#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 11 _journal_issue 4 _journal_year 2020 _journal_page_first 261 _journal_page_last 275 #=============================================================================== data_5h _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C16 H14 Cl O S' _chemical_formula_sum 'C16 H14 Cl O S' _chemical_formula_weight 289.78 _chemical_melting_point ? 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' 'O' 'O' 0.0106 0.0060 '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' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7517(6) _cell_length_b 8.8376(9) _cell_length_c 12.6049(12) _cell_angle_alpha 109.538(3) _cell_angle_beta 98.597(3) _cell_angle_gamma 90.417(3) _cell_volume 699.52(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3898 _cell_measurement_temperature 290 _cell_measurement_theta_max 29.644 _cell_measurement_theta_min 3.057 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.410 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 302 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 28754 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.644 _diffrn_reflns_theta_min 3.057 _diffrn_ambient_temperature 290 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type Bruker _diffrn_measurement_method SAINT _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source graphite _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 200 _diffrn_standards_number 3898 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2687 _reflns_number_total 3898 _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. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_collection 'APEX (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_molecular_graphics 'PLATON(Spek, 2009)' _computing_publication_material 'PLATON(Spek, 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2015)' _refine_diff_density_max 0.501 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.090 _refine_ls_extinction_coef 0.244(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 176 _refine_ls_number_reflns 3898 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1374 _refine_ls_R_factor_gt 0.1101 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+3.4200P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2374 _refine_ls_wR_factor_ref 0.2481 _refine_special_details ; Refined as a 2-component twin. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 0.4027(3) 0.6717(2) 0.65397(15) 0.0595(5) Uani 1 1 d . . . . . Cl1 Cl 0.5894(3) 0.9926(3) 0.6694(2) 0.0888(8) Uani 1 1 d . . . . . C10 C 0.0567(9) 0.7222(8) 0.7172(6) 0.0552(15) Uani 1 1 d . . . . . H10 H -0.052651 0.773103 0.747165 0.066 Uiso 1 1 calc R U . . . C9 C 0.2309(10) 0.8048(8) 0.7196(5) 0.0536(15) Uani 1 1 d . . . . . C6 C 0.4153(10) 1.0702(9) 0.7588(6) 0.0592(17) Uani 1 1 d . . . . . C16 C 0.2401(10) 0.5065(8) 0.6267(5) 0.0526(15) Uani 1 1 d . . . . . C2 C 0.1246(11) 1.0606(9) 0.8526(6) 0.0641(19) Uani 1 1 d . . . . . H2 H -0.002932 1.015122 0.846718 0.077 Uiso 1 1 calc R U . . . C11 C 0.0568(10) 0.5534(8) 0.6654(5) 0.0538(15) Uani 1 1 d . . . . . C3 C 0.2009(11) 1.2225(8) 0.9427(6) 0.0596(17) Uani 1 1 d . . . . . C5 C 0.4441(11) 1.2487(10) 0.8154(6) 0.0629(17) Uani 1 1 d . . . . . C1 C 0.2699(9) 0.9778(8) 0.7727(5) 0.0510(14) Uani 1 1 d . . . . . O1 O 0.5888(9) 1.3239(7) 0.8065(5) 0.0864(19) Uani 1 1 d . . . . . C12 C -0.0925(11) 0.4344(9) 0.6483(7) 0.0630(18) Uani 1 1 d . . . . . H12 H -0.214340 0.462937 0.673028 0.076 Uiso 1 1 calc R U . . . C4 C 0.2827(11) 1.3271(8) 0.8833(6) 0.0622(18) Uani 1 1 d . . . . . H4A H 0.173539 1.349860 0.832506 0.075 Uiso 1 1 calc R U . . . H4B H 0.337728 1.428727 0.939982 0.075 Uiso 1 1 calc R U . . . C14 C 0.1199(13) 0.2316(10) 0.5578(6) 0.069(2) Uani 1 1 d . . . . . H14 H 0.139717 0.123696 0.521714 0.083 Uiso 1 1 calc R U . . . C15 C 0.2717(12) 0.3477(9) 0.5739(6) 0.0658(19) Uani 1 1 d . . . . . H15 H 0.393315 0.318103 0.549226 0.079 Uiso 1 1 calc R U . . . C8 C 0.0285(14) 1.2995(10) 1.0004(8) 0.079(2) Uani 1 1 d . . . . . H8A H -0.076711 1.312557 0.944457 0.119 Uiso 1 1 calc R U . . . H8B H 0.074169 1.402763 1.055890 0.119 Uiso 1 1 calc R U . . . H8C H -0.021666 1.232034 1.037670 0.119 Uiso 1 1 calc R U . . . C13 C -0.0619(12) 0.2758(9) 0.5954(7) 0.071(2) Uani 1 1 d . . . . . H13 H -0.162703 0.197298 0.584549 0.086 Uiso 1 1 calc R U . . . C7 C 0.3647(15) 1.2010(12) 1.0334(7) 0.090(3) Uani 1 1 d . . . . . H7A H 0.316541 1.124317 1.063910 0.136 Uiso 1 1 calc R U . . . H7B H 0.399164 1.302354 1.093644 0.136 Uiso 1 1 calc R U . . . H7C H 0.481245 1.162979 0.999676 0.136 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 0.0520(9) 0.0646(10) 0.0542(9) 0.0075(8) 0.0149(7) -0.0027(8) Cl1 0.0743(13) 0.0841(14) 0.1003(16) 0.0089(12) 0.0439(12) -0.0131(11) C10 0.046(3) 0.056(4) 0.059(4) 0.014(3) 0.010(3) -0.002(3) C9 0.052(3) 0.060(4) 0.044(3) 0.012(3) 0.008(3) -0.003(3) C6 0.052(3) 0.067(4) 0.055(4) 0.015(3) 0.007(3) -0.005(3) C16 0.057(3) 0.059(4) 0.040(3) 0.013(3) 0.010(3) 0.002(3) C2 0.062(4) 0.056(4) 0.068(4) 0.007(3) 0.024(3) -0.005(3) C11 0.053(3) 0.057(4) 0.049(3) 0.016(3) 0.005(3) -0.003(3) C3 0.067(4) 0.054(4) 0.056(4) 0.015(3) 0.013(3) 0.008(3) C5 0.060(4) 0.068(4) 0.058(4) 0.022(3) 0.002(3) -0.011(3) C1 0.047(3) 0.055(3) 0.047(3) 0.014(3) 0.005(2) -0.002(3) O1 0.080(4) 0.076(4) 0.098(4) 0.021(3) 0.018(3) -0.025(3) C12 0.055(4) 0.061(4) 0.070(4) 0.019(3) 0.010(3) -0.006(3) C4 0.063(4) 0.051(4) 0.063(4) 0.012(3) 0.001(3) -0.002(3) C14 0.088(6) 0.059(4) 0.052(4) 0.008(3) 0.010(4) 0.001(4) C15 0.075(5) 0.064(4) 0.052(4) 0.008(3) 0.017(3) -0.001(4) C8 0.098(6) 0.060(4) 0.083(5) 0.018(4) 0.038(5) 0.015(4) C13 