data_007b-20020 _vrf_RINTA01_007b-20020 ; PROBLEM: RESPONSE: The diffraction data was not ideal due to crystal quality. The crystal was very small and produced weak diffraction. ; _vrf_PLAT230_007b-20020 ; PROBLEM: RESPONSE: The diffraction data was not ideal and the subsequent model was based on weak, twinned data. ; _vrf_PLAT234_007b-20020 ; PROBLEM: RESPONSE: See response to PLAT230 ; _vrf_PLAT241_007b-20020 ; PROBLEM: RESPONSE: See response to PLAT230 ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H29 N2, C6 H2 N3 O9 S' _chemical_formula_sum 'C29 H31 N5 O9 S' _chemical_formula_weight 625.65 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 8.1117(3) _cell_length_b 19.7564(8) _cell_length_c 18.3015(9) _cell_angle_alpha 90 _cell_angle_beta 92.656(4) _cell_angle_gamma 90 _cell_volume 2929.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 9876 _cell_measurement_theta_min 3.2430 _cell_measurement_theta_max 58.5180 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_F_000 1312 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 1.529 _shelx_estimated_absorpt_T_min 0.941 _shelx_estimated_absorpt_T_max 0.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.41680 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 5182 _diffrn_reflns_av_unetI/netI 0.0743 _diffrn_reflns_av_R_equivalents 0.2324 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.294 _diffrn_reflns_theta_max 66.601 _diffrn_reflns_theta_full 66.601 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 5182 _reflns_number_gt 3141 _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 0.189(5). 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 isoproplyl and phenyl group are disordered over two positions. The phenyl site occupancies were freely refined to 0.88/0.12. The chemically equivalent C-C distances were restrained to be similar. Due to the small electron density, the thermal parameters of the minor component were constrained to be identical to the major. The site occupacies of the isopropyl were refined to 0.82/12, and a similar approach was used for refining the atomic and thermal parameters. ; _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^)+(0.0939P)^2^+4.9072P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary SHELXT _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5182 _refine_ls_number_parameters 413 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1490 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.2395 _refine_ls_wR_factor_gt 0.2056 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.045 _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 0.74339(16) 0.36517(6) 0.51796(8) 0.0458(4) Uani 1 1 d . . . . . O1 O 0.7866(5) 0.34529(18) 0.5928(2) 0.0567(11) Uani 1 1 d . . . . . O2 O 0.5875(4) 0.33896(17) 0.4896(2) 0.0462(10) Uani 1 1 d . . . . . O3 O 0.8781(4) 0.35844(19) 0.4690(2) 0.0550(11) Uani 1 1 d . . . . . O4 O 0.4952(5) 0.4105(2) 0.6366(2) 0.0582(11) Uani 1 1 d . . . . . O5 O 0.6636(6) 0.4633(2) 0.7127(2) 0.0602(11) Uani 1 1 d . . . . . O6 O 0.7469(5) 0.69234(18) 0.6192(2) 0.0545(11) Uani 1 1 d . . . . . O7 O 0.7770(5) 0.70571(19) 0.5027(2) 0.0536(11) Uani 1 1 d . . . . . O8 O 0.6988(5) 0.4451(2) 0.3641(2) 0.0534(10) Uani 1 1 d . . . . . O9 O 0.9471(5) 0.4883(2) 0.3766(2) 0.0549(10) Uani 1 1 d . . . . . N3 N 0.6079(6) 0.4507(2) 0.6512(3) 0.0475(12) Uani 1 1 d . . . . . N4 N 0.7567(5) 0.6712(2) 0.5564(3) 0.0451(12) Uani 1 1 d . . . . . N5 N 0.8105(6) 0.4752(2) 0.3993(3) 0.0462(11) Uani 1 1 d . . . . . C24 C 0.7191(6) 0.4565(2) 0.5264(3) 0.0384(13) Uani 1 1 d . . . . . C25 C 0.6741(6) 0.4893(3) 0.5898(3) 0.0386(12) Uani 1 1 d . . . . . C26 C 0.6843(6) 0.5581(3) 0.6016(3) 0.0428(13) Uani 1 1 d . . . . . H26 H 0.6529 0.5779 0.6462 0.051 Uiso 1 1 calc R U . . . C27 C 0.7420(6) 0.5970(2) 0.5458(3) 0.0399(13) Uani 1 1 d . . . . . C28 