data_5 _audit_creation_date 2019-07-03 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C19 H20 N2 O2 S' _chemical_formula_sum 'C19 H20 N2 O2 S' _chemical_formula_weight 340.43 _chemical_melting_point ? _chemical_oxdiff_formula 'C1 H1 O1 N1 S1' 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' _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 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6946(4) _cell_length_b 9.1589(4) _cell_length_c 18.4833(9) _cell_angle_alpha 90 _cell_angle_beta 99.212(4) _cell_angle_gamma 90 _cell_volume 1787.10(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2863 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.4140 _cell_measurement_theta_min 3.5130 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79963 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour white _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 720 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_unetI/netI 0.0438 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.884 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 12439 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.884 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.248 _diffrn_reflns_theta_min 3.504 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0233 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.884 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 21.00 61.00 1.00 3.50 -- 18.63 -99.00 120.00 40 2 \w -82.00 10.00 1.00 3.50 -- -18.94 -77.00-150.00 92 3 \w -28.00 -3.00 1.00 3.50 -- -18.94 -57.00 -30.00 25 4 \w -44.00 50.00 1.00 3.50 -- -18.94 77.00 -30.00 94 5 \w -86.00 10.00 1.00 3.50 -- -18.94 -19.00 30.00 96 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0574039000 _diffrn_orient_matrix_UB_12 -0.0376108000 _diffrn_orient_matrix_UB_13 0.0124405000 _diffrn_orient_matrix_UB_21 0.0171017000 _diffrn_orient_matrix_UB_22 0.0063342000 _diffrn_orient_matrix_UB_23 -0.0353817000 _diffrn_orient_matrix_UB_31 0.0303832000 _diffrn_orient_matrix_UB_32 0.0674509000 _diffrn_orient_matrix_UB_33 0.0102301000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2736 _reflns_number_total 4302 _reflns_odcompleteness_completeness 99.67 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _refine_diff_density_max 0.513 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 4302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0610 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.9385P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1444 _refine_ls_wR_factor_ref 0.1756 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Riding coordinates: N004(H004) 2.b Secondary CH2 refined with riding coordinates: C00H(H00H,H00I) 2.c Aromatic/amide H refined with riding coordinates: C00A(H00A), C00B(H00B), C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00J), C00J(H00K), C00K(H00L), C00L(H00M) 2.d Idealised Me refined as rotating group: