data_TR2THNO3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H33 N4 S3, 3(N O3)' _chemical_formula_sum 'C21 H33 N7 O9 S3' _chemical_formula_weight 623.72 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_cell_setting 'Monoclinic' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.906(3) _cell_length_b 16.193(4) _cell_length_c 17.823(6) _cell_angle_alpha 90 _cell_angle_beta 95.252(10) _cell_angle_gamma 90 _cell_volume 2846.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(5) _cell_measurement_reflns_used 5155 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.4 _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.321 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(5) _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 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method '\w and \f scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20961 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 26.4 _reflns_number_total 5797 _reflns_number_gt 3906 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0777P)^2^+3.1114P] 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 0.0027(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5797 _refine_ls_number_parameters 379 _refine_ls_number_restraints 123 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1665 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.001 _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 0.3000(2) 0.32198(14) 0.19367(13) 0.0245(5) Uani 1 1 d . . . O2 O 0.3494(2) 0.32523(13) 0.31512(13) 0.0241(5) Uani 1 1 d . . . O3 O 0.1386(2) 0.31865(14) 0.26880(13) 0.0259(5) Uani 1 1 d . . . O4 O 0.2981(2) 0.49509(15) -0.07985(14) 0.0294(6) Uani 1 1 d . . . O5 O 0.3338(2) 0.47947(16) 0.04134(14) 0.0325(6) Uani 1 1 d . . . O6 O 0.1295(2) 0.49292(16) -0.01051(14) 0.0337(6) Uani 1 1 d . . . O7 O -0.1538(2) 0.47887(14) 0.31332(13) 0.0283(6) Uani 1 1 d . . . O8 O -0.1008(2) 0.48834(15) 0.43377(14) 0.0309(6) Uani 1 1 d . . . O9 O -0.3123(2) 0.48822(15) 0.38905(14) 0.0283(6) Uani 1 1 d . . . N1 N 0.2544(3) 0.51358(16) 0.25956(15) 0.0198(6) Uani 1 1 d . . . N2 N 0.1547(3) 0.41737(16) 0.40474(15) 0.0220(6) Uani 1 1 d . . . H21N H 0.1506 0.3883 0.3602 0.026 Uiso 1 1 calc R . . H22N H 0.0679 0.4327 0.4130 0.026 Uiso 1 1 calc R . . N3 N 0.5452(3) 0.42505(16) 0.25071(15) 0.0205(6) Uani 1 1 d . . . H31N H 0.5988 0.4423 0.2926 0.025 Uiso 1 1 calc R . . H32N H 0.4774 0.3924 0.2667 0.025 Uiso 1 1 calc R . . N4 N 0.0786(3) 0.41775(16) 0.12354(15) 0.0206(6) Uani 