data_22dub_vj04 _audit_creation_date 2022-04-29 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _shelx_SHELXL_version_number '2018/3' loop_ _audit_author_name _audit_author_email _audit_author_address 'Josef, V.' nena.josef@fau.de ; OC1-Dube DCP ; 'FH, ' '' ; OC-Operators DCP ; _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 'C18 H13 N O S' _chemical_formula_sum 'C18 H13 N O S' _chemical_formula_weight 291.35 _chemical_melting_point ? _chemical_oxdiff_formula 'C18 H13 N O S' _chemical_oxdiff_usercomment VJ32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 '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/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.7326(2) _cell_length_b 8.0758(2) _cell_length_c 25.2164(6) _cell_angle_alpha 90 _cell_angle_beta 94.539(2) _cell_angle_gamma 90 _cell_volume 1366.74(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3244 _cell_measurement_temperature 152.9(8) _cell_measurement_theta_max 71.6550 _cell_measurement_theta_min 5.7350 _shelx_estimated_absorpt_T_max 0.760 _shelx_estimated_absorpt_T_min 0.670 _exptl_absorpt_coefficient_mu 2.070 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear dark red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 608 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -3 1 13 0.0840 -4 0 -2 0.0807 2 -1 -14 0.0534 4 0 8 0.0834 0 1 16 0.0930 -2 4 3 0.1159 -4 -2 4 0.0537 0 -5 -1 0.0575 4 2 -4 0.0865 3 3 -3 0.0859 -4 3 -4 0.1006 -4 -1 10 0.0793 0 -3 13 0.0675 4 -2 2 0.0718 3 2 -12 0.0754 0 3 -12 0.1049 1 5 6 0.0822 _exptl_crystal_recrystallization_method 'The material was recrystallised from a mixture of n-heptane and DCM by solvent layering' _exptl_crystal_size_max 0.206 _exptl_crystal_size_mid 0.176 _exptl_crystal_size_min 0.141 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -2.7458 1.0755 13.0519 -0.6004 0.1451 0.7864 -4.2444 0.4229 -2.3890 0.4033 -0.0949 0.9101 2.1979 -1.0751 -14.3476 0.7107 -0.1713 -0.6823 3.6405 -0.0386 7.9502 -0.6941 0.1648 -0.7007 -0.1677 0.9068 16.1101 -0.9402 0.2254 0.2554 -2.4471 4.2573 3.3980 -0.3084 -0.6449 0.6993 -3.9736 -2.0386 3.5744 0.2250 0.4762 0.8501 -0.4347 -5.2108 -0.6917 0.4290 0.9009 -0.0660 4.0819 1.6792 -3.7619 -0.1974 -0.4186 -0.8865 3.3344 3.3462 -2.6444 -0.3214 -0.6779 -0.6612 -3.5407 2.6321 -3.8804 0.2832 -0.5237 0.8035 -3.5342 -0.9745 10.1411 -0.2422 0.4420 0.8637 -0.1358 -3.2408 12.8537 -0.4761 0.8750 0.0880 3.8883 -2.2164 1.6382 -0.2127 0.3945 -0.8939 2.9385 1.6675 -11.7672 0.3263 -0.5971 -0.7328 -0.2760 3.3324 -12.4705 0.4778 -0.8784 0.0091 0.6307 4.8514 5.5451 -0.6860 -0.7242 0.0707 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_unetI/netI 0.0198 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.938 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 4106 _diffrn_reflns_point_group_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.938 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.544 _diffrn_reflns_theta_min 3.517 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 152.9(8) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.6144 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.938 _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 -115.00 -15.00 1.00 1.03 -- -42.69 -57.00 0.00 100 2 \w 12.00 70.00 1.00 1.03 -- 42.69 -99.00-150.00 58 3 \w 116.00 176.00 1.00 4.14 -- 102.49 125.00-120.00 60 4 \w 107.00 176.00 1.00 4.14 -- 102.49 77.00 -60.00 69 5 \w 98.00 167.00 1.00 4.14 -- 102.49 125.00 90.00 69 6 \w 103.00 164.00 1.00 4.14 -- 102.49 77.00 0.00 61 7 \w 35.00 113.00 1.00 4.14 -- 102.49-125.00 -60.00 78 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0708312000 _diffrn_orient_matrix_UB_12 -0.0690903000 _diffrn_orient_matrix_UB_13 -0.0552091000 _diffrn_orient_matrix_UB_21 -0.0084994000 _diffrn_orient_matrix_UB_22 -0.1753375000 _diffrn_orient_matrix_UB_23 0.0237738000 _diffrn_orient_matrix_UB_31 -0.2182269000 _diffrn_orient_matrix_UB_32 0.0292973000 _diffrn_orient_matrix_UB_33 0.0119302000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2342 _reflns_number_total 2494 _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 1.171.41.93a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _refine_diff_density_max 0.316 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.048 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 191 _refine_ls_number_reflns 2494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0355 _refine_ls_restrained_S_all 1.062 _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^)+(0.0509P)^2^+0.7069P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.0970 