############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section A. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section A, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_IRELOH _database_code_depnum_ccdc_archive 'CCDC 1870980' #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic 2018-07-17 _journal_date_accepted 2018-10-02 _journal_name_full 'Acta Crystallographica, Section A' _journal_year 2019 _journal_volume 75 _journal_issue 1 _journal_page_first 0 _journal_page_last 0 _journal_paper_category FA _journal_paper_doi 10.1107/S2053273318013918 _journal_coeditor_code TD5055 #============================================================================== _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 O5' _chemical_formula_weight 290.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0000 0.0000 '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' 'O' 'O' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.0150(16) _cell_length_b 10.015(2) _cell_length_c 17.703(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1421.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 77 _cell_measurement_reflns_used 6096 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_F_000 238 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 0.081 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 77 _diffrn_radiation_wavelength 0.02508 _diffrn_radiation_type 'Electron diffraction' _diffrn_source 'FEG 200[kV]' _diffrn_measurement_device_type 'FEI Polara TEM' _diffrn_measurement_method 'Rotation method' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6096 _diffrn_reflns_av_unetI/netI 0.1609 _diffrn_reflns_av_R_equivalents 0.1576 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.081 _diffrn_reflns_theta_max 0.882 _diffrn_reflns_theta_full 0.862 _diffrn_measured_fraction_theta_max 0.834 _diffrn_measured_fraction_theta_full 0.853 _diffrn_reflns_Laue_measured_fraction_max 0.834 _diffrn_reflns_Laue_measured_fraction_full 0.853 _diffrn_reflns_point_group_measured_fraction_max 0.835 _diffrn_reflns_point_group_measured_fraction_full 0.859 _reflns_number_total 2295 _reflns_number_gt 1899 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.723 _reflns_Friedel_fraction_max 0.837 _reflns_Friedel_fraction_full 0.868 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _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^)+(0.1527P)^2^+0.8359P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; All f" are zero, so absolute structure could not be determined ; _refine_ls_abs_structure_Flack ? _chemical_absolute_configuration ? _refine_ls_number_reflns 2295 _refine_ls_number_parameters 196 _refine_ls_number_restraints 156 _refine_ls_R_factor_all 0.1681 _refine_ls_R_factor_gt 0.1495 _refine_ls_wR_factor_ref 0.3690 _refine_ls_wR_factor_gt 0.3531 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.750 _refine_ls_shift/su_mean 0.017 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 C1 C 0.810(2) 0.3379(15) 0.5236(7) 0.023(3) Uani 1 1 d . U . . . O1 O 0.871(3) 0.2401(14) 0.4944(8) 0.052(5) Uani 1 1 d . U . . . C2 C 0.743(2) 0.3366(14) 0.6037(7) 0.021(3) Uani 1 1 d . U . . . H2A H 0.6241 0.3183 0.6018 0.025 Uiso 1 1 calc R U . . . H2B H 0.7953 0.2638 0.6309 0.025 Uiso 1 1 calc R U . . . C4 C 0.9276(18) 0.5014(12) 0.6708(6) 0.015(3) Uani 1 1 d . U . . . H4 H 1.0184 0.4500 0.6558 0.018 Uiso 1 1 calc R U . . . C3 C 0.7692(17) 0.4633(13) 0.6478(6) 0.014(3) Uani 1 1 d . U . . . C5 C 0.9551(19) 0.6101(13) 0.7141(7) 0.016(3) Uani 1 1 d . U . . . O5 O 1.1117(15) 0.6509(12) 0.7373(6) 0.023(3) Uani 1 1 d . U . . . H5 H 1.191(7) 0.586(6) 0.724(3) 0.024(15) Uiso 1 1 calc R . . . . C6 C 0.821(2) 0.6935(14) 0.7361(8) 0.021(3) Uani 1 1 d . U . . . H6 H 0.8403 0.7693 0.7651 0.025 Uiso 1 1 calc R U . . . C7 C 0.6643(18) 0.6610(13) 0.7140(6) 0.014(2) Uani 1 1 d . U . . . O7 O 0.5304(15) 0.7381(11) 0.7321(5) 0.017(2) Uani 1 1 d . U . . . H7 H 0.573(3) 0.828(7) 0.761(4) 0.026 Uiso 1 1 calc R U . . . C8 C 0.6326(17) 0.5495(12) 0.6692(6) 0.011(2) Uani 1 1 d . U . . . C9 C 0.4559(19) 0.5178(12) 0.6472(6) 0.016(3) Uani 1 1 d . U . . . O9 O 0.3622(17) 0.4667(11) 0.6916(6) 0.022(2) Uani 1 1 d . U . . . C10 C 0.4020(18) 0.5592(13) 0.5710(6) 0.017(3) Uani 1 1 d . U . . . H10 H 0.2927 0.5413 0.5565 0.020 Uiso 1 1 calc R U . . . C11 C 0.5025(19) 0.6216(13) 0.5212(6) 0.017(3) Uani 1 1 d . U . . . H11 H 0.6089 0.6463 0.5368 0.020 Uiso 1 1 calc R U . . . C12 C 0.451(2) 0.6529(14) 0.4422(6) 0.018(3) Uani 1 1 d . U . . . H12A H 0.4776 0.7452 0.4308 0.021 Uiso 1 1 calc R U . . . H12B H 0.3310 0.6419 0.4374 0.021 Uiso 1 1 calc R U . . . C13 C 0.5394(19) 0.5610(14) 0.3853(7) 0.021(3) Uani 1 1 d . U . . . H13A H 0.5183 0.4690 0.3995 0.025 Uiso 1 1 calc R U . . . H13B H 0.4905 0.5750 0.3358 0.025 Uiso 1 1 calc R U . . . C14 C 0.7287(19) 0.5817(15) 0.3794(7) 0.022(3) Uani 1 1 d . U . . . H14A H 0.7567 0.5944 0.3266 0.026 Uiso 1 1 calc R U . . . H14B H 0.7569 0.6636 0.4057 0.026 Uiso 1 1 calc R U . . . C15 C 0.8381(19) 0.4702(14) 0.4106(7) 0.021(3) Uani 1 1 d . U . . . H15 H 0.8107 0.3869 0.3843 0.025 Uiso 1 1 calc R U . . . C16 C 1.0191(18) 0.4938(14) 0.4046(7) 0.022(3) Uani 1 1 d . U . . . H16A H 1.0780 0.4253 0.4316 0.032 Uiso 1 1 calc R U . . . H16B H 1.0457 0.5794 0.4259 0.032 Uiso 1 1 calc R U . . . H16C H 1.0516 0.4921 0.3524 0.032 Uiso 1 1 calc R U . . . O16 O 0.7941(16) 0.4563(11) 0.4903(5) 0.019(2) Uani 1 1 d . U . . . 