) 0.0383(11) Uani 0.508(4) 1 d PDU D 7 C11P C 0.1884(5) 0.1909(2) 0.5132(4) 0.0421(12) Uani 0.508(4) 1 d PDU D 7 H11B H 0.1810 0.2230 0.4654 0.051 Uiso 0.508(4) 1 calc PR D 7 C12P C 0.1002(5) 0.1456(2) 0.4829(4) 0.0419(12) Uani 0.508(4) 1 d PDU D 7 H12A H 0.0362 0.1467 0.4145 0.050 Uiso 0.508(4) 1 calc PR D 7 C13P C 0.1040(5) 0.0985(2) 0.5513(4) 0.0369(12) Uani 0.508(4) 1 d PDU D 7 C14P C 0.2046(9) 0.0996(4) 0.6462(7) 0.039(2) Uani 0.508(4) 1 d PDU D 7 H14A H 0.2147 0.0682 0.6957 0.047 Uiso 0.508(4) 1 calc PR D 7 C15P C 0.2899(10) 0.1459(3) 0.6693(7) 0.0381(19) Uani 0.508(4) 1 d PDU D 7 H15P H 0.3585 0.1449 0.7352 0.046 Uiso 0.508(4) 1 calc PR D 7 C16P C 0.0022(7) 0.0496(3) 0.5263(5) 0.0525(15) Uani 0.508(4) 1 d PDU D 7 H16R H -0.0630 0.0573 0.4570 0.079 Uiso 0.508(4) 1 calc PR D 7 H16S H -0.0521 0.0449 0.5882 0.079 Uiso 0.508(4) 1 calc PR D 7 H16T H 0.0557 0.0150 0.5175 0.079 Uiso 0.508(4) 1 calc PR D 7 N21P N 0.2138(5) 0.1732(2) 0.6453(3) 0.0399(12) Uani 0.492(4) 1 d PDU D 8 C21P C 0.0754(5) 0.1801(2) 0.6009(4) 0.0399(12) Uani 0.492(4) 1 d PDU D 8 H21P H 0.0399 0.2176 0.5907 0.048 Uiso 0.492(4) 1 calc PR D 8 C22P C -0.0167(5) 0.1362(2) 0.5697(4) 0.0414(13) Uani 0.492(4) 1 d PDU D 8 H22A H -0.1125 0.1439 0.5385 0.050 Uiso 0.492(4) 1 calc PR D 8 C23P C 0.0303(6) 0.0805(3) 0.5837(4) 0.0369(12) Uani 0.492(4) 1 d PDU D 8 C24P C 0.1702(8) 0.0734(3) 0.6319(7) 0.0390(18) Uani 0.492(4) 1 d PDU D 8 H24A H 0.2067 0.0363 0.6466 0.047 Uiso 0.492(4) 1 calc PR D 8 C25P C 0.2571(10) 0.1191(4) 0.6586(7) 0.034(2) Uani 0.492(4) 1 d PDU D 8 H25A H 0.3538 0.1122 0.6882 0.041 Uiso 0.492(4) 1 calc PR D 8 C26P C -0.0709(7) 0.0319(3) 0.5520(5) 0.0561(16) Uani 0.492(4) 1 d PDU D 8 H26A H -0.0201 -0.0040 0.5669 0.084 Uiso 0.492(4) 1 calc PR D 8 H26B H -0.1096 0.0344 0.4721 0.084 Uiso 0.492(4) 1 calc PR D 8 H26C H -0.1486 0.0339 0.5962 0.084 Uiso 0.492(4) 1 calc PR D 8 O1W O 0.1837(8) 0.2013(3) 0.2723(6) 0.0656(19) Uani 0.28 1 d PU E 9 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 0.0230(9) 0.0215(12) 0.0157(7) -0.0001(9) 0.0059(6) 0.0012(9) N2 0.0176(8) 0.0169(13) 0.0161(7) -0.0006(9) 0.0044(6) 0.0002(9) N3 0.0179(7) 0.0180(13) 0.0153(7) -0.0026(9) 0.0045(5) 0.0014(10) O1 0.024(3) 0.048(2) 0.004(6) 0.000(5) 0.007(4) 0.0057(18) O2 0.0223(18) 0.048(4) 0.0232(18) 0.005(3) 0.0095(12) 0.006(3) O3 0.020(2) 0.071(5) 