data_ca050221_1_1 _audit_creation_date 2021-02-10 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226) ; _shelx_SHELXL_version_number '2018/3' loop_ _audit_author_name _audit_author_email _audit_author_address 'Georgiev, T.' tony.georgiev@org.chem.ethz.ch LOC-Carreira _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_acknowledgements ; X-Ray services provided by SMoCC - The Small Molecule Crystallography Center of ETH Zurich. ; _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 3-phenyl-1-tosyl-1,2-diazaspirol[4,4]non-2-en-6-ol _chemical_formula_moiety 'C20 H22 N2 O3 S' _chemical_formula_sum 'C20 H22 N2 O3 S' _chemical_formula_weight 370.45 _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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.5364(7) _cell_length_b 10.9885(16) _cell_length_c 25.521(4) _cell_angle_alpha 90 _cell_angle_beta 95.158(4) _cell_angle_gamma 90 _cell_volume 1825.6(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3142 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 27.99 _cell_measurement_theta_min 3.04 _shelx_estimated_absorpt_T_max 0.984 _shelx_estimated_absorpt_T_min 0.950 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0799 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.9014. The \l/2 correction factor is 0.0000. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plank _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_unetI/netI 0.0550 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 16584 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.328 _diffrn_reflns_theta_min 2.019 _diffrn_ambient_temperature 100.0(1) _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 8.33 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'kappa-stage diffractometer' _diffrn_measurement_device_type 'Bruker/Nonius Kappa Apex2' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'double mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatec I\ms high brilliance' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3268 _reflns_number_total 4525 _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 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _refine_diff_density_max 0.332 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.060 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 249 _refine_ls_number_reflns 4525 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0449 _refine_ls_restrained_S_all 1.031 _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^)+(0.0435P)^2^+0.7484P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0988 _refine_ls_wR_factor_ref 0.1107 _refine_special_details 'One disordered methylene group.' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O1-H1 0.93 with sigma of 0.02 C5-C4 \\sim C5A-C4 with sigma of 0.02 C6-C5 \\sim C6-C5A with sigma of 0.02 3. Rigid body (RIGU) restrains C4, C5, C5A, C6 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(H4BC)=Sof(H4BD)=Sof(H6BC)=Sof(H6BD)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(1) Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H6AA)=Sof(H6AB)=FVAR(1) 5.a Ternary CH refined with riding coordinates: C7(H7) 5.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C6(H6AA,H6AB), C6(H6BC,H6BD), C5A(H5AA,H5AB) 5.c Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19) 5.d Idealised Me refined as rotating group: C20(H20A,H20B,H20C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.43563(6) 0.41176(4) 0.66474(2) 0.01693(12) Uani 1 1 d . . . . . O1 O -0.05404(19) 0.60275(12) 0.65474(5) 0.0241(3) Uani 1 1 d D . . . . H1 H -0.178(3) 0.573(2) 0.6510(9) 0.036 Uiso 1 1 d D U . . . O2 O 0.64539(18) 0.39699(11) 0.65356(6) 0.0230(3) Uani 1 1 d . . . . . O3 O 0.35707(19) 0.34253(11) 0.70616(5) 0.0227(3) Uani 1 1 d . . . . . N1 N 0.4101(2) 0.55484(12) 0.68166(6) 0.0158(3) Uani 1 1 d . . . . . N2 N 0.4829(2) 0.63855(13) 0.64576(6) 0.0166(3) Uani 1 1 d . . . . . C1 C 0.4093(2) 0.74407(15) 0.65558(7) 0.0154(4) Uani 1 1 d . . . . . C2 C 0.2697(3) 0.74497(15) 0.69906(7) 0.0192(4) Uani 1 1 d . . . . . H2A H 0.132982 0.778025 0.686634 0.023 Uiso 1 1 calc R U . . . H2B H 0.328700 0.794373 0.729156 0.023 Uiso 1 1 calc R U . . . C3 C 0.2541(3) 0.60933(15) 0.71474(7) 0.0163(4) Uani 1 1 d . . . . . C4 C 0.3042(3) 0.58465(19) 0.77361(8) 0.0271(4) Uani 1 1 d D . . . . H4AA H 0.387384 0.509593 0.778736 0.033 Uiso 0.440(16) 1 calc R U P A 1 H4AB H 0.383965 0.653244 0.790240 0.033 Uiso 0.440(16) 1 calc R U P A 1 H4BC H 0.423530 0.633071 0.788359 0.033 Uiso 0.560(16) 1 calc R U P A 2 H4BD H 0.330776 0.497227 0.780696 0.033 Uiso 0.560(16) 1 calc R U P A 2 C5 C 0.1017(10) 0.5701(10) 0.7986(3) 0.0311(17) Uani 0.440(16) 1 d D . P A 1 H5A H 0.096827 0.624400 0.829392 0.037 Uiso 0.440(16) 1 calc R U P A 1 H5B H 0.082171 0.484940 0.809815 0.037 Uiso 0.440(16) 1 calc R U P A 1 C6 C -0.0684(3) 0.60775(19) 0.75246(9) 0.0296(5) Uani 1 1 d D . . . . H6AA H -0.201055 0.566495 0.756089 0.036 Uiso 0.440(16) 1 calc R U P A 1 H6AB H -0.090039 0.696906 0.751117 0.036 Uiso 0.440(16) 1 calc R U P A 1 H6BC H -0.142559 0.684874 0.744091 0.036 Uiso 0.560(16) 1 calc R U P A 2 H6BD H -0.167637 0.546949 0.763556 0.036 Uiso 0.560(16) 1 calc R U P A 2 C7 C 0.0330(3) 0.56172(16) 0.70434(7) 0.0177(4) Uani 1 1 d . . . . . H7 H 0.034776 0.470728 0.704643 0.021 Uiso 1 1 calc R U . . . C8 C 0.4639(3) 0.85144(15) 0.62540(7) 0.0181(4) Uani 1 1 d . . . . . C9 C 0.3332(3) 0.95254(16) 0.62087(8) 0.0253(4) Uani 1 1 d . . . . . H9 H 0.212525 0.953540 0.639016 0.030 Uiso 1 1 calc R U . . . C10 C 0.3786(4) 1.05143(18) 0.59003(9) 0.0332(5) Uani 1 1 d . . . . . H10 H 0.287635 1.118962 0.586608 0.040 Uiso 1 1 calc R U . . . C11 C 0.5553(4) 1.05171(19) 0.56443(9) 0.0370(6) Uani 1 1 d . . . . . H11 H 0.585345 1.119114 0.543117 0.044 Uiso 1 1 calc R U . . . C12 C 0.6896(4) 0.9537(2) 0.56971(10) 0.0376(6) Uani 1 1 d . . . . . H12 H 0.812847 0.954864 0.552643 0.045 Uiso 1 1 calc R U . . . C13 C 0.6438(3) 0.85397(18) 0.59988(8) 0.0267(4) Uani 1 1 d . . . . . H13 H 0.735733 0.786882 0.603196 0.032 Uiso 1 1 calc R U . . . C14 C 0.2818(3) 0.38397(15) 0.60570(8) 0.0173(4) Uani 1 1 d . . . . . C15 C 0.3609(3) 0.39866(17) 0.55738(8) 0.0228(4) Uani 1 1 d . . . . . H15 H 0.498214 0.425790 0.555837 0.027 Uiso 1 1 calc R U . . . C16 C 0.2382(3) 0.37350(17) 0.51124(8) 0.0257(4) Uani 1 1 d . . . . . H16 H 0.292621 0.383646 0.478233 0.031 Uiso 1 1 calc R U . . . C17 C 0.0355(3) 0.33340(17) 0.51286(8) 0.0235(4) Uani 1 1 d . . . . . C18 C -0.0395(3) 0.31983(18) 0.56169(8) 0.0263(5) Uani 1 1 d . . . . . H18 H -0.176784 0.292878 0.563455 0.032 Uiso 1 1 calc R U . . . C19 C 0.0809(3) 0.34460(17) 0.60795(8) 0.0232(4) Uani 1 1 d . . . . . H19 H 0.026346 0.334733 0.640966 0.028 Uiso 1 1 calc R U . . . C20 C -0.0981(3) 0.3047(2) 0.46310(9) 0.0330(5) Uani 1 1 d . . . . . H20A H -0.052976 0.353147 0.434017 0.049 Uiso 1 1 calc R U . . . H20B H -0.241355 0.324476 0.468030 0.049 Uiso 1 1 calc R U . . . H20C H -0.086878 0.217991 0.454935 0.049 Uiso 1 1 calc R U . . . C5A C 0.1011(9) 0.6275(10) 0.7954(2) 0.0400(18) Uani 0.560(16) 1 d D . P A 2 H5AA H 0.074745 0.579885 0.827026 0.048 Uiso 0.560(16) 1 calc R U P A 2 H5AB H 0.110323 0.714698 0.805129 0.048 Uiso 0.560(16) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0108(2) 0.01176(19) 0.0278(3) 0.00152(18) -0.00105(17) 0.00091(15) O1 0.0118(7) 0.0308(7) 0.0291(8) 0.0026(6) -0.0021(6) -0.0022(5) O2 0.0107(6) 0.0187(6) 0.0392(9) -0.0005(6) -0.0002(6) 0.0029(5) O3 0.0194(7) 0.0179(6) 0.0303(8) 0.0062(6) -0.0014(6) -0.0004(5) N1 0.0118(7) 0.0131(7) 0.0227(8) 0.0010(6) 0.0027(6) -0.0009(5) N2 0.0121(7) 0.0137(7) 0.0240(8) 0.0020(6) 0.0013(6) -0.0019(6) C1 0.0115(8) 0.0156(8) 0.0184(9) -0.0023(7) -0.0027(7) -0.0019(6) C2 0.0190(9) 0.0156(8) 0.0228(10) -0.0029(7) 0.0011(8) -0.0009(7) C3 0.0143(9) 0.0159(8) 0.0186(9) -0.0028(7) 0.0008(7) -0.0011(6) C4 0.0331(11) 0.0275(10) 0.0201(10) -0.0003(8) -0.0013(9) -0.0094(9) C5 0.036(3) 0.034(4) 0.025(3) -0.004(3) 0.006(2) -0.002(3) C6 0.0258(11) 0.0314(11) 0.0337(12) -0.0067(9) 0.0142(9) -0.0027(9) C7 0.0136(9) 0.0181(8) 0.0212(10) -0.0022(7) 0.0010(7) -0.0014(7) C8 0.0214(9) 0.0135(8) 0.0187(9) -0.0014(7) -0.0015(7) -0.0021(7) C9 0.0300(11) 0.0168(9) 