data_shenvi158_0m_a _audit_creation_date 2018-10-23 _audit_creation_method ; Olex2 1.2-beta (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2016/6' _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. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C30 H34 O7' _chemical_formula_sum 'C30 H34 O7' _chemical_formula_weight 506.57 _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' '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 8.7120(4) _cell_length_b 22.5701(10) _cell_length_c 13.2257(6) _cell_angle_alpha 90 _cell_angle_beta 100.619(3) _cell_angle_gamma 90 _cell_volume 2556.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1986 _cell_measurement_temperature 100 _cell_measurement_theta_max 23.688 _cell_measurement_theta_min 2.390 _shelx_estimated_absorpt_T_max 0.973 _shelx_estimated_absorpt_T_min 0.970 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0483 before and 0.0433 after correction. The Ratio of minimum to maximum transmission is 0.9286. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1080 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.3 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_unetI/netI 0.0748 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 17895 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.132 _diffrn_reflns_theta_min 2.749 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_type fine-focus _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3758 _reflns_number_total 5638 _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 V8.38A (?, 2016)' _computing_data_collection 'APEX2 v2014.11-0 (Bruker, 2014)' _computing_data_reduction 'SAINT V8.38A (?, 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 0.332 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 339 _refine_ls_number_reflns 5638 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0480 _refine_ls_restrained_S_all 1.010 _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^)+(0.0368P)^2^+0.7632P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.1068 _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, All O(H) groups 2.a Ternary CH refined with riding coordinates: C11(H11), C30(H30) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C9(H9A,H9B), C13(H13A,H13B), C25(H25A,H25B) 2.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19) 2.d Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B, H29C) 2.e Idealised tetrahedral OH refined as rotating group: O7(H7) 2.f : C23(H23) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 0.50743(15) 0.39164(6) 0.53927(10) 0.0163(3) Uani 1 1 d . . . . . O2 O 0.45891(14) 0.46356(6) 0.64758(10) 0.0149(3) Uani 1 1 d . . . . . O3 O 0.44179(14) 0.34255(6) 0.73410(10) 0.0141(3) Uani 1 1 d . . . . . O4 O 0.32403(14) 0.25615(5) 0.57210(10) 0.0141(3) Uani 1 1 d . . . . . O5 O 0.31631(15) 0.27173(6) 0.80806(10) 0.0179(3) Uani 1 1 d . . . . . O6 O 0.08731(14) 0.27874(5) 0.46634(10) 0.0136(3) Uani 1 1 d . . . . . O7 O -0.03389(15) 0.28474(6) 0.76343(10) 0.0181(3) Uani 1 1 d . . . . . H7 H 0.029903 0.269134 0.811411 0.027 Uiso 1 1 calc GR . . . . C1 C 0.6112(2) 0.58006(8) 0.72350(15) 0.0166(4) Uani 1 1 d . . . . . H1 H 0.545890 0.587402 0.658860 0.020 Uiso 1 1 calc R . . . . C2 C 0.6548(2) 0.62657(9) 0.79130(16) 0.0188(4) Uani 1 1 d . . . . . H2 H 0.619047 0.665562 0.773010 0.023 Uiso 1 1 calc R . . . . C3 C 0.7506(2) 0.61632(9) 0.88572(16) 0.0202(5) Uani 1 1 d . . . . . H3 H 0.781654 0.648236 0.931792 0.024 Uiso 1 1 calc R . . . . C4 C 0.8005(2) 0.55923(9) 0.91228(16) 0.0218(5) Uani 1 1 d . . . . . H4 H 0.865610 0.552061 0.977058 0.026 Uiso 1 1 calc R . . . . C5 C 0.7565(2) 0.51232(9) 0.84525(15) 0.0175(4) Uani 1 1 d . . . . . H5 H 0.790554 0.473259 0.864567 0.021 Uiso 1 1 calc R . . . . C6 C 0.6626(2) 0.52256(8) 0.74968(15) 0.0145(4) Uani 1 1 d . . . . . C7 C 0.6278(2) 0.47288(9) 0.67346(16) 0.0179(4) Uani 1 1 d . . . . . H7A H 0.668723 0.482722 0.610476 0.021 Uiso 1 1 calc R . . . . H7B H 0.679640 0.436156 0.703161 0.021 Uiso 1 1 calc R . . . . C8 C 0.4157(2) 0.41971(8) 0.57840(14) 0.0123(4) Uani 1 1 d . . . . . C9 C 0.2396(2) 0.41376(8) 0.55151(15) 