C00N(H00N,H00O,H00P), C00O(H00Q,H00R,H00S) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _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 S001 S 0.79240(6) -0.02566(7) 0.51445(4) 0.0513(2) Uani 1 1 d . . . . . O002 O 0.68465(17) -0.1168(2) 0.51473(12) 0.0636(5) Uani 1 1 d . . . . . O003 O 0.91311(17) -0.0746(2) 0.55106(12) 0.0703(6) Uani 1 1 d . . . . . N004 N 0.8132(2) 0.0017(2) 0.42983(12) 0.0492(5) Uani 1 1 d . . . . . H004 H 0.8407 -0.0764 0.4119 0.059 Uiso 1 1 d R . . . . N005 N 0.8225(2) 0.5380(2) 0.35821(13) 0.0558(6) Uani 1 1 d . . . . . C006 C 0.7138(2) 0.0661(3) 0.37767(14) 0.0449(6) Uani 1 1 d . . . . . C007 C 0.7588(2) 0.1456(3) 0.54913(13) 0.0470(6) Uani 1 1 d . . . . . C008 C 0.8643(2) 0.4197(3) 0.32417(15) 0.0497(6) Uani 1 1 d . . . . . C009 C 0.7364(2) 0.1935(3) 0.34153(15) 0.0487(6) Uani 1 1 d . . . . . C00A C 0.8246(3) 0.6576(3) 0.31423(19) 0.0649(8) Uani 1 1 d . . . . . H00A H 0.8004 0.7516 0.3249 0.078 Uiso 1 1 calc R . . . . C00B C 0.6350(2) 0.1944(3) 0.54107(16) 0.0575(7) Uani 1 1 d . . . . . H00B H 0.5694 0.1367 0.5175 0.069 Uiso 1 1 calc R . . . . C00C C 0.5950(3) -0.0007(3) 0.36435(17) 0.0587(7) Uani 1 1 d . . . . . H00C H 0.5814 -0.0879 0.3876 0.070 Uiso 1 1 calc R . . . . C00D C 0.8560(3) 0.2326(3) 0.58326(16) 0.0626(8) Uani 1 1 d . . . . . H00D H 0.9396 0.2014 0.5877 0.075 Uiso 1 1 calc R . . . . C00E C 0.8927(3) 0.4674(3) 0.25887(16) 0.0602(7) Uani 1 1 d . . . . . H00E H 0.9237 0.4102 0.2241 0.072 Uiso 1 1 calc R . . . . C00F C 0.8673(3) 0.6164(4) 0.25311(18) 0.0686(8) Uani 1 1 d . . . . . H00F H 0.8781 0.6763 0.2140 0.082 Uiso 1 1 calc R . . . . C00G C 0.4977(3) 0.0629(4) 0.31657(18) 0.0674(8) Uani 1 1 d . . . . . H00G H 0.4174 0.0213 0.3097 0.081 Uiso 1 1 calc R . . . . C00H C 0.8648(2) 0.2691(3) 0.35517(18) 0.0611(8) Uani 1 1 d . . . . . H00H H 0.8936 0.2740 0.4076 0.073 Uiso 1 1 calc R . . . . H00I H 0.9251 0.2101 0.3340 0.073 Uiso 1 1 calc R . . . . C00I C 0.8279(4) 0.3654(4) 0.61057(17) 0.0760(10) Uani 1 1 d . . . . . H00J H 0.8937 0.4229 0.6341 0.091 Uiso 1 1 calc R . . . . C00J C 0.6098(3) 0.3284(4) 0.56808(19) 0.0742(9) Uani 1 1 d . . . . . H00K H 0.5265 0.3612 0.5620 0.089 Uiso 1 1 calc R . . . . C00K C 0.6373(3) 0.2496(4) 0.29177(19) 0.0724(9) Uani 1 1 d . . . . . H00L H 0.6510 0.3333 0.2656 0.087 Uiso 1 1 calc R . . . . C00L C 0.5191(3) 0.1855(4) 0.27976(19) 0.0761(9) Uani 1 1 d . . . . . H00M H 0.4543 0.2265 0.2464 0.091 Uiso 1 1 calc R . . . . C00M C 0.7056(4) 0.4169(4) 0.60444(18) 0.0727(9) Uani 1 1 d . . . . . C00N C 0.7826(4) 0.5393(5) 0.4295(2) 0.1027(14) Uani 1 1 d . . . . . H00N H 0.7390 0.4500 0.4364 0.154 Uiso 1 1 calc GR . . . . H00O H 0.7268 0.6205 0.4324 0.154 Uiso 1 1 calc GR . . . . H00P H 0.8555 0.5483 0.4670 0.154 Uiso 1 1 calc GR . . . . C00O C 0.6766(5) 0.5621(4) 0.6353(3) 0.1227(18) Uani 1 1 d . . . . . H00Q H 0.7089 0.5644 0.6869 0.184 Uiso 1 1 calc GR . . . . H00R H 0.5865 0.5767 0.6279 0.184 Uiso 1 1 calc GR . . . . H00S H 0.7156 0.6382 0.6111 0.184 Uiso 1 1 calc GR . . . . 