# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1579 data_bq _audit_creation_method SHELXL-97 _chemical_name_systematic ; Endothelin inhibitor BQ123 Na: cyclo(-D-Trp-D-Asp-Pro-D-Val-Leu-),Na ; _chemical_name_common BQ123 _chemical_formula_moiety '4(C31 H41 N6 O7 Na), 8(C3 H8 O), 10(H2 O)' _chemical_formula_sum 'C148 H248 N24 Na4 O46' _chemical_formula_weight 3191.66 _chemical_compound_source 'synthesis (from BACHEM)' 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 25.399(5) _cell_length_b 34.717(5) _cell_length_c 25.74(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22693(24) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6864 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Crystals was grown from aqueous iso-propanol. At data collection, crystal was moved to 100% glycerol and was mounted on cryo-loop (Hampton Reseach, USA). And then, crystal was quickly frozened under the nitorgen stream (100K). ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.83400 _diffrn_radiation_type 'double monochromated beam' _diffrn_radiation_source 'synchrotron (SPring8)' _diffrn_radiation_monochromator 'diamond' _diffrn_measurement_device_type 'Rigaku RAXIS-4' _diffrn_measurement_method 'region-profit' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35804 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 31.42 _reflns_number_total 35332 _reflns_number_gt 31000 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Rigaku Process 4.0' _computing_cell_refinement 'Rigaku Process 4.0' _computing_data_reduction 'Rigaku Process 4.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson 1996)' _computing_publication_material 'PARST (Nardelli, 1983)' _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 fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1687P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0116(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(3) _refine_ls_number_reflns 35332 _refine_ls_number_parameters 2088 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2241 _refine_ls_wR_factor_gt 0.2146 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 5.873 _refine_ls_shift/su_mean 0.285 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na_1 Na 0.25282(5) 1.02547(4) 0.28470(5) 0.0597(3) Uani 1 d . . . Na_2 Na 0.03721(5) 0.73421(4) 0.51177(5) 0.0611(3) Uani 1 d . . . Na_3 Na 0.23094(6) 0.90913(4) 0.55407(5) 0.0625(3) Uani 1 d . . . Na_4 Na 0.33041(5) 0.83606(4) 0.53719(5) 0.0624(3) Uani 1 d . . . N_11 N 0.31014(11) 1.00904(9) 0.15184(11) 0.0588(6) Uani 1 d . . . H0_11 H 0.3126 0.9948 0.1791 0.071 Uiso 1 calc R . . CA_11 C 0.35479(14) 1.03406(12) 0.13837(14) 0.0610(8) Uani 1 d . . . HA_11 H 0.3603 1.0326 0.1007 0.073 Uiso 1 calc R . . CB_11 C 0.40417(14) 1.01842(13) 0.16536(16) 0.0666(9) Uani 1 d . . . HB1_11 H 0.4003 1.0211 0.2027 0.080 Uiso 1 calc R . . HB2_11 H 0.4079 0.9912 0.1575 0.080 Uiso 1 calc R . . CG_11 C 0.45335(15) 1.03968(12) 0.14790(17) 0.0687(9) Uani 1 d . . . CD1_11 C 0.47924(18) 1.06821(14) 0.1718(2) 0.0789(11) Uani 1 d . . . HD1_11 H 0.4683 1.0800 0.2024 0.095 Uiso 1 calc R . . NE1_11 N 0.52460(15) 1.07776(12) 0.14481(18) 0.0838(10) Uani 1 d . . . HE1_11 H 0.5468 1.0954 0.1533 0.101 Uiso 1 calc R . . CE2_11 C 0.52779(17) 1.05410(14) 0.10221(19) 0.0761(11) Uani 1 d . . . CZ2_11 C 0.56699(19) 1.05264(17) 0.0640(2) 0.0930(15) Uani 1 d . . . HZ2_11 H 0.5960 1.0690 0.0647 0.112 Uiso 1 calc R . . CH2_11 C 0.5602(2) 1.02566(19) 0.0252(2) 0.0992(16) Uani 1 d . . . HH2_11 H 0.5855 1.0234 -0.0007 0.119 Uiso 1 calc R . . CZ3_11 C 0.5160(2) 1.00165(19) 0.0240(2) 0.0971(15) Uani 1 d . . . HZ3_11 H 0.5125 0.9842 -0.0032 0.116 Uiso 1 calc R . . CE3_11 C 0.47774(18) 1.00285(14) 0.06170(17) 0.0767(10) Uani 1 d . . . HE3_11 H 0.4490 0.9863 0.0608 0.092 Uiso 1 calc R . . CD2_11 C 0.48381(16) 1.03060(13) 0.10235(16) 0.0697(9) Uani 1 d . . . C_11 C 0.34041(13) 1.07542(11) 0.15213(13) 0.0572(8) Uani 1 d . . . O_11 O 0.33023(10) 1.09920(8) 0.11855(9) 0.0637(6) Uani 1 d . . . N_12 N 0.33782(12) 1.08355(9) 0.20301(11) 0.0605(7) Uani 1 d . . . H0_12 H 0.3531 1.0684 0.2248 0.073 Uiso 1 calc R . . CA_12 C 0.31023(15) 1.11694(12) 0.22233(14) 0.0622(8) Uani 1 d . . . HA_12 H 0.3133 1.1377 0.1966 0.075 Uiso 1 calc R . . CB_12 C 0.33539(15) 1.13054(11) 0.27340(14) 0.0616(8) Uani 1 d . . . HB1_12 H 0.3164 1.1530 0.2856 0.074 Uiso 1 calc R . . HB2_12 H 0.3713 1.1384 0.2664 0.074 Uiso 1 calc R . . CG_12 C 0.33598(15) 1.10020(12) 0.31716(14) 0.0638(9) Uani 1 d . . . OD1_12 O 0.32388(11) 1.06654(8) 0.30745(9) 0.0643(6) Uani 1 d . . . OD2_12 O 0.35037(12) 1.11290(9) 0.36155(10) 0.0731(7) Uani 1 d . . . C_12 C 0.25211(14) 1.10724(11) 0.22940(13) 0.0583(8) Uani 1 d . . . O_12 O 0.23666(10) 1.07305(8) 0.22585(9) 0.0608(6) Uani 1 d . . . N_13 N 0.21843(12) 1.13488(9) 0.24156(11) 0.0581(6) Uani 1 d . . . CA_13 C 0.16370(15) 1.12658(11) 0.25759(14) 0.0611(8) Uani 1 d . . . HA_13 H 0.1636 1.1151 0.2924 0.073 Uiso 1 calc R . . CB_13 C 0.13773(16) 1.16610(12) 0.25932(17) 0.0703(9) Uani 1 d . . . HB1_13 H 0.1364 1.1757 0.2947 0.084 Uiso 1 calc R . . HB2_13 H 0.1022 1.1649 0.2457 0.084 Uiso 1 calc R . . CG_13 C 0.17237(17) 1.19198(13) 0.22530(17) 0.0718(10) Uani 1 d . . . HG1_13 H 0.1639 1.1890 0.1888 0.086 Uiso 1 calc R . . HG2_13 H 0.1687 1.2189 0.2349 0.086 Uiso 1 calc R . . CD_13 C 0.22696(16) 1.17729(11) 0.23718(17) 0.0668(9) Uani 1 d . . . HD1_13 H 0.2513 1.1834 0.2093 0.080 Uiso 1 calc R . . HD2_13 H 0.2402 1.1880 0.2695 0.080 Uiso 1 calc R . . C_13 C 0.13764(14) 1.09942(12) 0.21953(14) 0.0617(8) Uani 1 d . . . O_13 O 0.13065(11) 1.10880(8) 0.17403(10) 0.0675(6) Uani 1 d . . . N_14 N 0.12001(12) 1.06581(9) 0.23955(11) 0.0593(7) Uani 1 d . . . H0_14 H 0.1168 1.0632 0.2726 0.071 Uiso 1 calc R . . CA_14 C 0.10636(14) 1.03403(11) 0.20508(13) 0.0597(8) Uani 1 d . . . HA_14 H 0.0974 1.0443 0.1708 0.072 Uiso 1 calc R . . CB_14 C 0.06011(15) 1.01046(12) 0.22556(15) 0.0661(9) Uani 1 d . . . HB_14 H 0.0692 1.0008 0.2602 0.079 Uiso 1 calc R . . CG1_14 C 0.05005(18) 0.97563(14) 0.18957(19) 0.0794(11) Uani 1 d . . . HG1A_14 H 0.0453 0.9845 0.1545 0.119 Uiso 1 calc R . . HG1B_14 H 0.0189 0.9623 0.2008 0.119 Uiso 1 calc R . . HG1C_14 H 0.0796 0.9585 0.1910 0.119 Uiso 1 calc R . . CG2_14 C 0.01095(16) 1.03557(14) 0.23026(19) 0.0765(11) Uani 1 d . . . HG2A_14 H 0.0183 1.0571 0.2525 0.115 Uiso 1 calc R . . HG2B_14 H -0.0173 1.0206 0.2447 0.115 Uiso 1 calc R . . HG2C_14 H 0.0010 1.0447 0.1965 0.115 Uiso 1 calc R . . C_14 C 0.15625(14) 1.00929(11) 0.20050(13) 0.0585(8) Uani 1 d . . . O_14 O 0.17645(10) 0.99579(7) 0.24080(9) 0.0597(5) Uani 1 d . . . N_15 N 0.17549(12) 1.00338(9) 0.15335(11) 0.0587(6) Uani 1 d . . . H0_15 H 0.1593 1.0133 0.1272 0.070 Uiso 1 calc R . . CA_15 C 0.22334(14) 0.98051(11) 0.14368(14) 0.0591(8) Uani 1 d . . . HA_15 H 0.2350 0.9690 0.1765 0.071 Uiso 1 calc R . . CB_15 C 0.21324(16) 0.94852(12) 0.10441(14) 0.0646(9) Uani 1 d . . . HB1_15 H 0.2442 0.9322 0.1029 0.078 Uiso 1 calc R . . HB2_15 H 0.2089 0.9601 0.0704 0.078 Uiso 1 calc R . . CG_15 C 0.16533(17) 0.92300(12) 0.11529(15) 0.0687(9) Uani 1 d . . . HG_15 H 0.1339 0.9393 0.1137 0.082 Uiso 1 calc R . . CD1_15 C 0.1675(2) 0.90466(14) 0.16938(17) 0.0818(12) Uani 1 d . . . HD1A_15 H 0.1373 0.8884 0.1742 0.123 Uiso 1 calc R . . HD1B_15 H 0.1675 0.9245 0.1953 0.123 Uiso 1 calc R . . HD1C_15 H 0.1990 0.8896 0.1725 0.123 Uiso 1 calc R . . CD2_15 C 0.1601(2) 0.89243(15) 0.07391(19) 0.0884(14) Uani 1 d . . . HD2A_15 H 0.1910 0.8765 0.0739 0.133 Uiso 1 calc R . . HD2B_15 H 0.1563 0.9045 0.0406 0.133 Uiso 1 calc R . . HD2C_15 H 0.1297 0.8768 0.0810 0.133 Uiso 1 calc R . . C_15 C 0.26593(14) 1.00733(11) 0.12382(13) 0.0588(8) Uani 1 d . . . O_15 O 0.25976(10) 1.02610(7) 0.08276(9) 0.0608(6) Uani 1 d . . . N_21 N 0.33784(13) 1.05070(10) 0.42967(12) 0.0644(7) Uani 1 d . . . H0_21 H 0.3426 1.0715 0.4122 0.077 Uiso 1 calc R . . CA_21 C 0.38266(15) 1.02639(11) 0.44192(14) 0.0608(8) Uani 1 d . . . HA_21 H 0.3862 1.0251 0.4798 0.073 Uiso 1 calc R . . CB_21 C 0.43288(17) 1.04496(13) 0.41970(18) 0.0722(10) Uani 1 d . . . HB1_21 H 0.4291 1.0476 0.3824 0.087 Uiso 1 calc R . . HB2_21 H 0.4367 1.0706 0.4342 0.087 Uiso 1 calc R . . CG_21 