####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_s5834a _database_code_depnum_ccdc_archive 'CCDC 2129464' loop_ _audit_author_name _audit_author_address 'Soumitra Agasti' ;University of Manchester United Kingdom ; _audit_update_record ; 2021-12-17 deposited with the CCDC. 2022-10-03 downloaded from the CCDC. ; _audit_creation_date 2021-05-26 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number 2018/3 _audit_contact_author_address ? _audit_contact_author_email ? _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 H23 N O' _chemical_formula_sum 'C18 H23 N O' _chemical_formula_weight 269.37 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.0176(8) _cell_length_b 12.8217(9) _cell_length_c 11.5215(8) _cell_angle_alpha 90 _cell_angle_beta 106.552(7) _cell_angle_gamma 90 _cell_volume 1418.53(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1827 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 28.8140 _cell_measurement_theta_min 3.9790 _shelx_estimated_absorpt_T_max 0.985 _shelx_estimated_absorpt_T_min 0.977 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.0723 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.850 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6091 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.850 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.065 _diffrn_reflns_theta_min 3.558 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0714 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.850 _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 -41.00 -15.00 1.00 4.00 -- -19.09 -77.00 120.00 26 2 \w -23.00 46.00 1.00 4.00 -- -19.09 57.00 -30.00 69 3 \w -6.00 25.00 1.00 4.00 -- 20.18 77.00 60.00 31 4 \w -30.00 67.00 1.00 4.00 -- 20.18 -19.00 0.00 97 ; _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 0.0658756000 _diffrn_orient_matrix_UB_12 -0.0238809000 _diffrn_orient_matrix_UB_13 0.0080764000 _diffrn_orient_matrix_UB_21 -0.0333939000 _diffrn_orient_matrix_UB_22 -0.0459960000 _diffrn_orient_matrix_UB_23 -0.0282087000 _diffrn_orient_matrix_UB_31 0.0020939000 _diffrn_orient_matrix_UB_32 0.0193255000 _diffrn_orient_matrix_UB_33 -0.0571335000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\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 2326 _reflns_number_total 3239 _reflns_odcompleteness_completeness 99.70 _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 1.171.41.108a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.327 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.061 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 3239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0626 _refine_ls_restrained_S_all 1.038 _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^)+(0.0503P)^2^+0.9583P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1372 _refine_ls_wR_factor_ref 0.1549 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Ternary CH refined with riding coordinates: C005(H005), C006(H006), C00D(H00I), C00F(H00L), C00H(H00O) 2.b Secondary CH2 refined with riding coordinates: C008(H00A,H00B), C009(H00C,H00D), C00A(H00E,H00F), C00C(H00G,H00H), C00E(H00J, H00K), C00G(H00M,H00N), C00I(H00P,H00Q), C00J(H00R,H00S), C00K(H00T,H00U) ; _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 O001 O 0.62560(16) 0.68495(14) 0.86099(13) 0.0243(4) Uani 1 1 d . . . . . N002 N 0.6389(2) 0.97702(17) 0.78722(18) 0.0316(5) Uani 1 1 d . . . . . C00A C 0.8033(2) 0.53646(18) 0.80824(19) 0.0182(5) Uani 1 1 d . . . . . H00E H 0.816494 0.553156 0.894678 0.022 Uiso 1 1 calc R U . . . H00F H 0.727020 0.484811 0.783043 0.022 Uiso 1 1 calc R U . . . C00B C 0.6013(2) 0.91815(19) 0.7101(2) 0.0213(5) Uani 1 1 d . . . . . C00C C 0.9979(2) 0.64244(19) 0.62396(19) 0.0214(5) Uani 1 1 d . . . . . H00G H 0.974510 0.706561 0.574448 0.026 Uiso 1 1 calc R U . . . H00H H 1.084995 0.613206 0.612950 0.026 Uiso 1 1 calc R U . . . C00D C 0.5528(2) 0.84238(17) 0.61198(18) 0.0176(5) Uani 1 1 d . . . . . H00I H 0.622446 0.834349 0.565347 0.021 Uiso 1 1 calc R U . . . C00E C 0.9164(2) 0.46332(19) 0.65820(19) 0.0217(5) Uani 1 1 d . . . . . H00J H 1.002585 0.432458 0.647168 0.026 Uiso 1 1 calc R U . . . H00K H 0.840387 0.411707 0.631134 0.026 