data_shelxl _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H22 F N O2 S' _chemical_formula_sum 'C15 H22 F N O2 S' _chemical_formula_weight 299.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.2800(8) _cell_length_b 19.188(2) _cell_length_c 12.9030(15) _cell_angle_alpha 90 _cell_angle_beta 96.840(5) _cell_angle_gamma 90 _cell_volume 1543.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5950 _cell_measurement_theta_min 1.10 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.288 _exptl_crystal_F_000 640 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 0.221 _shelx_estimated_absorpt_T_min 0.957 _shelx_estimated_absorpt_T_max 0.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_reflns_number 15988 _diffrn_reflns_av_unetI/netI 0.0476 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.911 _diffrn_reflns_theta_max 30.031 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 4406 _reflns_number_gt 3132 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _refine_special_details ; ENTER TEXT OF LETTER ; _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^)+(0.0547P)^2^+0.0351P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4406 _refine_ls_number_parameters 201 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.41115(6) 0.76354(2) 0.33723(3) 0.02004(11) Uani 1 1 d . . . . . F1 F 0.30269(17) 0.86196(6) 0.57822(10) 0.0398(4) Uani 0.880(3) 1 d D . P A 1 C2 C 0.0991(5) 0.75761(13) 0.55837(19) 0.0279(4) Uani 0.880(3) 1 d D . P A 1 H2A H -0.0078 0.7941 0.5358 0.033 Uiso 0.880(3) 1 calc R U P A 1 H2B H 0.0428 0.7291 0.6129 0.033 Uiso 0.880(3) 1 calc R U P A 1 C3 C 0.3091(4) 0.79094(11) 0.60170(18) 0.0230(5) Uani 0.880(3) 1 d D . P A 1 H3 H 0.3391 0.7832 0.6787 0.028 Uiso 0.880(3) 1 calc R U P A 1 O1 O 0.63983(16) 0.76147(6) 0.33645(8) 0.0266(3) Uani 1 1 d . . . . . O2 O 0.27360(17) 0.72977(5) 0.25594(8) 0.0248(2) Uani 1 1 d . . . . . N1 N 0.36325(18) 0.72835(6) 0.44708(9) 0.0188(3) Uani 1 1 d . . . . . C1 C 0.1373(2) 0.71132(7) 0.46482(11) 0.0191(3) Uani 1 1 d D . . . . H1A H 0.0427 0.7263 0.4050 0.023 Uiso 0.880(3) 1 d R U P A 1 H1B H 0.0459 0.7248 0.4031 0.023 Uiso 0.120(3) 1 d R U P A 2 C4 C 0.4784(2) 0.75662(8) 0.54480(11) 0.0234(3) Uani 1 1 d D . . . . H4A H 0.5479 0.7198 0.5864 0.028 Uiso 0.880(3) 1 d R U P A 1 H4B H 0.5847 0.7899 0.5297 0.028 Uiso 0.880(3) 1 d R U P A 1 C5 C 0.1047(2) 0.63220(8) 0.48075(12) 0.0233(3) Uani 1 1 d . . . . . C6 C 0.1476(3) 0.59333(9) 0.38168(14) 0.0379(4) Uani 1 1 d . . . . . H6A H 0.0488 0.6101 0.3224 0.045 Uiso 1 1 calc R U . . . H6B H 0.1257 0.5433 0.3910 0.045 Uiso 1 1 calc R U . . . H6C H 0.2957 0.6017 0.3682 0.045 Uiso 1 1 calc R U . . . C7 C -0.1292(2) 0.61990(9) 0.49890(14) 0.0320(4) Uani 1 1 d . . . . . H7A H -0.1581 0.5697 0.4992 0.038 Uiso 1 1 calc R U . . . H7B H -0.2246 0.6421 0.4429 0.038 