0.0215(17) -0.004(3) 0.0068(15) 0.013(3) O4 0.033(2) 0.060(4) 0.014(2) -0.005(3) 0.0033(16) 0.013(3) C1 0.0171(8) 0.0180(13) 0.0169(8) 0.0009(9) 0.0033(6) 0.0009(10) C2 0.0185(9) 0.0186(13) 0.0165(7) 0.0014(8) 0.0053(6) 0.0010(8) C3 0.011(5) 0.0385(19) 0.007(2) -0.0018(17) -0.003(2) -0.0039(16) C4 0.0167(8) 0.0165(13) 0.0157(7) -0.0038(10) 0.0025(6) 0.0009(10) C5 0.027(3) 0.043(4) 0.0092(18) 0.000(2) 0.0038(16) 0.004(2) C6 0.027(3) 0.035(4) 0.014(2) 0.000(2) 0.0052(18) 0.001(3) C7 0.0234(19) 0.030(3) 0.025(3) -0.002(2) 0.005(2) -0.005(2) C8 0.031(3) 0.0365(17) 0.043(4) 0.006(2) 0.005(2) 0.0056(15) C9 0.060(5) 0.042(2) 0.034(3) 0.0042(19) 0.010(2) -0.011(3) C10 0.048(3) 0.038(2) 0.077(5) 0.006(3) 0.008(3) 0.0036(16) C11 0.054(5) 0.0492(18) 0.024(7) -0.0153(17) 0.020(3) -0.0259(19) C12 0.104(3) 0.0303(19) 0.047(5) -0.013(2) 0.023(2) -0.0177(15) C13 0.155(10) 0.020(4) 0.056(6) 0.011(4) 0.029(6) 0.009(5) C14 0.072(5) 0.038(2) 0.089(8) -0.005(5) -0.008(5) 0.006(3) C15 0.020(2) 0.042(3) 0.019(2) -0.001(2) -0.0011(16) 0.008(2) C16 0.032(2) 0.036(2) 0.033(2) 0.0031(15) 0.0054(14) 0.0004(14) C17 0.042(3) 0.048(3) 0.032(2) 0.003(2) 0.0045(18) 0.0054(19) C18 0.049(3) 0.042(3) 0.056(3) -0.010(2) 0.006(2) -0.002(2) N1A 0.0230(9) 0.0215(12) 0.0157(7) -0.0001(9) 0.0059(6) 0.0012(9) N2A 0.0176(8) 0.0169(13) 0.0161(7) -0.0006(9) 0.0044(6) 0.0002(9) N3A 0.0179(7) 0.0180(13) 0.0153(7) -0.0026(9) 0.0045(5) 0.0014(10) O1A 0.024(3) 0.048(2) 0.004(6) 0.000(5) 0.007(4) 0.0057(18) O2A 0.0140(18) 0.045(5) 0.0154(18) 0.004(3) 0.0051(13) 0.006(3) O3A 0.027(3) 0.060(5) 0.025(2) -0.007(4) 0.0117(17) -0.001(4) O4A 0.038(2) 0.062(5) 0.011(2) -0.009(3) 0.0072(16) -0.013(3) C1A 0.0171(8) 0.0180(13) 0.0169(8) 0.0009(9) 0.0033(6) 0.0009(10) C2A 0.0185(9) 0.0186(13) 0.0165(7) 0.0014(8) 0.0053(6) 0.0010(8) C3A 0.011(5) 0.0385(19) 0.007(2) -0.0018(17) -0.003(2) -0.0039(16) C4A 0.0167(8) 0.0165(13) 0.0157(7) -0.0038(10) 0.0025(6) 0.0009(10) C5A 0.015(2) 0.034(4) 0.0094(19) -0.006(2) 0.0026(15) -0.0031(19) C6A 0.029(3) 0.042(5) 0.020(3) -0.007(3) 0.013(2) -0.010(3) C7A 0.0234(19) 0.030(3) 0.025(3) -0.002(2) 0.005(2) -0.005(2) C8A 0.031(3) 0.0365(17) 0.043(4) 0.006(2) 0.005(2) 0.0056(15) C9A 0.060(5) 0.042(2) 0.034(3) 0.0042(19) 0.010(2) -0.011(3) C10A 0.048(3) 0.038(2) 0.077(5) 0.006(3) 0.008(3) 0.0036(16) C11A 0.054(5) 0.0492(18) 0.024(7) -0.0153(17) 