1 1 d . . . H41N H 0.1549 0.3914 0.1450 0.025 Uiso 1 1 calc R . . H42N H 0.0985 0.4385 0.0778 0.025 Uiso 1 1 calc R . . N5 N 0.2623(3) 0.32081(16) 0.25918(16) 0.0210(6) Uani 1 1 d . . . N6 N 0.2557(3) 0.48856(16) -0.01670(16) 0.0224(6) Uani 1 1 d . . . N7 N -0.1891(3) 0.48548(16) 0.37824(16) 0.0227(6) Uani 1 1 d . . . C1 C 0.1936(3) 0.54226(19) 0.32765(18) 0.0219(7) Uani 1 1 d . . . H1A H 0.0936 0.5387 0.3185 0.026 Uiso 1 1 calc R . . H1B H 0.2176 0.6010 0.3366 0.026 Uiso 1 1 calc R . . C2 C 0.2393(3) 0.4929(2) 0.39796(19) 0.0236(7) Uani 1 1 d . . . H2C H 0.3352 0.4766 0.3963 0.028 Uiso 1 1 calc R . . H2D H 0.2332 0.5281 0.4430 0.028 Uiso 1 1 calc R . . C3 C 0.2116(3) 0.3627(2) 0.46817(19) 0.0234(7) Uani 1 1 d . A . H3C H 0.2992 0.3394 0.4556 0.028 Uiso 1 1 calc R . . H3D H 0.2289 0.3961 0.5146 0.028 Uiso 1 1 calc R . . C4 C 0.1169(3) 0.2937(2) 0.48238(18) 0.0245(7) Uani 1 1 d D . . S1 S 0.15651(19) 0.19311(12) 0.45638(11) 0.0290(6) Uiso 0.581(5) 1 d PD A 1 C7 C 0.0040(10) 0.2960(6) 0.5160(5) 0.042(3) Uiso 0.581(5) 1 d PD A 1 H7 H -0.0305 0.3455 0.5355 0.050 Uiso 0.581(5) 1 calc PR A 1 S1A S -0.0378(4) 0.31275(18) 0.52140(16) 0.0338(8) Uani 0.419(5) 1 d PD A 2 C7A C 0.1330(10) 0.2086(6) 0.4746(6) 0.030(3) Uiso 0.419(5) 1 d PD A 2 H7A H 0.2132 0.1849 0.4585 0.036 Uiso 0.419(5) 1 calc PR A 2 C5 C 0.0179(4) 0.1587(2) 0.4929(2) 0.0348(9) Uani 1 1 d D . . H5 H -0.0015 0.1013 0.4937 0.042 Uiso 0.581(5) 1 calc PR A 1 H5A H 0.0052 0.1009 0.4863 0.042 Uiso 0.419(5) 1 calc PR A 2 C6 C -0.0663(4) 0.2136(2) 0.5212(2) 0.0367(9) Uani 1 1 d D A . H6 H -0.1511 0.2029 0.5402 0.044 Uiso 0.581(5) 1 calc PR A 1 H6A H -0.1452 0.1937 0.5419 0.044 Uiso 0.419(5) 1 calc PR A 2 C8 C 0.3931(3) 0.5473(2) 0.25934(19) 0.0223(7) Uani 1 1 d . . . H8A H 0.4363 0.5478 0.3117 0.027 Uiso 1 1 calc R . . H8B H 0.3871 0.6052 0.2414 0.027 Uiso 1 1 calc R . . C9 C 0.4831(3) 0.49900(19) 0.21020(19) 0.0225(7) Uani 1 1 d . . . H9A H 0.4286 0.4807 0.1639 0.027 Uiso 1 1 calc R . . H9B H 0.5561 0.5355 0.1951 0.027 Uiso 1 1 calc R . . C10 C 0.6291(4) 0.3749(2) 0.20170(19) 0.0241(7) Uani 1 1 d . B . H10A H 0.7072 0.4083 0.1884 0.029 Uiso 1 1 calc R . . H10B H 0.5739 0.3605 0.1544 0.029 Uiso 1 1 calc R . . C11 C 0.6801(3) 0.29715(19) 0.24037(18) 0.0221(7) Uani 1 1 d D . . S2 S 0.81161(19) 0.29485(11) 0.31125(15) 0.0317(6) Uani 0.587(5) 1 d PD B 1 C14 C 0.6317(11) 0.2202(6) 0.2251(6) 0.044(4) Uiso 0.587(5) 1 d PD B 1 H14 H 0.5622 0.2074 0.1866 0.053 Uiso 0.587(5) 1 calc PR B 1 