0.071(5) 0.063(4) 0.072(5) 0.015(4) 0.003(4) -0.016(4) C7 0.109(7) 0.095(7) 0.057(4) 0.020(4) -0.005(4) 0.018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C9 1.752(7) . ? S1 C16 1.727(7) . ? Cl1 C6 1.736(7) . ? C10 H10 0.9300 . ? C10 C9 1.370(9) . ? C10 C11 1.415(9) . ? C9 C1 1.454(9) . ? C6 C5 1.495(10) . ? C6 C1 1.340(9) . ? C16 C11 1.412(9) . ? C16 C15 1.371(10) . ? C2 H2 0.9300 . ? C2 C3 1.527(9) . ? C2 C1 1.525(9) . ? C11 C12 1.391(9) . ? C3 C4 1.517(10) . ? C3 C8 1.510(10) . ? C3 C7 1.528(11) . ? C5 O1 1.218(8) . ? C5 C4 1.514(10) . ? C12 H12 0.9300 . ? C12 C13 1.368(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C14 H14 0.9300 . ? C14 C15 1.388(10) . ? C14 C13 1.393(11) . ? C15 H15 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C13 H13 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 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 C16 S1 C9 92.2(3) . . ? C9 C10 H10 122.7 . . ? C9 C10 C11 114.6(6) . . ? C11 C10 H10 122.7 . . ? C10 C9 S1 110.5(5) . . ? C10 C9 C1 124.7(6) . . ? C1 C9 S1 124.8(5) . . ? C5 C6 Cl1 112.8(5) . . ? C1 C6 Cl1 122.6(6) . . ? C1 C6 C5 124.6(6) . . ? C11 C16 S1 111.1(5) . . ? C15 C16 S1 127.7(5) . . ? C15 C16 C11 121.1(6) . . ? C3 C2 H2 122.0 . . ? C1 C2 H2 122.0 . . ? C1 C2 C3 116.1(6) . . ? C16 C11 C10 111.7(6) . . ? C12 C11 C10 129.9(6) . . ? C12 C11 C16 118.4(6) . . ? C2 C3 C7 111.0(7) . . ? C4 C3 C2 108.1(6) . . ? C4 C3 C7 110.2(7) . . ? C8 C3 C2 108.9(6) . . ? C8 C3 C4 110.4(6) . . ? C8 C3 C7 108.4(7) . . ? C6 C5 C4 115.6(6) . . ? O1 C5 C6 121.3(7) . . ? O1 C5 C4 123.1(7) . . ? C9 C1 C2 114.6(5) . . ? C6 C1 C9 127.8(6) . . ? C6 C1 C2 117.6(6) . . ? C11 C12 H12 119.7 . . ? C13 C12 C11 120.7(7) . . ? C13 C12 H12 119.7 . . ? C3 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C5 C4 C3 112.5(6) . . ? C5 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C15 C14 H14 119.8 . . ? C15 C14 C13 120.4(7) . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 119.2(7) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C13 C14 120.1(7) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 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 S1 C9 C1 C6 17.2(10) . . . . ? S1 C9 C1 C2 -163.2(5) . . . . ? S1 C16 C11 C10 -0.8(7) . . . . ? S1 C16 C11 C12 179.0(6) . . . . ? S1 C16 C15 C14 -178.8(6) . . . . ? Cl1 C6 C5 O1 -7.1(10) . . . . ? Cl1 C6 C5 C4 172.9(5) . . . . ? Cl1 C6 C1 C9 0.3(11) . . . . ? Cl1 C6 C1 C2 -179.3(6) . . . . ? C10 C9 C1 C6 -165.0(7) . . . . ? C10 C9 C1 C2 14.6(10) . . . . ? C10 C11 C12 C13 179.9(8) . . . . ? C9 S1 C16 C11 1.1(5) . . . . ? C9 S1 C16 C15 -179.7(7) . . . . ? C9 C10 C11 C16 -0.1(9) . . . . ? C9 C10 C11 C12 -179.9(7) . . . . ? C6 C5 C4 C3 35.6(9) . . . . ? C16 S1 C9 C10 -1.1(5) . . . . ? C16 S1 C9 C1 176.9(6) . . . . ? C16 C11 C12 C13 0.1(11) . . . . ? C2 C3 C4 C5 -56.1(8) . . . . ? C11 