C 0.48204(18) 1.02210(15) 0.4311(2) 0.0811(11) Uani 1 d . . . CD1_21 C 0.5085(2) 0.99998(17) 0.3975(3) 0.1028(17) Uani 1 d . . . HD1_21 H 0.4997 0.9957 0.3629 0.123 Uiso 1 calc R . . NE1_21 N 0.55251(18) 0.98406(15) 0.4241(3) 0.122(2) Uani 1 d . . . HE1_21 H 0.5752 0.9686 0.4107 0.146 Uiso 1 calc R . . CE2_21 C 0.5533(2) 0.99707(19) 0.4738(3) 0.1036(17) Uani 1 d . . . CZ2_21 C 0.5910(3) 0.9883(3) 0.5079(5) 0.141(3) Uani 1 d . . . HZ2_21 H 0.6196 0.9725 0.5004 0.169 Uiso 1 calc R . . CH2_21 C 0.5823(4) 1.0058(4) 0.5569(5) 0.168(5) Uani 1 d . . . HH2_21 H 0.6068 1.0015 0.5832 0.202 Uiso 1 calc R . . CZ3_21 C 0.5384(3) 1.0295(3) 0.5680(3) 0.133(3) Uani 1 d . . . HZ3_21 H 0.5342 1.0398 0.6011 0.160 Uiso 1 calc R . . CE3_21 C 0.5013(2) 1.0374(2) 0.5295(2) 0.1058(18) Uani 1 d . . . HE3_21 H 0.4724 1.0532 0.5357 0.127 Uiso 1 calc R . . CD2_21 C 0.51011(19) 1.01987(17) 0.4794(3) 0.0980(16) Uani 1 d . . . C_21 C 0.37520(14) 0.98557(11) 0.42154(14) 0.0592(8) Uani 1 d . . . O_21 O 0.38699(10) 0.95726(8) 0.44856(10) 0.0637(6) Uani 1 d . . . N_22 N 0.35588(12) 0.98252(9) 0.37312(11) 0.0592(7) Uani 1 d . . . H0_22 H 0.3552 1.0026 0.3536 0.071 Uiso 1 calc R . . CA_22 C 0.33623(14) 0.94665(11) 0.35282(13) 0.0583(8) Uani 1 d . . . HA_22 H 0.3429 0.9266 0.3788 0.070 Uiso 1 calc R . . CB_22 C 0.36357(15) 0.93435(12) 0.30202(14) 0.0620(8) Uani 1 d . . . HB1_22 H 0.4007 0.9403 0.3053 0.074 Uiso 1 calc R . . HB2_22 H 0.3606 0.9066 0.2991 0.074 Uiso 1 calc R . . CG_22 C 0.34404(15) 0.95182(11) 0.25168(14) 0.0618(8) Uani 1 d . . . OD1_22 O 0.31655(10) 0.98153(8) 0.25295(10) 0.0641(6) Uani 1 d . . . OD2_22 O 0.35674(13) 0.93395(9) 0.21073(10) 0.0777(8) Uani 1 d . . . C_22 C 0.27669(14) 0.95034(11) 0.34636(13) 0.0585(8) Uani 1 d . . . O_22 O 0.25490(9) 0.98254(7) 0.35108(9) 0.0599(6) Uani 1 d . . . N_23 N 0.24698(12) 0.91948(9) 0.33481(12) 0.0609(7) Uani 1 d . . . CA_23 C 0.19078(14) 0.92389(11) 0.32348(15) 0.0612(8) Uani 1 d . . . HA_23 H 0.1864 0.9360 0.2893 0.073 Uiso 1 calc R . . CB_23 C 0.17028(16) 0.88284(11) 0.32151(15) 0.0650(8) Uani 1 d . . . HB1_23 H 0.1431 0.8802 0.2952 0.078 Uiso 1 calc R . . HB2_23 H 0.1558 0.8753 0.3549 0.078 Uiso 1 calc R . . CG_23 C 0.21826(16) 0.85835(13) 0.30786(17) 0.0698(9) Uani 1 d . . . HG1_23 H 0.2138 0.8319 0.3193 0.084 Uiso 1 calc R . . HG2_23 H 0.2250 0.8586 0.2708 0.084 Uiso 1 calc R . . CD_23 C 0.26213(16) 0.87814(12) 0.33751(17) 0.0686(9) Uani 1 d . . . HD1_23 H 0.2636 0.8693 0.3732 0.082 Uiso 1 calc R . . HD2_23 H 0.2960 0.8737 0.3211 0.082 Uiso 1 calc R . . C_23 C 0.16423(14) 0.94863(11) 0.36463(14) 0.0612(8) Uani 1 d . . . O_23 O 0.16550(10) 0.93867(8) 0.41083(9) 0.0637(6) Uani 1 d . . . N_24 N 0.13760(12) 0.97968(9) 0.34845(11) 0.0607(7) Uani 1 d . . . H0_24 H 0.1280 0.9814 0.3165 0.073 Uiso 1 calc R . . CA_24 C 0.12468(15) 1.01068(11) 0.38481(14) 0.0616(8) Uani 1 d . . . HA_24 H 0.1236 1.0002 0.4202 0.074 Uiso 1 calc R . . CB_24 C 0.07164(16) 1.02956(13) 0.37233(16) 0.0711(10) Uani 1 d . . . HB_24 H 0.0735 1.0401 0.3371 0.085 Uiso 1 calc R . . CG1_24 C 0.02766(17) 1.00062(15) 0.37388(19) 0.0815(11) Uani 1 d . . . HG1A_24 H 0.0342 0.9808 0.3487 0.122 Uiso 1 calc R . . HG1B_24 H -0.0050 1.0132 0.3660 0.122 Uiso 1 calc R . . HG1C_24 H 0.0257 0.9894 0.4079 0.122 Uiso 1 calc R . . CG2_24 C 0.06169(19) 1.06283(16) 0.4099(2) 0.0867(13) Uani 1 d . . . HG2A_24 H 0.0287 1.0748 0.4017 0.130 Uiso 1 calc R . . HG2B_24 H 0.0895 1.0814 0.4067 0.130 Uiso 1 calc R . . HG2C_24 H 0.0607 1.0532 0.4448 0.130 Uiso 1 calc R . . C_24 C 0.17045(14) 1.03935(11) 0.38058(13) 0.0591(8) Uani 1 d . . . O_24 O 0.18242(10) 1.05339(8) 0.33824(9) 0.0611(6) Uani 1 d . . . N_25 N 0.19644(13) 1.04647(10) 0.42487(12) 0.0639(7) Uani 1 d . . . H0_25 H 0.1836 1.0379 0.4535 0.077 Uiso 1 calc R . . CA_25 C 0.24579(15) 1.06829(11) 0.42653(15) 0.0634(8) Uani 1 d . . . HA_25 H 0.2543 1.0769 0.3912 0.076 Uiso 1 calc R . . CB_25 C 0.24285(19) 1.10330(13) 0.46172(17) 0.0748(10) Uani 1 d . . . HB1_25 H 0.2779 1.1140 0.4652 0.090 Uiso 1 calc R . . HB2_25 H 0.2316 1.0950 0.4959 0.090 Uiso 1 calc R . . CG_25 C 0.2057(2) 1.13525(15) 0.4431(2) 0.0861(13) Uani 1 d . . . HG_25 H 0.1702 1.1243 0.4409 0.103 Uiso 1 calc R . . CD1_25 C 0.2203(2) 1.15065(15) 0.3894(2) 0.0943(15) Uani 1 d . . . HD1A_25 H 0.2565 1.1585 0.3893 0.141 Uiso 1 calc R . . HD1B_25 H 0.1984 1.1723 0.3812 0.141 Uiso 1 calc R . . HD1C_25 H 0.2151 1.1308 0.3639 0.141 Uiso 1 calc R . . CD2_25 C 0.2047(3) 1.1675(2) 0.4843(3) 0.126(2) Uani 1 d . . . HD2A_25 H 0.2001 1.1564 0.5182 0.189 Uiso 1 calc R . . HD2B_25 H 0.1760 1.1848 0.4772 0.189 Uiso 1 calc R . . HD2C_25 H 0.2373 1.1815 0.4833 0.189 Uiso 1 calc R . . C_25 C 0.28936(15) 1.04120(11) 0.44522(13) 0.0600(8) Uani 1 d . . . O_25 O 0.28075(10) 1.01371(8) 0.47454(10) 0.0653(6) Uani 1 d . . . N_31 N -0.11279(12) 0.74181(9) 0.59411(11) 0.0599(7) Uani 1 d . . . H0_31 H -0.0966 0.7622 0.6043 0.072 Uiso 1 calc R . . CA_31 C -0.12536(15) 0.71193(11) 0.63170(14) 0.0623(8) Uani 1 d . . . HA_31 H -0.1637 0.7087 0.6329 0.075 Uiso 1 calc R . . CB_31 C -0.10599(17) 0.72463(13) 0.68588(14) 0.0676(9) Uani 1 d . . . HB1_31 H -0.0678 0.7256 0.6859 0.081 Uiso 1 calc R . . HB2_31 H -0.1190 0.7504 0.6931 0.081 Uiso 1 calc R . . CG_31 C -0.12389(18) 0.69812(13) 0.72751(15) 0.0718(10) Uani 1 d . . . CD1_31 C -0.10178(19) 0.66385(13) 0.74156(16) 0.0762(10) Uani 1 d . . . HD1_31 H -0.0711 0.6537 0.7274 0.091 Uiso 1 calc R . . NE1_31 N -0.13166(17) 0.64617(11) 0.78017(14) 0.0788(9) Uani 1 d . . . HE1_31 H -0.1247 0.6245 0.7949 0.095 Uiso 1 calc R . . CE2_31 C -0.17419(19) 0.66938(13) 0.79048(16) 0.0751(10) Uani 1 d . . . CZ2_31 N -0.2146(2) 0.66470(16) 0.82602(19) 0.1059(14) Uani 1 d . . . HZ2_31 H -0.2154 0.6451 0.8465 0.127 Uiso 1 calc R . . CH2_31 C -0.2531(2) 0.69210(19) 0.8276(2) 0.1002(16) Uani 1 d . . . HH2_31 H -0.2810 0.6892 0.8508 0.120 Uiso 1 calc R . . CZ3_31 C -0.2517(2) 0.72426(18) 0.7953(2) 0.0936(14) Uani 1 d . . . HZ3_31 H -0.2789 0.7422 0.7969 0.112 Uiso 1 calc R . . CE3_31 C -0.2106(2) 0.73005(16) 0.7609(2) 0.0848(12) Uani 1 d . . . HE3_31 H -0.2096 0.7518 0.7400 0.102 Uiso 1 calc R . . CD2_31 C -0.17043(18) 0.70238(13) 0.75840(16) 0.0728(10) Uani 1 d . . . C_31 C -0.10037(14) 0.67347(12) 0.61581(14) 0.0615(8) Uani 1 d . . . O_31 O -0.12463(10) 0.64283(8) 0.62238(10) 0.0648(6) Uani 1 d . . . N_32 N -0.05161(11) 0.67486(9) 0.59670(12) 0.0592(7) Uani 1 d . . . H0_32 H -0.0326 0.6950 0.6018 0.071 Uiso 1 calc R . . CA_32 C -0.03010(14) 0.64261(11) 0.56718(13) 0.0599(8) Uani 1 d . . . HA_32 H -0.0564 0.6219 0.5678 0.072 Uiso 1 calc R . . CB_32 C 0.02020(15) 0.62667(12) 0.59106(16) 0.0657(9) Uani 1 d . . . HB1_32 H 0.0299 0.6035 0.5722 0.079 Uiso 1 calc R . . HB2_32 H 0.0127 0.6192 0.6266 0.079 Uiso 1 calc R . . CG_32 C 0.06780(16) 0.65377(14) 0.59158(17) 0.0734(10) Uani 1 d . . . OD1_32 O 0.06547(11) 0.68500(10) 0.57049(11) 0.0766(7) Uani 1 d . . . OD2_32 O 0.10847(15) 0.64099(12) 0.6138(2) 0.1258(17) Uani 1 d . . . C_32 C -0.02370(13) 0.65515(11) 0.51140(13) 0.0562(7) Uani 1 d . . . O_32 O -0.02579(10) 0.68996(8) 0.49938(9) 0.0615(6) Uani 1 d . . . N_33 N -0.01410(11) 0.62903(8) 0.47488(12) 0.0566(6) Uani 1 d . . . CA_33 C -0.00469(14) 0.64156(11) 0.42097(14) 0.0595(8) Uani 1 d . . . HA_33 H 0.0307 0.6527 0.4181 0.071 Uiso 1 calc R . . CB_33 C -0.00756(16) 0.60446(12) 0.38955(15) 0.0662(9) Uani 1 d . . . HB1_33 H 0.0275 0.5953 0.3809 0.079 Uiso 1 calc R . . HB2_33 H -0.0271 0.6085 0.3576 0.079 Uiso 1 calc R . . CG_33 C -0.03591(16) 0.57566(12) 0.42462(16) 0.0680(9) Uani 1 d . . . HG1_33 H -0.0738 0.5781 0.4212 0.082 Uiso 1 calc R . . HG2_33 H -0.0257 0.5495 0.4163 0.082 Uiso 1 calc R . . CD_33 C -0.01832(16) 0.58643(11) 0.47840(15) 0.0640(8) Uani 1 d . . . HD1_33 H -0.0441 0.5788 0.5042 0.077 Uiso 1 calc R . . HD2_33 H 0.0154 0.5748 0.4868 0.077 Uiso 1 calc R . . C_33 C -0.04563(14) 0.67139(12) 0.40482(14) 0.0603(8) Uani 1 d . . . O_33 O -0.09323(9) 0.66533(8) 0.41099(10) 0.0611(6) Uani 1 d . . . N_34 N -0.02565(12) 0.70285(9) 0.38119(12) 0.0611(7) Uani 1 d . . . H0_34 H 0.0061 0.7029 0.3695 0.073 Uiso 1 calc R . . CA_34 C -0.05896(14) 0.73676(11) 0.37596(14) 0.0617(8) Uani 1 d . . . HA_34 H -0.0951 