Uiso 1 1 calc R U . . . C00F C 0.3268(2) 0.77100(19) 0.54538(19) 0.0212(5) Uani 1 1 d . . . . . H00L H 0.225839 0.762551 0.501421 0.025 Uiso 1 1 calc R U . . . C00G C 1.0561(2) 0.56945(19) 0.8342(2) 0.0222(5) Uani 1 1 d . . . . . H00M H 1.070385 0.586163 0.920733 0.027 Uiso 1 1 calc R U . . . H00N H 1.143766 0.539788 0.824981 0.027 Uiso 1 1 calc R U . . . C00H C 0.9380(2) 0.48956(18) 0.7924(2) 0.0202(5) Uani 1 1 d . . . . . H00O H 0.962292 0.424677 0.842093 0.024 Uiso 1 1 calc R U . . . C00I C 0.4310(2) 0.68349(18) 0.53931(19) 0.0205(5) Uani 1 1 d . . . . . H00P H 0.471958 0.689185 0.470858 0.025 Uiso 1 1 calc R U . . . H00Q H 0.398143 0.611863 0.547927 0.025 Uiso 1 1 calc R U . . . C00J C 0.3773(2) 0.75761(19) 0.68507(19) 0.0201(5) Uani 1 1 d . . . . . H00R H 0.336071 0.697638 0.716677 0.024 Uiso 1 1 calc R U . . . H00S H 0.375308 0.822094 0.731807 0.024 Uiso 1 1 calc R U . . . C00K C 0.4045(2) 0.86834(18) 0.52460(19) 0.0199(5) Uani 1 1 d . . . . . H00T H 0.365012 0.932665 0.549169 0.024 Uiso 1 1 calc R U . . . H00U H 0.405856 0.874583 0.439308 0.024 Uiso 1 1 calc R U . . . C003 C 0.6341(2) 0.68380(17) 0.75728(18) 0.0158(4) Uani 1 1 d . . . . . C004 C 0.7632(2) 0.63628(16) 0.73173(17) 0.0136(4) Uani 1 1 d . . . . . C005 C 1.0188(2) 0.66874(19) 0.75820(19) 0.0200(5) Uani 1 1 d . . . . . H005 H 1.096132 0.720494 0.785406 0.024 Uiso 1 1 calc R U . . . C006 C 0.8796(2) 0.56271(18) 0.58275(18) 0.0188(5) Uani 1 1 d . . . . . H006 H 0.866116 0.545462 0.495520 0.023 Uiso 1 1 calc R U . . . C007 C 0.5189(2) 0.73469(17) 0.65978(18) 0.0163(4) Uani 1 1 d . . . . . C008 C 0.8834(2) 0.71601(17) 0.77321(18) 0.0172(5) Uani 1 1 d . . . . . H00A H 0.859916 0.780386 0.724167 0.021 Uiso 1 1 calc R U . . . H00B H 0.896415 0.734599 0.859130 0.021 Uiso 1 1 calc R U . . . C009 C 0.7437(2) 0.60934(18) 0.59786(18) 0.0180(5) Uani 1 1 d . . . . . H00C H 0.718936 0.673079 0.547834 0.022 Uiso 1 1 calc R U . . . H00D H 0.666897 0.558462 0.570019 0.022 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 O001 0.0260(9) 0.0349(10) 0.0142(7) 0.0035(7) 0.0091(6) 0.0092(8) N002 0.0427(13) 0.0210(11) 0.0283(11) -0.0036(10) 0.0057(9) -0.0008(10) C00A 0.0190(11) 0.0181(11) 0.0176(10) 0.0038(9) 0.0053(8) 0.0016(9) C00B 0.0228(12) 0.0188(12) 0.0227(11) 0.0035(10) 0.0071(9) 0.0020(10) C00C 0.0205(11) 0.0268(13) 0.0185(11) 0.0016(10) 0.0081(9) 0.0013(10) C00D 0.0224(11) 0.0165(11) 0.0139(10) 0.0011(9) 0.0051(8) 0.0014(9) C00E 0.0185(11) 0.0212(12) 0.0252(11) -0.0039(10) 0.0061(9) 0.0052(9) C00F 0.0163(10) 0.0257(13) 0.0203(11) 0.0018(10) 0.0033(8) 0.0024(10) C00G 0.0190(11) 0.0270(13) 0.0196(11) -0.0002(10) 0.0038(9) 0.0026(10) C00H 0.0210(11) 0.0174(11) 0.0211(10) 0.0037(10) 0.0043(8) 0.0051(9) C00I 0.0210(11) 0.0204(12) 0.0192(11) -0.0024(10) 0.0043(9) 0.0006(10) C00J 0.0170(11) 0.0226(12) 0.0210(11) 0.0023(10) 0.0059(8) 0.0018(9) C00K 0.0236(11) 0.0207(12) 0.0151(10) 0.0012(9) 0.0050(8) 0.0060(10) C003 0.0196(11) 0.0131(10) 0.0148(10) 0.0001(9) 0.0052(8) -0.0011(9) C004 0.0162(10) 0.0136(10) 0.0115(9) 0.0004(8) 0.0049(7) 0.0008(8) C005 0.0180(11) 0.0239(12) 0.0175(10) -0.0046(10) 0.0043(8) -0.0049(9) C006 0.0199(11) 0.0220(12) 0.0147(10) -0.0050(9) 0.0053(8) 0.0017(9) C007 0.0169(10) 0.0154(11) 0.0176(10) -0.0004(9) 0.0066(8) 0.0005(9) C008 0.0213(11) 0.0156(11) 0.0146(10) -0.0024(9) 0.0049(8) -0.0031(9) C009 0.0204(11) 0.0198(12) 0.0131(9) -0.0029(9) 0.0035(8) 0.0008(9) _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 O001 C003 1.222(2) . ? N002 C00B 1.145(3) . ? C00A H00E 0.9900 . ? C00A H00F 0.9900 . ? C00A C00H 1.536(3) . ? C00B C00D 1.465(3) . ? C00C H00G 0.9900 . ? C00C H00H 0.9900 . ? C00D H00I 1.0000 . ? C00D C00K 1.575(3) . ? C00E H00J 0.9900 . ? C00E H00K 0.9900 . ? C00E C00H 1.536(3) . ? C00F H00L 1.0000 . ? C00F C00I 1.547(3) . ? C00F C00J 1.553(3) . ? C00F C00K 1.525(3) . ? C00G H00M 0.9900 . ? C00G H00N 0.9900 . ? C00G C00H 1.535(3) . ? C00H H00O 1.0000 . ? C00I H00P 0.9900 . ? C00I H00Q 0.9900 . ? C00J H00R 0.9900 . ? C00J H00S 0.9900 . ? C00K H00T 0.9900 . ? C00K H00U 0.9900 . ? C003 C004 1.532(3) . ? C003 C007 1.510(3) . ? C004 C00A 1.541(3) . ? C004 C008 1.548(3) . ? C004 C009 1.538(3) . ? C005 C00C 1.538(3) . ? C005 C00G 1.530(3) . ? C005 H005 1.0000 . ? C005 C008 1.540(3) . ? C006 C00C 1.535(3) . ? C006 C00E 1.527(3) . ? C006 H006 1.0000 . ? C006 C009 1.541(3) . ? C007 C00D 1.559(3) . ? C007 C00I 1.561(3) . ? C007 C00J 1.555(3) . ? C008 H00A 0.9900 . ? C008 H00B 0.9900 . ? C009 H00C 0.9900 . ? C009 H00D 0.9900 . ? 