data_tx3757 _audit_creation_date 2020-11-03 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _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 'C14 H17 N O4' _chemical_formula_sum 'C14 H17 N O4' _chemical_formula_weight 263.28 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_usercomment 'C H N O' 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' _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 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.2799(2) _cell_length_b 5.20460(10) _cell_length_c 12.4362(2) _cell_angle_alpha 90 _cell_angle_beta 91.2890(10) _cell_angle_gamma 90 _cell_volume 665.20(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9006 _cell_measurement_temperature 169.99(11) _cell_measurement_theta_max 74.7900 _cell_measurement_theta_min 3.5440 _shelx_estimated_absorpt_T_max 0.969 _shelx_estimated_absorpt_T_min 0.567 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'translucent light colourless' _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 280 _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 12599 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.954 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.606 _diffrn_reflns_theta_min 3.555 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 169.99(11) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.982 _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 -73.00 26.00 0.50 0.05 -- -47.20 83.00 82.00 198 2 \w -24.00 73.00 0.50 0.05 -- 47.20 -83.00 -37.00 194 3 \w -168.00 -79.00 0.50 0.50 -- -99.00 -83.00 -37.00 178 4 \w 31.00 129.00 0.50 0.50 -- 103.25 -83.00 -37.00 196 5 \w 86.00 169.00 0.50 0.50 -- 103.25 83.00 82.00 166 6 \w -120.00 -74.00 0.50 0.05 -- -47.20-125.00 90.00 92 7 \w -23.00 28.00 0.50 0.05 -- -47.20 19.00 60.00 102 8 \w -120.00 -32.00 0.50 0.05 -- -47.20 -57.00 -90.00 176 9 \w -23.00 28.00 0.50 0.05 -- -47.20 19.00 120.00 102 10 \w -26.00 47.00 0.50 0.05 -- 47.20 -38.00-120.00 146 11 \w -68.00 -26.00 0.50 0.50 -- -99.00 61.00 0.00 84 12 \w -168.00 -86.00 0.50 0.50 -- -99.00 -45.00-120.00 164 13 \w -168.00 -82.00 0.50 0.50 -- -99.00 -61.00 60.00 172 14 \w -112.00 -26.00 0.50 0.50 -- -99.00 125.00-120.00 172 15 \w -168.00 -82.00 0.50 0.50 -- -99.00 -61.00 -90.00 172 16 \w -168.00 -86.00 0.50 0.50 -- -99.00 -45.00-150.00 164 17 \w -68.00 -26.00 0.50 0.50 -- -99.00 61.00 -90.00 84 18 \w -68.00 -26.00 0.50 0.50 -- -99.00 61.00 -60.00 84 19 \w -124.00 -26.00 0.50 0.50 -- -99.00 83.00 82.00 196 20 \w -68.00 -26.00 0.50 0.50 -- -99.00 61.00 30.00 84 21 \w 31.00 75.00 0.50 0.50 -- 103.25 -61.00-120.00 88 22 \w 91.00 169.00 0.50 0.50 -- 103.25 45.00-120.00 156 23 \w 31.00 75.00 0.50 0.50 -- 103.25 -61.00 90.00 88 24 \w 91.00 169.00 