0.7285 0.3686 0.074 Uiso 1 calc R . . CB_34 C -0.04033(16) 0.76442(12) 0.33237(15) 0.0676(9) Uani 1 d . . . HB_34 H -0.0046 0.7731 0.3410 0.081 Uiso 1 calc R . . CG1_34 C -0.03807(17) 0.74372(14) 0.28034(15) 0.0729(10) Uani 1 d . . . HG1A_34 H -0.0727 0.7352 0.2709 0.109 Uiso 1 calc R . . HG1B_34 H -0.0150 0.7219 0.2830 0.109 Uiso 1 calc R . . HG1C_34 H -0.0250 0.7610 0.2542 0.109 Uiso 1 calc R . . CG2_34 C -0.0754(2) 0.79919(14) 0.3308(2) 0.0867(13) Uani 1 d . . . HG2A_34 H -0.0649 0.8156 0.3026 0.130 Uiso 1 calc R . . HG2B_34 H -0.0725 0.8130 0.3629 0.130 Uiso 1 calc R . . HG2C_34 H -0.1112 0.7912 0.3258 0.130 Uiso 1 calc R . . C_34 C -0.05749(14) 0.75693(11) 0.42843(14) 0.0587(8) Uani 1 d . . . O_34 O -0.01535(9) 0.77133(8) 0.44506(10) 0.0617(6) Uani 1 d . . . N_35 N -0.10202(11) 0.75658(9) 0.45590(12) 0.0603(7) Uani 1 d . . . H0_35 H -0.1299 0.7475 0.4414 0.072 Uiso 1 calc R . . CA_35 C -0.10594(14) 0.77068(11) 0.50895(14) 0.0605(8) Uani 1 d . . . HA_35 H -0.0708 0.7783 0.5207 0.073 Uiso 1 calc R . . CB_35 C -0.14221(15) 0.80569(12) 0.51218(16) 0.0655(9) Uani 1 d . . . HB1_35 H -0.1481 0.8119 0.5484 0.079 Uiso 1 calc R . . HB2_35 H -0.1760 0.7991 0.4970 0.079 Uiso 1 calc R . . CG_35 C -0.12029(16) 0.84152(13) 0.48430(19) 0.0729(10) Uani 1 d . . . HG_35 H -0.1126 0.8342 0.4483 0.088 Uiso 1 calc R . . CD1_35 C -0.1608(2) 0.87326(15) 0.4830(2) 0.0914(14) Uani 1 d . . . HD1A_35 H -0.1703 0.8802 0.5178 0.137 Uiso 1 calc R . . HD1B_35 H -0.1915 0.8645 0.4647 0.137 Uiso 1 calc R . . HD1C_35 H -0.1464 0.8953 0.4655 0.137 Uiso 1 calc R . . CD2_35 C -0.06871(18) 0.85507(14) 0.5092(2) 0.0812(12) Uani 1 d . . . HD2A_35 H -0.0539 0.8755 0.4888 0.122 Uiso 1 calc R . . HD2B_35 H -0.0443 0.8340 0.5107 0.122 Uiso 1 calc R . . HD2C_35 H -0.0756 0.8642 0.5438 0.122 Uiso 1 calc R . . C_35 C -0.12581(13) 0.73825(11) 0.54393(14) 0.0584(8) Uani 1 d . . . O_35 O -0.15347(9) 0.71162(7) 0.52749(10) 0.0612(6) Uani 1 d . . . N_41 N 0.17701(13) 0.71027(10) 0.58329(12) 0.0658(7) Uani 1 d . . . H0_41 H 0.1552 0.6914 0.5860 0.079 Uiso 1 calc R . . CA_41 C 0.19206(16) 0.73146(11) 0.62964(15) 0.0654(9) Uani 1 d . . . HA_41 H 0.2306 0.7323 0.6314 0.078 Uiso 1 calc R . . CB_41 C 0.1715(2) 0.71017(13) 0.67793(16) 0.0752(10) Uani 1 d . . . HB1_41 H 0.1334 0.7083 0.6756 0.090 Uiso 1 calc R . . HB2_41 H 0.1854 0.6842 0.6777 0.090 Uiso 1 calc R . . CG_41 C 0.18533(19) 0.72864(14) 0.72826(17) 0.0776(11) Uani 1 d . . . CD1_41 C 0.1563(2) 0.75210(15) 0.75893(18) 0.0842(12) Uani 1 d . . . HD1_41 H 0.1228 0.7610 0.7508 0.101 Uiso 1 calc R . . NE1_41 N 0.1830(2) 0.76086(12) 0.80343(15) 0.0901(12) Uani 1 d . . . HE1_41 H 0.1712 0.7751 0.8281 0.108 Uiso 1 calc R . . CE2_41 C 0.2311(2) 0.74369(15) 0.80302(19) 0.0868(13) Uani 1 d . . . CZ2_41 C 0.2719(3) 0.74373(19) 0.8393(2) 0.109(2) Uani 1 d . . . HZ2_41 H 0.2688 0.7566 0.8708 0.131 Uiso 1 calc R . . CH2_41 C 0.3174(3) 0.7237(2) 0.8264(3) 0.1124(19) Uani 1 d . . . HH2_41 H 0.3459 0.7241 0.8491 0.135 Uiso 1 calc R . . CZ3_41 C 0.3213(3) 0.7033(2) 0.7814(3) 0.1068(17) Uani 1 d . . . HZ3_41 H 0.3518 0.6895 0.7745 0.128 Uiso 1 calc R . . CE3_41 C 0.2806(2) 0.70288(16) 0.7461(2) 0.0890(13) Uani 1 d . . . HE3_41 H 0.2840 0.6887 0.7155 0.107 Uiso 1 calc R . . CD2_41 C 0.2351(2) 0.72322(14) 0.75556(18) 0.0805(12) Uani 1 d . . . C_41 C 0.17141(14) 0.77289(11) 0.62622(13) 0.0603(8) Uani 1 d . . . O_41 O 0.20100(10) 0.80078(8) 0.63072(11) 0.0673(6) Uani 1 d . . . N_42 N 0.11905(12) 0.77652(10) 0.61892(13) 0.0654(7) Uani 1 d . . . H0_42 H 0.0991 0.7568 0.6239 0.078 Uiso 1 calc R . . CA_42 C 0.09534(15) 0.81259(12) 0.60303(14) 0.0625(8) Uani 1 d . . . HA_42 H 0.1192 0.8336 0.6126 0.075 Uiso 1 calc R . . CB_42 C 0.04252(15) 0.81937(12) 0.62990(15) 0.0646(8) Uani 1 d . . . HB1_42 H 0.0478 0.8176 0.6671 0.078 Uiso 1 calc R . . HB2_42 H 0.0311 0.8454 0.6223 0.078 Uiso 1 calc R . . CG_42 C -0.00132(14) 0.79182(11) 0.61466(14) 0.0614(8) Uani 1 d . . . OD1_42 O 0.00990(11) 0.76280(9) 0.58936(11) 0.0725(7) Uani 1 d . . . OD2_42 O -0.04771(11) 0.80027(9) 0.62897(12) 0.0744(7) Uani 1 d . . . C_42 C 0.09020(13) 0.81184(11) 0.54412(14) 0.0582(8) Uani 1 d . . . O_42 O 0.09850(10) 0.78210(8) 0.51866(10) 0.0623(6) Uani 1 d . . . N_43 N 0.07512(11) 0.84447(9) 0.51940(11) 0.0593(7) Uani 1 d . . . CA_43 C 0.06618(14) 0.84435(11) 0.46257(13) 0.0585(8) Uani 1 d . . . HA_43 H 0.0319 0.8326 0.4550 0.070 Uiso 1 calc R . . CB_43 C 0.06469(16) 0.88698(11) 0.44801(15) 0.0648(8) Uani 1 d . . . HB1_43 H 0.0289 0.8952 0.4412 0.078 Uiso 1 calc R . . HB2_43 H 0.0858 0.8918 0.4173 0.078 Uiso 1 calc R . . CG_43 C 0.08762(17) 0.90855(13) 0.49562(16) 0.0698(9) Uani 1 d . . . HG1_43 H 0.1257 0.9102 0.4937 0.084 Uiso 1 calc R . . HG2_43 H 0.0731 0.9343 0.4984 0.084 Uiso 1 calc R . . CD_43 C 0.07044(16) 0.88363(12) 0.54068(15) 0.0651(8) Uani 1 d . . . HD1_43 H 0.0933 0.8871 0.5705 0.078 Uiso 1 calc R . . HD2_43 H 0.0345 0.8893 0.5508 0.078 Uiso 1 calc R . . C_43 C 0.10981(14) 0.82152(11) 0.43486(14) 0.0610(8) Uani 1 d . . . O_43 O 0.15699(9) 0.83054(8) 0.43962(10) 0.0623(6) Uani 1 d . . . N_44 N 0.09204(12) 0.79428(9) 0.40242(11) 0.0594(7) Uani 1 d . . . H0_44 H 0.0594 0.7943 0.3937 0.071 Uiso 1 calc R . . CA_44 C 0.12712(15) 0.76434(11) 0.38143(15) 0.0636(8) Uani 1 d . . . HA_44 H 0.1630 0.7747 0.3795 0.076 Uiso 1 calc R . . CB_44 C 0.11107(16) 0.75040(13) 0.32811(15) 0.0694(9) Uani 1 d . . . HB_44 H 0.0766 0.7379 0.3313 0.083 Uiso 1 calc R . . CG1_44 C 0.1505(2) 0.72027(16) 0.30914(19) 0.0850(12) Uani 1 d . . . HG1A_44 H 0.1848 0.7317 0.3065 0.127 Uiso 1 calc R . . HG1B_44 H 0.1398 0.7109 0.2757 0.127 Uiso 1 calc R . . HG1C_44 H 0.1516 0.6992 0.3333 0.127 Uiso 1 calc R . . CG2_44 C 0.10582(18) 0.78293(14) 0.28922(16) 0.0748(10) Uani 1 d . . . HG2A_44 H 0.0828 0.8024 0.3030 0.112 Uiso 1 calc R . . HG2B_44 H 0.0915 0.7731 0.2574 0.112 Uiso 1 calc R . . HG2C_44 H 0.1399 0.7939 0.2827 0.112 Uiso 1 calc R . . C_44 C 0.12595(14) 0.73190(11) 0.42160(14) 0.0613(8) Uani 1 d . . . O_44 O 0.08375(10) 0.71462(8) 0.43004(10) 0.0628(6) Uani 1 d . . . N_45 N 0.17061(12) 0.72427(10) 0.44674(12) 0.0632(7) Uani 1 d . . . H0_45 H 0.1992 0.7354 0.4368 0.076 Uiso 1 calc R . . CA_45 C 0.17256(15) 0.69750(12) 0.49088(15) 0.0636(8) Uani 1 d . . . HA_45 H 0.1365 0.6901 0.4999 0.076 Uiso 1 calc R . . CB_45 C 0.20380(15) 0.66110(13) 0.47895(18) 0.0712(10) Uani 1 d . . . HB1_45 H 0.2378 0.6685 0.4650 0.085 Uiso 1 calc R . . HB2_45 H 0.2101 0.6475 0.5113 0.085 Uiso 1 calc R . . CG_45 C 0.17797(18) 0.63372(14) 0.4412(2) 0.0810(11) Uani 1 d . . . HG_45 H 0.1683 0.6478 0.4096 0.097 Uiso 1 calc R . . CD1_45 C 0.12803(19) 0.61589(15) 0.4657(2) 0.0881(13) Uani 1 d . . . HD1A_45 H 0.1372 0.6031 0.4975 0.132 Uiso 1 calc R . . HD1B_45 H 0.1130 0.5976 0.4420 0.132 Uiso 1 calc R . . HD1C_45 H 0.1029 0.6359 0.4728 0.132 Uiso 1 calc R . . CD2_45 C 0.2149(2) 0.60109(19) 0.4272(3) 0.112(2) Uani 1 d . . . HD2A_45 H 0.2421 0.6106 0.4047 0.168 Uiso 1 calc R . . HD2B_45 H 0.1956 0.5811 0.4098 0.168 Uiso 1 calc R . . HD2C_45 H 0.2305 0.5909 0.4583 0.168 Uiso 1 calc R . . C_45 C 0.19624(14) 0.71927(12) 0.53635(15) 0.0644(9) Uani 1 d . . . O_45 O 0.23170(12) 0.74266(10) 0.52988(11) 0.0828(9) Uani 1 d . . . O1_51 O 0.1285(2) 0.81273(11) 0.87363(15) 0.1118(13) Uani 1 d D . . H1_51 H 0.1491 0.8306 0.8782 0.168 Uiso 1 calc R . . C1_51 C 0.1031(4) 0.8043(2) 0.9198(3) 0.142(3) Uani 1 d D . . H1A_51 H 0.0672 0.8124 0.9113 0.170 Uiso 1 calc R . . C2_51 C 0.1128(7) 0.8268(3) 0.9639(3) 0.208(6) Uani 1 d D . . H2A_51 H 0.1499 0.8273 0.9709 0.313 Uiso 1 calc R . . H2B_51 H 0.0945 0.8161 0.9932 0.313 Uiso 1 calc R . . H2C_51 H 0.1006 0.8526 0.9580 0.313 Uiso 1 calc R . . C3_51 C 0.0953(7) 0.7627(3) 0.9264(5) 0.225(7) Uani 1 d D . . H3A_51 H 0.0647 0.7548 0.9073 0.337 Uiso 1 calc R . . H3B_51 H 0.0905 0.7570 0.9626 0.337 Uiso 1 calc R . . H3C_51 H 0.1257 0.7492 0.9137 0.337 Uiso 1 calc R . . O1_52 O 0.12926(19) 0.56663(16) 0.6188(3) 0.160(2) Uani 1 d D . . H1_52 H 0.1293 0.5854 0.5994 0.240 Uiso 1 calc R . . C1_52 C 0.1802(3) 0.5594(3) 0.6355(5) 0.166(4) Uani 1 d D . . H1A_52 H 0.1792 0.5647 0.6729 0.199 Uiso 1 calc R . . C2_52 C 0.2207(4) 0.5865(5) 0.6148(8) 0.249(9) Uani 1 d D . . H2A_52 