Uiso 1 1 calc R U . . . H7C H -0.1543 0.6400 0.5662 0.038 Uiso 1 1 calc R U . . . C8 C 0.2536(3) 0.60352(9) 0.57353(14) 0.0355(4) Uani 1 1 d . . . . . H8A H 0.2183 0.5546 0.5848 0.043 Uiso 1 1 calc R U . . . H8B H 0.2349 0.6306 0.6362 0.043 Uiso 1 1 calc R U . . . H8C H 0.4028 0.6071 0.5589 0.043 Uiso 1 1 calc R U . . . C9 C 0.3375(2) 0.85227(8) 0.33790(11) 0.0212(3) Uani 1 1 d . . . . . C10 C 0.1228(2) 0.87110(8) 0.31558(12) 0.0250(3) Uani 1 1 d . . . . . H10 H 0.0166 0.8368 0.2959 0.030 Uiso 1 1 calc R U . . . C11 C 0.0663(2) 0.94046(8) 0.32249(13) 0.0275(4) Uani 1 1 d . . . . . H11 H -0.0799 0.9535 0.3067 0.033 Uiso 1 1 calc R U . . . C12 C 0.2193(3) 0.99192(8) 0.35214(13) 0.0281(4) Uani 1 1 d . . . . . C13 C 0.4336(3) 0.97188(9) 0.37150(13) 0.0306(4) Uani 1 1 d . . . . . H13 H 0.5407 1.0062 0.3894 0.037 Uiso 1 1 calc R U . . . C14 C 0.4927(2) 0.90266(8) 0.36499(12) 0.0263(3) Uani 1 1 d . . . . . H14 H 0.6392 0.8897 0.3791 0.032 Uiso 1 1 calc R U . . . C15 C 0.1518(3) 1.06610(9) 0.36549(15) 0.0390(4) Uani 1 1 d . . . . . H15A H 0.2732 1.0972 0.3587 0.047 Uiso 1 1 calc R U . . . H15B H 0.1048 1.0720 0.4347 0.047 Uiso 1 1 calc R U . . . H15C H 0.0333 1.0776 0.3117 0.047 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 0.0187(2) 0.02601(19) 0.01592(18) -0.00002(14) 0.00424(14) 0.00059(14) F1 0.0373(7) 0.0256(6) 0.0594(9) -0.0038(5) 0.0178(6) -0.0026(5) C2 0.0221(10) 0.0325(8) 0.0309(9) -0.0075(7) 0.0106(7) -0.0029(7) C3 0.0262(8) 0.0235(14) 0.0198(9) -0.0013(7) 0.0047(7) -0.0004(8) O1 0.0194(5) 0.0370(6) 0.0245(6) 0.0029(5) 0.0070(4) 0.0029(5) O2 0.0283(6) 0.0299(6) 0.0155(5) -0.0030(4) 0.0004(4) -0.0007(5) N1 0.0153(6) 0.0266(6) 0.0144(6) -0.0004(5) 0.0013(5) -0.0005(5) C1 0.0159(7) 0.0230(7) 0.0182(7) -0.0002(6) 0.0017(5) 0.0007(6) C4 0.0186(7) 0.0345(8) 0.0164(7) -0.0022(6) -0.0005(6) -0.0018(6) C5 0.0236(8) 0.0225(7) 0.0240(8) 0.0031(6) 0.0037(6) -0.0004(6) C6 0.0521(11) 0.0250(8) 0.0376(10) -0.0048(8) 0.0099(9) -0.0037(8) C7 0.0281(9) 0.0276(8) 0.0402(10) 0.0046(8) 0.0037(7) -0.0050(7) C8 0.0311(9) 0.0349(9) 0.0396(10) 0.0153(8) 0.0001(8) -0.0004(7) C9 0.0211(7) 0.0257(7) 0.0171(7) 0.0020(6) 0.0039(6) -0.0010(6) C10 0.0218(8) 0.0262(8) 0.0270(8) 0.0010(7) 0.0026(6) -0.0028(6) C11 0.0225(8) 0.0289(8) 0.0318(9) 0.0036(7) 0.0062(7) 0.0020(6) C12 0.0344(9) 0.0248(8) 0.0267(8) 0.0034(7) 0.0108(7) -0.0017(7) C13 0.0295(9) 0.0294(8) 0.0338(9) -0.0003(7) 0.0071(7) -0.0102(7) C14 0.0208(8) 0.0305(8) 0.0281(8) 0.0026(7) 0.0054(6) -0.0047(6) C15 0.0470(11) 0.0286(9) 0.0436(11) -0.0005(8) 0.0147(9) -0.0011(8) _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 1.4320(11) . ? S1 O1 1.4380(11) . ? S1 N1 1.6300(12) . ? S1 C9 1.7647(15) . ? F1 C3 1.396(2) . ? C2 C3 1.512(3) . ? C2 C1 1.540(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.513(3) . ? C3 H3 1.0000 . ? N1 C4 1.4799(17) . ? N1 C1 1.5001(17) . ? C1 C5 1.5488(19) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C5 C8 1.531(2) . ? C5 C6 1.531(2) . ? C5 C7 1.533(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.388(2) . ? C9 C10 1.392(2) . ? C10 C11 1.383(2) . ? C10 H10 0.9500 . ? C11 C12 1.399(2) . ? C11 H11 0.9500 . ? C12 C13 1.393(2) . ? C12 C15 1.501(2) . ? C13 C14 1.384(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 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 O2 S1 O1 119.88(7) . . ? O2 S1 N1 106.96(6) . . ? O1 S1 N1 106.41(6) . . ? O2 S1 C9 107.73(7) . . ? O1 S1 C9 106.82(7) . . ? N1 S1 C9 108.65(7) . . ? C3 C2 C1 108.9(2) . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? F1 C3 C2 109.36(18) . . ? F1 C3 C4 108.87(15) . . ? C2 C3 C4 105.6(2) . . ? F1 C3 H3 110.9 . . ? C2 C3 H3 110.9 . . ? C4 C3 H3 110.9 . . ? C4 N1 C1 108.97(11) . . ? C4 N1 S1 117.83(10) . . ? C1 N1 S1 119.92(9) . . ? N1 C1 C2 103.44(15) . . ? N1 C1 C5 112.08(11) . . ? C2 C1 C5 115.21(16) . . ? C2' C1 C5 114.9(7) . . ? N1 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? C5 C1 H1A 108.7 . . ? N1 C1 H1B 107.3 . . ? C2' C1 H1B 107.8 . . ? C5 C1 H1B 107.4 . . ? N1 C4 C3 105.81(14) . . ? N1 C4 H4A 110.5 . . ? C3 C4 H4A 110.3 . . ? N1 C4 H4B 110.6 . . ? C3 C4 H4B 110.8 . . ? H4A C4 H4B 108.8 . . ? C8 C5 C6 109.04(14) . . ? C8 C5 C7 109.40(13) . . ? C6 C5 C7 108.62(13) . . ? C8 C5 C1 112.23(12) . . ? C6 C5 C1 109.12(12) . . ? C7 C5 C1 108.37(12) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 120.34(14) . . ? C14 C9 S1 119.78(12) . . ? C10 C9 S1 119.82(11) . . ? C11 C10 C9 119.06(14) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 121.59(15) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C13 C12 C11 118.12(15) . . ? C13 C12 C15 121.41(15) . . ? C11 C12 C15 120.44(15) . . ? C14 C13 C12 120.94(15) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C9 119.90(15) . . ? C13 C14 H14 120.1 . . ? C9 C14 H14 120.1 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 C1 C2 C3 F1 108.88(19) . . . . ? C1 C2 C3 C4 -8.1(2) . . . . ? O2 S1 N1 C4 -177.11(10) . . . . ? O1 S1 N1 C4 53.63(12) . . . . ? C9 S1 N1 C4 -61.07(12) . . . . ? O2 S1 N1 C1 -40.39(12) . . . . ? O1 S1 N1 C1 -169.65(10) . . . . ? C9 S1 N1 C1 75.65(11) . . . . ? C4 N1 C1 C2 22.67(17) . . . . ? S1 N1 C1 C2 -117.46(14) . . . . ? C4 N1 C1 C5 -102.04(13) . . . . ? S1 N1 C1 C5 117.83(12) . . . . ? C3 C2 C1 N1 -8.5(2) . . . . ? C3 C2 C1 C5 114.2(2) . . . . ? C1 N1 C4 C3 -28.43(16) . . . . ? S1 N1 C4 C3 112.64(13) . . . . ? F1 C3 C4 N1 -95.44(18) . . . . ? C2 C3 C4 N1 21.9(2) . . . . ? N1 C1 C5 C8 58.74(16) . . . . ? C2 C1 C5 C8 -59.2(2) . . . . ? N1 C1 C5 C6 -62.23(16) . . . . ? C2 C1 C5 C6 179.85(17) . . . . ? N1 C1 C5 C7 179.65(12) . . . . ? C2 C1 C5 C7 61.74(19) . . . . ? O2 S1 C9 C14 -146.94(12) . . . . ? O1 S1 C9 C14 -16.92(14) . . . . ? N1 S1 C9 C14 97.51(13) . . . . ? O2 S1 C9 C10 35.79(14) . . . . ? O1 S1 C9 C10 165.81(12) . . . . ? N1 S1 C9 C10 -79.76(13) . . . . ? C14 C9 C10 C11 -1.1(2) . . . . ? S1 C9 C10 C11 176.20(12) . . . . ? C9 C10 C11 C12 -0.5(2) . . . . ? C10 C11 C12 C13 2.1(2) . . . . ? C10 C11 C12 C15 -176.15(16) . . . . ? C11 C12 C13 C14 -2.1(2) . . . . ? C15 C12 C13 C14 176.11(15) . . . . ? C12 C13 C14 C9 0.6(2) . . . . ? C10 C9 C14 C13 1.0(2) . . . . ? S1 C9 C14 C13 -176.24(12) . . . . ? 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 C3 H3 O1 1.00 2.66 3.476(2) 139.4 4_576 C4 H4C O2 0.96 2.64 3.1182(18) 111.3 4_676 _refine_diff_density_max 0.338 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.056 _shelxl_version_number 2013-2 _shelx_res_file ; TITL _m130513b CELL 0.71075 6.28000 19.18800 12.90300 90.000 96.840 90.000 ZERR 4 0.00080 0.00200 0.00150 0.000 0.005 0.000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC C H N O F S UNIT 60 88 4 8 4 4 L.S. 5 ACTA FMAP 2 PLAN -5 bond $h conf sadi .01 f1 c4 f1 c2 f1' c3' f1' c1 sadi .01 f1 c3 f1' c2' dfix 1.54 .01 c1 c2 c1 c2' c2 c3 c2' c3' c3 c4 c3' c4 SIZE 0.200 0.200 0.200 eadp c3 c3' eadp c2 c2' HTAB EQIV $1 x-1/2, -y+3/2, z+1/2 HTAB C3 O1_$1 HTAB C2' O2_$1 HTAB C3' O1_$1 EQIV $2 x+1/2, -y+3/2, z+1/2 HTAB C4 O2_$2 WPDB -2 SHEL 99999.000000 0.000000 TEMP -160.0 WGHT 0.054700 0.035100 FVAR 2.05948 0.87976 S1 6 0.411146 0.763542 0.337235 11.00000 0.01870 0.02601 = 0.01592 -0.00002 0.00424 0.00059 PART 1 F1 5 0.302688 0.861956 0.578221 21.00000 0.03725 0.02560 = 0.05940 -0.00380 0.01781 -0.00259 C2 1 0.099090 0.757607 0.558369 21.00000 0.02212 0.03246 = 0.03089 -0.00754 0.01062 -0.00293 AFIX 23 H2A 2 -0.007799 0.794127 0.535757 21.00000 -1.20000 H2B 2 0.042810 0.729065 0.612948 21.00000 -1.20000 AFIX 0 C3 1 0.309084 0.790938 0.601702 21.00000 0.02621 0.02346 = 0.01980 -0.00133 0.00474 -0.00042 AFIX 13 H3 2 0.339069 0.783215 0.678704 21.00000 -1.20000 PART 2 AFIX 0 AFIX 13 AFIX 0 AFIX 23 PART 0 AFIX 0 O1 4 0.639835 0.761471 0.336451 11.00000 0.01938 0.03700 = 0.02446 0.00294 0.00696 0.00286 O2 4 0.273596 0.729767 0.255936 11.00000 0.02832 0.02990 = 0.01554 -0.00297 0.00040 -0.00066 N1 3 0.363248 0.728347 0.447081 11.00000 0.01534 0.02659 = 0.01442 -0.00044 0.00130 -0.00054 C1 1 0.137275 0.711320 0.464819 11.00000 0.01595 0.02304 = 0.01821 -0.00024 0.00174 0.00073 PART 1 AFIX 3 H1A 2 0.042675 0.726250 0.404999 21.00000 -1.20000 PART 2 H1B 2 0.045885 0.724840 0.403119 -21.00000 -1.20000 PART 0 AFIX 0 C4 1 0.478422 0.756618 0.544799 11.00000 0.01863 0.03451 = 0.01640 -0.00223 -0.00048 -0.00184 PART 1 AFIX 3 H4A 2 0.547903 0.719828 0.586438 21.00000 -1.20000 H4B 2 0.584672 0.789878 0.529668 21.00000 -1.20000 PART 0 AFIX 0 C5 1 0.104743 0.632200 0.480751 11.00000 0.02360 0.02246 = 0.02404 0.00307 0.00367 -0.00039 C6 1 0.147588 0.593335 0.381678 11.00000 0.05206 0.02500 = 0.03760 -0.00479 0.00990 -0.00374 AFIX 137 H6A 2 0.048799 0.610131 0.322420 11.00000 -1.20000 H6B 2 0.125662 0.543268 0.391036 11.00000 -1.20000 H6C 2 0.295725 0.601730 0.368171 11.00000 -1.20000 AFIX 0 C7 1 -0.129157 0.619898 0.498899 11.00000 0.02813 0.02760 = 0.04024 0.00460 0.00365 -0.00496 AFIX 137 H7A 2 -0.158071 0.569715 0.499219 11.00000 -1.20000 H7B 2 -0.224601 0.642124 0.442879 11.00000 -1.20000 H7C 2 -0.154322 0.639993 0.566199 11.00000 -1.20000 AFIX 0 C8 1 0.253570 0.603521 0.573532 11.00000 0.03111 0.03492 = 0.03961 0.01530 0.00013 -0.00041 AFIX 137 H8A 2 0.218339 0.554562 0.584831 11.00000 -1.20000 H8B 2 0.234865 0.630563 0.636242 11.00000 -1.20000 H8C 2 0.402789 0.607076 0.558924 11.00000 -1.20000 AFIX 0 C9 1 0.337454 0.852275 0.337898 11.00000 0.02110 0.02571 = 0.01707 0.00197 0.00394 -0.00097 C10 1 0.122802 0.871097 0.315584 11.00000 0.02178 0.02620 = 0.02696 0.00100 0.00260 -0.00277 AFIX 43 H10 2 0.016618 0.836778 0.295890 11.00000 -1.20000 AFIX 0 C11 1 0.066320 0.940458 0.322489 11.00000 0.02253 0.02889 = 0.03178 0.00364 0.00624 0.00204 AFIX 43 H11 2 -0.079905 0.953471 0.306716 11.00000 -1.20000 AFIX 0 C12 1 0.219316 0.991923 0.352140 11.00000 0.03435 0.02480 = 0.02675 0.00338 0.01083 -0.00172 C13 1 0.433578 0.971878 0.371498 11.00000 0.02947 0.02940 = 0.03377 -0.00025 0.00709 -0.01022 AFIX 43 H13 2 0.540671 1.006202 0.389419 11.00000 -1.20000 AFIX 0 C14 1 0.492650 0.902656 0.364991 11.00000 0.02080 0.03052 = 0.02812 0.00262 0.00540 -0.00466 AFIX 43 H14 2 0.639217 0.889663 0.379052 11.00000 -1.20000 AFIX 0 C15 1 0.151812 1.066104 0.365487 11.00000 0.04695 0.02859 = 0.04358 -0.00051 0.01474 -0.00108 AFIX 137 H15A 2 0.273248 1.097175 0.358747 11.00000 -1.20000 H15B 2 0.104762 1.071965 0.434702 11.00000 -1.20000 H15C 2 0.033350 1.077607 0.311728 11.00000 -1.20000 AFIX 0 HKLF 4 REM _m130513b REM R1 = 0.0421 for 3132 Fo > 4sig(Fo) and 0.0638 for all 4406 data REM 201 parameters refined using 13 restraints END WGHT 0.0547 0.0363 REM Instructions for potential hydrogen bonds HTAB C3 O1_$1 HTAB C4 O2_$2 REM Highest difference peak 0.338, deepest hole -0.380, 1-sigma level 0.056 Q1 1 0.3982 0.7713 0.5780 11.00000 0.05 0.34 Q2 1 0.3097 0.8570 0.6418 11.00000 0.05 0.30 Q3 1 0.3635 0.8212 0.3400 11.00000 0.05 0.29 Q4 1 0.4264 0.7277 0.4807 11.00000 0.05 0.26 Q5 1 0.1247 0.6696 0.4761 11.00000 0.05 0.26 ; _shelx_res_checksum 70066 _shelx_hkl_file ; 0 1 0 3.45 3.75 0 0 -1 2.16 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89.96 1 1 0 8956.61 83.77 1 1 0 8608.87 85.45 -1 1 0 8625.10 86.69 -1 0 141312.97 237.75 -1 0 140443.61 257.20 1 0 -142309.51 267.00 -1 0 141719.42 291.65 1 0 -139191.50 245.43 1 0 -140554.48 228.24 0 3 1 2072.21 72.94 0 -3 -1 3327.44 