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: N22(H22), C1(H1), C14(H14), C15(H15), C16(H16), C17(H17), C24(H24), C25(H25), C26(H26), C27(H27) 2.b Idealised Me refined as rotating group: C30(H30A,H30B,H30C) ; _atom_sites_solution_hydrogens geom _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 S12 S 0.24030(6) 0.66057(5) 0.48412(2) 0.02820(15) Uani 1 1 d . . . . . O20 O 0.69234(17) 0.73160(16) 0.58707(5) 0.0303(3) Uani 1 1 d . . . . . N22 N 0.5285(2) 0.56370(17) 0.66568(5) 0.0245(3) Uani 1 1 d . . . . . H22 H 0.620695 0.623551 0.651890 0.029 Uiso 1 1 calc R U . . . C1 C 0.2811(2) 0.5605(2) 0.58633(6) 0.0243(3) Uani 1 1 d . . . . . H1 H 0.150585 0.522532 0.575498 0.029 Uiso 1 1 calc R U . . . C11 C 0.3706(2) 0.6428(2) 0.54782(6) 0.0236(3) Uani 1 1 d . . . . . C13 C 0.4366(2) 0.7697(2) 0.45889(6) 0.0248(3) Uani 1 1 d . . . . . C14 C 0.4406(3) 0.8282(2) 0.40710(7) 0.0290(4) Uani 1 1 d . . . . . H14 H 0.331514 0.810182 0.381491 0.035 Uiso 1 1 calc R U . . . C15 C 0.6085(3) 0.9136(2) 0.39393(7) 0.0302(4) Uani 1 1 d . . . . . H15 H 0.613887 0.954700 0.358769 0.036 Uiso 1 1 calc R U . . . C16 C 0.7700(3) 0.9406(2) 0.43129(7) 0.0302(4) Uani 1 1 d . . . . . H16 H 0.883236 1.000004 0.421459 0.036 Uiso 1 1 calc R U . . . C17 C 0.7650(2) 0.8809(2) 0.48250(7) 0.0278(4) Uani 1 1 d . . . . . H17 H 0.874673 0.898149 0.507969 0.033 Uiso 1 1 calc R U . . . C18 C 0.5974(2) 0.7950(2) 0.49638(6) 0.0237(3) Uani 1 1 d . . . . . C19 C 0.5699(2) 0.7239(2) 0.54906(6) 0.0241(3) Uani 1 1 d . . . . . C21 C 0.3458(2) 0.5204(2) 0.63998(6) 0.0238(3) Uani 1 1 d . . . . . C23 C 0.5419(2) 0.4984(2) 0.71582(6) 0.0242(3) Uani 1 1 d . . . . . C24 C 0.6965(2) 0.5084(2) 0.75645(7) 0.0272(4) Uani 1 1 d . . . . . H24 H 0.815158 0.568568 0.751868 0.033 Uiso 1 1 calc R U . . . C25 C 0.6684(3) 0.4268(2) 0.80331(7) 0.0292(4) Uani 1 1 d . . . . . H25 H 0.771522 0.429407 0.831286 0.035 Uiso 1 1 calc R U . . . C26 C 0.4918(3) 0.3396(2) 0.81102(7) 0.0300(4) Uani 1 1 d . . . . . H26 H 0.478149 0.285690 0.844010 0.036 Uiso 1 1 calc R U . . . C27 C 0.3383(3) 0.3313(2) 0.77150(7) 0.0284(4) Uani 1 1 d . . . . . H27 H 0.218949 0.273220 0.777046 0.034 Uiso 1 1 calc R U . . . C28 C 0.3627(2) 0.4111(2) 0.72262(6) 0.0247(3) Uani 1 1 d . . . . . C29 C 0.2393(2) 0.4266(2) 0.67445(6) 0.0250(3) Uani 1 1 d . . . . . C30 C 0.0368(3) 0.3520(2) 0.66309(7) 0.0316(4) Uani 1 1 d . . . . . H30A H -0.050863 0.431997 0.643660 0.047 Uiso 1 1 calc R U . . . H30B H -0.018616 0.323162 0.696678 0.047 Uiso 1 1 calc R U . . . H30C H 0.047306 0.251888 0.641513 0.047 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S12 0.0248(2) 0.0331(3) 0.0256(2) 0.00062(15) -0.00471(15) -0.00330(15) O20 0.0274(6) 0.0364(7) 0.0264(6) -0.0018(5) -0.0019(5) -0.0065(5) N22 0.0218(7) 0.0278(7) 0.0235(7) 0.0003(5) -0.0007(5) -0.0031(5) C1 0.0205(8) 0.0255(8) 0.0263(8) -0.0040(6) -0.0013(6) -0.0005(6) C11 0.0236(8) 0.0223(8) 0.0240(7) -0.0035(6) -0.0035(6) 0.0014(6) C13 0.0232(8) 0.0234(8) 0.0272(8) -0.0022(6) -0.0011(6) 0.0023(6) C14 0.0286(9) 0.0310(9) 0.0264(8) -0.0003(7) -0.0047(6) 0.0025(7) C15 0.0341(9) 0.0310(9) 0.0252(8) 0.0031(7) 0.0010(7) 0.0029(7) C16 0.0277(9) 0.0315(9) 0.0317(9) -0.0006(7) 0.0036(7) -0.0020(7) C17 0.0248(8) 0.0300(9) 0.0282(8) -0.0032(7) -0.0013(6) -0.0005(7) C18 0.0247(8) 0.0219(8) 0.0241(8) -0.0037(6) -0.0005(6) 0.0026(6) C19 0.0266(8) 0.0204(8) 0.0256(8) -0.0033(6) 0.0039(6) 0.0022(6) C21 0.0210(8) 0.0247(8) 0.0253(8) -0.0038(6) -0.0007(6) 0.0000(6) C23 0.0256(8) 0.0228(8) 0.0242(7) -0.0014(6) 0.0012(6) 0.0010(6) C24 0.0264(8) 0.0268(9) 0.0278(8) -0.0025(7) -0.0017(6) 0.0000(7) C25 0.0340(9) 0.0260(9) 0.0265(8) -0.0024(7) -0.0043(7) 0.0023(7) C26 0.0385(10) 0.0267(9) 0.0247(8) 0.0009(6) 0.0027(7) 0.0018(7) C27 0.0307(9) 0.0268(9) 0.0280(8) -0.0007(7) 0.0042(7) -0.0014(7) C28 0.0256(8) 0.0226(8) 0.0259(8) -0.0028(6) 0.0019(6) 0.0009(6) C29 0.0229(8) 0.0254(8) 0.0266(8) -0.0040(6) 0.0017(6) 0.0001(6) C30 0.0254(9) 0.0388(10) 0.0307(9) -0.0035(7) 0.0018(7) -0.0064(7) _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 S12 C11 1.7739(16) . ? S12 C13 1.7494(17) . ? O20 C19 1.215(2) . ? N22 H22 0.8800 . ? N22 C21 1.389(2) . ? N22 C23 1.366(2) . ? C1 H1 0.9500 . ? C1 C11 1.356(2) . ? C1 C21 1.426(2) . ? C11 C19 1.492(2) . ? C13 C14 1.391(2) . ? C13 C18 1.395(2) . ? C14 H14 0.9500 . ? C14 C15 1.387(3) . ? C15 H15 0.9500 . ? C15 C16 1.398(2) . ? C16 H16 0.9500 . ? C16 C17 1.381(2) . ? C17 H17 0.9500 . ? C17 C18 1.392(2) . ? C18 C19 1.472(2) . ? C21 C29 1.394(2) . ? C23 C24 1.404(2) . ? C23 C28 1.419(2) . ? C24 H24 0.9500 . ? C24 C25 