H 0.2332 0.5773 0.5819 0.373 Uiso 1 calc R . . H2B_52 H 0.2495 0.5881 0.6388 0.373 Uiso 1 calc R . . H2C_52 H 0.2053 0.6116 0.6104 0.373 Uiso 1 calc R . . C3_52 C 0.1912(7) 0.5171(4) 0.6321(11) 0.376(18) Uani 1 d D . . H3A_52 H 0.1601 0.5030 0.6413 0.563 Uiso 1 calc R . . H3B_52 H 0.2192 0.5106 0.6555 0.563 Uiso 1 calc R . . H3C_52 H 0.2014 0.5107 0.5972 0.563 Uiso 1 calc R . . O1_53 O -0.09240(19) 0.86232(13) 0.6695(3) 0.150(2) Uani 1 d D . . H1_53 H -0.0818 0.8415 0.6575 0.224 Uiso 1 d . . . C1_53 C -0.1474(3) 0.8628(3) 0.6673(5) 0.178(5) Uani 1 d D . . H1A_53 H -0.1526 0.8707 0.6310 0.213 Uiso 1 calc R . . C2_53 C -0.1661(3) 0.8987(2) 0.6947(5) 0.171(4) Uani 1 d D . . H2A_53 H -0.1491 0.9006 0.7280 0.257 Uiso 1 calc R . . H2B_53 H -0.2035 0.8975 0.6994 0.257 Uiso 1 calc R . . H2C_53 H -0.1574 0.9209 0.6742 0.257 Uiso 1 calc R . . C3_53 C -0.1794(3) 0.8297(2) 0.6688(4) 0.130(2) Uani 1 d D . . H3A_53 H -0.1647 0.8103 0.6466 0.195 Uiso 1 calc R . . H3B_53 H -0.2142 0.8361 0.6570 0.195 Uiso 1 calc R . . H3C_53 H -0.1811 0.8202 0.7038 0.195 Uiso 1 calc R . . O1_54 O 0.0497(4) 0.8008(3) 0.7872(4) 0.221(4) Uani 1 d D . . H1_54 H 0.0728 0.8125 0.8030 0.331 Uiso 1 calc R . . C1_54 C 0.0008(5) 0.8152(4) 0.8012(5) 0.189(5) Uani 1 d D . . H1A_54 H -0.0056 0.8137 0.8387 0.226 Uiso 1 calc R . . C2_54 C -0.0385(5) 0.7936(4) 0.7705(5) 0.197(5) Uani 1 d D . . H2A_54 H -0.0302 0.7957 0.7342 0.295 Uiso 1 calc R . . H2B_54 H -0.0729 0.8040 0.7767 0.295 Uiso 1 calc R . . H2C_54 H -0.0378 0.7669 0.7806 0.295 Uiso 1 calc R . . C3_54 C -0.0030(8) 0.8575(4) 0.7799(10) 0.329(16) Uani 1 d D . . H3A_54 H -0.0047 0.8752 0.8085 0.493 Uiso 1 calc R . . H3B_54 H -0.0340 0.8600 0.7589 0.493 Uiso 1 calc R . . H3C_54 H 0.0275 0.8630 0.7592 0.493 Uiso 1 calc R . . O1_55 O 0.36303(14) 0.93046(10) 0.10321(12) 0.0887(9) Uani 1 d D . . H1_55 H 0.3568 0.9338 0.1341 0.133 Uiso 1 calc R . . C1_55 C 0.3982(2) 0.89778(17) 0.09724(19) 0.0930(14) Uani 1 d D . . H1A_55 H 0.3803 0.8747 0.1104 0.112 Uiso 1 calc R . . C2_55 C 0.4079(3) 0.8927(2) 0.0401(2) 0.122(2) Uani 1 d D . . H2A_55 H 0.3758 0.8972 0.0214 0.183 Uiso 1 calc R . . H2B_55 H 0.4200 0.8670 0.0336 0.183 Uiso 1 calc R . . H2C_55 H 0.4341 0.9108 0.0289 0.183 Uiso 1 calc R . . C3_55 C 0.4495(3) 0.9027(2) 0.1267(3) 0.1136(19) Uani 1 d D . . H3A_55 H 0.4673 0.9253 0.1144 0.170 Uiso 1 calc R . . H3B_55 H 0.4713 0.8806 0.1212 0.170 Uiso 1 calc R . . H3C_55 H 0.4422 0.9055 0.1631 0.170 Uiso 1 calc R . . O1_56 O 0.0716(5) 0.6290(3) 0.7265(4) 0.279(7) Uani 1 d D . . H1_56 H 0.0783 0.6328 0.6958 0.418 Uiso 1 calc R . . C1_56 C 0.0719(7) 0.6641(5) 0.7533(5) 0.261(11) Uani 1 d D . . H1A_56 H 0.1079 0.6742 0.7514 0.314 Uiso 1 calc R . . C2_56 C 0.0365(5) 0.6935(6) 0.7277(9) 0.279(12) Uani 1 d D . . H2A_56 H 0.0567 0.7088 0.7039 0.419 Uiso 1 calc R . . H2B_56 H 0.0213 0.7099 0.7538 0.419 Uiso 1 calc R . . H2C_56 H 0.0089 0.6805 0.7092 0.419 Uiso 1 calc R . . C3_56 C 0.0596(8) 0.6587(7) 0.8086(6) 0.322(13) Uani 1 d D . . H3A_56 H 0.0226 0.6539 0.8126 0.483 Uiso 1 calc R . . H3B_56 H 0.0691 0.6815 0.8276 0.483 Uiso 1 calc R . . H3C_56 H 0.0792 0.6371 0.8218 0.483 Uiso 1 calc R . . O1_57 O 0.0992(5) 0.5532(4) 0.7601(5) 0.190(7) Uani 0.546(14) d PD . . H1_57 H 0.0918 0.5756 0.7535 0.285 Uiso 0.546(14) calc PR . . C1_57 C 0.0630(6) 0.5281(5) 0.7342(7) 0.161(7) Uani 0.546(14) d PD . . H1A_57 H 0.0638 0.5338 0.6969 0.193 Uiso 0.546(14) calc PR . . C2_57 C 0.0079(4) 0.5372(4) 0.7551(6) 0.124(5) Uani 0.546(14) d PD . . H2A_57 H 0.0085 0.5371 0.7923 0.187 Uiso 0.546(14) calc PR . . H2B_57 H -0.0165 0.5180 0.7430 0.187 Uiso 0.546(14) calc PR . . H2C_57 H -0.0030 0.5621 0.7429 0.187 Uiso 0.546(14) calc PR . . C3_57 C 0.0752(10) 0.4857(6) 0.7420(13) 0.259(19) Uani 0.546(14) d PD . . H3A_57 H 0.1076 0.4795 0.7248 0.388 Uiso 0.546(14) calc PR . . H3B_57 H 0.0472 0.4705 0.7276 0.388 Uiso 0.546(14) calc PR . . H3C_57 H 0.0784 0.4804 0.7784 0.388 Uiso 0.546(14) calc PR . . O1_58 O -0.0804(11) 0.9160(5) 0.3538(10) 0.42(2) Uani 0.75(2) d PD . . H1_58 H -0.1000 0.9346 0.3502 0.626 Uiso 0.75(2) calc PR . . C1_58 C -0.0479(8) 0.9122(6) 0.3093(8) 0.215(9) Uani 0.75(2) d PD . . H1A_58 H -0.0663 0.8907 0.2926 0.259 Uiso 0.75(2) calc PR . . C2_58 C -0.0603(8) 0.9418(6) 0.2719(9) 0.224(10) Uani 0.75(2) d PD . . H2A_58 H -0.0409 0.9648 0.2800 0.335 Uiso 0.75(2) calc PR . . H2B_58 H -0.0973 0.9472 0.2730 0.335 Uiso 0.75(2) calc PR . . H2C_58 H -0.0508 0.9331 0.2377 0.335 Uiso 0.75(2) calc PR . . C3_58 C 0.0056(8) 0.8947(7) 0.3120(8) 0.244(11) Uani 0.75(2) d PD . . H3A_58 H 0.0282 0.9108 0.3326 0.366 Uiso 0.75(2) calc PR . . H3B_58 H 0.0198 0.8924 0.2776 0.366 Uiso 0.75(2) calc PR . . H3C_58 H 0.0033 0.8697 0.3276 0.366 Uiso 0.75(2) calc PR . . O1_61 O 0.25022(11) 0.93634(8) 0.47283(10) 0.0681(6) Uani 1 d . . . O2_62 O 0.34888(11) 0.96517(8) 0.54955(10) 0.0673(6) Uani 1 d . . . O3_63 O 0.31296(10) 0.89348(8) 0.58534(10) 0.0659(6) Uani 1 d . . . O4_64 O -0.25205(10) 0.71483(9) 0.58296(11) 0.0707(6) Uani 1 d . . . O5_65 O 0.30217(10) 0.78253(8) 0.58705(10) 0.0663(6) Uani 1 d . . . O6_66 O 0.21873(11) 0.84480(8) 0.53109(11) 0.0724(7) Uani 1 d . . . O7_67 O 0.16060(11) 1.01800(9) 0.52218(10) 0.0715(7) Uani 1 d . . . O8_68 O 0.32547(15) 0.87735(10) 0.46972(12) 0.0883(9) Uani 1 d . . . O9_69 O 0.1796(5) 0.5251(4) 0.8202(5) 0.121(4) Uani 0.36 d P . . O10_70 O -0.0641(13) 0.7150(6) 0.8814(14) 0.231(15) Uani 0.31 d P . . O11_71 O -0.104(2) 0.7514(8) 0.8833(14) 0.20(2) Uani 0.16 d P . . O12_72 O 0.0718(6) 1.2099(11) 0.4180(11) 0.226(13) Uani 0.23 d P . . O13_73 O 0.5990(13) 1.1054(7) 0.4546(9) 0.269(13) Uani 0.25 d P . . O14_74 O 0.0469(11) 0.6427(6) 0.2648(7) 0.124(8) Uani 0.21 d P . . O15_75 O 0.1549(11) 0.5145(10) 0.8725(9) 0.221(18) Uani 0.23 d P . . O16_76 O -0.2003(8) 0.9886(7) 0.5969(11) 0.185(8) Uani 0.33 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 Na_1 0.0597(7) 0.0722(8) 0.0471(7) 0.0050(5) -0.0003(5) 0.0010(6) Na_2 0.0531(7) 0.0746(8) 0.0556(7) -0.0052(6) 0.0025(6) -0.0067(6) Na_3 0.0622(8) 0.0755(9) 0.0497(7) -0.0022(6) -0.0002(6) 0.0011(6) Na_4 0.0592(7) 0.0749(8) 0.0530(7) -0.0017(6) 0.0005(6) 0.0027(6) N_11 0.0561(16) 0.0737(18) 0.0465(15) 0.0036(12) 0.0001(12) -0.0034(13) CA_11 0.0564(19) 0.080(2) 0.0465(17) 0.0015(15) 0.0020(14) 0.0027(16) CB_11 0.0534(19) 0.087(3) 0.059(2) 0.0028(17) -0.0030(15) 0.0072(17) CG_11 0.056(2) 0.079(2) 0.071(2) 0.0092(18) -0.0049(17) 0.0053(17) CD1_11 0.065(2) 0.090(3) 0.082(3) 0.001(2) 0.000(2) 0.002(2) NE1_11 0.062(2) 0.081(2) 0.108(3) 0.012(2) -0.0097(19) -0.0050(16) CE2_11 0.063(2) 0.088(3) 0.077(3) 0.014(2) 0.0026(19) 0.0044(19) CZ2_11 0.064(3) 0.108(4) 0.106(4) 0.035(3) 0.008(2) 0.002(2) CH2_11 0.089(3) 0.128(4) 0.081(3) 0.012(3) 0.022(3) 0.003(3) CZ3_11 0.088(3) 0.133(4) 0.070(3) -0.004(3) 0.010(2) 0.011(3) CE3_11 0.070(2) 0.093(3) 0.068(2) 0.004(2) -0.0009(19) 0.006(2) CD2_11 0.060(2) 0.083(3) 0.066(2) 0.0103(18) 0.0000(17) 0.0107(18) C_11 0.0493(17) 0.075(2) 0.0471(18) 0.0033(14) 0.0033(13) -0.0017(14) O_11 0.0671(15) 0.0753(15) 0.0487(13) 0.0072(11) -0.0022(11) -0.0023(11) N_12 0.0568(16) 0.0761(19) 0.0485(15) 0.0009(12) -0.0008(12) 0.0054(13) CA_12 0.0563(19) 0.078(2) 0.0524(19) 0.0011(15) 0.0046(14) 0.0001(16) CB_12 0.063(2) 0.071(2) 0.0508(19) 0.0017(14) -0.0004(15) -0.0003(16) CG_12 0.060(2) 0.080(3) 0.0510(19) 0.0019(15) -0.0029(15) -0.0016(17) OD1_12 0.0712(16) 0.0704(16) 0.0513(13) 0.0016(10) -0.0036(11) -0.0082(12) OD2_12 0.0850(18) 0.0832(18) 0.0510(14) -0.0013(12) -0.0075(12) -0.0078(14) C_12 0.0560(18) 0.073(2) 0.0458(17) 0.0059(14) 0.0000(14) -0.0011(15) O_12 0.0561(13) 0.0765(17) 0.0499(13) 0.0039(10) 0.0001(10) -0.0002(11) N_13 0.0577(16) 0.0631(17) 0.0534(16) 0.0044(12) 0.0026(12) 0.0007(12) CA_13 0.0579(19) 0.076(2) 0.0493(18) 0.0048(14) 0.0051(14) 0.0047(16) CB_13 0.064(2) 0.076(2) 0.071(2) 0.0003(18) 0.0087(18) 0.0072(17) CG_13 0.068(2) 0.077(2) 0.071(2) 0.0070(18) 0.0017(18) 0.0066(18) CD_13 0.065(2) 0.066(2) 0.070(2) 0.0081(16) 0.0063(17) -0.0032(16) C_13 0.058(2) 0.078(2) 0.0495(19) 0.0051(15) 0.0053(14) 0.0044(16) O_13 0.0682(16) 0.0833(18) 0.0511(14) 0.0086(11) -0.0005(11) 0.0001(12) N_14 0.0593(16) 0.0726(18) 0.0459(15) 