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 C1 0.038(9) 0.015(5) 0.016(5) -0.002(4) 0.002(5) 0.009(5) O1 0.104(14) 0.016(6) 0.036(6) 0.005(5) 0.021(8) 0.028(7) C2 0.033(8) 0.011(6) 0.018(5) -0.003(4) 0.001(5) 0.008(5) C4 0.022(6) 0.007(5) 0.016(5) 0.000(4) 0.000(4) 0.001(4) C3 0.024(6) 0.008(5) 0.010(5) 0.001(4) -0.005(4) 0.002(4) C5 0.022(6) 0.005(5) 0.020(6) -0.001(4) 0.003(4) 0.001(4) O5 0.025(6) 0.026(7) 0.020(5) -0.006(5) 0.007(4) -0.002(4) C6 0.023(5) 0.014(7) 0.025(6) -0.018(5) 0.002(4) -0.001(4) C7 0.022(6) 0.006(5) 0.014(5) -0.005(4) 0.003(4) 0.001(4) O7 0.028(6) 0.009(5) 0.015(4) 0.001(4) 0.001(4) 0.010(4) C8 0.025(5) 0.002(5) 0.007(4) 0.002(4) -0.005(4) 0.001(3) C9 0.029(6) 0.011(6) 0.008(4) 0.000(4) -0.001(4) -0.007(4) O9 0.033(6) 0.012(6) 0.020(4) 0.008(4) 0.001(4) -0.003(4) C10 0.026(7) 0.018(7) 0.006(4) 0.003(4) -0.005(4) -0.011(5) C11 0.027(8) 0.015(7) 0.008(4) 0.010(4) -0.004(4) -0.004(5) C12 0.028(8) 0.014(7) 0.010(5) 0.006(4) -0.002(4) 0.007(5) C13 0.034(7) 0.017(7) 0.012(5) 0.009(5) 0.002(5) 0.003(5) C14 0.032(6) 0.020(7) 0.013(5) 0.013(5) -0.001(4) 0.005(5) C15 0.032(7) 0.013(7) 0.017(5) 0.001(5) -0.005(4) 0.009(5) C16 0.036(7) 0.009(7) 0.020(6) 0.002(5) -0.001(5) 0.008(5) O16 0.036(7) 0.013(5) 0.009(4) -0.001(3) -0.005(4) 0.011(4) _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 C1 O1 1.210(19) . ? C1 O16 1.331(18) . ? C1 C2 1.517(18) . ? C2 C3 1.505(18) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C5 1.350(18) . ? C4 C3 1.386(19) . ? C4 H4 0.9300 . ? C3 C8 1.445(18) . ? C5 O5 1.382(18) . ? C5 C6 1.41(2) . ? O5 H5 0.94(8) . ? C6 C7 1.36(2) . ? C6 H6 0.9300 . ? C7 O7 1.360(17) . ? C7 C8 1.393(17) . ? O7 H7 1.09(7) . ? C8 C9 1.503(19) . ? C9 O9 1.201(18) . ? C9 C10 1.476(15) . ? C10 C11 1.348(17) . ? C10 H10 0.9300 . ? C11 C12 1.493(16) . ? C11 H11 0.9300 . ? C12 C13 1.538(18) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.54(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.523(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O16 1.461(16) . ? C15 C16 1.47(2) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 C1 O16 124.8(13) . . ? O1 C1 C2 122.4(13) . . ? O16 C1 C2 112.8(11) . . ? C3 C2 C1 115.4(12) . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? C1 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C5 C4 C3 122.5(13) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C3 C8 116.9(11) . . ? C4 C3 C2 120.8(12) . . ? C8 C3 C2 122.2(12) . . ? C4 C5 O5 123.7(13) . . ? C4 C5 C6 120.5(14) . . ? O5 C5 C6 115.7(12) . . ? C5 O5 H5 109.5 . . ? C7 C6 C5 118.9(12) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C6 C7 O7 121.9(12) . . ? C6 C7 C8 121.7(12) . . ? O7 C7 C8 116.4(12) . . ? C7 O7 H7 109.5 . . ? C7 C8 C3 119.3(12) . . ? C7 C8 C9 119.3(11) . . ? C3 C8 C9 121.3(11) . . ? O9 C9 C10 122.3(14) . . ? O9 C9 C8 120.6(11) . . ? C10 C9 C8 117.0(11) . . ? C11 C10 C9 123.6(13) . . ? C11 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? C10 C11 C12 123.0(14) . . ? C10 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C11 C12 C13 111.1(11) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 114.8(12) . . ? C14 C13 H13A 108.6 . . ? C12 C13 H13A 108.6 . . ? C14 C13 H13B 108.6 . . ? C12 C13 H13B 108.6 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C13 116.4(12) . . ? C15 C14 H14A 108.2 . . ? C13 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? C13 C14 H14B 108.2 . . ? H14A C14 H14B 107.3 . . ? O16 C15 C16 108.8(11) . . ? O16 C15 C14 106.3(11) . . ? C16 C15 C14 115.0(12) . . ? O16 C15 H15 108.9 . . ? C16 C15 H15 108.9 . . ? C14 C15 H15 108.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 O16 C15 119.3(11) . . ? _refine_diff_density_max 0.172 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.052 _shelx_res_file ; N14_a.res created by SHELXL-2014/7 TITL N14_a.res in P2(1)2(1)2(1) REM Old TITL N14 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.235, Rweak 0.226, Alpha 0.039, Orientation as input REM Flack x = -1.759 ( 5.350 ) from Parsons' quotients REM Formula found by SHELXT: C19 O2 CELL 0.02508 8.0150 10.0149 17.7032 90.000 90.000 90.000 ZERR 4.000 0.0016 0.0020 0.0036 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C 0.208 0.922 0.702 5.018 1.144 16.523 0.425 47.300 0.030 = 0.0 0.0 11.500 0.770 12.010 SFAC H 0.042 0.991 0.103 3.924 0.205 11.597 0.170 31.984 0.006 = 0.0 0.0 0.620 0.310 1.000 SFAC O 0.237 0.799 0.649 3.654 0.800 10.924 0.261 29.964 0.035 = 0.0 0.0 18.200 0.660 16.000 UNIT 64 72 20 L.S. 10 BOND $H RIGU ACTA XNPD 0.001 LIST 6 FMAP 2 PLAN 20 WGHT 0.152700 0.835900 FVAR 2.52846 C1 1 0.809895 0.337888 0.523582 11.00000 0.03829 0.01456 = 0.01617 -0.00157 0.00243 0.00878 O1 3 0.870920 0.240113 0.494415 11.00000 0.10408 0.01613 = 0.03611 0.00512 0.02075 0.02814 C2 1 0.742826 0.336644 0.603726 11.00000 0.03325 0.01101 = 0.01767 -0.00285 0.00124 0.00775 AFIX 23 H2A 2 0.624078 0.318270 0.601791 11.00000 -1.20000 H2B 2 0.795307 0.263766 0.630891 11.00000 -1.20000 AFIX 0 C4 1 0.927579 0.501373 0.670824 11.00000 0.02187 0.00686 = 0.01575 0.00002 0.00023 0.00143 AFIX 43 H4 2 1.018385 0.450000 0.655827 11.00000 -1.20000 AFIX 0 C3 1 0.769204 0.463319 0.647841 11.00000 0.02376 0.00774 = 0.01022 0.00146 -0.00523 0.00173 C5 1 0.955071 0.610117 0.714129 11.00000 0.02210 0.00482 = 0.02018 -0.00125 0.00298 0.00071 O5 3 1.111674 0.650947 0.737258 11.00000 0.02473 0.02558 = 0.01968 -0.00648 0.00685 -0.00239 AFIX 148 H5 2 1.191112 0.585737 0.723772 11.00000 0.02350 AFIX 0 C6 1 0.821107 0.693480 0.736074 11.00000 0.02260 0.01402 = 0.02508 -0.01769 0.00183 -0.00062 AFIX 43 H6 2 0.840284 0.769305 0.765132 11.00000 -1.20000 AFIX 0 C7 