0.50 0.50 -- 103.25 45.00 -60.00 156 25 \w 31.00 106.00 0.50 0.50 -- 103.25 -94.00 0.00 150 26 \w 31.00 75.00 0.50 0.50 -- 103.25 -61.00 150.00 88 27 \w 31.00 111.00 0.50 0.50 -- 103.25-125.00 120.00 160 28 \w 87.00 169.00 0.50 0.50 -- 103.25 61.00 0.00 164 29 \w 91.00 169.00 0.50 0.50 -- 103.25 45.00 30.00 156 30 \w 31.00 75.00 0.50 0.50 -- 103.25 -61.00 0.00 88 31 \w -120.00 -32.00 0.50 0.05 -- -47.20 -57.00 120.00 176 32 \w -120.00 -24.00 0.50 0.05 -- -47.20 -77.00 30.00 192 33 \w -120.00 -24.00 0.50 0.05 -- -47.20 -77.00 90.00 192 34 \w -120.00 -34.00 0.50 0.05 -- -47.20 -38.00 -60.00 172 35 \w -120.00 -32.00 0.50 0.05 -- -47.20 -57.00-150.00 176 36 \w -120.00 -32.00 0.50 0.05 -- -47.20 -57.00-180.00 176 37 \w -27.00 30.00 0.50 0.05 -- 47.20 -19.00 150.00 114 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0675127000 _diffrn_orient_matrix_UB_12 -0.2392005000 _diffrn_orient_matrix_UB_13 0.0482483000 _diffrn_orient_matrix_UB_21 0.0262480000 _diffrn_orient_matrix_UB_22 -0.0998361000 _diffrn_orient_matrix_UB_23 -0.1141073000 _diffrn_orient_matrix_UB_31 0.1311710000 _diffrn_orient_matrix_UB_32 0.1432445000 _diffrn_orient_matrix_UB_33 0.0011379000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _reflns_Friedel_coverage 0.745 _reflns_Friedel_fraction_full 0.992 _reflns_Friedel_fraction_max 0.919 _reflns_number_gt 2553 _reflns_number_total 2644 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _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 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.159 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.038 _refine_ls_abs_structure_details ; Flack x determined using 1062 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.08(6) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2644 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0316 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.0940P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.0823 _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,H) groups 2.a Ternary CH refined with riding coordinates: C1(H1), C5(H5) 2.b Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B), C8(H8A,H8B) 2.c Aromatic/amide H refined with riding coordinates: C10(H10), C11(H11), C12(H12), C14(H14), C13(H13) 2.d X=CH2 refined with riding coordinates: N1(H1A,H1B) ; _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 O1 O 0.65708(12) 0.3718(2) 0.30398(9) 0.0271(3) Uani 1 1 d . . . . . O3 O 0.57386(14) 0.7265(3) 0.44110(10) 0.0328(3) Uani 1 1 d . . . . . O2 O 0.58181(14) -0.0657(3) 0.09644(10) 0.0362(3) Uani 1 1 d . . . . . O4 O 0.71561(13) 0.5971(3) 0.57018(10) 0.0371(4) Uani 1 1 d . . . . . N1 N 0.57369(16) 0.3687(3) 0.10135(12) 0.0330(4) Uani 1 1 d . . . . . H1A H 0.532887 0.379525 0.040392 0.040 Uiso 1 1 calc R . . . . H1B H 0.593516 0.505880 0.136597 0.040 Uiso 1 1 calc R . . . . C7 C 0.65804(17) 0.5835(4) 0.47250(13) 0.0275(4) Uani 1 1 d . . . . . C6 C 0.60587(17) 0.1415(3) 0.14081(13) 0.0265(4) Uani 1 1 d . . . . . C1 C 0.67948(17) 0.1361(4) 0.24802(13) 0.0268(4) Uani 1 1 d . . . . . H1 H 0.645183 -0.005314 0.291009 0.032 Uiso 1 1 calc R . . . . C5 C 0.71109(17) 0.3573(4) 0.41042(13) 0.0275(4) Uani 1 1 d . . . . . H5 H 0.678621 0.199696 0.443575 0.033 Uiso 1 1 calc R . . . . C4 C 0.85871(18) 0.3381(4) 0.40700(15) 0.0331(4) Uani 1 1 d . . . . . H4A H 0.895018 0.327949 0.479542 0.040 Uiso 1 1 calc R . . . . H4B H 0.893872 0.489493 0.372663 0.040 Uiso 1 1 calc R . . . . C9 C 0.74162(19) 0.8171(4) 0.74004(14) 0.0354(5) Uani 1 1 d . . . . . C10 C 0.7332(2) 0.6575(5) 0.82872(17) 0.0405(5) Uani 1 1 d . . . . . H10 H 0.676522 0.518195 0.826969 0.049 Uiso 1 1 calc R . . . . C3 C 0.89521(19) 0.0970(4) 0.34358(17) 0.0373(5) Uani 1 1 d . . . . . H3A H 0.988434 0.094479 0.333153 0.045 Uiso 1 1 calc R . . . . H3B H 0.872349 -0.054864 0.384220 0.045 Uiso 1 1 calc R . . . . C2 C 0.82416(19) 0.0922(4) 0.23408(16) 0.0359(4) Uani 1 1 d . . . . . H2A H 0.859039 0.225120 0.188246 0.043 Uiso 1 1 calc R . . . . H2B H 0.837882 -0.072475 0.199644 0.043 Uiso 1 1 calc R . . . . C11 C 0.8092(2) 0.7053(5) 0.92030(17) 0.0467(6) Uani 1 1 d . . . . . H11 H 0.802789 0.598486 0.979907 0.056 Uiso 1 1 calc R . . . . C12 C 0.8931(2) 0.9078(6) 0.92316(17) 0.0472(6) Uani 1 1 d . . . . . H12 H 0.943979 0.938450 0.984612 0.057 Uiso 1 1 calc R . . . . C14 C 0.8269(2) 1.0227(5) 0.74445(19) 0.0463(5) Uani 1 1 d . . . . . H14 H 0.833067 1.131837 0.685558 0.056 Uiso 1 1 calc R . . . . C8 C 0.6548(2) 0.7809(6) 0.64306(18) 0.0542(7) Uani 1 1 d . . . . . H8A H 0.570725 0.716583 0.664574 0.065 Uiso 1 1 calc R . . . . H8B H 0.641569 0.944019 0.606727 0.065 Uiso 1 1 calc R . . . . C13 C 0.9029(2) 1.0674(5) 0.8354(2) 0.0522(6) Uani 1 1 d . . . . . H13 H 0.960577 1.205007 0.837382 0.063 Uiso 1 1 calc R . . . . 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 O1 0.0345(6) 0.0256(6) 0.0209(5) -0.0020(5) -0.0056(4) 0.0020(5) O3 0.0409(7) 0.0314(7) 0.0260(6) -0.0008(5) -0.0040(5) 0.0032(6) O2 0.0564(9) 0.0222(7) 0.0294(7) -0.0037(5) -0.0124(6) 0.0002(6) O4 0.0386(7) 0.0483(9) 0.0240(6) -0.0094(6) -0.0071(5) 0.0105(7) N1 0.0515(9) 0.0223(8) 0.0247(7) -0.0009(6) -0.0119(7) -0.0010(7) C7 0.0301(8) 0.0311(10) 0.0213(7) -0.0010(7) -0.0029(6) -0.0048(8) C6 0.0331(8) 0.0230(8) 0.0231(8) -0.0006(7) -0.0020(6) -0.0017(8) C1 0.0369(9) 0.0205(8) 0.0227(7) -0.0012(7) -0.0042(7) -0.0005(8) C5 0.0353(9) 0.0260(9) 0.0210(7) 0.0002(7) -0.0054(6) -0.0025(8) C4 0.0354(9) 