data_cu_mkcisc8_0m_a _audit_creation_date 2021-07-18 _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 'C32 H42 O2' _chemical_formula_sum 'C32 H42 O2' _chemical_formula_weight 458.65 _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' 0.0181 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' '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 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.7965(7) _cell_length_b 12.4119(4) _cell_length_c 11.1170(4) _cell_angle_alpha 90 _cell_angle_beta 114.9890(10) _cell_angle_gamma 90 _cell_volume 2600.94(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9889 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 68.28 _cell_measurement_theta_min 4.26 _shelx_estimated_absorpt_T_max 0.947 _shelx_estimated_absorpt_T_min 0.879 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.6688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1114 before and 0.0791 after correction. The Ratio of minimum to maximum transmission is 0.8881. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'Block' _exptl_crystal_F_000 1000 _exptl_crystal_size_max 0.246 _exptl_crystal_size_mid 0.235 _exptl_crystal_size_min 0.102 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 20224 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.286 _diffrn_reflns_theta_min 4.265 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2166 _reflns_number_total 2374 _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 'SAINT V8.40A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40A (?, 2016)' _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 0.478 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.119 _refine_ls_extinction_coef 0.0073(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 2374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0433 _refine_ls_restrained_S_all 1.149 _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^)+(0.0667P)^2^+1.4039P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1100 _refine_ls_wR_factor_ref 0.1260 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C2(H2) 2.b Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C13(H13A,H13B), C3(H3A,H3B), C12(H12A,H12B), C14(H14A,H14B) 2.c Aromatic/amide H refined with riding coordinates: C7(H7) 2.d Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C) ; _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 0.36041(5) 0.12037(7) 0.54899(8) 0.0231(3) Uani 1 1 d . . . . . C5 C 0.41551(6) 0.38045(10) 0.70155(11) 0.0195(3) Uani 1 1 d . . . . . C4 C 0.36206(6) 0.40524(10) 0.74382(12) 0.0217(3) Uani 1 1 d . . . . . C6 C 0.30920(6) 0.33115(11) 0.72831(12) 0.0232(3) Uani 1 1 d . . . . . C1 C 0.46477(7) 0.47245(9) 0.73319(11) 0.0202(3) Uani 1 1 d . . . . . C9 C 0.41360(6) 0.28645(9) 0.63148(11) 0.0189(3) Uani 1 1 d . . . . . C8 