0.0285(11) -0.0020(8) -0.0005(9) 0.0022(8) C10 0.0471(14) 0.0146(9) 0.0368(13) 0.0005(9) -0.0029(11) 0.0039(9) C11 0.0594(16) 0.0192(10) 0.0320(13) 0.0066(9) 0.0009(11) -0.0064(10) C12 0.0430(14) 0.0299(11) 0.0418(15) 0.0102(10) 0.0145(11) -0.0044(10) C13 0.0294(11) 0.0210(9) 0.0301(12) 0.0044(8) 0.0053(9) 0.0003(8) C14 0.0136(9) 0.0105(8) 0.0276(10) -0.0026(7) 0.0000(7) 0.0015(6) C15 0.0167(10) 0.0199(9) 0.0322(11) 0.0016(8) 0.0032(8) -0.0024(7) C16 0.0265(11) 0.0233(10) 0.0275(11) 0.0016(8) 0.0029(9) -0.0010(8) C17 0.0205(10) 0.0190(9) 0.0302(12) -0.0064(8) -0.0017(8) 0.0034(7) C18 0.0125(9) 0.0302(10) 0.0362(12) -0.0146(9) 0.0023(8) -0.0023(8) C19 0.0159(9) 0.0250(10) 0.0290(11) -0.0098(8) 0.0041(8) -0.0012(7) C20 0.0279(11) 0.0368(12) 0.0331(13) -0.0100(10) -0.0034(9) 0.0018(9) C5A 0.046(3) 0.050(4) 0.027(3) -0.017(3) 0.019(2) -0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O2 1.4346(13) . ? S1 O3 1.4344(14) . ? S1 N1 1.6429(15) . ? S1 C14 1.7614(19) . ? O1 H1 0.871(16) . ? O1 C7 1.414(2) . ? N1 N2 1.411(2) . ? N1 C3 1.505(2) . ? N2 C1 1.289(2) . ? C1 C2 1.499(3) . ? C1 C8 1.470(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.549(2) . ? C3 C4 1.533(3) . ? C3 C7 1.537(2) . ? C4 H4AA 0.9900 . ? C4 H4AB 0.9900 . ? C4 H4BC 0.9900 . ? C4 H4BD 0.9900 . ? C4 C5 1.529(7) . ? C4 C5A 1.558(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.599(7) . ? C6 H6AA 0.9900 . ? C6 H6AB 0.9900 . ? C6 H6BC 0.9900 . ? C6 H6BD 0.9900 . ? C6 C7 1.533(3) . ? C6 C5A 1.502(6) . ? C7 H7 1.0000 . ? C8 C9 1.400(3) . ? C8 C13 1.395(3) . ? C9 H9 0.9500 . ? C9 C10 1.389(3) . ? C10 H10 0.9500 . ? C10 C11 1.377(3) . ? C11 H11 0.9500 . ? C11 C12 1.389(3) . ? C12 H12 0.9500 . ? C12 C13 1.387(3) . ? C13 H13 0.9500 . ? C14 C15 1.389(3) . ? C14 C19 1.389(3) . ? C15 H15 0.9500 . ? C15 C16 1.392(3) . ? C16 H16 0.9500 . ? C16 C17 1.400(3) . ? C17 C18 1.388(3) . ? C17 C20 1.508(3) . ? C18 H18 0.9500 . ? C18 C19 1.385(3) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C5A H5AA 0.9900 . ? C5A H5AB 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 O2 S1 N1 106.39(7) . . ? O2 S1 C14 107.01(9) . . ? O3 S1 O2 119.90(8) . . ? O3 S1 N1 105.20(8) . . ? O3 S1 C14 108.89(8) . . ? N1 S1 C14 109.09(8) . . ? C7 O1 H1 105.9(16) . . ? N2 N1 S1 113.89(12) . . ? N2 N1 C3 112.96(13) . . ? C3 N1 S1 128.18(11) . . ? C1 N2 N1 107.85(15) . . ? N2 C1 C2 114.38(15) . . ? N2 C1 C8 120.51(16) . . ? C8 C1 C2 125.11(15) . . ? C1 C2 H2A 110.9 . . ? C1 C2 H2B 110.9 . . ? C1 C2 C3 104.10(14) . . ? H2A C2 H2B 109.0 . . ? C3 C2 H2A 110.9 . . ? C3 C2 H2B 110.9 . . ? N1 C3 C2 100.03(13) . . ? N1 C3 C4 112.55(14) . . ? N1 C3 C7 116.19(14) . . ? C4 C3 C2 114.22(15) . . ? C4 C3 C7 102.94(15) . . ? C7 C3 C2 111.44(14) . . ? C3 C4 H4AA 110.1 . . ? C3 C4 H4AB 110.1 . . ? C3 C4 H4BC 111.7 . . ? C3 C4 H4BD 111.7 . . ? C3 C4 C5A 100.5(3) . . ? H4AA C4 H4AB 108.4 . . ? H4BC C4 H4BD 109.4 . . ? C5 C4 C3 108.1(3) . . ? C5 C4 H4AA 110.1 . . ? C5 C4 H4AB 110.1 . . ? C5A C4 H4BC 111.7 . . ? C5A C4 H4BD 111.7 . . ? C4 C5 H5A 111.0 . . ? C4 C5 H5B 111.0 . . ? C4 C5 C6 103.7(4) . . ? H5A C5 H5B 109.0 . . ? C6 C5 H5A 111.0 . . ? C6 C5 H5B 111.0 . . ? C5 C6 H6AA 111.7 . . ? C5 C6 H6AB 111.7 . . ? H6AA C6 H6AB 109.4 . . ? H6BC C6 H6BD 108.6 . . ? C7 C6 C5 100.5(3) . . ? C7 C6 H6AA 111.7 . . ? C7 C6 H6AB 111.7 . . ? C7 C6 H6BC 110.4 . . ? C7 C6 H6BD 110.4 . . ? C5A C6 H6BC 110.4 . . ? C5A C6 H6BD 110.4 . . ? C5A C6 C7 106.8(3) . . ? O1 C7 C3 110.03(15) . . ? O1 C7 C6 116.33(16) . . ? O1 C7 H7 109.2 . . ? C3 C7 H7 109.2 . . ? C6 C7 C3 102.53(15) . . ? C6 C7 H7 109.2 . . ? C9 C8 C1 120.34(17) . . ? C13 C8 C1 121.00(16) . . ? C13 C8 C9 118.65(17) . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.5(2) . . ? C10 C9 H9 119.7 . . ? C9 C10 H10 120.0 . . ? C11 C10 C9 120.09(19) . . ? C11 C10 H10 120.0 . . ? C10 C11 H11 119.9 . . ? C10 C11 C12 120.1(2) . . ? C12 C11 H11 119.9 . . ? C11 C12 H12 120.0 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C8 C13 H13 119.7 . . ? C12 C13 C8 120.52(19) . . ? C12 C13 H13 119.7 . . ? C15 C14 S1 120.66(14) . . ? C19 C14 S1 119.20(15) . . ? C19 C14 C15 120.13(18) . . ? C14 C15 H15 120.1 . . ? C14 C15 C16 119.74(18) . . ? C16 C15 H15 120.1 . . ? C15 C16 H16 119.6 . . ? C15 C16 C17 120.82(19) . . ? C17 C16 H16 119.6 . . ? C16 C17 C20 121.24(19) . . ? C18 C17 C16 118.14(18) . . ? C18 C17 C20 120.61(18) . . ? C17 C18 H18 119.2 . . ? C19 C18 C17 121.67(18) . . ? C19 C18 H18 119.2 . . ? C14 C19 H19 120.2 . . ? C18 C19 C14 119.50(19) . . ? C18 C19 H19 120.2 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4 C5A H5AA 110.3 . . ? C4 C5A H5AB 110.3 . . ? C6 C5A C4 107.0(3) . . ? C6 C5A H5AA 110.3 . . ? C6 C5A H5AB 110.3 . . ? H5AA C5A H5AB 108.6 . . ? 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 S1 N1 N2 C1 164.01(12) . . . . ? S1 N1 C3 C2 -161.62(13) . . . . ? S1 N1 C3 C4 76.74(18) . . . . ? S1 N1 C3 C7 -41.6(2) . . . . ? S1 C14 C15 C16 178.51(14) . . . . ? S1 C14 C19 C18 -178.50(14) . . . . ? O2 S1 N1 N2 50.83(13) . . . . ? O2 S1 N1 C3 -156.18(14) . . . . ? O2 S1 C14 C15 -24.01(16) . . . . ? O2 S1 C14 C19 154.68(14) . . . . ? O3 S1 N1 N2 179.03(11) . . . . ? O3 S1 N1 C3 -27.98(16) . . . . ? O3 S1 C14 C15 -154.97(14) . . . . ? O3 S1 C14 C19 23.71(16) . . . . ? N1 S1 C14 C15 90.71(15) . . . . ? N1 S1 C14 C19 -90.60(15) . . . . ? N1 N2 C1 C2 -1.8(2) . . . . ? N1 N2 C1 C8 178.06(14) . . . . ? N1 C3 C4 C5 -146.1(5) . . . . ? N1 C3 C4 C5A -169.4(4) . . . . ? N1 C3 C7 O1 -70.03(18) . . . . ? N1 C3 C7 C6 165.59(15) . . . . ? N2 N1 C3 C2 -8.43(17) . . . . ? N2 N1 C3 C4 -130.07(15) . . . . ? N2 N1 C3 C7 111.62(16) . . . . ? N2 C1 C2 C3 -3.6(2) . . . . ? N2 C1 C8 C9 155.65(18) . . . . ? N2 C1 C8 C13 -23.0(3) . . . . ? C1 C2 C3 N1 6.69(16) . . . . ? C1 C2 C3 C4 127.12(16) . . . . ? C1 C2 C3 C7 -116.74(16) . . . . ? C1 C8 C9 C10 -176.46(18) . . . . ? C1 C8 C13 C12 177.29(19) . . . . ? C2 C1 C8 C9 -24.6(3) . . . . ? C2 C1 C8 C13 156.77(18) . . . . ? C2 C3 C4 C5 100.7(5) . . . . ? C2 C3 C4 C5A 77.4(4) . . . . ? C2 C3 C7 O1 43.7(2) . . . . ? C2 C3 C7 C6 -80.72(18) . . . . ? C3 N1 N2 C1 6.82(19) . . . . ? C3 C4 C5 C6 -8.3(7) . . . . ? C3 C4 C5A C6 29.1(6) . . . . ? C4 C3 C7 O1 166.51(14) . . . . ? C4 C3 C7 C6 42.13(18) . . . . ? C4 C5 C6 C7 33.6(6) . . . . ? C5 C6 C7 O1 -166.7(4) . . . . ? C5 C6 C7 C3 -46.6(4) . . . . ? C7 C3 C4 C5 -20.3(5) . . . . ? C7 C3 C4 C5A -43.6(4) . . . . ? C7 C6 C5A C4 -3.7(7) . . . . ? C8 C1 C2 C3 176.64(16) . . . . ? C8 C9 C10 C11 -1.3(3) . . . . ? C9 C8 C13 C12 -1.4(3) . . . . ? C9 C10 C11 C12 -0.6(3) . . . . ? C10 C11 C12 C13 1.4(4) . . . . ? C11 C12 C13 C8 -0.4(3) . . . . ? C13 C8 C9 C10 2.2(3) . . . . ? C14 S1 N1 N2 -64.29(13) . . . . ? C14 S1 N1 C3 88.70(16) . . . . ? C14 C15 C16 C17 0.0(3) . . . . ? C15 C14 C19 C18 0.2(3) . . . . ? C15 C16 C17 C18 0.2(3) . . . . ? C15 C16 C17 C20 -179.42(18) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C17 C18 C19 C14 0.0(3) . . . . ? C19 C14 C15 C16 -0.2(3) . . . . ? C20 C17 C18 C19 179.45(18) . . . . ? C5A C6 C7 O1 -143.5(5) . . . . ? C5A C6 C7 C3 -23.4(5) . . . . ? _shelx_res_file ; TITL ca050221_1_1_a.res in P2(1)/c ca050221_1_1.res created by SHELXL-2018/3 at 10:18:59 on 10-Feb-2021 REM Old TITL ca050221_1_1 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.134, Rweak 0.005, Alpha 0.030 REM 0.536 for 209 systematic absences, Orientation as input REM Formula found by SHELXT: C20 N2 O3 S CELL 0.71073 6.5364 10.9885 25.5206 90 95.158 90 ZERR 4 0.0007 0.0016 0.0036 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 80 88 8 12 4 SADI C5 C4 C5A C4 RIGU C4 C5 C5A C6 SADI C6 C5 C6 C5A DFIX 0.93 O1 H1 L.S. 9 PLAN 20 SIZE 0.08 0.1 0.26 TEMP -173.16 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.043500 0.748400 FVAR 0.57236 0.43982 S1 5 0.435635 0.411765 0.664741 11.00000 0.01076 0.01176 = 0.02776 0.00152 -0.00105 0.00091 O1 4 -0.054043 0.602750 0.654741 11.00000 0.01179 0.03080 = 0.02912 0.00262 -0.00212 -0.00224 H1 2 -0.178161 0.573273 0.651044 11.00000 -1.50000 O2 4 0.645393 0.396989 0.653557 11.00000 0.01065 0.01874 = 0.03916 -0.00055 -0.00023 0.00291 O3 4 0.357069 0.342529 0.706162 11.00000 0.01939 0.01790 = 0.03027 0.00620 -0.00144 -0.00044 N1 3 0.410074 0.554842 0.681663 