0.0317(10) 0.0317(9) -0.0046(8) -0.0087(7) 0.0016(8) C9 0.0351(10) 0.0459(12) 0.0250(8) -0.0099(8) -0.0017(7) 0.0109(9) C10 0.0393(10) 0.0404(11) 0.0419(11) 0.0000(10) 0.0001(8) -0.0023(9) C3 0.0339(9) 0.0355(11) 0.0420(10) -0.0071(9) -0.0097(8) 0.0068(8) C2 0.0385(10) 0.0347(11) 0.0342(9) -0.0095(8) -0.0022(8) 0.0054(8) C11 0.0482(12) 0.0613(16) 0.0307(10) 0.0083(10) -0.0012(8) 0.0054(11) C12 0.0459(12) 0.0613(15) 0.0338(10) -0.0125(11) -0.0112(9) 0.0062(11) C14 0.0535(13) 0.0478(13) 0.0379(11) 0.0090(9) 0.0042(10) 0.0041(11) C8 0.0485(13) 0.0804(19) 0.0332(10) -0.0230(11) -0.0103(9) 0.0265(12) C13 0.0472(12) 0.0489(14) 0.0600(14) -0.0062(12) -0.0049(11) -0.0089(11) _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 O1 C1 1.432(2) . ? O1 C5 1.4259(18) . ? O3 C7 1.200(2) . ? O2 C6 1.234(2) . ? O4 C7 1.341(2) . ? O4 C8 1.467(3) . ? N1 C6 1.319(2) . ? C7 C5 1.516(2) . ? C6 C1 1.518(2) . ? C1 C2 1.519(3) . ? C5 C4 1.522(3) . ? C4 C3 1.533(3) . ? C9 C10 1.385(3) . ? C9 C14 1.384(3) . ? C9 C8 1.496(3) . ? C10 C11 1.389(3) . ? C3 C2 1.531(3) . ? C11 C12 1.362(4) . ? C12 C13 1.377(4) . ? C14 C13 1.379(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 C5 O1 C1 110.01(13) . . ? C7 O4 C8 114.11(14) . . ? O3 C7 O4 124.21(17) . . ? O3 C7 C5 125.52(15) . . ? O4 C7 C5 110.23(14) . . ? O2 C6 N1 124.81(15) . . ? O2 C6 C1 117.86(16) . . ? N1 C6 C1 117.33(15) . . ? O1 C1 C6 109.18(14) . . ? O1 C1 C2 110.67(14) . . ? C6 C1 C2 111.88(14) . . ? O1 C5 C7 107.13(14) . . ? O1 C5 C4 110.18(14) . . ? C7 C5 C4 115.82(14) . . ? C5 C4 C3 108.89(15) . . ? C10 C9 C8 121.3(2) . . ? C14 C9 C10 118.90(19) . . ? C14 C9 C8 119.7(2) . . ? C9 C10 C11 120.1(2) . . ? C2 C3 C4 110.70(15) . . ? C1 C2 C3 110.18(15) . . ? C12 C11 C10 120.3(2) . . ? C11 C12 C13 120.2(2) . . ? C13 C14 C9 120.6(2) . . ? O4 C8 C9 108.99(16) . . ? C12 C13 C14 119.9(2) . . ? _shelx_res_file ; TITL tx3757_a.res in P2(1) tx3757.res created by SHELXL-2018/3 at 06:46:09 on 03-Nov-2020 REM Old TITL TX3757 in P2(1)/m REM SHELXT solution in P2(1): R1 0.120, Rweak 0.030, Alpha 0.002 REM 0.963 for 3 systematic absences, Orientation as input REM Flack x = -0.027 ( 0.053 ) from 1069 Parsons' quotients REM Formula found by SHELXT: C12 O5 CELL 1.54184 10.2799 5.2046 12.4362 90 91.289 90 ZERR 2 0.0002 0.0001 0.0002 0 0.001 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O UNIT 28 34 2 8 L.S. 4 PLAN 5 SIZE 0.04 0.04 0.8 BOND LIST 6 fmap 2 ACTA REM REM REM WGHT 0.047300 0.094000 FVAR 1.28787 O1 4 0.657082 0.371844 0.303977 11.00000 0.03454 0.02558 = 0.02087 -0.00201 -0.00555 0.00198 O3 4 0.573857 0.726532 0.441097 11.00000 0.04092 0.03139 = 0.02596 -0.00076 -0.00402 0.00321 O2 4 0.581813 -0.065719 0.096440 11.00000 0.05642 0.02222 = 0.02936 -0.00366 -0.01244 0.00017 O4 4 0.715613 0.597082 0.570180 11.00000 0.03864 0.04831 = 0.02395 -0.00939 -0.00713 0.01050 N1 3 0.573690 0.368667 0.101354 11.00000 0.05154 0.02229 = 0.02465 -0.00092 -0.01191 -0.00097 AFIX 93 H1A 2 0.532887 0.379525 0.040392 11.00000 -1.20000 H1B 2 0.593516 0.505880 0.136597 11.00000 -1.20000 AFIX 0 C7 1 0.658035 0.583488 0.472497 11.00000 0.03005 0.03110 = 0.02126 -0.00102 -0.00293 -0.00485 C6 1 0.605869 0.141521 0.140810 11.00000 0.03311 0.02304 = 0.02314 -0.00058 -0.00201 -0.00169 C1 1 0.679480 0.136108 0.248017 11.00000 0.03690 0.02054 = 0.02265 -0.00120 -0.00416 -0.00052 AFIX 13 H1 2 0.645183 -0.005314 0.291009 11.00000 -1.20000 AFIX 0 C5 1 0.711085 0.357298 0.410420 11.00000 0.03528 0.02605 = 0.02098 0.00023 -0.00539 -0.00246 AFIX 13 H5 2 0.678621 0.199696 0.443575 11.00000 -1.20000 AFIX 0 C4 1 0.858711 0.338081 0.406996 11.00000 0.03540 0.03173 = 0.03170 -0.00456 -0.00870 0.00156 AFIX 23 H4A 2 0.895018 0.327949 0.479542 11.00000 -1.20000 H4B 2 0.893872 0.489493 0.372663 11.00000 -1.20000 AFIX 0 C9 1 0.741617 0.817066 0.740040 11.00000 0.03510 0.04587 = 0.02502 -0.00993 -0.00170 0.01090 C10 1 0.733177 0.657517 0.828725 11.00000 0.03926 0.04039 = 0.04194 -0.00002 0.00011 -0.00226 AFIX 43 H10 2 0.676522 0.518195 0.826969 11.00000 -1.20000 AFIX 0 C3 1 0.895214 0.097016 0.343578 11.00000 0.03395 0.03553 = 0.04198 -0.00705 -0.00971 0.00676 AFIX 23 H3A 2 0.988434 0.094479 0.333153 11.00000 -1.20000 H3B 2 0.872349 -0.054864 0.384220 11.00000 -1.20000 AFIX 0 C2 1 0.824161 0.092239 0.234077 11.00000 0.03850 0.03475 = 0.03421 -0.00949 -0.00225 0.00544 AFIX 23 H2A 2 0.859039 0.225120 0.188246 11.00000 -1.20000 H2B 2 0.837882 -0.072475 0.199644 11.00000 -1.20000 AFIX 0 C11 1 0.809206 0.705267 0.920300 11.00000 0.04818 0.06127 = 0.03066 0.00832 -0.00116 0.00542 AFIX 43 H11 2 0.802789 0.598486 0.979907 11.00000 -1.20000 AFIX 0 C12 1 0.893107 0.907801 0.923165 11.00000 0.04593 0.06126 = 0.03378 -0.01246 -0.01124 0.00616 AFIX 43 H12 2 0.943979 0.938450 0.984612 11.00000 -1.20000 AFIX 0 C14 1 0.826910 1.022729 0.744447 11.00000 0.05353 0.04776 = 0.03786 0.00898 0.00420 0.00415 AFIX 43 H14 2 0.833067 1.131837 0.685558 11.00000 -1.20000 AFIX 0 C8 1 0.654799 0.780872 0.643061 11.00000 0.04846 0.08039 = 0.03318 -0.02296 -0.01025 0.02647 AFIX 23 H8A 2 0.570725 0.716583 0.664574 11.00000 -1.20000 H8B 2 0.641569 0.944019 0.606727 11.00000 -1.20000 AFIX 0 C13 1 0.902871 1.067386 0.835366 11.00000 0.04725 0.04890 = 0.06004 -0.00620 -0.00486 -0.00893 AFIX 43 H13 2 0.960577 1.205007 0.837382 11.00000 -1.20000 AFIX 0 HKLF 4 REM tx3757_a.res in P2(1) REM wR2 = 0.0823, GooF = S = 1.049, Restrained GooF = 1.049 for all data REM R1 = 0.0316 for 