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 H00E C00A H00F 108.1 . . ? C00H C00A H00E 109.5 . . ? C00H C00A H00F 109.5 . . ? C00H C00A C004 110.61(17) . . ? C004 C00A H00E 109.5 . . ? C004 C00A H00F 109.5 . . ? N002 C00B C00D 179.6(3) . . ? H00G C00C H00H 108.3 . . ? C005 C00C H00G 109.8 . . ? C005 C00C H00H 109.8 . . ? C006 C00C H00G 109.8 . . ? C006 C00C H00H 109.8 . . ? C006 C00C C005 109.20(17) . . ? C00B C00D H00I 110.7 . . ? C00B C00D C00K 113.48(18) . . ? C00B C00D C007 111.88(17) . . ? C00K C00D H00I 110.7 . . ? C007 C00D H00I 110.7 . . ? C007 C00D C00K 98.76(17) . . ? H00J C00E H00K 108.2 . . ? C00H C00E H00J 109.8 . . ? C00H C00E H00K 109.8 . . ? C006 C00E H00J 109.8 . . ? C006 C00E H00K 109.8 . . ? C006 C00E C00H 109.39(18) . . ? C00I C00F H00L 119.8 . . ? C00I C00F C00J 86.68(16) . . ? C00J C00F H00L 119.8 . . ? C00K C00F H00L 119.8 . . ? C00K C00F C00I 101.88(17) . . ? C00K C00F C00J 102.90(18) . . ? H00M C00G H00N 108.2 . . ? C00H C00G H00M 109.8 . . ? C00H C00G H00N 109.8 . . ? C005 C00G H00M 109.8 . . ? C005 C00G H00N 109.8 . . ? C005 C00G C00H 109.60(18) . . ? C00A C00H C00E 109.20(18) . . ? C00A C00H H00O 109.6 . . ? C00E C00H H00O 109.6 . . ? C00G C00H C00A 109.04(18) . . ? C00G C00H C00E 109.70(19) . . ? C00G C00H H00O 109.6 . . ? C00F C00I H00P 114.9 . . ? C00F C00I H00Q 114.9 . . ? C00F C00I C007 82.63(16) . . ? H00P C00I H00Q 111.9 . . ? C007 C00I H00P 114.9 . . ? C007 C00I H00Q 114.9 . . ? C00F C00J H00R 114.9 . . ? C00F C00J H00S 114.9 . . ? C00F C00J C007 82.63(15) . . ? H00R C00J H00S 111.9 . . ? C007 C00J H00R 114.9 . . ? C007 C00J H00S 114.9 . . ? C00D C00K H00T 112.0 . . ? C00D C00K H00U 112.0 . . ? C00F C00K C00D 99.03(17) . . ? C00F C00K H00T 112.0 . . ? C00F C00K H00U 112.0 . . ? H00T C00K H00U 109.6 . . ? O001 C003 C004 119.38(18) . . ? O001 C003 C007 118.07(19) . . ? C007 C003 C004 122.47(17) . . ? C00A C004 C008 108.59(17) . . ? C003 C004 C00A 108.50(16) . . ? C003 C004 C008 107.63(17) . . ? C003 C004 C009 114.17(17) . . ? C009 C004 C00A 108.97(17) . . ? C009 C004 C008 108.85(17) . . ? C00C C005 H005 109.4 . . ? C00C C005 C008 109.11(17) . . ? C00G C005 C00C 109.51(19) . . ? C00G C005 H005 109.4 . . ? C00G C005 C008 110.03(18) . . ? C008 C005 H005 109.4 . . ? C00C C006 H006 109.2 . . ? C00C C006 C009 109.63(18) . . ? C00E C006 C00C 109.83(18) . . ? C00E C006 H006 109.2 . . ? C00E C006 C009 109.73(17) . . ? C009 C006 H006 109.2 . . ? C00D C007 C00I 100.53(16) . . ? C00J C007 C00D 101.58(17) . . ? C00J C007 C00I 86.12(16) . . ? C003 C007 C00D 116.62(18) . . ? C003 C007 C00I 126.71(18) . . ? C003 C007 C00J 119.13(17) . . ? C004 C008 H00A 109.7 . . ? C004 C008 H00B 109.7 . . ? C005 C008 C004 109.77(18) . . ? C005 C008 H00A 109.7 . . ? C005 C008 H00B 109.7 . . ? H00A C008 H00B 108.2 . . ? C004 C009 C006 109.68(17) . . ? C004 C009 H00C 109.7 . . ? C004 C009 H00D 109.7 . . ? C006 C009 H00C 109.7 . . ? C006 C009 H00D 109.7 . . ? H00C C009 H00D 108.2 . . ? 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 O001 C003 C004 C00A 40.8(3) . . . . ? O001 C003 C004 C008 -76.5(2) . . . . ? O001 C003 C004 C009 162.5(2) . . . . ? O001 C003 C007 C00D 105.2(2) . . . . ? O001 C003 C007 C00I -125.9(2) . . . . ? O001 C003 C007 C00J -17.3(3) . . . . ? C00A C004 C008 C005 58.6(2) . . . . ? C00A C004 C009 C006 -58.8(2) . . . . ? C00B C00D C00K C00F -118.42(19) . . . . ? C00C C005 C00G C00H -59.9(2) . . . . ? C00C C005 C008 C004 60.6(2) . . . . ? C00C C006 C00E C00H 59.9(2) . . . . ? C00C C006 C009 C004 -60.3(2) . . . . ? C00D C007 C00I C00F -66.72(17) . . . . ? C00D C007 C00J C00F 65.77(17) . . . . ? C00E C006 C00C C005 -60.1(2) . . . . ? C00E C006 C009 C004 60.4(2) . . . . ? C00G C005 C00C C006 59.9(2) . . . . ? C00G C005 C008 C004 -59.6(2) . . . . ? C00I C00F C00J C007 34.53(16) . . . . ? C00I C00F C00K C00D -45.09(19) . . . . ? C00I C007 C00D C00B 163.84(17) . . . . ? C00I C007 