52.66 0 3 1 3078.75 51.23 0 -3 -1 3133.28 39.34 0 -3 -1 3082.67 51.65 0 3 -1 3191.97 52.01 0 3 1 3121.04 39.99 0 -3 1 3255.87 55.24 -1 -1 113192.25 117.18 -1 1 113431.85 114.73 1 1 -113391.32 123.06 1 -1 -113636.77 118.34 1 -1 -113608.35 120.10 1 1 -113230.77 108.20 -1 1 113476.64 124.56 -1 -1 114266.01 114.11 -1 0 -122718.68 170.62 1 0 122306.13 133.18 -1 0 -121407.44 149.94 1 0 122930.96 174.26 1 0 122018.19 155.37 0 -2 -2 2374.00 83.70 0 -2 2 2294.73 85.64 0 2 -2 1565.69 57.95 0 2 2 2460.42 87.41 0 -2 2 2339.61 82.63 0 2 -2 2154.50 73.11 0 2 2 2479.57 87.99 0 -2 -2 2535.35 89.55 -1 2 0 127.54 10.11 1 -2 0 127.50 10.70 -1 2 0 112.68 15.27 -1 -2 0 121.57 15.60 1 2 0 129.81 42.87 1 -2 0 125.03 15.09 1 -2 0 132.88 12.71 1 2 0 123.74 17.57 -1 2 0 127.88 14.08 1 2 0 126.47 19.89 -1 1 -193832.95 546.95 -1 1 -197070.84 541.25 1 1 199764.20 3015.28 1 -1 198251.40 2967.22 1 1 197630.05 2952.87 1 -2 -1 6048.83 81.10 -1 -2 1 5793.98 79.79 -1 2 1 6104.94 72.77 1 -2 -1 6214.51 78.25 -1 -2 1 5849.92 74.43 1 2 -1 5889.21 80.29 1 2 -1 5639.37 69.95 -1 2 1 4124.01 69.15 0 4 015250.98 121.38 0 4 015664.05 136.62 0 4 015851.64 138.00 0 -4 015434.49 139.01 -1 0 2 15.91 9.11 1 0 -2 11.11 10.81 1 0 -2 7.16 14.79 -1 0 2 16.50 9.48 -1 -2 -111280.81 76.46 1 2 110932.71 72.37 -1 2 -111485.54 104.31 -1 2 -111563.94 76.88 1 -2 111847.60 105.79 1 -2 111344.60 74.67 1 2 111766.51 124.04 -1 2 -111706.57 114.43 -1 -2 -111827.49 129.97 -1 -1 224672.08 172.49 1 1 -225859.01 200.30 -1 1 224153.19 194.07 1 -1 -225521.31 152.63 -1 1 224607.95 148.03 1 -1 -224760.97 197.62 -1 -1 224685.25 197.33 1 -1 -224807.76 193.36 1 1 -225269.86 173.08 0 -3 -2 741.02 36.08 0 3 2 742.12 38.65 0 -3 -2 721.27 37.61 0 -3 2 799.29 47.27 0 3 -2 781.96 37.59 0 3 2 748.23 42.13 0 3 -2 771.74 38.46 0 -3 -2 702.99 29.89 0 -3 2 786.30 38.56 0 4 1 1518.77 59.37 0 4 -1 1592.17 77.28 0 4 1 1519.38 53.06 0 -4 -1 1384.49 54.96 0 -4 -1 1528.38 52.94 0 -4 1 1653.20 65.20 0 -4 -1 1566.96 61.03 0 4 1 1496.08 57.79 1 3 010292.97 110.21 1 -3 011343.54 138.49 1 -3 010684.76 87.12 -1 -3 010548.17 117.40 -1 3 0 9841.81 107.71 -1 3 010429.52 85.15 1 -3 010292.44 91.02 -1 3 010421.00 95.73 -1 3 1 7169.03 56.68 1 -3 -1 7344.38 84.42 -1 3 1 7545.75 94.33 -1 3 1 7547.55 88.44 1 3 -1 7263.57 94.57 1 -3 -1 7455.91 62.37 1 -3 -1 7484.12 92.16 1 3 -1 7125.98 90.35 -1 -3 1 7511.13 95.18 0 0 -3 14.76 13.00 0 0 -3 10.73 12.03 0 0 3 24.22 11.47 0 0 3 13.10 10.98 1 -2 -210800.72 76.25 -1 2 210272.26 71.78 1 -2 -210593.86 113.73 -1 -2 210590.69 123.43 -1 2 210571.74 115.24 1 2 -210339.74 113.08 1 2 -2 9899.59 113.04 1 -2 -210197.93 122.97 -1 2 210831.39 120.03 -1 -2 210591.11 108.05 1 0 2 14.39 12.88 -1 0 -2 3.30 18.78 1 0 2 8.80 4.03 -1 0 -2 2.77 4.82 0 -1 370625.61 467.00 0 1 -370501.50 443.74 0 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