C 0.7854(6) 0.5704(2) 0.4803(3) 0.0377(12) Uani 1 1 d . . . . . H28 H 0.8237 0.5982 0.4423 0.045 Uiso 1 1 calc R U . . . C29 C 0.7704(6) 0.5005(3) 0.4724(3) 0.0392(12) Uani 1 1 d . . . . . N1 N 0.8360(6) 0.2522(2) 0.7152(3) 0.0541(13) Uani 1 1 d . . . . . H1 H 0.8362 0.2829 0.6718 0.065 Uiso 1 1 calc R U . . . N2 N 0.2811(9) 0.0102(4) 0.4985(5) 0.110(3) Uani 1 1 d . . . . . C1 C 0.9365(8) 0.2887(4) 0.7757(4) 0.0674(19) Uani 1 1 d . . . . . H1A H 0.9928 0.2546 0.8086 0.081 Uiso 1 1 calc R U . . . C2 C 0.8277(10) 0.3337(3) 0.8201(4) 0.074(2) Uani 1 1 d . . . . . H2B H 0.7719 0.3650 0.7839 0.088 Uiso 0.817(12) 1 calc R U P A 2 H2A H 0.7801 0.3706 0.7883 0.088 Uiso 0.183(12) 1 calc R U P A 1 C3 C 0.6893(10) 0.2959(4) 0.8554(4) 0.079(2) Uani 1 1 d . . . . . H3 H 0.7330 0.2810 0.9048 0.095 Uiso 1 1 calc R U . . . C4 C 0.6396(9) 0.2325(4) 0.8134(4) 0.073(2) Uani 1 1 d . . . . . H4A H 0.7132 0.1947 0.8289 0.088 Uiso 1 1 calc R U . . . H4B H 0.5252 0.2199 0.8242 0.088 Uiso 1 1 calc R U . . . C5 C 0.6509(7) 0.2443(3) 0.7335(3) 0.0524(15) Uani 1 1 d . . . . . H5 H 0.5965 0.2888 0.7225 0.063 Uiso 1 1 calc R U . . . C6 C 0.5674(7) 0.1929(3) 0.6836(4) 0.0577(16) Uani 1 1 d . . . . . C7 C 0.4983(8) 0.2134(3) 0.6159(4) 0.0630(17) Uani 1 1 d . . . . . H7 H 0.5011 0.2598 0.6025 0.076 Uiso 1 1 calc R U . . . C8 C 0.4262(9) 0.1670(3) 0.5681(4) 0.071(2) Uani 1 1 d . . . . . H8 H 0.3790 0.1815 0.5223 0.086 Uiso 1 1 calc R U . . . C9 C 0.4224(9) 0.0986(4) 0.5870(4) 0.076(2) Uani 1 1 d . . . . . C10 C 0.4897(9) 0.0768(4) 0.6539(4) 0.080(2) Uani 1 1 d . . . . . H10 H 0.4879 0.0302 0.6668 0.096 Uiso 1 1 calc R U . . . C11 C 0.5595(8) 0.1241(3) 0.7016(4) 0.0679(19) Uani 1 1 d . . . . . H11 H 0.6035 0.1096 0.7480 0.082 Uiso 1 1 calc R U . . . C12 C 0.3424(10) 0.0493(4) 0.5365(5) 0.085(2) Uani 1 1 d . . . . . C13 C 1.0765(11) 0.3349(8) 0.7360(8) 0.190(8) Uani 1 1 d . . . . . H13A H 1.0202 0.3708 0.7067 0.229 Uiso 1 1 calc R U . . . H13B H 1.1478 0.3571 0.7743 0.229 Uiso 1 1 calc R U . . . C14 C 1.1742(15) 0.2974(7) 0.6913(9) 0.193(7) Uani 1 1 d . . . . . H14A H 1.2126 0.2565 0.7171 0.290 Uiso 1 1 calc R U . . . H14B H 1.2695 0.3245 0.6781 0.290 Uiso 1 1 calc R U . . . H14C H 1.1098 0.2845 0.6468 0.290 Uiso 1 1 calc R U . . . C15A C 0.910(7) 0.372(3) 0.913(3) 0.079(3) Uani 0.183(12) 1 d . . P A 1 H15A H 0.9322 0.3349 0.9486 0.094 Uiso 0.183(12) 1 calc R U P A 1 H15B H 1.0148 0.3959 0.9059 0.094 Uiso 0.183(12) 1 calc R U P A 1 C15B C 0.9304(14) 0.3790(5) 0.8715(7) 0.079(3) Uani 0.817(12) 1 d . . P A 2 H15C H 0.9896 0.4125 0.8422 0.094 Uiso 0.817(12) 1 calc R U P A 2 H15D H 0.8556 0.4042 0.9030 0.094 Uiso 0.817(12) 1 calc R U P A 2 C16A C 0.813(7) 0.411(3) 0.938(3) 0.120(5) Uani 0.183(12) 1 d . . P A 1 H16A H 0.7981 0.4501 0.9056 0.180 Uiso 0.183(12) 1 calc R U P A 1 H16B H 0.8549 0.4263 0.9865 0.180 Uiso 0.183(12) 1 calc R U P A 1 H16C H 0.7064 0.3883 0.9431 0.180 Uiso 0.183(12) 1 calc R U P A 1 C16B C 1.0517(15) 0.3416(6) 0.9185(7) 0.120(5) Uani 0.817(12) 1 d . . P A 2 H16D H 0.9938 0.3096 0.9492 0.180 Uiso 0.817(12) 1 calc R U P A 2 H16E H 1.1150 0.3735 0.9496 0.180 Uiso 0.817(12) 1 calc R U P A 2 H16F H 1.1269 0.3167 0.8878 0.180 Uiso 0.817(12) 1 calc R U P A 2 C17 C 0.5376(12) 0.3410(5) 0.8677(5) 0.113(3) Uani 1 1 d . . . . . H17A H 0.4821 0.3518 0.8204 0.170 Uiso 1 1 calc R U . . . H17B H 0.5735 0.3830 0.8921 0.170 Uiso 1 1 calc R U . . . H17C H 0.4610 0.3169 0.8983 0.170 Uiso 1 1 calc R U . . . C19B C 0.9671(10) 0.1404(4) 0.7420(5) 0.059(2) Uani 0.876(10) 1 d D . P B 2 H19B H 0.9707 0.1497 0.7929 0.071 Uiso 0.876(10) 1 calc R U P B 2 C20A C 1.0197(16) 0.0789(5) 0.7157(7) 0.092(3) Uani 0.876(10) 1 d D . P B 2 H20A H 1.0608 0.0456 0.7493 0.111 Uiso 0.876(10) 1 calc R U P B 2 C21A C 1.0139(17) 0.0647(5) 0.6408(6) 0.119(5) Uani 0.876(10) 1 d D . P B 2 H21A H 1.0520 0.0222 0.6241 