0.0126(4) Uani 1 1 d . . . . . H9A H 0.205303 0.425251 0.478602 0.015 Uiso 1 1 calc R . . . . H9B H 0.192588 0.442218 0.593956 0.015 Uiso 1 1 calc R . . . . C10 C 0.17506(19) 0.35166(8) 0.56698(14) 0.0105(4) Uani 1 1 d . . . . . C11 C 0.2415(2) 0.30004(8) 0.51080(14) 0.0117(4) Uani 1 1 d . . . . . H11 H 0.299475 0.314672 0.457131 0.014 Uiso 1 1 calc R . . . . C12 C 0.4809(2) 0.24616(9) 0.55514(15) 0.0166(4) Uani 1 1 d . . . . . H12A H 0.479194 0.240634 0.481448 0.025 Uiso 1 1 calc GR . . . . H12B H 0.523800 0.210622 0.592618 0.025 Uiso 1 1 calc GR . . . . H12C H 0.546221 0.280427 0.579845 0.025 Uiso 1 1 calc GR . . . . C13 C 0.5911(2) 0.32355(9) 0.79333(15) 0.0158(4) Uani 1 1 d . . . . . H13A H 0.673662 0.329818 0.752092 0.019 Uiso 1 1 calc R . . . . H13B H 0.586448 0.280638 0.808019 0.019 Uiso 1 1 calc R . . . . C14 C 0.6328(2) 0.35706(8) 0.89349(14) 0.0134(4) Uani 1 1 d . . . . . C15 C 0.5318(2) 0.39646(8) 0.92793(15) 0.0158(4) Uani 1 1 d . . . . . H15 H 0.432303 0.404160 0.886862 0.019 Uiso 1 1 calc R . . . . C16 C 0.5751(2) 0.42478(8) 1.02222(15) 0.0168(4) Uani 1 1 d . . . . . H16 H 0.505482 0.451878 1.045226 0.020 Uiso 1 1 calc R . . . . C17 C 0.7194(2) 0.41353(9) 1.08254(15) 0.0198(5) Uani 1 1 d . . . . . H17 H 0.748596 0.432680 1.147198 0.024 Uiso 1 1 calc R . . . . C18 C 0.8217(2) 0.37422(9) 1.04858(16) 0.0220(5) Uani 1 1 d . . . . . H18 H 0.920762 0.366475 1.090105 0.026 Uiso 1 1 calc R . . . . C19 C 0.7795(2) 0.34628(9) 0.95424(15) 0.0180(4) Uani 1 1 d . . . . . H19 H 0.850104 0.319802 0.930789 0.022 Uiso 1 1 calc R . . . . C20 C 0.3155(2) 0.31184(8) 0.74819(14) 0.0131(4) Uani 1 1 d . . . . . C21 C 0.1661(2) 0.33666(8) 0.68191(14) 0.0116(4) Uani 1 1 d . . . . . C22 C 0.1204(2) 0.38971(9) 0.73486(15) 0.0152(4) Uani 1 1 d . . . . . C23 C 0.0855(2) 0.43297(10) 0.77576(16) 0.0238(5) Uani 1 1 d . . . . . H23 H 0.057513 0.467714 0.808624 0.029 Uiso 1 1 calc R . . . . C24 C 0.0096(2) 0.33050(8) 0.50406(14) 0.0111(4) Uani 1 1 d . . . . . C25 C -0.0851(2) 0.30876(8) 0.58301(14) 0.0136(4) Uani 1 1 d . . . . . H25A H -0.150424 0.341094 0.602785 0.016 Uiso 1 1 calc R . . . . H25B H -0.153683 0.275405 0.554980 0.016 Uiso 1 1 calc R . . . . C26 C -0.0845(2) 0.36563(8) 0.41251(14) 0.0128(4) Uani 1 1 d . . . . . C27 C -0.1370(2) 0.42584(8) 0.44747(16) 0.0183(4) Uani 1 1 d . . . . . H27A H -0.203853 0.445533 0.389468 0.027 Uiso 1 1 calc GR . . . . H27B H -0.045182 0.450509 0.472101 0.027 Uiso 1 1 calc GR . . . . H27C H -0.195644 0.419982 0.503212 0.027 Uiso 1 1 calc GR . . . . C28 C -0.2322(2) 0.32947(9) 0.36751(15) 0.0169(4) Uani 1 1 d . . . . . H28A H -0.201726 0.289387 0.350656 0.025 Uiso 1 1 calc GR . . . . H28B H -0.287573 0.348899 0.305052 0.025 Uiso 1 1 calc GR . . . . H28C H -0.300912 0.327211 0.418311 0.025 Uiso 1 1 calc GR . . . . C29 C 0.0081(2) 0.37405(9) 0.32554(15) 0.0171(4) Uani 1 1 d . . . . . H29A H 0.105129 0.395465 0.351850 0.026 Uiso 1 1 calc GR . . . . H29B H -0.054570 0.396835 0.269651 0.026 Uiso 1 1 calc GR . . . . H29C H 0.033044 0.335229 0.299550 0.026 Uiso 1 1 calc GR . . . . C30 C 0.0347(2) 0.28886(8) 0.67442(14) 0.0133(4) Uani 1 1 d . . . . . H30 H 0.077337 0.249325 0.659502 0.016 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0156(7) 0.0167(7) 0.0174(7) -0.0032(6) 0.0055(6) -0.0017(5) O2 0.0106(7) 0.0138(7) 0.0195(8) -0.0039(6) 0.0006(5) -0.0030(5) O3 0.0103(6) 0.0162(7) 0.0141(7) 0.0031(6) -0.0020(5) -0.0006(5) O4 0.0109(6) 0.0134(7) 0.0178(7) 0.0027(6) 0.0024(5) 0.0031(5) O5 0.0176(7) 0.0182(8) 0.0176(8) 0.0049(6) 0.0024(6) -0.0008(6) O6 0.0103(6) 0.0118(7) 0.0180(7) -0.0036(6) 0.0001(5) 0.0000(5) O7 0.0140(7) 0.0257(8) 0.0150(7) 0.0062(6) 0.0041(5) 0.0013(6) C1 0.0138(10) 0.0201(11) 0.0163(11) 0.0006(9) 0.0041(8) 0.0010(8) C2 0.0175(10) 0.0143(10) 0.0272(12) -0.0010(9) 0.0106(9) 0.0002(8) C3 0.0170(10) 0.0190(11) 0.0259(12) -0.0089(9) 0.0072(9) -0.0058(8) C4 0.0152(10) 0.0280(12) 0.0207(12) -0.0031(10) -0.0009(8) -0.0021(8) C5 0.0131(9) 0.0159(11) 0.0234(11) 0.0007(9) 0.0029(8) -0.0007(8) C6 0.0087(9) 0.0163(11) 0.0194(11) -0.0023(9) 0.0051(8) -0.0024(7) C7 0.0094(9) 0.0176(11) 0.0268(12) -0.0061(9) 