0.020(3) -0.0259(19) C12A 0.104(3) 0.0303(19) 0.047(5) -0.013(2) 0.023(2) -0.0177(15) C13A 0.052(4) 0.028(6) 0.037(5) 0.010(3) 0.010(3) -0.002(3) C14A 0.072(5) 0.038(2) 0.089(8) -0.005(5) -0.008(5) 0.006(3) C15A 0.009(2) 0.034(3) 0.018(2) 0.0084(18) 0.0020(15) -0.0004(17) C16A 0.032(2) 0.036(2) 0.033(2) 0.0031(15) 0.0054(14) 0.0004(14) C17A 0.023(2) 0.046(3) 0.030(2) 0.017(2) -0.0031(18) -0.0051(19) C18A 0.035(3) 0.025(3) 0.094(5) 0.002(3) 0.024(3) -0.001(2) N21 0.0243(9) 0.008(5) 0.0138(12) -0.001(4) 0.0075(8) 0.002(4) N22 0.0170(8) 0.042(5) 0.0127(14) -0.005(2) 0.0059(9) 0.0005(16) N23 0.0193(19) 0.0460(11) 0.0155(16) -0.0073(11) 0.0070(9) -0.0063(14) O21 0.015(3) 0.033(6) 0.011(4) -0.005(3) 0.007(2) 0.001(3) O22 0.015(3) 0.037(8) 0.013(4) -0.014(4) 0.000(3) -0.015(3) O23 0.026(2) 0.038(5) 0.007(3) -0.008(3) 0.000(2) -0.009(2) O24 0.077(7) 0.032(4) 0.017(3) -0.006(2) 0.020(3) 0.002(3) C21 0.0214(10) 0.0257(8) 0.0195(9) -0.0004(6) 0.0073(6) -0.0015(6) C22 0.0161(8) 0.0164(13) 0.0154(7) -0.0030(10) 0.0033(6) 0.0010(10) C23 0.0166(7) 0.0184(13) 0.0147(7) -0.0042(9) 0.0039(6) 0.0011(10) C24 0.0179(8) 0.0155(13) 0.0135(7) -0.0002(10) 0.0034(6) -0.0002(10) C25 0.0216(11) 0.0233(11) 0.0164(8) -0.0005(8) 0.0044(7) -0.0012(8) C26 0.0198(8) 0.0186(13) 0.0154(8) 0.0004(9) 0.0039(6) 0.0015(10) C27 0.0253(12) 0.0268(9) 0.0245(11) -0.0009(8) 0.0059(9) -0.0004(8) C28 0.035(3) 0.026(3) 0.016(3) 0.011(3) 0.009(2) 0.003(2) C29 0.044(3) 0.032(4) 0.020(3) -0.007(3) 0.005(3) -0.005(2) C30 0.044(4) 0.0357(18) 0.043(5) -0.003(3) 0.013(3) 0.010(3) C31 0.0247(11) 0.021(4) 0.0191(18) 0.0043(19) 0.0076(15) -0.001(3) C32 0.026(3) 0.025(4) 0.024(4) 0.009(2) 0.002(2) 0.006(2) C33 0.049(3) 0.037(3) 0.046(3) 0.016(2) 0.015(2) 0.011(2) C34 0.045(3) 0.054(3) 0.027(2) 0.011(2) -0.004(2) 0.001(2) C35 0.032(3) 0.024(3) 0.021(3) -0.009(2) 0.009(2) 0.005(2) C36 0.045(3) 0.029(2) 0.023(2) -0.0016(17) 0.0097(18) -0.0100(18) C37 0.048(3) 0.047(3) 0.038(3) -0.006(2) 0.021(2) -0.021(2) C38 0.068(4) 0.034(3) 0.042(3) 0.011(2) 0.010(2) -0.008(2) N21A 0.0243(9) 0.008(5) 0.0138(12) -0.001(4) 0.0075(8) 0.002(4) N22A 0.0170(8) 0.042(5) 0.0127(14) -0.005(2) 0.0059(9) 0.0005(16) N23A 0.0193(19) 0.0460(11) 0.0155(16) -0.0073(11) 0.0070(9) -0.0063(14) O21A 0.015(3) 0.033(6) 0.011(4) -0.005(3) 0.007(2) 0.001(3) O22A 0.015(3) 0.037(8) 