0.142 Uiso 0.876(10) 1 calc R U P B 2 C22A C 0.9526(17) 0.1123(5) 0.5906(6) 0.115(4) Uani 0.876(10) 1 d D . P B 2 H22A H 0.9464 0.1021 0.5399 0.137 Uiso 0.876(10) 1 calc R U P B 2 C23A C 0.9005(12) 0.1749(4) 0.6152(4) 0.070(3) Uani 0.876(10) 1 d D . P B 2 H23A H 0.8604 0.2083 0.5815 0.084 Uiso 0.876(10) 1 calc R U P B 2 C23B C 0.991(5) 0.1997(17) 0.6274(14) 0.070(3) Uani 0.124(10) 1 d DG . P B 1 H23B H 0.9710 0.2401 0.6002 0.084 Uiso 0.124(10) 1 calc R U P B 1 C18 C 0.9083(8) 0.1882(3) 0.6911(3) 0.0580(16) Uani 1 1 d DG . . . . C19A C 0.938(6) 0.1291(14) 0.731(2) 0.059(2) Uani 0.124(10) 1 d DG . P B 1 H19A H 0.8810 0.1212 0.7744 0.071 Uiso 0.124(10) 1 calc R U P B 1 C20B C 1.050(8) 0.082(2) 0.707(3) 0.092(3) Uani 0.124(10) 1 d DG . P B 1 H20B H 1.0697 0.0413 0.7343 0.111 Uiso 0.124(10) 1 calc R U P B 1 C21B C 1.132(7) 0.093(3) 0.643(3) 0.119(5) Uani 0.124(10) 1 d DG . P B 1 H21B H 1.2091 0.0608 0.6272 0.142 Uiso 0.124(10) 1 calc R U P B 1 C22B C 1.103(6) 0.152(3) 0.604(2) 0.115(4) Uani 0.124(10) 1 d DG . P B 1 H22B H 1.1597 0.1602 0.5601 0.137 Uiso 0.124(10) 1 calc R U P B 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 0.0378(7) 0.0299(7) 0.0686(10) 0.0007(7) -0.0097(7) -0.0015(6) O1 0.061(3) 0.035(2) 0.072(3) 0.0098(19) -0.018(2) 0.0006(18) O2 0.036(2) 0.0339(19) 0.068(3) 0.0015(17) -0.0117(18) -0.0088(16) O3 0.033(2) 0.039(2) 0.093(3) -0.014(2) 0.005(2) 0.0021(17) O4 0.048(2) 0.052(2) 0.074(3) 0.017(2) -0.005(2) -0.013(2) O5 0.074(3) 0.057(3) 0.049(3) 0.004(2) -0.005(2) -0.006(2) O6 0.055(3) 0.037(2) 0.071(3) -0.013(2) -0.007(2) 0.0019(18) O7 0.055(3) 0.035(2) 0.069(3) 0.011(2) -0.012(2) -0.0002(18) O8 0.042(2) 0.055(2) 0.063(3) -0.016(2) -0.0049(19) -0.0040(19) O9 0.041(2) 0.061(3) 0.063(3) -0.007(2) 0.0043(19) -0.0093(19) N3 0.046(3) 0.041(3) 0.055(3) 0.009(2) 0.000(2) 0.001(2) N4 0.040(3) 0.031(2) 0.063(3) -0.003(2) -0.010(2) 0.000(2) N5 0.043(3) 0.040(3) 0.054(3) 0.000(2) -0.006(2) -0.003(2) C24 0.026(3) 0.032(3) 0.057(3) 0.007(3) -0.008(2) -0.004(2) C25 0.032(3) 0.035(3) 0.048(3) 0.002(2) -0.007(2) 0.001(2) C26 0.034(3) 0.041(3) 0.053(3) -0.002(3) -0.007(2) 0.002(2) C27 0.037(3) 0.027(3) 0.054(3) -0.005(2) -0.012(3) 0.003(2) C28 0.029(3) 0.032(3) 0.051(3) 0.003(2) -0.003(2) -0.005(2) C29 0.030(3) 0.036(3) 0.050(3) -0.003(3) -0.006(2) 0.001(2) N1 0.053(3) 0.047(3) 0.061(3) 0.002(2) 0.000(2) -0.004(2) N2 0.088(5) 0.089(5) 0.151(7) -0.037(5) -0.027(5) 0.003(4) C1 0.051(4) 0.062(4) 0.089(5) -0.008(4) 0.001(3) -0.015(3) C2 0.086(5) 0.049(4) 0.085(5) -0.006(4) -0.009(4) -0.005(4) C3 0.091(6) 0.078(5) 0.070(5) -0.003(4) 0.006(4) -0.014(5) C4 0.065(4) 0.073(5) 0.082(5) 0.016(4) 0.003(4) -0.005(4) C5 0.047(3) 0.053(4) 0.058(4) 0.011(3) 0.004(3) 0.004(3) C6 0.045(3) 0.054(4) 0.073(4) 0.015(3) -0.005(3) -0.009(3) C7 0.057(4) 0.055(4) 0.076(5) 0.011(3) -0.013(3) 0.000(3) C8 0.068(5) 0.060(4) 0.084(5) 0.013(4) -0.024(4) 0.007(4) C9 0.069(5) 0.065(5) 0.093(6) 0.002(4) -0.016(4) 0.007(4) C10 0.071(5) 0.054(4) 0.112(6) 0.010(4) -0.032(4) -0.008(4) C11 0.059(4) 0.066(4) 0.077(5) 0.021(4) -0.018(4) -0.009(3) C12 0.073(5) 0.064(5) 0.116(7) -0.023(5) -0.027(5) 0.013(4) C13 0.053(6) 0.310(19) 0.211(13) -0.180(14) 0.038(7) -0.030(8) C14 0.097(9) 0.214(15) 0.269(18) -0.114(14) 0.024(10) -0.062(9) C15A 0.086(6) 0.065(6) 0.085(8) -0.018(7) 0.002(7) -0.004(5) C15B 0.086(6) 0.065(6) 0.085(8) -0.018(7) 0.002(7) -0.004(5) C16A 0.100(9) 0.113(9) 0.143(10) -0.057(8) -0.042(8) 0.029(7) C16B 0.100(9) 0.113(9) 0.143(10) -0.057(8) -0.042(8) 0.029(7) C17 0.101(7) 0.121(8) 0.120(8) -0.033(6) 0.039(6) -0.015(6) C19B 0.052(4) 0.054(4) 0.070(5) 0.013(4) 0.004(4) 0.003(4) C20A 0.102(8) 0.067(5) 0.111(8) 0.023(5) 0.038(6) 0.032(5) C21A 0.167(13) 0.061(6) 0.132(10) -0.005(7) 0.060(9) 0.033(7) C22A 0.180(13) 0.075(7) 0.091(7) -0.011(6) 0.030(8) 0.029(7) C23A 0.088(7) 0.063(5) 0.059(5) 