0.0038(8) -0.0029(8) C8 0.0167(10) 0.0097(10) 0.0103(10) 0.0025(8) 0.0020(8) -0.0025(8) C9 0.0115(9) 0.0123(10) 0.0130(10) 0.0006(8) -0.0004(7) -0.0005(7) C10 0.0078(9) 0.0105(10) 0.0126(10) 0.0000(8) 0.0003(7) 0.0003(7) C11 0.0087(9) 0.0116(10) 0.0136(10) 0.0008(8) -0.0009(7) -0.0001(7) C12 0.0130(10) 0.0183(11) 0.0189(11) -0.0004(9) 0.0035(8) 0.0059(8) C13 0.0092(9) 0.0203(11) 0.0168(11) 0.0029(9) -0.0005(8) 0.0025(8) C14 0.0132(9) 0.0138(10) 0.0136(10) 0.0025(8) 0.0031(7) -0.0018(7) C15 0.0125(9) 0.0176(11) 0.0164(11) 0.0027(9) 0.0001(8) 0.0008(8) C16 0.0197(10) 0.0125(10) 0.0191(11) 0.0009(9) 0.0057(8) 0.0007(8) C17 0.0221(11) 0.0232(12) 0.0133(11) -0.0036(9) 0.0009(8) -0.0027(8) C18 0.0147(10) 0.0287(12) 0.0204(12) -0.0009(10) -0.0029(8) 0.0006(9) C19 0.0121(9) 0.0227(11) 0.0188(11) 0.0002(9) 0.0019(8) 0.0015(8) C20 0.0143(9) 0.0142(10) 0.0109(10) -0.0027(8) 0.0028(7) -0.0006(7) C21 0.0110(9) 0.0127(10) 0.0108(10) -0.0010(8) 0.0013(7) 0.0022(7) C22 0.0126(9) 0.0213(11) 0.0114(10) 0.0004(9) 0.0016(8) -0.0013(8) C23 0.0245(11) 0.0226(12) 0.0253(12) -0.0061(10) 0.0076(9) 0.0024(9) C24 0.0104(9) 0.0090(9) 0.0136(10) -0.0022(8) 0.0016(7) 0.0000(7) C25 0.0107(9) 0.0134(10) 0.0165(10) -0.0004(8) 0.0022(7) -0.0012(7) C26 0.0109(9) 0.0131(10) 0.0142(10) 0.0008(8) 0.0013(7) 0.0003(7) C27 0.0164(10) 0.0146(11) 0.0224(11) 0.0004(9) -0.0003(8) 0.0030(8) C28 0.0129(10) 0.0181(11) 0.0181(11) 0.0001(9) -0.0011(8) -0.0013(8) C29 0.0142(10) 0.0218(11) 0.0146(11) 0.0009(9) 0.0006(8) -0.0016(8) C30 0.0107(9) 0.0148(10) 0.0151(10) 0.0006(8) 0.0042(7) -0.0014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C8 1.209(2) . ? O2 C7 1.463(2) . ? O2 C8 1.353(2) . ? O3 C13 1.454(2) . ? O3 C20 1.342(2) . ? O4 C11 1.393(2) . ? O4 C12 1.443(2) . ? O5 C20 1.202(2) . ? O6 C11 1.446(2) . ? O6 C24 1.482(2) . ? O7 H7 0.8400 . ? O7 C30 1.418(2) . ? C1 H1 0.9500 . ? C1 C2 1.387(3) . ? C1 C6 1.396(3) . ? C2 H2 0.9500 . ? C2 C3 1.387(3) . ? C3 H3 0.9500 . ? C3 C4 1.385(3) . ? C4 H4 0.9500 . ? C4 C5 1.389(3) . ? C5 H5 0.9500 . ? C5 C6 1.393(3) . ? C6 C7 1.501(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.515(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.538(2) . ? C10 C11 1.550(3) . ? C10 C21 1.573(3) . ? C10 C24 1.599(2) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.510(3) . ? C14 C15 1.386(3) . ? C14 C19 1.400(2) . ? C15 H15 0.9500 . ? C15 C16 1.390(3) . ? C16 H16 0.9500 . ? C16 C17 1.383(3) . ? C17 H17 0.9500 . ? C17 C18 1.390(3) . ? C18 H18 0.9500 . ? C18 C19 1.386(3) . ? C19 H19 0.9500 . ? C20 C21 1.535(2) . ? C21 C22 1.479(3) . ? C21 C30 1.563(2) . ? C22 C23 1.182(3) . ? C23 H23 0.9500 . ? C24 C25 1.526(3) . ? C24 C26 1.550(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C30 1.512(2) . ? C26 C27 1.532(3) . ? C26 C28 1.547(2) . ? C26 C29 1.534(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30 1.0000 . ? 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 O2 C7 113.96(14) . . ? C20 O3 C13 116.59(15) . . ? C11 O4 C12 115.01(14) . . ? C11 O6 C24 92.79(12) . . ? C30 O7 H7 109.5 . . ? C2 C1 H1 119.8 . . ? C2 C1 C6 120.40(18) . . ? C6 C1 H1 119.8 . . ? C1 C2 H2 119.9 . . ? C3 C2 C1 120.23(18) . . ? C3 C2 H2 119.9 . . ? C2 C3 H3 120.3 . . ? C4 C3 C2 119.48(19) . . ? C4 C3 H3 120.3 . . ? C3 C4 H4 119.6 . . ? C3 C4 C5 120.71(18) . . ? C5 C4 H4 119.6 . . ? C4 C5 H5 120.0 . . ? C4 C5 C6 119.99(18) . . ? C6 C5 H5 120.0 . . ? C1 C6 C7 120.81(17) . . ? C5 C6 C1 119.18(18) . . ? C5 C6 C7 119.85(17) . . ? O2 C7 C6 109.54(15) . . ? O2 C7 H7A 109.8 . . ? O2 C7 H7B 109.8 . . ? C6 C7 H7A 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? O1 C8 O2 123.32(17) . . ? O1 C8 C9 125.02(17) . . ? O2 C8 C9 111.53(15) . . ? C8 C9 H9A 108.4 . . ? C8 C9 H9B 108.4 . . ? C8 C9 C10 115.38(15) . . ? H9A C9 H9B 107.5 . . ? C10 C9 H9A 108.4 . . ? C10 C9 H9B 108.4 . . ? C9 C10 C11 116.31(16) . . ? C9 C10 C21 114.15(15) . . ? C9 C10 C24 121.31(14) . . ? C11 C10 C21 112.99(14) . . ? C11 C10 C24 84.63(12) . . ? C21 C10 C24 103.79(14) . . ? O4 C11 O6 109.96(14) . . ? O4 C11 C10 116.98(15) . . ? O4 C11 H11 112.0 . . ? O6 C11 C10 92.51(13) . . ? O6 C11 