data_cpd1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; gene113 ; _chemical_name_common cpd1 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H23 Cl F N O4 S' _chemical_formula_weight 415.89 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.010(5) _cell_length_b 9.223(2) _cell_length_c 9.454(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.101(5) _cell_angle_gamma 90.00 _cell_volume 1889.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1681 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.27 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9336 _exptl_absorpt_correction_T_max 0.9931 _exptl_absorpt_process_details TWINABS _diffrn_refln_scan_width 0.5 _diffrn_refln_scan_rate 30 _space_group.centring_type primitive _space_group.IT_number 14 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 5279 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0917 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.39 _reflns_number_total 5279 _reflns_number_gt 3938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-2011' _computing_structure_refinement 'SHELXL-97' _computing_molecular_graphics 'ORTEP-32' _computing_publication_material 'WinGX' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5279 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.17004(15) 0.9364(3) -0.1406(4) 0.0144(8) Uani 1 1 d . . . C2 C 0.16829(15) 0.9325(4) -0.3022(4) 0.0174(8) Uani 1 1 d . . . H2A H 0.1739 0.8315 -0.3330 0.021 Uiso 1 1 calc R . . H2B H 0.2025 0.9918 -0.3266 0.021 Uiso 1 1 calc R . . C3 C 0.10670(15) 0.9912(3) -0.3815(4) 0.0166(8) Uani 1 1 d . . . H3 H 0.1060 0.9871 -0.4875 0.020 Uiso 1 1 calc R . . C4 C 0.05382(16) 0.9005(4) -0.3435(4) 0.0215(9) Uani 1 1 d . . . H4A H 0.0140 0.9386 -0.3949 0.026 Uiso 1 1 calc R . . H4B H 0.0580 0.7989 -0.3743 0.026 Uiso 1 1 calc R . . C5 C 0.05482(16) 0.9054(4) -0.1822(4) 0.0191(9) Uani 1 1 d . . . H5 H 0.0204 0.8452 -0.1572 0.023 Uiso 1 1 calc R . . C6 C 0.11666(14) 0.8481(4) -0.1042(4) 0.0187(8) Uani 1 1 d . . . H6A H 0.1175 0.8516 0.0008 0.022 Uiso 1 1 calc R . . H6B H 0.1214 0.7456 -0.1315 0.022 Uiso 1 1 calc R . . C7 C 0.16202(15) 1.0940(3) -0.0957(4) 0.0179(8) Uani 1 1 d . . . H7A H 0.1963 1.1537 -0.1191 0.022 Uiso 1 1 calc R . . H7B H 0.1632 1.0988 0.0093 0.022 Uiso 1 1 calc R . . C8 C 0.10003(16) 1.1542(4) -0.1748(4) 0.0176(9) Uani 1 1 d . . . H8 H 0.0952 1.2570 -0.1452 0.021 Uiso 1 1 calc R . . C9 C 0.09945(16) 1.1475(4) -0.3359(4) 0.0188(9) Uani 1 1 d . . . H9A H 0.0601 1.1875 -0.3881 0.023 Uiso 1 1 calc R . . H9B H 0.1336 1.2070 -0.3602 0.023 Uiso 1 1 calc R . . C10 C 0.04777(15) 1.0630(3) -0.1364(4) 0.0200(8) Uani 1 1 d . . . H10A H 0.0077 1.1019 -0.1857 0.024 Uiso 1 1 calc R . . H10B H 0.0485 1.0673 -0.0315 0.024 Uiso 1 1 calc R . . C11 C 0.23079(15) 0.8843(3) -0.0562(4) 0.0184(8) Uani 1 1 d . . . H11A H 0.2647 0.9474 -0.0759 0.022 Uiso 1 1 calc R . . H11B H 0.2297 0.8884 0.0480 0.022 Uiso 1 1 calc R . . C12 C 0.27900(14) 0.6540(3) -0.0033(4) 0.0136(7) Uani 1 1 d . . . C13 C 0.31244(14) 0.7038(4) 0.1250(4) 0.0151(8) Uani 1 1 d . . . H13 H 0.3124 0.8039 0.1485 0.018 Uiso 1 1 calc R . . C14 C 0.34552(15) 0.6071(4) 0.2175(3) 0.0129(8) Uani 1 1 d . . . C15 C 0.34977(14) 0.4600(4) 0.1881(4) 0.0136(7) Uani 1 1 d . . . C16 C 0.31762(14) 0.4133(4) 0.0566(4) 0.0155(8) Uani 1 1 d . . . H16 H 0.3197 0.3141 0.0309 0.019 Uiso 1 1 calc R . . C17 C 0.28307(14) 0.5063(3) -0.0367(3) 0.0139(8) Uani 1 1 d . . . C18 C 0.38682(15) 0.3616(4) 0.2950(4) 0.0139(8) Uani 1 1 d . . . C19 C 0.52490(13) 0.2464(4) 0.4235(4) 0.0203(8) Uani 1 1 d . . . H19A H 0.5547 0.1841 0.4844 0.030 Uiso 1 1 calc R . . H19B H 0.5073 0.3156 0.4837 0.030 Uiso 1 1 calc R . . H19C H 0.5457 0.2993 0.3558 0.030 Uiso 1 1 calc R . . N1 N 0.41915(11) 0.2569(3) 0.2320(3) 0.0158(6) Uani 1 1 d . . . H1 H 0.4143 0.2527 0.1377 0.019 Uiso 1 1 calc R . . O1 O 0.24119(9) 0.7367(2) -0.0982(2) 0.0173(5) Uani 1 1 d . . . O2 O 0.38932(11) 0.3704(3) 0.4215(3) 0.0193(6) Uani 1 1 d . . . O3 O 0.49018(10) 0.0549(2) 0.2256(2) 0.0223(6) Uani 1 1 d . . . O4 O 0.43344(10) 0.0714(2) 0.4278(3) 0.0227(6) Uani 1 1 d . . . F1 F 0.37668(8) 0.6607(2) 0.3418(2) 0.0220(5) Uani 1 1 d . . . S1 S 0.46632(4) 0.14020(9) 0.32861(10) 0.0161(2) Uani 1 1 d . . . Cl1 Cl 0.24243(4) 0.44238(9) -0.19768(10) 0.0247(2) Uani 1 1 d . . . 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 0.0173(19) 0.0114(19) 0.0149(19) 0.0004(15) 0.0037(16) 0.0029(16) C2 0.0151(19) 0.0114(19) 0.026(2) -0.0002(16) 0.0058(17) 0.0009(16) C3 0.0225(19) 0.0155(19) 0.0119(19) -0.0015(14) 0.0031(15) 0.0013(15) C4 0.019(2) 0.019(2) 0.025(2) -0.0041(17) 0.0003(18) 0.0008(16) C5 0.0151(19) 0.014(2) 0.029(2) 0.0012(17) 0.0063(17) -0.0011(15) C6 0.0219(18) 0.0156(19) 0.019(2) 0.0006(15) 0.0042(16) 0.0050(15) C7 0.0196(18) 0.0151(19) 0.018(2) -0.0011(14) 0.0016(16) 0.0008(14) C8 0.025(2) 0.0100(19) 0.018(2) -0.0002(16) 0.0035(17) 0.0049(16) C9 0.020(2) 0.018(2) 0.019(2) 0.0039(17) 0.0027(17) 0.0027(17) C10 0.0208(18) 0.0185(19) 0.021(2) 0.0023(16) 0.0056(15) 0.0050(15) C11 0.0244(19) 0.0096(17) 0.020(2) -0.0025(15) 0.0014(16) 0.0031(15) C12 0.0135(16) 0.0142(17) 0.0136(19) 0.0039(15) 0.0037(16) 0.0012(14) C13 0.0141(17) 0.0108(19) 0.020(2) 0.0010(14) 0.0020(15) 0.0011(14) C14 0.0106(17) 0.0183(19) 0.0096(18) -0.0040(14) 0.0008(14) -0.0017(14) C15 0.0130(17) 0.0140(18) 0.0144(19) 0.0026(15) 0.0039(15) 0.0019(15) C16 0.0166(18) 0.0154(19) 0.015(2) 0.0001(14) 0.0047(15) -0.0002(14) C17 0.0133(17) 0.0155(18) 0.013(2) -0.0011(14) 0.0012(15) -0.0013(14) C18 0.0149(17) 0.0156(19) 0.011(2) 0.0015(16) 0.0021(16) 0.0001(16) C19 0.0175(17) 0.0171(17) 0.0230(19) -0.0018(15) -0.0051(17) 0.0015(16) N1 0.0195(14) 0.0197(15) 0.0073(14) 0.0023(13) -0.0006(13) 0.0078(14) O1 0.0205(11) 0.0112(11) 0.0188(13) -0.0005(10) 0.0000(12) 0.0064(10) O2 0.0221(13) 0.0251(15) 0.0111(15) 0.0013(11) 0.0042(11) 0.0044(11) O3 0.0287(14) 0.0171(13) 0.0204(14) -0.0050(11) 0.0025(11) 0.0069(12) O4 0.0208(13) 0.0200(14) 0.0281(16) 0.0148(11) 0.0062(11) -0.0007(11) F1 0.0249(11) 0.0181(11) 0.0196(11) -0.0046(9) -0.0052(9) 0.0026(8) S1 0.0161(4) 0.0138(4) 0.0174(5) 0.0023(4) 0.0003(4) 