data_erj21 _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 H13 N O2 S' _chemical_formula_weight 283.33 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system tetragonal _space_group_IT_number 78 _space_group_name_H-M_alt 'P 43' _space_group_name_Hall 'P 4cw' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 10.7582(6) _cell_length_b 10.7582(6) _cell_length_c 11.4283(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1322.70(17) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9949 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 28.45 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_density_meas not_measured _exptl_crystal_density_method not_measured _exptl_crystal_density_diffrn 1.423 _exptl_crystal_F_000 592 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.196 _exptl_crystal_size_min 0.182 _exptl_absorpt_coefficient_mu 0.245 _shelx_estimated_absorpt_T_min 0.941 _shelx_estimated_absorpt_T_max 0.957 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9257 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Bruker SADABS 2014/4' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15344 _diffrn_reflns_av_unetI/netI 0.0213 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.893 _diffrn_reflns_theta_max 28.656 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.945 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 3225 _reflns_number_gt 3084 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.862 _reflns_Friedel_fraction_max 0.920 _reflns_Friedel_fraction_full 1.000 _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 'Bruker APEX2 2014.9-0, 2014' _computing_cell_refinement 'Bruker SAINT 8.34a, 2013' _computing_data_reduction 'Bruker SAINT 8.34a, 2013' _computing_structure_solution 'Bruker SHELXTL 2013/1' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; A colorless crystal of approximate dimensions 0.250 x 0.196 x 0.182 mm was mounted on a glass fiber and transferred to a Bruker SMART APEX II diffractometer. The APEX2 program package was used to determine the unit-cell parameters and for data collection (60 sec/frame scan time for a sphere of diffraction data). The raw frame data was processed using SAINT and SADABS to yield the reflection data file. Subsequent calculations were carried out using the SHELXTL program. The diffraction symmetry was 4/m and the systematic absences were consistent with the tetragonal space group P43 that was later determined to be correct. The structure was solved by direct methods and refined on F2 by full-matrix least-squares techniques. The analytical scattering factors for neutral atoms were used throughout the analysis. Hydrogen atoms were located from a difference-Fourier map and refined (x,y,z and Uiso). At convergence, wR2 = 0.0661 and Goof = 1.065 for 233 variables