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 S001 0.0394(3) 0.0476(4) 0.0673(5) 0.0151(3) 0.0101(3) 0.0038(3) O002 0.0531(11) 0.0488(11) 0.0913(15) 0.0120(10) 0.0191(10) -0.0081(9) O003 0.0458(11) 0.0766(14) 0.0877(15) 0.0380(12) 0.0086(10) 0.0162(10) N004 0.0468(12) 0.0405(11) 0.0619(13) 0.0031(10) 0.0134(10) 0.0113(9) N005 0.0529(13) 0.0542(14) 0.0616(14) 0.0022(11) 0.0128(11) 0.0013(11) C006 0.0410(13) 0.0415(13) 0.0523(14) -0.0083(11) 0.0079(11) 0.0049(10) C007 0.0408(13) 0.0539(15) 0.0458(13) 0.0068(11) 0.0052(11) -0.0047(11) C008 0.0401(13) 0.0467(14) 0.0604(16) 0.0052(12) 0.0023(12) 0.0006(11) C009 0.0420(13) 0.0409(13) 0.0613(15) 0.0018(12) 0.0023(12) 0.0026(11) C00A 0.0499(16) 0.0476(16) 0.095(2) 0.0104(16) 0.0041(16) 0.0019(13) C00B 0.0409(14) 0.0587(17) 0.0741(18) -0.0095(14) 0.0122(13) -0.0045(12) C00C 0.0524(16) 0.0520(16) 0.0713(18) -0.0103(14) 0.0087(14) -0.0112(13) C00D 0.0528(16) 0.0672(19) 0.0620(17) 0.0066(15) -0.0083(13) -0.0113(14) C00E 0.0581(17) 0.0647(18) 0.0578(17) 0.0016(14) 0.0097(14) -0.0022(14) C00F 0.0598(18) 0.072(2) 0.073(2) 0.0290(17) 0.0055(15) -0.0063(15) C00G 0.0459(16) 0.075(2) 0.077(2) -0.0232(17) -0.0029(15) -0.0095(14) C00H 0.0452(15) 0.0507(16) 0.085(2) 0.0161(15) 0.0044(14) 0.0025(12) C00I 0.087(2) 0.077(2) 0.0590(18) -0.0036(17) -0.0030(17) -0.029(2) C00J 0.0641(19) 0.069(2) 0.095(2) -0.0129(18) 0.0291(18) 0.0044(16) C00K 0.0545(18) 0.066(2) 0.089(2) 0.0164(17) -0.0110(16) 0.0008(15) C00L 0.0534(17) 0.079(2) 0.086(2) 0.0000(19) -0.0196(16) 0.0023(16) C00M 0.103(3) 0.0581(19) 0.0617(19) -0.0071(15) 0.0271(19) -0.0107(19) C00N 0.117(3) 0.113(3) 0.089(3) -0.002(2) 0.049(3) 0.008(3) C00O 0.187(5) 0.076(3) 0.117(3) -0.037(2) 0.060(4) -0.023(3) _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 S001 O002 1.4238(19) . ? S001 O003 1.4304(19) . ? S001 N004 1.634(2) . ? S001 C007 1.753(3) . ? N004 H004 0.8600 . ? N004 C006 1.442(3) . ? N005 C008 1.364(3) . ? N005 C00A 1.366(4) . ? N005 C00N 1.449(4) . ? C006 C009 1.385(3) . ? C006 C00C 1.396(4) . ? C007 C00B 1.383(3) . ? C007 C00D 1.380(4) . ? C008 C00E 1.363(4) . ? C008 C00H 1.493(4) . ? C009 C00H 1.522(4) . ? C009 C00K 1.386(4) . ? C00A H00A 0.9300 . ? C00A C00F 1.339(4) . ? C00B H00B 0.9300 . ? C00B C00J 1.367(4) . ? C00C H00C 0.9300 . ? C00C C00G 1.381(4) . ? C00D H00D 0.9300 . ? C00D C00I 1.369(5) . ? C00E H00E 0.9300 . ? C00E C00F 1.392(4) . ? C00F H00F 0.9300 . ? C00G H00G 0.9300 . ? C00G C00L 1.351(5) . ? C00H H00H 0.9700 . ? C00H H00I 0.9700 . ? C00I H00J 0.9300 . ? C00I C00M 1.377(5) . ? C00J H00K 0.9300 . ? C00J C00M 1.393(5) . ? C00K H00L 0.9300 . ? C00K C00L 1.380(4) . ? C00L H00M 0.9300 . ? C00M C00O 1.500(5) . ? C00N H00N 0.9600 . ? C00N H00O 0.9600 . ? C00N H00P 0.9600 . ? C00O H00Q 0.9600 . ? C00O H00R 0.9600 . ? C00O H00S 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 O002 S001 O003 118.95(12) . . ? O002 S001 N004 109.12(12) . . ? O002 S001 C007 108.06(11) . . ? O003 S001 N004 