0.0030(4) Cl1 0.0351(5) 0.0171(4) 0.0180(5) -0.0006(4) -0.0058(4) 0.0006(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 C11 1.510(4) . ? C1 C6 1.518(5) . ? C1 C2 1.521(5) . ? C1 C7 1.533(4) . ? C2 C3 1.529(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C9 1.521(5) . ? C3 C4 1.527(5) . ? C3 H3 1.0000 . ? C4 C5 1.522(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.525(4) . ? C5 C10 1.532(4) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.540(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.519(5) . ? C8 C9 1.522(5) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O1 1.448(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O1 1.348(4) . ? C12 C13 1.382(4) . ? C12 C17 1.404(4) . ? C13 C14 1.366(4) . ? C13 H13 0.9500 . ? C14 F1 1.347(3) . ? C14 C15 1.392(4) . ? C15 C16 1.386(4) . ? C15 C18 1.490(4) . ? C16 C17 1.363(4) . ? C16 H16 0.9500 . ? C17 Cl1 1.728(3) . ? C18 O2 1.190(4) . ? C18 N1 1.393(4) . ? C19 S1 1.738(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N1 S1 1.655(3) . ? N1 H1 0.8800 . ? O3 S1 1.422(2) . ? O4 S1 1.430(2) . ? 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 C11 C1 C6 111.0(3) . . ? C11 C1 C2 112.8(3) . . ? C6 C1 C2 109.3(3) . . ? C11 C1 C7 106.8(3) . . ? C6 C1 C7 108.3(3) . . ? C2 C1 C7 108.4(3) . . ? C1 C2 C3 110.4(3) . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C9 C3 C4 109.3(3) . . ? C9 C3 C2 108.9(3) . . ? C4 C3 C2 109.7(3) . . ? C9 C3 H3 109.6 . . ? C4 C3 H3 109.6 . . ? C2 C3 H3 109.6 . . ? C5 C4 C3 110.0(3) . . ? 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 109.2(3) . . ? C4 C5 C10 109.1(3) . . ? C6 C5 C10 108.6(3) . . ? C4 C5 H5 110.0 . . ? C6 C5 H5 110.0 . . ? C10 C5 H5 110.0 . . ? C1 C6 C5 111.4(3) . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C1 C7 C8 110.0(3) . . ? C1 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? C1 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C10 C8 C9 110.0(3) . . ? C10 C8 C7 109.2(3) . . ? C9 C8 C7 108.8(3) . . ? C10 C8 H8 109.6 . . ? C9 C8 H8 109.6 . . ? C7 C8 H8 109.6 . . ? C3 C9 C8 109.8(3) . . ? C3 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C3 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C8 C10 C5 109.8(3) . . ? C8 C10 H10A 109.7 . . ? C5 C10 H10A 109.7 . . ? C8 C10 H10B 109.7 . . ? C5 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? O1 C11 C1 108.8(3) . . ? O1 C11 H11A 109.9 . . ? C1 C11 H11A 109.9 . . ? O1 C11 H11B 109.9 . . ? C1 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O1 C12 C13 124.6(3) . . ? O1 C12 C17 117.1(3) . . ? C13 C12 C17 118.3(3) . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? F1 C14 C13 116.9(3) . . ? F1 C14 C15 119.3(3) . . ? C13 C14 C15 123.8(3) . . ? C16 C15 C14 116.1(3) . . ? C16 C15 C18 123.5(3) . . ? C14 C15 C18 120.4(3) . . ? C17 C16 C15 121.6(3) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C12 121.0(3) . . ? C16 C17 Cl1 120.0(2) . . ? C12 C17 Cl1 119.0(2) . . ? O2 C18 N1 122.7(3) . . ? O2 C18 C15 124.3(3) . . ? N1 C18 C15 113.1(3) . . ? S1 C19 H19A 109.5 . . ? S1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? S1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 N1 S1 122.2(2) . . ? C18 N1 H1 118.9 . . ? S1 N1 H1 118.9 . . ? C12 O1 C11 117.3(2) . . ? O3 S1 O4 119.60(14) . . ? O3 S1 N1 104.68(14) . . ? O4 S1 N1 108.05(14) . . ? O3 S1 C19 109.61(16) . . ? O4 S1 C19 109.06(17) . . ? N1 S1 C19 104.78(15) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.296 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.069 _iucr_refine_instructions_details ; TITL twin4 in P2(1)/c CELL 0.71073 22.0103 9.2226 9.4538 90.000 100.101 90.000 ZERR 4.00 0.0050 0.0020 0.0020 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F S CL UNIT 76 92 4 16 4 4 4 MERG 0 FMAP 2 PLAN 25 SIZE 0.02 0.08 0.20 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP -173.00 WGHT 0.055200 BASF 0.72582 FVAR 0.55062 C1 1 0.170044 0.936366 -0.140641 11.00000 0.01725 0.01142 = 0.01486 0.00044 0.00368 0.00285 C2 1 0.168294 0.932505 -0.302153 11.00000 0.01514 0.01138 = 0.02642 -0.00020 0.00577 0.00085 AFIX 23 H2A 2 0.173946 0.831540 -0.332964 11.00000 -1.20000 H2B 2 0.202494 0.991797 -0.326600 11.00000 -1.20000 AFIX 0 C3 1 0.106700 0.991198 -0.381514 11.00000 0.02248 0.01551 = 0.01187 -0.00147 0.00309 0.00131 AFIX 13 H3 2 0.105950 0.987117 -0.487508 11.00000 -1.20000 AFIX 0 C4 1 0.053818 0.900460 -0.343531 11.00000 0.01949 0.01890 = 0.02495 -0.00407 0.00032 0.00082 AFIX 23 H4A 2 0.013950 0.938620 -0.394882 11.00000 -1.20000 H4B 2 0.057958 0.798856 -0.374269 11.00000 -1.20000 AFIX 0 C5 1 0.054824 0.905406 -0.182233 11.00000 0.01507 0.01372 = 0.02927 0.00118 0.00634 -0.00109 AFIX 13 H5 2 0.020430 0.845199 -0.157236 11.00000 -1.20000 AFIX 0 C6 1 0.116660 0.848051 -0.104192 11.00000 0.02187 0.01556 = 0.01879 0.00061 0.00418 0.00497 AFIX 23 H6A 2 0.117471 0.851579 0.000785 11.00000 -1.20000 H6B 2 0.121423 0.745591 -0.131509 11.00000 -1.20000 AFIX 0 C7 1 0.162017 1.093996 -0.095726 11.00000 0.01957 0.01509 = 0.01846 -0.00109 0.00157 0.00077 AFIX 23 H7A 2 0.196300 1.153717 -0.119102 11.00000 -1.20000 H7B 2 0.163220 1.098816 0.009343 11.00000 -1.20000 AFIX 0 C8 1 0.100032 1.154189 -0.174770 11.00000 0.02468 0.00998 = 0.01807 -0.00016 0.00349 0.00486 AFIX 13 H8 2 0.095156 1.257036 -0.145180 11.00000 -1.20000 AFIX 0 C9 1 0.099454 1.147535 -0.335863 11.00000 0.01981 0.01758 = 0.01889 0.00391 0.00273 0.00274 AFIX 23 H9A 2 0.060088 1.187461 -0.388097 11.00000 -1.20000 H9B 2 0.133626 1.206980 -0.360226 11.00000 -1.20000 AFIX 0 C10 1 0.047775 1.062961 -0.136449 11.00000 0.02083 0.01851 = 0.02136 0.00226 0.00563 0.00498 AFIX 23 H10A 2 0.007677 1.101856 -0.185674 11.00000 -1.20000 H10B 2 0.048472 1.067318 -0.031543 11.00000 -1.20000 AFIX 0 C11 1 0.230794 0.884303 -0.056209 11.00000 0.02442 0.00961 = 0.02031 -0.00250 0.00137 0.00305 AFIX 23 H11A 2 0.264726 0.947446 -0.075859 11.00000 -1.20000 H11B 2 0.229749 0.888351 0.047982 11.00000 -1.20000 AFIX 0 C12 1 0.278996 0.653952 -0.003282 11.00000 0.01346 0.01421 = 0.01360 0.00389 0.00372 0.00125 C13 1 0.312444 0.703761 0.124999 11.00000 0.01406 0.01085 = 0.02001 0.00100 0.00199 0.00107 AFIX 43 