refined against 3225 data (0.74 Å), R1 = 0.0269 for those 3084 data with I > 2.0sigma(I). The absolute structure was assigned by refinement of the Flack parameter. ; _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^)+(0.0389P)^2^+0.2374P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 1398 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.04(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 3225 _refine_ls_number_parameters 233 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.79023(4) 0.42937(4) 0.14431(4) 0.01307(12) Uani 1 1 d . . . . . O1 O 0.75845(16) 0.55011(14) 0.09780(14) 0.0213(3) Uani 1 1 d . . . . . O2 O 0.84576(15) 0.43125(14) 0.25869(13) 0.0197(3) Uani 1 1 d . . . . . N1 N 0.67129(16) 0.33495(15) 0.13866(17) 0.0152(3) Uani 1 1 d . . . . . C1 C 0.87713(18) 0.34689(18) 0.03965(17) 0.0133(4) Uani 1 1 d . . . . . C2 C 0.99476(19) 0.37791(19) -0.00261(18) 0.0153(4) Uani 1 1 d . . . . . C3 C 1.04651(19) 0.3013(2) -0.08783(18) 0.0177(4) Uani 1 1 d . . . . . C4 C 0.9807(2) 0.1980(2) -0.12834(18) 0.0183(4) Uani 1 1 d . . . . . C5 C 0.8630(2) 0.16914(19) -0.08587(18) 0.0172(4) Uani 1 1 d . . . . . C6 C 0.81037(18) 0.24526(18) -0.00040(17) 0.0136(4) Uani 1 1 d . . . . . C7 C 0.68335(18) 0.22798(18) 0.05700(17) 0.0133(4) Uani 1 1 d . . . . . C8 C 0.68217(19) 0.10458(19) 0.12767(19) 0.0157(4) Uani 1 1 d . . . . . C9 C 0.7837(2) 0.09858(18) 0.21344(19) 0.0162(4) Uani 1 1 d . . . . . C10 C 0.8653(2) 0.0950(2) 0.2833(2) 0.0203(4) Uani 1 1 d . . . . . C11 C 0.57768(18) 0.2333(2) -0.03404(18) 0.0145(4) Uani 1 1 d . . . . . C12 C 0.47427(19) 0.15528(19) -0.02804(18) 0.0162(4) Uani 1 1 d . . . . . C13 C 0.37897(19) 0.1650(2) -0.1105(2) 0.0195(4) Uani 1 1 d . . . . . C14 C 0.3859(2) 0.2518(2) -0.20019(19) 0.0215(5) Uani 1 1 d . . . . . C15 C 0.4885(2) 0.3302(2) -0.2060(2) 0.0244(5) Uani 1 1 d . . . . . C16 C 0.5830(2) 0.3214(2) -0.1232(2) 0.0210(4) Uani 1 1 d . . . . . H1 H 0.644(3) 0.320(2) 0.203(3) 0.020(7) Uiso 1 1 d . . . . . H2 H 1.039(2) 0.446(2) 0.021(2) 0.014(6) Uiso 1 1 d . . . . . H3 H 1.129(3) 0.321(2) -0.119(3) 0.022(7) Uiso 1 1 d . . . . . H4 H 1.017(3) 0.147(3) -0.185(3) 0.034(8) Uiso 1 1 d . . . . . H5 H 0.822(3) 0.101(3) -0.112(3) 0.034(8) Uiso 1 1 d . . . . . H8A H 0.608(2) 0.096(2) 0.170(2) 0.011(6) Uiso 1 1 d . . . . . H8B H 0.685(2) 0.032(2) 0.071(2) 0.013(6) Uiso 1 1 d . . . . . H10 H 0.931(3) 0.091(3) 0.336(3) 0.046(9) Uiso 1 1 d . . . . . H13 H 0.315(3) 0.115(3) -0.108(3) 0.024(7) Uiso 1 1 d . . . . . H14 H 0.325(3) 0.259(3) -0.254(3) 0.023(7) Uiso 1 1 d . . . . . H15 H 0.500(3) 0.389(3) -0.264(3) 0.042(9) Uiso 1 1 d . . . . . H16 H 0.651(3) 0.378(3) -0.125(2) 0.022(7) Uiso 1 1 d . . . . . H12 H 0.468(2) 0.097(3) 0.027(3) 0.020(6) Uiso 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 S1 0.0158(2) 0.0120(2) 