C 0.35960(6) 0.21247(10) 0.61689(11) 0.0202(3) Uani 1 1 d . . . . . C15 C 0.45949(7) -0.08895(11) 0.72064(13) 0.0280(3) Uani 1 1 d . . . . . H15A H 0.443307 -0.155175 0.749207 0.034 Uiso 1 1 calc R . . . . H15B H 0.443464 -0.026433 0.756152 0.034 Uiso 1 1 calc R . . . . C16 C 0.46282(6) 0.26167(10) 0.56731(12) 0.0213(3) Uani 1 1 d . . . . . H16A H 0.486574 0.327964 0.560204 0.032 Uiso 1 1 calc GR . . . . H16B H 0.435497 0.231853 0.478515 0.032 Uiso 1 1 calc GR . . . . H16C H 0.498420 0.209056 0.621471 0.032 Uiso 1 1 calc GR . . . . C2 C 0.42225(7) 0.57064(10) 0.74057(12) 0.0236(3) Uani 1 1 d . . . . . H2 H 0.454184 0.625699 0.802971 0.028 Uiso 1 1 calc R . . . . C13 C 0.34467(7) -0.06794(11) 0.50687(13) 0.0273(3) Uani 1 1 d . . . . . H13A H 0.327844 -0.060438 0.409630 0.033 Uiso 1 1 calc R . . . . H13B H 0.322249 -0.133176 0.523503 0.033 Uiso 1 1 calc R . . . . C3 C 0.37311(7) 0.51918(10) 0.79858(13) 0.0258(3) Uani 1 1 d . . . . . H3A H 0.396244 0.518919 0.896813 0.031 Uiso 1 1 calc R . . . . H3B H 0.327478 0.558347 0.768260 0.031 Uiso 1 1 calc R . . . . C10 C 0.37835(7) 0.62061(10) 0.60484(13) 0.0287(3) Uani 1 1 d . . . . . H10A H 0.410092 0.647565 0.566933 0.043 Uiso 1 1 calc GR . . . . H10B H 0.350142 0.680366 0.614682 0.043 Uiso 1 1 calc GR . . . . H10C H 0.346621 0.565965 0.545771 0.043 Uiso 1 1 calc GR . . . . C12 C 0.32050(7) 0.02980(10) 0.55940(13) 0.0247(3) Uani 1 1 d . . . . . H12A H 0.269140 0.042323 0.506536 0.030 Uiso 1 1 calc R . . . . H12B H 0.329109 0.018221 0.653093 0.030 Uiso 1 1 calc R . . . . C14 C 0.42519(7) -0.08358(10) 0.56946(13) 0.0269(3) Uani 1 1 d . . . . . H14A H 0.436169 -0.151035 0.534424 0.032 Uiso 1 1 calc R . . . . H14B H 0.446911 -0.023395 0.541260 0.032 Uiso 1 1 calc R . . . . C7 C 0.30937(6) 0.23325(10) 0.66561(12) 0.0229(3) Uani 1 1 d . . . . . H7 H 0.274598 0.180285 0.656308 0.027 Uiso 1 1 calc R . . . . C11 C 0.25146(7) 0.35226(12) 0.77366(13) 0.0293(3) Uani 1 1 d . . . . . H11A H 0.258015 0.304750 0.848368 0.044 Uiso 1 1 calc GR . . . . H11B H 0.205101 0.338184 0.700346 0.044 Uiso 1 1 calc GR . . . . H11C H 0.253760 0.427551 0.801730 0.044 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0270(5) 0.0194(5) 0.0257(5) -0.0035(3) 0.0139(4) -0.0062(3) C5 0.0202(6) 0.0193(6) 0.0185(6) 0.0032(4) 0.0077(5) 0.0026(5) C4 0.0226(6) 0.0235(6) 0.0188(6) 0.0025(5) 0.0087(5) 0.0045(5) C6 0.0204(6) 0.0295(7) 0.0196(6) 0.0035(5) 0.0085(5) 0.0045(5) C1 0.0266(6) 0.0163(6) 0.0187(6) 0.0001(4) 0.0106(5) 0.0009(5) C9 0.0195(6) 0.0188(6) 0.0183(6) 0.0027(4) 0.0079(5) 0.0012(4) C8 0.0214(6) 0.0192(6) 0.0186(6) 0.0008(4) 0.0070(5) 0.0000(5) C15 0.0283(8) 0.0270(7) 0.0317(7) -0.0003(5) 0.0156(6) -0.0015(5) C16 0.0237(6) 0.0201(6) 0.0222(6) -0.0028(5) 0.0119(5) -0.0021(5) C2 0.0269(7) 0.0181(6) 0.0253(6) -0.0018(5) 0.0105(5) 