2553 Fo > 4sig(Fo) and 0.0326 for all 2644 data REM 172 parameters refined using 1 restraints END WGHT 0.0473 0.0940 REM Highest difference peak 0.159, deepest hole -0.192, 1-sigma level 0.038 Q1 1 0.8126 0.8554 0.7342 11.00000 0.05 0.16 Q2 1 0.7872 0.3593 0.4082 11.00000 0.05 0.14 Q3 1 0.7517 0.1051 0.2468 11.00000 0.05 0.12 Q4 1 0.5729 0.8764 0.6322 11.00000 0.05 0.12 Q5 1 0.8868 0.2399 0.3668 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46.60 2 -2 4 1247.01 48.30 -2 2 -4 1200.32 47.72 2 2 4 1306.64 48.02 -2 -2 -4 1178.38 46.29 -2 2 -4 1141.16 46.41 2 2 4 1252.12 47.93 -2 -2 -4 1258.82 48.00 2 -2 4 1229.67 47.81 2 -2 4 1120.32 46.76 2 2 4 1280.98 47.11 2 2 5 18.25 2.47 2 -2 5 15.21 2.44 -2 2 -5 14.19 2.74 -2 -2 -5 12.17 2.13 2 -2 5 11.29 2.96 2 -2 5 10.60 2.30 -2 2 -5 14.53 2.88 2 2 5 11.50 2.62 2 2 5 11.59 2.31 -2 -2 -5 11.60 1.90 -2 -2 -5 13.62 2.77 2 -2 5 12.58 0.92 2 2 5 15.25 1.07 2 -2 6 37.84 4.09 2 2 6 49.69 4.37 -2 -2 -6 49.25 4.24 2 -2 6 43.94 5.13 -2 2 -6 47.03 4.74 2 2 6 47.18 2.22 -2 2 -6 43.39 4.71 2 -2 6 42.82 4.35 2 2 6 55.35 5.05 -2 -2 -6 50.72 3.98 -2 2 -6 47.24 2.26 2 2 6 44.26 2.27 2 -2 6 45.26 2.15 -2 2 -6 44.87 3.81 -2 -2 -6 50.06 4.86 -2 -2 -7 30.12 4.50 2 2 7 34.37 1.69 -2 2 -7 29.03 3.18 2 -2 7 31.14 1.62 -2 -2 -7 26.37 3.26 2 2 7 30.81 3.91 -2 -2 -7 34.25 1.67 -2 2 -7 31.72 1.67 2 -2 7 38.18 4.33 2 -2 7 34.75 5.04 -2 -2 -7 30.45 3.90 -2 2 -7 30.57 4.32 2 -2 7 27.52 3.84 2 2 7 38.01 4.59 -2 2 -7 30.14 1.83 -2 -2 -7 32.22 1.66 2 -2 7 31.43 1.74 2 2 7 31.75 1.87 2 -2 8 128.67 5.32 2 2 8 128.60 5.36 -2 -2 -8 135.13 9.88 -2 2 -8 130.51 5.36 -2 -2 -8 130.52 5.35 2 -2 8 129.92 8.92 2 2 8 134.94 8.93 -2 -2 -8 124.28 8.66 2 -2 8 131.22 10.14 -2 2 -8 134.04 9.65 2 -2 8 126.10 8.83 -2 -2 -8 119.99 8.12 -2 2 -8 138.46 5.58 -2 -2 -8 131.56 5.30 2 2 8 129.75 5.66 2 -2 8 127.32 5.40 -2 -2 -9 817.18 36.24 2 2 9 793.23 30.30 2 -2 9 826.46 30.30 -2 -2 -9 831.67 30.32 2 2 9 834.24 35.39 2 -2 9 797.49 35.29 -2 2 -9 798.02 30.30 -2 2 -9 799.02 35.91 2 -2 9 719.36 34.44 -2 2 -9 807.81 30.49 2 2 9 848.53 30.39 -2 -2 -9 799.75 30.22 2 2 9 823.71 30.57 2 -2 9 760.70 30.31 -2 -2 -10 168.76 11.63 2 -2 10 153.52 6.29 2 2 10 158.35 6.38 -2 -2 -10 134.43 10.72 -2 2 -10 148.07 10.98 -2 -2 -10 156.15 6.45 -2 2 -10 160.18 6.46 2 2 10 152.67 10.57 2 -2 10 149.27 10.65 -2 -2 -10 125.78 10.91 -2 2 -10 129.13 10.93 2 -2 10 116.95 9.82 -2 2 -10 156.54 6.58 2 2 10 156.26 6.38 2 2 10 152.78 6.83 2 2 10 147.87 10.84 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213.64 8.25 -2 -3 5 216.28 12.62 2 -3 -5 202.49 8.22 -2 3 5 203.00 8.20 2 -3 -5 212.34 11.89 2 3 -5 209.31 8.28 2 3 -5 218.11 8.37 2 -3 -5 212.28 8.25 -2 3 4 41.48 5.12 2 -3 -4 37.75 4.39 2 -3 -4 32.75 