C10 C9 S1 0.9(8) . . . . ? C11 C10 C9 C1 -177.2(6) . . . . ? C11 C16 C15 C14 0.4(11) . . . . ? C11 C12 C13 C14 -0.1(12) . . . . ? C3 C2 C1 C9 157.3(6) . . . . ? C3 C2 C1 C6 -23.0(10) . . . . ? C5 C6 C1 C9 179.1(7) . . . . ? C5 C6 C1 C2 -0.5(10) . . . . ? C1 C6 C5 O1 174.0(7) . . . . ? C1 C6 C5 C4 -6.0(10) . . . . ? C1 C2 C3 C4 50.6(9) . . . . ? C1 C2 C3 C8 170.6(7) . . . . ? C1 C2 C3 C7 -70.2(9) . . . . ? O1 C5 C4 C3 -144.5(8) . . . . ? C15 C16 C11 C10 179.9(7) . . . . ? C15 C16 C11 C12 -0.3(10) . . . . ? C15 C14 C13 C12 0.2(13) . . . . ? C8 C3 C4 C5 -175.0(6) . . . . ? C13 C14 C15 C16 -0.4(12) . . . . ? C7 C3 C4 C5 65.3(8) . . . . ? _shelx_res_file ; TITL d12_a.res in P-1 5h.res created by SHELXL-2018/3 at 22:01:56 on 12-Aug-2020 CELL 0.71073 6.7517 8.8376 12.6049 109.538 98.597 90.417 ZERR 2.00 0.0006 0.0009 0.0012 0.003 0.003 0.003 LATT 1 SFAC C H O S CL UNIT 24 26 2 2 2 L.S. 4 BOND $H TWIN -1 -0.011 0 0 1 -0 -0 -0.954 -1 HTAB ACTA CONF MERG 2 FMAP 2 PLAN 20 WGHT 0.001000 3.420000 EXTI 0.244453 BASF 0.17675 FVAR 1.96971 MOLE 1 S1 4 0.402750 0.671688 0.653966 11.00000 0.05198 0.06457 = 0.05419 0.00746 0.01491 -0.00266 CL1 5 0.589435 0.992585 0.669357 11.00000 0.07433 0.08409 = 0.10032 0.00892 0.04386 -0.01310 C10 1 0.056728 0.722244 0.717180 11.00000 0.04610 0.05638 = 0.05895 0.01375 0.00970 -0.00151 AFIX 43 H10 2 -0.052651 0.773103 0.747165 11.00000 -1.20000 AFIX 0 C9 1 0.230864 0.804774 0.719608 11.00000 0.05164 0.06012 = 0.04449 0.01184 0.00774 -0.00330 C6 1 0.415310 1.070181 0.758803 11.00000 0.05167 0.06667 = 0.05458 0.01529 0.00671 -0.00545 C16 1 0.240074 0.506527 0.626726 11.00000 0.05705 0.05869 = 0.04008 0.01307 0.01021 0.00177 C2 1 0.124631 1.060591 0.852558 11.00000 0.06179 0.05570 = 0.06840 0.00720 0.02418 -0.00480 AFIX 43 H2 2 -0.002932 1.015122 0.846718 11.00000 -1.20000 AFIX 0 C11 1 0.056768 0.553360 0.665357 11.00000 0.05289 0.05691 = 0.04885 0.01573 0.00543 -0.00300 C3 1 0.200900 1.222504 0.942730 11.00000 0.06730 0.05396 = 0.05598 0.01497 0.01321 0.00775 C5 1 0.444091 1.248671 0.815428 11.00000 0.06008 0.06795 = 0.05820 0.02193 0.00157 -0.01135 C1 1 0.269896 0.977838 0.772653 11.00000 0.04713 0.05537 = 0.04685 0.01372 0.00467 -0.00191 O1 3 0.588779 1.323933 0.806503 11.00000 0.07952 0.07609 = 0.09808 0.02125 0.01844 -0.02498 C12 1 -0.092506 0.434367 0.648264 11.00000 0.05457 0.06122 = 0.07010 0.01879 0.00961 -0.00633 AFIX 43 H12 2 -0.214340 0.462937 0.673028 11.00000 -1.20000 AFIX 0 C4 1 0.282704 1.327149 0.883328 11.00000 0.06336 0.05092 = 0.06339 0.01174 0.00086 -0.00202 AFIX 23 H4A 2 0.173539 1.349860 0.832506 11.00000 -1.20000 H4B 2 0.337728 1.428727 0.939982 11.00000 -1.20000 AFIX 0 C14 1 0.119909 0.231649 0.557832 11.00000 0.08821 0.05895 = 0.05230 0.00836 0.01046 0.00096 AFIX 43 H14 2 0.139717 0.123696 0.521714 11.00000 -1.20000 AFIX 0 