0.0115(2) -0.00016(18) 0.00031(18) 0.00057(18) O1 0.0300(9) 0.0142(7) 0.0196(7) 0.0024(6) 0.0040(6) 0.0049(6) O2 0.0223(8) 0.0225(7) 0.0144(7) -0.0015(6) -0.0026(6) -0.0018(6) N1 0.0153(8) 0.0159(8) 0.0143(8) -0.0016(7) 0.0026(7) -0.0009(6) C1 0.0153(9) 0.0135(9) 0.0110(8) 0.0003(7) -0.0006(7) 0.0027(7) C2 0.0136(9) 0.0160(9) 0.0163(9) 0.0023(8) -0.0026(7) -0.0013(8) C3 0.0122(9) 0.0231(10) 0.0177(12) 0.0043(8) 0.0010(8) 0.0027(7) C4 0.0193(10) 0.0195(10) 0.0162(10) -0.0003(8) 0.0011(8) 0.0063(8) C5 0.0200(10) 0.0161(9) 0.0154(10) -0.0008(8) -0.0004(8) 0.0017(8) C6 0.0132(9) 0.0144(9) 0.0131(9) 0.0016(7) -0.0005(7) 0.0011(7) C7 0.0126(9) 0.0148(9) 0.0126(9) -0.0005(7) 0.0008(7) -0.0001(7) C8 0.0151(9) 0.0151(9) 0.0170(10) 0.0018(8) 0.0002(8) -0.0024(7) C9 0.0181(10) 0.0128(9) 0.0178(10) 0.0013(7) 0.0023(8) -0.0009(8) C10 0.0225(10) 0.0195(10) 0.0187(10) 0.0016(8) -0.0025(9) -0.0011(8) C11 0.0130(9) 0.0170(9) 0.0134(9) -0.0023(7) 0.0019(7) 0.0015(7) C12 0.0167(9) 0.0180(10) 0.0140(10) -0.0003(8) 0.0016(7) -0.0003(8) C13 0.0133(9) 0.0251(11) 0.0201(10) -0.0043(9) 0.0010(9) -0.0014(8) C14 0.0162(10) 0.0325(12) 0.0159(10) -0.0017(9) -0.0027(8) 0.0063(9) C15 0.0216(10) 0.0303(12) 0.0213(11) 0.0089(9) -0.0004(9) 0.0030(9) C16 0.0167(9) 0.0239(10) 0.0223(11) 0.0063(9) 0.0010(8) -0.0012(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 1.4373(16) . ? S1 O1 1.4446(15) . ? S1 N1 1.6351(17) . ? S1 C1 1.758(2) . ? N1 C7 1.487(3) . ? N1 H1 0.81(3) . ? C1 C6 1.386(3) . ? C1 C2 1.395(3) . ? C2 C3 1.392(3) . ? C2 H2 0.91(3) . ? C3 C4 1.396(3) . ? C3 H3 0.98(3) . ? C4 C5 1.391(3) . ? C4 H4 0.94(3) . ? C5 C6 1.395(3) . ? C5 H5 0.90(3) . ? C6 C7 1.527(3) . ? C7 C11 1.542(3) . ? C7 C8 1.554(3) . ? C8 C9 1.469(3) . ? C8 H8A 0.94(2) . ? C8 H8B 1.01(3) . ? C9 C10 1.187(3) . ? C10 H10 0.93(4) . ? C11 C16 1.393(3) . ? C11 C12 1.395(3) . ? C12 C13 1.397(3) . ? C12 H12 0.89(3) . ? C13 C14 1.388(3) . ? C13 H13 0.87(3) . ? C14 C15 1.391(3) . ? C14 H14 0.90(3) . ? C15 C16 1.392(3) . ? C15 H15 0.92(4) . ? C16 H16 0.95(3) . ? 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 114.86(10) . . ? O2 S1 N1 111.71(10) . . ? O1 S1 N1 111.03(10) . . ? O2 S1 C1 113.88(9) . . ? O1 S1 C1 109.23(9) . . ? N1 S1 C1 94.34(9) . . ? C7 N1 S1 115.92(13) . . ? C7 N1 H1 116.9(19) . . ? S1 N1 H1 112(2) . . ? C6 C1 C2 122.99(19) . . ? C6 C1 S1 110.32(15) . . ? C2 C1 S1 126.66(16) . . ? C3 C2 C1 117.60(19) . . ? C3 C2 H2 118.0(16) . . ? C1 C2 H2 124.4(16) . . ? C2 C3 C4 120.00(19) . . ? C2 C3 H3 119.5(16) . . ? C4 C3 H3 120.5(16) . . ? C5 C4 C3 121.6(2) . . ? C5 C4 H4 119.2(19) . . ? C3 C4 H4 119.2(19) . . ? C4 C5 C6 118.9(2) . . ? C4 C5 H5 121(2) . . ? C6 C5 H5 120(2) . . ? C1 C6 C5 118.95(18) . . ? C1 C6 C7 114.70(17) . . ? C5 C6 C7 126.34(18) . . ? N1 C7 C6 104.68(15) . . ? N1 C7 C11 109.29(16) . . ? C6 