1 0.664330 0.660996 0.714044 11.00000 0.02154 0.00643 = 0.01395 -0.00464 0.00258 0.00096 O7 3 0.530389 0.738070 0.732053 11.00000 0.02758 0.00927 = 0.01517 0.00086 0.00103 0.01034 AFIX 148 H7 2 0.572869 0.828360 0.761004 11.00000 -1.50000 AFIX 0 C8 1 0.632594 0.549535 0.669221 11.00000 0.02465 0.00234 = 0.00691 0.00232 -0.00521 0.00084 C9 1 0.455865 0.517815 0.647188 11.00000 0.02854 0.01065 = 0.00794 0.00040 -0.00074 -0.00676 O9 3 0.362212 0.466684 0.691564 11.00000 0.03317 0.01200 = 0.01995 0.00772 0.00099 -0.00308 C10 1 0.401985 0.559232 0.570995 11.00000 0.02562 0.01810 = 0.00649 0.00320 -0.00461 -0.01134 AFIX 43 H10 2 0.292698 0.541307 0.556548 11.00000 -1.20000 AFIX 0 C11 1 0.502524 0.621620 0.521199 11.00000 0.02673 0.01538 = 0.00793 0.00995 -0.00364 -0.00382 AFIX 43 H11 2 0.608940 0.646317 0.536797 11.00000 -1.20000 AFIX 0 C12 1 0.450790 0.652860 0.442159 11.00000 0.02804 0.01438 = 0.01016 0.00582 -0.00156 0.00680 AFIX 23 H12A 2 0.477593 0.745156 0.430812 11.00000 -1.20000 H12B 2 0.331005 0.641873 0.437414 11.00000 -1.20000 AFIX 0 C13 1 0.539369 0.560976 0.385283 11.00000 0.03366 0.01720 = 0.01195 0.00935 0.00211 0.00340 AFIX 23 H13A 2 0.518288 0.468966 0.399486 11.00000 -1.20000 H13B 2 0.490494 0.575008 0.335790 11.00000 -1.20000 AFIX 0 C14 1 0.728714 0.581719 0.379399 11.00000 0.03175 0.01998 = 0.01319 0.01337 -0.00119 0.00515 AFIX 23 H14A 2 0.756738 0.594417 0.326582 11.00000 -1.20000 H14B 2 0.756894 0.663631 0.405708 11.00000 -1.20000 AFIX 0 C15 1 0.838119 0.470199 0.410574 11.00000 0.03161 0.01311 = 0.01693 0.00070 -0.00491 0.00935 AFIX 13 H15 2 0.810711 0.386895 0.384313 11.00000 -1.20000 AFIX 0 C16 1 1.019141 0.493814 0.404600 11.00000 0.03552 0.00949 = 0.01967 0.00193 -0.00054 0.00751 AFIX 137 H16A 2 1.077995 0.425342 0.431622 11.00000 -1.50000 H16B 2 1.045692 0.579391 0.425870 11.00000 -1.50000 H16C 2 1.051647 0.492092 0.352417 11.00000 -1.50000 AFIX 0 O16 3 0.794112 0.456344 0.490302 11.00000 0.03597 0.01257 = 0.00922 -0.00093 -0.00470 0.01128 HKLF 4 REM N14_a.res in P2(1)2(1)2(1) REM R1 = 0.1495 for 1899 Fo > 4sig(Fo) and 0.1681 for all 2295 data REM 196 parameters refined using 156 restraints END WGHT 0.1539 0.7772 REM Highest difference peak 0.172, deepest hole -0.188, 1-sigma level 0.052 Q1 1 0.8012 0.8018 0.3569 11.00000 0.05 0.17 Q2 1 0.5495 0.4611 0.5000 11.00000 0.05 0.16 Q3 1 0.6874 0.3859 0.5006 11.00000 0.05 0.16 Q4 1 0.8367 0.6986 0.3858 11.00000 0.05 0.16 Q5 1 1.0738 0.5385 0.3146 11.00000 0.05 0.16 Q6 1 0.3692 0.5020 0.4929 11.00000 0.05 0.16 Q7 1 0.5482 0.3830 0.5807 11.00000 0.05 0.16 Q8 1 0.7392 0.7640 0.3783 11.00000 0.05 0.16 Q9 1 0.4818 0.4715 0.5770 11.00000 0.05 0.15 Q10 1 0.9669 0.4391 0.2852 11.00000 0.05 0.14 Q11 1 0.9140 0.7678 0.3750 11.00000 0.05 0.14 Q12 1 0.4373 0.5063 0.7588 11.00000 0.05 0.14 Q13 1 0.3219 0.7585 0.3717 11.00000 0.05 0.14 Q14 1 1.1400 0.3551 0.2978 11.00000 0.05 0.14 Q15 1 1.0889 0.4730 0.7271 11.00000 0.05 0.13 Q16 1 0.8264 0.8460 0.7198 11.00000 0.05 0.13 Q17 1 0.2819 0.6408 0.5644 11.00000 0.05 0.13 Q18 1 0.6664 0.8701 0.7267 11.00000 0.05 0.13 Q19 1 0.4981 0.7705 0.3741 11.00000 0.05 0.13 Q20 1 0.8295 0.2455 0.3794 11.00000 0.05 0.13 ; _shelx_res_checksum 57192 _shelx_hkl_file ; 0 0 2 136.90 30.61 0 0 -2 132.69 29.61 0 0 4 35.12 10.89 0 0 -4 28.73 9.96 0 0 6 465.36 101.36 0 0 -6 475.14 103.51 0 0 8 1978.34 428.80 0 0 -8 2022.12 438.24 0 0 10 330.96 73.12 0 0 -10 338.68 74.71 0 0 12 829.36 180.75 0 0 -12 905.49 197.23 0 0 14 48.49 14.55 0 0 -14 50.67 15.03 0 0 16 37.75 12.49 0 0 -16 29.78 11.36 0 0 18 98.19 24.37 0 0 -18 112.44 27.49 0 0 20 13.32 8.67 0 0 -20 19.03 9.75 0 -1 2 1956.03 161.01 0 -1 2 2446.97 505.87 0 1 -2 2240.98 179.64 0 1 -2 3646.85 753.83 0 -1 3 1331.20 275.42 0 1 -3 1407.58 291.21 0 -1 4 9999.00 2066.75 0 1 -4 6343.57 1310.60 0 -1 5 703.11 152.60 0 -1 5 793.14 164.27 0 1 -5 721.99 156.63 0 1 -5 924.37 191.31 0 -1 6 3300.10 714.35 0 -1 6 3473.48 717.95 0 1 -6 3308.68 716.24 0 1 -6 3294.09 680.87 0 -1 7 6776.15 1465.94 0 -1 7 3724.95 769.88 0 1 -7 4567.79 988.74 0 1 -7 3852.84 796.40 0 1 8 2489.88 539.52 0 -1 8 1871.91 405.71 0 -1 8 1735.45 358.93 0 -1 -8 2702.73 585.60 0 1 -8 2132.83 462.18 0 1 -8 1932.00 399.62 0 1 9 35.88 12.01 0 -1 9 57.08 15.03 0 -1 9 38.63 10.70 0 -1 -9 95.27 23.21 0 1 -9 49.47 13.53 0 1 -9 68.83 16.00 0 1 10 30.75 11.78 0 -1 10 57.57 15.48 0 -1 10 19.23 7.67 0 -1 -10 79.61 20.49 0 1 -10 20.56 9.30 0 1 -10 40.86 11.59 0 1 11 3165.35 685.94 0 -1 11 2452.98 531.62 0 -1 11 2150.86 445.02 0 -1 -11 3075.23 666.37 0 1 -11 2454.69 531.97 0 1 -11 2070.18 428.20 0 1 12 920.94 200.75 0 -1 12 754.86 164.53 0 -1 12 689.20 143.34 0 -1 -12 862.57 188.05 0 1 -12 630.07 137.67 0 1 -12 628.95 130.81 0 1 13 240.75 54.20 0 -1 13 227.10 50.90 0 -1 13 265.38 56.26 0 -1 -13 315.94 70.22 0 1 -13 215.17 48.78 0 1 -13 231.05 49.13 0 1 14 317.82 70.84 0 -1 14 282.46 62.91 0 -1 14 313.45 66.29 0 -1 -14 396.10 87.54 0 1 -14 267.52 59.75 0 1 -14 310.79 65.69 0 1 15 112.95 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9.14 8.22 0 -2 19 13.65 7.65 0 -2 19 5.46 6.55 0 -2 -19 29.40 11.04 0 2 -19 7.42 7.86 0 2 -19 13.70 7.51 0 2 20 17.47 9.08 0 -2 20 6.64 7.05 0 -2 20 13.66 6.96 0 -2 -20 17.42 9.48 0 2 -20 4.73 7.60 0 2 -20 5.52 7.30 0 -2 21 -0.96 18.67 0 -2 -21 26.58 11.17 0 2 -21 13.87 8.39 0 2 -21 17.25 7.94 0 3 1 1688.24 148.92 0 -3 -1 1424.75 136.64 0 3 -1 1532.90 138.79 0 -3 3 -37.43 70.59 0 3 -3 -113.29 62.65 0 -3 4 1662.50 148.49 0 3 -4 1409.30 127.11 0 -3 5 -36.64 72.22 0 -3 5 27.92 9.78 0 3 -5 -66.95 63.35 0 3 -5 15.14 