0.0026(5) C13 0.0302(7) 0.0217(7) 0.0288(7) -0.0021(5) 0.0114(6) -0.0067(5) C3 0.0293(7) 0.0235(7) 0.0269(6) -0.0010(5) 0.0141(5) 0.0051(5) C10 0.0343(7) 0.0210(7) 0.0293(7) 0.0018(5) 0.0119(6) 0.0042(5) C12 0.0229(6) 0.0219(7) 0.0288(6) 0.0005(5) 0.0105(5) -0.0060(5) C14 0.0302(7) 0.0222(6) 0.0318(7) -0.0026(5) 0.0165(6) -0.0028(5) C7 0.0195(6) 0.0263(7) 0.0220(6) 0.0026(5) 0.0080(5) -0.0019(5) C11 0.0233(7) 0.0389(8) 0.0285(7) 0.0001(6) 0.0136(5) 0.0030(6) _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 C8 1.3739(15) . ? O1 C12 1.4306(14) . ? C5 C4 1.4115(17) . ? C5 C1 1.4740(17) . ? C5 C9 1.3941(17) . ? C4 C6 1.3870(18) . ? C4 C3 1.5184(17) . ? C6 C7 1.4016(18) . ? C6 C11 1.5087(17) . ? C1 C1 1.351(3) 2_656 ? C1 C2 1.5281(16) . ? C9 C8 1.4059(17) . ? C9 C16 1.5061(16) . ? C8 C7 1.3890(17) . ? C15 C15 1.529(3) 2_656 ? C15 C14 1.5248(19) . ? C2 C3 1.5574(18) . ? C2 C10 1.5269(18) . ? C13 C12 1.5210(18) . ? C13 C14 1.5301(19) . ? 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 C8 O1 C12 117.85(9) . . ? C4 C5 C1 108.50(10) . . ? C9 C5 C4 121.87(11) . . ? C9 C5 C1 129.39(11) . . ? C5 C4 C3 109.24(11) . . ? C6 C4 C5 120.56(11) . . ? C6 C4 C3 130.17(11) . . ? C4 C6 C7 117.92(11) . . ? C4 C6 C11 122.98(12) . . ? C7 C6 C11 119.10(12) . . ? C5 C1 C2 105.73(10) . . ? C1 C1 C5 129.01(7) 2_656 . ? C1 C1 C2 124.74(7) 2_656 . ? C5 C9 C8 116.35(11) . . ? C5 C9 C16 124.82(11) . . ? C8 C9 C16 118.79(11) . . ? O1 C8 C9 114.35(10) . . ? O1 C8 C7 123.68(11) . . ? C7 C8 C9 121.96(12) . . ? C14 C15 C15 112.88(14) . 2_656 ? C1 C2 C3 101.01(10) . . ? C10 C2 C1 112.89(10) . . ? C10 C2 C3 110.65(11) . . ? C12 C13 C14 113.72(11) . . ? C4 C3 C2 103.33(10) . . ? O1 C12 C13 107.37(10) . . ? C15 C14 C13 114.79(11) . . ? C8 C7 C6 121.01(12) . . ? _shelx_res_file ; TITL cu_mkcisc8_0m_a_a.res in C2/c cu_mkcisc8_0m_a.res created by SHELXL-2018/3 at 17:27:44 on 18-Jul-2021 REM Old TITL cu_MKcisC8_0m_a.res in C2/c REM SHELXT solution in C2/c: R1 0.128, Rweak 0.003, Alpha 0.028 REM 0.416 for 117 systematic absences, Orientation as input REM Formula found by SHELXT: C16 O CELL 1.54178 20.7965 12.4119 11.117 90 114.989 90 ZERR 4 0.0007 0.0004 0.0004 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H O UNIT 128 168 8 L.S. 10 PLAN 20 SIZE 0.102 0.235 0.246 TEMP -173.15 BOND list 4 fmap 2 ACTA REM REM REM WGHT 0.066700 1.403900 EXTI 0.007291 FVAR 0.57696 O1 3 0.360407 0.120366 0.548994 11.00000 0.02699 0.01944 = 0.02570 -0.00350 0.01388 -0.00624 C5 1 0.415507 0.380446 0.701548 11.00000 0.02020 0.01931 = 0.01846 0.00319 0.00775 0.00264 C4 1 0.362060 0.405237 0.743818 11.00000 0.02265 0.02347 = 0.01878 0.00248 0.00866 0.00446 C6 1 0.309196 0.331152 0.728306 11.00000 0.02045 0.02954 = 0.01964 0.00354 0.00845 0.00453 C1 1 0.464766 0.472449 0.733185 11.00000 0.02660 