C7 C11 111.43(16) . . ? N1 C7 C8 109.52(16) . . ? C6 C7 C8 109.54(16) . . ? C11 C7 C8 112.11(16) . . ? C9 C8 C7 112.23(17) . . ? C9 C8 H8A 106.2(15) . . ? C7 C8 H8A 111.0(14) . . ? C9 C8 H8B 111.6(14) . . ? C7 C8 H8B 109.0(14) . . ? H8A C8 H8B 106.7(19) . . ? C10 C9 C8 179.2(2) . . ? C9 C10 H10 178(2) . . ? C16 C11 C12 118.56(19) . . ? C16 C11 C7 119.24(18) . . ? C12 C11 C7 122.16(19) . . ? C11 C12 C13 120.5(2) . . ? C11 C12 H12 121.3(17) . . ? C13 C12 H12 118.2(17) . . ? C14 C13 C12 120.6(2) . . ? C14 C13 H13 119(2) . . ? C12 C13 H13 120(2) . . ? C13 C14 C15 119.1(2) . . ? C13 C14 H14 121.6(18) . . ? C15 C14 H14 119.3(18) . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15 124(2) . . ? C16 C15 H15 116(2) . . ? C15 C16 C11 120.9(2) . . ? C15 C16 H16 120.1(16) . . ? C11 C16 H16 119.0(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 N1 C7 -117.33(15) . . . . ? O1 S1 N1 C7 113.04(15) . . . . ? C1 S1 N1 C7 0.52(16) . . . . ? O2 S1 C1 C6 116.77(15) . . . . ? O1 S1 C1 C6 -113.34(15) . . . . ? N1 S1 C1 C6 0.71(16) . . . . ? O2 S1 C1 C2 -65.2(2) . . . . ? O1 S1 C1 C2 64.6(2) . . . . ? N1 S1 C1 C2 178.70(19) . . . . ? C6 C1 C2 C3 -0.8(3) . . . . ? S1 C1 C2 C3 -178.56(16) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C2 C3 C4 C5 0.2(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C2 C1 C6 C5 0.8(3) . . . . ? S1 C1 C6 C5 178.84(15) . . . . ? C2 C1 C6 C7 -179.80(18) . . . . ? S1 C1 C6 C7 -1.7(2) . . . . ? C4 C5 C6 C1 -0.2(3) . . . . ? C4 C5 C6 C7 -179.56(19) . . . . ? S1 N1 C7 C6 -1.5(2) . . . . ? S1 N1 C7 C11 -120.91(16) . . . . ? S1 N1 C7 C8 115.92(16) . . . . ? C1 C6 C7 N1 2.0(2) . . . . ? C5 C6 C7 N1 -178.63(19) . . . . ? C1 C6 C7 C11 120.00(19) . . . . ? C5 C6 C7 C11 -60.6(3) . . . . ? C1 C6 C7 C8 -115.36(19) . . . . ? C5 C6 C7 C8 64.0(3) . . . . ? N1 C7 C8 C9 -59.2(2) . . . . ? C6 C7 C8 C9 55.0(2) . . . . ? C11 C7 C8 C9 179.28(17) . . . . ? N1 C7 C11 C16 74.1(2) . . . . ? C6 C7 C11 C16 -41.1(2) . . . . ? C8 C7 C11 C16 -164.25(19) . . . . ? N1 C7 C11 C12 -103.7(2) . . . . ? C6 C7 C11 C12 141.10(19) . . . . ? C8 C7 C11 C12 17.9(3) . . . . ? C16 C11 C12 C13 0.6(3) . . . . ? C7 C11 C12 C13 178.41(19) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? C12 C13 C14 C15 -0.8(3) . . . . ? C13 C14 C15 C16 0.2(3) . . . . ? C14 C15 C16 C11 0.8(4) . . . . ? C12 C11 C16 C15 -1.2(3) . . . . ? C7 C11 C16 C15 -179.1(2) . . . . ? _refine_diff_density_max 0.306 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.042 _shelx_res_file ; erj21.res created by SHELXL-2014/7 TITL erj21 in P4(3) CELL 0.71073 10.75820 10.75820 11.42830 90.0000 90.0000 90.0000 ZERR 4.00 0.00060 0.00060 0.00070 0.0000 0.0000 0.0000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM -Y, X, 0.75+Z SYMM Y, -X, 0.25+Z SFAC C H N O S UNIT 64 52 4 8 4 TEMP -140.000 SIZE 