104.50(11) . . ? O003 S001 C007 109.27(13) . . ? N004 S001 C007 106.25(11) . . ? S001 N004 H004 110.4 . . ? C006 N004 S001 120.28(16) . . ? C006 N004 H004 110.1 . . ? C008 N005 C00A 109.0(2) . . ? C008 N005 C00N 126.3(3) . . ? C00A N005 C00N 124.8(3) . . ? C009 C006 N004 120.0(2) . . ? C009 C006 C00C 120.6(2) . . ? C00C C006 N004 119.4(2) . . ? C00B C007 S001 119.9(2) . . ? C00D C007 S001 120.0(2) . . ? C00D C007 C00B 120.1(3) . . ? N005 C008 C00H 122.6(2) . . ? C00E C008 N005 106.8(2) . . ? C00E C008 C00H 130.4(3) . . ? C006 C009 C00H 121.7(2) . . ? C006 C009 C00K 117.3(2) . . ? C00K C009 C00H 121.0(2) . . ? N005 C00A H00A 125.8 . . ? C00F C00A N005 108.5(3) . . ? C00F C00A H00A 125.8 . . ? C007 C00B H00B 120.3 . . ? C00J C00B C007 119.5(3) . . ? C00J C00B H00B 120.3 . . ? C006 C00C H00C 120.0 . . ? C00G C00C C006 119.9(3) . . ? C00G C00C H00C 120.0 . . ? C007 C00D H00D 120.4 . . ? C00I C00D C007 119.2(3) . . ? C00I C00D H00D 120.4 . . ? C008 C00E H00E 125.8 . . ? C008 C00E C00F 108.3(3) . . ? C00F C00E H00E 125.8 . . ? C00A C00F C00E 107.5(3) . . ? C00A C00F H00F 126.3 . . ? C00E C00F H00F 126.3 . . ? C00C C00G H00G 120.0 . . ? C00L C00G C00C 120.1(3) . . ? C00L C00G H00G 120.0 . . ? C008 C00H C009 114.1(2) . . ? C008 C00H H00H 108.7 . . ? C008 C00H H00I 108.7 . . ? C009 C00H H00H 108.7 . . ? C009 C00H H00I 108.7 . . ? H00H C00H H00I 107.6 . . ? C00D C00I H00J 118.8 . . ? C00D C00I C00M 122.4(3) . . ? C00M C00I H00J 118.8 . . ? C00B C00J H00K 119.1 . . ? C00B C00J C00M 121.7(3) . . ? C00M C00J H00K 119.1 . . ? C009 C00K H00L 118.9 . . ? C00L C00K C009 122.2(3) . . ? C00L C00K H00L 118.9 . . ? C00G C00L C00K 119.8(3) . . ? C00G C00L H00M 120.1 . . ? C00K C00L H00M 120.1 . . ? C00I C00M C00J 117.1(3) . . ? C00I C00M C00O 121.6(4) . . ? C00J C00M C00O 121.2(4) . . ? N005 C00N H00N 109.5 . . ? N005 C00N H00O 109.5 . . ? N005 C00N H00P 109.5 . . ? H00N C00N H00O 109.5 . . ? H00N C00N H00P 109.5 . . ? H00O C00N H00P 109.5 . . ? C00M C00O H00Q 109.5 . . ? C00M C00O H00R 109.5 . . ? C00M C00O H00S 109.5 . . ? H00Q C00O H00R 109.5 . . ? H00Q C00O H00S 109.5 . . ? H00R C00O H00S 109.5 . . ? _shelx_res_file ; 11-248.res created by SHELXL-2014/7 TITL 11-248_a.res in P2(1)/c REM Old TITL 11-248 in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.201, Rweak 0.338, Alpha 0.023, Orientation as input REM Formula found by SHELXT: C19 N2 O2 S CELL 0.71073 10.6946 9.1589 18.4833 90 99.212 90 ZERR 4 0.0004 0.0004 0.0009 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 76 80 8 8 4 L.S. 99 PLAN 5 BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.065000 0.938500 FVAR 0.63084 S001 5 0.792397 -0.025662 0.514455 11.00000 0.03937 0.04765 = 0.06728 0.01507 0.01009 0.00383 O002 4 0.684649 -0.116847 0.514725 11.00000 0.05312 0.04883 = 0.09130 0.01195 0.01912 -0.00809 O003 4 0.913110 -0.074642 0.551063 11.00000 0.04577 0.07663 = 0.08771 0.03795 0.00860 0.01624 N004 3 0.813156 0.001733 0.429826 11.00000 0.04683 0.04045 = 0.06192 0.00305 0.01341 0.01133 AFIX 3 H004 2 0.840676 -0.076387 0.411896 11.00000 -1.20000 AFIX 0 N005 3 0.822545 0.538047 0.358212 11.00000 0.05292 0.05416 = 0.06160 0.00223 0.01277 0.00127 C006 1 0.713766 0.066120 0.377666 11.00000 0.04103 0.04153 = 0.05235 -0.00835 0.00786 0.00488 C007 1 0.758766 0.145604 0.549133 11.00000 0.04080 0.05394 = 0.04576 0.00677 0.00520 -0.00471 C008 1 0.864338 0.419667 0.324169 11.00000 0.04014 0.04667 = 0.06036 0.00519 0.00235 0.00065 C009 1 0.736359 0.193541 0.341535 11.00000 0.04204 0.04087 = 0.06125 0.00176 0.00227 0.00257 C00A 1 0.824570 0.657564 0.314227 11.00000 0.04995 0.04760 = 0.09459 0.01037 0.00406 0.00193 AFIX 43 H00A 2 0.800352 0.751638 0.324919 11.00000 -1.20000 AFIX 0 C00B 1 0.634977 0.194444 0.541066 11.00000 0.04086 0.05868 = 0.07407 -0.00955 0.01218 -0.00448 AFIX 43 H00B 2 0.569369 0.136655 0.517451 11.00000 -1.20000 AFIX 0 C00C 1 0.595014 -0.000678 0.364347 11.00000 0.05242 0.05196 = 0.07131 -0.01031 0.00872 -0.01123 AFIX 43 H00C 2 0.581408 -0.087933 0.387620 11.00000 -1.20000 AFIX 0 C00D 1 0.856007 0.232603 0.583264 11.00000 0.05283 0.06722 = 0.06200 0.00665 -0.00832 -0.01131 AFIX 43 H00D 2 0.939627 0.201377 0.587655 11.00000 -1.20000 AFIX 0 C00E 1 0.892675 0.467401 0.258874 11.00000 0.05810 0.06469 = 0.05785 0.00157 0.00970 -0.00217 AFIX 43 H00E 2 0.923653 0.410231 0.224113 11.00000 -1.20000 AFIX 0 C00F 1 0.867320 0.616382 0.253109 11.00000 0.05977 0.07166 = 0.07270 0.02902 0.00553 -0.00635 AFIX 43 H00F 2 0.878099 0.676342 0.213970 11.00000 -1.20000 AFIX 0 C00G 1 0.497712 0.062921 0.316568 11.00000 0.04594 0.07470 = 0.07749 -0.02317 -0.00291 -0.00953 AFIX 43 H00G 2 0.417356 0.021319 0.309731 11.00000 -1.20000 AFIX 0 C00H 1 0.864774 0.269056 0.355174 11.00000 0.04520 0.05072 = 0.08533 0.01612 0.00435 0.00254 AFIX 23 H00H 2 0.893618 0.274031 0.407612 11.00000 -1.20000 H00I 2 0.925096 0.210111 0.334040 11.00000 -1.20000 AFIX 0 C00I 1 0.827890 0.365392 0.610572 11.00000 0.08700 0.07737 = 0.05895 -0.00359 -0.00299 -0.02911 AFIX 43 H00J 2 0.893721 0.422934 0.634133 11.00000 -1.20000 AFIX 0 C00J 1 0.609772 0.328365 0.568079 11.00000 0.06407 0.06913 = 0.09466 -0.01290 0.02910 0.00439 AFIX 43 H00K 2 0.526453 0.361175 0.562021 11.00000 -1.20000 AFIX 0 C00K 1 0.637324 0.249619 0.291772 11.00000 0.05451 0.06601 = 0.08931 0.01642 -0.01100 0.00082 AFIX 43 H00L 2 0.650995 0.333268 0.265605 11.00000 -1.20000 AFIX 0 C00L 1 0.519107 0.185464 0.279759 11.00000 0.05341 0.07885 = 0.08577 -0.00004 -0.01964 0.00234 AFIX 43 H00M 2 0.454297 0.226482 0.246400 11.00000 -1.20000 AFIX 0 C00M 1 0.705642 0.416932 0.604436 11.00000 0.10288 0.05812 = 0.06168 -0.00705 0.02711 -0.01070 C00N 1 0.782598 0.539300 0.429500 11.00000 0.11738 0.11281 = 0.08868 -0.00227 0.04913 0.00780 AFIX 137 H00N 2 0.739022 0.449966 0.436355 11.00000 -1.50000 H00O 2 0.726806 0.620454 0.432401 11.00000 -1.50000 H00P 2 0.855495 0.548312 0.466981 11.00000 -1.50000 AFIX 0 C00O 1 0.676556 0.562128 0.635346 