S2A S 0.5960(4) 0.2031(2) 0.22987(18) 0.0347(9) Uani 0.413(5) 1 d PD B 2 C14A C 0.7988(11) 0.2849(7) 0.2840(6) 0.027(3) Uiso 0.413(5) 1 d PD B 2 H14A H 0.8684 0.3250 0.2928 0.032 Uiso 0.413(5) 1 calc PR B 2 C12 C 0.8042(5) 0.1959(2) 0.3173(2) 0.0481(12) Uani 1 1 d D . . H12 H 0.8707 0.1662 0.3482 0.058 Uiso 0.587(5) 1 calc PR B 1 H12A H 0.8657 0.1747 0.3566 0.058 Uiso 0.413(5) 1 calc PR B 2 C13 C 0.7038(4) 0.1567(2) 0.2784(3) 0.0476(12) Uani 1 1 d D B . H13 H 0.6809 0.1001 0.2827 0.057 Uiso 0.587(5) 1 calc PR B 1 H13A H 0.6994 0.0982 0.2810 0.057 Uiso 0.413(5) 1 calc PR B 2 C15 C 0.1695(3) 0.5423(2) 0.19202(19) 0.0224(7) Uani 1 1 d . . . H15A H 0.2248 0.5430 0.1485 0.027 Uiso 1 1 calc R . . H15B H 0.1393 0.5995 0.2005 0.027 Uiso 1 1 calc R . . C16 C 0.0453(3) 0.4878(2) 0.17308(19) 0.0221(7) Uani 1 1 d . . . H16A H 0.0132 0.4659 0.2202 0.027 Uiso 1 1 calc R . . H16B H -0.0287 0.5213 0.1472 0.027 Uiso 1 1 calc R . . C17 C -0.0335(3) 0.3558(2) 0.11053(19) 0.0230(7) Uani 1 1 d . C . H17A H -0.0520 0.3305 0.1591 0.028 Uiso 1 1 calc R . . H17B H -0.1172 0.3838 0.0892 0.028 Uiso 1 1 calc R . . C18 C 0.0050(3) 0.2903(2) 0.0575(2) 0.0307(8) Uani 1 1 d D . . S3 S 0.0543(3) 0.19438(13) 0.07626(13) 0.0418(7) Uani 0.515(4) 1 d PD C 1 C19 C 0.0845(6) 0.1691(5) -0.0101(4) 0.0261(12) Uiso 0.515(4) 1 d PD C 1 H19 H 0.1132 0.1156 -0.0238 0.031 Uiso 0.515(4) 1 calc PR C 1 C20 C 0.0637(8) 0.2337(5) -0.0610(5) 0.0393(14) Uiso 0.515(4) 1 d PD C 1 H20 H 0.0787 0.2310 -0.1129 0.047 Uiso 0.515(4) 1 calc PR C 1 C21 C 0.0149(13) 0.3072(8) -0.0228(7) 0.043(3) Uiso 0.515(4) 1 d PD C 1 H21 H -0.0071 0.3584 -0.0468 0.051 Uiso 0.515(4) 1 calc PR C 1 S3A S 0.0466(3) 0.3010(2) -0.02796(18) 0.0496(10) Uani 0.485(4) 1 d PD C 2 C19A C 0.0767(7) 0.2000(5) -0.0394(5) 0.0261(12) Uiso 0.485(4) 1 d PD C 2 H19A H 0.1080 0.1765 -0.0835 0.031 Uiso 0.485(4) 1 calc PR C 2 C20A C 0.0501(8) 0.1559(5) 0.0234(5) 0.0393(14) Uiso 0.485(4) 1 d PD C 2 H20A H 0.0629 0.0978 0.0262 0.047 Uiso 0.485(4) 1 calc PR C 2 C21A C -0.0012(11) 0.2050(6) 0.0888(6) 0.043(3) Uiso 0.485(4) 1 d PD C 2 H21A H -0.0289 0.1865 0.1356 0.051 Uiso 0.485(4) 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 0.0271(13) 0.0264(12) 0.0203(13) -0.0009(10) 0.0038(10) 0.0031(10) O2 0.0248(13) 0.0253(12) 0.0212(12) 0.0018(9) -0.0040(10) -0.0002(10) O3 0.0212(13) 0.0277(13) 0.0285(13) 0.0001(10) 0.0011(10) -0.0031(10) O4 0.0329(14) 0.0335(14) 0.0228(13) 0.0031(10) 0.0072(11) 0.0009(11) O5 0.0246(13) 0.0488(16) 