0.0036(12) 0.0016(12) -0.0002(13) CA_14 0.0572(19) 0.077(2) 0.0449(17) -0.0014(14) -0.0040(14) 0.0036(16) CB_14 0.060(2) 0.080(2) 0.059(2) 0.0034(16) 0.0013(16) -0.0012(16) CG1_14 0.071(2) 0.088(3) 0.079(3) -0.003(2) 0.002(2) -0.016(2) CG2_14 0.057(2) 0.093(3) 0.080(3) 0.014(2) 0.0014(18) 0.0015(19) C_14 0.0571(18) 0.075(2) 0.0435(17) 0.0020(14) -0.0010(14) -0.0033(15) O_14 0.0612(13) 0.0731(15) 0.0447(12) 0.0030(10) 0.0018(10) 0.0032(11) N_15 0.0588(16) 0.0756(18) 0.0419(14) 0.0031(12) -0.0006(12) 0.0025(13) CA_15 0.0600(19) 0.065(2) 0.0520(18) 0.0013(14) 0.0008(14) 0.0046(15) CB_15 0.071(2) 0.074(2) 0.0484(18) -0.0013(15) 0.0021(15) -0.0032(17) CG_15 0.072(2) 0.077(2) 0.058(2) -0.0048(16) 0.0041(17) -0.0066(17) CD1_15 0.095(3) 0.087(3) 0.064(2) 0.0084(19) 0.007(2) -0.008(2) CD2_15 0.092(3) 0.099(3) 0.074(3) -0.021(2) 0.015(2) -0.029(3) C_15 0.0580(19) 0.070(2) 0.0481(18) -0.0004(14) 0.0001(14) 0.0067(15) O_15 0.0631(14) 0.0727(15) 0.0466(12) 0.0051(10) -0.0002(10) -0.0001(11) N_21 0.0635(18) 0.0746(19) 0.0552(17) 0.0031(13) -0.0013(13) -0.0014(14) CA_21 0.061(2) 0.071(2) 0.0502(18) -0.0001(14) -0.0063(15) -0.0006(15) CB_21 0.067(2) 0.078(3) 0.071(2) 0.0054(18) -0.0049(18) -0.0083(18) CG_21 0.065(2) 0.091(3) 0.087(3) 0.009(2) 0.002(2) -0.009(2) CD1_21 0.067(3) 0.101(4) 0.141(5) 0.001(3) 0.010(3) -0.006(2) NE1_21 0.068(3) 0.087(3) 0.210(7) 0.015(4) 0.014(3) 0.002(2) CE2_21 0.078(3) 0.099(4) 0.134(5) 0.018(4) -0.008(3) -0.003(3) CZ2_21 0.078(4) 0.134(6) 0.210(10) 0.068(6) -0.016(5) -0.012(4) CH2_21 0.095(5) 0.202(10) 0.208(11) 0.105(9) -0.053(6) -0.034(6) CZ3_21 0.099(5) 0.199(8) 0.101(4) 0.038(5) -0.022(4) -0.036(5) CE3_21 0.085(3) 0.144(5) 0.088(4) 0.016(3) -0.012(3) -0.025(3) CD2_21 0.062(3) 0.105(4) 0.126(5) 0.032(3) -0.010(3) -0.012(2) C_21 0.0551(18) 0.073(2) 0.0498(18) 0.0011(15) -0.0043(14) -0.0033(15) O_21 0.0648(15) 0.0759(16) 0.0504(13) 0.0042(11) -0.0072(11) 0.0032(11) N_22 0.0589(16) 0.0693(18) 0.0493(15) 0.0033(12) -0.0016(12) -0.0022(12) CA_22 0.0571(19) 0.073(2) 0.0450(17) 0.0012(14) -0.0029(14) -0.0008(15) CB_22 0.0570(19) 0.081(2) 0.0476(18) 0.0049(15) -0.0026(14) 0.0028(16) CG_22 0.062(2) 0.073(2) 0.0511(19) 0.0026(15) 0.0032(15) 0.0027(16) OD1_22 0.0613(14) 0.0803(16) 0.0507(13) 0.0070(11) 0.0024(10) 0.0053(12) OD2_22 0.098(2) 0.0859(19) 0.0493(15) 0.0019(12) 0.0044(13) 0.0149(15) C_22 0.0553(19) 0.076(2) 0.0440(17) 0.0026(14) 0.0013(14) 0.0015(16) O_22 0.0570(13) 0.0756(16) 0.0471(12) 0.0040(10) 0.0024(10) 0.0038(11) N_23 0.0562(16) 0.0726(19) 0.0540(16) 0.0018(12) -0.0024(12) 0.0046(13) CA_23 0.0576(19) 0.072(2) 0.0540(19) 0.0018(15) -0.0006(15) -0.0016(15) CB_23 0.062(2) 0.073(2) 0.060(2) 0.0025(16) -0.0047(16) -0.0032(16) CG_23 0.065(2) 0.079(2) 0.066(2) -0.0024(18) -0.0063(17) 0.0010(18) CD_23 0.066(2) 0.069(2) 0.071(2) 0.0024(16) -0.0092(18) 0.0028(16) C_23 0.0545(19) 0.078(2) 0.0512(19) 0.0017(15) -0.0031(14) -0.0033(15) O_23 0.0597(14) 0.0815(16) 0.0500(13) 0.0106(11) 0.0026(10) -0.0029(11) N_24 0.0619(17) 0.0752(19) 0.0451(15) 0.0009(12) -0.0008(12) 0.0004(13) CA_24 0.061(2) 0.074(2) 0.0494(18) -0.0001(15) 0.0044(15) 0.0017(16) CB_24 0.061(2) 0.093(3) 0.059(2) 0.0000(18) 0.0053(17) 0.0070(19) CG1_24 0.062(2) 0.109(3) 0.073(3) -0.004(2) 0.0042(19) 0.004(2) CG2_24 0.068(3) 0.102(3) 0.090(3) -0.015(3) 0.003(2) 0.013(2) C_24 0.0579(19) 0.074(2) 0.0456(18) 0.0046(14) -0.0024(14) 0.0073(15) O_24 0.0606(14) 0.0771(15) 0.0455(12) 0.0028(10) -0.0004(10) 0.0030(11) N_25 0.0628(17) 0.084(2) 0.0444(15) 0.0041(13) 0.0014(12) 0.0018(14) CA_25 0.067(2) 0.072(2) 0.0507(19) 0.0003(15) -0.0052(15) 0.0022(16) CB_25 0.080(3) 0.086(3) 0.059(2) -0.0028(18) -0.0089(19) 0.008(2) CG_25 0.086(3) 0.086(3) 0.086(3) -0.016(2) -0.011(2) 0.015(2) CD1_25 0.100(4) 0.078(3) 0.104(4) 0.011(2) -0.022(3) 0.014(2) CD2_25 0.132(5) 0.105(4) 0.142(6) -0.039(4) -0.037(4) 0.036(4) C_25 0.065(2) 0.072(2) 0.0430(17) -0.0025(14) -0.0008(14) -0.0014(15) O_25 0.0656(15) 0.0813(17) 0.0491(13) 0.0033(11) -0.0017(11) 0.0055(12) N_31 0.0586(16) 0.0688(18) 0.0524(16) 0.0012(12) 0.0011(12) -0.0053(13) CA_31 0.0569(19) 0.076(2) 0.0539(19) -0.0048(15) 0.0022(15) -0.0024(15) CB_31 0.069(2) 0.082(2) 0.052(2) -0.0062(16) 0.0006(16) -0.0047(18) CG_31 0.079(3) 0.085(3) 0.051(2) -0.0035(17) -0.0036(17) -0.005(2) CD1_31 0.085(3) 0.085(3) 0.058(2) 0.0004(18) -0.0009(19) 0.004(2) NE1_31 0.092(3) 0.077(2) 0.067(2) 0.0076(16) -0.0013(18) 0.0007(18) CE2_31 0.084(3) 0.084(3) 0.057(2) 0.0036(17) -0.0005(19) -0.010(2) CZ2_31 0.119(4) 0.114(4) 0.085(3) 0.004(2) 0.015(3) -0.016(3) CH2_31 0.094(4) 0.123(4) 0.083(3) -0.004(3) 0.022(3) -0.006(3) CZ3_31 0.082(3) 0.114(4) 0.085(3) 0.000(3) 0.016(2) 0.005(3) CE3_31 0.085(3) 0.096(3) 0.074(3) 0.000(2) 0.009(2) -0.003(2) CD2_31 0.076(3) 0.085(3) 0.057(2) -0.0022(17) -0.0001(18) -0.005(2) C_31 0.0513(18) 0.086(2) 0.0478(18) -0.0034(15) 0.0020(14) -0.0029(16) O_31 0.0606(14) 0.0768(16) 0.0568(14) -0.0002(11) 0.0048(11) -0.0117(11) N_32 0.0517(15) 0.0716(18) 0.0543(16) -0.0011(12) 0.0021(12) -0.0045(12) CA_32 0.0559(18) 0.075(2) 0.0492(18) -0.0037(14) 0.0042(14) -0.0052(15) CB_32 0.057(2) 0.078(2) 0.063(2) 0.0014(16) -0.0031(16) 0.0012(16) CG_32 0.059(2) 0.092(3) 0.069(2) -0.008(2) -0.0054(18) 0.0003(19) OD1_32 0.0648(16) 0.099(2) 0.0663(17) 0.0081(15) -0.0046(13) -0.0158(14) OD2_32 0.071(2) 0.094(3) 0.212(5) -0.009(3) -0.059(3) 0.0051(18) C_32 0.0492(17) 0.065(2) 0.0540(19) 0.0043(14) 0.0017(13) -0.0039(13) O_32 0.0543(13) 0.0745(17) 0.0557(14) 0.0000(11) 0.0002(10) -0.0045(11) N_33 0.0556(15) 0.0592(16) 0.0551(16) -0.0047(12) 0.0018(12) -0.0041(12) CA_33 0.0495(17) 0.076(2) 0.0524(18) -0.0059(15) 0.0014(14) -0.0045(15) CB_33 0.061(2) 0.080(2) 0.058(2) -0.0107(16) -0.0002(16) 0.0033(17) CG_33 0.064(2) 0.077(2) 0.063(2) -0.0074(17) 0.0069(17) -0.0047(17) CD_33 0.062(2) 0.066(2) 0.064(2) -0.0014(15) 0.0047(16) -0.0013(15) C_33 0.0504(18) 0.080(2) 0.0503(18) -0.0037(15) 0.0019(14) -0.0056(15) O_33 0.0529(13) 0.0751(15) 0.0553(13) -0.0026(11) 0.0005(10) -0.0045(11) N_34 0.0512(15) 0.0799(19) 0.0521(16) -0.0014(13) 0.0034(12) -0.0009(13) CA_34 0.0525(18) 0.076(2) 0.057(2) -0.0012(16) -0.0014(15) -0.0050(15) CB_34 0.067(2) 0.081(3) 0.055(2) 0.0006(16) 0.0000(16) -0.0135(18) CG1_34 0.073(2) 0.094(3) 0.051(2) 0.0007(18) -0.0004(17) -0.011(2) CG2_34 0.102(3) 0.083(3) 0.075(3) 0.015(2) -0.001(2) 0.006(2) C_34 0.0555(19) 0.068(2) 0.0522(18) 0.0003(14) 0.0014(14) -0.0033(15) O_34 0.0543(13) 0.0755(15) 0.0552(13) -0.0025(11) 0.0007(10) -0.0068(11) N_35 0.0484(15) 0.0759(19) 0.0564(17) 0.0011(13) -0.0010(12) -0.0055(12) CA_35 0.0505(17) 0.076(2) 0.0550(19) -0.0018(15) 0.0026(14) -0.0010(15) CB_35 0.0535(19) 0.078(2) 0.065(2) 0.0032(17) 0.0057(16) -0.0014(16) CG_35 0.059(2) 0.078(3) 0.082(3) 0.0081(19) 0.0076(18) -0.0026(18) CD1_35 0.073(3) 0.089(3) 0.112(4) 0.021(3) 0.011(3) 0.004(2) CD2_35 0.063(2) 0.079(3) 0.102(3) -0.002(2) 0.010(2) -0.0062(19) C_35 0.0485(17) 0.075(2) 0.0521(19) -0.0009(15) 0.0008(13) 0.0039(15) O_35 0.0510(12) 0.0735(15) 0.0590(14) -0.0029(11) 0.0006(10) -0.0037(11) N_41 0.0633(18) 0.078(2) 0.0562(17) -0.0054(13) 0.0049(14) -0.0136(14) CA_41 0.066(2) 0.074(2) 0.056(2) -0.0022(16) -0.0001(16) -0.0079(17) CB_41 0.088(3) 0.078(3) 0.060(2) 0.0050(17) -0.002(2) -0.011(2) CG_41 0.083(3) 0.087(3) 0.063(2) 0.0053(19) 0.005(2) -0.002(2) CD1_41 0.102(3) 0.089(3) 0.061(2) 0.004(2) 0.007(2) -0.004(2) NE1_41 0.125(4) 0.087(3) 0.058(2) -0.0048(17) 0.010(2) -0.014(2) CE2_41 0.112(4) 0.082(3) 0.066(3) -0.001(2) -0.002(2) -0.006(3) CZ2_41 0.158(6) 0.104(4) 0.066(3) 0.009(3) -0.022(3) -0.034(4) CH2_41 0.120(5) 0.120(5) 0.097(4) 0.013(3) -0.028(4) -0.001(4) CZ3_41 0.103(4) 0.116(4) 0.101(4) 0.018(3) -0.022(3) -0.008(3) CE3_41 0.093(3) 0.094(3) 0.080(3) 0.011(2) -0.006(3) -0.001(3) CD2_41 0.100(3) 0.079(3) 0.062(2) 0.0070(18) -0.002(2) -0.010(2) C_41 0.0534(19) 0.079(2) 0.0486(18) -0.0012(15) 0.0022(14) -0.0039(16) O_41 0.0543(14) 0.0761(16) 0.0715(16) -0.0073(12) -0.0034(11) -0.0070(11) N_42 0.0553(17) 0.080(2) 0.0607(18) 0.0071(14) -0.0056(13) -0.0140(14) CA_42 0.0562(19) 0.077(2) 0.0543(19) 0.0012(15) -0.0014(15) -0.0048(16) CB_42 0.059(2) 0.081(2) 0.054(2) -0.0052(16) 0.0071(15) -0.0046(16) CG_42 