data_007a-20018 _vrf_RINTA01_007a-20018 ; PROBLEM: RESPONSE: The crystal was twinned, the reflections were weak, and the diffraction was not ideal diffraction. ; _vrf_PLAT430_007a-20018 ; PROBLEM: RESPONSE: All non-hydrogen atoms were found in the difference map and freely refined. ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H2 N3 O9 S, C16 H26 N, 0.5(C7 H8)' _chemical_formula_sum 'C25.50 H32 N4 O9 S' _chemical_formula_weight 570.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.09190(10) _cell_length_b 21.6444(3) _cell_length_c 15.4490(2) _cell_angle_alpha 90 _cell_angle_beta 90.1140(10) _cell_angle_gamma 90 _cell_volume 2705.80(6) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 41131 _cell_measurement_theta_min 3.0680 _cell_measurement_theta_max 66.5540 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_F_000 1204 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.160 _exptl_absorpt_coefficient_mu 1.583 _shelx_estimated_absorpt_T_min 0.722 _shelx_estimated_absorpt_T_max 0.786 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'microfocus rotating anode' _diffrn_measurement_device_type 'Rigaku Saturn 944+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 22.2 _diffrn_reflns_number 4779 _diffrn_reflns_av_unetI/netI 0.0472 _diffrn_reflns_av_R_equivalents 0.1818 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.515 _diffrn_reflns_theta_max 66.639 _diffrn_reflns_theta_full 66.639 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 4779 _reflns_number_gt 4483 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_cell_refinement 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'CIFTAB-2014/2 (Sheldrick, 2014)' _refine_special_details ; This data was refined as a 2-component twin. The fractional volume contribution of the minor twin component was freely refined to a converged value of 0.2331(16). 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. The hydrogen atoms were first found in the difference map, then generated geometrically and refined as riding atoms with C-H distances = 0.95 - 0.99 angstroms and Uiso(H) = 1.2 times Ueq(C) for CH and CH2 groups and Uiso(H) = 1.5 times Ueq(C) for CH3 groups. The only exception is H1, which was found in the difference map and freely refined. The toluene crystallized near the inversion center. The best model was obtained by suppressing the special position constraints and placing a whole model toluene (see Guzei, I. A. (2014). J. Appl. Crystallogr. 47, 806-809). The model was then allowed to freely refine at half occupancy. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+4.8493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary SHELXT _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4779 _refine_ls_number_parameters 384 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.22499(11) 0.87279(4) 1.01892(5) 0.0238(2) Uani 1 1 d . . . . . O1 O 0.2968(3) 0.84645(12) 0.94266(15) 0.0288(6) Uani 1 1 d . . . . . O2 O 0.0561(3) 0.85579(13) 1.03446(19) 0.0352(6) Uani 1 1 d . . . . . O3 O 0.3277(4) 0.86797(12) 1.09595(17) 0.0322(6) Uani 1 1 d . . . . . O4 O 0.4356(3) 0.98881(14) 1.17821(17) 0.0369(7) Uani 1 1 d . . . . . O5 O 0.1719(3) 0.97297(13) 1.18842(16) 0.0337(6) Uani 1 1 d . . . . . O6 