1.379(2) . ? C25 H25 0.9500 . ? C25 C26 1.408(3) . ? C26 H26 0.9500 . ? C26 C27 1.379(2) . ? C27 H27 0.9500 . ? C27 C28 1.412(2) . ? C28 C29 1.422(2) . ? C29 C30 1.497(2) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 S12 C11 92.10(8) . . ? C21 N22 H22 125.5 . . ? C23 N22 H22 125.5 . . ? C23 N22 C21 109.02(14) . . ? C11 C1 H1 113.9 . . ? C11 C1 C21 132.15(15) . . ? C21 C1 H1 113.9 . . ? C1 C11 S12 118.16(12) . . ? C1 C11 C19 130.55(15) . . ? C19 C11 S12 111.29(12) . . ? C14 C13 S12 125.74(13) . . ? C14 C13 C18 120.96(16) . . ? C18 C13 S12 113.30(12) . . ? C13 C14 H14 121.0 . . ? C15 C14 C13 118.08(16) . . ? C15 C14 H14 121.0 . . ? C14 C15 H15 119.3 . . ? C14 C15 C16 121.42(16) . . ? C16 C15 H15 119.3 . . ? C15 C16 H16 120.0 . . ? C17 C16 C15 120.00(16) . . ? C17 C16 H16 120.0 . . ? C16 C17 H17 120.4 . . ? C16 C17 C18 119.29(15) . . ? C18 C17 H17 120.4 . . ? C13 C18 C19 114.09(15) . . ? C17 C18 C13 120.25(15) . . ? C17 C18 C19 125.67(15) . . ? O20 C19 C11 126.29(15) . . ? O20 C19 C18 124.48(15) . . ? C18 C19 C11 109.23(14) . . ? N22 C21 C1 125.34(15) . . ? N22 C21 C29 109.05(14) . . ? C29 C21 C1 125.58(15) . . ? N22 C23 C24 130.11(15) . . ? N22 C23 C28 108.00(14) . . ? C24 C23 C28 121.90(15) . . ? C23 C24 H24 121.5 . . ? C25 C24 C23 117.00(16) . . ? C25 C24 H24 121.5 . . ? C24 C25 H25 118.9 . . ? C24 C25 C26 122.11(16) . . ? C26 C25 H25 118.9 . . ? C25 C26 H26 119.4 . . ? C27 C26 C25 121.15(16) . . ? C27 C26 H26 119.4 . . ? C26 C27 H27 120.8 . . ? C26 C27 C28 118.42(16) . . ? C28 C27 H27 120.8 . . ? C23 C28 C29 107.33(14) . . ? C27 C28 C23 119.41(15) . . ? C27 C28 C29 133.26(16) . . ? C21 C29 C28 106.61(14) . . ? C21 C29 C30 127.24(15) . . ? C28 C29 C30 126.13(15) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 S12 C11 C19 O20 -179.92(14) . . . . ? S12 C11 C19 C18 0.10(16) . . . . ? S12 C13 C14 C15 179.56(13) . . . . ? S12 C13 C18 C17 -179.64(13) . . . . ? S12 C13 C18 C19 0.52(18) . . . . ? N22 C21 C29 C28 -0.58(18) . . . . ? N22 C21 C29 C30 -179.08(16) . . . . ? N22 C23 C24 C25 -179.11(17) . . . . ? N22 C23 C28 C27 -179.97(14) . . . . ? N22 C23 C28 C29 -0.20(18) . . . . ? C1 C11 C19 O20 -0.6(3) . . . . ? C1 C11 C19 C18 179.44(17) . . . . ? C1 C21 C29 C28 177.33(15) . . . . ? C1 C21 C29 C30 -1.2(3) . . . . ? C11 S12 C13 C14 179.57(16) . . . . ? C11 S12 C13 C18 -0.38(13) . . . . ? C11 C1 C21 N22 1.0(3) . . . . ? C11 C1 C21 C29 -176.53(17) . . . . ? C13 S12 C11 C1 -179.28(14) . . . . ? C13 S12 C11 C19 0.15(12) . . . . ? C13 C14 C15 C16 0.1(3) . . . . ? C13 C18 C19 O20 179.63(15) . . . . ? C13 C18 C19 C11 -0.39(19) . . . . ? C14 C13 C18 C17 0.4(2) . . . . ? C14 C13 C18 C19 -179.43(15) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? C15 C16 C17 C18 -0.4(3) . . . . ? C16 C17 C18 C13 0.1(2) . . . . ? C16 C17 C18 C19 179.89(16) . . . . ? C17 C18 C19 O20 -0.2(3) . . . . ? C17 C18 C19 C11 179.77(16) . . . . ? C18 C13 C14 C15 -0.5(3) . . . . ? C21 N22 C23 C24 -179.99(16) . . . . ? C21 N22 C23 C28 -0.16(18) . . . . ? C21 C1 C11 S12 177.74(15) . . . . ? C21 C1 C11 C19 -1.6(3) . . . . ? C23 N22 C21 C1 -177.45(15) . . . . ? C23 N22 C21 C29 0.47(19) . . . . ? C23 C24 C25 C26 -1.2(2) . . . . ? C23 C28 C29 C21 0.47(18) . . . . ? C23 C28 C29 C30 179.00(16) . . . . ? C24 C23 C28 C27 -0.1(2) . . . . ? C24 C23 C28 C29 179.65(15) . . . . ? C24 C25 C26 C27 0.4(3) . . . . ? C25 C26 C27 C28 0.6(3) . . . . ? C26 C27 C28 C23 -0.7(2) . . . . ? C26 C27 C28 C29 179.58(17) . . . . ? C27 C28 C29 C21 -179.80(18) . . . . ? C27 C28 C29 C30 -1.3(3) . . . . ? C28 C23 C24 C25 1.1(2) . . . . ? _shelx_res_file ; TITL 22dub_vj04_auto_a.res in P2(1)/n 22dub_vj04.res created by SHELXL-2018/3 at 15:24:18 on 29-Apr-2022 REM Old TITL 22Dub_VJ04_auto in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.090, Rweak 0.093, Alpha 0.023, Orientation as input REM Formula found by SHELXT: C15 N O S CELL 1.54184 6.7326 8.0758 25.2164 90 94.539 90 ZERR 4 0.0002 0.0002 0.0006 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O S UNIT 72 52 4 4 4 L.S. 10 PLAN 10 SIZE 0.14 0.18 0.21 TEMP -120 CONF MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.050900 0.706900 FVAR 0.87491 S12 5 0.240302 0.660572 0.484125 11.00000 0.02481 0.03309 = 0.02561 0.00062 -0.00471 -0.00330 O20 4 0.692339 0.731597 0.587070 11.00000 0.02743 0.03641 = 0.02645 -0.00185 -0.00191 -0.00650 N22 3 0.528452 0.563701 0.665681 11.00000 0.02177 0.02779 = 0.02351 0.00025 -0.00066 -0.00306 AFIX 43 H22 2 0.620695 0.623551 0.651890 11.00000 -1.20000 AFIX 0 C1 1 0.281063 0.560538 0.586328 11.00000 0.02050 0.02554 = 0.02634 -0.00398 -0.00131 -0.00051 AFIX 43 