C00D C00K 44.08(18) . . . . ? C00I C007 C00J C00F -34.21(16) . . . . ? C00J C00F C00I C007 -34.39(15) . . . . ? C00J C00F C00K C00D 44.20(19) . . . . ? C00J C007 C00D C00B 75.7(2) . . . . ? C00J C007 C00D C00K -44.08(18) . . . . ? C00J C007 C00I C00F 34.35(15) . . . . ? C00K C00F C00I C007 68.11(17) . . . . ? C00K C00F C00J C007 -66.91(18) . . . . ? C003 C004 C00A C00H -176.25(17) . . . . ? C003 C004 C008 C005 175.85(16) . . . . ? C003 C004 C009 C006 179.79(18) . . . . ? C003 C007 C00D C00B -55.5(2) . . . . ? C003 C007 C00D C00K -175.27(17) . . . . ? C003 C007 C00I C00F 158.3(2) . . . . ? C003 C007 C00J C00F -164.6(2) . . . . ? C004 C00A C00H C00E -59.5(2) . . . . ? C004 C00A C00H C00G 60.3(2) . . . . ? C004 C003 C007 C00D -71.7(3) . . . . ? C004 C003 C007 C00I 57.3(3) . . . . ? C004 C003 C007 C00J 165.9(2) . . . . ? C005 C00G C00H C00A -59.9(2) . . . . ? C005 C00G C00H C00E 59.7(2) . . . . ? C006 C00E C00H C00A 59.9(2) . . . . ? C006 C00E C00H C00G -59.5(2) . . . . ? C007 C00D C00K C00F 0.14(18) . . . . ? C007 C003 C004 C00A -142.34(19) . . . . ? C007 C003 C004 C008 100.3(2) . . . . ? C007 C003 C004 C009 -20.6(3) . . . . ? C008 C004 C00A C00H -59.5(2) . . . . ? C008 C004 C009 C006 59.5(2) . . . . ? C008 C005 C00C C006 -60.6(2) . . . . ? C008 C005 C00G C00H 60.1(2) . . . . ? C009 C004 C00A C00H 58.9(2) . . . . ? C009 C004 C008 C005 -59.9(2) . . . . ? C009 C006 C00C C005 60.5(2) . . . . ? C009 C006 C00E C00H -60.7(2) . . . . ? _shelx_res_file ; TITL s5834a_a.res in P2(1)/c s5834a.res created by SHELXL-2018/3 at 12:16:35 on 26-May-2021 REM Old TITL s5834a in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.169, Rweak 0.353, Alpha 0.029 REM 0.830 for 140 systematic absences, Orientation as input REM Formula found by SHELXT: C18 N O CELL 0.71073 10.0176 12.8217 11.5215 90 106.552 90 ZERR 4 0.0008 0.0009 0.0008 0 0.007 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 72 92 4 4 L.S. 10 PLAN 1 SIZE 0.25 0.2 0.3 TEMP -173.14(10) CONF BOND list 4 fmap 2 53 MORE -1 BOND $H ACTA REM REM REM WGHT 0.050300 0.958300 FVAR 0.88579 O001 4 0.625602 0.684954 0.860992 11.00000 0.02604 0.03487 = 0.01421 0.00346 0.00912 0.00922 N002 3 0.638861 0.977023 0.787215 11.00000 0.04274 0.02095 = 0.02832 -0.00363 0.00565 -0.00077 C003 1 0.634126 0.683798 0.757283 11.00000 0.01962 0.01311 = 0.01476 0.00013 0.00516 -0.00109 C004 1 0.763169 0.636283 0.731735 11.00000 0.01622 0.01364 = 0.01148 0.00038 0.00494 0.00084 C005 1 1.018829 0.668737 0.758202 11.00000 0.01804 0.02392 = 0.01747 -0.00464 0.00429 -0.00485 AFIX 13 H005 2 1.096132 0.720494 0.785406 11.00000 -1.20000 AFIX 0 C006 1 0.879551 0.562707 0.582750 11.00000 0.01992 0.02202 = 0.01466 -0.00502 0.00531 0.00175 AFIX 13 H006 2 0.866116 0.545462 0.495520 11.00000 -1.20000 AFIX 0 C007 1 0.518908 0.734686 0.659776 11.00000 0.01693 0.01538 = 0.01756 -0.00035 0.00658 0.00052 C008 1 0.883357 0.716010 0.773209 11.00000 0.02133 0.01560 = 0.01455 -0.00241 0.00493 -0.00315 AFIX 23 H00A 2 0.859916 0.780386 0.724167 11.00000 -1.20000 H00B 2 0.896415 0.734599 0.859130 11.00000 -1.20000 AFIX 0 C009 1 0.743720 0.609344 0.597859 11.00000 0.02035 0.01980 = 0.01309 -0.00289 0.00349 0.00075 AFIX 23 H00C 2 0.718936 0.673079 0.547834 11.00000 -1.20000 H00D 2 0.666897 0.558462 0.570019 11.00000 -1.20000 AFIX 0 C00A 1 0.803277 0.536465 0.808236 11.00000 0.01899 0.01809 = 0.01756 0.00383 0.00531 0.00162 AFIX 23 H00E 2 0.816494 0.553156 0.894678 11.00000 -1.20000 H00F 2 0.727020 0.484811 0.783043 11.00000 -1.20000 AFIX 0 C00B 1 0.601310 0.918150 0.710104 11.00000 0.02281 0.01880 = 0.02266 0.00351 0.00706 0.00196 C00C 1 0.997941 0.642440 0.623957 11.00000 0.02054 0.02679 = 0.01848 0.00163 0.00813 0.00132 AFIX 23 H00G 2 0.974510 0.706561 0.574448 11.00000 -1.20000 H00H 2 1.084995 0.613206 0.612950 11.00000 -1.20000 AFIX 0 C00D 1 0.552782 0.842375 0.611985 11.00000 0.02235 0.01646 = 0.01390 0.00110 0.00506 0.00144 AFIX 13 H00I 2 0.622446 0.834349 0.565347 11.00000 -1.20000 AFIX 0 C00E 1 0.916431 0.463318 0.658203 11.00000 0.01849 0.02125 = 0.02517 -0.00389 0.00609 0.00523 AFIX 23 H00J 2 1.002585 0.432458 0.647168 11.00000 -1.20000 H00K 2 0.840387 0.411707 0.631134 11.00000 -1.20000 AFIX 0 C00F 1 