O 0.3264(3) 1.18041(12) 0.99070(18) 0.0339(6) Uani 1 1 d . . . . . O7 O 0.2508(3) 1.16213(12) 0.85873(17) 0.0329(6) Uani 1 1 d . . . . . O8 O 0.0212(3) 0.90471(13) 0.85420(18) 0.0357(6) Uani 1 1 d . . . . . O9 O 0.2153(4) 0.94062(15) 0.77269(18) 0.0482(8) Uani 1 1 d . . . . . N2 N 0.2968(4) 0.98434(14) 1.14788(19) 0.0274(7) Uani 1 1 d . . . . . N3 N 0.2833(4) 1.14609(14) 0.93266(19) 0.0269(7) Uani 1 1 d . . . . . N4 N 0.1414(4) 0.93734(15) 0.8408(2) 0.0299(7) Uani 1 1 d . . . . . C17 C 0.2251(4) 0.95518(16) 0.9950(2) 0.0222(7) Uani 1 1 d . . . . . C18 C 0.1975(4) 0.97796(17) 0.9116(2) 0.0244(7) Uani 1 1 d . . . . . C19 C 0.2173(4) 1.03955(16) 0.8889(2) 0.0247(7) Uani 1 1 d . . . . . H19 H 0.1971 1.0534 0.8315 0.030 Uiso 1 1 calc R U . . . C20 C 0.2676(4) 1.07998(16) 0.9529(2) 0.0246(7) Uani 1 1 d . . . . . C21 C 0.2982(4) 1.06111(16) 1.0361(2) 0.0255(7) Uani 1 1 d . . . . . H21 H 0.3336 1.0896 1.0791 0.031 Uiso 1 1 calc R U . . . C22 C 0.2758(4) 0.99940(16) 1.0554(2) 0.0235(7) Uani 1 1 d . . . . . N1 N 0.1891(4) 0.73039(14) 0.72043(18) 0.0239(6) Uani 1 1 d . . . . . H1 H 0.217(5) 0.698(2) 0.681(3) 0.035(11) Uiso 1 1 d . . . . . C1 C 0.1032(5) 0.77553(18) 0.6611(2) 0.0295(8) Uani 1 1 d . . . . . H1A H 0.0672 0.8120 0.6947 0.035 Uiso 1 1 calc R U . . . H1B H 0.0038 0.7558 0.6358 0.035 Uiso 1 1 calc R U . . . C2 C 0.2172(5) 0.79589(17) 0.5892(2) 0.0297(8) Uani 1 1 d . . . . . H2A H 0.1612 0.8281 0.5544 0.036 Uiso 1 1 calc R U . . . H2B H 0.2395 0.7603 0.5508 0.036 Uiso 1 1 calc R U . . . C3 C 0.3815(5) 0.82150(17) 0.6226(2) 0.0264(8) Uani 1 1 d . . . . . H3 H 0.3584 0.8601 0.6560 0.032 Uiso 1 1 calc R U . . . C4 C 0.4630(4) 0.77417(17) 0.6844(2) 0.0241(7) Uani 1 1 d . . . . . H4 H 0.4796 0.7351 0.6509 0.029 Uiso 1 1 calc R U . . . C5 C 0.3464(4) 0.75913(17) 0.7601(2) 0.0241(7) Uani 1 1 d . . . . . H5 H 0.3147 0.7989 0.7885 0.029 Uiso 1 1 calc R U . . . C6 C 0.4920(5) 0.83787(19) 0.5470(2) 0.0332(9) Uani 1 1 d . . . . . H6A H 0.5294 0.7999 0.5185 0.050 Uiso 1 1 calc R U . . . H6B H 0.5879 0.8611 0.5679 0.050 Uiso 1 1 calc R U . . . H6C H 0.4300 0.8632 0.5055 0.050 Uiso 1 1 calc R U . . . C7 C 0.6334(5) 0.79547(18) 0.7162(2) 0.0293(8) Uani 1 1 d . . . . . H7A H 0.6816 0.7625 0.7528 0.035 Uiso 1 1 calc R U . . . H7B H 0.7064 0.8008 0.6654 0.035 Uiso 1 1 calc R U . . . C8 C 0.6324(5) 0.8554(2) 0.7676(3) 0.0411(10) Uani 1 1 d . . . . . H8A H 0.5904 0.8889 0.7311 0.062 Uiso 1 1 calc R U . . . H8B H 0.7451 0.8651 0.7866 0.062 Uiso 1 1 calc R U . . . H8C H 0.5610 0.8507 0.8183 0.062 Uiso 1 1 calc R U . . . C9 C 0.4164(5) 0.71642(18) 0.8293(2) 0.0277(8) Uani 1 1 d . . . . . H9A H 0.5137 0.7368 0.8557 0.033 Uiso 1 1 calc R U . . . H9B H 0.3324 0.7116 0.8753 0.033 Uiso 1 1 calc R U . . . C10 C 0.4681(5) 0.65245(18) 0.7991(2) 0.0317(9) Uani 1 1 d . . . . . H10A H 0.5531 0.6563 0.7543 0.048 Uiso 1 1 calc R U . . . H10B H 0.3720 0.6307 0.7752 0.048 Uiso 1 1 calc R U . . . H10C H 0.5126 0.6291 0.8482 0.048 Uiso 1 1 calc R U . . . C11 C 0.0731(4) 0.70589(18) 0.7856(2) 0.0253(8) Uani 1 1 d . . . . . C12 C 0.0262(5) 0.64511(19) 0.7774(2) 0.0310(8) Uani 1 1 d . . . . . H12 H 0.0653 0.6209 0.7304 0.037 Uiso 1 1 calc R U . . . C13 C -0.0786(5) 0.6197(2) 0.8384(3) 0.0388(10) Uani 1 1 d . . . . . H13 H -0.1110 0.5777 0.8339 0.047 Uiso 1 1 calc R U . . . C14 C -0.1359(5) 0.6557(2) 0.9057(3) 0.0381(10) Uani 1 1 d . . . . . H14 H -0.2075 0.6384 0.9478 0.046 Uiso 1 1 calc R U . . . C15 C -0.0892(5) 0.7171(2) 0.9119(3) 0.0352(9) Uani 1 1 d . . . . . H15 H -0.1302 0.7418 0.9579 0.042 Uiso 1 1 calc R U . . . C16 C 0.0168(5) 0.7428(2) 0.8517(2) 0.0304(8) Uani 1 1 d . . . . . H16 H 0.0499 0.7848 0.8560 0.036 Uiso 1 1 calc R U . . . C23 C 0.757(3) 1.0071(14) 0.5665(17) 0.163(9) Uani 0.5 1 d . U P A -1 H23A H 0.7490 1.0071 0.6298 0.244 Uiso 0.5 1 calc R U P A -1 H23B H 0.8254 0.9721 0.5479 0.244 Uiso 0.5 1 calc R U P A -1 H23C H 0.8086 1.0458 0.5473 0.244 Uiso 0.5 1 calc R U P A -1 C24 C 0.5835(13) 1.0014(6) 0.5266(9) 0.102(4) Uani 0.5 1 d G U P A -1 C25 C 0.5465(15) 0.9999(5) 0.4388(8) 0.096(4) Uani 0.5 1 d G U P A -1 H25 H 0.6321 1.0047 0.3973 0.116 Uiso 0.5 1 calc R U P A -1 C26 C 0.3842(18) 0.9914(4) 0.4116(6) 0.095(4) Uani 0.5 1 d G U P A -1 H26 H 0.3589 0.9903 0.3515 0.114 Uiso 0.5 1 calc R U P A -1 C27 C 0.2590(13) 0.9844(4) 0.4723(9) 0.106(4) Uani 0.5 1 d G U P A -1 H27 H 0.1481 0.9786 0.4537 0.128 Uiso 0.5 1 calc R U P A -1 C28 C 0.2961(14) 0.9859(4) 0.5601(8) 0.102(4) Uani 0.5 1 d G U P A -1 H28 H 0.2105 0.9812 0.6016 0.123 Uiso 0.5 1 calc R U P A -1 C29 C 0.4583(17) 0.9944(5) 0.5873(6) 0.088(4) Uani 0.5 1 d G U P A -1 H29 H 0.4836 0.9955 0.6474 0.106 Uiso 0.5 1 calc R U P A -1 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 S1 0.0249(4) 0.0230(4) 0.0234(4) 0.0003(3) 0.0005(3) 0.0006(3) O1 0.0321(14) 0.0278(13) 0.0264(13) -0.0029(10) -0.0021(11) 0.0043(12) O2 0.0259(14) 0.0306(14) 0.0492(17) 0.0033(13) 0.0085(12) -0.0040(11) O3 0.0437(16) 0.0257(14) 0.0273(13) 0.0026(11) 0.0009(12) 0.0037(12) O4 0.0358(16) 0.0444(17) 0.0303(14) -0.0001(12) -0.0107(12) 0.0011(13) O5 0.0382(15) 0.0365(15) 0.0264(13) 0.0012(11) 0.0082(12) 0.0002(13) O6 0.0364(15) 0.0246(13) 0.0409(15) -0.0042(12) 0.0024(13) -0.0040(11) O7 0.0374(15) 0.0315(14) 0.0298(14) 0.0082(11) 0.0022(12) -0.0023(12) O8 0.0327(15) 0.0332(15) 0.0411(16) -0.0012(12) -0.0099(12) -0.0045(12) O9 0.062(2) 0.0552(19) 0.0275(15) -0.0118(13) 0.0050(15) -0.0120(17) N2 0.0331(17) 0.0245(15) 0.0246(15) -0.0027(12) -0.0005(14) 0.0009(14) N3 0.0228(15) 0.0275(16) 0.0303(16) 0.0003(13) 0.0043(13) -0.0013(13) N4 0.0334(17) 0.0289(17) 0.0273(16) -0.0019(13) -0.0056(14) 0.0014(14) C17 0.0174(16) 0.0251(17) 0.0241(17) -0.0003(14) -0.0004(14) -0.0004(14) C18 0.0232(17) 0.0277(18) 0.0222(17) -0.0048(14) -0.0015(14) -0.0008(15) C19 0.0239(17) 0.0295(19) 0.0207(16) 0.0040(14) -0.0012(14) 0.0012(15) C20 0.0238(17) 0.0228(17) 0.0271(17) -0.0012(14) 0.0026(14) -0.0005(14) C21 0.0223(16) 0.0270(19) 0.0271(18) -0.0047(14) 0.0029(15) -0.0020(15) C22 0.0191(16) 0.0268(18) 0.0246(17) -0.0016(14) 0.0024(14) 0.0006(15) N1 0.0249(15) 0.0239(15) 0.0228(14) -0.0017(12) -0.0020(12) 0.0006(12) C1 0.0278(19) 0.029(2) 0.031(2) 0.0016(16) -0.0080(16) 0.0032(16) C2 0.035(2) 0.0280(19) 0.0257(18) 0.0009(15) -0.0056(16) 0.0015(17) C3 0.0305(19) 0.0230(18) 0.0256(18) -0.0041(15) -0.0034(15) -0.0007(15) C4 0.0247(17) 0.0261(18) 0.0216(17) -0.0024(14) -0.0007(14) 0.0003(15) C5 0.0211(16) 0.0288(19) 0.0224(17) -0.0053(15) -0.0042(14) -0.0016(15) C6 