4.60 -2 -3 4 36.20 4.41 2 3 -4 29.00 3.70 2 -3 -4 34.89 4.12 -2 3 4 34.85 4.71 -2 3 4 37.57 1.96 -2 3 4 32.12 3.29 -2 3 4 37.93 1.93 2 3 -4 38.74 2.03 2 -3 -4 40.97 1.95 2 3 -4 39.23 2.00 2 3 -4 38.31 2.06 2 -3 -4 40.81 1.92 2 -3 -3 47.05 4.46 2 -3 -3 38.82 4.68 -2 -3 3 29.84 3.37 2 -3 -3 37.13 4.24 2 3 -3 33.67 3.87 -2 -3 3 33.01 3.99 -2 3 3 44.36 4.86 -2 3 3 33.76 4.32 -2 3 3 37.66 3.71 -2 3 3 39.03 1.94 -2 3 3 38.41 1.87 2 -3 -3 40.62 1.86 2 3 -3 37.51 1.90 -2 3 3 33.42 1.87 2 3 -3 38.08 1.97 2 -3 -3 38.56 1.83 -2 3 3 35.66 1.81 -2 3 3 36.86 1.81 2 -3 -2 94.29 7.23 -2 -3 2 107.22 6.66 -2 -3 2 100.35 7.15 2 3 -2 107.98 6.59 2 -3 -2 99.18 6.96 -2 3 2 104.53 7.27 -2 3 2 102.22 7.29 -2 3 2 101.68 4.20 -2 3 2 116.48 6.92 2 3 -2 95.30 4.19 2 -3 -2 101.86 4.11 2 3 -2 104.77 4.20 -2 3 2 99.13 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13.51 1.63 11 -1 -4 14.86 1.66 11 1 -4 14.38 1.64 11 1 -4 15.80 1.49 11 -1 -4 15.92 1.34 11 1 -3 1.92 1.26 11 -1 -3 0.51 0.90 11 1 -3 2.25 1.47 11 -1 -3 3.13 1.34 11 -1 -3 2.33 1.54 11 1 -3 -0.49 1.50 11 1 -3 1.52 1.19 11 -1 -3 2.05 1.02 11 -1 -2 8.55 1.16 11 1 -2 8.28 1.64 11 -1 -2 7.35 1.45 11 -1 -2 5.52 1.67 11 1 -2 5.92 1.71 11 1 -2 9.76 1.46 11 -1 -2 9.36 1.23 11 -1 -1 3.48 1.08 11 1 -1 1.29 1.50 11 -1 -1 3.86 1.39 11 -1 -1 4.28 1.71 11 1 -1 1.34 1.64 11 1 -1 4.30 1.35 11 -1 -1 4.13 1.13 11 1 0 21.62 1.91 11 1 0 23.61 1.89 11 -1 0 25.84 1.72 11 -1 0 22.81 1.85 11 -1 0 21.32 2.06 11 1 0 23.59 2.02 11 1 0 22.10 1.82 11 -1 0 24.85 1.68 11 1 1 53.47 2.82 11 -1 1 51.02 2.70 11 -1 1 49.17 2.70 11 -1 1 48.18 2.80 11 -1 1 55.17 2.97 11 1 1 53.44 2.91 11 1 1 57.92 2.76 11 -1 1 59.21 2.71 11 1 2 25.41 1.91 11 -1 2 26.79 1.78 11 -1 2 22.63 1.73 11 -1 2 24.46 2.00 11 -1 2 27.32 2.11 11 1 2 24.48 2.05 11 1 2 27.39 1.84 11 -1 2 28.56 1.70 11 -1 3 22.82 1.87 11 1 3 19.42 1.81 11 -1 3 22.50 1.84 11 1 3 22.72 1.58 11 -1 3 22.63 1.49 11 1 3 20.16 1.63 11 -1 3 18.58 1.50 11 -1 4 7.20 1.46 11 1 4 7.52 1.43 11 -1 4 7.99 1.50 11 1 4 8.17 1.14 11 -1 4 9.12 1.07 11 1 4 6.78 1.18 11 -1 4 7.97 1.21 -11 1 -4 5.53 0.96 11 -1 5 27.84 1.66 11 1 5 25.31 1.57 11 -1 5 26.44 1.52 11 -1 5 25.75 1.75 11 1 5 27.63 1.73 11 -1 5 26.62 1.83 -11 1 -6 20.97 1.38 11 -1 6 25.95 1.50 11 1 6 24.92 1.43 11 -1 6 26.22 1.39 11 -1 6 25.87 1.54 11 1 6 26.16 1.52 11 1 7 9.55 0.75 11 -1 7 8.72 0.72 11 2 -6 5.06 0.91 11 2 -5 62.04 2.84 11 -2 -5 59.82 2.72 11 2 -4 94.15 4.01 11 -2 -4 101.19 3.92 11 -2 -4 82.95 3.70 11 -2 -4 90.16 3.67 11 2 -3 2.66 1.15 11 -2 -3 1.67 1.00 11 -2 -3 1.84 1.01 11 -2 -3 1.90 0.75 11 2 -2 12.78 1.40 11 2 -2 12.70 1.57 11 -2 -2 10.65 1.32 11 -2 -2 10.22 1.25 11 -2 -2 11.54 0.99 11 2 -1 8.31 1.29 11 2 -1 8.46 1.51 11 -2 -1 8.28 1.23 11 -2 -1 5.93 0.91 