0.326839 0.770996 0.545384 11.00000 0.01634 0.02569 = 0.02033 0.00181 0.00325 0.00237 AFIX 13 H00L 2 0.225839 0.762551 0.501421 11.00000 -1.20000 AFIX 0 C00G 1 1.056089 0.569447 0.834154 11.00000 0.01904 0.02704 = 0.01956 -0.00018 0.00384 0.00259 AFIX 23 H00M 2 1.070385 0.586163 0.920733 11.00000 -1.20000 H00N 2 1.143766 0.539788 0.824981 11.00000 -1.20000 AFIX 0 C00H 1 0.938047 0.489562 0.792372 11.00000 0.02096 0.01739 = 0.02106 0.00369 0.00428 0.00506 AFIX 13 H00O 2 0.962292 0.424677 0.842093 11.00000 -1.20000 AFIX 0 C00I 1 0.430995 0.683486 0.539309 11.00000 0.02095 0.02040 = 0.01925 -0.00238 0.00428 0.00062 AFIX 23 H00P 2 0.471958 0.689185 0.470858 11.00000 -1.20000 H00Q 2 0.398143 0.611863 0.547927 11.00000 -1.20000 AFIX 0 C00J 1 0.377290 0.757609 0.685065 11.00000 0.01705 0.02263 = 0.02104 0.00229 0.00595 0.00183 AFIX 23 H00R 2 0.336071 0.697638 0.716677 11.00000 -1.20000 H00S 2 0.375308 0.822094 0.731807 11.00000 -1.20000 AFIX 0 C00K 1 0.404451 0.868345 0.524598 11.00000 0.02356 0.02073 = 0.01506 0.00118 0.00498 0.00600 AFIX 23 H00T 2 0.365012 0.932665 0.549169 11.00000 -1.20000 H00U 2 0.405856 0.874583 0.439308 11.00000 -1.20000 AFIX 0 HKLF 4 REM s5834a_a.res in P2(1)/c REM wR2 = 0.1549, GooF = S = 1.038, Restrained GooF = 1.038 for all data REM R1 = 0.0626 for 2326 Fo > 4sig(Fo) and 0.0883 for all 3239 data REM 181 parameters refined using 0 restraints END WGHT 0.0503 0.9583 REM Highest difference peak 0.327, deepest hole -0.261, 1-sigma level 0.061 Q1 1 0.7615 0.6336 0.6743 11.00000 0.05 0.33 ; _shelx_res_checksum 74031 _shelx_hkl_file ; 0 0 2 9998.21 59.39 0 0 2 9999.00 67.59 0 0 -2 9893.13 56.81 0 0 3 1.82 1.51 0 0 -3 0.96 1.14 0 0 3 3.22 1.61 0 0 -3 0.66 1.19 0 0 -4 106.01 10.16 0 0 4 107.48 8.87 0 0 -4 103.59 8.41 0 0 4 87.58 9.11 0 0 5 18.10 4.45 0 0 -5 32.37 6.20 0 0 5 30.27 7.17 0 0 6 249.42 19.40 0 0 -6 279.06 17.31 0 0 -7 163.80 14.49 0 0 7 105.15 8.46 0 0 7 129.80 15.64 0 0 7 150.65 17.36 0 0 8 62.36 11.14 0 0 8 54.36 10.92 0 0 8 62.72 6.59 0 0 -8 77.97 10.59 0 0 9 4.28 4.86 0 0 -9 3.63 3.34 0 0 10 41.54 10.11 0 0 -10 36.55 7.95 0 0 -11 -2.27 2.46 0 0 11 0.28 4.46 0 0 12 21.34 8.54 0 0 13 2.07 6.80 0 0 14 82.15 18.96 0 1 2 3488.12 42.01 0 1 -2 3574.99 27.56 0 -1 -2 3487.20 42.79 0 -1 -2 3580.61 40.68 0 1 2 3512.76 43.17 0 -1 -2 3554.17 45.25 0 -1 2 3522.90 27.71 0 1 3 487.83 18.53 0 -1 3 441.18 12.97 0 -1 -3 469.82 17.89 0 1 3 452.95 18.07 0 -1 -3 493.61 20.10 0 1 -3 455.74 12.80 0 -1 3 453.88 17.12 0 1 -4 1606.88 28.95 0 -1 4 1547.43 29.74 0 -1 -4 1614.91 36.63 0 -1 -4 1609.91 41.65 0 -1 4 1638.12 37.66 0 1 4 1592.46 38.52 0 1 4 1578.10 38.04 0 1 5 1451.29 41.17 0 -1 -5 1501.02 38.53 0 -1 5 1493.50 34.01 0 -1 5 1529.63 41.26 0 1 -5 1539.63 32.12 0 1 6 389.88 10.11 0 -1 6 365.10 22.21 0 -1 -6 397.69 21.60 0 1 6 382.27 23.53 0 -1 6 356.69 18.95 0 1 -6 413.90 18.52 0 1 7 2.78 0.94 0 -1 7 -0.96 1.65 0 -1 -7 -0.56 2.27 0 1 7 1.54 2.63 0 1 -7 -0.07 1.14 0 -1 8 16.40 3.90 0 -1 8 23.94 6.90 0 1 -8 19.53 4.59 0 -1 -8 21.05 5.94 0 1 8 23.37 7.13 0 1 -9 -0.59 2.22 0 1 9 -0.78 2.69 0 -1 9 -1.60 3.26 0 -1 -9 3.71 3.66 0 -1 -10 -5.35 4.49 0 1 -10 4.41 3.68 0 1 10 1.22 3.66 0 -1 10 -6.06 4.40 0 1 11 -5.09 4.42 0 -1 11 -4.73 6.08 0 -1 -11 0.42 2.15 0 -1 12 317.83 31.94 0 1 12 405.46 37.16 0 -1 13 79.48 17.45 0 1 13 78.39 17.18 0 1 14 21.73 10.41 0 -1 14 7.18 5.57 0 -2 -1 5994.66 58.00 0 2 1 6077.98 59.44 0 -2 -2 383.02 9.98 0 -2 -2 392.58 16.87 0 2 2 387.65 16.89 0 -2 3 39.81 3.56 0 2 3 52.32 6.99 0 -2 -3 41.33 5.77 0 -2 -3 51.07 7.00 0 -2 -3 33.66 5.45 0 -2 -4 196.03 14.30 0 -2 4 195.62 9.24 0 2 4 178.56 14.29 0 2 -5 84.23 7.04 0 -2 5 80.47 7.10 0 2 5 101.65 12.14 0 -2 5 75.06 9.09 0 -2 -5 81.77 10.18 0 -2 6 49.71 6.37 0 -2 -6 53.36 8.47 0 -2 6 53.79 8.49 0 2 -6 54.63 6.25 0 2 6 60.98 9.92 0 -2 -7 652.35 31.26 0 2 7 658.00 34.65 0 -2 7 670.64 25.68 0 -2 7 650.61 31.39 0 2 -7 632.83 23.94 0 2 -8 477.99 22.04 0 -2 8 482.00 29.19 0 2 8 457.05 30.91 0 -2 -8 478.07 28.59 0 2 9 91.80 15.02 0 -2 9 68.33 11.80 0 -2 -9 83.81 12.60 0 2 -9 71.12 9.44 0 -2 10 685.89 39.08 0 2 10 692.18 44.02 0 -2 -10 623.32 35.97 0 -2 11 292.85 29.07 0 2 11 287.32 29.99 0 -2 -11 291.74 26.00 0 2 12 3.96 4.45 0 -2 -12 1.26 