8.28 0 -3 7 74.77 17.96 0 3 -7 90.81 20.95 0 -3 8 3653.71 755.64 0 3 -8 3465.75 716.67 0 -3 10 3108.70 643.03 0 3 -10 3084.67 637.97 0 -3 11 49.72 13.34 0 3 -11 24.98 9.28 0 -3 12 897.76 186.50 0 3 -12 755.72 157.15 0 -3 13 97.67 22.50 0 3 -13 88.92 20.89 0 -3 14 743.28 154.57 0 3 -14 615.56 134.67 0 3 -14 783.95 162.98 0 -3 15 14.06 8.00 0 -3 15 54.76 13.96 0 3 -15 30.78 10.99 0 3 -15 36.52 11.25 0 -3 16 12.53 7.79 0 -3 16 16.14 7.65 0 3 -16 11.86 8.12 0 3 -16 10.54 7.32 0 -3 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115.18 29.48 6 7 -2 119.73 29.09 -6 -7 -2 190.62 43.75 -6 -7 -2 130.38 30.86 6 7 2 138.19 33.96 6 7 2 163.76 39.12 -6 -7 2 186.68 42.55 -6 -7 2 123.25 30.55 6 7 -3 73.35 20.88 6 7 -3 83.78 22.08 -6 -7 -3 90.38 22.73 -6 -7 -3 82.85 22.02 6 7 3 65.31 19.43 -6 -7 3 83.21 20.66 -6 -7 3 81.97 23.83 6 7 -4 29.34 12.87 6 7 -4 59.06 18.25 -6 -7 -4 47.88 14.31 -6 -7 -4 49.68 16.58 6 7 4 96.47 28.68 6 7 4 46.26 15.75 -6 -7 4 68.65 17.39 -6 -7 4 59.80 19.91 6 7 -5 9.23 9.55 6 7 -5 21.30 11.96 -6 -7 -5 23.03 9.82 -6 -7 -5 41.34 15.50 6 7 5 12.46 10.51 6 7 5 19.01 13.66 -6 -7 5 18.86 7.97 -6 -7 5 26.06 16.90 6 7 -6 22.62 10.89 6 7 -6 43.98 15.33 -6 -7 -6 46.30 13.95 -6 -7 -6 47.56 18.35 6 7 6 35.06 13.72 6 7 6 40.28 14.62 -6 -7 6 51.50 13.52 -6 -7 6 42.51 18.27 6 7 -7 2.01 8.68 6 7 -7 5.14 11.90 -6 -7 -7 10.14 9.09 6 7 7 9.90 10.39 6 7 7 23.18 10.98 -6 -7 7 12.14 6.89 -6 -7 7 6.66 14.18 6 7 -8 23.00 10.48 6 7 -8 26.94 14.78 -6 -7 -8 41.59 13.82 -6 -7 -8 57.09 20.21 6 7 8 28.83 12.98 6 7 8 41.09 13.29 -6 -7 8 42.93 11.62 -6 -7 8 43.28 17.37 6 7 -9 3.24 7.37 -6 -7 -9 5.92 8.49 -6 -7 -9 22.33 12.64 6 7 9 17.43 10.94 6 7 9 12.62 9.25 -6 -7 9 34.90 9.80 -6 -7 9 5.30 12.31 -6 -7 -10 23.58 10.51 -6 -7 -10 48.18 15.35 -6 -7 10 44.70 11.42 -6 -7 10 16.98 13.13 -6 -7 -11 24.92 10.75 -6 -7 -11 31.40 12.20 -6 -7 11 34.62 9.16 -6 -7 11 31.03 14.28 6 8 0 13.35 11.37 6 8 0 12.71 10.42 -6 -8 0 16.84 8.58 -6 -8 0 18.07 13.80 6 8 -1 12.13 11.33 6 8 -1 3.43 10.25 -6 -8 -1 11.63 8.18 -6 -8 -1 20.51 12.91 6 8 1 9.95 10.81 6 8 1 20.58 11.16 -6 -8 1 14.87 8.59 -6 -8 1 3.67 14.50 6 8 -2 60.94 19.29 6 8 -2 41.42 15.40 -6 -8 -2 89.26 22.59 -6 -8 -2 102.39 25.41 6 8 2 59.73 18.75 6 8 2 34.13 12.89 -6 -8 2 130.46 30.84 6 8 -3 51.40 17.47 -6 -8 -3 97.59 24.47 -6 -8 -3 73.98 19.71 6 8 3 67.65 20.44 6 8 3 50.14 15.41 -6 -8 3 74.82 19.27 6 8 -4 34.53 14.63 -6 -8 -4 65.01 18.00 -6 -8 -4 77.10 19.99 6 8 4 51.28 17.97 6 8 4 62.18 17.19 -6 -8 4 126.08 29.77 -6 -8 4 53.14 18.61 6 8 -5 39.58 15.05 -6 -8 -5 51.02 15.17 -6 -8 -5 36.84 12.66 6 8 5 29.83 14.01 6 8 5 44.13 13.81 -6 -8 5 25.00 13.92 6 8 -6 3.60 9.05 -6 -8 -6 21.82 10.16 -6 -8 -6 21.33 9.93 6 8 6 28.44 10.66 6 8 6 33.28 12.33 -6 -8 6 8.34 11.12 6 8 -7 21.93 9.14 -6 -8 -7 4.42 8.21 -6 -8 -7 2.13 8.15 6 8 7 -7.14 23.98 -6 -8 7 6.80 9.84 6 8 -8 -6.47 136.21 -6 -8 -8 8.60 8.42 -6 -8 -8 0.02 8.18 -6 -8 8 1.05 9.11 -6 -8 -9 27.52 11.01 -6 -8 -9 21.82 9.52 -6 -8 9 10.81 10.12 -6 -9 0 33.25 12.57 -6 -9 -1 13.92 10.20 -6 -9 1 13.03 9.81 -6 -9 -2 14.04 9.98 -6 -9 2 10.19 9.71 -6 -9 -3 53.51 16.25 -6 -9 -3 14.72 9.90 -6 -9 3 12.33 11.11 -6 -9 -4 51.13 15.15 -6 -9 -4 28.67 11.29 6 9 4 0.57 3.06 -6 -9 -5 18.87 9.43 -6 -9 -5 4.80 8.90 6 9 5 0.46 2.09 -6 -9 -6 15.51 9.07 -6 -9 -6 9.63 8.88 6 9 6 -0.05 6.38 -7 -1 -11 12.39 8.31 -7 -1 -12 4.14 7.46 -7 -1 -13 6.34 7.67 -7 -1 -14 4.67 7.55 -7 -2 -6 7.58 8.64 -7 -2 -7 37.21 12.70 7 2 7 27.37 12.85 -7 -2 -8 4.73 8.62 7 2 8 5.24 9.78 -7 -2 -9 77.96 20.27 7 2 9 94.67 24.74 -7 -2 -10 53.86 15.31 7 2 10 38.40 13.65 -7 -2 -11 30.81 11.33 7 2 11 27.11 11.41 -7 -2 -12 23.21 10.41 -7 -2 -13 23.97 10.20 -7 -3 -2 168.31 39.03 -7 -3 -3 72.11 19.22 7 3 3 65.03 18.36 -7 -3 -4 46.35 14.29 7 3 4 108.06 27.10 -7 -3 -5 25.36 11.04 7 3 5 34.52 13.57 -7 -3 -6 15.58 9.74 7 3 6 17.23 10.64 -7 -3 -7 44.50 14.21 7 3 7 13.60 10.40 -7 -3 -8 45.75 14.31 7 3 8 53.87 16.50 -7 -3 -9 40.55 13.07 7 3 9 63.34 18.07 -7 -3 -10 39.94 12.90 7 3 10 47.69 15.25 -7 -3 -11 6.92 8.04 7 3 11 12.45 11.07 -7 -3 -12 17.59 9.10 -7 -3 -13 3.69 7.86 7 4 0 44.30 14.79 -7 -4 0 108.40 26.44 7 4 -1 35.67 13.47 -7 -4 -1 32.79 11.85 7 4 1 29.68 12.29 -7 -4 1 28.19 11.04 7 4 -2 33.43 13.14 -7 -4 -2 39.82 13.14 7 4 2 28.49 12.16 -7 -4 2 32.94 11.57 -7 -4 -3 22.83 10.32 7 4 3 37.54 13.52 -7 -4 3 33.69 11.38 -7 -4 -4 19.90 9.78 7 4 4 30.02 12.26 -7 -4 -5 62.18 17.51 7 4 5 58.62 17.52 -7 -4 -6 5.84 8.59 7 4 6 15.52 10.74 -7 -4 -7 10.13 8.44 7 4 7 8.46 8.87 -7 -4 -8 34.92 12.09 7 4 8 26.30 11.35 -7 -4 -9 72.94 19.55 7 4 9 65.33 18.59 -7 -4 -10 6.93 8.66 7 4 10 8.70 9.99 -7 -4 -11 25.40 10.63 -7 -4 -12 14.37 8.80 7 5 0 15.70 10.81 7 5 0 28.14 15.10 -7 -5 0 20.03 9.66 7 5 -1 30.43 12.80 7 5 -1 35.26 16.73 -7 -5 -1 33.86 11.92 7 5 1 38.16 13.78 7 5 1 42.42 16.98 -7 -5 1 26.53 10.46 7 5 -2 41.70 14.63 7 5 -2 55.30 19.81 -7 -5 -2 35.32 12.41 7 5 2 36.53 13.41 7 5 2 57.21 19.19 -7 -5 2 49.58 14.45 7 5 -3 56.47 17.13 7 5 -3 49.83 18.62 -7 -5 -3 44.43 13.94 7 5 3 33.40 12.73 7 5 3 49.75 18.02 -7 -5 3 36.79 11.84 7 5 -4 50.82 15.60 7 5 -4 79.55 24.61 -7 -5 -4 45.94 14.02 -7 -5 -4 71.78 23.25 7 5 4 45.77 14.73 7 5 4 64.12 21.00 -7 -5 4 54.96 14.79 7 5 -5 17.42 9.81 7 5 -5 13.17 17.57 -7 -5 -5 9.34 8.17 -7 -5 -5 66.44 21.66 7 5 5 21.23 10.76 7 5 5 16.26 15.70 -7 -5 5 24.12 8.89 7 5 -6 9.07 8.35 -7 -5 -6 15.17 9.01 -7 -5 -6 15.75 13.97 7 5 6 14.92 9.96 7 5 6 12.99 14.33 -7 -5 6 17.46 7.67 -7 -5 -7 13.35 9.04 -7 -5 -7 31.89 15.66 7 5 7 21.83 10.51 7 5 7 28.39 15.54 -7 -5 7 10.79 6.47 -7 -5 -8 7.43 8.52 -7 -5 -8 7.43 