0.01630 = 0.01872 0.00014 0.01060 0.00092 C9 1 0.413598 0.286448 0.631481 11.00000 0.01945 0.01882 = 0.01830 0.00268 0.00789 0.00120 C8 1 0.359599 0.212469 0.616885 11.00000 0.02141 0.01924 = 0.01859 0.00079 0.00704 0.00004 C15 1 0.459486 -0.088947 0.720638 11.00000 0.02832 0.02701 = 0.03171 -0.00029 0.01556 -0.00155 AFIX 23 H15A 2 0.443307 -0.155175 0.749207 11.00000 -1.20000 H15B 2 0.443464 -0.026433 0.756152 11.00000 -1.20000 AFIX 0 C16 1 0.462821 0.261666 0.567314 11.00000 0.02370 0.02013 = 0.02224 -0.00285 0.01191 -0.00214 AFIX 137 H16A 2 0.486574 0.327964 0.560204 11.00000 -1.50000 H16B 2 0.435497 0.231853 0.478515 11.00000 -1.50000 H16C 2 0.498420 0.209056 0.621471 11.00000 -1.50000 AFIX 0 C2 1 0.422255 0.570640 0.740570 11.00000 0.02688 0.01806 = 0.02533 -0.00177 0.01045 0.00257 AFIX 13 H2 2 0.454184 0.625699 0.802971 11.00000 -1.20000 AFIX 0 C13 1 0.344669 -0.067938 0.506869 11.00000 0.03022 0.02166 = 0.02882 -0.00213 0.01144 -0.00674 AFIX 23 H13A 2 0.327844 -0.060438 0.409630 11.00000 -1.20000 H13B 2 0.322249 -0.133176 0.523503 11.00000 -1.20000 AFIX 0 C3 1 0.373106 0.519182 0.798583 11.00000 0.02929 0.02353 = 0.02690 -0.00104 0.01406 0.00508 AFIX 23 H3A 2 0.396244 0.518919 0.896813 11.00000 -1.20000 H3B 2 0.327478 0.558347 0.768260 11.00000 -1.20000 AFIX 0 C10 1 0.378346 0.620608 0.604835 11.00000 0.03429 0.02104 = 0.02933 0.00175 0.01194 0.00421 AFIX 137 H10A 2 0.410092 0.647565 0.566933 11.00000 -1.50000 H10B 2 0.350142 0.680366 0.614682 11.00000 -1.50000 H10C 2 0.346621 0.565965 0.545771 11.00000 -1.50000 AFIX 0 C12 1 0.320502 0.029803 0.559400 11.00000 0.02290 0.02188 = 0.02875 0.00052 0.01050 -0.00605 AFIX 23 H12A 2 0.269140 0.042323 0.506536 11.00000 -1.20000 H12B 2 0.329109 0.018221 0.653093 11.00000 -1.20000 AFIX 0 C14 1 0.425185 -0.083577 0.569461 11.00000 0.03023 0.02219 = 0.03182 -0.00264 0.01653 -0.00280 AFIX 23 H14A 2 0.436169 -0.151035 0.534424 11.00000 -1.20000 H14B 2 0.446911 -0.023395 0.541260 11.00000 -1.20000 AFIX 0 C7 1 0.309369 0.233246 0.665614 11.00000 0.01952 0.02633 = 0.02201 0.00257 0.00800 -0.00188 AFIX 43 H7 2 0.274598 0.180285 0.656308 11.00000 -1.20000 AFIX 0 C11 1 0.251460 0.352258 0.773661 11.00000 0.02334 0.03895 = 0.02845 0.00008 0.01365 0.00295 AFIX 137 H11A 2 0.258015 0.304750 0.848368 11.00000 -1.50000 H11B 2 0.205101 0.338184 0.700346 11.00000 -1.50000 H11C 2 0.253760 0.427551 0.801730 11.00000 -1.50000 AFIX 0 HKLF 4 REM cu_mkcisc8_0m_a_a.res in C2/c REM wR2 = 0.1260, GooF = S = 1.149, Restrained GooF = 1.149 for all data REM R1 = 0.0433 for 2166 Fo > 4sig(Fo) and 0.0495 for all 2374 data REM 158 parameters refined using 0 restraints END WGHT 0.0667 1.4039 REM Highest difference peak 0.478, deepest hole -0.340, 1-sigma level 0.119 Q1 1 0.5000 -0.0893 0.7500 10.50000 0.05 0.48 Q2 1 0.4358 -0.1132 0.7593 11.00000 0.05 0.33 Q3 1 0.3152 -0.0978 0.4654 11.00000 0.05 0.33 Q4 1 0.4489 -0.0916 0.6594 11.00000 0.05 0.33 Q5 1 0.4791 -0.1018 0.6672 11.00000 0.05 0.31 Q6 1 0.3804 -0.0792 0.5435 11.00000 0.05 0.29 Q7 1 0.2890 0.7240 0.6298 11.00000 0.05 0.27 Q8 1 0.4458 0.5268 0.7436 11.00000 0.05 0.27 Q9 1 0.3980 0.5531 0.7745 11.00000 0.05 0.27 Q10 1 0.2611 0.3499 0.8569 11.00000 0.05 0.27 Q11 1 0.4283 0.6620 0.7206 11.00000 0.05 0.26 Q12 1 0.3886 0.7486 0.6019 11.00000 0.05 0.25 Q13 1 0.3997 0.5925 0.6686 11.00000 0.05 0.25 Q14 1 0.3152 0.6609 0.6039 11.00000 0.05 0.23 Q15 1 0.3561 0.4655 0.7695 11.00000 0.05 0.23 Q16 1 0.3282 0.7501 0.5879 11.00000 0.05 0.23 Q17 1 0.2301 0.2709 0.8184 11.00000 0.05 0.23 Q18 1 0.4769 -0.1850 0.6009 11.00000 0.05 0.23 Q19 1 0.4706 0.6863 0.6190 11.00000 0.05 0.23 Q20 1 0.2801 0.3383 0.7650 11.00000 0.05 0.23 ; _shelx_res_checksum 84756 _shelx_hkl_file ; 2 0 0 242.88 15.00 2 0 0 215.18 15.30 2 0 0 256.47 14.90 6 0 0 9.20 1.80 6 0 0 11.00 1.50 6 0 0 17.70 3.60 6 0 0 9.90 1.00 6 0 0 11.20 1.40 -8 0 0 307.47 21.20 8 0 0 281.97 19.00 8 0 0 290.07 18.30 8 0 0 280.57 19.00 10 0 0 2110.29 126.59 10 0 0 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292.27 20.50 -6 -2 10 289.27 20.80 -6 2 10 280.87 21.40 -6 2 10 279.37 22.00 -6 2 10 311.67 20.60 -6 2 10 323.57 20.40 -6 2 10 287.47 21.00 -6 2 10 288.07 21.10 -4 -2 10 59.69 5.50 -4 -2 10 61.79 6.50 -4 -2 10 55.59 6.90 -4 -2 10 49.20 6.30 -4 -2 10 58.39 5.70 -4 2 10 53.39 6.10 -4 2 10 47.50 6.10 -4 2 10 49.90 5.60 -4 2 10 46.90 6.70 -4 2 10 50.89 5.30 -4 2 10 54.59 5.40 -2 -2 10 -0.80 1.70 -2 -2 10 0.80 2.20 -2 -2 10 0.40 1.80 -2 -2 10 -0.20 1.00 -2 -2 10 2.80 2.50 -2 2 10 0.20 2.20 -2 2 10 -0.30 2.10 -2 2 10 0.40 1.20 -2 2 10 0.30 2.90 0 -2 10 1.90 1.80 0 -2 10 1.50 1.40 0 -2 10 0.70 1.10 0 -2 10 -0.50 1.50 0 -2 10 -0.30 1.30 0 2 10 1.00 1.20 0 2 10 -1.10 1.50 0 2 10 3.10 1.90 0 2 10 2.00 1.50 2 -2 10 25.30 3.70 2 -2 10 29.10 4.20 2 -2 10 23.80 3.60 2 -2 10 24.20 3.20 2 2 10 18.70 3.40 -2 2 -10 15.80 3.20 2 2 10 20.40 3.30 2 2 10 18.70 3.80 2 2 10 17.10 3.40 4 -2 10 13.90 2.60 4 -2 10 21.60 3.50 -4 -2 -10 23.50 3.50 4 -2 10 17.30 2.80 4 -2 10 19.90 3.00 4 2 10 17.10 3.10 4 2 10 14.50 3.00 -4 2 -10 23.20 3.50 4 2 10 14.10 2.80 4 2 10 22.30 3.00 6 -2 10 125.09 8.50 6 -2 10 119.49 8.70 6 -2 10 108.89 8.50 -6 -2 -10 117.29 8.50 6 -2 10 106.69 9.00 6 2 10 112.59 8.90 6 2 10 119.29 9.00 6 2 10 105.09 8.40 -21 -3 10 0.00 0.90 -21 -3 10 -0.20 1.10 -21 3 10 0.70 1.10 21 3 -10 -0.80 1.10 -21 3 10 0.50 1.00 -19 -3 10 1.80 1.30 -19 -3 10 2.00 1.30 19 3 -10 -0.50 1.60 -19 3 10 3.30 1.50 -19 3 10 -0.80 2.50 -19 3 10 2.30 1.40 -17 -3 10 132.69 10.10 -17 -3 10 126.39 9.80 -17 -3 10 126.29 9.60 -17 3 10 115.49 9.80 -17 3 10 126.29 10.10 -17 3 10 121.89 9.90 17 3 -10 119.69 