0.000(4) 0.001(4) 0.007(5) C23B 0.088(7) 0.063(5) 0.059(5) 0.000(4) 0.001(4) 0.007(5) C18 0.054(4) 0.053(4) 0.068(4) 0.007(3) 0.004(3) 0.008(3) C19A 0.052(4) 0.054(4) 0.070(5) 0.013(4) 0.004(4) 0.003(4) C20B 0.102(8) 0.067(5) 0.111(8) 0.023(5) 0.038(6) 0.032(5) C21B 0.167(13) 0.061(6) 0.132(10) -0.005(7) 0.060(9) 0.033(7) C22B 0.180(13) 0.075(7) 0.091(7) -0.011(6) 0.030(8) 0.029(7) _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 O2 1.441(4) . ? S1 O3 1.451(4) . ? S1 O1 1.452(4) . ? S1 C24 1.823(5) . ? O4 N3 1.231(6) . ? O5 N3 1.220(6) . ? O6 N4 1.230(6) . ? O7 N4 1.213(6) . ? O8 N5 1.240(5) . ? O9 N5 1.230(6) . ? N3 C25 1.478(7) . ? N4 C27 1.483(6) . ? N5 C29 1.478(7) . ? C24 C25 1.393(7) . ? C24 C29 1.393(7) . ? C25 C26 1.379(7) . ? C26 C27 1.377(8) . ? C26 H26 0.9500 . ? C27 C28 1.369(7) . ? C28 C29 1.394(7) . ? C28 H28 0.9500 . ? N1 C18 1.471(7) . ? N1 C1 1.526(8) . ? N1 C5 1.561(7) . ? N1 H1 1.0000 . ? N2 C12 1.138(9) . ? C1 C2 1.515(10) . ? C1 C13 1.650(15) . ? C1 H1A 1.0000 . ? C2 C3 1.517(10) . ? C2 C15B 1.518(12) . ? C2 C15A 1.95(5) . ? C2 H2B 1.0000 . ? C2 H2A 1.0000 . ? C3 C4 1.514(10) . ? C3 C17 1.544(12) . ? C3 H3 1.0000 . ? C4 C5 1.488(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.505(9) . ? C5 H5 1.0000 . ? C6 C7 1.396(8) . ? C6 C11 1.400(9) . ? C7 C8 1.378(9) . ? C7 H7 0.9500 . ? C8 C9 1.394(9) . ? C8 H8 0.9500 . ? C9 C10 1.387(10) . ? C9 C12 1.473(11) . ? C10 C11 1.382(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C14 1.381(15) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15A C16A 1.21(7) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C15B C16B 1.475(16) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19B C20A 1.381(9) . ? C19B C18 1.395(8) . ? C19B H19B 0.9500 . ? C20A C21A 1.398(11) . ? C20A H20A 0.9500 . ? C21A C22A 1.391(10) . ? C21A H21A 0.9500 . ? C22A C23A 1.388(9) . ? C22A H22A 0.9500 . ? C23A C18 1.412(8) . ? C23A H23A 0.9500 . ? C23B C18 1.3900 . ? C23B C22B 1.3900 . ? C23B H23B 0.9500 . ? C18 C19A 1.3900 . ? C19A C20B 1.3900 . ? C19A H19A 0.9500 . ? C20B C21B 1.3900 . ? C20B H20B 0.9500 . ? C21B C22B 1.3900 . ? C21B H21B 0.9500 . ? C22B H22B 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 O2 S1 O3 114.7(2) . . ? O2 S1 O1 114.3(2) . . ? O3 S1 O1 113.7(3) . . ? O2 S1 C24 106.8(2) . . ? O3 S1 C24 103.3(2) . . ? O1 S1 C24 102.2(2) . . ? O5 N3 O4 124.9(5) . . ? O5 N3 C25 117.6(5) . . ? O4 N3 C25 117.4(5) . . ? O7 N4 O6 125.7(5) . . ? O7 N4 C27 117.6(5) . . ? O6 N4 C27 116.7(5) . . ? O9 N5 O8 125.0(5) . . ? O9 N5 C29 118.4(4) . . ? O8 N5 C29 116.5(5) . . ? C25 C24 C29 113.6(5) . . ? C25 C24 S1 124.3(4) . . ? C29 C24 S1 121.4(4) . . ? C26 C25 C24 124.9(5) . . ? C26 C25 N3 114.3(5) . . ? C24 C25 N3 120.8(4) . . ? C27 C26 C25 117.0(5) . . ? C27 C26 H26 121.5 . . ? C25 C26 H26 121.5 . . ? C28 C27 C26 123.1(5) . . ? C28 C27 N4 118.1(5) . . ? C26 C27 N4 118.9(5) . . ? C27 C28 C29 116.5(5) . . ? C27 C28 H28 121.7 . . ? C29 C28 H28 121.7 . . ? C24 C29 C28 124.9(5) . . ? C24 C29 N5 121.0(5) . . ? C28 C29 N5 114.1(5) . . ? C18 N1 C1 114.7(5) . . ? C18 N1 C5 112.3(5) . . ? C1 N1 C5 112.3(5) . . ? C18 N1 H1 105.6 . . ? C1 N1 H1 105.6 . . ? C5 N1 H1 105.6 . . ? C2 C1 N1 111.2(5) . . ? C2 C1 C13 110.0(7) . . ? N1 C1 C13 107.3(6) . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C13 C1 H1A 109.4 . . ? C1 C2 C3 113.6(6) . . ? C1 C2 C15B 111.2(7) . . ? C3 C2 C15B 115.0(8) . . ? C1 C2 C15A 120.9(19) . . ? C3 C2 C15A 92.8(18) . . ? C1 C2 H2B 105.3 . . ? C3 C2 H2B 105.3 . . ? C15B C2 H2B 105.3 . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C15A C2 H2A 109.4 . . ? C4 C3 C2 112.1(6) . . ? C4 C3 C17 110.9(7) . . ? C2 C3 C17 112.8(7) . . ? C4 C3 H3 106.9 . . ? C2 C3 H3 106.9 . . ? C17 C3 H3 106.9 . . ? C5 C4 C3 110.0(6) . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C5 C6 116.4(5) . . ? C4 C5 N1 109.3(5) . . ? C6 C5 N1 110.4(5) . . ? C4 C5 H5 106.8 . . ? C6 C5 H5 106.8 . . ? N1 C5 H5 106.8 . . ? C7 C6 C11 117.9(6) . . ? C7 C6 C5 119.6(5) . . ? C11 C6 C5 122.4(6) . . ? C8 C7 C6 120.8(6) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.0(7) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.5(7) . . ? C10 C9 C12 119.5(7) . . ? C8 C9 C12 120.0(7) . . ? C11 C10 C9 118.7(7) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C6 122.0(6) . . ? C10 C11 H11 119.0 . . ? C6 C11 H11 119.0 . . ? N2 C12 C9 178.7(10) . . ? C14 C13 C1 113.0(12) . . ? C14 C13 H13A 109.0 . . ? C1 C13 H13A 109.0 . . ? C14 C13 H13B 109.0 . . ? C1 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16A C15A C2 112(4) . . ? C16A C15A H15A 109.2 . . ? C2 C15A H15A 109.2 . . ? C16A C15A H15B 109.2 . . ? C2 C15A H15B 109.2 . . ? H15A C15A H15B 107.9 . . ? C16B C15B C2 113.4(8) . . ? C16B C15B H15C 108.9 . . ? C2 C15B H15C 108.9 . . ? C16B C15B H15D 108.9 . . ? C2 C15B H15D 108.9 . . ? H15C C15B H15D 107.7 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C3 C17 H17A 109.5 . . ? C3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20A C19B C18 117.7(8) . . ? C20A C19B H19B 121.2 . . ? C18 C19B H19B 121.2 . . ? C19B C20A C21A 121.4(8) . . ? C19B C20A H20A 119.3 . . ? C21A C20A H20A 119.3 . . ? C22A C21A C20A 120.4(9) . . ? C22A C21A H21A 119.8 . . ? C20A C21A H21A 119.8 . . ? C23A C22A C21A 119.6(9) . . ? C23A C22A H22A 120.2 . . ? C21A C22A H22A 120.2 . . ? C22A C23A C18 118.9(8) . . ? C22A C23A H23A 120.6 . . ? C18 C23A H23A 120.6 . . ? C18 C23B C22B 120.0 . . ? C18 C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C23B C18 C19A 120.0 . . ? C19B C18 C23A 122.0(7) . . ? C23B C18 N1 109.0(13) . . ? C19A C18 N1 128.7(14) . . ? C19B C18 N1 120.7(6) . . ? C23A C18 N1 117.0(5) . . ? C20B C19A C18 120.0 . . ? C20B C19A H19A 120.0 . . ? C18 C19A H19A 120.0 . . ? C19A C20B C21B 120.0 . . ? C19A C20B H20B 120.0 . . ? C21B C20B H20B 120.0 . . ? C20B C21B C22B 120.0 . . ? C20B C21B H21B 120.0 . . ? C22B C21B H21B 120.0 . . ? C21B C22B C23B 120.0 . . ? C21B C22B H22B 120.0 . . ? C23B C22B H22B 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 O2 S1 C24 C25 93.2(4) . . . . ? O3 S1 C24 C25 -145.4(4) . . . . ? O1 S1 C24 C25 -27.1(5) . . . . ? O2 S1 C24 C29 -97.3(4) . . . . ? O3 S1 C24 C29 24.1(5) . . . . ? O1 S1 C24 C29 142.3(4) . . . . ? C29 C24 C25 C26 -2.7(7) . . . . ? S1 C24 C25 C26 167.5(4) . . . . ? C29 C24 C25 N3 176.6(4) . . . . ? S1 C24 C25 N3 -13.2(7) . . . . ? O5 N3 C25 C26 -46.8(6) . . . . ? O4 N3 C25 C26 130.0(5) . . . . ? O5 N3 C25 C24 133.8(5) . . . . ? O4 N3 C25 C24 -49.4(7) . . . . ? C24 C25 C26 C27 0.6(8) . . . . ? N3 C25 C26 C27 -178.7(4) . . . . ? C25 C26 C27 C28 1.3(7) . . . . ? C25 C26 C27 N4 -179.4(4) . . . . ? O7 N4 C27 C28 13.2(7) . . . . ? O6 N4 C27 C28 -167.0(4) . . . . ? O7 N4 C27 C26 -166.2(5) . . . . ? O6 N4 C27 C26 13.7(7) . . . . ? C26 C27 C28 C29 -0.8(7) . . . . ? N4 C27 C28 C29 179.8(4) . . . . ? C25 C24 C29 C28 3.3(7) . . . . ? S1 C24 C29 C28 -167.3(4) . . . . ? C25 C24 C29 N5 -175.3(4) . . . . ? S1 C24 C29 N5 14.2(6) . . . . ? C27 C28 C29 C24 -1.7(7) . . . . ? C27 C28 C29 N5 177.0(4) . . . . ? O9 N5 C29 C24 -124.8(5) . . . . ? O8 N5 C29 C24 59.0(6) . . . . ? O9 N5 C29 C28 56.5(6) . . . . ? O8 N5 C29 C28 -119.7(5) . . . . ? C18 N1 C1 C2 -154.5(6) . . . . ? C5 N1 C1 C2 -24.8(7) . . . . ? C18 N1 C1 C13 85.1(8) . . . . ? C5 N1 C1 C13 -145.1(7) . . . . ? N1 C1 C2 C3 58.1(8) . . . . ? C13 C1 C2 C3 176.9(7) . . . . ? N1 C1 C2 C15B -170.3(7) . . . . ? C13 C1 C2 C15B -51.5(10) . . . . ? N1 C1 C2 C15A 167(2) . . . . ? C13 C1 C2 C15A -74(2) . . . . ? C1 C2 C3 C4 -26.4(9) . . . . ? C15B C2 C3 C4 -156.1(7) . . . . ? C15A C2 C3 C4 -152.0(18) . . . . ? C1 C2 C3 C17 -152.5(7) . . . . ? C15B C2 C3 C17 77.8(9) . . . . ? C15A C2 C3 C17 81.9(19) . . . . ? C2 C3 C4 C5 -36.0(9) . . . . ? C17 C3 C4 C5 91.1(8) . . . . ? C3 C4 C5 C6 -165.6(6) . . . . ? C3 C4 C5 N1 68.7(7) . . . . ? C18 N1 C5 C4 95.2(6) . . . . ? C1 N1 C5 C4 -35.7(7) . . . . ? C18 N1 C5 C6 -34.0(6) . . . . ? C1 N1 C5 C6 -164.9(5) . . . . ? C4 C5 C6 C7 147.7(6) . . . . ? N1 C5 C6 C7 -87.1(7) . . . . ? C4 C5 C6 C11 -34.1(9) . . . . ? N1 C5 C6 C11 91.1(7) . . . . ? C11 C6 C7 C8 -0.6(10) . . . . ? C5 C6 C7 C8 177.7(6) . . . . ? C6 C7 C8 C9 -0.4(11) . . . . ? C7 C8 C9 C10 0.5(12) . . . . ? C7 C8 C9 C12 178.8(7) . . . . ? C8 C9 C10 C11 0.4(12) . . . . ? C12 C9 C10 C11 -177.9(7) . . . . ? C9 C10 C11 C6 -1.4(12) . . . . ? C7 C6 C11 C10 1.5(11) . . . . ? C5 C6 C11 C10 -176.7(7) . . . . ? C2 C1 C13 C14 -176.6(11) . . . . ? N1 C1 C13 C14 -55.4(13) . . . . ? C1 C2 C15B C16B -53.1(13) . . . . ? C3 C2 C15B C16B 77.8(12) . . . . ? C18 C19B C20A C21A -0.3(16) . . . . ? C19B C20A C21A C22A -1(2) . . . . ? C20A C21A C22A C23A 1(2) . . . . ? C21A C22A C23A C18 -1.2(17) . . . . ? C22B C23B C18 C19A 0.0 . . . . ? C22B C23B C18 N1 164.0(19) . . . . ? C20A C19B C18 C23A 0.6(12) . . . . ? C20A C19B C18 N1 174.3(8) . . . . ? C22A C23A C18 C19B 0.2(13) . . . . ? C22A C23A C18 N1 -173.8(9) . . . . ? C1 N1 C18 C23B -99(2) . . . . ? C5 N1 C18 C23B 131(2) . . . . ? C1 N1 C18 C19A 63(3) . . . . ? C5 N1 C18 C19A -66(3) . . . . ? C1 N1 C18 C19B 47.1(8) . . . . ? C5 N1 C18 C19B -82.6(7) . . . . ? C1 N1 C18 C23A -138.9(7) . . . . ? C5 N1 C18 C23A 91.4(7) . . . . ? C23B C18 C19A C20B 0.0 . . . . ? N1 C18 C19A C20B -161(2) . . . . ? C18 C19A C20B C21B 0.0 . . . . ? C19A C20B C21B C22B 0.0 . . . . ? C20B C21B C22B C23B 0.0 . . . . ? C18 C23B C22B C21B 0.0 . . . . ? 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 O1 1.00 1.93 2.911(6) 167.4 . _refine_diff_density_max 0.581 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.076 _shelx_res_file ; 007b-20020.res created by SHELXL-2014/7 TITL 007b-20020 CELL 1.54184 8.1117 19.7564 18.3015 90 92.656 90 ZERR 4 0.0003 0.0008 0.0009 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 116 124 20 36 4 SADI C18 C23A C18 C23B C23A C22A C23B C22B C22A C21A C22B C21B C20A C21A = C20B C21B C19B C20A C19A C20B C18 C19B C18 C19A EADP C15B C15A EADP C16A C16B EADP C23A C23B EADP C22A C22B EADP C21A C21B EADP C20A C20B EADP C19B C19A L.S. 30 SIZE 0.04 0.04 0.02 TEMP -180 CONF HTAB N1 O1 MORE -1 BOND $H ACTA WGHT 0.093900 4.907200 BASF 0.18945 FVAR 10.85865 0.12370 0.18307 S1 5 0.743385 0.365169 0.517963 11.00000 0.03777 0.02991 = 0.06861 0.00065 -0.00971 -0.00146 O1 4 0.786562 0.345286 0.592813 11.00000 0.06059 0.03534 = 0.07217 0.00981 -0.01765 0.00056 O2 4 0.587462 0.338962 0.489589 11.00000 0.03557 0.03395 = 0.06783 0.00151 -0.01170 -0.00877 O3 4 0.878137 0.358439 0.468995 11.00000 0.03328 0.03914 = 0.09276 -0.01368 0.00530 0.00208 O4 4 0.495185 0.410454 0.636559 11.00000 0.04761 0.05195 = 0.07419 0.01672 -0.00477 -0.01311 O5 4 0.663617 0.463293 0.712696 11.00000 0.07380 0.05651 = 0.04949 0.00428 -0.00544 -0.00619 O6 4 0.746893 0.692345 0.619242 11.00000 0.05451 0.03708 = 0.07109 -0.01300 -0.00729 0.00186 O7 4 0.777003 0.705713 0.502716 11.00000 0.05469 0.03548 = 0.06918 0.01089 -0.01236 -0.00021 O8 4 0.698770 0.445122 0.364073 11.00000 0.04150 0.05506 = 0.06300 -0.01614 -0.00493 -0.00404 O9 4 0.947141 0.488288 0.376576 11.00000 0.04060 0.06083 = 0.06334 -0.00685 0.00434 -0.00933 N3 3 0.607879 0.450696 0.651164 11.00000 0.04570 0.04137 = 0.05506 0.00895 -0.00049 0.00116 N4 3 0.756732 0.671187 0.556359 11.00000 0.03988 0.03121 = 0.06297 -0.00330 -0.00975 0.00001 N5 3 0.810515 0.475172 0.399337 11.00000 0.04333 0.04015 = 0.05424 0.00003 -0.00567 -0.00334 C24 1 0.719102 0.456542 0.526361 11.00000 0.02590 0.03193 = 0.05651 0.00706 -0.00788 -0.00355 C25 1 0.674120 0.489276 0.589834 11.00000 0.03234 0.03498 = 0.04765 0.00246 -0.00671 0.00115 C26 1 0.684288 