0.013(4) -0.014(4) 0.000(3) -0.015(3) O23A 0.045(4) 0.035(5) 0.013(3) -0.008(3) 0.013(2) -0.020(3) O24A 0.030(3) 0.041(6) 0.014(3) -0.011(3) 0.010(2) -0.014(4) C21A 0.0214(10) 0.0257(8) 0.0195(9) -0.0004(6) 0.0073(6) -0.0015(6) C22A 0.0161(8) 0.0164(13) 0.0154(7) -0.0030(10) 0.0033(6) 0.0010(10) C23A 0.0166(7) 0.0184(13) 0.0147(7) -0.0042(9) 0.0039(6) 0.0011(10) C24A 0.0179(8) 0.0155(13) 0.0135(7) -0.0002(10) 0.0034(6) -0.0002(10) C25A 0.0216(11) 0.0233(11) 0.0164(8) -0.0005(8) 0.0044(7) -0.0012(8) C26A 0.0198(8) 0.0186(13) 0.0154(8) 0.0004(9) 0.0039(6) 0.0015(10) C27A 0.0253(12) 0.0268(9) 0.0245(11) -0.0009(8) 0.0059(9) -0.0004(8) C28A 0.040(3) 0.019(3) 0.020(4) 0.001(3) 0.010(3) 0.005(2) C29A 0.039(3) 0.039(4) 0.032(4) -0.007(3) 0.007(3) -0.010(3) C30A 0.044(4) 0.0357(18) 0.043(5) -0.003(3) 0.013(3) 0.010(3) C31A 0.0247(11) 0.021(4) 0.0191(18) 0.0043(19) 0.0076(15) -0.001(3) C32A 0.036(4) 0.037(4) 0.021(4) 0.012(3) 0.010(3) 0.008(3) C33A 0.043(3) 0.039(3) 0.035(2) 0.013(2) 0.014(2) 0.002(2) C34A 0.049(3) 0.050(3) 0.041(3) 0.011(2) 0.010(2) 0.015(2) C35A 0.026(3) 0.037(4) 0.017(3) -0.010(2) 0.000(2) 0.000(2) C36A 0.045(3) 0.044(3) 0.029(2) -0.003(2) 0.008(2) -0.009(2) C37A 0.058(4) 0.052(4) 0.098(5) -0.002(4) -0.030(4) -0.017(3) C38A 0.058(4) 0.035(3) 0.072(4) -0.002(3) 0.000(3) -0.006(2) N1P 0.022(4) 0.022(6) 0.031(5) 0.009(4) 0.002(3) -0.004(3) C1P 0.067(8) 0.049(6) 0.015(5) -0.001(4) -0.017(4) -0.009(5) C2P 0.069(9) 0.043(7) 0.035(5) -0.006(5) -0.018(6) 0.002(5) C3P 0.050(5) 0.029(8) 0.046(8) 0.000(6) -0.007(5) -0.020(4) C4P 0.031(4) 0.045(4) 0.025(4) 0.009(3) -0.010(3) 0.000(3) C5P 0.021(3) 0.036(4) 0.028(3) 0.011(3) -0.009(3) 0.001(2) C6P 0.082(3) 0.076(4) 0.055(4) -0.007(3) 0.021(3) -0.033(3) N01P 0.058(4) 0.026(4) 0.030(3) 0.010(2) 0.005(2) 0.002(2) C01P 0.054(4) 0.059(4) 0.028(5) -0.009(3) 0.008(3) -0.014(3) C02P 0.052(4) 0.038(4) 0.049(3) -0.010(3) 0.007(3) -0.007(3) C03P 0.052(4) 0.038(4) 0.033(4) -0.002(3) -0.003(3) -0.010(3) C04P 0.055(3) 0.050(4) 0.048(3) -0.006(3) 0.019(3) -0.005(2) C05P 0.063(4) 0.032(2) 0.052(3) -0.012(2) 0.022(3) -0.013(2) C06P 0.082(3) 0.076(4) 0.055(4) -0.007(3) 0.021(3) -0.033(3) N11P 0.045(3) 0.034(2) 0.035(2) -0.0028(18) 0.003(2) 0.0054(19) C11P 0.055(3) 0.032(3) 0.035(3) 0.005(2) -0.005(2) 0.010(2) C12P 0.048(3) 0.040(3) 0.034(3) -0.001(2) -0.003(2) 0.009(2) C13P 