0.0230(13) -0.0003(11) -0.0044(11) 0.0047(11) O6 0.0183(13) 0.0519(16) 0.0308(14) 0.0165(12) 0.0016(10) 0.0018(11) O7 0.0342(14) 0.0287(13) 0.0226(13) -0.0030(10) 0.0060(11) -0.0048(11) O8 0.0245(13) 0.0405(15) 0.0263(14) -0.0078(11) -0.0058(11) 0.0047(11) O9 0.0189(13) 0.0336(14) 0.0322(14) -0.0029(11) 0.0018(10) 0.0023(10) N1 0.0207(14) 0.0186(13) 0.0201(14) 0.0004(11) 0.0018(11) 0.0007(11) N2 0.0221(15) 0.0215(14) 0.0224(15) 0.0001(11) 0.0017(12) -0.0015(11) N3 0.0203(14) 0.0206(14) 0.0206(14) 0.0020(11) 0.0014(11) 0.0001(11) N4 0.0216(14) 0.0212(14) 0.0187(14) 0.0008(11) -0.0008(11) 0.0020(11) N5 0.0218(15) 0.0158(13) 0.0252(16) 0.0018(11) 0.0004(12) 0.0000(11) N6 0.0249(16) 0.0179(14) 0.0239(16) 0.0017(11) 0.0002(12) 0.0001(11) N7 0.0262(16) 0.0159(13) 0.0254(16) -0.0020(11) 0.0001(12) -0.0011(11) C1 0.0253(17) 0.0178(15) 0.0227(17) -0.0038(13) 0.0028(14) 0.0004(13) C2 0.0263(18) 0.0231(17) 0.0215(17) -0.0010(13) 0.0018(14) -0.0035(14) C3 0.0285(19) 0.0188(16) 0.0225(18) 0.0001(13) 0.0002(14) 0.0015(14) C4 0.0271(19) 0.0267(18) 0.0194(17) 0.0026(14) 0.0010(14) 0.0017(14) S1A 0.0360(18) 0.0301(14) 0.0370(15) 0.0063(10) 0.0129(12) -0.0003(13) C5 0.036(2) 0.032(2) 0.036(2) 0.0062(16) -0.0037(17) 0.0003(16) C6 0.039(2) 0.039(2) 0.033(2) 0.0108(17) 0.0045(18) 0.0020(17) C8 0.0233(18) 0.0197(16) 0.0236(18) 0.0007(13) 0.0005(14) -0.0032(13) C9 0.0236(17) 0.0195(16) 0.0244(18) 0.0027(13) 0.0024(14) 0.0004(13) C10 0.0254(18) 0.0254(18) 0.0223(18) 0.0018(14) 0.0061(14) 0.0039(14) C11 0.0226(17) 0.0202(16) 0.0235(17) -0.0012(13) 0.0023(14) 0.0000(13) S2 0.0339(11) 0.0201(9) 0.0386(14) -0.0010(8) -0.0111(9) 0.0037(6) S2A 0.0281(17) 0.0250(14) 0.0499(18) -0.0010(12) -0.0031(13) -0.0003(13) C12 0.061(3) 0.041(2) 0.039(2) -0.0100(19) -0.011(2) 0.031(2) C13 0.057(3) 0.0191(19) 0.070(3) -0.0044(19) 0.022(2) -0.0050(18) C15 0.0267(18) 0.0175(16) 0.0223(17) 0.0023(13) -0.0004(14) 0.0020(13) C16 0.0229(17) 0.0240(17) 0.0194(17) -0.0018(13) 0.0014(13) 0.0046(13) C17 0.0211(17) 0.0224(16) 0.0252(18) 0.0021(14) 0.0009(14) -0.0014(13) C18 0.0235(19) 0.0250(18) 0.041(2) -0.0057(16) -0.0081(16) 0.0013(14) S3 0.0531(17) 0.0343(12) 0.0368(13) -0.0018(9) -0.0028(11) 0.0053(10) S3A 0.0385(17) 0.0641(18) 0.0497(16) -0.0414(13) 0.0237(13) -0.0241(14) _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 N5 1.258(4) . ? O2 N5 1.260(3) . ? O3 N5 1.254(4) . ? O4 N6 1.241(4) . ? O5 N6 1.243(4) . ? O6 N6 1.266(4) . ? O7 N7 1.244(4) . ? O8 N7 1.260(4) . ? O9 N7 1.253(4) . ? N1 