12.65 7 5 8 9.26 9.44 7 5 8 17.35 13.89 -7 -5 8 8.63 6.11 -7 -5 -9 2.59 8.09 -7 -5 -9 23.22 13.43 7 5 9 6.68 9.08 7 5 9 12.51 13.30 -7 -5 -10 5.74 8.03 -7 -5 -10 13.78 12.86 7 5 10 2.81 12.93 -7 -5 -11 5.84 8.04 -7 -5 -11 -5.49 11.54 -7 -5 -12 6.60 12.39 7 6 0 94.67 24.43 7 6 0 92.52 26.77 -7 -6 0 73.54 19.00 -7 -6 0 74.15 24.20 7 6 -1 9.44 9.53 7 6 -1 25.62 17.11 -7 -6 -1 8.01 7.61 -7 -6 -1 30.49 18.02 7 6 1 5.14 9.13 7 6 1 9.30 15.22 -7 -6 1 11.42 7.83 -7 -6 1 14.17 16.90 7 6 -2 20.98 10.79 7 6 -2 38.56 18.46 -7 -6 -2 21.66 9.19 -7 -6 -2 20.61 16.93 7 6 2 29.99 11.98 7 6 2 30.66 16.82 -7 -6 2 29.89 10.19 -7 -6 2 38.92 18.20 7 6 -3 7.50 9.01 7 6 -3 12.41 15.64 -7 -6 -3 3.46 7.34 -7 -6 -3 -2.77 15.13 7 6 3 8.30 9.01 7 6 3 21.58 15.78 -7 -6 3 5.59 6.88 -7 -6 3 37.90 20.82 7 6 -4 31.40 11.91 7 6 -4 22.26 17.19 -7 -6 -4 27.56 10.56 -7 -6 -4 43.01 18.07 7 6 4 14.36 9.74 7 6 4 16.02 16.14 -7 -6 4 17.18 8.02 -7 -6 4 39.58 18.85 7 6 -5 28.96 11.72 7 6 -5 9.41 16.42 -7 -6 -5 21.03 10.02 -7 -6 -5 20.20 15.47 7 6 5 27.23 11.88 7 6 5 41.58 19.19 -7 -6 5 19.00 8.42 -7 -6 5 45.43 19.65 7 6 -6 59.61 17.05 -7 -6 -6 57.44 16.90 -7 -6 -6 105.57 28.19 7 6 6 70.56 20.32 7 6 6 93.90 26.62 -7 -6 6 88.32 21.40 -7 -6 6 62.14 22.56 7 6 -7 22.37 10.23 -7 -6 -7 34.12 16.64 -7 -6 -7 29.29 11.70 7 6 7 40.12 14.78 7 6 7 40.78 16.99 -7 -6 7 29.88 9.66 -7 -6 7 29.22 17.49 7 6 -8 11.43 8.24 -7 -6 -8 11.75 9.11 -7 -6 -8 12.34 13.92 7 6 8 18.45 9.56 7 6 8 -3.48 14.22 -7 -6 8 9.66 6.20 -7 -6 8 10.50 14.91 7 6 -9 35.38 10.76 -7 -6 -9 26.01 11.17 -7 -6 -9 22.15 14.89 -7 -6 9 10.47 5.81 -7 -6 9 25.54 15.58 -7 -6 -10 7.01 8.58 -7 -6 -10 15.46 13.98 -7 -6 10 12.57 5.75 -7 -6 10 9.17 13.71 7 7 0 6.03 11.56 7 7 0 8.45 14.03 -7 -7 0 47.27 14.13 -7 -7 0 20.08 16.10 7 7 -1 11.32 11.38 7 7 -1 5.19 14.99 -7 -7 -1 12.78 8.83 -7 -7 -1 9.65 14.14 7 7 1 13.19 11.85 7 7 1 29.31 16.27 -7 -7 1 6.93 8.30 -7 -7 1 19.46 16.00 7 7 -2 24.28 12.85 -7 -7 -2 45.93 14.14 -7 -7 -2 43.09 17.11 7 7 2 30.57 15.22 7 7 2 38.66 16.92 -7 -7 2 42.31 13.08 -7 -7 2 48.28 20.44 7 7 -3 10.54 11.01 -7 -7 -3 26.48 10.88 -7 -7 -3 25.75 14.44 7 7 3 31.28 15.05 7 7 3 28.84 14.78 -7 -7 3 28.24 10.45 -7 -7 3 48.76 22.58 7 7 -4 20.46 11.51 -7 -7 -4 26.69 14.21 -7 -7 -4 24.83 10.78 7 7 4 6.18 12.78 7 7 4 47.34 16.35 -7 -7 4 25.79 9.84 -7 -7 4 45.27 19.68 7 7 -5 0.83 9.67 -7 -7 -5 22.68 10.52 -7 -7 -5 18.54 13.29 7 7 5 43.81 14.32 -7 -7 5 30.33 10.39 -7 -7 5 7.68 15.23 7 7 -6 26.97 10.73 -7 -7 -6 36.03 12.87 -7 -7 -6 17.84 12.98 7 7 6 -9.70 247.45 -7 -7 6 31.09 10.17 -7 -7 6 50.68 20.60 7 7 -7 7.65 23.57 -7 -7 -7 41.03 13.84 -7 -7 -7 8.33 12.13 7 7 7 -0.91 17.00 -7 -7 7 11.58 6.96 -7 -7 7 5.14 16.47 7 7 -8 -1.47 16.08 -7 -7 -8 30.17 12.14 -7 -7 -8 18.84 12.74 -7 -7 8 13.75 6.90 -7 -7 8 9.23 15.45 -7 -8 0 14.51 8.09 -7 -8 0 11.41 11.66 -7 -8 -1 11.36 7.86 -7 -8 -1 5.29 10.83 -7 -8 1 9.02 7.23 -7 -8 1 1.44 12.81 -7 -8 -2 7.44 7.54 -7 -8 -2 15.57 10.26 -7 -8 2 13.79 7.76 -7 -8 2 13.20 14.03 -7 -8 -3 15.37 8.47 -7 -8 -3 15.92 10.45 -7 -8 3 10.56 7.30 -7 -8 -4 14.70 8.53 -7 -8 -4 12.46 9.76 -7 -8 4 10.80 7.25 -7 -8 -5 23.66 10.18 -7 -8 -5 9.17 10.35 -7 -8 5 21.53 8.55 -8 -2 -8 9.64 8.78 -8 -2 -9 24.65 10.49 -8 -2 -10 5.71 8.02 -8 -2 -11 8.90 8.24 -8 -3 -4 16.85 8.94 -8 -3 -5 5.49 7.59 8 3 5 5.37 8.49 -8 -3 -6 10.02 8.41 8 3 6 5.23 8.54 -8 -3 -7 34.68 12.37 8 3 7 11.60 10.02 -8 -3 -8 30.73 11.84 8 3 8 32.04 13.05 -8 -3 -9 5.02 8.04 -8 -3 -10 5.95 7.68 -8 -4 0 1.71 6.92 -8 -4 -1 4.42 7.21 8 4 1 13.40 9.36 -8 -4 1 5.53 6.89 -8 -4 -2 7.72 7.63 8 4 2 16.29 10.06 -8 -4 -3 27.40 10.45 8 4 3 13.19 9.57 -8 -4 -4 10.10 8.22 8 4 4 15.89 9.88 -8 -4 -5 14.03 9.00 8 4 5 7.03 9.40 -8 -4 -6 10.34 8.93 8 4 6 18.91 10.93 -8 -4 -7 29.11 11.31 8 4 7 25.00 10.42 -8 -4 -8 12.78 9.05 -8 -4 -9 14.47 9.04 -8 -4 -10 9.62 8.39 8 5 0 30.91 13.19 -8 -5 0 19.32 9.08 8 5 -1 24.52 12.02 -8 -5 -1 1.28 7.47 8 5 1 19.66 11.26 -8 -5 1 15.61 8.56 8 5 -2 18.99 11.29 -8 -5 -2 15.35 8.57 8 5 2 17.78 10.82 -8 -5 2 11.07 7.91 8 5 -3 13.86 10.38 -8 -5 -3 14.39 8.67 8 5 3 18.99 10.99 -8 -5 3 17.30 8.55 8 5 -4 10.02 9.57 -8 -5 -4 18.39 9.36 8 5 4 11.60 10.20 -8 -5 4 16.14 8.09 -8 -5 -5 10.05 8.64 8 5 5 18.10 9.94 -8 -5 5 13.60 7.65 -8 -5 -6 53.30 16.04 8 5 6 35.33 12.23 -8 -5 6 34.31 11.23 -8 -5 -7 21.66 10.33 8 5 7 -0.44 13.79 -8 -5 -8 16.84 9.55 -8 -6 0 20.69 9.23 -8 -6 0 12.29 14.49 -8 -6 -1 28.44 10.67 -8 -6 -1 14.44 14.75 -8 -6 1 27.23 10.07 -8 -6 1 18.11 15.27 -8 -6 -2 22.20 9.58 -8 -6 -2 8.81 13.51 -8 -6 2 6.71 7.14 -8 -6 2 6.95 14.75 -8 -6 -3 11.64 8.18 -8 -6 -3 17.60 14.24 8 6 3 0.05 50.46 -8 -6 3 6.69 6.91 -8 -6 3 12.54 18.25 -8 -6 -4 5.78 7.73 -8 -6 -4 14.07 13.86 8 6 4 -5.64 132.44 -8 -6 4 6.69 6.81 -8 -6 -5 22.21 9.92 -8 -6 -5 25.97 15.20 8 6 5 -3.97 45.97 -8 -6 5 9.60 7.16 -8 -6 -6 41.10 13.57 -8 -6 -6 49.51 18.22 -8 -6 6 50.96 13.89 -8 -7 0 6.41 6.84 -8 -7 0 -6.28 15.96 -8 -7 -1 12.08 7.72 -8 -7 -1 22.38 16.73 -8 -7 1 6.24 6.90 -8 -7 -2 10.25 7.77 -8 -7 -2 -10.06 14.46 -8 -7 2 6.97 6.79 -9 -3 -6 -0.09 7.83 -9 -3 -7 26.27 11.40 -9 -4 -1 10.57 7.95 -9 -4 -2 11.81 8.15 -9 -4 -3 22.92 9.78 -9 -4 -4 11.14 8.30 -9 -4 -5 3.05 7.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 79605 data_EPICZA _database_code_depnum_ccdc_archive 'CCDC 1870981' _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3.27 H2.91 N0.36 O1.09 S0.36' _chemical_formula_weight 76.