0.036(3) 0.040(3) 0.037(3) -0.011(2) 0.016(2) 0.003(2) C14P 0.046(7) 0.031(7) 0.044(5) 0.002(5) 0.015(5) -0.004(4) C15P 0.057(5) 0.027(5) 0.029(3) -0.006(4) 0.004(3) 0.005(3) C16P 0.054(4) 0.050(4) 0.059(4) -0.014(3) 0.024(3) -0.008(3) N21P 0.047(3) 0.043(3) 0.031(2) 0.005(2) 0.009(2) 0.014(2) C21P 0.037(3) 0.045(3) 0.038(3) 0.007(2) 0.006(2) 0.014(2) C22P 0.035(3) 0.056(3) 0.034(3) 0.006(2) 0.0065(19) 0.014(2) C23P 0.039(3) 0.044(3) 0.030(3) 0.000(2) 0.011(2) 0.008(2) C24P 0.037(4) 0.041(5) 0.039(3) 0.008(4) 0.006(3) 0.007(3) C25P 0.037(6) 0.033(9) 0.033(4) 0.004(6) 0.003(4) 0.009(4) C26P 0.048(4) 0.067(4) 0.056(4) 0.001(3) 0.016(3) -0.005(3) O1W 0.071(5) 0.052(4) 0.077(5) 0.012(4) 0.022(4) 0.009(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 N1 C1 1.466(6) . ? N2 C2 1.334(8) . ? N2 C3 1.473(10) . ? N3 C4 1.437(6) . ? N3 C5 1.457(6) . ? O1 C2 1.33(3) . ? O2 C4 1.249(9) . ? O3 C6 1.241(10) . ? O4 C6 1.236(9) . ? C1 C7 1.527(4) . ? C1 C2 1.528(4) . ? C3 C4 1.525(4) . ? C3 C11 1.545(5) . ? C5 C6 1.543(4) . ? C5 C15 1.551(4) . ? C7 C8 1.540(4) . ? C8 C9 1.537(4) . ? C8 C10 1.542(4) . ? C11 C12 1.538(5) . ? C12 C14 1.542(5) . ? C12 C13 1.551(5) . ? C15 C16 1.525(4) . ? C16 C17 1.526(4) . ? C16 C18 1.532(4) . ? N1A C1A 1.504(7) . ? N2A C2A 1.346(9) . ? N2A C3A 1.483(11) . ? N3A C4A 1.317(7) . ? N3A C5A 1.470(7) . ? O1A C2A 1.11(4) . ? O2A C4A 1.207(11) . ? O3A C6A 1.266(13) . ? O4A C6A 1.268(12) . ? C1A C2A 1.531(4) . ? C1A C7A 1.535(5) . ? C3A C4A 1.534(5) . ? C3A C11A 1.545(5) . ? C5A C15A 1.540(4) . ? C5A C6A 1.543(4) . ? C7A C8A 1.544(5) . ? C8A C9A 1.537(4) . ? C8A C10A 1.544(5) . ? C11A C12A 1.539(5) . ? C12A C14A 1.540(5) . ? C12A C13A 1.549(5) . ? C15A C16A 1.535(5) . ? C16A C18A 1.530(5) . ? C16A C17A 1.531(4) . ? N21 C21 1.42(3) . ? N22 C22 1.341(11) . ? N22 C23 1.420(10) . ? N23 C24 1.351(12) . ? N23 C25 1.467(11) . ? O21 C22 1.18(3) . ? O22 C24 1.26(2) . ? O23 C26 1.246(10) . ? O24 C26 1.242(10) . ? C21 C22 1.536(4) . ? C21 C27 1.543(5) . ? C23 C24 1.530(4) . ? C23 C31 1.536(4) . ? C25 C35 1.534(4) . ? C25 C26 1.537(4) . ? C27 C28 1.534(4) . ? C28 C29 1.533(5) . ? C28 C30 1.538(5) . ? C31 C32 1.541(5) . ? C32 C33 1.528(5) . ? C32 C34 1.535(5) . ? C35 C36 1.521(4) . ? C36 C37 1.527(4) . ? C36 C38 1.532(4) . ? N21A C21A 1.56(3) . ? N22A C22A 1.351(11) . ? N22A C23A 1.503(10) . ? N23A