10.50 -15 -3 10 34.30 4.10 -15 -3 10 35.10 4.00 -15 -3 10 31.30 3.90 -15 3 10 27.40 4.30 -15 3 10 31.10 4.20 -15 3 10 32.80 4.10 -13 -3 10 79.29 7.10 -13 -3 10 97.99 9.70 -13 -3 10 81.79 7.30 -13 -3 10 89.39 7.90 -13 3 10 71.89 7.30 -13 3 10 71.49 7.40 -13 3 10 82.99 7.40 -11 -3 10 69.09 7.20 -11 -3 10 88.29 7.80 -11 -3 10 99.49 7.80 -11 3 10 85.69 8.10 -11 3 10 94.99 7.60 -11 3 10 75.69 10.70 -11 3 10 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5 10 58.79 5.30 -1 5 10 62.99 7.00 1 5 -10 61.99 6.20 -1 5 10 48.40 6.00 -1 5 10 53.69 5.80 1 -5 10 5.80 2.00 1 -5 10 5.30 1.60 1 -5 10 5.60 2.00 1 -5 10 4.00 1.60 1 5 10 5.50 2.20 -1 5 -10 5.80 1.80 1 5 10 2.30 1.30 1 5 10 1.70 1.50 1 5 10 2.50 1.70 3 -5 10 46.40 4.90 3 -5 10 45.30 4.40 3 -5 10 53.49 5.40 3 -5 10 49.90 4.30 -3 -5 -10 51.19 5.40 3 5 10 48.20 5.10 3 5 10 52.09 5.30 3 5 10 53.29 5.70 3 5 10 49.80 4.40 5 -5 10 111.39 8.60 5 -5 10 106.69 8.60 -5 -5 -10 116.59 8.50 5 5 10 108.59 8.60 5 5 10 123.79 8.70 5 5 10 111.59 7.90 -18 -6 10 211.48 13.20 18 -6 -10 194.18 13.30 -18 -6 10 170.68 13.10 -18 -6 10 187.38 13.00 -18 6 10 188.18 13.30 -18 6 10 172.48 13.10 -18 6 10 175.18 13.10 -16 -6 10 28.90 3.60 16 -6 -10 25.40 4.00 -16 -6 10 29.20 3.50 -16 6 10 26.10 4.80 -16 6 10 26.00 3.50 -14 -6 10 277.07 19.10 14 -6 -10 272.57 19.50 -14 -6 10 302.17 19.20 -14 -6 10 268.97 19.20 -14 6 10 263.87 19.60 -14 6 10 268.67 19.10 -14 6 10 293.27 20.00 -12 -6 10 274.87 18.40 -12 -6 10 279.17 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10 41.30 4.80 0 -6 10 38.60 4.40 0 6 10 45.50 5.10 0 6 10 34.40 4.40 0 6 10 44.50 4.90 0 6 -10 42.10 4.30 0 6 10 41.20 5.40 2 -6 10 14.60 2.70 -2 -6 -10 14.10 3.00 2 -6 10 11.20 1.90 2 -6 10 17.20 2.70 2 -6 10 16.20 2.20 2 6 10 13.00 2.80 2 6 10 13.90 2.50 2 6 10 10.90 2.60 2 6 10 13.60 2.60 -2 6 -10 25.10 4.00 -4 -6 -10 62.79 6.60 4 -6 10 49.40 3.80 4 -6 10 47.10 4.50 4 6 10 48.20 4.60 4 6 10 35.00 4.20 4 6 10 46.80 4.70 4 6 10 57.19 4.80 -17 -7 10 32.50 3.20 -17 -7 10 34.60 3.30 -17 -7 10 28.40 2.90 -17 7 10 24.00 3.00 -17 7 10 28.70 3.30 -17 7 10 28.20 3.50 -15 -7 10 84.79 8.60 -15 -7 10 96.69 7.20 -15 -7 10 92.09 7.20 -15 7 10 90.69 7.80 -15 7 10 93.49 7.70 13 -7 -10 349.57 23.40 -13 -7 10 355.06 23.00 -13 -7 10 381.66 23.30 -13 -7 10 335.07 22.60 -13 7 10 336.67 23.50 -13 7 10 291.87 22.50 -13 7 10 351.86 23.90 -11 -7 10 430.76 28.50 -11 -7 10 453.25 28.90 -11 -7 10 425.16 28.70 -11 7 10 416.16 29.50 -9 -7 10 336.17 22.30 -9 -7 10 354.06 22.80 -9 -7 10 331.57 22.50 -9 7 10 317.77 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6.60 -16 -2 12 70.09 6.00 -16 -2 12 79.29 6.50 -16 2 12 82.29 6.80 -16 2 12 80.49 6.50 -14 -2 12 100.69 7.90 -14 -2 12 106.09 8.00 -14 -2 12 97.39 7.60 -14 2 12 94.79 7.80 -12 -2 12 59.59 5.00 -12 -2 12 59.19 4.90 -12 2 12 