0.042(2) 0.029(2) 0.0285(19) -0.0009(16) 0.0028(17) -0.0025(18) C7 0.0244(18) 0.034(2) 0.0295(19) -0.0056(16) 0.0005(15) -0.0041(16) C8 0.031(2) 0.051(3) 0.042(2) -0.017(2) -0.0021(18) -0.0097(19) C9 0.0239(17) 0.036(2) 0.0234(18) 0.0001(16) -0.0001(14) -0.0024(16) C10 0.033(2) 0.035(2) 0.0270(19) 0.0055(16) -0.0010(16) 0.0063(17) C11 0.0189(16) 0.034(2) 0.0231(17) -0.0014(15) -0.0012(14) 0.0008(15) C12 0.0302(19) 0.035(2) 0.0281(19) -0.0051(17) -0.0006(16) -0.0026(17) C13 0.038(2) 0.043(2) 0.035(2) -0.0004(19) 0.0048(18) -0.0093(19) C14 0.027(2) 0.056(3) 0.031(2) 0.0033(19) 0.0039(17) -0.0028(19) C15 0.0284(19) 0.048(3) 0.029(2) -0.0073(18) -0.0008(16) 0.0077(18) C16 0.0267(18) 0.036(2) 0.0280(19) -0.0018(16) -0.0008(15) 0.0011(17) C23 0.163(11) 0.15(2) 0.174(16) -0.001(15) -0.047(11) 0.002(11) C24 0.143(9) 0.042(7) 0.121(8) -0.011(6) -0.033(7) 0.017(7) C25 0.155(10) 0.027(7) 0.107(8) -0.004(6) -0.023(7) 0.020(7) C26 0.157(10) 0.028(6) 0.100(8) -0.008(6) -0.032(7) 0.020(7) C27 0.148(10) 0.034(6) 0.136(8) -0.010(6) -0.037(8) 0.030(7) C28 0.145(9) 0.039(6) 0.123(8) -0.016(6) -0.029(7) 0.031(7) C29 0.147(9) 0.031(7) 0.086(8) -0.008(5) -0.035(7) 0.021(6) _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 S1 O1 1.433(3) . ? S1 O2 1.436(3) . ? S1 O3 1.454(3) . ? S1 C17 1.821(3) . ? O4 N2 1.220(4) . ? O5 N2 1.215(4) . ? O6 N3 1.215(4) . ? O7 N3 1.222(4) . ? O8 N4 1.219(4) . ? O9 N4 1.214(4) . ? N2 C22 1.475(4) . ? N3 C20 1.470(5) . ? N4 C18 1.474(5) . ? C17 C18 1.397(5) . ? C17 C22 1.398(5) . ? C18 C19 1.388(5) . ? C19 C20 1.381(5) . ? C19 H19 0.9500 . ? C20 C21 1.370(5) . ? C21 C22 1.380(5) . ? C21 H21 0.9500 . ? N1 C11 1.477(5) . ? N1 C1 1.509(4) . ? N1 C5 1.542(4) . ? N1 H1 0.96(5) . ? C1 C2 1.510(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.529(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C6 1.515(5) . ? C3 C4 1.547(5) . ? C3 H3 1.0000 . ? C4 C7 1.534(5) . ? C4 C5 1.538(5) . ? C4 H4 1.0000 . ? C5 C9 1.522(5) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.521(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.520(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.375(5) . ? C11 C12 1.375(6) . ? C12 C13 1.382(6) . ? C12 H12 0.9500 . ? C13 C14 1.381(6) . ? C13 H13 0.9500 . ? C14 C15 1.385(6) . ? C14 H14 0.9500 . ? C15 C16 1.383(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C23 C24 1.54(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 H29 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 O1 S1 O2 115.02(17) . . ? O1 S1 O3 114.36(15) . . ? O2 S1 O3 112.80(17) . . ? O1 S1 C17 102.85(15) . . ? O2 S1 C17 106.58(16) . . ? O3 S1 C17 103.66(15) . . ? O5 N2 O4 125.8(3) . . ? O5 N2 C22 116.7(3) . . ? O4 N2 C22 117.3(3) . . ? O6 N3 O7 125.2(3) . . ? O6 N3 C20 117.6(3) . . ? O7 N3 C20 117.2(3) . . ? O9 N4 O8 125.1(3) . . ? O9 N4 C18 117.2(3) . . ? O8 N4 C18 117.7(3) . . ? C18 C17 C22 114.8(3) . . ? C18 C17 S1 122.2(3) . . ? C22 C17 S1 122.4(3) . . ? C19 C18 C17 123.6(3) . . ? C19 C18 N4 114.9(3) . . ? C17 C18 N4 121.5(3) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 H19 121.2 . . ? C18 C19 H19 121.2 . . ? C21 C20 C19 122.3(3) . . ? C21 C20 N3 118.3(3) . . ? C19 C20 N3 119.3(3) . . ? C20 C21 C22 117.8(3) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? C21 C22 C17 123.8(3) . . ? C21 C22 N2 114.1(3) . . ? C17 C22 N2 121.9(3) . . ? C11 N1 C1 110.7(3) . . ? C11 N1 C5 113.5(3) . . ? C1 N1 C5 111.0(3) . . ? C11 N1 H1 108(3) . . ? C1 N1 H1 102(3) . . ? C5 N1 H1 111(3) . . ? N1 C1 C2 110.8(3) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C1 C2 C3 112.9(3) . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C6 C3 C2 109.8(3) . . ? C6 C3 C4 112.3(3) . . ? C2 C3 C4 109.7(3) . . ? C6 C3 H3 108.3 . . ? C2 C3 H3 108.3 . . ? C4 C3 H3 108.3 . . ? C7 C4 C5 111.9(3) . . ? C7 C4 C3 112.3(3) . . ? C5 C4 C3 110.3(3) . . ? C7 C4 H4 107.3 . . ? C5 C4 H4 107.3 . . ? C3 C4 H4 107.3 . . ? C9 C5 C4 115.7(3) . . ? C9 C5 N1 109.9(3) . . ? C4 C5 N1 106.9(3) . . ? C9 C5 H5 108.0 . . ? C4 C5 H5 108.0 . . ? N1 C5 H5 108.0 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C4 114.7(3) . . ? C8 C7 H7A 108.6 . . ? C4 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? C4 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C5 116.1(3) . . ? C10 C9 H9A 108.3 . . ? C5 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C5 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 122.2(4) . . ? C16 C11 N1 120.7(3) . . ? C12 C11 N1 117.1(3) . . ? C11 C12 C13 119.1(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 119.8(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 120.1(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.5(4) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C11 C16 C15 118.3(4) . . ? C11 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 120.0 . . ? C25 C24 C23 126.0(13) . . ? C29 C24 C23 113.9(13) . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C24 120.0 . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 S1 C17 C18 35.4(3) . . . . ? O2 S1 C17 C18 -85.9(3) . . . . ? O3 S1 C17 C18 154.8(3) . . . . ? O1 S1 C17 C22 -135.1(3) . . . . ? O2 S1 C17 C22 103.6(3) . . . . ? O3 S1 C17 C22 -15.7(3) . . . . ? C22 C17 C18 C19 -0.3(5) . . . . ? S1 C17 C18 C19 -171.5(3) . . . . ? C22 C17 C18 N4 -179.2(3) . . . . ? S1 C17 C18 N4 9.6(5) . . . . ? O9 N4 C18 C19 49.4(5) . . . . ? O8 N4 C18 C19 -128.1(4) . . . . ? O9 N4 C18 C17 -131.6(4) . . . . ? O8 N4 C18 C17 50.8(5) . . . . ? C17 C18 C19 C20 0.2(6) . . . . ? N4 C18 C19 C20 179.1(3) . . . . ? C18 C19 C20 C21 0.3(5) . . . . ? C18 C19 C20 N3 -177.4(3) . . . . ? O6 N3 C20 C21 1.6(5) . . . . ? O7 N3 C20 C21 -177.9(3) . . . . ? O6 N3 C20 C19 179.4(3) . . . . ? O7 N3 C20 C19 -0.2(5) . . . . ? C19 C20 C21 C22 -0.6(5) . . . . ? N3 C20 C21 C22 177.1(3) . . . . ? C20 C21 C22 C17 0.4(5) . . . . ? C20 C21 C22 N2 -174.7(3) . . . . ? C18 C17 C22 C21 0.0(5) . . . . ? S1 C17 C22 C21 171.2(3) . . . . ? C18 C17 C22 N2 174.8(3) . . . . ? S1 C17 C22 N2 -14.1(5) . . . . ? O5 N2 C22 C21 106.6(4) . . . . ? O4 N2 C22 C21 -68.2(4) . . . . ? O5 N2 C22 C17 -68.7(4) . . . . ? O4 N2 C22 C17 116.6(4) . . . . ? C11 N1 C1 C2 -174.5(3) . . . . ? C5 N1 C1 C2 58.4(4) . . . . ? N1 C1 C2 C3 -53.9(4) . . . . ? C1 C2 C3 C6 177.2(3) . . . . ? C1 C2 C3 C4 53.3(4) . . . . ? C6 C3 C4 C7 54.3(4) . . . . ? C2 C3 C4 C7 176.7(3) . . . . ? C6 C3 C4 C5 179.9(3) . . . . ? C2 C3 C4 C5 -57.7(4) . . . . ? C7 C4 C5 C9 -50.0(4) . . . . ? C3 C4 C5 C9 -175.9(3) . . . . ? C7 C4 C5 N1 -172.7(3) . . . . ? C3 C4 C5 N1 61.4(4) . . . . ? C11 N1 C5 C9 46.2(4) . . . . ? C1 N1 C5 C9 171.8(3) . . . . ? C11 N1 C5 C4 172.5(3) . . . . ? C1 N1 C5 C4 -61.9(4) . . . . ? C5 C4 C7 C8 -63.5(4) . . . . ? C3 C4 C7 C8 61.3(4) . . . . ? C4 C5 C9 C10 -60.3(4) . . . . ? N1 C5 C9 C10 60.8(4) . . . . ? C1 N1 C11 C16 -71.3(4) . . . . ? C5 N1 C11 C16 54.4(4) . . . . ? C1 N1 C11 C12 109.3(4) . . . . ? C5 N1 C11 C12 -125.0(3) . . . . ? C16 C11 C12 C13 -1.2(6) . . . . ? N1 C11 C12 C13 178.2(3) . . . . ? C11 C12 C13 C14 0.7(6) . . . . ? C12 C13 C14 C15 0.3(6) . . . . ? C13 C14 C15 C16 -0.9(6) . . . . ? C12 C11 C16 C15 0.6(6) . . . . ? N1 C11 C16 C15 -178.8(3) . . . . ? C14 C15 C16 C11 0.5(6) . . . . ? C29 C24 C25 C26 0.0 . . . . ? C23 C24 C25 C26 176.7(18) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C24 0.0 . . . . ? C25 C24 C29 C28 0.0 . . . . ? C23 C24 C29 C28 -177.1(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O3 0.96(5) 2.13(5) 3.082(4) 169(4) 4_575 _refine_diff_density_max 0.500 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.067 _shelx_res_file ; 007a-20018.res created by SHELXL-2014/7 TITL 007a-20018 CELL 1.54184 8.0919 21.6444 15.449 90 90.114 90 ZERR 4 0.0001 0.0003 0.0002 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 102 128 16 36 4 EQIV $1 +X,1.5-Y,-0.5+Z HTAB N1 O3_$1 SIMU C23 > C29 RIGU C23 > C29 L.S. 30 SIZE 0.22 0.18 0.16 TEMP -180 CONF MORE -1 BOND $H ACTA OMIT 6 1 8 WGHT 0.050300 4.849300 BASF 0.23312 FVAR 10.29401 S1 5 0.224994 0.872793 1.018918 11.00000 0.02491 0.02296 = 0.02345 0.00032 0.00050 0.00063 O1 4 0.296778 0.846454 0.942663 11.00000 0.03215 0.02785 = 0.02637 -0.00287 -0.00212 0.00429 O2 4 0.056058 0.855793 1.034455 11.00000 0.02587 0.03065 = 0.04923 0.00334 0.00849 -0.00401 O3 4 0.327694 0.867974 1.095949 11.00000 0.04368 0.02570 = 0.02731 0.00260 0.00091 0.00368 O4 4 0.435601 0.988809 1.178206 11.00000 0.03581 0.04441 = 0.03032 -0.00011 -0.01073 0.00106 O5 4 0.171866 0.972970 1.188415 11.00000 0.03820 0.03647 = 0.02644 0.00115 0.00818 0.00016 O6 4 0.326408 1.180414 0.990701 11.00000 0.03637 0.02458 = 0.04088 -0.00422 0.00242 -0.00395 O7 4 0.250807 1.162131 0.858728 11.00000 0.03740 0.03149 = 0.02982 0.00824 0.00223 -0.00226 O8 4 0.021245 0.904715 0.854204 11.00000 0.03274 0.03316 = 0.04113 -0.00118 -0.00986 -0.00455 O9 4 0.215268 0.940621 0.772692 11.00000 0.06201 0.05521 = 0.02750 -0.01176 0.00501 -0.01205 N2 3 0.296792 0.984343 1.147880 11.00000 0.03313 0.02452 = 0.02459 -0.00273 -0.00051 0.00085 N3 3 0.283295 1.146092 0.932658 11.00000 0.02277 0.02750 = 0.03034 0.00030 0.00428 -0.00134 N4 3 0.141364 0.937343 0.840822 11.00000 0.03339 0.02887 = 0.02727 -0.00187 -0.00563 0.00137 C17 1 0.225054 0.955182 0.994977 11.00000 0.01739 0.02512 = 0.02410 -0.00031 -0.00043 -0.00044 C18 1 0.197522 0.977965 0.911607 11.00000 0.02323 0.02768 = 0.02218 -0.00483 -0.00155 -0.00084 C19 1 0.217327 1.039546 0.888915 11.00000 0.02391 0.02948 = 0.02072 0.00397 -0.00117 0.00118 AFIX 43 H19 2 0.197079 1.053377 0.831506 11.00000 -1.20000 AFIX 0 C20 1 0.267579 1.079976 0.952920 11.00000 0.02382 0.02277 = 0.02711 -0.00118 0.00264 -0.00050 C21 1 0.298158 1.061105 1.036102 11.00000 0.02231 0.02700 = 0.02713 -0.00471 0.00286 -0.00200 AFIX 43 H21 2 0.333580 