11 2 0 27.99 1.79 11 2 0 27.51 1.97 11 -2 0 23.89 1.49 11 -2 0 27.52 1.82 11 -2 0 30.66 1.93 11 -2 0 25.70 1.71 11 -2 0 27.95 1.51 11 -2 1 10.05 1.04 11 -2 1 12.78 1.36 -11 2 -1 9.36 0.94 11 -2 1 11.69 1.57 11 -2 1 11.47 1.24 11 -2 1 10.56 0.98 11 -2 2 37.39 1.88 11 -2 2 36.05 2.02 -11 2 -2 32.20 1.81 11 -2 2 36.86 1.91 11 -2 2 40.01 2.19 11 -2 2 37.61 1.78 11 -2 3 2.96 0.85 -11 2 -3 3.09 0.81 -11 2 -3 2.90 0.85 11 -2 3 2.99 0.98 11 -2 3 3.55 0.70 11 -2 3 2.54 0.95 11 -2 3 4.93 1.31 -11 2 -4 13.21 1.08 11 -2 4 16.73 1.15 11 -2 5 28.95 1.60 -11 2 -5 24.60 1.42 11 -2 5 28.91 1.47 11 -2 6 2.71 0.61 -11 2 -6 2.76 0.59 11 -3 -3 5.78 0.73 11 -3 -2 0.12 0.68 11 -3 -1 7.82 0.90 11 -3 -1 5.66 0.96 -11 3 0 5.91 0.67 11 -3 0 7.65 0.91 11 -3 0 7.08 1.01 -11 3 -1 1.20 0.61 11 -3 1 -0.30 0.74 11 -3 1 1.42 0.90 -11 3 -2 3.66 0.63 11 -3 3 35.52 1.65 12 0 -6 2.68 0.59 12 0 -5 32.92 1.53 12 0 -5 23.66 1.51 12 0 -4 9.62 1.04 12 0 -4 8.00 0.95 12 0 -3 0.44 0.87 12 0 -3 0.18 0.86 12 0 -2 -0.38 0.95 12 0 -2 1.68 0.93 12 0 -1 38.26 1.96 12 0 -1 32.30 1.91 12 0 0 72.64 3.13 12 0 0 66.02 3.12 12 0 1 7.57 1.08 12 0 1 6.74 1.12 12 0 2 122.85 4.81 12 0 2 112.02 4.81 12 0 3 10.94 1.11 12 0 4 50.11 2.32 12 0 4 53.37 2.31 12 0 4 50.61 2.35 12 0 5 38.03 1.71 12 0 5 37.39 1.72 12 1 -5 6.06 0.70 12 1 -5 6.38 0.88 12 1 -4 20.60 1.45 12 -1 -4 21.67 1.38 12 -1 -4 26.31 1.33 12 1 -4 25.03 1.35 12 1 -3 19.89 1.34 12 -1 -3 13.82 1.05 12 1 -3 16.13 1.37 12 -1 -3 17.33 1.27 12 -1 -3 18.06 1.32 12 1 -3 15.97 1.29 12 -1 -3 20.52 1.19 12 1 -3 22.02 1.27 12 -1 -2 0.17 0.70 12 -1 -2 0.20 0.89 12 -1 -2 1.17 1.01 12 1 -2 -0.35 0.99 12 -1 -2 0.11 0.78 12 1 -2 0.19 0.87 12 -1 -1 9.36 1.00 12 -1 -1 10.07 1.10 12 -1 -1 10.13 1.24 12 1 -1 8.05 1.20 12 1 -1 10.03 1.10 12 -1 -1 9.17 1.01 12 -1 0 50.12 2.46 12 1 0 49.50 2.42 12 1 0 55.03 2.40 12 -1 0 54.13 2.37 12 1 0 49.26 2.44 12 -1 0 46.27 2.34 12 -1 1 4.79 1.10 12 1 1 3.68 1.06 12 1 1 4.11 0.92 12 -1 1 4.43 0.87 12 1 1 6.05 1.03 12 -1 1 4.64 0.92 12 -1 2 20.58 1.44 12 1 2 20.72 1.40 12 1 2 21.35 1.34 12 -1 2 22.84 1.31 12 1 2 19.30 1.37 12 -1 2 20.53 1.35 12 -1 3 97.61 4.02 12 1 3 92.73 3.99 12 1 3 104.14 4.00 12 -1 3 106.81 4.01 12 1 3 92.91 3.99 12 -1 3 100.45 4.04 12 1 4 12.94 0.94 12 -1 4 13.05 0.91 12 -1 4 15.63 1.02 12 -2 -3 7.25 0.75 12 -2 -1 1.42 0.71 12 -2 0 0.71 0.69 12 -2 1 35.60 1.68 0 0 0 0.00 0.00 TITL TX3757 in P2(1)/m REM P2(1)/m (#11 in standard setting) CELL 1.54184 10.279928 5.204566 12.436210 90.0000 91.2895 90.0000 ZERR 3.00 0.000151 0.000078 0.000168 0.0000 0.0013 0.0000 LATT 1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 6767 _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 1.306 _oxdiff_exptl_absorpt_empirical_full_min 0.811