50.49 5.50 -12 2 12 41.10 4.90 -12 2 12 41.90 5.30 -10 -2 12 7.70 2.10 -10 -2 12 7.80 1.90 -10 -2 12 5.30 1.90 -10 -2 12 11.60 2.20 -10 2 12 9.50 2.50 -10 2 12 8.30 1.80 -10 2 12 6.90 3.30 -10 2 12 10.30 3.40 -10 2 12 6.70 2.20 -8 -2 12 52.59 4.60 -8 -2 12 46.70 7.10 -8 -2 12 51.99 4.60 -8 2 12 35.70 4.80 -8 2 12 39.40 5.00 -8 2 12 42.90 4.10 -8 2 12 40.30 4.10 -8 2 12 40.30 4.70 -6 -2 12 70.89 5.70 -6 -2 12 67.29 5.80 -6 -2 12 68.99 6.20 -6 -2 12 48.50 6.70 -6 2 12 63.99 6.00 -6 2 12 66.09 6.10 -6 2 12 62.29 6.50 -6 2 12 69.79 5.40 -6 2 12 51.29 6.30 -4 -2 12 27.90 3.00 -4 -2 12 23.50 3.50 -4 -2 12 22.40 2.70 -4 -2 12 16.70 3.10 -4 2 12 18.90 2.50 -4 2 12 23.50 3.30 -4 2 12 19.50 3.20 -4 2 12 15.40 3.00 -2 -2 12 105.49 8.00 -2 -2 12 98.79 7.90 -2 -2 12 98.19 7.40 -2 2 12 93.69 7.60 -2 2 12 95.89 7.80 -2 2 12 76.69 7.70 -2 2 12 99.89 7.20 0 -2 12 12.10 2.00 0 -2 12 16.50 2.60 0 2 12 15.50 2.60 0 2 12 12.90 2.30 0 2 12 10.60 2.00 0 2 12 16.60 2.10 -17 -3 12 1.90 1.20 -17 -3 12 3.50 1.20 -17 -3 12 4.10 1.30 -17 3 12 4.10 1.40 -17 3 12 2.00 1.00 -15 -3 12 85.39 6.40 -15 -3 12 74.69 6.10 -15 -3 12 74.79 6.10 -15 3 12 73.39 6.20 -15 3 12 68.49 6.40 -13 -3 12 1.00 1.20 -13 -3 12 2.30 1.30 -13 -3 12 1.60 1.10 -13 3 12 1.60 1.20 -13 3 12 1.20 1.30 -13 3 12 0.90 1.60 -11 -3 12 207.38 14.00 -11 -3 12 162.98 13.90 -11 -3 12 228.08 15.10 -11 -3 12 234.68 14.40 -11 3 12 176.58 15.70 -11 3 12 202.68 13.90 -11 3 12 186.08 14.20 -9 -3 12 209.68 13.60 -9 -3 12 217.68 13.50 -9 -3 12 197.98 13.50 -9 3 12 194.38 13.60 -9 3 12 165.68 12.70 -9 3 12 155.68 13.50 -9 3 12 174.28 13.60 -7 -3 12 671.43 42.00 -7 -3 12 616.14 42.00 -7 -3 12 697.53 43.10 -7 3 12 642.14 42.30 -7 3 12 684.23 41.90 -7 3 12 605.24 42.10 -7 3 12 620.64 42.50 -7 3 12 649.93 41.70 -5 -3 12 63.39 5.10 -5 -3 12 68.79 6.00 -5 -3 12 59.19 5.60 -5 -3 12 62.89 5.80 -5 3 12 61.09 5.70 -5 3 12 60.99 6.20 -5 3 12 58.69 5.50 -5 3 12 55.69 5.80 -3 -3 12 106.59 8.10 -3 -3 12 119.09 9.00 -3 -3 12 119.99 9.00 -3 -3 12 117.89 8.60 -3 3 12 117.99 9.10 -3 3 12 114.89 8.80 -3 3 12 109.79 9.30 -1 -3 12 0.20 1.10 -1 -3 12 -0.10 0.90 -1 -3 12 0.40 0.80 -1 3 12 0.20 1.00 -1 3 12 1.00 0.90 -1 3 12 2.50 1.30 -1 3 12 1.40 1.00 -16 4 12 159.38 11.80 -16 4 12 180.78 12.30 -14 -4 12 39.70 3.60 -14 -4 12 28.20 3.40 -14 -4 12 33.20 3.40 -14 4 12 33.90 3.70 -14 4 12 27.70 3.20 -14 4 12 23.50 4.20 -12 -4 12 82.99 7.20 -12 -4 12 82.49 6.40 -12 -4 12 78.49 6.40 -12 4 12 73.19 6.50 -12 4 12 78.49 6.70 -12 4 12 69.89 6.00 -10 -4 12 30.20 3.80 -10 -4 12 27.90 3.20 -10 4 12 23.10 3.40 -10 4 12 19.20 3.00 -10 4 12 18.20 3.60 -8 -4 12 40.60 4.00 -8 -4 12 42.40 4.40 -8 -4 12 37.90 3.90 -8 4 12 34.00 4.50 -8 4 12 34.20 4.00 -8 4 12 35.90 4.20 -6 -4 12 22.80 2.70 -6 -4 12 22.20 3.40 -6 -4 12 22.50 2.80 -6 4 12 17.10 3.00 -6 4 12 21.00 