H1 2 0.150585 0.522532 0.575498 11.00000 -1.20000 AFIX 0 C11 1 0.370591 0.642760 0.547817 11.00000 0.02364 0.02230 = 0.02398 -0.00347 -0.00345 0.00137 C13 1 0.436566 0.769673 0.458886 11.00000 0.02321 0.02335 = 0.02720 -0.00225 -0.00111 0.00232 C14 1 0.440609 0.828206 0.407096 11.00000 0.02863 0.03098 = 0.02637 -0.00026 -0.00465 0.00255 AFIX 43 H14 2 0.331514 0.810182 0.381491 11.00000 -1.20000 AFIX 0 C15 1 0.608493 0.913624 0.393928 11.00000 0.03414 0.03095 = 0.02521 0.00307 0.00102 0.00292 AFIX 43 H15 2 0.613887 0.954700 0.358769 11.00000 -1.20000 AFIX 0 C16 1 0.770027 0.940597 0.431293 11.00000 0.02766 0.03148 = 0.03166 -0.00059 0.00359 -0.00197 AFIX 43 H16 2 0.883236 1.000004 0.421459 11.00000 -1.20000 AFIX 0 C17 1 0.764969 0.880862 0.482496 11.00000 0.02475 0.02998 = 0.02816 -0.00315 -0.00133 -0.00051 AFIX 43 H17 2 0.874673 0.898149 0.507969 11.00000 -1.20000 AFIX 0 C18 1 0.597383 0.795048 0.496377 11.00000 0.02470 0.02191 = 0.02414 -0.00368 -0.00050 0.00258 C19 1 0.569936 0.723934 0.549062 11.00000 0.02656 0.02041 = 0.02560 -0.00328 0.00389 0.00218 C21 1 0.345782 0.520383 0.639984 11.00000 0.02098 0.02472 = 0.02525 -0.00380 -0.00067 0.00003 C23 1 0.541872 0.498428 0.715818 11.00000 0.02558 0.02276 = 0.02415 -0.00135 0.00116 0.00101 C24 1 0.696514 0.508352 0.756451 11.00000 0.02641 0.02680 = 0.02780 -0.00247 -0.00169 -0.00004 AFIX 43 H24 2 0.815158 0.568568 0.751868 11.00000 -1.20000 AFIX 0 C25 1 0.668425 0.426766 0.803307 11.00000 0.03398 0.02601 = 0.02651 -0.00243 -0.00431 0.00232 AFIX 43 H25 2 0.771522 0.429407 0.831286 11.00000 -1.20000 AFIX 0 C26 1 0.491795 0.339643 0.811018 11.00000 0.03850 0.02674 = 0.02472 0.00094 0.00269 0.00182 AFIX 43 H26 2 0.478149 0.285690 0.844010 11.00000 -1.20000 AFIX 0 C27 1 0.338269 0.331282 0.771504 11.00000 0.03071 0.02682 = 0.02804 -0.00071 0.00424 -0.00145 AFIX 43 H27 2 0.218949 0.273220 0.777046 11.00000 -1.20000 AFIX 0 C28 1 0.362695 0.411088 0.722619 11.00000 0.02560 0.02263 = 0.02589 -0.00276 0.00186 0.00090 C29 1 0.239280 0.426571 0.674448 11.00000 0.02291 0.02538 = 0.02661 -0.00404 0.00168 0.00012 C30 1 0.036788 0.351960 0.663094 11.00000 0.02536 0.03879 = 0.03069 -0.00347 0.00177 -0.00637 AFIX 137 H30A 2 -0.050863 0.431997 0.643660 11.00000 -1.50000 H30B 2 -0.018616 0.323162 0.696678 11.00000 -1.50000 H30C 2 0.047306 0.251888 0.641513 11.00000 -1.50000 AFIX 0 HKLF 4 REM 22dub_vj04_auto_a.res in P2(1)/n REM wR2 = 0.0970, GooF = S = 1.062, Restrained GooF = 1.062 for all data REM R1 = 0.0355 for 2342 Fo > 4sig(Fo) and 0.0371 for all 2494 data REM 191 parameters refined using 0 restraints END WGHT 0.0509 0.7069 REM Highest difference peak 0.316, deepest hole -0.238, 1-sigma level 0.048 Q1 1 -0.0021 0.3376 0.6258 11.00000 0.05 0.32 Q2 1 0.0350 0.2357 0.6741 11.00000 0.05 0.24 Q3 1 0.5815 0.7591 0.5255 11.00000 0.05 0.22 Q4 1 0.4391 0.5401 0.6503 11.00000 0.05 0.20 Q5 1 0.4619 0.6772 0.5524 11.00000 0.05 0.20 Q6 1 0.3631 0.5754 0.5620 11.00000 0.05 0.20 Q7 1 0.4557 0.4443 0.7195 11.00000 0.05 0.19 Q8 1 0.1281 0.5880 0.4726 11.00000 0.05 0.19 Q9 1 0.1654 0.5450 0.4703 11.00000 0.05 0.18 Q10 1 -0.0605 0.4105 0.6797 11.00000 0.05 0.18 ; _shelx_res_checksum 56441 _shelx_hkl_file ; 0 0 2 1719.31 9.70 0 0 3 0.31 0.33 0 0 4 3304.22 19.20 0 0 5 0.07 0.57 0 0 6 586.66 10.09 0 0 7 0.95 0.91 0 0 8 96.07 4.89 0 0 9 -0.28 0.84 0 0 10 602.52 13.56 0 0 11 1.36 1.40 0 0 12 2352.70 30.45 0 0 13 0.44 1.24 0 0 14 15.44 2.96 0 0 15 0.25 1.16 0 0 16 584.33 18.58 0 0 17 1.58 1.54 0 0 17 2.18 0.84 0 0 18 19.97 3.81 0 0 18 17.53 1.80 0 0 19 0.42 0.73 0 0 20 1.59 0.95 0 0 21 0.27 0.78 0 0 22 155.70 5.56 0 0 23 0.71 0.85 0 0 24 3.35 1.10 0 0 25 -0.52 0.85 0 0 26 185.53 5.68 0 0 27 0.63 0.69 0 0 28 366.71 7.08 0 0 29 1.12 0.61 0 0 30 206.70 4.45 0 1 0 0.38 0.22 0 1 -1 939.51 5.59 0 1 1 905.03 7.34 0 1 2 7.09 0.74 0 1 3 1179.56 10.37 0 1 4 306.17 6.08 0 -1 5 953.03 12.30 0 1 5 933.20 11.61 0 -1 6 35.09 2.67 0 1 6 37.79 2.65 0 1 7 897.76 13.59 0 -1 7 891.51 14.01 0 1 8 2120.49 22.52 0 -1 8 2128.17 23.00 0 -1 9 739.68 14.56 0 1 9 711.43 13.98 0 -1 10 2047.88 25.87 0 1 10 2093.99 25.45 0 1 11 252.07 9.43 0 -1 11 257.81 9.74 0 1 12 1848.65 27.02 0 -1 12 1897.93 27.76 0 1 13 702.24 17.56 0 -1 13 661.23 17.29 0 -1 14 1420.24 26.46 0 1 14 1451.56 26.41 0 1 15 306.22 12.84 0 1 16 421.00 7.80 0 1 16 431.16 15.90 0 1 17 101.00 8.15 0 1 17 105.02 4.05 0 1 18 538.26 9.41 0 1 18 514.10 19.02 0 1 19 68.87 7.28 0 -1 19 65.01 3.48 0 1 19 64.50 3.41 0 1 20 1258.22 15.09 0 -1 20 1256.77 15.47 0 1 21 385.64 8.50 0 -1 21 369.51 8.50 0 1 22 86.30 4.11 0 -1 22 85.16 4.20 0 -1 23 699.32 