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0000 0.0000 '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' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.996(2) _cell_length_b 12.452(2) _cell_length_c 13.218(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1809.8(6) _cell_formula_units_Z 22 _cell_measurement_temperature 77 _cell_measurement_reflns_used 12039 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_F_000 321 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 0.083 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 77 _diffrn_radiation_wavelength 0.02508 _diffrn_radiation_type 'Electron diffraction' _diffrn_source 'FEG 200[kV]' _diffrn_measurement_device_type 'FEI Polara TEM' _diffrn_measurement_method 'Rotation method' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12039 _diffrn_reflns_av_unetI/netI 0.1665 _diffrn_reflns_av_R_equivalents 0.1904 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.079 _diffrn_reflns_theta_max 0.877 _diffrn_reflns_theta_full 0.862 _diffrn_measured_fraction_theta_max 0.895 _diffrn_measured_fraction_theta_full 0.923 _diffrn_reflns_Laue_measured_fraction_max 0.895 _diffrn_reflns_Laue_measured_fraction_full 0.923 _diffrn_reflns_point_group_measured_fraction_max 0.873 _diffrn_reflns_point_group_measured_fraction_full 0.906 _reflns_number_total 2998 _reflns_number_gt 2342 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.702 _reflns_Friedel_fraction_max 0.843 _reflns_Friedel_fraction_full 0.883 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _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^)+(0.1854P)^2^+0.9670P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; All f" are zero, so absolute structure could not be determined ; _refine_ls_abs_structure_Flack ? _chemical_absolute_configuration ? _refine_ls_number_reflns 2998 _refine_ls_number_parameters 259 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.1721 _refine_ls_R_factor_gt 0.1543 _refine_ls_wR_factor_ref 0.3896 _refine_ls_wR_factor_gt 0.3760 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.034 _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 0.7984(7) 0.3219(5) 0.5081(6) 0.0254(17) Uani 1 1 d . U . . . O1 O 0.5400(13) 0.2158(11) 0.3831(12) 0.039(4) Uani 1 1 d . U . . . N1 N 0.7280(14) 0.4348(9) 0.3405(10) 0.027(3) Uani 1 1 d . U . . . C1 C 0.6810(14) 0.3656(10) 0.4151(11) 0.023(3) Uani 1 1 d . U . . . S2 S 0.9344(7) 0.2838(5) 0.4030(6) 0.0277(18) Uani 1 1 d . U . . . O2 O 0.8537(16) 0.4581(11) 0.2014(11) 0.042(4) Uani 1 1 d . U . . . N2 N 0.7280(12) 0.2250(9) 0.3017(10) 0.021(2) Uani 1 1 d . U . . . C2 C 0.8116(16) 0.4010(10) 0.2681(12) 0.027(3) Uani 1 1 d . U . . . C3 C 0.8385(14) 0.2819(10) 0.2857(11) 0.023(3) Uani 1 1 d . U . . . O3 O 0.8144(18) 0.6618(11) 0.2491(11) 0.047(4) Uani 1 1 d . U . . . H3 H 0.8313 0.6057 0.2199 0.010(12) Uiso 1 1 calc R . . . . C4 C 0.6393(15) 0.2610(11) 0.3613(13) 0.029(3) Uani 1 1 d . U . . . O4 O 0.4359(16) 0.6233(12) 0.4985(12) 0.045(3) Uani 1 1 d . U . . . C5 C 0.5791(16) 0.4273(11) 0.4681(12) 0.030(3) Uani 1 1 d . U . . . H5A H 0.5016 0.4178 0.4343 0.036 Uiso 1 1 calc R U . . . H5B H 0.5715 0.4068 0.5387 0.036 Uiso 1 1 calc R U . . . O5 O 0.5520(16) 0.0155(12) 0.2995(13) 0.046(4) Uani 1 1 d . U . . . H5 H 0.5281 0.0737 0.3207 0.08(4) Uiso 1 1 calc R . . . . C8 C 0.5357(17) 0.6304(13) 0.4689(12) 0.033(3) Uani 1 1 d . U . . . C7 C 0.6809(17) 0.5476(11) 0.3510(13) 0.033(3) Uani 1 1 d . U . . . H7 H 0.6164 0.5604 0.3013 0.040 Uiso 1 1 calc R U . . . C6 C 0.6256(16) 0.5381(13) 0.4569(13) 0.034(3) Uani 1 1 d . U . . . H6 H 0.6909 0.5484 0.5063 0.041 Uiso 1 1 calc R U . . . O6 O 0.9479(18) 0.0480(11) 0.0560(13) 0.049(4) Uani 1 1 d . U . . . C9 C 0.5955(19) 0.7324(14) 0.4278(13) 0.043(4) Uani 1 1 d . U . . . H9 H 0.5551 0.7973 0.4375 0.052 Uiso 1 1 calc R U . . . C10 C 0.697(2) 0.7345(15) 0.3811(14) 0.050(4) Uani 1 1 d . U . . . H10 H 0.7283 0.8022 0.3664 0.060 Uiso 1 1 calc R U . . . C11 C 0.7746(19) 0.6391(12) 0.3464(13) 0.038(4) Uani 1 1 d . U . . . H11 H 0.8429 0.6261 0.3924 0.045 Uiso 1 1 calc R U . . . C12 C 0.7255(15) 0.1276(10) 0.2392(11) 0.023(3) Uani 1 1 d . U . . . H12 H 0.6803 0.1437 0.1771 0.028 Uiso 1 1 calc R U . . . C13 C 0.8615(16) 0.1162(11) 0.2116(13) 0.032(3) Uani 1 1 d . U . . . H13 H 0.9054 0.0869 0.2699 0.038 Uiso 1 1 calc R U . . . C14 C 0.9007(16) 0.2280(11) 0.1949(13) 0.034(4) Uani 1 1 d . U . . . H14A H 0.8710 0.2561 0.1310 0.04(2) Uiso 1 1 calc R . . . . H14B H 0.9885 0.2352 0.1977 0.07(3) Uiso 1 1 calc R . . . . C15 C 0.8725(18) 0.0384(12) 0.1235(14) 0.039(4) Uani 1 1 d . U . . . C16 C 0.7930(16) -0.0565(11) 0.1330(12) 0.031(3) Uani 1 1 d . U . . . H16 H 0.8013 -0.1130 0.0875 0.038 Uiso 1 1 calc R U . . . C17 C 0.7094(16) -0.0623(11) 0.2059(12) 0.032(3) Uani 1 1 d . U . . . H17 H 0.6655 -0.1261 0.2094 0.038 Uiso 1 1 calc R U . . . C18 C 0.6782(15) 0.0204(10) 0.2819(12) 0.028(3) Uani 1 1 d . U . . . H18 H 0.7212 0.0045 0.3451 0.034 Uiso 1 1 calc R U . . . 