H11 112.0 . . ? C10 C11 H11 112.0 . . ? O4 C12 H12A 109.5 . . ? O4 C12 H12B 109.5 . . ? O4 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 H13A 109.3 . . ? O3 C13 H13B 109.3 . . ? O3 C13 C14 111.81(15) . . ? H13A C13 H13B 107.9 . . ? C14 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C15 C14 C13 123.02(16) . . ? C15 C14 C19 119.39(18) . . ? C19 C14 C13 117.57(17) . . ? C14 C15 H15 119.8 . . ? C14 C15 C16 120.40(17) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 120.0 . . ? C17 C16 C15 120.06(19) . . ? C17 C16 H16 120.0 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 119.98(19) . . ? C18 C17 H17 120.0 . . ? C17 C18 H18 119.9 . . ? C19 C18 C17 120.13(18) . . ? C19 C18 H18 119.9 . . ? C14 C19 H19 120.0 . . ? C18 C19 C14 120.03(19) . . ? C18 C19 H19 120.0 . . ? O3 C20 C21 111.27(16) . . ? O5 C20 O3 125.12(16) . . ? O5 C20 C21 123.54(17) . . ? C20 C21 C10 116.28(15) . . ? C20 C21 C30 108.57(15) . . ? C22 C21 C10 110.42(15) . . ? C22 C21 C20 107.43(14) . . ? C22 C21 C30 109.30(16) . . ? C30 C21 C10 104.68(14) . . ? C23 C22 C21 178.4(2) . . ? C22 C23 H23 180.0 . . ? O6 C24 C10 89.25(12) . . ? O6 C24 C25 108.35(14) . . ? O6 C24 C26 110.43(15) . . ? C25 C24 C10 106.80(14) . . ? C25 C24 C26 115.10(15) . . ? C26 C24 C10 123.40(15) . . ? C24 C25 H25A 110.7 . . ? C24 C25 H25B 110.7 . . ? H25A C25 H25B 108.8 . . ? C30 C25 C24 105.20(14) . . ? C30 C25 H25A 110.7 . . ? C30 C25 H25B 110.7 . . ? C27 C26 C24 111.24(15) . . ? C27 C26 C28 108.09(15) . . ? C27 C26 C29 110.12(16) . . ? C28 C26 C24 108.28(15) . . ? C29 C26 C24 111.93(15) . . ? C29 C26 C28 106.99(15) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O7 C30 C21 114.11(15) . . ? O7 C30 C25 110.42(15) . . ? O7 C30 H30 109.5 . . ? C21 C30 H30 109.5 . . ? C25 C30 C21 103.60(14) . . ? C25 C30 H30 109.5 . . ? _shelx_res_file ; TITL shenvi158_0m_a.res in P2(1)/c shenvi158_0m_a.res created by SHELXL-2016/6 at 10:38:22 on 23-Oct-2018 REM Old TITL shenvi158_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.144, Rweak 0.007, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C29 O8 CELL 0.71073 8.712 22.5701 13.2257 90 100.619 90 ZERR 4 0.0004 0.001 0.0006 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 120 136 28 L.S. 10 PLAN 20 SIZE 0.3 0.32 0.33 TEMP -173.15 BOND $H LIST 6 fmap 2 ACTA OMIT 0 2 0 OMIT 0 1 1 REM REM REM WGHT 0.036800 0.763200 FVAR 0.56024 O1 3 0.507428 0.391635 0.539272 11.00000 0.01558 0.01674 = 0.01744 -0.00321 0.00553 -0.00172 O2 3 0.458911 0.463556 0.647582 11.00000 0.01061 0.01379 = 0.01955 -0.00394 0.00063 -0.00304 O3 3 0.441794 0.342550 0.734096 11.00000 0.01029 0.01623 = 0.01405 0.00307 -0.00201 -0.00058 O4 3 0.324031 0.256153 0.572095 11.00000 0.01092 0.01337 = 0.01782 0.00271 0.00242 0.00313 O5 3 0.316307 0.271727 0.808057 11.00000 0.01756 0.01825 = 0.01759 0.00490 0.00236 -0.00077 O6 3 0.087310 0.278736 0.466337 11.00000 0.01025 0.01178 = 0.01797 -0.00357 0.00014 -0.00003 O7 3 -0.033885 0.284738 0.763429 11.00000 0.01399 0.02573 = 0.01500 0.00624 0.00412 0.00126 AFIX 147 H7 2 0.029903 0.269134 0.811411 11.00000 -1.50000 AFIX 0 C1 1 0.611167 0.580059 0.723497 11.00000 0.01381 0.02006 = 0.01633 0.00055 0.00409 0.00097 AFIX 43 H1 2 0.545890 0.587402 0.658860 11.00000 -1.20000 AFIX 0 C2 1 0.654837 0.626569 0.791300 11.00000 0.01749 0.01427 = 0.02724 -0.00099 0.01060 0.00025 AFIX 43 H2 2 0.619047 0.665562 0.773010 11.00000 -1.20000 AFIX 0 C3 1 0.750596 0.616323 0.885721 11.00000 0.01695 0.01900 = 0.02589 -0.00893 0.00716 -0.00582 AFIX 43 H3 2 0.781654 0.648236 0.931792 11.00000 -1.20000 AFIX 0 C4 1 0.800543 0.559226 0.912279 11.00000 0.01521 0.02799 = 0.02067 -0.00306 -0.00091 -0.00209 AFIX 43 H4 2 0.865610 0.552061 0.977058 11.00000 -1.20000 AFIX 0 C5 1 0.756548 0.512322 0.845246 11.00000 0.01309 0.01591 = 0.02343 0.00066 0.00289 -0.00065 AFIX 43 H5 2 0.790554 0.473259 0.864567 11.00000 -1.20000 AFIX 0 C6 1 0.662558 0.522557 0.749681 11.00000 0.00870 0.01634 = 0.01942 -0.00232 0.00512 -0.00244 C7 1 0.627776 0.472882 0.673464 11.00000 0.00939 0.01765 = 0.02679 -0.00611 0.00376 -0.00286 AFIX 23 H7A 2 0.668723 0.482722 0.610476 11.00000 -1.20000 H7B 2 0.679640 0.436156 0.703161 11.00000 -1.20000 AFIX 0 C8 1 0.415676 0.419710 0.578398 11.00000 0.01673 0.00968 = 0.01031 0.00251 0.00204 -0.00252 C9 1 0.239602 0.413764 0.551510 11.00000 0.01155 0.01225 = 0.01305 0.00057 -0.00045 -0.00055 AFIX 23 H9A 2 0.205303 0.425251 0.478602 11.00000 -1.20000 H9B 2 0.192588 0.442218 0.593956 11.00000 -1.20000 AFIX 0 C10 1 0.175063 0.351663 0.566983 11.00000 0.00780 0.01054 = 0.01262 0.00002 0.00027 0.00027 C11 1 0.241513 0.300039 0.510800 11.00000 0.00866 0.01161 = 0.01357 0.00080 -0.00090 -0.00006 AFIX 13 H11 2 0.299475 0.314672 0.457131 11.00000 -1.20000 AFIX 0 C12 1 0.480889 0.246158 0.555142 11.00000 0.01301 0.01826 = 0.01886 -0.00042 0.00347 0.00595 AFIX 137 H12A 2 0.479194 0.240634 0.481448 11.00000 -1.50000 H12B 2 0.523800 0.210622 0.592618 11.00000 -1.50000 H12C 2 0.546221 0.280427 0.579845 11.00000 -1.50000 AFIX 0 C13 1 0.591057 0.323546 0.793332 11.00000 0.00921 0.02031 = 0.01679 0.00285 -0.00047 0.00248 AFIX 23 H13A 2 0.673662 0.329818 0.752092 11.00000 -1.20000 H13B 2 0.586448 0.280638 0.808019 11.00000 -1.20000 AFIX 0 C14 1 0.632757 0.357065 0.893489 11.00000 0.01317 0.01375 = 0.01357 0.00250 0.00309 -0.00180 C15 1 0.531756 0.396458 0.927929 11.00000 0.01246 0.01761 = 0.01638 0.00267 0.00012 0.00080 AFIX 43 H15 2 0.432303 0.404160 0.886862 11.00000 -1.20000 AFIX 0 C16 1 0.575087 0.424775 1.022219 11.00000 0.01969 0.01254 = 0.01910 0.00091 0.00572 0.00069 AFIX 43 H16 2 0.505482 0.451878 1.045226 11.00000 -1.20000 AFIX 0 C17 1 0.719390 0.413533 1.082545 11.00000 0.02209 0.02316 = 0.01333 -0.00358 0.00088 -0.00265 AFIX 43 H17 2 0.748596 0.432680 1.147198 11.00000 -1.20000 AFIX 0 C18 1 0.821688 0.374216 1.048575 11.00000 0.01468 0.02868 = 0.02037 -0.00092 -0.00291 0.00061 AFIX 43 H18 2 0.920762 0.366475 1.090105 11.00000 -1.20000 AFIX 0 C19 1 0.779466 0.346282 0.954244 11.00000 0.01207 0.02274 = 0.01881 0.00022 0.00193 0.00148 AFIX 43 H19 2 0.850104 0.319802 0.930789 11.00000 -1.20000 AFIX 0 C20 1 0.315521 0.311841 0.748188 11.00000 0.01434 0.01424 = 0.01087 -0.00270 0.00283 -0.00063 C21 1 0.166150 0.336659 0.681915 11.00000 0.01098 0.01271 = 0.01075 -0.00101 0.00126 0.00218 C22 1 0.120353 0.389715 0.734862 11.00000 0.01257 0.02130 = 0.01137 0.00043 0.00159 -0.00131 C23 1 0.085508 0.432966 0.775763 11.00000 0.02453 0.02261 = 0.02526 -0.00613 0.00758 0.00235 AFIX 163 H23 2 0.057513 0.467714 0.808624 11.00000 -1.20000 AFIX 0 C24 1 0.009625 0.330501 0.504062 11.00000 0.01044 0.00903 = 0.01364 -0.00221 0.00160 0.00002 C25 1 -0.085052 0.308763 0.583013 11.00000 0.01072 0.01336 = 0.01647 -0.00041 0.00223 -0.00124 AFIX 23 H25A 2 -0.150424 0.341094 0.602785 11.00000 -1.20000 H25B 2 -0.153683 0.275405 0.554980 11.00000 -1.20000 AFIX 0 C26 1 -0.084526 0.365627 0.412505 11.00000 0.01086 0.01307 = 0.01421 0.00079 0.00130 0.00026 C27 1 -0.137032 0.425839 0.447472 11.00000 0.01640 0.01461 = 0.02235 0.00040 -0.00026 0.00303 AFIX 137 H27A 2 -0.203853 0.445533 0.389468 11.00000 -1.50000 H27B 2 -0.045182 0.450509 0.472101 11.00000 -1.50000 H27C 2 -0.195644 0.419982 0.503212 11.00000 -1.50000 AFIX 0 C28 1 -0.232219 0.329467 0.367507 11.00000 0.01292 0.01808 = 0.01808 0.00006 -0.00108 -0.00130 AFIX 137 H28A 2 -0.201726 0.289387 0.350656 11.00000 -1.50000 H28B 2 -0.287573 0.348899 0.305052 11.00000 -1.50000 H28C 2 -0.300912 0.327211 0.418311 11.00000 -1.50000 AFIX 0 C29 1 0.008135 0.374050 0.325537 11.00000 0.01424 0.02177 = 0.01458 0.00089 0.00055 -0.00159 AFIX 137 H29A 2 0.105129 0.395465 0.351850 11.00000 -1.50000 H29B 2 -0.054570 0.396835 0.269651 11.00000 -1.50000 H29C 2 0.033044 0.335229 0.299550 11.00000 -1.50000 AFIX 0 C30 1 0.034704 0.288858 0.674420 11.00000 0.01070 0.01478 = 0.01506 0.00064 0.00424 -0.00142 AFIX 13 H30 2 0.077337 0.249325 0.659502 11.00000 -1.20000 AFIX 0 HKLF 4 REM shenvi158_0m_a.res in P2(1)/c REM R1 = 0.0480 for 3758 Fo > 4sig(Fo) and 0.0873 for all 5638 data REM 339 parameters refined using 0 restraints END WGHT 0.0368 0.7595 REM Highest difference peak 0.332, deepest hole -0.261, 1-sigma level 0.058 Q1 1 0.0895 0.3482 0.5350 11.00000 0.05 0.33 Q2 1 0.2351 