11.84 0 1 23 719.53 11.64 0 1 24 72.78 3.74 0 -1 24 72.15 3.80 0 1 25 140.63 5.01 0 -1 25 140.03 5.12 0 1 26 4.25 1.10 0 -1 26 3.24 0.95 0 -1 27 77.91 3.49 0 1 27 76.38 3.42 0 1 28 14.93 1.48 0 -1 28 14.06 1.48 0 1 29 106.69 3.47 0 -1 29 103.90 3.46 0 1 30 97.24 2.96 0 -1 30 97.15 3.00 0 2 0 9.09 0.92 0 2 1 741.15 9.08 0 2 -1 729.29 7.15 0 2 1 753.48 8.74 0 2 2 9239.79 32.98 0 2 3 9556.31 34.96 0 2 4 1096.72 12.79 0 2 5 479.29 9.11 0 2 6 157.91 5.61 0 2 7 1874.70 20.61 0 2 8 10.71 1.82 0 2 9 95.64 5.34 0 2 10 298.40 9.91 0 2 11 853.40 17.62 0 2 12 16.58 2.74 0 2 13 97.64 6.70 0 2 14 105.43 7.45 0 2 15 253.89 11.91 0 2 16 15.37 1.53 0 2 16 17.35 3.43 0 2 17 518.50 18.46 0 2 17 480.63 8.56 0 2 18 1.07 0.75 0 2 18 -1.40 1.56 0 2 19 783.11 24.28 0 2 19 756.40 11.34 0 2 20 81.18 3.83 0 2 20 73.93 7.67 0 -2 21 8.49 1.44 0 2 21 10.70 1.50 0 2 22 307.29 7.49 0 -2 22 297.41 7.69 0 2 23 104.75 4.40 0 -2 23 102.64 4.56 0 2 24 4.02 1.04 0 -2 24 3.82 1.12 0 2 25 59.18 3.19 0 -2 25 60.85 3.33 0 2 26 54.64 2.91 0 -2 26 53.02 2.99 0 -2 27 32.55 2.19 0 2 27 31.50 2.11 0 2 28 263.59 5.52 0 -2 28 265.27 5.65 0 2 29 6.50 0.87 0 -2 29 6.41 0.90 0 -2 30 46.52 1.90 0 2 -30 45.87 2.05 0 3 0 0.14 0.39 0 3 1 166.03 4.92 0 3 1 168.69 5.36 0 3 -1 169.66 4.28 0 3 2 287.73 6.90 0 3 2 267.70 6.73 0 3 3 2642.43 22.54 0 3 3 2589.72 21.49 0 3 4 467.84 9.36 0 3 5 20.82 2.13 0 3 6 18.69 2.22 0 3 7 289.69 8.78 0 3 8 592.68 13.18 0 3 9 480.66 12.54 0 3 10 41.42 3.94 0 3 11 1.30 1.15 0 3 12 4.73 1.89 0 3 13 8.47 2.15 0 3 14 379.34 14.26 0 3 15 2.43 0.81 0 3 15 3.83 2.02 0 3 16 14.52 1.55 0 3 16 16.84 3.19 0 3 17 26.73 4.33 0 3 17 28.37 2.16 0 3 17 24.89 2.07 0 3 18 149.49 10.31 0 3 18 143.60 4.73 0 3 18 152.86 4.98 0 3 19 3.66 1.98 0 3 19 2.40 0.92 0 3 19 2.10 0.74 0 3 20 148.04 10.74 0 3 20 143.69 5.01 0 3 20 140.07 4.62 0 -3 21 140.74 5.29 0 3 21 138.71 4.95 0 -3 22 1.29 0.88 0 3 22 2.42 0.96 0 -3 23 317.19 7.60 0 3 23 317.64 7.24 0 3 24 74.58 3.46 0 -3 24 81.00 3.77 0 3 25 3.24 0.85 0 -3 25 3.62 0.92 0 3 26 111.43 3.78 0 -3 26 117.38 4.02 0 3 27 349.31 6.16 0 -3 27 354.49 6.44 0 3 28 0.91 0.48 0 -3 28 0.92 0.49 0 -3 29 77.68 2.41 0 3 -29 80.74 2.82 0 4 0 105.90 4.96 0 4 1 254.56 6.86 0 4 1 231.64 7.15 0 4 2 135.88 5.43 0 4 2 112.48 5.04 0 4 3 46.95 3.28 0 4 3 49.20 3.45 0 4 4 246.01 8.04 0 4 4 224.87 7.37 0 4 5 36.74 3.16 0 4 5 38.16 3.52 0 4 6 1617.49 21.51 0 4 6 1569.89 22.77 0 4 7 0.82 0.96 0 4 7 2.24 0.97 0 4 8 22.79 2.75 0 4 9 396.27 11.98 0 4 10 516.50 14.35 0 4 11 10.60 2.15 0 4 11 11.88 1.38 0 4 12 39.48 2.47 0 4 12 39.33 4.37 0 4 13 510.52 8.89 0 4 14 108.47 4.19 0 4 15 474.27 8.79 0 4 15 461.66 8.10 0 4 16 0.58 0.72 0 4 16 1.84 0.81 0 4 17 450.49 8.32 0 4 17 436.93 8.60 0 4 18 83.86 3.65 0 4 18 83.98 3.83 0 4 19 449.94 8.47 0 4 19 452.18 8.80 0 4 20 125.90 4.48 0 4 20 132.93 4.70 0 4 21 193.85 5.47 0 4 21 185.60 5.43 0 -4 21 204.52 6.00 0 4 22 155.37 4.73 0 4 22 155.01 4.79 0 -4 22 160.02 5.18 0 4 23 0.24 0.53 0 -4 23 1.00 0.84 0 4 24 416.20 7.17 0 -4 24 423.39 7.71 0 -4 25 40.45 2.26 0 4 25 39.20 2.07 0 -4 26 16.85 1.28 0 -4 26 17.84 1.39 0 4 -27 0.88 0.55 0 -4 27 0.93 0.42 0 4 -28 269.40 4.84 0 5 5 64.68 3.09 0 5 6 78.83 3.45 0 5 7 12.82 1.47 0 5 8 182.57 5.35 0 5 9 33.52 4.04 0 5 9 39.74 2.56 0 5 10 4.17 1.03 0 5 10 3.89 1.60 0 5 11 1.69 0.84 0 5 11 -0.72 1.24 0 5 12 662.02 20.24 0 5 12 712.47 11.09 0 5 13 122.05 8.90 0 5 13 133.66 4.90 0 5 14 1391.17 15.93 0 5 14 1346.70 30.36 0 5 15 186.70 5.90 0 5 15 180.29 11.37 0 5 16 1124.01 14.48 0 5 17 251.68 6.83 0 5 18 20.69 2.01 0 5 19 4.43 1.10 0 5 20 172.00 5.35 0 -5 20 164.69 4.96 0 -5 21 39.68 2.36 0 5 21 39.33 2.46 0 5 22 58.65 2.81 0 -5 22 53.85 2.61 0 5 23 117.57 3.63 0 5 -24 125.70 3.94 0 5 -25 127.10 3.62 0 6 0 93.36 3.79 0 6 1 281.95 6.61 0 6 2 14.07 1.60 0 6 3 330.98 7.37 0 6 4 775.82 11.46 0 6 5 26.44 2.23 0 6 6 194.03 5.87 0 6 7 0.32 0.75 0 6 8 802.34 12.21 0 6 9 0.69 0.81 0 6 10 9.37 1.55 0 6 11 142.94 5.31 0 6 12 5.96 1.35 0 6 13 31.56 2.58 0 6 14 76.48 3.92 0 6 15 64.09 3.55 0 6 16 13.40 1.74 0 6 17 1.54 0.85 0 6 18 49.16 2.92 0 6 19 11.95 1.44 0 6 20 0.13 0.53 0 6 21 5.78 0.95 0 6 22 13.33 1.23 0 6 23 -0.40 0.41 0 7 0 -0.02 0.57 0 7 1 247.43 6.53 0 7 2 8.85 1.39 0 7 3 347.10 7.97 0 7 4 255.08 6.92 0 7 5 178.51 5.84 0 7 6 1.67 0.94 0 7 7 234.08 6.73 0 7 8 10.87 1.64 0 7 9 90.83 4.25 0 7 10 15.94 1.91 0 7 11 34.61 2.66 0 7 12 99.38 4.39 0 7 13 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3 0 64.34 7.41 -5 3 -1 230.46 6.61 5 3 1 250.26 14.36 -5 3 -1 232.98 6.60 -5 3 -2 86.71 4.09 -5 3 -2 86.04 4.03 5 3 3 1.16 1.96 -5 3 -3 3.31 1.11 -5 