11.00000 0.01184 0.01307 = 0.02267 0.00096 0.00272 -0.00086 N2 3 0.482925 0.638554 0.645757 11.00000 0.01206 0.01369 = 0.02403 0.00201 0.00127 -0.00194 C1 1 0.409307 0.744067 0.655578 11.00000 0.01147 0.01559 = 0.01842 -0.00229 -0.00275 -0.00191 C2 1 0.269692 0.744967 0.699062 11.00000 0.01902 0.01561 = 0.02276 -0.00285 0.00111 -0.00090 AFIX 23 H2A 2 0.132982 0.778025 0.686634 11.00000 -1.20000 H2B 2 0.328700 0.794373 0.729156 11.00000 -1.20000 AFIX 0 C3 1 0.254089 0.609334 0.714743 11.00000 0.01427 0.01593 = 0.01856 -0.00279 0.00080 -0.00110 C4 1 0.304224 0.584654 0.773609 11.00000 0.03310 0.02754 = 0.02010 -0.00031 -0.00130 -0.00940 PART 1 AFIX 23 H4AA 2 0.387384 0.509593 0.778736 21.00000 -1.20000 H4AB 2 0.383965 0.653244 0.790240 21.00000 -1.20000 AFIX 23 PART 2 H4BC 2 0.423530 0.633071 0.788359 -21.00000 -1.20000 H4BD 2 0.330776 0.497227 0.780696 -21.00000 -1.20000 AFIX 0 PART 1 C5 1 0.101669 0.570072 0.798582 21.00000 0.03565 0.03375 = 0.02459 -0.00388 0.00639 -0.00244 AFIX 23 H5A 2 0.096827 0.624400 0.829392 21.00000 -1.20000 H5B 2 0.082171 0.484940 0.809815 21.00000 -1.20000 AFIX 0 PART 0 C6 1 -0.068420 0.607749 0.752463 11.00000 0.02578 0.03141 = 0.03375 -0.00670 0.01419 -0.00269 PART 1 AFIX 23 H6AA 2 -0.201055 0.566495 0.756089 21.00000 -1.20000 H6AB 2 -0.090039 0.696906 0.751117 21.00000 -1.20000 AFIX 23 PART 2 H6BC 2 -0.142559 0.684874 0.744091 -21.00000 -1.20000 H6BD 2 -0.167637 0.546949 0.763556 -21.00000 -1.20000 AFIX 0 PART 0 C7 1 0.033033 0.561724 0.704339 11.00000 0.01365 0.01807 = 0.02117 -0.00215 0.00097 -0.00142 AFIX 13 H7 2 0.034776 0.470728 0.704643 11.00000 -1.20000 AFIX 0 C8 1 0.463889 0.851436 0.625399 11.00000 0.02144 0.01352 = 0.01871 -0.00135 -0.00151 -0.00208 C9 1 0.333199 0.952541 0.620867 11.00000 0.03003 0.01681 = 0.02851 -0.00204 -0.00053 0.00216 AFIX 43 H9 2 0.212525 0.953540 0.639016 11.00000 -1.20000 AFIX 0 C10 1 0.378604 1.051432 0.590034 11.00000 0.04705 0.01463 = 0.03680 0.00047 -0.00294 0.00390 AFIX 43 H10 2 0.287635 1.118962 0.586608 11.00000 -1.20000 AFIX 0 C11 1 0.555269 1.051706 0.564434 11.00000 0.05935 0.01918 = 0.03201 0.00664 0.00094 -0.00643 AFIX 43 H11 2 0.585345 1.119114 0.543117 11.00000 -1.20000 AFIX 0 C12 1 0.689551 0.953661 0.569711 11.00000 0.04305 0.02992 = 0.04183 0.01023 0.01451 -0.00439 AFIX 43 H12 2 0.812847 0.954864 0.552643 11.00000 -1.20000 AFIX 0 C13 1 0.643804 0.853967 0.599883 11.00000 0.02936 0.02105 = 0.03010 0.00444 0.00533 0.00026 AFIX 43 H13 2 0.735733 0.786882 0.603196 11.00000 -1.20000 AFIX 0 C14 1 0.281782 0.383967 0.605701 11.00000 0.01357 0.01047 = 0.02760 -0.00262 -0.00003 0.00152 C15 1 0.360887 0.398665 0.557384 11.00000 0.01666 0.01990 = 0.03215 0.00160 0.00316 -0.00235 AFIX 43 H15 2 0.498214 0.425790 0.555837 11.00000 -1.20000 AFIX 0 C16 1 0.238192 0.373499 0.511241 11.00000 0.02647 0.02329 = 0.02754 0.00161 0.00287 -0.00098 AFIX 43 H16 2 0.292621 0.383646 0.478233 11.00000 -1.20000 AFIX 0 C17 1 0.035479 0.333403 0.512856 11.00000 0.02051 0.01899 = 0.03023 -0.00642 -0.00167 0.00338 C18 1 -0.039476 0.319834 0.561694 11.00000 0.01250 0.03025 = 0.03619 -0.01463 0.00233 -0.00232 AFIX 43 H18 2 -0.176784 0.292878 0.563455 11.00000 -1.20000 AFIX 0 C19 1 0.080861 0.344603 0.607954 11.00000 0.01592 0.02498 = 0.02899 -0.00977 0.00412 -0.00122 AFIX 43 H19 2 0.026346 0.334733 0.640966 11.00000 -1.20000 AFIX 0 C20 1 -0.098130 0.304745 0.463104 11.00000 0.02787 0.03677 = 0.03312 -0.00998 -0.00337 0.00185 AFIX 137 H20A 2 -0.052976 0.353147 0.434017 11.00000 -1.50000 H20B 2 -0.241355 0.324476 0.468030 11.00000 -1.50000 H20C 2 -0.086878 0.217991 0.454935 11.00000 -1.50000 AFIX 0 PART 2 C5A 1 0.101072 0.627529 0.795401 -21.00000 0.04601 0.05023 = 0.02669 -0.01657 0.01894 -0.02595 AFIX 23 H5AA 2 0.074745 0.579885 0.827026 -21.00000 -1.20000 H5AB 2 0.110323 0.714698 0.805129 -21.00000 -1.20000 AFIX 0 HKLF 4 REM ca050221_1_1_a.res in P2(1)/c REM wR2 = 0.1107, GooF = S = 1.029, Restrained GooF = 1.031 for all data REM R1 = 0.0449 for 3268 Fo > 4sig(Fo) and 0.0725 for all 4525 data REM 249 parameters refined using 18 restraints END WGHT 0.0435 0.7484 