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 0.029(4) 0.013(3) 0.035(4) 0.003(3) -0.001(3) -0.006(3) O1 0.033(6) 0.023(6) 0.062(9) -0.011(6) 0.019(6) -0.007(5) N1 0.039(7) 0.013(4) 0.028(5) -0.003(4) 0.004(5) -0.003(4) C1 0.029(6) 0.013(5) 0.027(5) -0.002(4) -0.003(5) -0.008(4) S2 0.031(4) 0.014(3) 0.038(4) -0.003(3) 0.006(3) -0.006(3) O2 0.067(10) 0.023(6) 0.035(6) -0.002(5) 0.019(7) -0.011(6) N2 0.023(5) 0.010(4) 0.028(5) -0.004(4) -0.003(4) -0.006(4) C2 0.042(8) 0.006(5) 0.034(6) -0.002(4) 0.009(6) -0.008(4) C3 0.030(6) 0.003(4) 0.037(6) -0.004(4) 0.005(5) -0.006(4) O3 0.082(11) 0.019(6) 0.040(7) 0.005(5) 0.007(7) -0.012(7) C4 0.033(6) 0.012(5) 0.042(7) -0.007(5) 0.006(5) -0.006(4) O4 0.045(7) 0.041(7) 0.050(8) -0.015(6) -0.008(6) 0.010(6) C5 0.034(7) 0.030(6) 0.027(7) -0.005(5) 0.001(6) -0.002(5) O5 0.043(7) 0.034(8) 0.061(10) -0.011(7) -0.005(7) -0.013(6) C8 0.045(7) 0.026(6) 0.028(7) -0.008(5) -0.012(6) 0.008(5) C7 0.048(8) 0.014(5) 0.037(7) -0.006(4) -0.002(6) -0.002(5) C6 0.040(7) 0.024(5) 0.040(7) -0.004(5) -0.004(6) 0.000(5) O6 0.072(10) 0.019(6) 0.056(8) -0.014(5) 0.011(7) -0.005(7) C9 0.067(9) 0.025(6) 0.037(9) -0.002(6) -0.010(7) 0.008(6) C10 0.074(9) 0.029(7) 0.046(9) -0.003(6) -0.005(7) -0.001(6) C11 0.056(8) 0.023(6) 0.034(7) 0.003(5) -0.002(6) -0.008(6) C12 0.037(6) 0.010(5) 0.023(6) -0.001(4) -0.011(5) 0.000(4) C13 0.039(7) 0.009(5) 0.047(7) -0.015(5) -0.005(6) -0.006(5) C14 0.043(8) 0.008(5) 0.050(7) -0.010(5) 0.011(6) -0.002(5) C15 0.054(9) 0.013(6) 0.048(8) -0.018(5) -0.003(6) -0.002(6) C16 0.046(8) 0.009(5) 0.039(7) -0.009(5) -0.017(6) 0.005(5) C17 0.042(8) 0.011(6) 0.042(7) -0.002(5) -0.019(6) 0.004(5) C18 0.042(7) 0.011(5) 0.032(7) 0.002(5) -0.013(6) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.864(16) . ? S1 S2 2.096(11) . ? O1 C4 1.26(2) . ? N1 C2 1.39(2) . ? N1 C1 1.409(19) . ? N1 C7 1.504(19) . ? C1 C5 1.53(2) . ? C1 C4 1.554(18) . ? S2 C3 1.876(17) . ? O2 C2 1.22(2) . ? N2 C4 1.33(2) . ? N2 C3 1.422(19) . ? N2 C12 1.468(17) . ? C2 C3 1.529(19) . ? C3 C14 1.54(2) . ? O3 C11 1.39(2) . ? O3 H3 0.8200 . ? O4 C8 1.17(2) . ? C5 C6 1.48(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? O5 C18 1.41(2) . ? O5 H5 0.8200 . ? C8 C6 1.52(2) . ? C8 C9 1.53(2) . ? C7 C6 1.53(2) . ? C7 C11 1.54(2) . ? C7 H7 0.9800 . ? C6 H6 0.9800 . ? O6 C15 1.22(2) . ? C9 C10 1.28(3) . ? C9 H9 0.9300 . ? C10 C11 1.53(2) . ? C10 H10 0.9300 . ? C11 H11 0.9800 . ? C12 C18 1.540(19) . ? C12 C13 1.55(2) . ? C12 H12 0.9800 . ? C13 C14 1.47(2) . ? C13 C15 1.52(2) . ? C13 H13 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.47(2) . ? C16 C17 1.33(2) . ? C16 H16 0.9300 . ? C17 C18 1.48(2) . ? C17 H17 0.9300 . ? C18 H18 0.9800 . ? 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 S1 S2 97.1(6) . . ? C2 N1 C1 122.6(12) . . ? C2 N1 C7 125.0(12) . . ? C1 N1 C7 112.3(12) . . ? N1 C1 C5 106.4(12) . . ? N1 C1 C4 107.5(12) . . ? C5 C1 C4 114.5(12) . . ? N1 C1 S1 112.8(11) . . ? C5 C1 S1 110.6(11) . . ? C4 C1 S1 105.2(10) . . ? C3 S2 S1 98.6(6) . . ? C4 N2 C3 123.1(11) . . ? C4 N2 C12 126.7(12) . . ? C3 N2 C12 110.1(12) . . ? O2 C2 N1 124.7(13) . . ? O2 C2 C3 126.9(14) . . ? N1 C2 C3 108.4(12) . . ? N2 C3 C2 109.9(12) . . ? N2 C3 C14 106.2(11) . . ? C2 C3 C14 113.0(12) . . ? N2 C3 S2 111.3(10) . . ? C2 C3 S2 102.9(10) . . ? C14 C3 S2 113.6(12) . . ? C11 O3 H3 109.5 . . ? O1 C4 N2 128.3(13) . . ? O1 C4 C1 121.7(14) . . ? N2 C4 C1 109.7(12) . . ? C6 C5 C1 99.8(13) . . ? C6 C5 H5A 111.8 . . ? C1 C5 H5A 111.8 . . ? C6 C5 H5B 111.8 . . ? C1 C5 H5B 111.8 . . ? H5A C5 H5B 109.5 . . ? C18 O5 H5 109.5 . . ? O4 C8 C6 126.0(17) . . ? O4 C8 C9 125.8(17) . . ? C6 C8 C9 108.1(15) . . ? N1 C7 C6 98.6(12) . . ? N1 C7 C11 117.2(15) . . ? C6 C7 C11 111.1(13) . . ? N1 C7 H7 109.8 . . ? C6 C7 H7 109.8 . . ? C11 C7 H7 109.8 . . ? C5 C6 C8 118.0(15) . . ? C5 C6 C7 107.5(13) . . ? C8 C6 C7 107.2(14) . . ? C5 C6 H6 107.9 . . ? C8 C6 H6 107.9 . . ? C7 C6 H6 107.9 . . ? C10 C9 C8 124.3(17) . . ? C10 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? C9 C10 C11 128.0(18) . . ? C9 C10 H10 116.0 . . ? C11 C10 H10 116.0 . . ? O3 C11 C10 107.1(14) . . ? O3 C11 C7 113.5(14) . . ? C10 C11 C7 101.0(15) . . ? O3 C11 H11 111.6 . . ? C10 C11 H11 111.6 . . ? C7 C11 H11 111.6 . . ? N2 C12 C18 121.0(12) . . ? N2 C12 C13 101.0(11) . . ? C18 C12 C13 109.5(12) . . ? N2 C12 H12 108.2 . . ? C18 C12 H12 108.2 . . ? C13 C12 H12 108.2 . . ? C14 C13 C15 117.6(15) . . ? C14 C13 C12 103.4(13) . . ? C15 C13 C12 108.4(13) . . ? C14 C13 H13 109.0 . . ? C15 C13 H13 109.0 . . ? C12 C13 H13 109.0 . . ? C13 C14 C3 99.5(12) . . ? C13 C14 H14A 111.9 . . ? C3 C14 H14A 111.9 . . ? C13 C14 H14B 111.9 . . ? C3 C14 H14B 111.9 . . ? H14A C14 H14B 109.6 . . ? O6 C15 C16 122.8(14) . . ? O6 C15 C13 123.4(15) . . ? C16 C15 C13 113.5(15) . . ? C17 C16 C15 120.9(13) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 127.8(14) . . ? C16 C17 H17 116.1 . . ? C18 C17 H17 116.1 . . ? O5 C18 C17 108.1(14) . . ? O5 C18 C12 115.6(13) . . ? C17 C18 C12 106.0(13) . . ? O5 C18 H18 109.0 . . ? C17 C18 H18 109.0 . . ? C12 C18 H18 109.0 . . ? _refine_diff_density_max 0.201 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.059 _shelx_res_file ; N15_a.res created by SHELXL-2014/7 TITL N15_a.res in P2(1)2(1)2(1) REM Old TITL N15 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.245, Rweak 0.225, Alpha 0.039, Orientation as input REM Flack x = -0.461 ( 0.174 ) from Parsons' quotients REM Formula found by SHELXT: C20 N2 O4 S2 CELL 0.02508 10.9956 12.4519 13.2180 90.000 90.000 90.000 ZERR 22.000 0.0021 0.0024 0.0026 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C 0.208 0.922 0.702 5.018 1.144 16.523 0.425 47.300 0.030 = 0.0 0.0 11.500 0.770 12.010 SFAC H 0.042 0.991 0.103 3.924 0.205 11.597 0.170 31.984 0.006 = 0.0 0.0 0.620 0.310 1.000 SFAC N 0.216 0.843 0.649 4.055 0.968 12.693 0.345 36.058 0.032 = 0.0 0.0 11.700 0.700 14.010 SFAC O 0.237 0.799 0.649 3.654 0.800 10.924 0.261 29.964 0.035 = 0.0 0.0 18.200 0.660 16.000 SFAC S 0.499 0.835 1.156 4.857 2.422 16.388 1.010 45.850 0.072 = 0.0 0.0 12.000 1.030 32.060 UNIT 72 64 8 24 8 L.S. 10 BOND $H RIGU XNPD 0.001 ACTA LIST 6 FMAP 2 PLAN 20 WGHT 0.185400 0.967000 FVAR 2.06476 S1 5 0.798387 0.321881 0.508120 11.00000 0.02875 0.01264 = 0.03478 