0.3193 0.7040 11.00000 0.05 0.31 Q3 1 -0.1493 0.3491 0.3935 11.00000 0.05 0.28 Q4 1 0.6056 0.3419 0.8551 11.00000 0.05 0.26 Q5 1 0.2037 0.3808 0.5644 11.00000 0.05 0.25 Q6 1 0.1660 0.3450 0.6196 11.00000 0.05 0.25 Q7 1 0.2105 0.3302 0.5450 11.00000 0.05 0.24 Q8 1 0.6844 0.5576 0.7165 11.00000 0.05 0.23 Q9 1 0.5693 0.3632 0.9252 11.00000 0.05 0.23 Q10 1 -0.0472 0.3428 0.4573 11.00000 0.05 0.22 Q11 1 0.1305 0.2499 0.6800 11.00000 0.05 0.22 Q12 1 0.7723 0.3975 1.0545 11.00000 0.05 0.22 Q13 1 -0.0219 0.3210 0.5505 11.00000 0.05 0.21 Q14 1 0.1862 0.4776 0.7555 11.00000 0.05 0.21 Q15 1 -0.1110 0.4328 0.5190 11.00000 0.05 0.20 Q16 1 0.1075 0.3101 0.6829 11.00000 0.05 0.20 Q17 1 1.0292 0.5196 0.9569 11.00000 0.05 0.20 Q18 1 0.9275 0.4909 0.9348 11.00000 0.05 0.20 Q19 1 0.8927 0.5210 0.9987 11.00000 0.05 0.20 Q20 1 -0.1293 0.3336 0.7236 11.00000 0.05 0.20 ; _shelx_res_checksum 38207 _shelx_hkl_file ; 2 0 0 34.3641 5.19948 2 2 0 0 42.4709 5.21558 1 -2 0 0 47.7983 5.48481 2 -2 0 0 40.9455 5.61781 1 3 0 0 0.85266 4.42879 2 3 0 0 -1.4015 5.25474 1 -3 0 0 8.52230 5.10710 1 4 0 0 319.977 17.4715 1 -4 0 0 311.047 19.0546 3 -5 0 0 2.76700 6.27706 3 5 0 0 -0.9974 6.28679 1 6 0 0 3.70868 7.65980 1 -6 0 0 2.76015 6.87428 3 -7 0 0 164.307 19.6507 3 7 0 0 172.033 18.3801 1 -8 0 0 -10.514 6.95435 3 8 0 0 -4.7946 9.92467 1 -9 0 0 282.763 29.5943 3 9 0 0 270.089 28.2644 1 -10 0 0 0.00397 10.7557 3 10 0 0 -2.8788 13.6065 1 -2 -1 0 425.169 17.3544 1 -2 -1 0 465.067 17.5159 2 2 -1 0 432.474 16.8406 1 -2 -1 0 438.188 18.4637 3 -2 1 0 457.159 16.8073 1 2 1 0 430.787 17.3866 2 -2 1 0 458.261 15.9233 2 2 1 0 486.080 17.8443 1 -3 -1 0 12.4521 6.89250 3 3 -1 0 9.67742 5.32188 1 3 1 0 3.10918 5.56785 1 -3 1 0 11.1187 5.13102 1 -3 1 0 2.97560 4.01780 2 3 1 0 19.5072 5.84942 2 -4 -1 0 413.481 21.8953 3 4 -1 0 412.075 19.7654 1 4 1 0 408.753 19.4336 2 4 1 0 387.853 19.0585 1 -5 -1 0 54.2076 9.94237 3 5 -1 0 47.5679 9.57020 1 5 1 0 46.6747 9.79841 1 -5 1 0 36.8566 10.3508 3 6 -1 0 273.483 21.5589 1 -6 -1 0 271.315 23.3155 3 6 1 0 282.714 20.2362 1 -6 1 0 280.847 23.3231 3 -7 -1 0 274.072 25.5480 3 7 -1 0 335.857 22.9969 1 7 1 0 325.214 23.3143 1 -7 1 0 271.521 25.9112 3 8 -1 0 25.8542 11.9228 1 -8 -1 0 29.2980 11.8012 3 -8 1 0 14.2515 12.6180 3 8 1 0 25.2878 12.1543 1 -9 -1 0 -11.913 8.14742 3 9 -1 0 18.6401 12.7767 1 9 1 0 13.9653 13.1312 1 -9 1 0 12.0852 11.0800 3 -10 -1 0 78.7570 21.7530 3 10 -1 0 123.087 21.2103 1 10 1 0 92.2848 20.7815 1 -10 1 0 84.3551 19.4229 3 0 -2 0 -0.5376 0.67715 2 0 -2 0 0.06897 0.73029 1 0 2 0 -0.0912 1.04984 2 -1 -2 0 2293.37 67.2572 1 -1 2 0 2338.06 66.2096 1 1 2 0 2318.79 67.2569 3 1 2 0 2285.11 67.3628 2 -2 -2 0 324.442 13.8111 1 -2 -2 0 330.569 14.1492 2 2 -2 0 301.976 13.3426 1 -2 -2 0 336.412 14.7054 3 -2 2 0 324.159 13.1468 1 2 2 0 321.167 14.6666 2 2 2 0 327.515 14.7590 1 -2 2 0 336.170 11.9363 2 -3 -2 0 1383.79 46.5929 3 3 -2 0 1312.98 44.0008 1 -3 2 0 1370.37 42.2370 2 3 2 0 1347.89 45.2630 1 -3 2 0 1421.83 43.6793 1 3 2 0 1314.56 44.9121 2 4 -2 0 144.493 12.4627 1 -4 -2 0 121.383 12.5181 3 4 2 0 122.571 12.4077 1 4 2 0 115.776 11.8309 2 5 -2 0 282.521 17.3797 1 -5 -2 0 295.945 18.8934 3 5 2 0 253.775 17.7618 1 -6 -2 0 165.396 17.8688 3 6 -2 0 188.361 17.9221 1 -6 2 0 166.619 17.6405 3 6 2 0 150.289 16.9923 1 -7 -2 0 1.30102 9.80445 3 7 -2 0 27.3079 10.3505 1 7 2 0 4.96195 6.99096 1 -7 2 0 -1.5482 9.62204 3 8 -2 0 159.951 20.0712 1 -8 -2 0 173.883 23.3487 3 8 2 0 187.106 22.2450 1 -8 2 0 165.492 22.0515 3 9 -2 0 -14.398 10.7838 1 -9 -2 0 2.54402 9.67737 3 9 2 0 14.0726 12.9253 1 -9 2 0 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16.7151 12.0371 2 2 -9 -14 -13.537 9.41210 1 -2 9 14 -5.1216 8.90792 2 1 -9 -14 124.715 17.4257 1 -1 -9 14 169.058 23.8530 2 -1 9 14 167.739 24.3579 2 0 -9 14 133.182 21.3903 2 0 9 14 107.395 21.8956 2 1 -9 14 24.8102 14.0706 2 1 9 14 17.1967 16.2276 2 2 -9 14 10.0800 15.1389 2 2 9 14 22.4860 17.2033 2 3 9 14 27.3271 18.4490 2 6 -10 -14 35.0795 15.3422 1 -6 10 14 35.9158 17.6824 2 5 -10 -14 77.3691 17.6519 1 -5 10 14 23.4497 16.2515 2 4 -10 -14 4.16282 13.3168 1 -4 10 14 33.3868 17.2612 2 3 -10 -14 22.3520 12.8514 1 -3 10 14 5.08508 14.8873 2 2 -10 -14 -0.8453 10.9006 1 -2 10 14 45.0076 17.4420 2 1 -10 -14 13.0407 11.6467 1 -1 -10 14 -7.7661 12.0672 2 -1 10 14 10.8027 15.8390 2 0 -10 -14 19.1732 11.4425 1 0 -10 14 28.7327 14.1885 2 0 10 14 -3.2612 10.0663 2 1 -10 14 17.5305 13.5654 2 1 10 14 27.7574 17.9044 2 2 10 14 49.2321 19.5135 2 3 10 14 11.0587 12.7285 2 6 -11 -14 -6.4394 13.2969 1 -6 11 14 -17.831 12.1087 2 5 -11 -14 84.9701 19.3248 1 -5 11 14 31.4792 13.8401 2 4 -11 -14 42.4951 14.8090 1 -4 11 14 66.5935 19.7831 2 3 -11 -14 10.7879 12.6605 1 -3 11 14 40.2570 15.3689 2 2 -11 -14 3.76715 11.4806 1 -2 11 14 14.8100 15.5783 2 -1 -11 14 95.8060 19.6371 2 1 -11 -14 66.2583 16.2028 1 -1 11 14 60.7536 17.6411 2 0 -11 -14 30.9728 12.9725 1 0 -11 14 20.4273 14.0063 2 0 11 14 15.8381 13.0292 2 1 -11 14 4.66060 11.6250 2 1 11 14 18.3958 15.6863 2 2 11 14 23.4996 16.7566 2 5 -12 -14 2.99412 13.2523 1 -5 12 14 -7.9299 13.2062 2 4 -12 -14 24.9617 14.9400 1 -4 12 14 43.3869 15.7250 2 3 -12 -14 150.297 21.6903 1 -3 12 14 148.232 25.5975 2 2 -12 -14 19.5524 14.3286 1 -2 12 14 -10.356 12.4314 2 1 -12 -14 67.7380 15.3196 1 -1 -12 14 92.1806 19.2960 2 -1 12 14 41.0625 17.6925 2 0 -12 -14 231.596 23.4838 1 0 -12 14 259.684 28.2978 2 0 12 14 245.538 31.3797 2 1 12 14 257.100 31.0832 2 2 12 14 161.918 27.9145 2 5 -13 -14 13.4650 13.9473 1 -5 13 14 20.7305 16.3816 2 4 -13 -14 86.1887 18.9361 1 -4 13 14 94.8769 22.1222 2 3 -13 -14 15.1965 14.9433 1 -3 13 14 8.85116 11.5093 2 2 -13 -14 10.3577 12.7758 1 -2 13 14 26.2757 15.9855 2 -1 -13 14 151.151 22.8464 2 1 -13 -14 194.835 23.5397 1 -1 13 14 154.339 26.6050 2 0 -13 -14 104.805 19.0944 1 0 -13 14 71.2044 17.6576 2 0 13 14 61.1730 21.1652 2 -1 -13 -14 6.13578 14.4500 1 1 13 14 -11.243 9.51166 2 2 13 14 26.3935 18.4693 2 4 -14 -14 -9.5259 12.6093 1 -4 14 14 6.23996 15.2175 2 3 -14 -14 44.7202 16.0625 1 -3 14 14 52.0505 19.0118 2 2 -14 -14 141.613 21.7937 1 -2 14 14 108.964 23.2918 2 1 -14 -14 17.2672 13.9148 1 -1 14 14 19.3894 13.5088 2 0 -14 -14 37.1156 15.1420 1 0 14 14 41.5235 15.6299 2 -1 -14 -14 20.8154 13.2141 1 1 14 14 11.3033 15.9646 2 4 -15 -14 173.752 25.1837 1 -4 15 14 117.025 21.3717 2 3 -15 -14 6.41254 13.7667 1 -3 15 14 0.74282 15.5524 2 2 -15 -14 -17.478 11.7602 1 -2 15 14 -5.0564 14.2415 2 1 -15 -14 127.353 20.5589 1 -1 15 14 176.953 27.9013 2 0 -15 -14 6.16114 12.8063 1 0 15 14 22.2193 16.5720 2 -3 16 14 21.9632 16.6988 2 2 -16 -14 -7.8526 11.8097 1 -2 16 14 5.27032 15.7039 2 1 -16 -14 31.8884 15.0755 1 -1 16 14 20.8238 14.3215 2 -5 0 15 -2.4381 10.7317 2 -4 0 15 31.1722 17.1015 2 -3 0 15 24.9849 15.9833 2 -2 0 15 10.2999 14.6569 2 -1 0 15 9.14079 13.3562 2 0 0 15 13.2284 14.5980 2 1 0 15 13.5688 14.8426 2 2 0 15 -16.460 13.2498 2 3 0 15 14.4298 16.3822 2 -6 1 15 44.1154 16.4241 2 -5 1 15 194.831 27.1685 2 -4 -1 15 45.9428 19.2937 2 -4 1 15 42.1132 18.2668 2 -3 -1 15 34.2635 14.8331 2 -3 1 15 71.8000 19.7450 2 -2 -1 15 303.883 32.7214 2 -2 1 15 241.250 30.2057 2 -1 -1 15 23.7333 15.2733 2 -1 1 15 21.3954 15.8355 2 0 -1 15 6.96835 15.1342 2 0 1 15 7.60512 15.1283 2 1 -1 15 42.4773 15.5485 2 1 1 15 32.6642 17.5592 2 2 -1 15 -11.170 13.4883 2 2 1 15 14.9476 15.7333 2 3 -1 15 60.4005 18.8751 2 3 1 15 30.9922 17.7397 2 6 -2 -15 1.04584 11.4308 1 -6 2 15 -4.9983 14.9328 2 -5 2 15 18.1004 17.0683 2 -4 -2 15 34.7249 15.7909 2 -4 2 15 62.9729 19.3275 2 -3 -2 15 1.31058 10.6789 2 -3 2 15 4.39255 15.2633 2 -2 -2 15 46.2821 17.6638 2 -2 2 15 53.1625 15.7570 2 -1 -2 15 53.8404 17.6141 2 -1 2 15 58.7791 18.9411 2 0 -2 15 14.3098 14.4057 2 0 2 15 36.1432 17.5141 2 1 -2 15 5.10912 14.1252 2 1 2 15 1.93509 14.5503 2 2 -2 15 104.853 19.8833 2 2 2 15 112.690 23.3135 2 3 -2 15 7.12007 15.5454 2 3 2 15 78.5768 20.5239 2 6 -3 -15 65.2522 16.1723 1 -6 3 15 107.723 23.1910 2 5 -3 -15 349.534 30.7435 1 -5 3 15 342.819 36.4909 2 -4 -3 15 5.37142 11.8491 2 -4 3 15 13.7021 12.6157 2 -3 -3 15 19.1574 12.9799 2 -3 3 15 35.8474 14.4028 2 -2 -3 15 27.4222 15.6392 2 -2 3 15 16.0891 12.5758 2 -1 -3 15 -7.6438 12.9697 2 -1 3 15 5.13371 13.8853 2 0 -3 15 22.9380 15.2927 2 0 3 15 15.5960 15.9654 2 1 -3 15 