0.558140 0.601610 11.00000 0.03430 0.04059 = 0.05272 -0.00205 -0.00693 0.00199 AFIX 43 H26 2 0.652868 0.577873 0.646210 11.00000 -1.20000 AFIX 0 C27 1 0.742035 0.596994 0.545807 11.00000 0.03659 0.02740 = 0.05441 -0.00531 -0.01203 0.00290 C28 1 0.785374 0.570439 0.480325 11.00000 0.02917 0.03244 = 0.05112 0.00338 -0.00329 -0.00456 AFIX 43 H28 2 0.823668 0.598215 0.442279 11.00000 -1.20000 AFIX 0 C29 1 0.770368 0.500503 0.472401 11.00000 0.03015 0.03647 = 0.05030 -0.00339 -0.00587 0.00141 N1 3 0.835989 0.252193 0.715195 11.00000 0.05350 0.04701 = 0.06148 0.00173 0.00049 -0.00370 AFIX 13 H1 2 0.836244 0.282935 0.671792 11.00000 -1.20000 AFIX 0 N2 3 0.281109 0.010205 0.498550 11.00000 0.08763 0.08932 = 0.15081 -0.03663 -0.02686 0.00300 C1 1 0.936508 0.288730 0.775692 11.00000 0.05114 0.06211 = 0.08874 -0.00796 0.00099 -0.01529 AFIX 13 H1A 2 0.992822 0.254637 0.808620 11.00000 -1.20000 AFIX 0 C2 1 0.827745 0.333701 0.820142 11.00000 0.08602 0.04910 = 0.08464 -0.00619 -0.00928 -0.00461 PART 2 AFIX 13 H2B 2 0.771872 0.365038 0.783934 -31.00000 -1.20000 AFIX 13 PART 1 H2A 2 0.780109 0.370589 0.788260 31.00000 -1.20000 AFIX 0 PART 0 C3 1 0.689265 0.295915 0.855377 11.00000 0.09054 0.07805 = 0.06975 -0.00250 0.00633 -0.01380 AFIX 13 H3 2 0.733036 0.281010 0.904764 11.00000 -1.20000 AFIX 0 C4 1 0.639632 0.232523 0.813378 11.00000 0.06463 0.07255 = 0.08191 0.01558 0.00341 -0.00539 AFIX 23 H4A 2 0.713218 0.194686 0.828900 11.00000 -1.20000 H4B 2 0.525161 0.219934 0.824172 11.00000 -1.20000 AFIX 0 C5 1 0.650899 0.244284 0.733467 11.00000 0.04701 0.05269 = 0.05758 0.01119 0.00411 0.00441 AFIX 13 H5 2 0.596494 0.288783 0.722459 11.00000 -1.20000 AFIX 0 C6 1 0.567357 0.192913 0.683625 11.00000 0.04544 0.05401 = 0.07289 0.01492 -0.00488 -0.00947 C7 1 0.498333 0.213358 0.615872 11.00000 0.05666 0.05517 = 0.07560 0.01115 -0.01292 -0.00008 AFIX 43 H7 2 0.501137 0.259804 0.602545 11.00000 -1.20000 AFIX 0 C8 1 0.426176 0.166958 0.568093 11.00000 0.06781 0.06003 = 0.08390 0.01291 -0.02360 0.00682 AFIX 43 H8 2 0.379039 0.181535 0.522277 11.00000 -1.20000 AFIX 0 C9 1 0.422370 0.098621 0.587010 11.00000 0.06887 0.06468 = 0.09255 0.00237 -0.01620 0.00675 C10 1 0.489697 0.076790 0.653933 11.00000 0.07089 0.05444 = 0.11178 0.00956 -0.03170 -0.00790 AFIX 43 H10 2 0.487875 0.030214 0.666775 11.00000 -1.20000 AFIX 0 C11 1 0.559527 0.124133 0.701601 11.00000 0.05853 0.06610 = 0.07720 0.02130 -0.01848 -0.00925 AFIX 43 H11 2 0.603546 0.109559 0.747971 11.00000 -1.20000 AFIX 0 C12 1 0.342351 0.049283 0.536541 11.00000 0.07306 0.06408 = 0.11637 -0.02252 -0.02690 0.01349 C13 1 1.076534 0.334861 0.736039 11.00000 0.05331 0.31011 = 0.21089 -0.17956 0.03758 -0.03032 AFIX 23 H13A 2 1.020203 0.370825 0.706653 11.00000 -1.20000 H13B 2 1.147819 0.357102 0.774294 11.00000 -1.20000 AFIX 0 C14 1 1.174175 0.297367 0.691256 11.00000 0.09744 0.21411 = 0.26920 -0.11424 0.02358 -0.06186 AFIX 137 H14A 2 1.212572 0.256478 0.717144 11.00000 -1.50000 H14B 2 1.269467 0.324500 0.678067 11.00000 -1.50000 H14C 2 1.109762 0.284523 0.646785 11.00000 -1.50000 AFIX 0 PART 1 C15A 1 0.909601 0.372045 0.913198 31.00000 0.08570 0.06521 = 0.08498 -0.01753 0.00178 -0.00445 AFIX 23 H15A 2 0.932187 0.334907 0.948576 31.00000 -1.20000 H15B 2 1.014847 0.395943 0.905912 31.00000 -1.20000 AFIX 0 PART 2 C15B 1 0.930381 0.378966 0.871530 -31.00000 0.08570 0.06521 = 0.08498 -0.01753 0.00178 -0.00445 AFIX 23 H15C 2 0.989575 0.412451 0.842206 -31.00000 -1.20000 H15D 2 0.855608 0.404197 0.902984 -31.00000 -1.20000 AFIX 0 PART 1 C16A 1 0.812732 0.410997 0.938279 31.00000 0.09964 0.11349 = 0.14250 -0.05741 -0.04188 0.02937 AFIX 137 H16A 2 0.798130 0.450079 0.905643 31.00000 -1.50000 H16B 2 0.854944 0.426305 0.986527 31.00000 -1.50000 H16C 2 0.706389 0.388267 0.943052 31.00000 -1.50000 AFIX 0 PART 2 C16B 1 1.051675 0.341554 0.918496 -31.00000 