0.00345 -0.00086 -0.00551 O1 4 0.540048 0.215828 0.383062 11.00000 0.03308 0.02256 = 0.06238 -0.01127 0.01897 -0.00665 N1 3 0.728040 0.434828 0.340456 11.00000 0.03900 0.01279 = 0.02792 -0.00350 0.00372 -0.00277 C1 1 0.681011 0.365635 0.415131 11.00000 0.02852 0.01328 = 0.02718 -0.00211 -0.00314 -0.00843 S2 5 0.934430 0.283783 0.403014 11.00000 0.03141 0.01380 = 0.03779 -0.00280 0.00571 -0.00603 O2 4 0.853672 0.458139 0.201403 11.00000 0.06654 0.02280 = 0.03539 -0.00239 0.01905 -0.01056 N2 3 0.728022 0.225041 0.301732 11.00000 0.02337 0.00999 = 0.02845 -0.00393 -0.00265 -0.00622 C2 1 0.811596 0.400991 0.268054 11.00000 0.04152 0.00604 = 0.03450 -0.00239 0.00889 -0.00821 C3 1 0.838470 0.281945 0.285661 11.00000 0.02991 0.00262 = 0.03693 -0.00441 0.00488 -0.00613 O3 4 0.814358 0.661823 0.249065 11.00000 0.08164 0.01891 = 0.03991 0.00453 0.00657 -0.01209 AFIX 147 H3 2 0.831338 0.605655 0.219923 11.00000 0.00957 AFIX 0 C4 1 0.639271 0.261018 0.361269 11.00000 0.03317 0.01158 = 0.04155 -0.00730 0.00619 -0.00613 O4 4 0.435856 0.623309 0.498510 11.00000 0.04527 0.04118 = 0.04964 -0.01466 -0.00797 0.01014 C5 1 0.579097 0.427316 0.468130 11.00000 0.03385 0.02959 = 0.02703 -0.00543 0.00126 -0.00194 AFIX 23 H5A 2 0.501550 0.417765 0.434321 11.00000 -1.20000 H5B 2 0.571475 0.406842 0.538650 11.00000 -1.20000 AFIX 0 O5 4 0.552035 0.015471 0.299523 11.00000 0.04325 0.03380 = 0.06069 -0.01122 -0.00515 -0.01342 AFIX 147 H5 2 0.528129 0.073665 0.320681 11.00000 0.07836 AFIX 0 C8 1 0.535704 0.630388 0.468894 11.00000 0.04508 0.02575 = 0.02811 -0.00798 -0.01169 0.00843 C7 1 0.680892 0.547641 0.351042 11.00000 0.04806 0.01378 = 0.03727 -0.00637 -0.00233 -0.00219 AFIX 13 H7 2 0.616411 0.560398 0.301289 11.00000 -1.20000 AFIX 0 C6 1 0.625555 0.538143 0.456880 11.00000 0.03973 0.02393 = 0.03972 -0.00444 -0.00422 0.00049 AFIX 13 H6 2 0.690940 0.548403 0.506328 11.00000 -1.20000 AFIX 0 O6 4 0.947923 0.048033 0.055978 11.00000 0.07220 0.01892 = 0.05588 -0.01373 0.01094 -0.00484 C9 1 0.595513 0.732430 0.427846 11.00000 0.06709 0.02480 = 0.03750 -0.00232 -0.01011 0.00838 AFIX 43 H9 2 0.555141 0.797255 0.437503 11.00000 -1.20000 AFIX 0 C10 1 0.697373 0.734471 0.381123 11.00000 0.07433 0.02881 = 0.04624 -0.00320 -0.00486 -0.00094 AFIX 43 H10 2 0.728275 0.802225 0.366436 11.00000 -1.20000 AFIX 0 C11 1 0.774611 0.639100 0.346436 11.00000 0.05598 0.02329 = 0.03410 0.00296 -0.00226 -0.00772 AFIX 13 H11 2 0.842946 0.626137 0.392440 11.00000 -1.20000 AFIX 0 C12 1 0.725509 0.127615 0.239169 11.00000 0.03709 0.01012 = 0.02284 -0.00114 -0.01123 -0.00037 AFIX 13 H12 2 0.680270 0.143656 0.177102 11.00000 -1.20000 AFIX 0 C13 1 0.861489 0.116217 0.211628 11.00000 0.03945 0.00928 = 0.04721 -0.01509 -0.00454 -0.00566 AFIX 13 H13 2 0.905413 0.086898 0.269929 11.00000 -1.20000 AFIX 0 C14 1 0.900695 0.228040 0.194882 11.00000 0.04290 0.00800 = 0.05022 -0.01042 0.01079 -0.00204 AFIX 23 H14A 2 0.871018 0.256103 0.131031 11.00000 0.04488 H14B 2 0.988466 0.235249 0.197730 11.00000 0.06702 AFIX 0 C15 1 0.872502 0.038411 0.123533 11.00000 0.05408 0.01334 = 0.04845 -0.01792 -0.00273 -0.00201 C16 1 0.793018 -0.056476 0.133025 11.00000 0.04594 0.00889 = 0.03907 -0.00917 -0.01723 0.00453 AFIX 43 H16 2 0.801295 -0.112989 0.087542 11.00000 -1.20000 AFIX 0 C17 1 0.709444 -0.062341 0.205935 11.00000 0.04171 0.01068 = 0.04218 -0.00176 -0.01871 0.00364 AFIX 43 H17 2 0.665539 -0.126069 0.209431 11.00000 -1.20000 AFIX 0 C18 1 0.678235 0.020440 0.281931 11.00000 0.04155 0.01107 = 0.03180 0.00219 -0.01276 -0.00077 AFIX 13 H18 2 0.721222 0.004497 0.345118 11.00000 -1.20000 AFIX 0 HKLF 4 REM N15_a.res in P2(1)2(1)2(1) REM R1 = 0.1543 for 2342 Fo > 4sig(Fo) and 0.1721 for all 2998 data REM 259 parameters refined using 267 restraints END WGHT 0.1850 0.9470 REM Highest difference peak 0.201, deepest hole -0.215, 1-sigma level 0.059 Q1 1 0.7694 0.3364 0.3951 11.00000 0.05 0.20 Q2 1 0.9476 0.0513 0.2945 11.00000 0.05 0.19 Q3 1 0.8123 0.3231 0.4261 11.00000 0.05 0.18 Q4 1 0.9941 0.3370 0.2641 11.00000 0.05 0.18 Q5 1 0.5895 0.5371 0.5604 11.00000 0.05 0.17 Q6 1 0.5243 0.7912 0.3096 11.00000 0.05 0.16 Q7 1 0.5198 0.8320 0.3404 11.00000 0.05 0.16 Q8 1 1.0533 0.2375 0.2042 11.00000 0.05 0.16 Q9 1 0.8750 0.5903 0.1318 11.00000 0.05 0.16 Q10 1 0.6351 0.3466 0.5882 11.00000 0.05 0.16 Q11 1 0.5886 0.2880 0.6120 11.00000 0.05 0.16 Q12 1 0.7264 0.5805 0.1603 11.00000 0.05 0.15 Q13 1 1.0696 0.3994 0.1762 11.00000 0.05 0.15 Q14 1 0.7192 0.2896 0.4970 11.00000 0.05 0.15 Q15 1 0.7108 0.3560 0.5135 11.00000 0.05 0.14 Q16 1 1.0657 0.3236 0.1848 11.00000 0.05 0.14 Q17 1 0.4180 0.6230 0.6443 11.00000 0.05 0.14 Q18 1 0.5089 0.3867 0.6126 11.00000 0.05 0.14 Q19 1 0.8365 0.2811 0.0661 11.00000 0.05 0.14 Q20 1 0.8315 -0.2036 0.0115 11.00000 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5 -1 17.22 22.82 -11 -5 -1 16.29 21.02 11 5 1 23.49 29.38 11 5 1 16.95 26.14 -11 -5 1 29.53 24.20 -11 -5 1 12.30 21.37 11 -5 -1 20.75 21.07 -11 5 -1 11.06 20.82 11 -5 2 31.68 21.04 -11 5 2 34.16 23.59 11 5 -2 32.13 25.79 11 5 2 6.07 23.27 -11 -5 2 41.68 26.45 -11 -5 2 -2.52 22.42 11 -5 -2 23.03 22.52 -11 5 -2 16.93 23.44 11 -5 3 23.23 20.09 -11 -5 3 13.15 21.50 11 -5 -3 2.41 20.92 -11 -5 4 22.93 24.21 -11 -6 0 -2.24 20.55 -11 -6 -1 -3.46 21.24 -11 -6 1 7.43 21.40 -11 -6 -2 28.12 23.56 -11 -6 2 18.75 25.52 11 -7 -3 34.48 17.01 12 0 0 67.50 30.75 12 0 1 0.61 19.51 12 0 -1 -1.45 21.80 12 1 0 15.18 20.97 12 -1 0 31.24 23.71 12 -1 1 6.84 29.78 12 1 -1 35.97 26.09 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 76317