C15 1 0.271682 0.347692 0.573933 11.00000 0.07465 0.06401 = 0.05185 0.00813 0.01665 -0.00115 AFIX 43 H15 2 0.393315 0.318103 0.549226 11.00000 -1.20000 AFIX 0 C8 1 0.028465 1.299476 1.000444 11.00000 0.09754 0.06042 = 0.08274 0.01836 0.03804 0.01453 AFIX 137 H8A 2 -0.076711 1.312557 0.944457 11.00000 -1.50000 H8B 2 0.074169 1.402763 1.055890 11.00000 -1.50000 H8C 2 -0.021666 1.232034 1.037670 11.00000 -1.50000 AFIX 0 C13 1 -0.061910 0.275800 0.595415 11.00000 0.07076 0.06288 = 0.07157 0.01481 0.00317 -0.01613 AFIX 43 H13 2 -0.162703 0.197298 0.584549 11.00000 -1.20000 AFIX 0 C7 1 0.364690 1.201043 1.033421 11.00000 0.10884 0.09497 = 0.05714 0.02009 -0.00488 0.01815 AFIX 137 H7A 2 0.316541 1.124317 1.063910 11.00000 -1.50000 H7B 2 0.399164 1.302354 1.093644 11.00000 -1.50000 H7C 2 0.481245 1.162979 0.999676 11.00000 -1.50000 MOLE 2 AFIX 0 HKLF 4 REM d12_a.res in P-1 REM wR2 = 0.2481, GooF = S = 1.060, Restrained GooF = 1.060 for all data REM R1 = 0.1101 for 2687 Fo > 4sig(Fo) and 0.1374 for all 3898 data REM 176 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.501, deepest hole -0.497, 1-sigma level 0.090 Q1 1 0.3833 0.5509 0.6614 11.00000 0.05 0.50 Q2 1 0.6192 1.1220 0.6775 11.00000 0.05 0.50 Q3 1 0.5618 0.8573 0.6440 11.00000 0.05 0.45 Q4 1 0.4080 0.2012 0.6475 11.00000 0.05 0.42 Q5 1 0.4173 0.7914 0.6658 11.00000 0.05 0.41 Q6 1 0.0831 0.9706 0.8983 11.00000 0.05 0.40 Q7 1 0.4398 0.6772 0.6791 11.00000 0.05 0.40 Q8 1 0.3741 0.6643 0.6229 11.00000 0.05 0.39 Q9 1 0.6119 0.9830 0.6438 11.00000 0.05 0.38 Q10 1 0.5058 0.9954 0.6426 11.00000 0.05 0.38 Q11 1 0.2132 0.8839 0.6403 11.00000 0.05 0.37 Q12 1 0.3363 0.6744 0.6433 11.00000 0.05 0.34 Q13 1 0.0042 1.0714 0.7986 11.00000 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4.10 4 -6 9 13.20 7.10 -5 6 -9 14.40 11.50 5 -6 9 8.40 4.80 5 -6 9 23.50 10.80 5 -6 9 10.40 7.90 5 -6 9 19.20 6.80 -6 6 -9 -1.60 8.70 -6 6 -9 0.00 15.00 -6 6 -9 -4.10 13.90 -6 6 -9 10.50 9.70 6 -6 9 -0.90 10.50 6 -6 9 -4.80 8.60 8 5 -9 -3.00 11.50 -8 -5 9 35.50 10.20 -8 -5 9 8.20 13.80 7 5 -9 -3.60 12.40 7 5 -9 10.40 13.00 -7 -5 9 2.50 10.10 -7 -5 9 -1.90 7.30 6 5 -9 7.80 9.50 6 5 -9 18.30 8.50 -6 -5 9 3.40 6.70 -6 -5 9 7.40 7.90 -6 -5 9 13.70 10.70 -6 -5 9 22.10 11.30 5 5 -9 3.70 7.60 5 5 -9 19.10 7.00 5 5 -9 3.00 2.60 -5 -5 9 7.30 7.80 -5 -5 9 4.30 10.60 -5 -5 9 5.70 9.30 -5 -5 9 -2.60 6.20 4 5 -9 45.40 12.50 4 5 -9 60.69 7.30 -4 -5 9 64.69 14.40 -4 -5 9 60.09 9.20 -4 -5 9 45.60 8.60 -4 -5 9 59.69 11.80 -4 -5 9 61.09 5.00 -4 -5 9 56.89 6.90 3 5 -9 30.50 9.60 3 5 -9 51.09 8.80 3 5 -9 21.00 4.30 -3 -5 9 48.50 11.50 -3 -5 9 30.20 3.40 -3 -5 9 40.80 12.40 -3 -5 9 40.90 6.60 2 5 -9 28.80 9.90 -2 -5 9 40.80 6.00 1 5 -9 458.15 35.50 1 5 -9 592.94 38.90 1 5 -9 517.25 35.80 1 5 -9 546.35 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6.30 8.80 -6 