C24A 1.346(11) . ? N23A C25A 1.448(11) . ? O21A C22A 1.29(3) . ? O22A C24A 1.20(2) . ? O23A C26A 1.246(10) . ? O24A C26A 1.272(9) . ? C21A C22A 1.529(4) . ? C21A C27A 1.538(5) . ? C23A C24A 1.531(4) . ? C23A C31A 1.535(4) . ? C25A C26A 1.543(4) . ? C25A C35A 1.552(4) . ? C27A C28A 1.537(4) . ? C28A C29A 1.531(5) . ? C28A C30A 1.539(5) . ? C31A C32A 1.540(5) . ? C32A C34A 1.527(5) . ? C32A C33A 1.535(5) . ? C35A C36A 1.533(4) . ? C36A C37A 1.527(4) . ? C36A C38A 1.531(4) . ? N1P C5P 1.329(11) . ? N1P C1P 1.338(12) . ? C1P C2P 1.372(13) . ? C2P C3P 1.378(12) . ? C3P C4P 1.363(12) . ? C3P C6P 1.57(2) . ? C4P C5P 1.379(7) . ? N01P C01P 1.340(8) . ? N01P C05P 1.358(9) . ? C01P C02P 1.378(8) . ? C02P C03P 1.369(9) . ? C03P C04P 1.374(8) . ? C03P C06P 1.468(14) . ? C04P C05P 1.376(6) . ? N11P C15P 1.322(9) . ? N11P C11P 1.340(5) . ? C11P C12P 1.376(7) . ? C12P C13P 1.383(7) . ? C13P C14P 1.377(10) . ? C13P C16P 1.509(8) . ? C14P C15P 1.367(9) . ? N21P C25P 1.347(9) . ? N21P C21P 1.355(6) . ? C21P C22P 1.373(7) . ? C22P C23P 1.394(7) . ? C23P C24P 1.380(9) . ? C23P C26P 1.511(9) . ? C24P C25P 1.369(10) . ? 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 C2 N2 C3 115.5(8) . . ? C4 N3 C5 131.7(4) . . ? N1 C1 C7 109.0(4) . . ? N1 C1 C2 108.2(4) . . ? C7 C1 C2 110.0(6) . . ? O1 C2 N2 120.2(13) . . ? O1 C2 C1 124.8(13) . . ? N2 C2 C1 114.8(6) . . ? N2 C3 C4 103.3(7) . . ? N2 C3 C11 118(2) . . ? C4 C3 C11 94.5(9) . . ? O2 C4 N3 119.4(5) . . ? O2 C4 C3 119.0(8) . . ? N3 C4 C3 120.0(8) . . ? N3 C5 C6 107.7(4) . . ? N3 C5 C15 108.6(3) . . ? C6 C5 C15 111.6(4) . . ? O4 C6 O3 124.7(6) . . ? O4 C6 C5 116.8(5) . . ? O3 C6 C5 118.5(6) . . ? C1 C7 C8 115.2(5) . . ? C9 C8 C7 113.2(5) . . ? C9 C8 C10 108.9(4) . . ? C7 C8 C10 106.0(5) . . ? C12 C11 C3 106.7(11) . . ? C11 C12 C14 126(2) . . ? C11 C12 C13 101.0(11) . . ? C14 C12 C13 118.8(10) . . ? C16 C15 C5 117.6(3) . . ? C15 C16 C17 112.2(3) . . ? C15 C16 C18 107.6(3) . . ? C17 C16 C18 111.4(3) . . ? C2A N2A C3A 127.1(11) . . ? C4A N3A C5A 112.9(5) . . ? N1A C1A C2A 106.3(5) . . ? N1A C1A C7A 108.2(5) . . ? C2A C1A C7A 113.2(7) . . ? O1A C2A N2A 130.5(18) . . ? O1A C2A C1A 114.3(17) . . ? N2A C2A C1A 115.0(7) . . ? N2A C3A C4A 113.2(9) . . ? N2A C3A C11A 102(2) . . ? C4A C3A C11A 125.3(11) . . ? O2A C4A N3A 129.0(7) . . ? O2A C4A C3A 122.1(10) . . ? N3A C4A C3A 