2.53 0 -2 13 23.20 9.04 0 2 13 56.97 14.89 0 2 14 158.86 26.87 0 -2 14 115.88 21.72 0 3 0 -1.16 1.79 0 -3 0 0.03 1.51 0 -3 -1 220.00 13.11 0 3 1 207.19 12.98 0 -3 1 222.50 10.90 0 -3 -2 61.37 7.73 0 3 2 67.95 8.11 0 -3 -2 55.23 5.22 0 -3 -3 41.57 6.28 0 -3 -3 50.37 4.32 0 -3 -3 41.54 6.87 0 -3 -4 1089.93 15.60 0 -3 4 1097.04 21.01 0 -3 -4 1094.39 37.11 0 -3 5 32.75 4.22 0 -3 -5 33.51 6.93 0 -3 6 158.83 14.46 0 -3 6 139.50 9.62 0 -3 -6 172.26 17.10 0 -3 7 82.70 11.44 0 -3 -7 96.73 12.99 0 -3 7 105.07 9.56 0 -3 8 1153.12 44.81 0 -3 8 1137.50 33.83 0 3 8 1095.56 49.96 0 -3 -8 1207.96 47.59 0 -3 -9 30.38 8.34 0 -3 9 47.17 9.61 0 3 9 42.39 10.30 0 -3 -10 457.37 32.36 0 3 10 443.45 35.95 0 -3 10 496.46 32.97 0 -3 -11 74.65 13.76 0 -3 11 80.47 14.14 0 -3 -12 26.88 8.40 0 -3 13 108.87 19.89 0 -3 14 61.72 15.78 0 4 0 149.46 11.77 0 -4 0 151.69 11.36 0 -4 1 3749.43 53.05 0 4 1 3723.87 62.92 0 -4 -1 3807.73 60.73 0 -4 -2 1966.26 37.92 0 -4 -2 2036.39 48.05 0 -4 2 1972.04 35.35 0 -4 -3 2779.37 59.77 0 -4 -3 2598.38 40.30 0 -4 -4 192.53 9.58 0 -4 -4 209.08 17.80 0 -4 5 105.26 7.10 0 -4 -5 113.62 5.64 0 -4 -5 110.33 13.44 0 -4 -6 880.48 39.61 0 -4 6 826.57 21.40 0 -4 -7 85.22 12.73 0 -4 7 76.81 7.31 0 -4 7 85.15 11.45 0 -4 8 891.19 39.80 0 -4 -8 883.55 43.15 0 -4 9 890.69 41.88 0 -4 -9 972.04 47.28 0 -4 -10 1.93 2.93 0 -4 10 4.55 3.99 0 -4 -11 23.12 8.22 0 -4 -12 10.69 6.63 0 -4 -13 93.29 17.28 0 5 0 0.88 2.07 0 -5 0 3.10 2.79 0 -5 1 121.97 10.78 0 -5 -1 152.31 13.50 0 -5 -2 514.21 22.49 0 -5 -2 587.80 28.31 0 -5 2 581.56 22.21 0 -5 3 598.26 21.27 0 -5 -3 607.93 22.85 0 -5 -3 589.38 29.65 0 -5 -4 84.04 7.81 0 -5 -4 79.81 12.08 0 -5 -5 236.61 11.31 0 -5 5 221.29 10.73 0 -5 6 14.25 2.75 0 -5 -6 15.65 5.58 0 -5 -7 102.86 15.09 0 -5 7 84.59 6.89 0 -5 8 4.92 4.08 0 -5 -8 4.19 5.04 0 -5 -9 313.04 28.12 0 -5 9 300.54 24.40 0 -5 10 214.19 21.60 0 -5 -10 228.65 24.99 0 -5 -11 21.31 8.17 0 -5 -12 56.48 13.52 0 -5 -13 13.07 6.96 0 -6 0 299.89 19.63 0 -6 -1 24.04 5.82 0 -6 1 31.48 6.37 0 -6 -2 326.40 22.51 0 -6 2 344.73 18.93 0 -6 -3 184.03 19.41 0 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28.07 10.66 9 9 1 13.92 8.15 9 9 2 6.15 6.04 9 9 3 11.96 7.39 9 -10 -7 0.11 3.90 9 10 -7 3.56 4.24 9 -10 -6 137.52 27.48 9 10 -6 138.30 26.24 9 10 -5 41.13 14.35 9 10 -4 11.36 7.27 9 10 -3 459.47 45.63 9 10 -2 20.16 10.03 9 10 -1 99.38 21.28 9 10 0 89.07 20.45 9 10 1 37.80 12.83 9 10 2 1.31 4.49 -9 -10 -2 -3.25 4.62 9 10 3 49.44 14.62 9 11 -4 1.23 4.52 9 11 -3 44.76 15.53 9 11 -2 184.07 29.87 9 11 -1 4.20 6.08 9 11 0 96.47 21.47 9 11 1 24.09 10.46 -9 -11 -1 36.93 12.23 9 11 2 9.32 7.87 -10 0 11 7.21 4.51 -10 0 10 19.33 10.60 10 0 -10 3.34 3.01 10 0 -9 -0.31 2.86 10 0 -8 237.91 27.84 10 0 -7 12.24 6.91 10 0 -6 135.77 20.95 10 0 -5 -7.45 5.48 10 0 -4 116.38 20.14 10 0 -3 1.37 3.84 10 0 -2 0.85 2.97 10 0 -1 -3.08 4.73 10 0 0 63.83 16.10 10 0 1 -9.75 6.41 10 0 2 6.25 5.63 10 0 3 2.41 2.92 10 0 4 28.45 10.96 10 0 5 9.22 6.32 10 0 6 41.49 13.13 -10 1 11 -4.17 5.94 -10 -1 11 1.75 5.04 10 1 -11 5.83 5.91 -10 1 10 195.19 30.60 10 -1 -10 241.33 27.67 10 1 -10 191.37 26.00 10 -1 -9 -1.75 2.91 -10 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5.35 10 3 3 40.83 12.69 10 -3 3 48.27 13.10 10 3 4 6.63 5.43 10 -3 4 13.89 8.87 10 3 5 59.46 15.22 10 -3 5 58.55 15.49 10 -3 6 15.98 8.72 10 -3 6 32.16 12.52 10 4 -11 69.75 16.72 10 -4 -11 80.33 19.03 -10 4 11 62.31 17.76 10 -4 -10 25.69 11.08 -10 4 10 6.59 4.26 10 4 -10 29.58 11.33 10 -4 -9 39.63 11.38 -10 4 9 37.62 12.56 10 4 -9 63.04 15.94 10 -4 -8 24.49 9.26 -10 4 8 18.02 7.74 10 4 -8 39.52 12.73 10 -4 -7 -2.15 2.30 -10 4 7 -0.20 2.33 10 4 -7 -6.86 7.51 10 -4 -6 17.52 7.13 -10 4 6 17.71 7.77 10 4 -6 27.44 10.58 10 -4 -5 66.10 14.86 -10 4 5 53.83 12.94 10 4 -5 71.71 16.68 -10 4 4 22.70 7.51 10 4 -4 30.77 11.47 10 -4 -4 18.41 8.05 10 4 -3 3.27 5.41 10 4 -2 10.68 6.02 10 4 -1 8.00 6.06 10 4 0 10.38 7.50 10 4 1 51.14 14.17 10 4 2 7.33 5.96 10 -4 3 20.29 8.36 10 4 3 10.85 6.45 10 -4 4 39.65 12.01 10 4 4 26.62 10.13 10 -4 5 17.94 8.38 10 -4 6 4.80 5.79 10 -5 -11 24.31 11.22 10 5 -11 18.02 9.20 -10 5 11 9.65 6.46 10 5 -10 12.99 7.32 10 -5 -10 7.47 6.69 -10 5 10 5.05 6.49 -10 5 9 256.38 33.15 10 -5 -9 