5 -9 -0.50 14.10 6 -5 9 2.00 7.40 6 -5 9 -1.20 9.70 8 4 -9 6.10 15.20 -8 -4 9 8.50 12.50 -8 -4 9 -0.70 10.70 7 4 -9 15.90 11.20 7 4 -9 8.40 11.50 -7 -4 9 11.30 8.60 -7 -4 9 1.00 12.10 -7 -4 9 -0.70 9.10 6 4 -9 114.09 21.90 6 4 -9 89.79 8.80 -6 -4 9 100.69 8.80 -6 -4 9 124.29 14.00 -6 -4 9 84.19 9.50 -6 -4 9 114.39 15.70 5 4 -9 5.90 7.00 5 4 -9 4.50 2.90 5 4 -9 11.50 6.60 5 4 -9 -4.70 12.10 5 4 -9 10.60 7.40 -5 -4 9 6.10 7.90 -5 -4 9 20.50 10.20 -5 -4 9 21.40 8.10 -5 -4 9 13.00 5.90 -5 -4 9 8.50 5.50 4 4 -9 706.13 46.40 4 4 -9 692.03 42.80 4 4 -9 632.24 46.00 -4 -4 9 667.73 44.00 -4 -4 9 669.43 44.30 -4 -4 9 729.83 40.40 -4 -4 9 639.44 42.10 -4 -4 9 741.33 44.20 -4 -4 9 681.43 47.10 3 4 -9 106.89 10.10 3 4 -9 119.49 9.80 3 4 -9 116.69 13.20 3 4 -9 129.09 14.40 3 4 -9 118.69 8.60 -3 -4 9 116.39 9.20 -3 -4 9 123.39 13.90 -3 -4 9 120.29 7.90 -3 -4 9 117.69 11.40 -3 -4 9 99.69 14.90 2 4 -9 135.29 10.80 2 4 -9 114.39 10.90 2 4 -9 115.69 9.20 2 4 -9 114.19 9.50 2 4 -9 102.39 13.60 -2 -4 9 123.99 9.70 -2 -4 9 82.99 9.60 -2 -4 9 137.09 14.00 -2 -4 9 105.09 13.20 1 4 -9 157.18 16.60 -1 -4 9 159.68 10.70 0 4 -9 48.00 6.30 0 4 -9 35.80 4.70 0 4 -9 49.70 10.10 0 -4 9 44.40 5.80 -1 4 -9 13.20 8.70 -1 4 -9 5.70 4.10 -1 4 -9 3.70 3.60 -1 4 -9 5.70 4.80 -1 4 -9 -2.10 8.00 1 -4 9 8.40 7.00 1 -4 9 9.10 3.70 1 -4 9 13.20 4.80 1 -4 9 10.50 9.40 1 -4 9 9.00 2.30 -2 4 -9 229.68 17.30 -2 4 -9 266.47 20.00 -2 4 -9 266.37 20.20 -2 4 -9 246.28 16.70 -2 4 -9 263.17 18.90 2 -4 9 256.87 21.50 2 -4 9 244.08 17.30 2 -4 9 227.98 19.60 2 -4 9 269.47 25.30 2 -4 9 236.48 18.10 -3 4 -9 49.00 5.60 -3 4 -9 39.80 4.80 -3 4 -9 38.80 7.50 -3 4 -9 54.19 11.30 3 -4 9 60.79 10.00 3 -4 9 30.30 5.40 -4 4 -9 67.99 7.50 -4 4 -9 95.99 13.00 -4 4 -9 94.89 9.80 4 -4 9 74.29 7.50 4 -4 9 102.89 14.40 4 -4 9 59.99 7.40 4 -4 9 87.99 6.30 -5 4 -9 10.20 9.40 -5 4 -9 6.30 7.60 -5 4 -9 -10.80 11.20 -5 4 -9 5.80 10.40 5 -4 9 0.10 7.70 5 -4 9 6.20 7.00 5 -4 9 15.10 8.10 5 -4 9 20.20 5.50 -6 4 -9 -1.90 9.70 -6 4 -9 3.40 9.10 -6 4 -9 -0.30 12.40 6 -4 9 1.50 9.30 6 -4 9 7.60 7.60 -7 4 -9 16.50 18.10 -7 4 -9 6.90 11.00 7 -4 9 0.70 10.60 8 3 -9 2.10 14.80 -8 -3 9 4.10 11.30 -8 -3 9 1.00 7.50 7 3 -9 166.68 13.50 -7 -3 9 137.69 13.00 -7 -3 9 178.08 18.70 -7 -3 9 149.19 12.60 6 3 -9 240.88 15.20 6 3 -9 223.18 15.60 6 3 -9 267.87 23.30 6 3 -9 227.78 18.90 -6 -3 9 241.88 22.40 -6 -3 9 220.58 17.60 -6 -3 9 271.37 20.90 -6 -3 9 251.47 16.10 5 3 -9 551.74 41.40 5 3 -9 625.54 37.30 5 3 -9 650.23 38.30 5 3 -9 665.83 42.60 -5 -3 9 622.94 40.00 -5 -3 9 583.34 40.20 -5 -3 9 650.03 43.20 -5 -3 9 594.44 40.50 -5 -3 9 575.24 39.50 4 3 -9 962.50 59.49 4 3 -9 855.21 60.59 4 3 -9 946.31 56.39 4 3 -9 1011.60 56.89 4 3 -9 971.00 58.19 -4 -3 9 842.22 53.59 -4 -3 9 1007.20 57.09 -4 -3 9 966.10 58.29 -4 -3 9 857.61 57.59 -4 -3 9 998.50 61.19 -4 -3 9 963.80 57.99 