C1 1.478(4) . ? N1 C15 1.479(4) . ? N1 C8 1.479(4) . ? N2 C2 1.494(4) . ? N2 C3 1.505(4) . ? N2 H21N 0.9200 . ? N2 H22N 0.9200 . ? N3 C10 1.499(4) . ? N3 C9 1.501(4) . ? N3 H31N 0.9200 . ? N3 H32N 0.9200 . ? N4 C16 1.493(4) . ? N4 C17 1.499(4) . ? N4 H41N 0.9200 . ? N4 H42N 0.9200 . ? C1 C2 1.519(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.495(5) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 C7 1.317(10) . ? C4 C7A 1.395(10) . ? C4 S1 1.747(4) . ? C4 S1A 1.767(5) . ? S1 C5 1.668(4) . ? C7 C6 1.512(10) . ? C7 H7 0.9500 . ? S1A C6 1.630(5) . ? C7A C5 1.459(10) . ? C7A H7A 0.9500 . ? C5 C6 1.348(5) . ? C5 H5 0.9500 . ? C5 H5A 0.9500 . ? C6 H6 0.9500 . ? C6 H6A 0.9500 . ? C8 C9 1.522(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.501(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C14 1.353(10) . ? C11 C14A 1.363(10) . ? C11 S2 1.730(4) . ? C11 S2A 1.737(5) . ? S2 C12 1.607(4) . ? C14 C13 1.532(10) . ? C14 H14 0.9500 . ? S2A C13 1.512(5) . ? C14A C12 1.557(10) . ? C14A H14A 0.9500 . ? C12 C13 1.321(6) . ? C12 H12 0.9500 . ? C12 H12A 0.9500 . ? C13 H13 0.9500 . ? C13 H13A 0.9500 . ? C15 C16 1.526(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.494(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C21 1.471(12) . ? C18 C21A 1.493(10) . ? C18 S3A 1.624(5) . ? C18 S3 1.652(4) . ? S3 C19 1.647(7) . ? C19 C20 1.388(10) . ? C19 H19 0.9500 . ? C20 C21 1.473(12) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? S3A C19A 1.679(8) . ? C19A C20A 1.374(11) . ? C19A H19A 0.9500 . ? C20A C21A 1.536(11) . ? C20A H20A 0.9500 . ? C21A H21A 0.9500 . ? 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 C1 N1 C15 109.0(3) . . ? C1 N1 C8 109.6(3) . . ? C15 N1 C8 110.0(2) . . ? C2 N2 C3 111.6(2) . . ? C2 N2 H21N 109.3 . . ? C3 N2 H21N 109.3 . . ? C2 N2 H22N 109.3 . . ? C3 N2 H22N 109.3 . . ? H21N N2 H22N 108.0 . . ? C10 N3 C9 112.1(2) . . ? C10 N3 H31N 109.2 . . ? C9 N3 H31N 109.2 . . ? C10 N3 H32N 109.2 . . ? C9 N3 H32N 109.2 . . ? H31N N3 H32N 107.9 . . ? C16 N4 C17 113.5(3) . . ? C16 N4 H41N 108.9 . . ? C17 N4 H41N 108.9 . . ? C16 N4 H42N 108.9 . . ? C17 N4 H42N 108.9 . . ? H41N N4 H42N 107.7 . . ? O3 N5 O1 120.3(3) . . ? O3 N5 O2 120.1(3) . . ? O1 N5 O2 119.6(3) . . ? O4 N6 O5 121.9(3) . . ? O4 N6 O6 119.5(3) . . ? O5 N6 O6 118.6(3) . . ? O7 N7 O9 120.5(3) . . ? O7 N7 O8 120.0(3) . . ? O9 N7 O8 119.6(3) . . ? N1 C1 C2 113.5(3) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C1 111.7(3) . . ? N2 C2 H2C 109.3 . . ? C1 C2 H2C 109.3 . . ? N2 C2 H2D 109.3 . . ? C1 C2 H2D 109.3 . . ? H2C C2 H2D 107.9 . . ? C4 C3 N2 111.7(3) . . ? C4 C3 H3C 109.3 . . ? N2 C3 H3C 109.3 . . ? C4 C3 H3D 109.3 . . ? N2 C3 H3D 109.3 . . ? H3C C3 H3D 107.9 . . ? C7 C4 C7A 100.6(6) . . ? C7 C4 C3 128.9(5) . . ? C7A C4 C3 129.9(5) . . ? C7 C4 S1 111.6(5) . . ? C3 C4 S1 119.5(3) . . ? C7A C4 S1A 108.9(5) . . ? C3 C4 S1A 121.1(3) . . ? S1 C4 S1A 119.4(2) . . ? C5 S1 C4 89.7(2) . . ? C4 C7 C6 114.7(7) . . ? C4 C7 H7 122.7 . . ? C6 C7 H7 122.7 . . ? C6 S1A C4 89.0(3) . . ? C4 C7A C5 115.2(8) . . ? C4 C7A H7A 122.4 . . ? C5 C7A H7A 122.4 . . ? C6 C5 C7A 104.0(5) . . ? C6 C5 S1 119.0(3) . . ? C6 C5 H5 120.5 . . ? C7A C5 H5 135.1 . . ? S1 C5 H5 120.5 . . ? C6 C5 H5A 128.0 . . ? C7A C5 H5A 128.0 . . ? S1 C5 H5A 112.7 . . ? C5 C6 C7 104.8(5) . . ? C5 C6 S1A 122.5(4) . . ? C5 C6 H6 127.6 . . ? C7 C6 H6 127.6 . . ? S1A C6 H6 109.8 . . ? C5 C6 H6A 118.8 . . ? C7 C6 H6A 136.2 . . ? S1A C6 H6A 118.8 . . ? N1 C8 C9 113.9(3) . . ? N1 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N3 C9 C8 111.7(3) . . ? N3 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? N3 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? N3 C10 C11 111.6(3) . . ? N3 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N3 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C14 C11 C14A 104.6(7) . . ? C14 C11 C10 125.6(5) . . ? C14A C11 C10 128.4(5) . . ? C14 C11 S2 110.9(5) . . ? C10 C11 S2 123.6(2) . . ? C14A C11 S2A 108.3(5) . . ? C10 C11 S2A 123.2(3) . . ? S2 C11 S2A 112.4(2) . . ? C12 S2 C11 92.0(2) . . ? C11 C14 C13 110.9(7) . . ? C11 C14 H14 124.6 . . ? C13 C14 H14 124.6 . . ? C13 S2A C11 93.8(3) . . ? C11 C14A C12 110.5(7) . . ? C11 C14A H14A 124.8 . . ? C12 C14A H14A 124.8 . . ? C13 C12 C14A 104.3(5) . . ? C13 C12 S2 118.7(3) . . ? C14A C12 S2 18.7(4) . . ? C13 C12 H12 120.6 . . ? C14A C12 H12 133.4 . . ? S2 C12 H12 120.6 . . ? C13 C12 H12A 127.9 . . ? C14A C12 H12A 127.9 . . ? S2 C12 H12A 112.3 . . ? C12 C13 S2A 121.3(3) . . ? C12 C13 C14 106.8(5) . . ? C12 C13 H13 126.6 . . ? S2A C13 H13 111.3 . . ? C14 C13 H13 126.6 . . ? C12 C13 H13A 119.3 . . ? S2A C13 H13A 119.3 . . ? C14 C13 H13A 132.7 . . ? N1 C15 C16 112.7(3) . . ? N1 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N1 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N4 C16 C15 110.6(3) . . ? N4 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C18 C17 N4 110.1(3) . . ? C18 C17 H17A 109.6 . . ? N4 