197.79 24.99 10 5 -9 164.98 26.18 10 -5 -8 50.93 13.44 -10 5 8 54.99 14.89 10 5 -8 52.71 15.17 10 -5 -7 -1.30 4.98 -10 5 7 2.72 4.86 10 5 -7 -0.93 6.46 10 -5 -6 8.16 7.24 -10 5 6 0.52 2.46 10 5 -6 3.01 3.99 -10 5 5 15.02 6.60 10 5 -5 12.33 7.56 10 -5 -5 0.80 3.34 -10 5 4 1.88 3.32 10 5 -4 2.23 4.55 10 5 -3 13.87 7.51 10 5 -2 5.88 6.19 10 5 -1 227.89 29.47 10 5 0 117.38 21.25 10 5 1 62.35 15.62 10 5 2 58.48 14.97 10 5 3 4.39 5.06 10 5 4 2.02 3.57 10 -5 4 7.33 6.12 10 -5 5 15.38 8.28 10 -5 6 4.34 3.30 10 6 -12 194.64 30.36 10 -6 -12 243.88 34.29 10 -6 -11 90.87 21.38 10 6 -11 86.25 19.30 10 -6 -10 185.68 30.41 10 6 -10 204.57 30.42 -10 6 10 193.30 29.63 10 6 -9 143.24 24.89 10 -6 -9 140.60 26.49 -10 6 9 131.35 23.71 10 -6 -8 8.44 4.82 -10 6 8 9.37 6.98 10 6 -8 8.80 3.83 10 -6 -7 46.51 13.29 -10 6 7 39.61 11.96 10 6 -7 31.38 12.00 -10 6 6 32.55 10.12 10 6 -6 33.37 11.05 10 -6 -6 37.03 11.75 -10 6 5 -8.01 5.04 10 6 -5 -0.17 2.66 10 6 -4 -0.67 3.64 10 6 -3 9.95 5.73 10 6 -2 3.91 5.32 10 6 -1 94.74 19.35 10 6 0 26.76 11.54 10 6 1 25.07 10.32 10 6 2 129.98 23.06 10 6 3 41.42 13.06 10 6 4 83.07 18.37 10 7 -11 -5.65 8.10 10 -7 -10 3.71 6.30 10 7 -10 24.23 11.37 -10 7 10 16.72 9.78 10 -7 -9 26.07 11.50 10 7 -9 27.55 11.63 -10 7 9 43.07 13.58 10 -7 -8 119.00 20.44 10 7 -8 138.57 25.17 -10 7 8 127.18 22.09 -10 7 7 39.62 12.09 10 -7 -7 32.76 10.84 10 7 -7 17.77 9.11 -10 7 6 -2.04 3.99 10 7 -6 1.62 4.54 10 7 -5 15.51 8.06 10 7 -4 4.31 4.81 10 7 -3 -2.75 7.28 10 7 -2 9.81 7.21 10 7 -1 0.63 3.67 10 7 0 44.20 14.41 10 7 1 1.98 3.70 10 7 2 183.53 27.47 10 7 3 21.15 9.64 10 -8 -9 25.71 12.25 10 8 -9 39.50 13.76 10 8 -8 27.67 12.14 10 -8 -8 8.24 5.27 10 8 -7 6.66 5.48 10 8 -6 -0.80 5.25 10 8 -5 4.52 3.56 10 8 -4 31.04 12.30 10 8 -3 91.09 20.11 10 8 -2 143.60 25.24 10 8 -1 117.82 22.62 10 8 0 -1.91 2.43 10 8 1 105.98 21.42 10 8 2 11.64 7.45 10 8 3 134.97 24.02 10 9 -6 11.49 8.20 10 9 -5 12.41 7.73 10 9 -4 130.81 25.01 10 9 -3 86.95 20.49 10 9 -2 79.24 19.35 10 9 -1 120.06 23.47 10 9 0 84.29 19.80 10 9 1 -3.43 5.28 10 9 2 48.62 15.39 10 9 3 14.55 8.81 10 10 -1 62.34 17.70 11 0 -10 13.11 7.97 -11 0 10 3.40 3.67 11 0 -9 -3.29 5.56 11 0 -8 57.50 14.73 11 0 -7 1.28 2.76 11 0 -6 72.22 16.54 11 0 -5 3.88 6.20 11 0 -4 634.65 49.12 11 0 -3 -0.11 3.60 11 0 -2 13.39 7.30 11 0 -1 5.44 3.81 11 0 0 77.41 18.43 11 0 1 -14.33 8.17 11 0 2 120.36 22.55 11 0 3 -6.37 6.08 11 0 4 -1.59 5.56 11 -1 -10 186.35 26.07 -11 1 10 206.16 32.17 11 1 -10 189.74 27.51 11 -1 -9 3.70 3.84 -11 1 9 12.00 8.47 11 1 -9 1.08 3.37 11 -1 -8 58.06 14.17 11 1 -8 57.65 14.75 -11 1 8 66.59 17.22 11 -1 -7 2.40 5.15 11 1 -7 33.24 11.60 11 -1 -6 14.86 7.30 11 1 -6 -1.39 5.70 11 -1 -5 80.14 16.72 11 1 -5 105.32 19.82 11 -1 -4 12.81 7.27 11 1 -4 12.94 6.91 11 -1 -3 193.20 27.34 11 1 -3 145.11 23.87 11 -1 -2 8.23 6.55 11 1 -2 13.35 8.37 11 -1 -1 14.96 7.16 11 1 -1 27.04 10.95 11 -1 0 52.08 14.90 11 1 0 75.80 17.46 11 -1 1 14.05 8.22 11 1 1 4.33 5.67 11 -1 2 12.38 8.66 11 1 2 16.27 8.81 11 -1 3 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10.78 11 3 -7 10.46 4.93 11 -3 -6 19.43 8.81 11 3 -6 13.71 6.74 11 -3 -5 4.83 5.07 11 3 -5 9.28 6.76 -11 3 5 0.12 2.19 11 -3 -4 43.64 14.20 11 3 -4 32.46 12.27 -11 3 4 23.20 8.18 11 -3 -3 43.92 13.24 11 3 -3 31.66 11.28 11 -3 -2 14.15 8.99 11 3 -2 7.16 5.76 11 -3 -1 8.71 7.51 11 3 -1 -3.76 7.49 11 3 0 -2.18 4.78 11 -3 0 -1.18 4.02 11 3 1 6.81 5.89 11 -3 1 -5.96 6.65 11 3 2 24.58 10.10 11 -3 2 23.02 11.09 11 3 3 144.54 24.67 11 -3 3 185.27 29.48 11 3 4 36.17 12.26 11 4 -11 36.34 12.50 11 -4 -11 28.57 12.00 -11 4 10 14.41 7.65 11 4 -10 17.14 8.28 11 -4 -9 91.48 18.08 -11 4 9 102.77 21.54 11 4 -9 110.59 21.92 11 -4 -8 21.19 9.23 -11 4 8 19.54 9.89 11 4 -8 15.08 7.30 11 -4 -7 5.11 4.65 -11 4 7 4.09 4.09 11 4 -7 -0.56 3.47 11 -4 -6 70.24 16.26 -11 4 6 78.64 16.62 11 4 -6 86.00 19.04 11 -4 -5 49.16 14.16 -11 4 5 38.16 11.33 11 4 -5 35.29 12.47 11 -4 -4 10.69 6.13 11 4 -4 16.32 8.56 11 4 -3 17.11 9.20 11 -4 -3 0.63 6.67 11 4 -2 109.34 21.11 11 -4 -2 107.18 21.71 11 4 -1 89.64 19.06 11 -4 -1 98.98 21.03 11 4 0 7.93 5.35 11 4 1 14.35 8.87 11 4 2 -6.13 4.77 11 4 3 31.03 11.39 11 4 4 100.41 20.85 11 5 -11 26.68 11.54 11 -5 -11 23.62 11.45 11 5 -10 -0.92 5.82 11 -5 -10 11.85 10.01 -11 5 10 19.13 10.38 11 -5 -9 -4.00 5.60 -11 5 9 12.08 8.04 11 5 -9 10.55 6.45 11 -5 -8 14.99 8.64 -11 5 8 20.55 9.63 11 5 -8 7.29 5.92 11 -5 -7 6.11 5.95 -11 5 7 9.42 6.63 11 5 -7 16.86 9.50 11 -5 -6 18.28 9.12 -11 5 6 0.99 3.80 11 5 -6 16.83 8.60 11 -5 -5 11.37 7.10 11 5 -5 11.13 7.98 11 5 -4 -5.34 4.13 11 -5 -4 -13.33 7.95 11 5 -3 17.07 9.24 11 5 -2 281.62 34.48 11 5 -1 111.55 21.41 11 5 0 402.39 41.60 11 5 1 -12.09 7.59 11 5 2 -5.53 4.81 11 5 3 8.61 5.57 11 5 4 24.75 9.87 11 -6 -10 34.00 14.30 -11 6 10 11.55 6.65 11 6 -9 11.11 8.24 -11 6 9 9.69 7.01 11 -6 -8 65.07 15.94 -11 6 8 59.41 15.23 11 6 -8 62.63 18.35 11 -6 -7 3.86 4.93 -11 6 7 4.66 2.64 11 6 -7 8.38 8.47 11 -6 -6 73.81 17.43 11 6 -6 102.59 21.56 11 6 -5 -1.10 6.35 11 -6 -5 -3.43 3.45 11 6 -4 -1.06 5.66 11 6 -3 24.73 10.74 11 6 -2 9.62 7.48 11 6 -1 23.64 11.21 11 6 0 199.93 29.64 11 6 1 11.90 8.41 11 6 2 8.02 6.02 11 6 3 36.16 13.20 -11 7 9 3.19 5.03 11 -7 -8 4.39 4.49 -11 7 8 11.41 6.75 11 -7 -7 11.89 7.44 11 7 -7 29.44 12.37 11 7 -6 -0.23 4.34 11 -7 -6 10.93 8.19 11 7 -5 1.14 3.60 11 7 -4 15.48 8.62 11 7 -3 24.60 11.56 11 7 -2 38.27 13.64 11 7 -1 183.25 29.25 11 7 0 87.79 20.13 11 7 1 113.29 23.05 11 -8 -7 -4.60 3.94 12 0 -10 31.98 11.55 12 0 -9 4.67 5.01 12 0 -8 66.39 17.28 12 0 -7 9.56 7.28 12 0 -6 88.76 19.39 12 0 -5 12.29 8.70 12 0 -4 209.64 30.38 12 0 -3 -1.94 4.56 12 0 -2 209.82 30.53 12 0 -1 5.39 5.34 12 0 0 34.18 12.56 12 -1 -10 298.71 34.98 12 1 -10 286.40 35.39 12 -1 -9 41.80 13.24 -12 1 9 38.36 14.15 12 1 -9 40.38 13.17 12 -1 -8 5.02 3.78 12 1 -8 -0.21 6.14 -12 1 8 9.01 7.94 12 -1 -7 10.78 7.22 12 1 -7 9.28 7.00 12 -1 -6 -11.94 7.61 12 1 -6 1.25 3.37 12 -1 -5 57.27 15.67 12 1 -5 35.30 11.64 12 -1 -4 1.61 4.57 12 1 -4 7.06 8.03 12 -1 -3 190.65 29.20 12 1 -3 221.24 31.27 12 -1 -2 123.29 23.78 12 1 -2 156.30 26.14 12 -1 -1 2.89 4.00 12 1 -1 5.80 6.41 12 -1 0 8.54 6.78 12 1 0 11.74 7.79 12 2 -11 128.11 24.26 12 -2 -10 0.61 3.06 12 2 -10 7.04 7.14 12 -2 -9 -1.43 5.21 -12 2 9 -0.27 2.72 12 2 -9 1.20 5.23 12 -2 -8 30.52 12.03 -12 2 8 27.11 11.17 12 2 -8 26.75 10.57 12 -2 -7 135.94 24.11 12 2 -7 101.33 20.85 -12 2 7 106.94 21.33 12 -2 -6 17.48 8.98 12 2 -6 3.00 2.51 -12 2 6 15.13 8.12 12 -2 -5 28.19 12.04 12 2 -5 41.99 13.80 -12 2 5 29.98 10.66 12 -2 -4 6.27 7.16 12 2 -4 -0.76 4.14 12 -2 -3 6.79 7.11 12 2 -3 15.01 8.99 12 -2 -2 80.01 19.08 12 2 -2 57.45 16.33 12 -2 -1 69.37 17.47 12 2 -1 45.64 14.55 12 2 0 5.45 5.82 12 3 -10 -2.23 6.15 -12 3 9 310.65 39.08 12 -3 -9 304.62 35.32 12 3 -9 326.13 38.99 12 -3 -8 38.61 12.80 -12 3 8 28.21 11.52 12 3 -8 35.31 13.26 12 -3 -7 1.82 3.25 -12 3 7 10.24 7.17 12 3 -7 -2.64 6.84 12 -3 -6 40.08 13.28 -12 3 6 61.21 15.71 12 -3 -5 24.06 10.36 12 3 -5 21.92 9.73 12 -3 -4 198.15 29.82 12 3 -4 225.96 31.89 12 -3 -3 6.96 5.33 12 3 -3 -2.89 4.47 12 -3 -2 11.44 5.25 12 3 -2 7.93 4.80 12 -3 -1 54.26 16.29 12 3 -1 101.63 21.89 12 3 0 43.01 14.43 12 -4 -9 146.95 24.62 -12 4 9 106.14 22.74 12 -4 -8 7.93 6.63 -12 4 8 15.51 8.04 12 4 -8 10.02 7.26 12 -4 -7 65.17 17.00 -12 4 7 55.85 15.25 12 4 -7 94.15 21.40 12 -4 -6 9.35 6.96 12 4 -6 26.42 11.43 12 -4 -5 2.07 3.96 12 4 -5 1.54 5.12 12 -4 -4 5.67 4.71 12 4 -4 8.19 6.73 12 -4 -3 -4.63 6.46 12 4 -3 4.75 5.74 12 -4 -2 171.22 28.54 12 4 -2 78.51 19.18 12 -5 -9 12.00 6.99 -12 5 9 7.10 5.49 12 -5 -8 27.37 11.38 -12 5 8 16.02 8.21 12 -5 -7 39.06 13.39 12 -5 -6 -4.39 5.07 12 -5 -5 22.11 10.20 12 -5 -4 56.13 16.23 12 -5 -3 12.00 8.49 -12 6 9 18.49 9.32 12 -6 -8 23.82 10.54 12 -6 -7 25.86 11.00 12 -6 -6 34.91 13.09 12 -6 -5 -3.49 4.14 12 -7 -8 -4.56 6.26 12 -7 -7 39.25 13.58 -13 1 8 239.66 35.04 -13 1 7 -12.46 8.03 -13 2 8 58.41 17.29 -13 2 7 23.37 10.95 -13 3 8 -5.68 5.96 0 0 0 0.00 0.00 TITL s5834a in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 10.017628 12.821657 11.521469 90.0000 106.5518 90.0000 ZERR 6.00 0.000757 0.000847 0.000761 0.0000 0.0074 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 66.00 60.00 6.00 6.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 61470 _olex2_date_sample_data_collection 2021-05-25 _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 1.194 _oxdiff_exptl_absorpt_empirical_full_min 0.845