3.20 -6 4 12 18.20 2.80 -6 4 12 15.40 2.60 -4 -4 12 164.68 11.30 -4 -4 12 157.48 10.80 -4 -4 12 161.98 11.20 -4 -4 12 154.98 10.50 -4 4 12 149.69 11.30 -4 4 12 138.79 10.80 -4 4 12 124.09 11.30 -2 -4 12 26.70 2.60 -2 -4 12 23.70 2.90 -2 -4 12 19.00 2.30 -2 -4 12 26.50 3.00 -2 4 12 24.30 2.90 -2 4 12 20.50 3.20 -2 4 12 19.80 2.80 -15 -5 12 57.39 4.40 -15 -5 12 38.40 4.70 -15 -5 12 60.29 4.40 -15 5 12 40.30 4.00 -15 5 12 48.30 4.50 -13 -5 12 0.70 0.90 -13 -5 12 0.50 0.80 -13 5 12 1.30 1.40 -13 5 12 -1.10 0.90 -13 5 12 0.50 1.10 -11 -5 12 131.39 9.40 -11 -5 12 134.99 9.40 -11 -5 12 140.19 10.10 -11 5 12 112.69 9.50 -11 5 12 114.59 9.60 -9 -5 12 8.30 1.80 -9 -5 12 6.00 1.60 -9 -5 12 7.10 1.60 -9 5 12 4.50 1.70 -9 5 12 8.40 2.20 -9 5 12 5.70 1.70 -7 -5 12 6.00 1.70 -7 -5 12 6.00 1.50 -7 -5 12 6.00 1.60 -7 5 12 6.20 1.80 -7 5 12 4.60 1.60 -7 5 12 4.00 1.70 -5 -5 12 58.19 4.70 -5 -5 12 61.99 4.90 -5 -5 12 61.39 5.20 -5 5 12 53.69 5.00 -5 5 12 55.49 5.30 -5 5 12 43.60 5.10 -3 -5 12 309.17 18.80 -3 -5 12 278.37 18.40 -3 -5 12 286.77 18.40 -3 5 12 273.27 18.90 -3 5 12 243.88 19.00 -12 -6 12 44.80 3.80 -12 6 12 41.30 4.20 -12 6 12 39.00 4.00 -10 -6 12 1.10 0.80 -10 -6 12 0.80 1.00 -10 -6 12 -0.40 1.30 -10 6 12 0.30 1.00 -10 6 12 -1.40 1.20 -10 6 12 -0.20 1.90 -8 -6 12 -0.50 0.80 -8 -6 12 -0.10 0.70 -8 -6 12 1.00 1.00 -8 6 12 -0.80 1.00 -8 6 12 -0.50 1.40 -8 6 12 -0.30 0.90 -6 -6 12 32.00 3.10 -6 -6 12 31.30 3.30 -6 -6 12 31.30 3.10 -6 6 12 30.40 3.40 -6 6 12 27.60 4.10 -14 0 13 0.50 1.00 -14 0 13 -0.60 0.80 -12 0 13 -3.30 2.20 -12 0 13 1.30 1.20 -12 0 13 -0.90 0.90 -10 0 13 0.30 1.00 -10 0 13 -0.10 1.10 -8 0 13 3.00 1.50 -8 0 13 0.10 1.40 -8 0 13 0.00 1.10 -6 0 13 -1.90 1.50 -6 0 13 0.50 1.50 -6 0 13 0.30 1.20 -15 -1 13 56.29 4.90 -15 1 13 70.99 5.80 -15 1 13 57.79 5.00 -13 -1 13 13.30 2.00 -13 -1 13 15.30 2.20 -13 -1 13 23.80 2.50 -13 1 13 19.30 3.10 -13 1 13 19.60 2.40 -11 -1 13 192.08 12.80 -11 1 13 179.78 13.00 -9 -1 13 47.90 3.80 -9 -1 13 46.70 3.90 -9 -1 13 41.90 4.10 -9 1 13 35.50 3.60 -7 -1 13 180.68 11.90 -7 -1 13 156.28 10.30 -7 -1 13 144.69 10.40 -7 1 13 155.08 10.60 -7 1 13 129.09 10.60 -5 1 13 45.00 4.20 -14 -2 13 5.10 1.20 -14 -2 13 7.70 1.50 -14 2 13 7.10 1.60 -14 2 13 3.90 1.40 -12 2 13 99.49 6.60 -12 2 13 77.29 7.10 -10 -2 13 0.70 0.80 -10 -2 13 -0.80 0.80 -10 2 13 -0.30 1.20 -10 2 13 -1.20 2.10 -8 -2 13 509.15 32.30 -8 -2 13 438.16 32.30 -8 -2 13 562.64 32.40 -6 -2 13 163.48 10.50 -6 2 13 163.08 10.80 -6 2 13 126.99 10.30 -13 -3 13 43.60 3.80 -13 3 13 40.20 4.20 -11 -3 13 9.20 1.60 -11 -3 13 6.40 1.40 -11 3 13 6.20 1.50 -9 -3 13 29.80 3.40 -9 -3 13 30.80 3.10 -9 -3 13 33.10 3.10 -9 3 13 33.90 4.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 72621 _olex2_submission_special_instructions 'No special instructions were received'