0.0552(19) 0.078(2) 0.0513(18) -0.0031(15) 0.0066(15) -0.0006(15) OD1_42 0.0602(15) 0.0873(19) 0.0701(16) -0.0190(13) 0.0094(12) -0.0089(13) OD2_42 0.0589(15) 0.0846(18) 0.0796(19) -0.0084(14) 0.0116(13) -0.0056(12) C_42 0.0480(17) 0.073(2) 0.0538(19) -0.0023(15) 0.0030(14) -0.0044(14) O_42 0.0559(13) 0.0750(16) 0.0559(14) -0.0028(11) 0.0029(10) -0.0056(11) N_43 0.0517(15) 0.0746(19) 0.0516(16) -0.0056(13) 0.0015(12) -0.0023(13) CA_43 0.0526(18) 0.073(2) 0.0495(18) 0.0026(14) -0.0009(14) -0.0024(15) CB_43 0.060(2) 0.074(2) 0.061(2) 0.0040(16) 0.0045(16) 0.0005(16) CG_43 0.069(2) 0.075(2) 0.065(2) 0.0002(17) 0.0004(17) -0.0053(18) CD_43 0.060(2) 0.076(2) 0.059(2) -0.0054(16) 0.0021(16) 0.0004(16) C_43 0.058(2) 0.077(2) 0.0480(18) 0.0038(14) -0.0002(14) -0.0088(16) O_43 0.0527(13) 0.0756(15) 0.0588(14) -0.0040(11) 0.0031(10) -0.0086(11) N_44 0.0536(15) 0.0739(18) 0.0505(16) -0.0036(12) -0.0003(12) -0.0029(13) CA_44 0.0545(18) 0.079(2) 0.057(2) -0.0029(16) 0.0023(15) -0.0098(16) CB_44 0.064(2) 0.088(3) 0.056(2) -0.0062(17) 0.0040(16) -0.0115(18) CG1_44 0.084(3) 0.106(3) 0.065(3) -0.015(2) 0.005(2) 0.006(2) CG2_44 0.074(2) 0.095(3) 0.056(2) -0.0048(18) 0.0029(18) -0.015(2) C_44 0.0545(19) 0.077(2) 0.0523(19) -0.0097(15) 0.0028(14) -0.0049(16) O_44 0.0522(13) 0.0780(16) 0.0582(14) -0.0030(11) 0.0003(10) -0.0081(11) N_45 0.0534(16) 0.084(2) 0.0521(16) -0.0077(13) 0.0014(12) -0.0071(14) CA_45 0.0561(19) 0.076(2) 0.059(2) -0.0037(15) 0.0022(15) -0.0068(16) CB_45 0.054(2) 0.085(3) 0.075(3) -0.0084(19) -0.0019(17) -0.0003(17) CG_45 0.070(3) 0.089(3) 0.084(3) -0.018(2) -0.006(2) 0.000(2) CD1_45 0.071(3) 0.090(3) 0.104(4) -0.018(2) -0.007(2) -0.005(2) CD2_45 0.077(3) 0.114(4) 0.144(5) -0.054(4) 0.003(3) 0.006(3) C_45 0.0532(19) 0.079(2) 0.061(2) -0.0028(16) -0.0037(15) -0.0034(17) O_45 0.0801(18) 0.110(2) 0.0585(15) -0.0037(14) 0.0029(13) -0.0411(17) O1_51 0.153(4) 0.091(2) 0.091(2) -0.0041(18) 0.036(2) -0.025(2) C1_51 0.211(9) 0.106(5) 0.110(5) 0.007(4) 0.063(5) -0.016(5) C2_51 0.365(19) 0.175(9) 0.085(5) 0.008(5) 0.029(8) -0.076(11) C3_51 0.350(18) 0.146(8) 0.178(10) 0.007(6) 0.095(11) -0.118(10) O1_52 0.096(3) 0.118(4) 0.267(8) 0.017(4) -0.049(4) -0.004(2) C1_52 0.088(4) 0.153(7) 0.257(12) 0.023(7) -0.028(6) 0.023(5) C2_52 0.107(6) 0.262(16) 0.38(2) 0.124(17) 0.013(10) 0.013(8) C3_52 0.225(17) 0.28(2) 0.62(5) 0.23(3) 0.00(2) 0.108(16) O1_53 0.108(3) 0.100(3) 0.241(6) -0.041(3) 0.078(4) -0.013(2) C1_53 0.091(4) 0.137(7) 0.304(14) -0.087(8) 0.070(6) -0.014(4) C2_53 0.106(5) 0.123(6) 0.284(13) -0.060(7) 0.044(7) 0.011(4) C3_53 0.111(5) 0.124(5) 0.154(7) -0.009(4) 0.039(4) 0.008(4) O1_54 0.167(7) 0.269(10) 0.227(9) -0.033(8) 0.008(6) 0.013(7) C1_54 0.169(10) 0.231(14) 0.165(10) -0.017(9) 0.000(8) 0.019(10) C2_54 0.216(12) 0.201(11) 0.173(10) 0.019(8) -0.011(9) -0.026(10) C3_54 0.26(2) 0.198(17) 0.53(4) -0.046(19) 0.15(3) -0.081(15) O1_55 0.102(2) 0.107(2) 0.0574(16) 0.0007(15) 0.0019(15) 0.0227(18) C1_55 0.105(4) 0.104(3) 0.070(3) -0.005(2) 0.003(3) 0.017(3) C2_55 0.160(6) 0.126(5) 0.081(4) -0.008(3) 0.005(4) 0.040(4) C3_55 0.108(4) 0.130(5) 0.103(4) 0.019(4) 0.010(3) 0.028(4) O1_56 0.376(16) 0.296(12) 0.164(7) 0.026(7) -0.055(9) -0.183(13) C1_56 0.276(19) 0.34(2) 0.173(11) -0.103(14) 0.101(13) -0.201(19) C2_56 0.111(8) 0.33(2) 0.40(3) -0.10(2) 0.044(12) -0.002(11) C3_56 0.28(2) 0.47(3) 0.221(17) 0.15(2) -0.008(16) -0.09(2) O1_57 0.164(11) 0.244(14) 0.161(11) 0.074(10) -0.064(9) -0.035(10) C1_57 0.148(13) 0.196(18) 0.139(13) -0.010(11) -0.038(11) -0.057(12) C2_57 0.093(8) 0.158(12) 0.122(10) 0.037(8) -0.003(7) -0.017(7) C3_57 0.18(2) 0.22(3) 0.38(5) 0.17(3) 0.05(3) 0.018(19) O1_58 0.59(4) 0.209(15) 0.45(3) 0.042(16) 0.36(3) 0.023(18) C1_58 0.190(19) 0.202(19) 0.26(2) 0.005(17) -0.025(17) -0.015(14) C2_58 0.208(18) 0.213(18) 0.25(2) 0.067(17) -0.001(16) -0.011(14) C3_58 0.190(18) 0.33(3) 0.21(2) -0.050(19) 0.001(15) 0.022(19) O1_61 0.0701(15) 0.0839(17) 0.0501(13) 0.0000(11) 0.0001(11) 0.0023(13) O2_62 0.0658(15) 0.0848(17) 0.0514(13) -0.0029(11) -0.0014(11) 0.0054(12) O3_63 0.0631(14) 0.0764(15) 0.0583(14) -0.0065(11) -0.0018(11) 0.0057(11) O4_64 0.0572(14) 0.0938(18) 0.0611(15) -0.0060(12) -0.0008(11) 0.0038(12) O5_65 0.0539(13) 0.0869(17) 0.0582(14) -0.0005(12) -0.0011(11) -0.0045(12) O6_66 0.0715(16) 0.0804(17) 0.0652(16) -0.0049(12) 0.0017(12) -0.0075(13) O7_67 0.0682(15) 0.0941(19) 0.0520(14) 0.0047(12) 0.0013(12) 0.0058(13) O8_68 0.107(2) 0.095(2) 0.0621(17) 0.0106(14) 0.0215(16) 0.0230(17) O9_69 0.095(7) 0.144(10) 0.124(9) 0.037(8) 0.001(6) -0.019(7) O10_70 0.27(3) 0.082(13) 0.34(4) -0.036(14) -0.12(3) -0.024(14) O11_71 0.39(6) 0.073(17) 0.15(3) -0.003(14) -0.10(3) -0.05(2) O12_72 0.044(7) 0.49(4) 0.15(2) 0.02(2) 0.015(10) -0.031(13) O13_73 0.37(3) 0.247(19) 0.188(17) -0.014(13) 0.045(18) -0.25(2) O14_74 0.19(2) 0.091(12) 0.086(11) 0.002(9) 0.050(13) -0.048(13) O15_75 0.20(2) 0.34(4) 0.125(16) 0.15(2) -0.072(16) -0.20(3) O16_76 0.130(13) 0.204(19) 0.22(2) -0.018(16) -0.030(14) 0.005(13) _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 Na_1 O_22 2.268(3) . ? Na_1 O_12 2.278(3) . ? Na_1 OD1_22 2.369(3) . ? Na_1 OD1_12 2.373(3) . ? Na_1 O_24 2.457(3) . ? Na_1 O_14 2.470(3) . ? Na_1 C_22 3.113(4) . ? Na_2 O_32 2.241(3) . ? Na_2 O_42 2.284(3) . ? Na_2 OD1_42 2.335(3) . ? Na_2 OD1_32 2.391(3) . ? Na_2 O_44 2.507(3) . ? Na_2 O_34 2.528(3) . ? Na_2 C_42 3.125(4) . ? Na_3 O_11 2.292(3) 2_575 ? Na_3 O3_63 2.298(3) . ? Na_3 O6_66 2.331(3) . ? Na_3 O1_61 2.346(4) . ? Na_3 O_15 2.378(3) 2_575 ? Na_3 Na_4 3.607(2) . ? Na_4 O8_68 2.255(4) . ? Na_4 O_33 2.354(3) 4_566 ? Na_4 O5_65 2.370(3) . ? Na_4 O_35 2.383(3) 4_566 ? Na_4 O3_63 2.389(3) . ? Na_4 O6_66 2.857(3) . ? N_11 C_15 1.336(5) . ? N_11 CA_11 1.470(5) . ? CA_11 C_11 1.523(6) . ? CA_11 CB_11 1.533(5) . ? CB_11 CG_11 1.519(6) . ? CG_11 CD1_11 1.339(7) . ? CG_11 CD2_11 1.440(6) . ? CD1_11 NE1_11 1.385(6) . ? NE1_11 CE2_11 1.372(7) . ? CE2_11 CD2_11 1.383(7) . ? CE2_11 CZ2_11 1.401(7) . ? CZ2_11 CH2_11 1.380(9) . ? CH2_11 CZ3_11 1.398(9) . ? CZ3_11 CE3_11 1.374(7) . ? CE3_11 CD2_11 1.430(7) . ? C_11 O_11 1.223(4) . ? C_11 N_12 1.341(5) . ? O_11 Na_3 2.292(3) 2_574 ? N_12 CA_12 1.443(5) . ? CA_12 C_12 1.525(5) . ? CA_12 CB_12 1.536(5) . ? CB_12 CG_12 1.542(5) . ? CG_12 OD1_12 1.234(5) . ? CG_12 OD2_12 1.278(5) . ? C_12 O_12 1.254(5) . ? C_12 N_13 1.323(5) . ? N_13 CA_13 1.478(5) . ? N_13 CD_13 1.493(5) . ? CA_13 C_13 1.512(6) . ? CA_13 CB_13 1.523(6) . ? CB_13 CG_13 1.532(6) . ? CG_13 CD_13 1.509(6) . ? C_13 O_13 1.228(5) . ? C_13 N_14 1.352(5) . ? N_14 CA_14 1.458(5) . ? CA_14 CB_14 1.525(6) . ? CA_14 C_14 1.535(5) . ? CB_14 CG2_14 1.527(6) . ? CB_14 CG1_14 1.544(6) . ? C_14 O_14 1.248(4) . ? C_14 N_15 1.324(5) . ? N_15 CA_15 1.473(5) . ? CA_15 C_15 1.516(5) . ? CA_15 CB_15 1.523(5) . ? CB_15 CG_15 1.531(6) . ? CG_15 CD2_15 1.509(6) . ? CG_15 CD1_15 1.532(6) . ? C_15 O_15 1.251(4) . ? O_15 Na_3 2.379(3) 2_574 ? N_21 C_25 1.336(5) . ? N_21 CA_21 1.452(5) . ? CA_21 C_21 1.523(5) . ? CA_21 CB_21 1.539(6) . ? CB_21 CG_21 1.508(7) . ? CG_21 CD1_21 1.337(8) . ? CG_21 CD2_21 1.437(8) . ? CD1_21 NE1_21 1.421(9) . ? NE1_21 CE2_21 1.357(10) . ? CE2_21 CZ2_21 1.335(11) . ? CE2_21 CD2_21 1.359(9) . ? CZ2_21 CH2_21 1.419(16) . ? CH2_21 CZ3_21 1.415(16) . ? CZ3_21 CE3_21 1.396(9) . ? CE3_21 CD2_21 1.442(10) . ? C_21 O_21 1.241(4) . ? C_21 N_22 1.344(5) . ? N_22 CA_22 1.440(5) . ? CA_22 C_22 1.527(5) . ? CA_22 CB_22 1.541(5) . ? CB_22 CG_22 1.514(5) . ? CG_22 OD1_22 1.246(5) . ? CG_22 OD2_22 1.265(5) . ? C_22 O_22 1.253(4) . ? C_22 N_23 1.344(5) . ? N_23 CA_23 1.465(5) . ? N_23 CD_23 1.488(5) . ? CA_23 CB_23 1.518(5) . ? CA_23 C_23 1.521(5) . ? CB_23 CG_23 1.527(6) . ? CG_23 CD_23 1.515(6) . ? C_23 O_23 1.239(5) . ? C_23 N_24 1.339(5) . ? N_24 CA_24 1.463(5) . ? CA_24 C_24 1.534(5) . ? CA_24 CB_24 1.532(6) . ? CB_24 CG1_24 1.503(7) . ? CB_24 CG2_24 1.527(6) . ? C_24 O_24 1.232(4) . ? C_24 N_25 1.340(5) . ? N_25 CA_25 1.465(5) . ? CA_25 CB_25 1.518(6) . ? CA_25 C_25 1.530(5) . ? CB_25 CG_25 1.533(6) . ? CG_25 CD1_25 1.529(8) . ? CG_25 CD2_25 1.543(8) . ? C_25 O_25 1.236(5) . ? N_31 C_35 1.339(5) . ? N_31 CA_31 1.454(5) . ? CA_31 C_31 1.534(6) . ? CA_31 