1.089572 1.079110 11.00000 -1.20000 AFIX 0 C22 1 0.275824 0.999402 1.055371 11.00000 0.01907 0.02682 = 0.02457 -0.00163 0.00242 0.00060 N1 3 0.189139 0.730389 0.720431 11.00000 0.02494 0.02389 = 0.02277 -0.00170 -0.00202 0.00057 H1 2 0.217403 0.697504 0.681438 11.00000 0.03521 C1 1 0.103245 0.775526 0.661067 11.00000 0.02776 0.02923 = 0.03134 0.00165 -0.00801 0.00317 AFIX 23 H1A 2 0.067206 0.812037 0.694699 11.00000 -1.20000 H1B 2 0.003779 0.755834 0.635842 11.00000 -1.20000 AFIX 0 C2 1 0.217246 0.795889 0.589235 11.00000 0.03532 0.02798 = 0.02568 0.00087 -0.00560 0.00150 AFIX 23 H2A 2 0.161208 0.828067 0.554354 11.00000 -1.20000 H2B 2 0.239523 0.760257 0.550810 11.00000 -1.20000 AFIX 0 C3 1 0.381505 0.821499 0.622611 11.00000 0.03047 0.02299 = 0.02560 -0.00407 -0.00336 -0.00066 AFIX 13 H3 2 0.358438 0.860099 0.656043 11.00000 -1.20000 AFIX 0 C4 1 0.462966 0.774168 0.684433 11.00000 0.02465 0.02613 = 0.02160 -0.00237 -0.00068 0.00032 AFIX 13 H4 2 0.479596 0.735132 0.650940 11.00000 -1.20000 AFIX 0 C5 1 0.346354 0.759132 0.760054 11.00000 0.02106 0.02881 = 0.02244 -0.00526 -0.00416 -0.00155 AFIX 13 H5 2 0.314677 0.798900 0.788487 11.00000 -1.20000 AFIX 0 C6 1 0.491955 0.837872 0.546956 11.00000 0.04235 0.02885 = 0.02851 -0.00092 0.00275 -0.00254 AFIX 137 H6A 2 0.529442 0.799916 0.518525 11.00000 -1.50000 H6B 2 0.587896 0.861142 0.567932 11.00000 -1.50000 H6C 2 0.429983 0.863150 0.505467 11.00000 -1.50000 AFIX 0 C7 1 0.633399 0.795470 0.716189 11.00000 0.02443 0.03390 = 0.02955 -0.00562 0.00055 -0.00408 AFIX 23 H7A 2 0.681594 0.762497 0.752779 11.00000 -1.20000 H7B 2 0.706387 0.800798 0.665381 11.00000 -1.20000 AFIX 0 C8 1 0.632373 0.855365 0.767614 11.00000 0.03055 0.05101 = 0.04169 -0.01669 -0.00209 -0.00971 AFIX 137 H8A 2 0.590441 0.888925 0.731088 11.00000 -1.50000 H8B 2 0.745057 0.865105 0.786551 11.00000 -1.50000 H8C 2 0.560958 0.850671 0.818349 11.00000 -1.50000 AFIX 0 C9 1 0.416418 0.716420 0.829260 11.00000 0.02394 0.03568 = 0.02338 0.00006 -0.00013 -0.00244 AFIX 23 H9A 2 0.513744 0.736817 0.855652 11.00000 -1.20000 H9B 2 0.332396 0.711556 0.875251 11.00000 -1.20000 AFIX 0 C10 1 0.468135 0.652452 0.799055 11.00000 0.03346 0.03466 = 0.02705 0.00549 -0.00099 0.00631 AFIX 137 H10A 2 0.553148 0.656298 0.754287 11.00000 -1.50000 H10B 2 0.372004 0.630739 0.775219 11.00000 -1.50000 H10C 2 0.512592 0.629076 0.848185 11.00000 -1.50000 AFIX 0 C11 1 0.073070 0.705893 0.785614 11.00000 0.01894 0.03394 = 0.02314 -0.00137 -0.00121 0.00077 C12 1 0.026194 0.645110 0.777374 11.00000 0.03016 0.03478 = 0.02808 -0.00511 -0.00060 -0.00256 AFIX 43 H12 2 0.065282 0.620874 0.730412 11.00000 -1.20000 AFIX 0 C13 1 -0.078578 0.619749 0.838353 11.00000 0.03819 0.04294 = 0.03527 -0.00039 0.00475 -0.00931 AFIX 43 H13 2 -0.111041 0.577685 0.833935 11.00000 -1.20000 AFIX 0 C14 1 -0.135909 0.655735 0.905702 11.00000 0.02740 0.05615 = 0.03067 0.00334 0.00387 -0.00284 AFIX 43 H14 2 -0.207531 0.638356 0.947831 11.00000 -1.20000 AFIX 0 C15 1 -0.089162 0.717125 0.911930 11.00000 0.02841 0.04828 = 0.02879 -0.00733 -0.00077 0.00769 AFIX 43 H15 2 -0.130249 0.741819 0.957943 11.00000 -1.20000 AFIX 0 C16 1 0.016813 0.742770 0.851734 11.00000 0.02667 0.03648 = 0.02804 -0.00178 -0.00075 0.00106 AFIX 43 