11.00000 0.18670 0.07578 = 0.11741 -0.03737 0.05982 -0.02319 AFIX 137 H00Q 2 0.708926 0.564402 0.686868 11.00000 -1.50000 H00R 2 0.586517 0.576719 0.627900 11.00000 -1.50000 H00S 2 0.715603 0.638218 0.611059 11.00000 -1.50000 AFIX 0 HKLF 4 REM 11-248_a.res in P2(1)/c REM R1 = 0.0610 for 2736 Fo > 4sig(Fo) and 0.0996 for all 4302 data REM 219 parameters refined using 0 restraints END WGHT 0.0650 0.9404 REM Highest difference peak 0.513, deepest hole -0.531, 1-sigma level 0.052 Q1 1 0.9017 0.0395 0.4276 11.00000 0.05 0.51 Q2 1 0.9433 0.0146 0.5734 11.00000 0.05 0.29 Q3 1 0.8154 0.0394 0.5454 11.00000 0.05 0.24 Q4 1 0.6581 0.0454 0.3880 11.00000 0.05 0.18 Q5 1 0.6630 0.2965 0.2174 11.00000 0.05 0.18 ; _shelx_res_checksum 41301 _shelx_hkl_file ; 0 0 3 -0.18 0.25 0 0 3 -0.08 0.26 0 0 4 94.95 5.46 0 0 -4 86.56 4.12 0 0 -4 86.45 5.37 0 0 4 88.20 4.23 0 0 5 1.36 0.87 0 0 -5 3.11 1.00 0 0 5 4.52 1.25 0 0 -5 2.12 1.15 0 0 6 42.73 3.75 0 0 6 38.12 4.46 0 0 -6 27.35 3.75 0 0 -6 30.44 3.07 0 0 7 22.11 3.77 0 0 7 19.08 2.95 0 0 8 61.72 6.32 0 0 -8 60.69 4.85 0 0 8 62.26 5.15 0 0 9 0.89 1.03 0 0 9 0.80 1.47 0 0 10 146.86 10.83 0 0 10 148.12 9.09 0 0 11 -0.17 0.97 0 0 11 -0.41 2.02 0 0 12 16.54 3.38 0 0 12 10.27 3.46 0 0 13 1.25 1.77 0 0 13 -1.38 1.90 0 0 14 8.61 3.10 0 0 14 12.08 3.27 0 0 15 0.02 2.34 0 0 15 -1.38 1.36 0 0 16 60.38 9.00 0 0 16 50.97 7.07 0 0 17 1.81 2.00 0 0 17 1.57 1.67 0 0 18 3.01 2.01 0 0 18 1.35 1.62 0 0 19 0.36 1.29 0 0 19 1.86 1.86 0 0 20 -4.33 2.85 0 0 20 -0.49 1.60 0 0 21 2.47 2.34 0 0 21 -0.29 1.36 0 0 22 1.92 2.20 0 0 22 -1.02 2.11 0 0 23 1.76 2.14 0 0 24 -3.83 2.88 0 0 25 -3.30 2.78 0 1 3 5032.60 34.72 0 -1 3 5120.30 24.61 0 1 -3 5231.37 24.47 0 -1 -3 5134.70 35.37 0 -1 -3 4939.34 28.56 0 1 3 5075.24 26.68 0 -1 -4 3879.43 30.53 0 1 4 4027.88 34.02 0 1 4 3847.09 28.60 0 1 -4 3974.72 25.68 0 -1 4 4041.84 41.69 0 -1 -4 3978.01 33.92 0 -1 4 4041.01 24.85 0 1 5 1894.91 23.20 0 1 -5 1860.81 19.41 0 -1 5 1921.97 19.53 0 -1 -5 1942.93 25.72 0 1 5 1944.73 25.75 0 -1 5 1939.08 31.58 0 -1 -5 1852.87 24.54 0 -1 -6 2.14 0.88 0 -1 -6 2.93 1.17 0 -1 6 2.52 0.85 0 1 6 1.73 0.82 0 -1 6 1.47 0.92 0 1 -6 2.56 0.83 0 1 6 2.64 0.90 0 1 7 92.68 6.44 0 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4.16 0 2 5 84.87 6.12 0 2 -6 127.79 5.63 0 2 6 131.84 5.93 0 -2 6 138.38 5.79 0 -2 6 124.69 9.47 0 2 6 148.02 8.55 0 -2 -6 130.06 6.58 0 2 -7 6.40 1.37 0 -2 7 5.77 1.31 0 2 7 4.40 1.13 0 -2 7 4.31 0.99 0 -2 -7 6.69 1.66 0 2 7 3.58 1.26 0 -2 8 534.86 13.20 0 2 8 545.75 18.15 0 -2 8 517.95 21.53 0 2 -8 523.22 13.57 0 -2 -8 509.75 15.88 0 2 8 506.83 14.34 0 2 9 15.68 3.13 0 -2 9 10.33 2.96 0 -2 9 15.02 2.40 0 -2 -9 11.00 2.47 0 2 -9 13.37 2.32 0 2 9 15.63 2.72 0 2 10 4.42 1.87 0 2 10 6.14 1.89 0 -2 10 6.05 2.88 0 -2 10 3.96 1.32 0 -2 11 74.94 6.17 0 2 11 74.81 7.64 0 -2 11 81.72 9.69 0 2 11 79.53 6.97 0 2 12 34.54 5.48 0 -2 12 28.88 4.02 0 2 12 28.54 4.49 0 -2 12 39.20 7.10 0 2 13 29.77 5.24 0 -2 13 36.25 4.85 