0.182 0.196 0.25 rem APEX2_2014.9-0, SAINT 8.34a, SADABS 2014/4, SHELXTL 2014/7 L.S. 12 ACTA 51 CONF BOND $H FMAP 2 PLAN 6 WGHT 0.038900 0.237400 FVAR 0.19975 S1 5 0.790235 0.429372 0.144314 11.00000 0.01580 0.01197 = 0.01145 -0.00016 0.00031 0.00057 O1 4 0.758448 0.550113 0.097801 11.00000 0.02998 0.01421 = 0.01961 0.00243 0.00404 0.00492 O2 4 0.845761 0.431249 0.258692 11.00000 0.02231 0.02248 = 0.01440 -0.00147 -0.00255 -0.00183 N1 3 0.671288 0.334946 0.138664 11.00000 0.01530 0.01593 = 0.01427 -0.00158 0.00257 -0.00090 C1 1 0.877132 0.346893 0.039648 11.00000 0.01532 0.01347 = 0.01102 0.00028 -0.00055 0.00271 C2 1 0.994761 0.377914 -0.002609 11.00000 0.01355 0.01600 = 0.01630 0.00227 -0.00258 -0.00135 C3 1 1.046514 0.301283 -0.087833 11.00000 0.01216 0.02311 = 0.01771 0.00428 0.00102 0.00271 C4 1 0.980671 0.198047 -0.128338 11.00000 0.01925 0.01949 = 0.01615 -0.00034 0.00108 0.00626 C5 1 0.863025 0.169136 -0.085875 11.00000 0.01999 0.01611 = 0.01539 -0.00080 -0.00039 0.00173 C6 1 0.810375 0.245264 -0.000399 11.00000 0.01324 0.01443 = 0.01305 0.00156 -0.00054 0.00108 C7 1 0.683350 0.227982 0.056995 11.00000 0.01257 0.01482 = 0.01259 -0.00054 0.00077 -0.00009 C8 1 0.682174 0.104576 0.127670 11.00000 0.01509 0.01512 = 0.01703 0.00176 0.00017 -0.00240 C9 1 0.783671 0.098583 0.213439 11.00000 0.01805 0.01284 = 0.01781 0.00131 0.00227 -0.00087 C10 1 0.865255 0.095033 0.283270 11.00000 0.02251 0.01951 = 0.01875 0.00156 -0.00250 -0.00111 C11 1 0.577683 0.233297 -0.034040 11.00000 0.01297 0.01702 = 0.01344 -0.00227 0.00188 0.00154 C12 1 0.474275 0.155282 -0.028044 11.00000 0.01671 0.01801 = 0.01401 -0.00028 0.00160 -0.00030 C13 1 0.378973 0.164996 -0.110540 11.00000 0.01330 0.02514 = 0.02008 -0.00430 0.00102 -0.00144 C14 1 0.385888 0.251784 -0.200187 11.00000 0.01617 0.03254 = 0.01593 -0.00169 -0.00266 0.00627 C15 1 0.488498 0.330240 -0.206044 11.00000 0.02160 0.03028 = 0.02125 0.00891 -0.00043 0.00295 C16 1 0.583015 0.321417 -0.123213 11.00000 0.01669 0.02395 = 0.02234 0.00626 0.00098 -0.00124 H1 2 0.643580 0.320451 0.202853 11.00000 0.02039 H2 2 1.039171 0.445937 0.020710 11.00000 0.01432 H3 2 1.128868 0.320704 -0.119154 11.00000 0.02242 H4 2 1.016675 0.146831 -0.185197 11.00000 0.03415 H5 2 0.821763 0.101356 -0.111535 11.00000 0.03359 H8A 2 0.608189 0.096294 0.170481 11.00000 0.01125 H8B 2 0.685249 0.032021 0.071112 11.00000 0.01349 H10 2 0.931348 0.091251 0.336213 11.00000 0.04608 H13 2 0.315310 0.115026 -0.107598 11.00000 0.02372 H14 2 0.324948 0.259399 -0.253871 11.00000 0.02264 H15 2 0.499836 0.389404 -0.263514 11.00000 0.04247 H16 2 0.650772 0.378214 -0.125035 11.00000 0.02235 H12 2 0.467881 0.097242 0.026899 11.00000 0.02008 HKLF 4 REM erj21 in P4(3) REM R1 = 0.0269 for 3084 Fo > 4sig(Fo) and 0.0295 for all 3225 data REM 233 parameters refined using 