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? N4 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C21 C18 C21A 123.0(7) . . ? C21 C18 C17 121.8(6) . . ? C21A C18 C17 113.5(5) . . ? C21A C18 S3A 118.2(5) . . ? C17 C18 S3A 128.2(3) . . ? C21 C18 S3 109.1(5) . . ? C17 C18 S3 128.9(3) . . ? S3A C18 S3 101.2(3) . . ? C19 S3 C18 96.9(3) . . ? C20 C19 S3 113.2(5) . . ? C20 C19 H19 123.4 . . ? S3 C19 H19 123.4 . . ? C19 C20 C21 110.0(8) . . ? C19 C20 H20 125.0 . . ? C21 C20 H20 125.0 . . ? C18 C21 C20 110.7(9) . . ? C18 C21 H21 124.7 . . ? C20 C21 H21 124.7 . . ? C18 S3A C19A 94.2(4) . . ? C20A C19A S3A 111.0(6) . . ? C20A C19A H19A 124.5 . . ? S3A C19A H19A 124.5 . . ? C19A C20A C21A 116.8(7) . . ? C19A C20A H20A 121.6 . . ? C21A C20A H20A 121.6 . . ? C18 C21A C20A 99.6(7) . . ? C18 C21A H21A 130.2 . . ? C20A C21A H21A 130.2 . . ? 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 C15 N1 C1 C2 159.3(3) . . . . ? C8 N1 C1 C2 -80.4(3) . . . . ? C3 N2 C2 C1 172.1(3) . . . . ? N1 C1 C2 N2 -85.6(3) . . . . ? C2 N2 C3 C4 171.6(3) . . . . ? N2 C3 C4 C7 -75.4(6) . . . . ? N2 C3 C4 C7A 115.6(6) . . . . ? N2 C3 C4 S1 107.7(3) . . . . ? N2 C3 C4 S1A -69.6(4) . . . . ? C7 C4 S1 C5 -0.2(5) . . . . ? C7A C4 S1 C5 26.9(18) . . . . ? C3 C4 S1 C5 177.2(3) . . . . ? S1A C4 S1 C5 -5.5(3) . . . . ? C7A C4 C7 C6 -8.1(8) . . . . ? C3 C4 C7 C6 -179.5(4) . . . . ? S1 C4 C7 C6 -2.4(8) . . . . ? S1A C4 C7 C6 148(3) . . . . ? C7 C4 S1A C6 -27(3) . . . . ? C7A C4 S1A C6 -1.5(4) . . . . ? C3 C4 S1A C6 -177.3(3) . . . . ? S1 C4 S1A C6 5.4(3) . . . . ? C7 C4 C7A C5 9.3(8) . . . . ? C3 C4 C7A C5 -179.4(4) . . . . ? S1 C4 C7A C5 -145(2) . . . . ? S1A C4 C7A C5 5.4(8) . . . . ? C4 C7A C5 C6 -7.0(8) . . . . ? C4 C7A C5 S1 152.7(19) . . . . ? C4 S1 C5 C6 3.3(3) . . . . ? C4 S1 C5 C7A -19.4(13) . . . . ? C7A C5 C6 C7 1.5(6) . . . . ? S1 C5 C6 C7 -4.8(5) . . . . ? C7A C5 C6 S1A 6.2(6) . . . . ? S1 C5 C6 S1A -0.1(4) . . . . ? C4 C7 C6 C5 4.4(8) . . . . ? C4 C7 C6 S1A -162.8(19) . . . . ? C4 S1A C6 C5 -3.1(4) . . . . ? C4 S1A C6 C7 11.5(13) . . . . ? C1 N1 C8 C9 158.7(3) . . . . ? C15 N1 C8 C9 -81.6(3) . . . . ? C10 N3 C9 C8 177.5(3) . . . . ? N1 C8 C9 N3 -82.9(3) . . . . ? C9 N3 C10 C11 -174.8(3) . . . . ? N3 C10 C11 C14 105.0(6) . . . . ? N3 C10 C11 C14A -91.1(7) . . . . ? N3 C10 C11 S2 -75.3(4) . . . . ? N3 C10 C11 S2A 93.7(3) . . . . ? C14 C11 S2 C12 1.8(5) . . . . ? C14A C11 S2 C12 -63(2) . . . . ? C10 C11 S2 C12 -177.9(3) . . . . ? S2A C11 S2 C12 12.1(3) . . . . ? C14A C11 C14 C13 