H16 2 0.049887 0.784778 0.855957 11.00000 -1.20000 AFIX 0 PART -1 C23 1 0.757469 1.007138 0.566531 10.50000 0.16328 0.15119 = 0.17387 -0.00054 -0.04717 0.00244 AFIX 33 H23A 2 0.748981 1.007128 0.629801 10.50000 -1.50000 H23B 2 0.825441 0.972124 0.547895 10.50000 -1.50000 H23C 2 0.808644 1.045793 0.547283 10.50000 -1.50000 AFIX 66 C24 1 0.583530 1.001431 0.526628 10.50000 0.14293 0.04226 = 0.12144 -0.01138 -0.03263 0.01686 C25 1 0.546491 0.999889 0.438760 10.50000 0.15506 0.02668 = 0.10747 -0.00352 -0.02348 0.01989 AFIX 43 H25 2 0.632070 1.004661 0.397287 10.50000 -1.20000 AFIX 65 C26 1 0.384237 0.991366 0.411572 10.50000 0.15685 0.02827 = 0.10024 -0.00765 -0.03242 0.02017 AFIX 43 H26 2 0.358923 0.990312 0.351517 10.50000 -1.20000 AFIX 65 C27 1 0.259020 0.984384 0.472252 10.50000 0.14776 0.03445 = 0.13645 -0.00970 -0.03750 0.03023 AFIX 43 H27 2 0.148127 0.978559 0.453670 10.50000 -1.20000 AFIX 65 C28 1 0.296057 0.985926 0.560121 10.50000 0.14516 0.03936 = 0.12272 -0.01558 -0.02890 0.03112 AFIX 43 H28 2 0.210477 0.981155 0.601593 10.50000 -1.20000 AFIX 65 C29 1 0.458310 0.994449 0.587310 10.50000 0.14731 0.03103 = 0.08609 -0.00828 -0.03490 0.02128 AFIX 43 H29 2 0.483623 0.995503 0.647365 10.50000 -1.20000 AFIX 0 HKLF 5 REM 007a-20018 REM R1 = 0.0581 for 4483 Fo > 4sig(Fo) and 0.0612 for all 4779 data REM 384 parameters refined using 87 restraints END WGHT 0.0503 4.8492 REM Highest difference peak 0.500, deepest hole -0.469, 1-sigma level 0.067 Q1 1 0.1825 0.9806 0.5269 11.00000 0.05 0.50 Q2 1 0.3140 0.9951 0.5218 11.00000 0.05 0.44 Q3 1 0.2465 0.8080 0.9670 11.00000 0.05 0.31 Q4 1 0.2282 0.8757 1.0900 11.00000 0.05 0.30 Q5 1 0.2248 0.8728 0.9545 11.00000 0.05 0.30 Q6 1 0.3754 0.8727 1.0464 11.00000 0.05 0.29 Q7 1 0.2752 0.9196 1.0423 11.00000 0.05 0.28 Q8 1 0.3380 0.8403 0.9842 11.00000 0.05 0.27 Q9 1 0.0865 0.9010 1.0476 11.00000 0.05 0.27 Q10 1 0.3062 1.1668 1.0446 11.00000 0.05 0.26 Q11 1 0.4144 1.0020 0.5842 11.00000 0.05 0.26 Q12 1 0.3627 0.9977 0.4280 11.00000 0.05 0.25 Q13 1 0.0057 0.7976 0.7210 11.00000 0.05 0.25 Q14 1 0.1960 0.9176 1.0060 11.00000 0.05 0.25 Q15 1 0.2363 1.0800 0.9974 11.00000 0.05 0.24 Q16 1 0.3057 0.8496 0.9176 11.00000 0.05 0.24 Q17 1 0.0272 1.0008 0.4574 11.00000 0.05 0.23 Q18 1 0.2194 0.9346 0.7057 11.00000 0.05 0.22 Q19 1 0.2042 0.9785 0.8545 11.00000 0.05 0.22 Q20 1 0.1810 0.7370 0.6565 11.00000 0.05 0.22 ; _shelx_res_checksum 27856 _shelx_hkl_file ; -1 0 0 51025 1736 -2 1 0 0 51025 1736 1 -2 0 0 3053339 91513 -2 2 0 0 3053339 91513 1 -3 0 0 84752 4942 -2 3 0 0 84752 4942 1 -4 0 0 719372 22079 -2 4 0 0 719372 22079 1 -5 0 0 6442 718 -2 5 0 0 6442 718 1 -6 0 0 17220 1280 -2 6 0 0 17220 1280 1 -7 0 0 71918 2840 -2 7 0 0 71918 2840 1 -8 0 0 6047 1017 -2 8 0 0 6047 1017 1 -9 0 0 25721 2488 -2 9 0 0 25721 2488 1 -1 -1 0 1329907 26288 -2 1 1 0 1329907 26288 1 -2 -1 0 173042 3695 -2 2 1 0 173042 3695 1 -3 -1 0 134742 2910 -2 3 1 0 134742 2910 1 -4 -1 0 140839 2389 -2 4 1 0 140839 2389 1 -5 -1 0 216818 3028 -2 5 1 0 216818 3028 1 -6 -1 0 193233 3920 -2 6 1 0 193233 3920 1 -7 -1 0 103040 2469 -2 7 1 0 103040 2469 1 -8 -1 0 29446 1485 -2 8 1 0 29446 1485 1 -9 -1 0 470 576 -2 9 1 0 470 576 1 0 -2 0 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