3 -3 3.13 1.11 -5 3 -4 476.21 9.64 -5 3 -4 478.99 9.19 5 3 5 13.03 3.50 -5 3 -5 16.31 1.93 -5 3 -5 16.60 1.80 5 3 6 133.49 10.81 -5 3 -6 125.29 5.04 -5 3 -6 127.14 4.62 -5 3 -7 65.24 3.71 -5 3 -7 61.45 3.19 -5 3 -8 555.43 10.64 -5 3 -9 205.27 6.56 -5 3 -10 4.11 1.25 -5 3 -11 3.34 1.08 -5 3 -12 563.94 10.63 -5 3 -13 29.01 2.50 -5 3 -14 23.60 2.23 -5 3 -15 45.29 2.93 -5 3 -16 140.39 4.90 -5 3 -17 2.47 0.89 -5 3 -18 301.60 6.58 -5 3 -19 69.87 3.01 -5 3 -20 148.55 4.03 -5 3 -21 6.26 0.82 -5 -4 22 1.00 0.51 -5 -4 21 33.68 1.95 -5 -4 20 15.82 1.48 -5 -4 19 72.06 3.15 -5 -4 18 39.46 2.46 -5 -4 17 144.11 4.79 -5 -4 16 71.63 3.46 -5 -4 15 65.60 3.40 -5 4 14 0.26 0.53 -5 -4 14 0.26 0.76 -5 -4 13 91.30 4.06 -5 4 13 86.73 3.66 -5 -4 12 108.57 4.46 -5 4 12 105.29 4.20 -5 4 11 8.56 1.34 -5 -4 11 7.53 1.36 -5 -4 10 158.33 5.35 -5 4 10 163.01 5.44 -5 -4 9 11.61 1.58 -5 4 9 11.32 1.62 -5 -4 8 108.34 4.41 -5 4 8 107.47 4.54 -5 4 7 13.01 1.80 -5 -4 7 12.27 1.53 -5 4 6 516.08 10.00 -5 4 5 128.69 5.04 -5 4 4 153.54 5.56 -5 4 3 33.83 2.73 -5 4 3 38.12 2.60 -5 4 2 8.31 1.51 -5 4 2 6.55 1.21 -5 4 1 219.35 6.62 -5 4 1 220.42 6.14 -5 4 0 89.59 4.23 -5 4 0 86.80 3.93 -5 4 -1 25.46 2.34 -5 4 -1 25.83 2.22 -5 4 -2 1.94 0.94 -5 4 -2 1.26 0.74 -5 4 -3 21.09 2.10 -5 4 -3 21.10 2.06 -5 4 -4 51.54 3.12 -5 4 -4 47.41 3.01 -5 4 -5 71.47 3.67 -5 4 -5 66.72 3.49 -5 4 -6 740.66 11.64 -5 4 -6 716.00 10.96 -5 4 -7 97.07 4.31 -5 4 -7 95.30 3.91 -5 4 -8 224.49 6.44 -5 4 -9 20.87 2.04 -5 4 -10 11.88 1.60 -5 4 -11 156.79 5.33 -5 4 -12 1.77 0.90 -5 4 -13 132.31 4.73 -5 4 -14 4.83 1.02 -5 4 -15 17.12 1.67 -5 4 -16 0.76 0.58 -5 4 -17 0.50 0.56 -5 4 -18 67.74 2.75 -5 4 -19 44.21 2.04 -5 -5 20 19.41 1.31 -5 -5 19 0.28 0.44 -5 -5 18 0.32 0.46 -5 -5 17 30.27 1.95 -5 -5 16 32.29 2.11 -5 -5 15 72.98 3.19 -5 5 14 0.16 0.48 -5 -5 14 0.71 0.62 -5 5 13 6.78 1.03 -5 -5 13 6.83 1.11 -5 -5 12 46.75 2.67 -5 5 12 49.09 2.69 -5 -5 11 348.91 7.21 -5 5 11 355.53 7.41 -5 5 10 0.80 0.71 -5 -5 10 1.08 0.73 -5 5 9 123.84 4.65 -5 5 8 91.25 4.06 -5 5 7 394.08 8.49 -5 5 6 46.38 3.05 -5 5 5 25.37 2.35 -5 5 4 20.63 2.12 -5 5 3 3.00 1.17 -5 5 2 19.45 2.11 -5 5 1 3.57 1.07 -5 5 0 29.66 2.53 -5 5 -1 531.85 10.05 -5 5 -2 71.96 3.71 -5 5 -3 211.74 6.21 -5 5 -4 68.50 3.51 -5 5 -4 74.22 3.35 -5 5 -5 94.50 3.79 -5 5 -5 89.55 3.88 -5 5 -6 1.47 0.73 -5 5 -6 0.72 0.69 -5 5 -7 131.34 4.46 -5 5 -7 129.96 4.33 -5 5 -8 2.38 0.80 -5 5 -9 49.69 2.71 -5 5 -10 7.30 1.12 -5 5 -11 11.65 1.32 -5 5 -12 24.78 1.82 -5 5 -13 39.19 2.18 -5 5 -14 17.30 1.42 5 5 15 1.49 0.60 -5 5 -15 2.21 0.57 5 5 16 6.97 0.89 -5 5 -16 7.09 0.83 5 5 17 6.97 0.81 -5 -6 15 301.64 4.86 -5 -6 14 36.13 1.77 -5 6 13 1.47 0.50 -5 6 12 41.37 2.14 -5 6 11 16.97 1.49 -5 6 10 4.28 0.91 -5 6 9 1.72 0.64 -5 6 8 45.34 2.65 -5 6 7 3.28 0.97 -5 6 6 142.30 4.79 -5 6 5 25.57 2.13 -5 6 4 8.78 1.40 -5 6 3 17.34 1.82 -5 6 2 1.82 0.88 -5 6 1 8.04 1.38 -5 6 0 104.02 4.25 -5 6 -1 206.45 5.86 -5 6 -2 51.90 2.95 -5 6 -3 50.82 2.85 -5 6 -4 27.29 2.07 -5 6 -5 120.17 4.09 -5 6 -6 52.10 2.59 5 6 10 6.14 0.86 5 6 11 355.49 5.56 5 6 12 1.69 0.48 5 6 13 262.48 4.43 -5 7 10 12.55 1.07 -5 7 9 59.86 2.40 -5 7 8 67.33 2.67 -5 7 7 61.89 2.66 -5 7 6 6.30 0.99 -5 7 5 30.70 2.00 -5 7 4 128.60 4.03 -5 7 3 196.73 4.99 -5 7 2 80.33 3.24 -5 7 1 19.65 1.63 -5 7 0 88.51 3.34 -5 7 -1 67.19 2.88 -5 7 -2 189.82 4.71 -5 7 -3 117.89 3.60 -5 7 -4 2.75 0.67 -5 7 -5 8.52 0.96 -6 0 22 3.49 0.61 -6 0 21 0.12 0.41 -6 0 20 52.06 2.47 -6 0 19 -0.43 0.62 -6 0 18 335.88 6.97 -6 0 17 0.41 0.73 -6 0 16 176.38 5.44 -6 0 15 0.47 0.76 -6 0 14 10.27 1.57 -6 0 13 -0.41 0.84 -6 0 12 231.33 6.76 -6 0 11 0.21 0.83 -6 0 11 6.29 1.65 -6 0 10 241.64 7.00 -6 0 10 252.62 6.75 -6 0 9 1.02 1.09 -6 0 9 0.19 0.83 -6 0 8 41.58 2.98 -6 0 8 43.70 2.95 -6 0 7 -0.34 0.97 -6 0 7 -0.32 0.80 -6 0 6 39.40 2.90 -6 0 6 37.85 2.77 -6 0 5 0.48 0.86 -6 0 5 0.64 0.81 -6 0 4 387.71 8.79 -6 0 4 389.96 8.66 -6 0 3 1.46 0.95 -6 0 3 1.08 0.82 -6 0 2 288.84 7.71 -6 0 2 298.31 7.55 -6 0 1 0.90 0.97 -6 0 1 -0.73 1.25 -6 0 0 310.50 7.89 -6 0 0 329.85 7.87 -6 0 -1 6.83 1.57 -6 0 -1 5.29 1.47 -6 0 -2 4967.23 31.52 -6 0 -2 4992.71 30.05 -6 0 -3 6.15 1.39 -6 0 -3 4.69 1.49 -6 0 -4 339.26 8.19 -6 0 -4 335.93 7.58 -6 0 -5 6.39 1.45 -6 0 -5 1.09 0.97 -6 0 -6 575.42 10.64 -6 0 -7 0.08 0.81 -6 0 -8 163.54 5.59 -6 0 -9 0.54 0.72 -6 0 -10 25.56 2.24 -6 0 -11 0.56 0.71 -6 0 -12 9.63 1.41 -6 0 -13 0.35 0.69 -6 0 -14 5.78 1.10 -6 0 -15 0.49 0.52 -6 0 -16 166.87 4.41 -6 0 -17 -0.23 0.42 -6 0 -18 67.76 2.34 -6 -1 22 54.14 2.14 -6 -1 21 24.21 1.62 -6 -1 20 3.60 0.81 -6 1 19 67.38 2.90 -6 -1 19 68.16 3.02 -6 1 18 302.88 