CB_31 1.543(5) . ? CB_31 CG_31 1.484(6) . ? CG_31 CD1_31 1.364(6) . ? CG_31 CD2_31 1.432(6) . ? CD1_31 NE1_31 1.393(6) . ? NE1_31 CE2_31 1.374(6) . ? CE2_31 CZ2_31 1.384(7) . ? CE2_31 CD2_31 1.415(6) . ? CZ2_31 CH2_31 1.366(8) . ? CH2_31 CZ3_31 1.393(9) . ? CZ3_31 CE3_31 1.384(7) . ? CE3_31 CD2_31 1.403(7) . ? C_31 O_31 1.241(5) . ? C_31 N_32 1.333(5) . ? N_32 CA_32 1.459(5) . ? CA_32 C_32 1.509(5) . ? CA_32 CB_32 1.522(5) . ? CB_32 CG_32 1.532(6) . ? CG_32 OD1_32 1.214(6) . ? CG_32 OD2_32 1.261(6) . ? C_32 O_32 1.249(5) . ? C_32 N_33 1.329(5) . ? N_33 CA_33 1.473(5) . ? N_33 CD_33 1.486(5) . ? CA_33 C_33 1.525(5) . ? CA_33 CB_33 1.523(5) . ? CB_33 CG_33 1.527(6) . ? CG_33 CD_33 1.502(6) . ? C_33 O_33 1.237(4) . ? C_33 N_34 1.349(5) . ? O_33 Na_4 2.354(3) 4_466 ? N_34 CA_34 1.456(5) . ? CA_34 C_34 1.522(5) . ? CA_34 CB_34 1.551(5) . ? CB_34 CG2_34 1.501(7) . ? CB_34 CG1_34 1.521(6) . ? C_34 O_34 1.256(4) . ? C_34 N_35 1.334(5) . ? N_35 CA_35 1.454(5) . ? CA_35 C_35 1.527(5) . ? CA_35 CB_35 1.527(5) . ? CB_35 CG_35 1.540(6) . ? CG_35 CD1_35 1.508(7) . ? CG_35 CD2_35 1.533(7) . ? C_35 O_35 1.236(4) . ? O_35 Na_4 2.383(3) 4_466 ? N_41 C_45 1.340(5) . ? N_41 CA_41 1.453(5) . ? CA_41 C_41 1.534(6) . ? CA_41 CB_41 1.538(6) . ? CB_41 CG_41 1.488(6) . ? CG_41 CD1_41 1.352(7) . ? CG_41 CD2_41 1.459(7) . ? CD1_41 NE1_41 1.365(7) . ? NE1_41 CE2_41 1.359(7) . ? CE2_41 CZ2_41 1.395(8) . ? CE2_41 CD2_41 1.417(7) . ? CZ2_41 CH2_41 1.390(10) . ? CH2_41 CZ3_41 1.360(10) . ? CZ3_41 CE3_41 1.376(8) . ? CE3_41 CD2_41 1.377(8) . ? C_41 O_41 1.231(4) . ? C_41 N_42 1.349(5) . ? N_42 CA_42 1.448(5) . ? CA_42 CB_42 1.528(5) . ? CA_42 C_42 1.522(5) . ? CB_42 CG_42 1.519(5) . ? CG_42 OD1_42 1.233(5) . ? CG_42 OD2_42 1.269(5) . ? C_42 O_42 1.241(4) . ? C_42 N_43 1.354(5) . ? N_43 CD_43 1.470(5) . ? N_43 CA_43 1.480(5) . ? CA_43 CB_43 1.527(5) . ? CA_43 C_43 1.538(5) . ? CB_43 CG_43 1.550(6) . ? CG_43 CD_43 1.511(6) . ? C_43 O_43 1.245(4) . ? C_43 N_44 1.340(5) . ? N_44 CA_44 1.472(5) . ? CA_44 CB_44 1.511(6) . ? CA_44 C_44 1.529(6) . ? CB_44 CG2_44 1.515(6) . ? CB_44 CG1_44 1.528(7) . ? C_44 O_44 1.247(4) . ? C_44 N_45 1.333(5) . ? N_45 CA_45 1.468(5) . ? CA_45 C_45 1.517(5) . ? CA_45 CB_45 1.524(6) . ? CB_45 CG_45 1.509(6) . ? CG_45 CD2_45 1.514(7) . ? CG_45 CD1_45 1.546(7) . ? C_45 O_45 1.224(5) . ? O1_51 C1_51 1.382(7) . ? C1_51 C2_51 1.402(11) . ? C1_51 C3_51 1.467(10) . ? O1_52 C1_52 1.386(8) . ? C1_52 C3_52 1.496(15) . ? C1_52 C2_52 1.493(12) . ? O1_53 C1_53 1.399(8) . ? C1_53 C3_53 1.408(9) . ? C1_53 C2_53 1.507(9) . ? O1_54 C1_54 1.387(12) . ? C1_54 C2_54 1.478(13) . ? C1_54 C3_54 1.569(15) . ? O1_55 C1_55 1.452(6) . ? C1_55 C3_55 1.517(8) . ? C1_55 C2_55 1.500(7) . ? O1_56 C1_56 1.400(14) . ? C1_56 C3_56 1.471(14) . ? C1_56 C2_56 1.511(16) . ? O1_57 C1_57 1.431(14) . ? C1_57 C2_57 1.532(15) . ? C1_57 C3_57 1.518(16) . ? O1_58 C1_58 1.418(16) . ? C1_58 C2_58 1.444(16) . ? C1_58 C3_58 1.490(16) . ? O9_69 O15_75 1.53(3) . ? O10_70 O11_71 1.62(6) . ? O15_75 O16_76 1.66(4) 3_546 ? O16_76 O15_75 1.66(4) 3_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O_22 Na_1 O_12 168.96(9) . . ? O_22 Na_1 OD1_22 79.68(10) . . ? O_12 Na_1 OD1_22 111.14(10) . . ? O_22 Na_1 OD1_12 101.02(9) . . ? O_12 Na_1 OD1_12 82.27(9) . . ? OD1_22 Na_1 OD1_12 87.26(10) . . ? O_22 Na_1 O_24 81.59(9) . . ? O_12 Na_1 O_24 87.46(10) . . ? OD1_22 Na_1 O_24 160.84(8) . . ? OD1_12 Na_1 O_24 100.26(9) . . ? O_22 Na_1 O_14 95.09(9) . . ? O_12 Na_1 O_14 81.78(9) . . ? OD1_22 Na_1 O_14 96.33(9) . . ? OD1_12 Na_1 O_14 163.87(8) . . ? O_24 Na_1 O_14 81.35(9) . . ? O_22 Na_1 C_22 20.06(9) . . ? O_12 Na_1 C_22 168.97(9) . . ? OD1_22 Na_1 C_22 60.22(10) . . ? OD1_12 Na_1 C_22 103.26(10) . . ? O_24 Na_1 C_22 100.74(10) . . ? O_14 Na_1 C_22 92.10(9) . . ? O_32 Na_2 O_42 175.20(9) . . ? O_32 Na_2 OD1_42 101.60(9) . . ? O_42 Na_2 OD1_42 80.02(9) . . ? O_32 Na_2 OD1_32 79.30(10) . . ? O_42 Na_2 OD1_32 105.45(10) . . ? OD1_42 Na_2 OD1_32 81.51(13) . . ? O_32 Na_2 O_44 91.79(9) . . ? O_42 Na_2 O_44 86.63(9) . . ? OD1_42 Na_2 O_44 166.61(9) . . ? OD1_32 Na_2 O_44 101.23(11) . . ? O_32 Na_2 O_34 82.87(9) . . ? O_42 Na_2 O_34 92.39(9) . . ? OD1_42 Na_2 O_34 101.96(11) . . ? OD1_32 Na_2 O_34 162.17(9) . . ? O_44 Na_2 O_34 79.48(10) . . ? O_32 Na_2 C_42 159.49(9) . . ? O_42 Na_2 C_42 19.66(9) . . ? OD1_42 Na_2 C_42 62.21(9) . . ? OD1_32 Na_2 C_42 108.57(10) . . ? O_44 Na_2 C_42 104.74(9) . . ? O_34 Na_2 C_42 88.21(9) . . ? O_11 Na_3 O3_63 109.34(10) 2_575 . ? O_11 Na_3 O6_66 88.44(9) 2_575 . ? O3_63 Na_3 O6_66 89.02(11) . . ? O_11 Na_3 O1_61 146.89(10) 2_575 . ? O3_63 Na_3 O1_61 102.60(11) . . ? O6_66 Na_3 O1_61 100.80(12) . . ? O_11 Na_3 O_15 87.80(9) 2_575 2_575 ? O3_63 Na_3 O_15 91.42(9) . 2_575 ? O6_66 Na_3 O_15 176.15(10) . 2_575 ? O1_61 Na_3 O_15 82.84(9) . 2_575 ? O_11 Na_3 Na_4 118.26(7) 2_575 . ? O3_63 Na_3 Na_4 40.62(7) . . ? O6_66 Na_3 Na_4 52.32(8) . . ? O1_61 Na_3 Na_4 91.70(8) . . ? O_15 Na_3 Na_4 129.26(6) 2_575 . ? O8_68 Na_4 O_33 119.67(12) . 4_566 ? O8_68 Na_4 O5_65 153.99(14) . . ? O_33 Na_4 O5_65 85.78(8) 4_566 . ? O8_68 Na_4 O_35 85.03(11) . 4_566 ? O_33 Na_4 O_35 103.89(9) 4_566 4_566 ? O5_65 Na_4 O_35 83.43(10) . 4_566 ? O8_68 Na_4 O3_63 81.87(13) . . ? O_33 Na_4 O3_63 82.88(8) 4_566 . ? O5_65 Na_4 O3_63 108.50(12) . . ? O_35 Na_4 O3_63 166.90(9) 4_566 . ? O8_68 Na_4 O6_66 80.50(12) . . ? O_33 Na_4 O6_66 148.34(9) 4_566 . ? O5_65 Na_4 O6_66 79.19(10) . . ? O_35 Na_4 O6_66 101.88(8) 4_566 . ? O3_63 Na_4 O6_66 75.85(9) . . ? O8_68 Na_4 Na_3 66.84(9) . . ? O_33 Na_4 Na_3 121.55(7) 4_566 . ? O5_65 Na_4 Na_3 105.92(8) . . ? O_35 Na_4 Na_3 133.87(6) 4_566 . ? O3_63 Na_4 Na_3 38.79(7) . . ? O6_66 Na_4 Na_3 40.22(7) . . ? C_15 N_11 CA_11 123.2(3) . . ? N_11 CA_11 C_11 108.5(3) . . ? N_11 CA_11 CB_11 108.4(3) . . ? C_11 CA_11 CB_11 115.1(3) . . ? CG_11 CB_11 CA_11 111.5(3) . . ? CD1_11 CG_11 CD2_11 105.8(4) . . ? CD1_11 CG_11 CB_11 128.9(4) . . ? CD2_11 CG_11 CB_11 125.2(4) . . ? CG_11 CD1_11 NE1_11 110.8(4) . . ? CE2_11 NE1_11 CD1_11 107.9(4) . . ? NE1_11 CE2_11 CD2_11 107.6(4) . . ? NE1_11 CE2_11 CZ2_11 128.7(5) . . ? CD2_11 CE2_11 CZ2_11 123.7(5) . . ? CH2_11 CZ2_11 CE2_11 116.4(5) . . ? CZ2_11 CH2_11 CZ3_11 121.4(5) . . ? CE3_11 CZ3_11 CH2_11 122.4(6) . . ? CZ3_11 CE3_11 CD2_11 117.4(5) . . ? CE2_11 CD2_11 CE3_11 118.8(4) . . ? CE2_11 CD2_11 CG_11 107.9(4) . . ? CE3_11 CD2_11 CG_11 133.2(4) . . ? O_11 C_11 N_12 122.5(4) . . ? O_11 C_11 CA_11 121.5(3) . . ? N_12 C_11 CA_11 115.9(3) . . ? C_11 O_11 Na_3 124.8(2) . 2_574 ? C_11 N_12 CA_12 121.9(3) . . ? N_12 CA_12 C_12 109.5(3) . . ? N_12 CA_12 CB_12 109.9(3) . . ? C_12 CA_12 CB_12 111.6(3) . . ? CA_12 CB_12 CG_12 114.8(3) . . ? OD1_12 CG_12 OD2_12 125.4(4) . . ? OD1_12 CG_12 CB_12 119.8(3) . . ? OD2_12 CG_12 CB_12 114.8(4) . . ? CG_12 OD1_12 Na_1 143.9(3) . . ? O_12 C_12 N_13 120.1(3) . . ? O_12 C_12 CA_12 120.2(3) . . ? N_13 C_12 CA_12 119.6(3) . . ? C_12 O_12 Na_1 125.6(2) . . ? C_12 N_13 CA_13 122.2(3) . . ? C_12 N_13 CD_13 127.1(3) . . ? CA_13 N_13 CD_13 110.5(3) . . ? N_13 CA_13 C_13 110.6(3) . . ? N_13 CA_13 CB_13 103.9(3) . . ? C_13 CA_13 CB_13 113.0(3) . . ? CA_13 CB_13 CG_13 105.2(3) . . ? CD_13 CG_13 CB_13 102.3(3) . . ? N_13 CD_13 CG_13 102.4(3) . . ? O_13 C_13 N_14 123.0(4) . . ? O_13 C_13 CA_13 121.0(3) . . ? N_14 C_13 CA_13 115.9(3) . . ? C_13 N_14 CA_14 120.0(3) . . ? N_14 CA_14 CB_14 112.3(3) . . ? N_14 CA_14 C_14 105.9(3) . . ? CB_14 CA_14 C_14 111.2(3) . . ? CG2_14 CB_14 CA_14 110.5(3) . . ? CG2_14 CB_14 CG1_14 111.0(4) . . ? CA_14 CB_14 CG1_14 109.9(3) . . ? O_14 C_14 N_15 123.5(3) . . ? O_14 C_14 CA_14 119.0(3) . . ? N_15 C_14 CA_14 117.5(3) . . ? C_14 O_14 Na_1 123.1(2) . . ? C_14 N_15 CA_15 122.9(3) . . ? N_15 CA_15 C_15 108.3(3) . . ? N_15 CA_15 CB_15 111.5(3) . . ? C_15 CA_15 CB_15 110.1(3) . . ? CA_15 CB_15 CG_15 115.7(3) . . ? CD2_15 CG_15 CD1_15 110.6(4) . . ? CD2_15 CG_15 CB_15 110.3(3) . . ? CD1_15 CG_15 CB_15 112.2(4) . . ? O_15 C_15 N_11 122.5(3) . . ? O_15 C_15 CA_15 121.0(3) . . ? N_11 C_15 CA_15 116.4(3) . . ? C_15 O_15 Na_3 137.9(2) . 