15.7(8) . . . . ? C10 C11 C14 C13 -177.3(4) . . . . ? S2 C11 C14 C13 3.0(8) . . . . ? S2A C11 C14 C13 -98(3) . . . . ? C14 C11 S2A C13 70(3) . . . . ? C14A C11 S2A C13 1.1(5) . . . . ? C10 C11 S2A C13 177.2(3) . . . . ? S2 C11 S2A C13 -12.7(3) . . . . ? C14 C11 C14A C12 -17.7(9) . . . . ? C10 C11 C14A C12 175.8(4) . . . . ? S2 C11 C14A C12 102(2) . . . . ? S2A C11 C14A C12 -8.4(8) . . . . ? C11 C14A C12 C13 13.3(8) . . . . ? C11 C14A C12 S2 -129.3(17) . . . . ? C11 S2 C12 C13 -7.3(4) . . . . ? C11 S2 C12 C14A 34.9(13) . . . . ? C14A C12 C13 S2A -13.8(6) . . . . ? S2 C12 C13 S2A -1.0(6) . . . . ? C14A C12 C13 C14 -3.1(7) . . . . ? S2 C12 C13 C14 9.7(6) . . . . ? C11 S2A C13 C12 8.6(4) . . . . ? C11 S2A C13 C14 -27.6(15) . . . . ? C11 C14 C13 C12 -7.7(8) . . . . ? C11 C14 C13 S2A 141(2) . . . . ? C1 N1 C15 C16 -80.5(3) . . . . ? C8 N1 C15 C16 159.3(3) . . . . ? C17 N4 C16 C15 172.8(3) . . . . ? N1 C15 C16 N4 -87.8(3) . . . . ? C16 N4 C17 C18 177.2(3) . . . . ? N4 C17 C18 C21 -70.2(7) . . . . ? N4 C17 C18 C21A 123.8(5) . . . . ? N4 C17 C18 S3A -58.3(4) . . . . ? N4 C17 C18 S3 104.3(4) . . . . ? C21 C18 S3 C19 -1.6(6) . . . . ? C21A C18 S3 C19 130.5(11) . . . . ? C17 C18 S3 C19 -176.6(4) . . . . ? S3A C18 S3 C19 -10.5(3) . . . . ? C18 S3 C19 C20 2.2(5) . . . . ? S3 C19 C20 C21 -2.0(9) . . . . ? C21A C18 C21 C20 -19.3(12) . . . . ? C17 C18 C21 C20 176.1(6) . . . . ? S3A C18 C21 C20 50(3) . . . . ? S3 C18 C21 C20 0.6(9) . . . . ? C19 C20 C21 C18 0.9(11) . . . . ? C21 C18 S3A C19A -122(3) . . . . ? C21A C18 S3A C19A -4.2(5) . . . . ? C17 C18 S3A C19A 178.0(4) . . . . ? S3 C18 S3A C19A 11.8(3) . . . . ? C18 S3A C19A C20A 1.9(5) . . . . ? S3A C19A C20A C21A 0.6(9) . . . . ? C21 C18 C21A C20A 17.0(10) . . . . ? C17 C18 C21A C20A -177.3(5) . . . . ? S3A C18 C21A C20A 4.6(7) . . . . ? S3 C18 C21A C20A -39.9(8) . . . . ? C19A C20A C21A C18 -3.1(9) . . . . ? 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 N2 H21N O3 0.92 1.98 2.895(4) 175.9 . N2 H21N O2 0.92 2.42 3.010(4) 121.9 . N2 H22N O8 0.92 1.96 2.869(4) 168.2 . N3 H32N O2 0.92 1.93 2.846(4) 171.4 . N3 H32N O1 0.92 2.38 3.044(4) 129.0 . N3 H31N O7 0.92 2.51 3.207(4) 132.3 1_655 N3 H31N O9 0.92 2.00 2.912(4) 170.6 1_655 N4 H41N O1 0.92 1.96 2.877(3) 171.7 . N4 H41N O3 0.92 2.52 3.058(4) 117.7 . N4 H42N O6 0.92 1.85 2.768(4) 172.7 . N4 H42N O5 0.92 2.56 3.196(4) 126.3 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.79 _refine_diff_density_min -0.83 _refine_diff_density_rms 0.083 # END OF CIF