6.43 -6 -1 18 315.19 6.75 -6 1 17 200.87 5.49 -6 -1 17 201.42 5.64 -6 1 16 58.77 3.12 -6 -1 16 61.10 3.24 -6 1 15 2.39 0.83 -6 -1 15 4.03 1.12 -6 1 14 331.15 7.71 -6 -1 14 320.67 7.69 -6 1 14 332.32 6.90 -6 1 13 8.82 1.51 -6 -1 13 6.87 1.38 -6 1 13 9.02 1.36 -6 1 12 437.62 9.27 -6 -1 12 437.67 9.22 -6 1 12 425.23 8.38 -6 1 11 293.10 7.68 -6 -1 11 297.15 7.60 -6 1 11 297.01 7.18 -6 1 10 110.15 4.77 -6 -1 10 108.94 4.66 -6 1 10 112.22 4.53 -6 -1 9 13.52 1.80 -6 1 9 11.12 1.70 -6 1 9 12.22 1.73 -6 1 8 77.67 4.03 -6 -1 8 75.06 3.88 -6 1 8 76.31 3.83 -6 1 7 48.75 3.26 -6 -1 7 43.55 2.99 -6 1 7 47.77 3.11 -6 1 6 141.84 5.47 -6 -1 6 138.86 5.21 -6 1 6 144.73 5.30 -6 -1 5 352.37 8.22 -6 -1 5 361.55 8.32 -6 1 5 357.74 8.30 -6 1 4 2.77 1.07 -6 -1 4 4.00 1.07 -6 -1 3 446.29 9.02 -6 1 3 446.63 9.62 -6 -1 3 455.92 9.35 -6 1 3 451.98 9.34 -6 -1 2 84.82 3.94 -6 1 2 86.58 4.24 -6 -1 2 96.80 4.43 -6 1 2 84.61 4.10 -6 1 1 184.43 6.18 -6 1 1 189.61 6.06 -6 1 0 7.43 1.48 -6 -1 0 5.16 1.30 -6 1 0 6.00 1.38 -6 -1 -1 209.07 6.25 -6 1 -1 212.47 6.62 -6 1 -1 207.64 6.27 -6 -1 -2 456.12 9.17 -6 1 -2 452.61 9.62 -6 1 -2 450.51 9.11 -6 -1 -3 208.07 6.20 -6 1 -3 214.56 6.65 -6 1 -3 203.03 6.07 -6 -1 -4 58.14 3.32 -6 1 -4 58.80 3.57 -6 1 -4 56.72 3.19 -6 -1 -5 148.97 5.24 -6 1 -5 160.17 5.74 -6 1 -5 154.13 5.07 -6 -1 -6 227.90 6.40 -6 1 -6 239.17 6.99 -6 1 -6 226.40 5.95 -6 1 -7 12.17 1.77 -6 -1 -7 10.80 1.49 -6 -1 -8 20.01 1.94 -6 1 -8 19.63 2.10 -6 -1 -9 101.32 4.13 -6 1 -9 105.68 4.57 -6 -1 -10 65.92 3.28 -6 1 -10 71.54 3.70 -6 -1 -11 0.56 0.61 -6 1 -11 -0.05 0.72 -6 -1 -12 313.88 6.68 -6 1 -12 303.82 7.30 -6 -1 -13 129.07 4.12 -6 1 -13 129.16 4.65 -6 -1 -14 305.34 5.98 -6 1 -14 305.58 6.84 -6 1 -15 26.08 2.00 -6 1 -16 260.32 5.75 -6 1 -17 100.02 3.35 -6 1 -18 72.76 2.61 -6 -2 22 0.69 0.42 -6 -2 21 3.17 0.68 -6 -2 20 503.81 7.37 -6 -2 19 27.92 1.93 -6 -2 18 26.88 1.99 -6 -2 17 40.44 2.50 -6 -2 16 26.90 2.13 -6 -2 15 21.40 1.98 -6 2 15 23.71 1.75 -6 2 14 4.24 0.94 -6 -2 14 5.04 1.16 -6 -2 13 223.72 6.34 -6 2 13 210.50 5.65 -6 -2 12 69.17 3.61 -6 2 12 71.20 3.42 -6 2 11 1.84 0.92 -6 -2 11 2.22 0.98 -6 2 10 11.30 1.55 -6 -2 10 12.27 1.67 -6 -2 9 141.82 5.17 -6 2 9 138.23 5.04 -6 -2 8 165.24 5.55 -6 2 8 167.96 5.62 -6 -2 7 41.97 2.84 -6 2 7 44.79 3.00 -6 -2 6 170.65 5.53 -6 2 6 175.72 5.83 -6 2 5 10.80 1.60 -6 -2 5 11.37 1.51 -6 2 4 4.62 1.25 -6 -2 4 4.37 1.06 -6 -2 3 125.02 4.56 -6 2 3 122.57 5.02 -6 2 3 119.44 4.84 -6 2 2 70.81 3.83 -6 2 2 68.82 3.70 -6 2 1 616.46 11.10 -6 2 1 634.48 10.98 -6 2 0 199.93 6.35 -6 2 0 194.64 6.08 -6 2 -1 80.60 4.07 -6 2 -1 73.37 3.79 -6 2 -2 191.91 6.23 -6 2 -2 162.31 5.49 -6 2 -3 293.74 7.74 -6 2 -3 291.60 7.24 -6 -2 -4 749.42 10.93 -6 2 -4 732.01 12.22 -6 2 -4 734.09 11.25 -6 -2 -5 9.33 1.33 -6 2 -5 9.95 1.65 -6 2 -5 10.25 1.44 -6 2 -6 139.36 5.32 -6 2 -6 132.05 4.53 -6 2 -7 220.95 6.68 -6 2 -8 40.38 2.89 -6 2 -9 276.98 7.33 -6 2 -10 117.33 4.72 -6 2 -11 30.03 2.44 -6 2 -12 7.26 1.31 -6 2 -13 60.82 3.15 -6 2 -14 6.88 1.16 -6 2 -15 73.05 3.18 -6 2 -16 2.51 0.76 -6 2 -17 76.36 2.87 -6 2 -18 46.56 2.08 -6 -3 20 1.96 0.57 -6 -3 19 21.36 1.55 -6 -3 18 19.24 1.56 -6 -3 17 87.69 3.39 -6 -3 16 26.22 1.98 -6 -3 15 108.49 4.02 -6 3 14 0.79 0.56 -6 -3 14 2.40 0.87 -6 -3 13 80.91 3.62 -6 3 13 79.23 3.34 -6 -3 12 95.90 3.98 -6 3 12 90.02 3.70 -6 -3 11 49.36 2.89 -6 3 11 46.51 2.78 -6 -3 10 46.44 2.82 -6 3 10 46.26 2.84 -6 -3 9 112.72 4.38 -6 3 9 114.02 4.48 -6 -3 8 49.33 2.90 -6 3 8 51.98 3.12 -6 -3 7 53.66 2.95 -6 3 7 54.10 3.24 -6 -3 6 71.34 3.36 -6 3 6 69.78 3.67 -6 3 5 245.02 6.84 -6 3 4 83.18 4.07 -6 3 3 4.83 1.23 -6 3 2 87.46 4.11 -6 3 2 86.96 4.14 -6 3 1 327.35 7.87 -6 3 1 324.05 7.82 -6 3 0 119.39 4.78 -6 3 0 120.72 4.76 -6 3 -1 31.29 2.53 -6 3 -1 28.72 2.41 -6 3 -2 49.06 3.16 -6 3 -2 42.97 2.86 -6 3 -3 161.17 5.52 -6 3 -3 152.51 5.17 -6 3 -4 0.53 0.70 -6 3 -4 1.03 0.87 -6 3 -5 117.78 4.75 -6 3 -5 116.47 4.32 -6 3 -6 298.46 7.48 -6 3 -6 294.59 6.58 -6 3 -7 109.26 4.51 -6 3 -8 106.42 4.40 -6 3 -9 5.14 1.17 -6 3 -10 123.62 4.59 -6 3 -11 162.95 5.14 -6 3 -12 1.05 0.69 -6 3 -13 26.06 1.98 -6 3 -14 59.45 2.81 -6 3 -15 16.51 1.46 -6 3 -16 27.12 1.72 -6 3 -17 78.19 2.64 -6 -4 18 120.03 3.22 -6 -4 17 204.67 4.46 -6 -4 16 43.77 2.20 -6 -4 15 188.19 4.64 -6 4 14 1.28 0.62 -6 -4 14 0.20 0.46 -6 4 13 0.46 0.48 -6 -4 13 0.70 0.55 -6 -4 12 78.96 3.24 -6 4 12 81.18 3.28 -6 -4 11 99.76 3.67 -6 4 11 98.76 3.73 -6 -4 10 83.16 3.36 -6 4 10 95.02 3.80 -6 -4 9 72.59 3.13 -6 4 9 70.45 3.38 -6 4 8 130.08 4.65 -6 4 7 29.84 2.35 -6 4 6 42.73 2.81 -6 4 5 41.07 2.80 -6 4 4 10.84 1.55 -6 4 3 44.48 2.95 -6 