103.7(8) . . ? N3A C5A C15A 114.6(4) . . ? N3A C5A C6A 106.7(5) . . ? C15A C5A C6A 114.4(4) . . ? O3A C6A O4A 126.0(7) . . ? O3A C6A C5A 118.4(8) . . ? O4A C6A C5A 115.7(7) . . ? C1A C7A C8A 119.8(6) . . ? C9A C8A C10A 108.8(5) . . ? C9A C8A C7A 112.7(7) . . ? C10A C8A C7A 110.0(6) . . ? C12A C11A C3A 124.7(14) . . ? C11A C12A C14A 96(3) . . ? C11A C12A C13A 118.1(13) . . ? C14A C12A C13A 101.2(11) . . ? C16A C15A C5A 117.1(4) . . ? C18A C16A C17A 110.8(5) . . ? C18A C16A C15A 109.3(5) . . ? C17A C16A C15A 113.5(4) . . ? C22 N22 C23 123.6(14) . . ? C24 N23 C25 119.5(14) . . ? N21 C21 C22 112.2(14) . . ? N21 C21 C27 96.8(11) . . ? C22 C21 C27 115.5(8) . . ? O21 C22 N22 129.5(16) . . ? O21 C22 C21 118.1(16) . . ? N22 C22 C21 111.3(12) . . ? N22 C23 C24 107.6(13) . . ? N22 C23 C31 105.1(13) . . ? C24 C23 C31 112.8(9) . . ? O22 C24 N23 127.3(13) . . ? O22 C24 C23 121.8(11) . . ? N23 C24 C23 110.1(8) . . ? N23 C25 C35 121.1(17) . . ? N23 C25 C26 108.9(12) . . ? C35 C25 C26 103.1(5) . . ? O24 C26 O23 120.0(11) . . ? O24 C26 C25 121.1(10) . . ? O23 C26 C25 118.7(9) . . ? C28 C27 C21 113.4(8) . . ? C29 C28 C27 113.5(5) . . ? C29 C28 C30 112.7(6) . . ? C27 C28 C30 109.2(5) . . ? C23 C31 C32 113.6(7) . . ? C33 C32 C34 109.3(5) . . ? C33 C32 C31 110.3(6) . . ? C34 C32 C31 112.6(9) . . ? C36 C35 C25 114.5(4) . . ? C35 C36 C37 111.0(4) . . ? C35 C36 C38 108.3(4) . . ? C37 C36 C38 110.7(4) . . ? C22A N22A C23A 124.6(14) . . ? C24A N23A C25A 127.5(15) . . ? C22A C21A C27A 103.3(7) . . ? C22A C21A N21A 107.0(13) . . ? C27A C21A N21A 120.6(12) . . ? O21A C22A N22A 121.0(15) . . ? O21A C22A C21A 123.1(16) . . ? N22A C22A C21A 115.6(11) . . ? N22A C23A C24A 105.4(12) . . ? N22A C23A C31A 114.7(13) . . ? C24A C23A C31A 107.6(8) . . ? O22A C24A N23A 121.1(14) . . ? O22A C24A C23A 117.6(12) . . ? N23A C24A C23A 120.5(9) . . ? N23A C25A C26A 108.7(12) . . ? N23A C25A C35A 100.4(18) . . ? C26A C25A C35A 116.3(6) . . ? O23A C26A O24A 130.8(10) . . ? O23A C26A C25A 116.9(9) . . ? O24A C26A C25A 112.2(9) . . ? C28A C27A C21A 118.2(8) . . ? C29A C28A C27A 112.2(5) . . ? C29A C28A C30A 109.9(6) . . ? C27A C28A C30A 107.3(5) . . ? C23A C31A C32A 116.9(7) . . ? C34A C32A C33A 110.4(5) . . ? C34A C32A C31A 109.3(6) . . ? C33A C32A C31A 112.0(8) . . ? C36A C35A C25A 117.5(6) . . ? C37A C36A C38A 109.9(4) . . ? C37A C36A C35A 