3 3 -9 81.49 7.50 3 3 -9 71.19 5.70 3 3 -9 75.09 10.30 3 3 -9 50.99 9.90 3 3 -9 83.09 6.40 -3 -3 9 71.99 12.00 -3 -3 9 55.39 8.50 -3 -3 9 63.09 13.40 2 3 -9 486.95 31.50 2 3 -9 502.95 30.20 2 3 -9 498.15 29.90 2 3 -9 419.76 32.10 -2 -3 9 496.95 31.60 -2 -3 9 536.85 30.40 -2 -3 9 458.75 33.20 -2 -3 9 390.66 30.30 -2 -3 9 412.36 30.90 1 3 -9 772.02 53.59 1 3 -9 881.31 52.99 1 3 -9 890.91 51.79 1 3 -9 868.91 53.29 -1 -3 9 883.11 52.79 -1 -3 9 850.21 53.59 -1 -3 9 874.11 51.69 -1 -3 9 874.31 54.59 -1 -3 9 768.32 51.79 0 3 -9 305.27 23.30 0 3 -9 329.27 21.40 0 3 -9 308.27 24.30 0 3 -9 315.27 21.90 0 3 -9 331.97 22.30 0 -3 9 321.57 21.70 0 -3 9 334.57 23.60 0 -3 9 298.07 21.50 0 -3 9 334.77 26.00 0 -3 9 364.56 25.50 -1 3 -9 369.26 23.10 -1 3 -9 339.97 25.40 -1 3 -9 381.66 22.80 -1 3 -9 337.77 23.50 -1 3 -9 348.97 25.50 1 -3 9 289.27 21.40 1 -3 9 332.27 28.10 1 -3 9 327.47 24.30 1 -3 9 375.86 26.30 1 -3 9 334.47 22.50 -2 3 -9 1531.75 93.89 -2 3 -9 1307.97 86.69 -2 3 -9 1502.45 89.59 -2 3 -9 1560.74 90.89 -2 3 -9 1642.94 90.39 2 -3 9 1419.46 86.99 2 -3 9 1563.14 91.29 2 -3 9 1572.54 89.49 2 -3 9 1461.35 89.69 2 -3 9 1688.03 95.99 2 -3 9 1551.14 90.09 -3 3 -9 233.28 21.00 -3 3 -9 240.08 21.50 -3 3 -9 293.67 19.20 -3 3 -9 311.37 22.70 3 -3 9 249.88 16.20 3 -3 9 299.17 21.70 3 -3 9 248.18 18.10 3 -3 9 289.47 18.90 -4 3 -9 64.19 9.80 -4 3 -9 80.49 8.40 -4 3 -9 114.79 9.90 4 -3 9 108.69 9.90 4 -3 9 91.79 8.90 -5 3 -9 81.39 13.80 -5 3 -9 55.49 11.60 5 -3 9 90.49 10.40 5 -3 9 76.39 9.10 -6 3 -9 9.10 12.40 -6 3 -9 -0.90 7.90 -6 3 -9 1.20 13.20 6 -3 9 5.50 7.80 6 -3 9 -4.20 8.20 6 -3 9 0.00 9.10 -7 3 -9 5.10 17.80 -7 3 -9 0.00 9.60 7 -3 9 2.40 10.90 7 -3 9 10.50 13.00 8 2 -9 7.00 14.80 -8 -2 9 24.80 10.40 -8 -2 9 19.50 7.80 7 2 -9 0.90 11.20 7 2 -9 10.00 8.10 7 2 -9 2.20 5.10 -7 -2 9 -0.60 10.50 -7 -2 9 2.40 7.60 -7 -2 9 -3.00 5.40 -7 -2 9 -7.10 15.70 6 2 -9 27.60 9.40 6 2 -9 14.90 4.60 6 2 -9 13.10 8.70 6 2 -9 8.70 11.00 6 2 -9 23.70 6.80 -6 -2 9 27.90 10.90 -6 -2 9 18.70 5.80 -6 -2 9 10.30 8.70 5 2 -9 17.10 5.10 5 2 -9 22.70 7.90 5 2 -9 17.80 4.90 5 2 -9 15.90 4.40 5 2 -9 26.40 9.20 -5 -2 9 32.70 7.10 -5 -2 9 22.30 4.70 -5 -2 9 25.30 7.50 -5 -2 9 25.50 4.70 -5 -2 9 22.50 10.20 4 2 -9 444.56 29.80 4 2 -9 422.76 28.10 4 2 -9 415.16 31.60 4 2 -9 456.05 27.70 4 2 -9 450.55 30.40 -4 -2 9 475.85 33.20 -4 -2 9 439.06 28.40 -4 -2 9 400.96 30.00 -4 -2 9 452.85 28.30 -4 -2 9 413.56 29.20 3 2 -9 66.99 7.20 3 2 -9 57.49 6.00 3 2 -9 69.59 9.60 3 2 -9 73.19 5.40 3 2 -9 70.49 8.90 -3 -2 9 68.29 6.20 -3 -2 9 76.69 9.70 -3 -2 9 58.79 11.10 -3 -2 9 68.99 9.60 -3 -2 9 67.99 7.10 2 2 -9 75.39 10.20 2 2 -9 79.69 8.60 2 2 -9 96.29 10.60 2 2 -9 77.29 6.30 2 2 -9 73.79 6.50 -2 -2 9 89.89 10.30 -2 -2 9 72.99 10.80 -2 -2 9 73.59 7.80 -2 -2 9 75.69 11.00 -2 -2 9 87.89 6.90 1 2 -9 62.79 9.30 1 2 -9 67.39 6.50 