1 restraints END WGHT 0.0387 0.2397 REM Highest difference peak 0.306, deepest hole -0.185, 1-sigma level 0.042 Q1 1 0.8461 0.3918 0.0907 11.00000 0.05 0.31 Q2 1 0.7242 0.3833 0.1466 11.00000 0.05 0.29 Q3 1 0.8456 0.4043 0.1940 11.00000 0.05 0.28 Q4 1 0.8148 0.4581 0.2091 11.00000 0.05 0.25 Q5 1 0.6188 0.2383 0.0135 11.00000 0.05 0.25 Q6 1 0.7464 0.4909 0.1405 11.00000 0.05 0.24 ; _shelx_res_checksum 76107 _shelx_hkl_file ; -1 0 0 44.84 0.86 0 1 0 45.35 0.86 0 -1 0 44.97 0.87 1 0 0 45.86 0.87 0 -1 0 46.02 0.86 1 0 0 44.98 0.85 -1 1 0 62.47 1.17 -1 -1 0 60.18 1.17 1 -1 0 58.24 1.15 1 1 0 59.80 1.16 -1 -1 0 63.78 1.15 1 -1 0 61.81 1.17 -1 -1 0 61.69 1.17 -2 -1 0 278.23 4.98 1 -2 0 260.26 4.93 -2 -1 0 263.64 4.94 -1 2 0 268.34 4.98 1 -2 0 272.57 4.99 2 1 0 271.85 4.98 -2 -1 0 263.80 4.98 1 -2 0 265.72 4.96 -2 0 0 159.04 3.00 0 -2 0 161.54 3.00 0 2 0 163.44 3.00 0 -2 0 159.17 3.00 2 0 0 157.14 2.97 2 0 0 160.46 3.00 -1 -2 0 8.00 0.21 -2 1 0 7.53 0.23 1 2 0 7.71 0.19 2 -1 0 8.17 0.23 1 2 0 7.67 0.22 -1 -2 0 7.88 0.24 2 -1 0 7.42 0.21 -2 -2 0 351.46 6.22 -2 2 0 344.80 6.27 2 2 0 333.42 6.24 -2 -2 0 335.81 6.27 2 -2 0 330.14 6.24 -2 -2 0 326.11 6.26 2 -2 0 338.25 6.27 -3 -2 0 85.05 1.74 -3 -2 0 90.78 1.74 2 -3 0 87.81 1.69 -3 -2 0 88.86 1.67 2 -3 0 88.46 1.76 -2 3 0 86.91 1.71 3 2 0 89.33 1.73 -2 3 0 88.39 1.75 -3 -1 0 33.89 0.69 -3 -1 0 31.85 0.70 3 1 0 32.81 0.71 3 1 0 31.04 0.64 1 -3 0 31.51 0.69 -1 3 0 31.74 0.70 1 -3 0 32.42 0.71 3 0 0 41.56 0.84 -3 0 0 41.94 0.89 0 -3 0 43.38 0.88 0 3 0 43.40 0.89 3 0 0 41.64 0.89 0 -3 0 41.39 0.89 3 -1 0 130.98 2.45 -1 -3 0 125.70 2.47 -1 -3 0 129.51 2.44 1 3 0 126.46 2.45 2 3 0 32.12 0.68 2 3 0 32.37 0.72 -2 -3 0 34.35 0.69 3 -2 0 31.64 0.72 3 -2 0 31.60 0.70 -3 2 0 32.08 0.73 -2 -3 0 31.96 0.73 -3 3 0 25.72 0.62 -3 -3 0 26.06 0.55 3 -3 0 25.85 0.63 -3 -3 0 25.94 0.63 3 -3 0 24.67 0.57 -3 -3 0 24.35 0.61 3 3 0 24.99 0.58 -4 -3 0 4.11 0.16 -4 -3 0 3.86 0.23 -3 4 0 3.63 0.19 -3 4 0 4.31 0.24 3 -4 0 3.97 0.18 -4 -3 0 4.36 0.24 4 3 0 3.91 0.21 3 -4 0 4.20 0.25 4 2 0 186.52 3.59 2 -4 0 191.74 3.59 4 2 0 194.11 3.68 -2 4 0 192.81 3.68 2 -4 0 195.86 3.70 -4 -2 0 187.43 3.68 -4 -2 0 200.04 3.67 2 -4 0 191.23 3.65 4 1 0 61.06 1.22 4 1 0 62.98 1.30 -1 4 0 62.01 1.29 -4 -1 0 66.11 1.27 1 -4 0 61.86 1.30 -4 -1 0 60.82 1.29 1 -4 0 62.31 1.29 0 -4 0 32.82 0.77 4 0 0 34.27 0.78 -4 0 0 33.18 0.77 0 -4 0 34.30 0.77 0 4 0 34.27 0.77 4 0 0 35.15 0.73 4 -1 0 11.03 0.35 1 4 0 10.86 0.34 -4 1 0 10.96 0.35 4 -1 0 11.74 0.34 -1 -4 0 11.24 0.33 -1 -4 0 11.22 0.37 4 -2 0 63.97 1.31 4 -2 0 60.60 1.30 -2 -4 0 65.63 1.28 -2 -4 0 62.11 1.33 2 4 0 62.11 1.31 2 4 0 63.51 1.24 -4 2 0 62.27 1.32 3 4 0 16.61 0.48 -3 -4 0 17.06 0.42 -3 -4 0 17.20 0.50 3 4 0 16.71 0.43 4 -3 0 16.99 0.49 -4 3 0 16.75 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