REM Highest difference peak 0.332, deepest hole -0.452, 1-sigma level 0.060 Q1 1 0.3486 0.3986 0.6316 11.00000 0.05 0.33 Q2 1 0.2570 0.6806 0.7114 11.00000 0.05 0.31 Q3 1 0.5422 0.6168 0.6191 11.00000 0.05 0.30 Q4 1 0.3256 0.5798 0.6984 11.00000 0.05 0.30 Q5 1 0.1436 0.5779 0.7084 11.00000 0.05 0.29 Q6 1 -0.0304 0.3252 0.4897 11.00000 0.05 0.28 Q7 1 0.3274 0.7443 0.6732 11.00000 0.05 0.28 Q8 1 0.3003 0.6011 0.7434 11.00000 0.05 0.27 Q9 1 0.4191 0.7993 0.6396 11.00000 0.05 0.26 Q10 1 0.4083 0.4923 0.6716 11.00000 0.05 0.25 Q11 1 0.3368 0.3632 0.5895 11.00000 0.05 0.25 Q12 1 0.0171 0.2953 0.5386 11.00000 0.05 0.24 Q13 1 0.4056 0.6956 0.6397 11.00000 0.05 0.24 Q14 1 0.4436 0.5903 0.6589 11.00000 0.05 0.23 Q15 1 0.2991 0.4162 0.5816 11.00000 0.05 0.23 Q16 1 0.4343 0.9178 0.6335 11.00000 0.05 0.23 Q17 1 -0.1047 0.3210 0.5609 11.00000 0.05 0.22 Q18 1 0.1775 0.3866 0.5996 11.00000 0.05 0.21 Q19 1 0.2988 0.4100 0.7260 11.00000 0.05 0.21 Q20 1 0.1394 0.3272 0.5177 11.00000 0.05 0.21 ; _shelx_res_checksum 27555 _shelx_hkl_file ; 1 0 0 2740.83 66.89 -1 0 0 2854.31 67.49 2 0 0 1526.75 50.29 3 0 0 3188.68 94.49 -4 0 0 71.79 2.40 4 0 0 80.39 19.30 5 0 0 5.70 14.70 6 0 0 397.66 48.70 7 0 0 22.50 19.90 0 -1 0 0.00 0.50 0 1 0 0.00 0.60 -1 -1 0 0.30 1.30 -1 -1 0 1.50 0.90 1 -1 0 3.70 5.90 1 -1 0 0.20 0.70 -1 1 0 -1.20 4.50 -1 1 0 1.50 0.80 1 1 0 0.90 0.80 1 1 0 1.10 1.20 -2 -1 0 26.80 2.10 2 -1 0 20.40 9.80 -2 -1 0 27.80 2.20 -2 1 0 26.70 1.50 2 1 0 42.50 11.00 3 -1 0 8.60 10.80 -3 -1 0 22.20 2.10 3 1 0 3.40 11.40 -3 1 0 19.10 1.30 4 -1 0 52.19 16.20 -4 -1 0 63.99 3.10 -4 -1 0 64.99 3.20 4 1 0 68.79 18.50 5 -1 0 -1.50 12.40 -5 -1 0 -1.50 1.00 -5 -1 0 -2.50 1.10 5 1 0 9.30 13.90 -6 -1 0 60.89 3.40 -6 -1 0 66.79 4.90 6 -1 0 64.49 24.60 -7 -1 0 7.70 2.80 7 -1 0 -5.70 16.00 8 -1 0 22.90 24.50 0 -2 0 988.90 20.00 0 2 0 966.50 22.70 0 2 0 963.40 20.00 -1 -2 0 1383.56 26.90 1 -2 0 1381.26 26.30 -1 -2 0 1371.96 29.70 1 2 0 1346.37 26.80 -1 2 0 1375.66 26.40 1 2 0 1284.47 28.80 2 -2 0 3.90 8.30 -2 -2 0 4.40 2.40 2 -2 0 4.60 1.30 -2 -2 0 4.90 1.70 2 2 0 3.70 1.80 2 2 0 8.90 2.60 -2 2 0 4.90 1.40 2 2 0 5.40 1.60 3 -2 0 78.19 16.80 -3 -2 0 82.29 5.50 -3 -2 0 76.49 4.20 -3 2 0 88.09 3.70 4 -2 0 31.60 15.90 -4 -2 0 37.40 4.30 -4 -2 0 38.00 3.50 -4 2 0 38.60 2.50 5 -2 0 48.00 18.60 -5 -2 0 28.10 3.20 -5 -2 0 26.20 3.10 -5 -2 0 32.20 4.40 -5 2 0 29.60 2.20 -6 -2 0 0.40 1.60 6 -2 0 4.70 15.50 -6 -2 0 0.60 2.60 -7 -2 0 23.80 5.20 7 -2 0 62.59 25.30 8 -2 0 70.89 31.20 -8 -2 0 64.99 8.00 0 -3 0 5.50 2.20 0 3 0 -1.20 1.70 0 3 0 -0.10 2.70 1 -3 0 887.91 19.80 -1 -3 0 924.11 24.00 -1 -3 0 870.71 20.20 1 3 0 885.61 20.40 1 3 0 892.11 23.10 -1 3 0 897.01 20.00 2 -3 0 0.80 8.40 -2 -3 0 11.40 2.50 2 -3 0 7.60 1.80 2 -3 0 5.40 1.70 -2 -3 0 4.80 3.00 2 3 0 6.50 2.10 2 3 0 2.70 2.50 -2 3 0 5.80 1.90 -3 -3 0 358.66 11.00 3 -3 0 341.07 8.60 -3 -3 0 350.66 13.20 3 -3 0 360.46 29.40 3 -3 0 350.86 8.60 -3 3 0 350.06 10.10 3 3 0 353.66 10.40 -4 -3 0 19.50 3.10 -4 -3 0 21.00 4.30 4 -3 0 34.90 15.10 -4 3 0 20.30 2.70 -5 -3 0 365.36 11.80 -5 -3 0 359.06 11.50 -5 -3 0 357.16 14.50 5 -3 0 289.77 37.70 -5 3 0 352.76 9.90 -6 -3 0 3.70 3.50 -6 -3 0 5.00 2.50 6 -3 0 -8.90 14.80 -6 3 0 5.70 1.60 -7 -3 0 0.80 3.90 7 -3 0 -0.20 18.70 -7 -3 0 4.90 2.70 8 -3 0 20.10 24.20 0 -4 0 9999.00 174.28 0 4 0 9763.02 184.38 0 4 0 9658.73 174.28 1 -4 0 162.88 7.20 -1 -4 0 155.48 7.50 1 4 0 149.09 7.50 -1 4 0 147.99 7.00 2 -4 0 327.57 10.40 -2 -4 0 305.77 14.00 2 -4 0 302.37 9.90 -2 -4 0 322.87 11.20 2 -4 0 380.56 27.00 -2 4 0 303.77 10.60 2 4 0 321.67 11.30 2 4 0 307.57 12.80 -3 -4 0 141.19 9.60 3 -4 0 147.69 23.20 3 -4 0 130.99 6.00 3 -4 0 137.19 6.00 -3 -4 0 142.19 7.40 3 4 0 132.19 6.90 -3 4 0 142.49 6.80 4 -4 0 1.60 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36.30 9.10 -3 -4 28 5.70 11.60 3 4 -28 31.10 8.10 -3 4 28 43.60 15.00 2 -4 -28 0.20 4.60 -2 4 28 12.10 11.40 2 4 -28 3.90 4.90 1 -4 -28 1.30 5.80 1 4 -28 1.50 5.00 0 -4 -28 -3.50 5.90 0 4 -28 -1.40 4.80 -1 -4 -28 23.20 8.10 -1 4 -28 15.60 7.40 -2 -4 -28 166.58 18.70 -2 4 -28 171.98 18.10 -3 -4 -28 46.20 11.30 -3 