4 2 79.12 3.87 -6 4 1 205.30 6.11 -6 4 0 61.59 3.18 -6 4 0 62.79 3.40 -6 4 -1 26.39 2.12 -6 4 -1 24.42 2.13 -6 4 -2 81.03 3.65 -6 4 -2 83.58 3.77 -6 4 -3 310.62 7.10 -6 4 -3 298.97 6.89 -6 4 -4 1.71 0.72 -6 4 -4 1.18 0.75 -6 4 -5 111.06 4.20 -6 4 -5 115.39 4.04 -6 4 -6 20.26 1.86 -6 4 -6 20.51 1.70 -6 4 -7 24.03 1.98 -6 4 -8 236.19 5.89 -6 4 -9 146.28 4.57 -6 4 -10 27.49 2.00 -6 4 -11 220.25 5.29 -6 4 -12 79.93 3.09 -6 4 -13 63.36 2.63 -6 4 -14 17.47 1.33 -6 4 -15 104.77 2.95 -6 5 13 4.93 0.73 -6 5 12 243.36 4.86 -6 5 11 14.68 1.34 -6 5 10 123.91 3.86 -6 5 9 15.23 1.47 -6 5 8 22.79 1.85 -6 5 7 37.27 2.37 -6 5 6 174.76 5.11 -6 5 5 1.65 0.84 -6 5 4 3.03 0.96 -6 5 3 17.33 1.75 -6 5 2 144.57 4.78 -6 5 1 8.26 1.27 -6 5 0 16.72 1.72 -6 5 -1 35.98 2.36 -6 5 -2 40.88 2.44 -6 5 -3 27.62 2.00 -6 5 -4 197.72 4.67 -6 5 -4 195.68 4.92 -6 5 -5 39.09 2.07 -6 5 -5 40.56 2.16 -6 5 -6 47.72 2.24 -6 5 -7 87.91 2.99 -6 5 -8 4.54 0.73 -6 5 -9 3.10 0.63 -6 5 -10 257.78 4.55 -6 6 10 219.94 4.15 -6 6 9 14.38 1.18 -6 6 8 82.11 2.82 -6 6 7 16.30 1.36 -6 6 6 103.12 3.36 -6 6 5 103.47 3.44 -6 6 4 113.40 3.63 -6 6 3 1.03 0.60 -6 6 2 127.98 3.89 -6 6 1 4.35 0.88 -6 6 0 1.90 0.62 -6 6 -1 29.16 1.80 -6 6 -2 73.13 2.74 -6 6 -3 50.27 2.18 -6 6 -4 22.54 1.40 -7 0 -4 0.78 0.74 -7 0 -5 39.19 2.51 -7 0 -6 1.43 0.78 -7 0 -7 416.00 7.69 -7 0 -8 0.26 0.67 -7 0 -9 355.18 6.65 -7 0 -10 0.70 0.61 -7 0 -11 1.17 0.54 -7 0 -12 -0.01 0.41 -7 -1 17 0.11 0.44 -7 -1 16 156.06 4.12 -7 -1 15 27.27 1.84 -7 -1 14 9.08 1.17 -7 -1 13 41.41 2.41 -7 -1 12 191.91 5.21 -7 -1 11 56.29 2.93 -7 -1 10 75.38 3.42 -7 -1 9 23.23 1.98 -7 1 9 30.15 2.28 -7 -1 8 10.85 1.44 -7 1 8 16.62 1.85 -7 1 7 61.06 3.23 -7 1 6 173.44 5.35 -7 1 5 84.24 3.83 -7 1 4 92.59 3.98 -7 1 3 11.28 1.57 -7 1 2 40.99 2.75 -7 1 1 239.60 6.27 -7 1 0 49.43 2.92 -7 1 -1 5.02 1.28 -7 1 -2 4.59 1.24 -7 1 -2 1.05 0.91 -7 1 -3 50.57 2.99 -7 1 -4 117.34 4.43 -7 1 -5 1.39 0.82 -7 1 -6 99.24 3.94 -7 1 -7 10.25 1.36 -7 1 -8 35.00 2.30 -7 1 -9 2.40 0.80 -7 1 -10 75.41 3.09 -7 1 -11 0.41 0.51 -7 1 -12 16.89 1.36 -7 1 -13 11.98 1.08 -7 -2 17 13.81 1.11 -7 -2 16 4.81 0.75 -7 -2 15 0.32 0.43 -7 -2 14 94.70 3.25 -7 -2 13 37.68 2.15 -7 -2 12 189.87 4.86 -7 2 12 186.04 4.55 -7 -2 11 27.85 1.95 -7 2 11 33.20 2.12 -7 -2 10 46.56 2.53 -7 2 10 44.18 2.46 -7 2 9 7.84 1.19 -7 -2 9 6.79 1.05 -7 -2 8 33.93 2.20 -7 2 8 34.09 2.30 -7 2 7 6.46 1.18 -7 2 6 59.24 3.08 -7 2 5 1.31 0.77 -7 2 4 217.41 5.93 -7 2 3 129.24 4.58 -7 2 2 368.83 7.72 -7 2 1 449.42 8.41 -7 2 0 746.33 10.70 -7 2 -1 5.53 1.18 -7 2 -2 307.02 7.14 -7 2 -2 282.09 6.40 -7 2 -3 30.85 2.31 -7 2 -3 32.49 2.16 -7 2 -4 38.16 2.51 -7 2 -4 40.57 2.33 -7 2 -5 10.31 1.39 -7 2 -5 13.12 1.35 -7 2 -6 114.90 4.14 -7 2 -7 95.83 3.70 -7 2 -8 225.79 5.50 -7 2 -9 45.60 2.43 -7 2 -10 7.79 1.05 -7 2 -11 91.03 3.14 -7 2 -12 36.25 1.89 -7 2 -13 25.72 1.49 -7 -3 14 284.32 4.85 -7 -3 13 6.55 0.84 -7 -3 12 85.20 2.85 -7 3 12 81.99 2.79 -7 3 11 2.49 0.68 -7 -3 11 3.22 0.66 -7 3 10 4.66 0.91 -7 -3 10 4.10 0.71 -7 -3 9 41.49 2.09 -7 3 9 39.60 2.26 -7 3 8 110.99 3.84 -7 3 7 20.08 1.75 -7 3 6 85.90 3.52 -7 3 5 194.73 5.31 -7 3 4 98.87 3.83 -7 3 3 -0.18 0.77 -7 3 2 2.65 0.90 -7 3 1 11.70 1.41 -7 3 0 231.45 5.68 -7 3 -1 36.18 2.27 -7 3 -2 54.34 2.66 -7 3 -3 6.28 1.00 -7 3 -4 143.20 4.42 -7 3 -4 131.31 3.79 -7 3 -5 20.23 1.70 -7 3 -6 13.99 1.40 -7 3 -7 20.37 1.60 -7 3 -8 141.64 4.00 -7 3 -9 0.55 0.52 -7 3 -10 164.82 3.96 -7 3 -11 11.62 1.06 -7 4 11 11.67 1.00 -7 4 10 64.84 2.43 -7 4 9 11.29 1.12 -7 4 8 144.54 3.93 -7 4 7 23.26 1.69 -7 4 6 127.04 3.87 -7 4 5 2.00 0.76 -7 4 4 423.16 7.16 -7 4 3 185.28 4.77 -7 4 2 96.12 3.43 -7 4 1 26.54 1.86 -7 4 0 248.19 5.36 -7 4 -1 274.06 5.49 -7 4 -2 6.54 0.95 -7 4 -3 73.56 2.64 -7 4 -4 15.70 1.19 -7 5 7 223.79 4.16 -7 5 6 47.16 1.99 -7 5 5 6.54 0.82 -7 5 4 3.99 0.69 -7 5 3 10.69 1.03 -7 5 2 74.79 2.56 -7 5 1 66.67 2.39 -7 5 0 5.45 0.73 TITL 22Dub_VJ04_auto in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 6.732582 8.075787 25.216371 90.0000 94.5392 90.0000 ZERR 4.00 0.000173 0.000233 0.000577 0.0000 0.0022 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O S UNIT 72.00 52.00 4.00 4.00 4.00 REM CrysAlisPro recorded range (K): Min=152.3; max=153.5; aver:152.9 TEMP -120 SIZE 0.14 0.18 0.21 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 12193 _olex2_date_sample_data_collection 2022-04-29 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a mylar loop in perfluoroether oil' _olex2_submission_original_sample_id VJ32 _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 1.111 _oxdiff_exptl_absorpt_empirical_full_min 0.924