0 -2 13 34.71 6.79 0 2 13 35.28 5.14 0 2 14 0.98 1.28 0 2 14 5.36 2.71 0 -2 14 1.55 1.31 0 -2 14 2.71 2.32 0 -2 15 5.83 3.90 0 -2 15 3.32 1.64 0 2 15 2.55 1.44 0 2 15 2.19 1.70 0 2 16 98.50 9.89 0 -2 16 113.84 9.98 0 2 16 102.81 11.00 0 -2 16 125.47 14.15 0 2 17 15.21 4.39 0 -2 17 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6.71 -12 -3 8 17.32 5.25 12 -3 -8 23.24 5.65 12 -3 -7 15.95 4.99 -12 3 7 9.95 4.18 -12 -3 7 4.12 2.06 12 -3 -7 21.16 5.57 -12 -3 6 9.49 5.07 -12 3 6 1.96 2.18 12 -3 -6 3.08 2.30 -12 -3 5 1.64 2.33 12 -3 -5 1.61 1.85 12 -3 -4 -1.76 1.88 -12 -3 4 -5.62 3.87 12 -3 -3 24.91 5.99 -12 -3 3 19.37 6.68 12 -3 -2 0.88 1.28 -12 -3 2 1.62 2.33 12 -3 -1 31.88 6.82 -12 -3 1 33.94 8.62 12 -3 0 -2.41 2.10 12 3 0 0.91 2.12 -12 -3 0 2.47 2.65 12 -3 1 19.74 5.34 12 3 1 14.42 4.51 -12 -3 -1 12.68 5.19 12 -3 2 0.04 1.66 12 3 2 3.01 2.22 -12 -3 -2 -3.72 3.35 12 -3 3 24.34 6.23 12 3 3 18.45 5.41 12 -3 4 0.72 1.42 12 3 4 2.39 2.87 12 -3 5 33.31 7.18 12 3 5 24.06 6.35 12 3 6 0.68 1.69 12 3 7 11.37 4.93 12 -4 -13 -1.54 2.67 -12 -4 13 2.98 2.77 12 -4 -12 3.97 3.14 -12 -4 12 5.18 3.20 12 -4 -11 19.57 5.66 -12 -4 11 11.46 4.51 12 -4 -10 25.59 6.58 -12 -4 10 23.93 6.25 12 -4 -9 19.98 5.89 -12 -4 9 15.74 5.05 12 -4 -8 19.78 5.80 -12 -4 8 13.27 4.50 12 -4 -7 -0.20 1.23 -12 -4 7 -3.58 2.49 12 -4 -6 16.85 5.06 -12 -4 6 4.86 3.52 -12 -4 6 8.26 3.48 12 -4 -5 0.17 1.60 12 -4 -5 0.30 1.17 -12 -4 4 15.10 6.18 12 -4 -4 19.37 5.53 -12 -4 3 8.43 4.62 12 -4 -3 -0.27 1.47 12 -4 -2 24.68 6.13 -12 -4 2 22.29 7.24 12 -4 -1 1.03 1.31 -12 -4 1 -0.53 1.85 12 -4 0 30.44 6.90 -12 -4 0 15.65 6.33 12 -4 1 -2.52 2.25 -12 -4 -1 -1.55 2.45 12 -4 2 27.10 6.66 12 4 2 40.82 8.13 -12 -4 -2 38.00 9.78 12 -4 3 3.01 2.58 12 4 3 4.00 2.78 -12 -4 -3 5.34 3.97 12 -4 4 15.03 5.11 12 4 4 15.91 5.17 12 4 5 2.37 2.23 12 4 6 9.70 4.69 12 4 7 -1.08 1.64 12 -5 -13 -0.12 1.33 12 -5 -12 3.83 3.34 -12 -5 12 2.68 2.39 12 -5 -11 12.80 5.05 -12 -5 11 17.13 5.43 12 -5 -10 13.88 5.14 -12 -5 10 7.15 3.76 12 -5 -9 10.55 4.58 -12 -5 9 10.23 4.03 12 -5 -8 -1.12 1.84 -12 -5 8 4.88 2.87 12 -5 -7 3.54 2.59 12 -5 -6 8.66 3.64 12 -5 -5 25.77 6.72 -12 -5 5 25.44 7.74 12 -5 -4 -2.24 2.20 -12 -5 4 0.36 1.85 12 -5 -4 1.86 2.14 12 -5 -3 12.26 4.85 -12 -5 3 14.51 6.21 12 -5 -3 18.72 5.61 -12 -5 2 1.11 2.93 12 -5 -2 3.45 2.60 -12 -5 1 41.50 10.39 12 -5 -1 32.19 7.31 12 -5 0 -1.99 2.27 -12 -5 0 1.24 2.09 12 -5 1 8.69 4.32 12 5 5 6.36 3.58 12 5 6 -4.59 3.29 12 6 -9 4.98 3.25 -13 0 12 -1.72 2.16 -13 0 11 4.58 3.37 -13 0 10 7.63 4.07 -13 0 9 5.22 3.65 -13 0 8 -1.22 1.96 -13 0 7 3.25 2.87 -13 0 6 -4.66 3.40 -13 0 5 -4.08 3.36 -13 0 4 -4.93 3.52 13 0 -3 3.06 2.15 -13 0 3 -2.47 2.56 13 0 -2 3.58 2.04 -13 0 2 11.05 5.12 13 0 -1 -1.87 1.76 -13 0 1 -0.77 1.91 13 0 0 15.58 4.76 13 0 1 -5.95 3.07 13 0 2 3.67 2.50 13 0 3 0.08 1.08 13 0 4 0.73 1.64 13 0 5 1.76 2.33 -13 1 13 10.48 4.82 -13 1 12 -3.03 2.76 -13 1 11 -0.61 1.60 -13 -1 11 -8.43 4.16 -13 -1 10 5.02 4.50 -13 1 10 -0.07 0.92 -13 -1 9 0.46 1.58 -13 1 9 5.02 3.35 -13 -1 8 -0.01 1.30 -13 1 8 -3.13 2.71 -13 -1 7 7.46 4.29 -13 1 7 6.10 4.34 -13 -1 6 5.06 3.63 -13 1 6 2.82 2.62 13 -1 -5 3.15 2.21 -13 -1 5 -3.73 3.20 -13 1 5 6.20 3.79 -13 -1 4 -2.64 2.65 -13 1 4 -0.26 1.09 13 -1 -3 -0.39 1.17 -13 -1 3 4.16 3.46 -13 1 3 -2.84 2.73 13 -1 -2 1.33 1.56 13 1 -2 1.89 1.19 -13 -1 2 -0.55 2.09 13 -1 -1 -1.15 1.66 13 1 -1 2.95 2.15 -13 -1 1 -0.36 2.97 13 -1 0 7.94 3.64 13 1 0 10.55 4.09 -13 -1 0 1.36 1.72 13 -1 1 8.20 3.63 13 1 1 5.20 3.20 13 -1 2 5.47 3.02 13 1 2 1.02 1.66 13 -1 3 4.92 3.12 13 1 3 -2.12 2.18 13 -1 4 5.76 3.23 13 1 4 7.41 3.68 13 1 5 2.39 2.30 -13 -2 11 0.59 1.72 -13 2 10 11.38 5.10 -13 -2 10 -1.25 1.86 -13 -2 9 -0.01 1.41 -13 2 9 -3.64 2.80 -13 -2 8 0.78 1.77 -13 2 8 1.40 1.89 13 -2 -7 4.49 2.51 -13 -2 7 3.99 4.03 -13 2 7 5.53 3.80 13 -2 -6 2.40 1.75 -13 -2 6 0.75 1.74 -13 2 6 -1.72 2.11 13 -2 -5 2.00 1.96 -13 -2 5 5.02 3.75 -13 2 5 5.12 3.31 13 -2 -4 -2.42 1.98 -13 -2 4 -0.87 2.03 13 -2 -3 2.43 2.09 -13 -2 3 -1.92 2.45 13 -2 -2 2.71 2.50 -13 -2 2 3.78 3.08 13 -2 -1 -1.67 1.89 -13 -2 1 4.85 2.83 13 -2 0 5.17 3.03 -13 -2 0 0.19 2.44 13 -2 1 1.20 1.77 13 2 1 3.15 2.49 13 -2 2 9.59 4.11 13 2 2 6.71 3.08 13 -2 3 1.56 1.26 13 2 3 -0.10 1.13 13 2 4 -3.15 2.65 13 2 5 17.59 5.63 -13 -3 11 1.47 2.02 13 -3 -10 4.16 2.63 -13 -3 10 -0.53 1.50 -13 -3 9 -10.29 4.35 13 -3 -8 2.88 2.21 13 -3 -7 3.84 2.55 -13 3 7 6.42 4.31 13 -3 -6 2.20 2.05 13 -3 -5 1.95 1.92 -13 -3 5 5.88 4.17 13 -3 -4 5.53 3.21 -13 -3 4 5.96 4.04 13 -3 -3 4.45 2.98 13 -3 -2 1.29 1.64 13 -3 -1 15.16 4.86 13 -3 0 -3.79 2.65 13 -3 1 4.25 2.45 13 3 3 16.38 5.47 13 3 4 9.50 4.11 13 3 5 3.93 2.97 13 -4 -12 -1.75 2.02 13 -4 -11 14.14 5.01 13 -4 -10 2.67 2.39 -13 -4 10 10.47 4.11 13 -4 -9 0.91 1.59 -13 -4 9 -2.63 2.29 13 -4 -8 7.80 3.85 -13 -4 8 2.66 1.86 13 -4 -8 3.14 2.38 13 -4 -7 1.58 1.61 13 -4 -7 0.88 1.32 13 -4 -6 1.87 1.98 13 -4 -5 3.89 2.92 13 -4 -4 9.70 4.09 13 -4 -3 12.12 4.41 13 -4 -2 -0.11 1.22 13 -4 -1 4.74 3.10 13 4 5 0.52 1.43 14 0 -1 -3.63 2.50 14 0 0 19.86 5.71 14 0 1 1.74 2.47 14 0 2 23.68 6.42 -14 1 10 2.25 2.63 -14 1 9 7.21 4.53 -14 1 8 0.32 1.42 -14 1 7 13.70 6.00 -14 1 6 2.25 1.63 -14 1 5 -4.38 3.34 -14 1 4 4.60 3.43 14 -1 -3 -1.13 1.54 14 -1 -2 0.91 1.34 14 -1 -1 9.13 3.90 14 -1 0 3.12 2.38 14 -1 1 18.31 5.84 14 1 1 12.10 4.81 14 1 2 9.41 4.39 -14 2 8 14.05 5.77 -14 2 7 -0.24 1.10 -14 2 6 24.42 7.36 14 -2 -4 5.05 2.87 14 -2 -3 -1.57 1.74 14 -2 -2 4.04 2.64 14 -2 -1 -0.26 1.76 14 -3 -6 0.71 1.41 14 -3 -5 13.70 4.88 14 -3 -4 0.02 1.30 TITL 11-248 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 10.694595 9.158862 18.483281 90.0000 99.2122 90.0000 ZERR 25.00 0.000413 0.000367 0.000896 0.0000 0.0044 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O S UNIT 25.00 25.00 25.00 25.00 25.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 43544 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.336 _oxdiff_exptl_absorpt_empirical_full_min 0.731