H13 2 0.312425 0.803901 0.148540 11.00000 -1.20000 AFIX 0 C14 1 0.345519 0.607130 0.217456 11.00000 0.01060 0.01826 = 0.00959 -0.00401 0.00077 -0.00173 C15 1 0.349770 0.459951 0.188098 11.00000 0.01299 0.01397 = 0.01438 0.00264 0.00391 0.00185 C16 1 0.317624 0.413348 0.056619 11.00000 0.01657 0.01538 = 0.01519 0.00015 0.00474 -0.00018 AFIX 43 H16 2 0.319736 0.314120 0.030948 11.00000 -1.20000 AFIX 0 C17 1 0.283074 0.506325 -0.036709 11.00000 0.01329 0.01553 = 0.01251 -0.00112 0.00121 -0.00128 C18 1 0.386818 0.361609 0.294980 11.00000 0.01486 0.01562 = 0.01126 0.00154 0.00215 0.00012 C19 1 0.524896 0.246373 0.423474 11.00000 0.01749 0.01710 = 0.02303 -0.00180 -0.00514 0.00153 AFIX 137 H19A 2 0.554745 0.184105 0.484394 11.00000 -1.50000 H19B 2 0.507255 0.315603 0.483722 11.00000 -1.50000 H19C 2 0.545721 0.299288 0.355803 11.00000 -1.50000 AFIX 0 N1 3 0.419150 0.256930 0.232036 11.00000 0.01946 0.01973 = 0.00728 0.00228 -0.00062 0.00782 AFIX 43 H1 2 0.414322 0.252749 0.137731 11.00000 -1.20000 AFIX 0 O1 4 0.241192 0.736688 -0.098235 11.00000 0.02053 0.01122 = 0.01884 -0.00047 -0.00004 0.00641 O2 4 0.389316 0.370449 0.421495 11.00000 0.02212 0.02506 = 0.01108 0.00126 0.00418 0.00437 O3 4 0.490179 0.054863 0.225602 11.00000 0.02873 0.01714 = 0.02043 -0.00499 0.00251 0.00690 O4 4 0.433440 0.071426 0.427838 11.00000 0.02078 0.01996 = 0.02806 0.01485 0.00616 -0.00075 F1 5 0.376680 0.660677 0.341845 11.00000 0.02494 0.01813 = 0.01963 -0.00458 -0.00523 0.00259 S1 6 0.466321 0.140203 0.328615 11.00000 0.01612 0.01384 = 0.01737 0.00231 0.00027 0.00296 CL1 7 0.242427 0.442383 -0.197677 11.00000 0.03510 0.01713 = 0.01800 -0.00063 -0.00582 0.00061 HKLF 5 REM twin4 in P2(1)/c REM R1 = 0.0516 for 3938 Fo > 4sig(Fo) and 0.0785 for all 5279 data REM 246 parameters refined using 0 restraints END WGHT 0.0551 0.0000 REM Highest difference peak 0.296, deepest hole -0.390, 1-sigma level 0.069 Q1 1 0.4613 0.1134 0.0758 11.00000 0.05 0.29 Q2 1 0.2981 0.4193 -0.2042 11.00000 0.05 0.27 Q3 1 0.2628 0.7977 0.1707 11.00000 0.05 0.27 Q4 1 0.1938 0.4618 -0.1859 11.00000 0.05 0.27 Q5 1 0.4690 0.1213 0.5970 11.00000 0.05 0.26 Q6 1 0.1339 0.9472 -0.3228 11.00000 0.05 0.25 Q7 1 0.1792 0.7713 -0.3192 11.00000 0.05 0.25 Q8 1 0.3880 0.3274 0.0458 11.00000 0.05 0.25 Q9 1 0.1010 0.7079 -0.3234 11.00000 0.05 0.24 Q10 1 0.1736 0.9378 -0.2142 11.00000 0.05 0.24 Q11 1 0.3182 0.6448 0.1853 11.00000 0.05 0.24 Q12 1 0.3404 0.4290 0.4439 11.00000 0.05 0.24 Q13 1 0.2043 0.9095 -0.1174 11.00000 0.05 0.24 Q14 1 0.1894 1.1622 0.0176 11.00000 0.05 0.23 Q15 1 0.5412 0.1480 0.4838 11.00000 0.05 0.23 Q16 1 0.1717 0.9977 -0.1181 11.00000 0.05 0.23 Q17 1 0.3694 0.4038 0.5468 11.00000 0.05 0.22 Q18 1 0.1448 0.6653 -0.2633 11.00000 0.05 0.22 Q19 1 0.4249 0.0827 0.1419 11.00000 0.05 0.22 Q20 1 0.3160 0.7484 0.1394 11.00000 0.05 0.22 Q21 1 0.2203 1.1478 -0.0920 11.00000 0.05 0.22 Q22 1 0.0601 0.9139 -0.6004 11.00000 0.05 0.22 Q23 1 0.3094 0.8623 0.1850 11.00000 0.05 0.22 Q24 1 0.2835 0.4865 -0.3003 11.00000 0.05 0.22 Q25 1 0.5413 0.1197 0.6160 11.00000 0.05 0.21 ;