0.09964 0.11349 = 0.14250 -0.05741 -0.04188 0.02937 AFIX 137 H16D 2 0.993810 0.309584 0.949244 -31.00000 -1.50000 H16E 2 1.114961 0.373528 0.949644 -31.00000 -1.50000 H16F 2 1.126858 0.316688 0.887810 -31.00000 -1.50000 AFIX 0 PART 0 C17 1 0.537644 0.341038 0.867671 11.00000 0.10149 0.12085 = 0.12021 -0.03279 0.03888 -0.01496 AFIX 137 H17A 2 0.482106 0.351798 0.820403 11.00000 -1.50000 H17B 2 0.573540 0.383030 0.892071 11.00000 -1.50000 H17C 2 0.461045 0.316928 0.898343 11.00000 -1.50000 AFIX 0 PART 2 C19B 1 0.967053 0.140355 0.741984 -21.00000 0.05227 0.05447 = 0.07025 0.01251 0.00379 0.00279 AFIX 43 H19B 2 0.970715 0.149749 0.792942 -21.00000 -1.20000 AFIX 0 C20A 1 1.019721 0.078901 0.715707 -21.00000 0.10152 0.06732 = 0.11088 0.02299 0.03817 0.03202 AFIX 43 H20A 2 1.060826 0.045581 0.749255 -21.00000 -1.20000 AFIX 0 C21A 1 1.013867 0.064650 0.640799 -21.00000 0.16738 0.06132 = 0.13247 -0.00509 0.05993 0.03265 AFIX 43 H21A 2 1.051951 0.022166 0.624063 -21.00000 -1.20000 AFIX 0 C22A 1 0.952579 0.112344 0.590640 -21.00000 0.17958 0.07511 = 0.09116 -0.01084 0.02965 0.02907 AFIX 43 H22A 2 0.946380 0.102132 0.539863 -21.00000 -1.20000 AFIX 0 C23A 1 0.900536 0.174932 0.615193 -21.00000 0.08821 0.06290 = 0.05915 0.00009 0.00100 0.00720 AFIX 43 H23A 2 0.860382 0.208303 0.581495 -21.00000 -1.20000 AFIX 66 PART 1 C23B 1 0.991049 0.199747 0.627432 21.00000 0.08821 0.06290 = 0.05915 0.00009 0.00100 0.00720 AFIX 43 H23B 2 0.971013 0.240093 0.600208 21.00000 -1.20000 AFIX 65 PART 0 C18 1 0.908272 0.188166 0.691068 11.00000 0.05371 0.05251 = 0.06788 0.00699 0.00367 0.00836 PART 1 C19A 1 0.937589 0.129134 0.730902 21.00000 0.05227 0.05447 = 0.07025 0.01251 0.00379 0.00279 AFIX 43 H19A 2 0.881014 0.121219 0.774395 21.00000 -1.20000 AFIX 65 C20B 1 1.049683 0.081684 0.707099 21.00000 0.10152 0.06732 = 0.11088 0.02299 0.03817 0.03202 AFIX 43 H20B 2 1.069720 0.041338 0.734323 21.00000 -1.20000 AFIX 65 C21B 1 1.132462 0.093264 0.643463 21.00000 0.16738 0.06132 = 0.13247 -0.00509 0.05993 0.03265 AFIX 43 H21B 2 1.209073 0.060834 0.627195 21.00000 -1.20000 AFIX 65 C22B 1 1.103146 0.152295 0.603629 21.00000 0.17958 0.07511 = 0.09116 -0.01084 0.02965 0.02907 AFIX 43 H22B 2 1.159722 0.160210 0.560136 21.00000 -1.20000 AFIX 0 HKLF 5 REM 007b-20020 REM R1 = 0.0910 for 3141 Fo > 4sig(Fo) and 0.1490 for all 5182 data REM 413 parameters refined using 66 restraints END WGHT 0.0938 4.9272 REM Highest difference peak 0.581, deepest hole -0.348, 1-sigma level 0.076 Q1 1 1.0925 0.3913 0.7354 11.00000 0.05 0.58 Q2 1 1.1793 0.4168 0.8176 11.00000 0.05 0.51 Q3 1 1.1333 0.2868 0.7613 11.00000 0.05 0.46 Q4 1 0.6821 0.3697 0.8727 11.00000 0.05 0.43 Q5 1 1.0692 0.3740 0.8518 11.00000 0.05 0.42 Q6 1 0.9462 0.3364 0.8137 11.00000 0.05 0.36 Q7 1 0.5632 0.2898 0.7668 11.00000 0.05 0.32 Q8 1 1.0930 0.3201 0.7980 11.00000 0.05 0.31 Q9 1 0.3178 0.0500 0.4551 11.00000 0.05 0.27 Q10 1 0.8737 0.0479 0.6200 11.00000 0.05 0.27 Q11 1 0.7556 0.4750 0.5020 11.00000 0.05 0.24 Q12 1 1.1061 0.4414 0.7635 11.00000 0.05 0.24 Q13 1 0.5287 0.1455 0.7548 11.00000 0.05 0.23 Q14 1 0.5286 0.4486 0.4767 11.00000 0.05 0.23 Q15 1 0.9039 0.0628 0.7019 11.00000 0.05 0.23 Q16 1 0.6727 0.0908 0.5771 11.00000 0.05 0.23 Q17 1 0.7615 0.5925 0.4006 11.00000 0.05 0.23 Q18 1 0.6625 0.4664 0.5272 11.00000 0.05 0.23 Q19 1 0.8753 0.2909 0.8485 11.00000 0.05 0.22 Q20 1 0.7142 0.4671 0.5605 11.00000 0.05 0.22 ; _shelx_res_checksum 8034 _shelx_hkl_file ; 1 0 0 3520 915 1 2 0 0 661529 17801 1 3 0 0 31184 3182 1 4 0 0 781353 14093 1 5 0 0 31639 3237 1 6 0 0 150424 6810 1 7 0 0 19076 4457 1 8 0 0 -3791 3791 1 9 0 0 6591 3455 1 1 1 0 1493544 33325 1 2 1 0 19273 1806 1 3 1 0 785227 14837 1 4 1 0 53357 3224 1 -5 -1 1 25900 1970 -2 5 1 0 25900 1970 1 6 1 0 23068 2600 1 7 1 0 1418 2529 1 8 1 0 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