1 2 -9 76.99 7.20 1 2 -9 85.09 6.50 1 2 -9 73.89 10.10 -1 -2 9 63.89 6.40 -1 -2 9 67.79 9.50 -1 -2 9 57.79 9.90 -1 -2 9 60.69 9.60 -1 -2 9 51.59 6.70 0 2 -9 106.99 8.60 0 2 -9 88.49 8.80 0 2 -9 109.59 8.60 0 2 -9 89.29 11.60 0 2 -9 89.99 8.10 0 -2 9 81.69 11.40 0 -2 9 82.29 12.10 0 -2 9 90.69 8.10 0 -2 9 74.49 11.10 0 -2 9 84.39 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12.50 -6 2 -9 0.50 13.20 6 -2 9 2.00 7.80 6 -2 9 6.50 8.90 6 -2 9 16.00 8.70 -7 2 -9 9.00 12.50 -7 2 -9 9.20 10.50 7 -2 9 4.30 11.30 8 1 -9 5.30 15.20 -8 -1 9 10.40 11.80 -8 -1 9 6.40 6.60 7 1 -9 69.69 14.40 7 1 -9 68.49 9.30 7 1 -9 61.09 7.70 -7 -1 9 93.99 23.00 -7 -1 9 59.49 8.30 -7 -1 9 65.79 16.10 -7 -1 9 54.89 7.60 6 1 -9 54.49 9.80 6 1 -9 23.70 5.80 6 1 -9 35.40 5.20 -6 -1 9 47.20 5.70 -6 -1 9 41.00 5.60 -6 -1 9 28.70 5.20 -6 -1 9 46.40 12.00 -6 -1 9 43.70 9.10 5 1 -9 109.19 11.60 5 1 -9 115.29 9.20 5 1 -9 139.89 12.70 5 1 -9 117.99 12.70 5 1 -9 98.99 9.30 -5 -1 9 124.09 15.70 -5 -1 9 105.69 9.00 -5 -1 9 128.49 12.50 -5 -1 9 104.09 9.10 -5 -1 9 114.19 7.70 4 1 -9 516.95 32.90 4 1 -9 467.95 35.90 4 1 -9 454.35 30.40 4 1 -9 501.85 32.30 4 1 -9 489.35 32.10 -4 -1 9 489.55 33.50 -4 -1 9 510.55 35.30 -4 -1 9 500.65 34.80 -4 -1 9 509.85 31.00 -4 -1 9 486.55 32.00 3 1 -9 188.08 14.90 3 1 -9 176.48 15.10 3 1 -9 184.18 15.90 3 1 -9 207.08 15.00 3 1 -9 183.98 12.70 -3 -1 9 190.18 15.70 -3 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41.40 -2 -5 10 552.44 38.30 -2 -5 10 536.05 36.10 1 5 -10 36.30 5.50 1 5 -10 32.10 10.60 1 5 -10 29.90 10.10 1 5 -10 28.40 6.20 -1 -5 10 13.00 12.80 -1 -5 10 20.40 9.30 -1 -5 10 36.20 5.50 0 5 -10 35.90 11.10 0 -5 10 27.20 9.00 0 -5 10 32.10 5.80 -1 5 -10 437.46 32.50 -1 5 -10 502.35 29.90 -1 5 -10 488.65 31.30 -1 5 -10 490.05 33.20 1 -5 10 450.15 33.60 1 -5 10 477.05 36.80 1 -5 10 399.96 30.10 1 -5 10 403.86 27.60 1 -5 10 474.35 29.60 -2 5 -10 48.40 9.50 -2 5 -10 41.60 4.60 -2 5 -10 26.40 9.80 -2 5 -10 24.20 5.50 2 -5 10 41.60 7.80 2 -5 10 44.60 6.10 2 -5 10 46.50 13.50 2 -5 10 51.29 11.40 2 -5 10 28.30 3.70 -3 5 -10 33.00 4.10 -3 5 -10 30.10 6.40 -3 5 -10 23.40 6.40 -3 5 -10 34.50 10.40 -3 5 -10 21.90 6.30 -3 5 -10 57.29 10.90 3 -5 10 38.40 11.70 3 -5 10 31.40 5.90 3 -5 10 27.90 6.70 3 -5 10 31.00 4.30 3 -5 10 34.90 22.50 3 -5 10 46.60 10.70 -4 5 -10 46.80 7.90 -4 5 -10 38.80 10.30 -4 5 -10 60.09 7.50 -4 5 -10 56.79 12.60 4 -5 10 74.79 5.90 4 -5 10 58.89 9.90 4 -5 10 86.19 11.70 4 -5 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0 3 -17 -4.30 17.40 0 -3 17 0.30 10.10 0 -3 17 1.40 13.00 0 -3 17 1.50 11.00 2 2 -17 22.40 16.80 2 2 -17 1.80 17.10 2 2 -17 3.00 15.80 2 2 -17 16.40 15.80 -2 -2 17 2.90 13.80 1 2 -17 7.20 17.00 1 2 -17 3.10 15.80 1 2 -17 2.00 17.30 -1 -2 17 4.50 9.80 -1 -2 17 1.10 15.50 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 35545