111.5(5) . . ? C38A C36A C35A 111.6(4) . . ? C5P N1P C1P 127.5(15) . . ? N1P C1P C2P 114.3(16) . . ? C1P C2P C3P 122.2(14) . . ? C4P C3P C2P 119.4(15) . . ? C4P C3P C6P 120.0(12) . . ? C2P C3P C6P 120.6(11) . . ? C3P C4P C5P 119.5(10) . . ? N1P C5P C4P 117.2(9) . . ? C01P N01P C05P 108.4(10) . . ? N01P C01P C02P 129.6(10) . . ? C03P C02P C01P 118.7(9) . . ? C02P C03P C04P 115.9(9) . . ? C02P C03P C06P 121.8(8) . . ? C04P C03P C06P 122.4(8) . . ? C03P C04P C05P 119.7(6) . . ? N01P C05P C04P 127.8(6) . . ? C15P N11P C11P 115.4(5) . . ? N11P C11P C12P 123.2(4) . . ? C11P C12P C13P 120.6(4) . . ? C14P C13P C12P 115.6(6) . . ? C14P C13P C16P 121.6(6) . . ? C12P C13P C16P 122.7(5) . . ? C15P C14P C13P 120.1(9) . . ? N11P C15P C14P 124.9(9) . . ? C25P N21P C21P 115.0(6) . . ? N21P C21P C22P 124.2(5) . . ? C21P C22P C23P 120.0(5) . . ? C24P C23P C22P 116.0(6) . . ? C24P C23P C26P 123.6(6) . . ? C22P C23P C26P 120.4(5) . . ? C25P C24P C23P 120.9(8) . . ? N21P C25P C24P 123.9(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 133.0(6) . . . . ? N2 C3 C4 N3 123.5(9) . . . . ? N3 C5 C6 O3 -30.8(7) . . . . ? N3 C5 C6 O4 149.9(5) . . . . ? C2 N2 C3 C4 -140.5(9) . . . . ? C4 N3 C5 C6 -133.2(5) . . . . ? C1 C2 N2 C3 172.8(8) . . . . ? C3 C4 N3 C5 -174.9(7) . . . . ? N1A C1A C2A N2A 130.4(8) . . . . ? N2A C3A C4A N3A 155.6(14) . . . . ? N3A C5A C6A O3A -12.6(7) . . . . ? N3A C5A C6A O4A 168.8(6) . . . . ? C2A N2A C3A C4A -115.9(14) . . . . ? C4A N3A C5A C6A -170.4(5) . . . . ? C1A C2A N2A C3A 162.8(9) . . . . ? C3A C4A N3A C5A 159.1(10) . . . . ? N21 C21 C22 N22 145.9(19) . . . . ? N22 C23 C24 N23 134(2) . . . . ? N23 C25 C26 O23 -9.4(18) . . . . ? N23 C25 C26 O24 175.8(19) . . . . ? C22 N22 C23 C24 -129(2) . . . . ? C24 N23 C25 C26 -150(3) . . . . ? C21 C22 N22 C23 164(2) . . . . ? C23 C24 N23 C25 -178(2) . . . . ? N21A C21A C22A N22A 122(2) . . . . ? N22A C23A C24A N23A 121(2) . . . . ? N23A C25A C26A O23A 3(2) . . . . ? N23A C25A C26A O24A -179.7(19) . . . . ? C22A N22A C23A C24A -113(3) . . . . ? C24A N23A C25A C26A -137(3) . . . . ? C21A C22A N22A C23A 173(2) . . . . ? C23A C24A N23A C25A 171(2) . . . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 0.252 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.039 #===END _chemical_name_common ;L-leucyl-L-leucyl-L-leucine - 4-methylpyridine clathrate (1:1:0.14) ;