4 -28 77.29 12.70 -4 5 28 8.80 10.60 3 -5 -28 104.59 14.10 -3 5 28 91.29 19.40 3 5 -28 107.49 13.40 2 -5 -28 5.30 6.50 2 5 -28 10.40 6.10 1 -5 -28 -7.00 5.30 1 5 -28 20.80 7.60 0 -5 -28 7.60 6.20 0 5 -28 2.50 5.40 -1 -5 -28 56.29 12.00 -1 5 -28 32.60 9.10 -2 -5 -28 -3.10 6.10 -2 5 -28 -5.80 5.30 -3 -5 -28 17.30 8.00 -3 5 -28 27.10 8.70 -4 6 28 -1.00 9.10 3 -6 -28 23.90 9.30 -3 6 28 34.60 13.40 3 6 -28 35.30 9.30 2 -6 -28 4.90 6.60 2 6 -28 6.40 5.90 1 -6 -28 2.70 6.30 1 6 -28 -9.70 3.70 0 -6 -28 65.39 12.20 0 6 -28 104.99 14.70 -1 -6 -28 110.89 16.70 -1 6 -28 102.69 14.80 -2 -6 -28 5.10 7.00 -2 6 -28 -2.20 5.30 3 7 -28 1.70 6.30 2 -7 -28 57.69 11.80 2 7 -28 52.29 10.80 1 -7 -28 -4.60 5.70 1 7 -28 -2.30 5.00 0 -7 -28 6.00 7.30 0 7 -28 6.90 5.50 -1 -7 -28 -0.10 6.20 -1 7 -28 -2.40 5.70 -2 -7 -28 25.80 9.50 -2 7 -28 19.60 8.00 2 -8 -28 2.50 7.10 1 -8 -28 1.90 6.60 1 8 -28 -1.30 6.00 0 -8 -28 -3.10 6.40 0 8 -28 13.30 7.00 -5 0 29 -10.50 8.90 -4 0 29 -1.60 10.30 -3 0 29 -12.20 9.70 3 0 -29 4.00 5.70 -2 0 29 -3.00 9.70 2 0 -29 1.10 5.10 1 0 -29 -3.30 4.40 0 0 -29 7.60 6.20 -1 0 -29 4.50 6.60 -2 0 -29 -2.80 5.40 -3 0 -29 -8.50 4.70 -5 -1 29 0.90 12.40 -5 1 29 8.10 11.10 -4 -1 29 9.10 11.60 -4 1 29 7.00 12.30 3 -1 -29 53.79 10.20 -3 -1 29 43.00 17.10 -3 1 29 65.49 18.10 3 1 -29 36.20 9.30 -2 -1 29 7.50 11.70 2 -1 -29 4.60 5.90 2 1 -29 5.30 5.70 -2 1 29 8.30 11.00 1 -1 -29 2.90 6.20 1 1 -29 4.40 5.60 0 -1 -29 2.30 5.40 0 1 -29 15.30 6.90 -1 -1 -29 4.80 5.70 -1 1 -29 5.80 6.10 -2 -1 -29 27.20 8.60 -2 1 -29 32.30 9.20 -3 -1 -29 87.69 13.70 -3 1 -29 60.79 12.40 -5 -2 29 38.50 17.00 -5 2 29 5.90 11.00 -4 -2 29 39.10 17.00 -4 2 29 5.60 10.30 -3 -2 29 9.50 13.20 3 -2 -29 3.80 5.60 3 2 -29 21.20 7.20 -3 2 29 7.00 10.70 2 -2 -29 25.20 7.60 2 2 -29 46.30 10.30 -2 2 29 29.70 14.00 1 -2 -29 170.18 17.70 1 2 -29 183.28 18.20 0 -2 -29 122.29 15.30 0 2 -29 118.19 14.50 -1 -2 -29 114.99 15.50 -1 2 -29 93.99 13.70 -2 -2 -29 85.69 13.80 -2 2 -29 89.49 13.40 -3 -2 -29 9.00 6.50 -3 2 -29 4.40 6.10 -4 -3 29 -1.50 12.00 -4 3 29 -9.30 9.40 -3 -3 29 24.50 14.00 3 -3 -29 6.00 6.30 -3 3 29 17.20 11.80 3 3 -29 9.80 6.10 2 -3 -29 15.90 6.70 2 3 -29 34.90 8.80 1 -3 -29 14.20 6.70 1 3 -29 9.80 6.50 0 -3 -29 0.80 5.70 0 3 -29 2.40 5.80 -1 -3 -29 19.40 7.60 -1 3 -29 11.40 7.40 -2 -3 -29 35.00 10.20 -2 3 -29 34.00 9.70 -3 -3 -29 7.20 6.40 -3 3 -29 11.50 7.10 -4 -4 29 32.70 17.20 -4 4 29 55.19 16.20 -3 -4 29 -1.70 12.60 3 -4 -29 -5.70 5.00 3 4 -29 -1.20 3.90 -3 4 29 -4.10 10.10 2 -4 -29 6.10 6.60 2 4 -29 1.50 5.00 1 -4 -29 49.10 10.40 1 4 -29 62.59 11.60 0 -4 -29 5.70 6.80 0 4 -29 6.60 6.50 -1 -4 -29 1.40 6.10 -1 4 -29 2.30 5.60 -2 -4 -29 -13.30 4.30 -2 4 -29 -1.30 5.70 -3 -4 -29 11.00 7.60 -3 4 -29 3.70 6.20 -4 5 29 11.50 12.10 3 -5 -29 163.88 18.20 3 5 -29 177.58 17.90 -3 5 29 180.08 26.50 2 -5 -29 2.00 5.50 2 5 -29 -2.50 4.70 1 -5 -29 28.50 9.30 1 5 -29 54.89 11.30 0 -5 -29 13.20 7.50 0 5 -29 10.20 7.10 -1 -5 -29 -0.30 6.50 -1 5 -29 0.80 6.30 -2 -5 -29 32.90 10.00 -2 5 -29 22.80 8.60 3 6 -29 3.80 6.00 2 -6 -29 25.90 9.20 2 6 -29 25.30 8.20 1 -6 -29 -2.80 5.70 1 6 -29 -8.10 4.40 0 -6 -29 38.40 11.10 0 6 -29 19.30 8.00 -1 -6 -29 57.49 12.20 -1 6 -29 51.39 11.00 -2 -6 -29 -0.10 6.70 -2 6 -29 11.00 7.10 2 -7 -29 -5.50 5.60 2 7 -29 -1.60 4.80 1 -7 -29 7.40 7.00 1 7 -29 -5.10 4.90 0 -7 -29 12.40 7.90 0 7 -29 7.90 6.80 -1 -7 -29 65.79 13.50 -1 7 -29 41.40 10.60 -4 0 30 132.59 26.00 3 0 -30 8.60 6.30 -3 0 30 22.90 13.80 2 0 -30 83.89 13.20 1 0 -30 -2.50 4.70 0 0 -30 25.70 8.40 -1 0 -30 43.90 11.10 -2 0 -30 30.90 9.60 -3 0 -30 0.60 5.40 -4 -1 30 36.90 16.50 -4 1 30 106.09 23.40 -3 -1 30 4.10 11.90 3 -1 -30 -0.60 5.30 3 1 -30 -6.30 4.70 -3 1 30 -1.50 9.80 2 -1 -30 87.19 12.90 2 1 -30 127.69 16.00 1 -1 -30 -1.50 5.30 1 1 -30 -4.70 4.40 0 -1 -30 10.80 6.00 0 1 -30 3.30 5.70 -1 -1 -30 3.10 6.10 -1 1 -30 16.90 8.40 -2 -1 -30 48.10 11.10 -2 1 -30 68.59 12.80 -3 -1 -30 20.80 8.30 -3 1 -30 4.60 6.80 -4 -2 30 2.80 14.00 -4 2 30 -6.90 10.10 -3 -2 30 -4.50 11.00 3 -2 -30 17.20 7.40 -3 2 30 6.70 11.20 3 2 -30 10.80 6.50 2 -2 -30 11.40 6.70 2 2 -30 27.30 9.20 1 -2 -30 7.10 6.00 1 2 -30 4.50 5.90 0 -2 -30 0.90 5.70 0 2 -30 18.80 7.80 -1 -2 -30 0.10 5.60 -1 2 -30 3.10 6.50 -2 -2 -30 36.40 9.80 -2 2 -30 37.60 10.30 -3 -2 -30 4.60 6.00 -3 2 -30 13.10 7.60 -4 -3 30 72.69 22.70 -4 3 30 41.70 16.70 3 -3 -30 -4.60 5.40 3 3 -30 7.00 6.00 -3 3 30 0.50 11.30 2 -3 -30 66.89 12.20 2 3 -30 69.99 12.20 1 -3 -30 13.50 7.40 1 3 -30 10.20 6.30 0 -3 -30 48.50 10.80 0 3 -30 43.70 10.60 -1 -3 -30 245.18 22.90 -1 3 -30 239.78 19.20 -2 -3 -30 119.79 16.40 -2 3 -30 98.89 15.10 -4 -4 30 2.40 14.40 -4 4 30 -11.20 9.40 3 -4 -30 4.00 6.00 -3 4 30 -9.20 9.60 3 4 -30 18.40 6.90 2 -4 -30 7.60 7.00 2 4 -30 9.00 6.90 1 -4 -30 -0.30 5.60 1 4 -30 -1.80 5.00 0 -4 -30 -3.80 5.60 0 4 -30 -1.90 5.60 -1 -4 -30 153.18 18.60 -1 4 -30 129.39 16.30 -2 -4 -30 7.70 7.70 -2 4 -30 -5.10 5.00 3 5 -30 50.59 10.80 2 -5 -30 15.40 7.70 2 5 -30 -3.20 5.10 1 -5 -30 3.80 6.90 1 5 -30 -0.40 5.00 0 -5 -30 54.49 11.60 0 5 -30 75.99 13.30 -1 -5 -30 -1.60 6.10 -1 5 -30 -5.00 5.30 -2 -5 -30 15.70 8.10 -2 5 -30 6.80 7.10 2 -6 -30 45.50 11.70 2 6 -30 39.00 9.30 1 -6 -30 28.90 9.80 1 6 -30 10.60 7.20 0 -6 -30 14.90 8.60 0 6 -30 33.70 9.70 -1 -6 -30 -2.50 5.40 -1 6 -30 7.50 7.10 -4 0 31 13.40 13.10 3 0 -31 8.90 6.40 -3 0 31 11.80 13.20 2 0 -31 2.70 5.80 1 0 -31 -0.80 5.60 0 0 -31 2.20 5.80 -1 0 -31 -2.10 5.80 -2 0 -31 0.90 5.50 -4 -1 31 -3.60 12.60 -4 1 31 34.00 15.60 3 -1 -31 27.30 9.00 -3 1 31 62.39 20.40 3 1 -31 12.50 6.90 2 -1 -31 1.30 6.30 2 1 -31 13.20 7.50 1 -1 -31 104.09 15.00 1 1 -31 106.29 14.70 0 -1 -31 28.60 9.10 0 1 -31 31.70 10.00 -1 -1 -31 32.30 9.80 -1 1 -31 37.50 9.40 -2 -1 -31 12.40 7.80 -2 1 -31 12.30 7.40 -4 -2 31 115.29 25.90 -4 2 31 127.19 25.30 3 -2 -31 7.90 7.50 3 2 -31 25.30 8.00 2 -2 -31 8.60 6.70 2 2 -31 13.10 7.50 1 -2 -31 0.60 5.90 1 2 -31 11.60 6.60 0 -2 -31 44.70 10.30 0 2 -31 54.09 11.60 -1 -2 -31 0.20 6.20 -1 2 -31 -9.90 4.50 -2 -2 -31 26.70 9.70 -2 2 -31 17.70 7.90 3 -3 -31 39.40 10.30 3 3 -31 38.90 9.60 2 -3 -31 5.50 6.50 2 3 -31 5.80 5.60 1 -3 -31 33.30 9.80 1 3 -31 43.10 10.60 0 -3 -31 10.60 7.70 0 3 -31 17.90 8.30 -1 -3 -31 10.70 6.90 -1 3 -31 6.20 6.20 -2 -3 -31 6.80 6.80 -2 3 -31 -3.30 5.30 3 4 -31 154.08 16.90 2 -4 -31 22.80 9.30 2 4 -31 21.30 8.20 1 -4 -31 124.49 17.00 1 4 -31 109.29 15.80 0 -4 -31 4.90 6.20 0 4 -31 13.70 7.30 -1 -4 -31 10.10 7.80 -1 4 -31 12.10 7.30 2 -5 -31 26.90 8.90 2 5 -31 21.90 8.50 1 -5 -31 5.70 6.70 1 5 -31 7.30 6.80 0 -5 -31 -7.30 5.60 0 5 -31 -7.00 5.20 -1 -5 -31 26.40 10.20 -1 5 -31 27.30 9.60 1 -6 -31 41.80 11.60 1 6 -31 27.00 9.60 3 0 -32 -1.80 5.70 2 0 -32 53.29 11.90 1 0 -32 70.49 12.70 0 0 -32 22.40 8.30 -1 0 -32 3.00 6.90 -2 0 -32 2.50 6.70 3 -1 -32 0.50 6.20 3 1 -32 -0.80 5.50 2 -1 -32 -8.60 4.50 2 1 -32 3.30 5.90 1 -1 -32 -0.80 5.80 1 1 -32 0.00 5.20 0 -1 -32 20.00 7.80 0 1 -32 6.00 7.20 -1 -1 -32 73.89 13.80 -1 1 -32 56.39 11.90 -2 -1 -32 26.50 9.60 -2 1 -32 19.90 8.70 3 -2 -32 6.10 6.60 3 2 -32 5.70 6.40 2 -2 -32 18.10 7.80 2 2 -32 11.90 7.00 1 -2 -32 50.99 11.70 1 2 -32 31.60 8.80 0 -2 -32 2.10 6.80 0 2 -32 3.30 6.80 -1 -2 -32 12.80 7.10 -1 2 -32 3.20 6.00 3 3 -32 93.39 13.70 2 -3 -32 21.10 8.00 2 3 -32 24.70 8.00 1 -3 -32 19.80 9.10 1 3 -32 11.20 7.90 0 -3 -32 128.69 17.60 0 3 -32 169.78 19.90 -1 -3 -32 41.50 11.30 -1 3 -32 59.19 12.30 2 -4 -32 -0.30 6.00 2 4 -32 5.50 6.30 1 -4 -32 4.90 6.60 1 4 -32 -5.10 6.00 0 -4 -32 -5.20 5.80 0 4 -32 3.60 5.80 -1 -4 -32 13.60 8.20 2 0 -33 13.30 7.70 1 0 -33 -7.10 4.30 0 0 -33 -6.00 5.40 -1 0 -33 1.50 6.50 2 -1 -33 60.69 11.90 2 1 -33 58.29 11.60 1 -1 -33 24.90 9.30 1 1 -33 17.30 7.60 0 -1 -33 5.00 6.50 0 1 -33 10.60 7.70 -1 -1 -33 3.40 7.40 -1 1 -33 -5.40 5.50 2 -2 -33 3.20 6.20 2 2 -33 5.30 6.40 1 -2 -33 5.20 7.20 1 2 -33 24.70 8.80 0 -2 -33 10.00 7.00 0 2 -33 12.40 7.70 1 -3 -33 1.30 6.50 1 3 -33 6.60 7.10 0 -3 -33 2.20 7.40 0 3 -33 0.50 6.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 8569 _olex2_date_sample_data_collection 2021-02-05 _olex2_date_sample_submission 2021-02-04 _olex2_submission_original_sample_id ca050221_1_1 _olex2_submission_special_instructions 'No special instructions were received'