2_574 ? C_25 N_21 CA_21 120.9(3) . . ? N_21 CA_21 C_21 111.6(3) . . ? N_21 CA_21 CB_21 109.0(3) . . ? C_21 CA_21 CB_21 111.4(3) . . ? CG_21 CB_21 CA_21 113.2(4) . . ? CD1_21 CG_21 CD2_21 106.2(5) . . ? CD1_21 CG_21 CB_21 126.4(5) . . ? CD2_21 CG_21 CB_21 127.4(5) . . ? CG_21 CD1_21 NE1_21 108.0(7) . . ? CE2_21 NE1_21 CD1_21 109.6(6) . . ? CZ2_21 CE2_21 NE1_21 123.6(9) . . ? CZ2_21 CE2_21 CD2_21 129.9(9) . . ? NE1_21 CE2_21 CD2_21 106.5(6) . . ? CE2_21 CZ2_21 CH2_21 112.0(9) . . ? CZ2_21 CH2_21 CZ3_21 123.5(8) . . ? CE3_21 CZ3_21 CH2_21 120.2(9) . . ? CZ3_21 CE3_21 CD2_21 116.5(7) . . ? CE2_21 CD2_21 CG_21 109.8(6) . . ? CE2_21 CD2_21 CE3_21 117.8(6) . . ? CG_21 CD2_21 CE3_21 132.4(5) . . ? O_21 C_21 N_22 123.1(3) . . ? O_21 C_21 CA_21 120.9(3) . . ? N_22 C_21 CA_21 116.0(3) . . ? C_21 N_22 CA_22 122.1(3) . . ? N_22 CA_22 C_22 108.1(3) . . ? N_22 CA_22 CB_22 113.0(3) . . ? C_22 CA_22 CB_22 112.2(3) . . ? CG_22 CB_22 CA_22 117.9(3) . . ? OD1_22 CG_22 OD2_22 124.8(3) . . ? OD1_22 CG_22 CB_22 119.5(3) . . ? OD2_22 CG_22 CB_22 115.6(3) . . ? CG_22 OD1_22 Na_1 157.6(2) . . ? O_22 C_22 N_23 119.0(3) . . ? O_22 C_22 CA_22 120.1(3) . . ? N_23 C_22 CA_22 120.9(3) . . ? O_22 C_22 Na_1 38.37(16) . . ? N_23 C_22 Na_1 116.5(2) . . ? CA_22 C_22 Na_1 108.6(2) . . ? C_22 O_22 Na_1 121.6(2) . . ? C_22 N_23 CA_23 120.5(3) . . ? C_22 N_23 CD_23 127.8(3) . . ? CA_23 N_23 CD_23 111.2(3) . . ? N_23 CA_23 CB_23 104.1(3) . . ? N_23 CA_23 C_23 110.6(3) . . ? CB_23 CA_23 C_23 113.7(3) . . ? CA_23 CB_23 CG_23 104.9(3) . . ? CD_23 CG_23 CB_23 102.6(3) . . ? N_23 CD_23 CG_23 102.9(3) . . ? O_23 C_23 N_24 122.4(4) . . ? O_23 C_23 CA_23 119.9(4) . . ? N_24 C_23 CA_23 117.5(3) . . ? C_23 N_24 CA_24 120.4(3) . . ? N_24 CA_24 C_24 105.2(3) . . ? N_24 CA_24 CB_24 112.2(3) . . ? C_24 CA_24 CB_24 112.0(3) . . ? CG1_24 CB_24 CG2_24 111.5(4) . . ? CG1_24 CB_24 CA_24 111.2(4) . . ? CG2_24 CB_24 CA_24 109.7(4) . . ? O_24 C_24 N_25 123.9(4) . . ? O_24 C_24 CA_24 120.4(3) . . ? N_25 C_24 CA_24 115.6(3) . . ? C_24 O_24 Na_1 121.3(2) . . ? C_24 N_25 CA_25 122.8(3) . . ? N_25 CA_25 CB_25 112.9(3) . . ? N_25 CA_25 C_25 108.1(3) . . ? CB_25 CA_25 C_25 109.9(3) . . ? CA_25 CB_25 CG_25 115.1(4) . . ? CD1_25 CG_25 CB_25 112.7(4) . . ? CD1_25 CG_25 CD2_25 111.8(5) . . ? CB_25 CG_25 CD2_25 108.8(4) . . ? O_25 C_25 N_21 122.4(4) . . ? O_25 C_25 CA_25 122.6(3) . . ? N_21 C_25 CA_25 114.9(3) . . ? C_35 N_31 CA_31 121.4(3) . . ? N_31 CA_31 C_31 110.7(3) . . ? N_31 CA_31 CB_31 109.1(3) . . ? C_31 CA_31 CB_31 111.0(3) . . ? CG_31 CB_31 CA_31 112.2(3) . . ? CD1_31 CG_31 CD2_31 106.4(4) . . ? CD1_31 CG_31 CB_31 127.3(4) . . ? CD2_31 CG_31 CB_31 126.1(4) . . ? CG_31 CD1_31 NE1_31 110.4(4) . . ? CE2_31 NE1_31 CD1_31 107.9(4) . . ? NE1_31 CE2_31 CZ2_31 129.9(4) . . ? NE1_31 CE2_31 CD2_31 108.0(4) . . ? CZ2_31 CE2_31 CD2_31 122.0(5) . . ? CH2_31 CZ2_31 CE2_31 118.0(5) . . ? CZ2_31 CH2_31 CZ3_31 121.4(5) . . ? CE3_31 CZ3_31 CH2_31 121.2(5) . . ? CZ3_31 CE3_31 CD2_31 118.6(5) . . ? CE3_31 CD2_31 CE2_31 118.6(4) . . ? CE3_31 CD2_31 CG_31 134.2(4) . . ? CE2_31 CD2_31 CG_31 107.2(4) . . ? O_31 C_31 N_32 122.8(4) . . ? O_31 C_31 CA_31 120.3(3) . . ? N_32 C_31 CA_31 116.8(3) . . ? C_31 N_32 CA_32 120.8(3) . . ? N_32 CA_32 C_32 108.3(3) . . ? N_32 CA_32 CB_32 112.5(3) . . ? C_32 CA_32 CB_32 113.5(3) . . ? CA_32 CB_32 CG_32 116.3(4) . . ? OD1_32 CG_32 OD2_32 123.8(4) . . ? OD1_32 CG_32 CB_32 120.4(4) . . ? OD2_32 CG_32 CB_32 115.7(4) . . ? CG_32 OD1_32 Na_2 159.3(3) . . ? O_32 C_32 N_33 119.5(3) . . ? O_32 C_32 CA_32 120.7(3) . . ? N_33 C_32 CA_32 119.7(3) . . ? C_32 O_32 Na_2 126.7(2) . . ? C_32 N_33 CA_33 119.6(3) . . ? C_32 N_33 CD_33 128.5(3) . . ? CA_33 N_33 CD_33 111.3(3) . . ? N_33 CA_33 C_33 110.3(3) . . ? N_33 CA_33 CB_33 104.0(3) . . ? C_33 CA_33 CB_33 113.4(3) . . ? CA_33 CB_33 CG_33 105.2(3) . . ? CD_33 CG_33 CB_33 104.0(3) . . ? N_33 CD_33 CG_33 102.3(3) . . ? O_33 C_33 N_34 124.3(4) . . ? O_33 C_33 CA_33 121.0(3) . . ? N_34 C_33 CA_33 114.6(3) . . ? C_33 O_33 Na_4 151.8(2) . 4_466 ? C_33 N_34 CA_34 118.5(3) . . ? N_34 CA_34 C_34 106.0(3) . . ? N_34 CA_34 CB_34 113.0(3) . . ? C_34 CA_34 CB_34 110.5(3) . . ? CG2_34 CB_34 CG1_34 112.2(4) . . ? CG2_34 CB_34 CA_34 109.7(4) . . ? CG1_34 CB_34 CA_34 110.8(3) . . ? O_34 C_34 N_35 123.1(3) . . ? O_34 C_34 CA_34 120.4(3) . . ? N_35 C_34 CA_34 116.4(3) . . ? C_34 O_34 Na_2 118.6(2) . . ? C_34 N_35 CA_35 123.6(3) . . ? N_35 CA_35 C_35 109.1(3) . . ? N_35 CA_35 CB_35 111.1(3) . . ? C_35 CA_35 CB_35 110.8(3) . . ? CA_35 CB_35 CG_35 113.5(3) . . ? CD1_35 CG_35 CD2_35 111.6(4) . . ? CD1_35 CG_35 CB_35 110.8(3) . . ? CD2_35 CG_35 CB_35 111.2(4) . . ? O_35 C_35 N_31 122.7(3) . . ? O_35 C_35 CA_35 122.5(3) . . ? N_31 C_35 CA_35 114.8(3) . . ? C_35 O_35 Na_4 148.9(2) . 4_466 ? C_45 N_41 CA_41 121.8(3) . . ? N_41 CA_41 C_41 109.8(3) . . ? N_41 CA_41 CB_41 109.3(3) . . ? C_41 CA_41 CB_41 112.4(3) . . ? CG_41 CB_41 CA_41 114.6(4) . . ? CD1_41 CG_41 CD2_41 105.6(4) . . ? CD1_41 CG_41 CB_41 129.7(5) . . ? CD2_41 CG_41 CB_41 124.7(4) . . ? CG_41 CD1_41 NE1_41 110.7(5) . . ? CE2_41 NE1_41 CD1_41 110.0(4) . . ? NE1_41 CE2_41 CZ2_41 131.4(5) . . ? NE1_41 CE2_41 CD2_41 106.9(5) . . ? CZ2_41 CE2_41 CD2_41 121.7(6) . . ? CH2_41 CZ2_41 CE2_41 117.2(6) . . ? CZ3_41 CH2_41 CZ2_41 121.5(6) . . ? CH2_41 CZ3_41 CE3_41 121.1(7) . . ? CZ3_41 CE3_41 CD2_41 120.4(6) . . ? CE3_41 CD2_41 CE2_41 118.1(5) . . ? CE3_41 CD2_41 CG_41 135.1(5) . . ? CE2_41 CD2_41 CG_41 106.8(5) . . ? O_41 C_41 N_42 122.8(4) . . ? O_41 C_41 CA_41 121.6(3) . . ? N_42 C_41 CA_41 115.6(3) . . ? C_41 N_42 CA_42 122.0(3) . . ? N_42 CA_42 CB_42 111.7(3) . . ? N_42 CA_42 C_42 107.6(3) . . ? CB_42 CA_42 C_42 112.2(3) . . ? CG_42 CB_42 CA_42 115.5(3) . . ? OD1_42 CG_42 OD2_42 123.8(4) . . ? OD1_42 CG_42 CB_42 118.8(3) . . ? OD2_42 CG_42 CB_42 117.4(3) . . ? CG_42 OD1_42 Na_2 150.2(3) . . ? O_42 C_42 N_43 119.7(3) . . ? O_42 C_42 CA_42 121.7(3) . . ? N_43 C_42 CA_42 118.5(3) . . ? O_42 C_42 Na_2 38.28(16) . . ? N_43 C_42 Na_2 118.3(2) . . ? CA_42 C_42 Na_2 108.5(2) . . ? C_42 O_42 Na_2 122.1(2) . . ? C_42 N_43 CD_43 128.4(3) . . ? C_42 N_43 CA_43 120.3(3) . . ? CD_43 N_43 CA_43 111.0(3) . . ? N_43 CA_43 CB_43 104.1(3) . . ? N_43 CA_43 C_43 110.4(3) . . ? CB_43 CA_43 C_43 113.8(3) . . ? CA_43 CB_43 CG_43 105.4(3) . . ? CD_43 CG_43 CB_43 102.8(3) . . ? N_43 CD_43 CG_43 102.7(3) . . ? O_43 C_43 N_44 124.3(4) . . ? O_43 C_43 CA_43 121.2(3) . . ? N_44 C_43 CA_43 114.2(3) . . ? C_43 N_44 CA_44 121.6(3) . . ? N_44 CA_44 CB_44 113.3(3) . . ? N_44 CA_44 C_44 105.1(3) . . ? CB_44 CA_44 C_44 111.9(3) . . ? CA_44 CB_44 CG2_44 112.6(4) . . ? CA_44 CB_44 CG1_44 109.4(4) . . ? CG2_44 CB_44 CG1_44 110.9(4) . . ? O_44 C_44 N_45 123.4(4) . . ? O_44 C_44 CA_44 119.3(3) . . ? N_45 C_44 CA_44 117.3(3) . . ? C_44 O_44 Na_2 114.9(2) . . ? C_44 N_45 CA_45 122.0(3) . . ? N_45 CA_45 C_45 107.1(3) . . ? N_45 CA_45 CB_45 112.7(3) . . ? C_45 CA_45 CB_45 111.2(3) . . ? CG_45 CB_45 CA_45 115.2(4) . . ? CB_45 CG_45 CD2_45 110.8(4) . . ? CB_45 CG_45 CD1_45 110.3(4) . . ? CD2_45 CG_45 CD1_45 107.8(5) . . ? O_45 C_45 N_41 123.1(4) . . ? O_45 C_45 CA_45 121.2(4) . . ? N_41 C_45 CA_45 115.8(3) . . ? O1_51 C1_51 C2_51 119.8(7) . . ? O1_51 C1_51 C3_51 111.8(7) . . ? C2_51 C1_51 C3_51 118.5(8) . . ? O1_52 C1_52 C3_52 109.6(10) . . ? O1_52 C1_52 C2_52 114.6(8) . . ? C3_52 C1_52 C2_52 117.9(12) . . ? O1_53 C1_53 C3_53 124.4(8) . . ? O1_53 C1_53 C2_53 107.8(6) . . ? C3_53 C1_53 C2_53 118.7(6) . . ? O1_54 C1_54 C2_54 106.4(11) . . ? O1_54 C1_54 C3_54 107.4(13) . . ? C2_54 C1_54 C3_54 104.3(13) . . ? O1_55 C1_55 C3_55 112.8(5) . . ? O1_55 C1_55 C2_55 107.2(4) . . ? C3_55 C1_55 C2_55 111.2(5) . . ? O1_56 C1_56 C3_56 111.3(14) . . ? O1_56 C1_56 C2_56 111.7(14) . . ? C3_56 C1_56 C2_56 112.5(17) . . ? O1_57 C1_57 C2_57 107.4(12) . . ? O1_57 C1_57 C3_57 113.4(17) . . ? C2_57 C1_57 C3_57 109.8(15) . . ? O1_58 C1_58 C2_58 110.3(17) . . ? O1_58 C1_58 C3_58 122.0(19) . . ? C2_58 C1_58 C3_58 121.4(18) . . ? Na_3 O3_63 Na_4 100.59(11) . . ? Na_3 O6_66 Na_4 87.47(10) . . ? O9_69 O15_75 O16_76 105(2) . 3_546 ? _diffrn_measured_fraction_theta_max 0.780 _diffrn_reflns_theta_full 31.42 _diffrn_measured_fraction_theta_full 0.780 _refine_diff_density_max 0.572 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.085 #=========================END