50.6624 17.8641 2 1 3 15 65.8882 20.4169 2 2 -3 15 185.648 26.1299 2 2 3 15 175.512 24.9375 2 3 -3 15 150.647 23.6244 2 3 3 15 125.294 23.4894 2 6 -4 -15 87.1629 18.0858 1 -6 4 15 69.5514 19.3524 2 5 -4 -15 171.924 20.6816 1 -5 4 15 179.856 26.0575 2 -4 4 15 102.132 22.7233 2 -3 -4 15 28.1547 13.7796 2 -3 4 15 26.5170 13.4759 2 -2 -4 15 -3.8426 14.5040 2 -2 4 15 9.72651 14.9869 2 -1 -4 15 -12.446 12.5894 2 -1 4 15 12.0228 15.5176 2 0 -4 15 12.8773 14.2724 2 0 4 15 22.1950 16.4575 2 1 -4 15 20.2461 15.0932 2 1 4 15 19.2732 15.7454 2 2 -4 15 12.9447 14.8095 2 2 4 15 -2.3425 10.4635 2 3 -4 15 -1.1685 13.0398 2 3 4 15 -9.2830 14.2784 2 6 -5 -15 113.516 20.0925 1 -6 5 15 98.7282 24.3021 2 5 -5 -15 47.4699 13.8967 1 -5 5 15 51.2720 18.9391 2 4 -5 -15 1.87056 10.3411 1 -4 5 15 33.8398 17.4264 2 -3 -5 15 46.2171 15.7930 2 -3 5 15 44.1939 18.6965 2 -2 -5 15 19.4231 16.0588 2 -2 5 15 25.9481 16.7744 2 -1 -5 15 10.3041 14.7075 2 -1 5 15 3.58375 11.1815 2 0 -5 15 40.7056 16.6275 2 0 5 15 41.8931 17.9429 2 1 -5 15 19.4144 15.1740 2 1 5 15 1.24634 15.3367 2 2 -5 15 25.4634 14.0837 2 2 5 15 8.91427 16.2302 2 6 -6 -15 40.2115 15.7552 1 -6 6 15 65.5443 21.8068 2 5 -6 -15 11.7070 12.3028 1 -5 6 15 -20.914 13.7362 2 4 -6 -15 -0.8440 9.22193 1 -4 6 15 2.23097 10.3029 2 -3 -6 15 16.5072 11.7601 2 -3 6 15 10.9446 14.4307 2 -2 -6 15 109.363 21.9658 2 -2 6 15 122.782 22.4458 2 -1 -6 15 38.0262 17.2985 2 -1 6 15 32.7508 14.6672 2 0 -6 15 1.99569 13.6955 2 0 6 15 2.85581 11.6030 2 1 -6 15 5.23856 13.0546 2 1 6 15 -4.0499 14.6331 2 2 -6 15 -2.9198 13.4304 2 2 6 15 21.5182 16.1254 2 6 -7 -15 62.2020 16.9216 1 -6 7 15 79.7074 22.2438 2 5 -7 -15 -14.302 11.2708 1 -5 7 15 10.2750 12.9535 2 4 -7 -15 20.9413 12.6524 1 -4 7 15 24.8721 17.4996 2 3 -7 -15 -4.3623 9.93499 1 -3 7 15 -2.3870 10.2241 2 -2 -7 15 31.1829 16.9964 2 -2 7 15 3.89042 11.7106 2 -1 -7 15 24.5481 14.6721 2 -1 7 15 25.0803 17.8501 2 0 -7 15 -15.364 12.3947 2 0 7 15 -13.052 9.13995 2 1 -7 15 8.42025 13.4230 2 1 7 15 -20.768 12.9839 2 2 -7 15 48.1616 16.6412 2 2 7 15 27.8746 19.7547 2 5 -8 -15 13.5185 13.7342 1 -5 8 15 24.8853 18.0207 2 4 -8 -15 13.5463 12.4745 1 -4 8 15 8.24722 11.1929 2 3 -8 -15 -1.0293 10.6459 1 -3 8 15 -12.219 14.4101 2 -2 -8 15 7.51610 11.3558 2 -2 8 15 5.36022 15.3966 2 -1 -8 15 50.4314 15.1322 2 -1 8 15 46.9383 18.8921 2 0 -8 15 27.2015 15.2991 2 0 8 15 -12.796 9.96479 2 1 -8 15 4.05885 13.2574 2 1 8 15 12.1782 16.0252 2 2 8 15 143.914 26.7368 2 5 -9 -15 -2.9976 10.8953 1 -5 9 15 26.8711 13.9179 2 4 -9 -15 5.77280 11.7456 1 -4 9 15 63.3957 19.5470 2 3 -9 -15 2.31438 11.3524 1 -3 9 15 6.24627 12.0251 2 2 -9 -15 -4.1057 9.11412 1 -2 -9 15 1.92812 14.3543 2 -2 9 15 -0.5174 14.6158 2 -1 -9 15 43.9939 16.8259 2 -1 9 15 23.4505 14.0962 2 0 -9 15 222.150 27.0702 2 0 9 15 172.078 28.3077 2 1 -9 15 52.0182 17.2096 2 1 9 15 68.1573 18.5651 2 2 9 15 64.1494 21.1830 2 5 -10 -15 23.2545 14.5108 1 -5 10 15 5.66335 16.2562 2 4 -10 -15 356.632 31.3611 1 -4 10 15 323.115 36.9328 2 3 -10 -15 26.3681 12.2521 1 -3 10 15 10.1424 15.4872 2 2 -10 -15 21.3057 11.8228 1 -2 -10 15 50.3047 17.8874 2 -2 10 15 5.73926 12.5149 2 -1 -10 15 19.1862 15.5929 2 -1 10 15 11.5358 15.6548 2 0 -10 15 12.4156 13.6089 2 0 10 15 -0.6631 15.0839 2 1 -10 15 56.5541 17.0017 2 1 10 15 60.1701 18.0372 2 4 -11 -15 19.6054 14.6232 1 -4 11 15 -6.2004 15.6365 2 3 -11 -15 -23.349 8.86032 1 -3 11 15 28.5833 16.5634 2 2 -11 -15 -18.081 9.09658 1 -2 11 15 9.78933 15.7738 2 -1 -11 15 -2.3643 9.56900 2 -1 11 15 -12.096 13.7502 2 0 -11 15 13.8103 14.0477 2 0 11 15 -7.0427 15.7218 2 1 11 15 103.830 21.5883 2 4 -12 -15 -9.5258 12.0110 1 -4 12 15 -5.8493 14.8240 2 3 -12 -15 10.7882 13.6749 1 -3 12 15 -9.6399 15.3147 2 2 -12 -15 89.5417 18.0653 1 -2 12 15 38.2769 16.1583 2 -1 -12 15 5.21498 14.0127 2 1 -12 -15 29.3426 14.3478 1 -1 12 15 0.07356 15.9332 2 0 -12 15 92.9649 20.6518 2 0 12 15 91.7502 20.7761 2 3 -13 -15 10.9271 12.9381 1 -3 13 15 30.3723 18.8868 2 2 -13 -15 -3.3491 11.8064 1 -2 13 15 -26.779 12.7212 2 -1 -13 15 19.0004 14.8243 2 1 -13 -15 -14.881 10.6585 1 -1 13 15 -6.5288 9.44379 2 -5 0 16 10.3257 13.7862 2 -4 0 16 5.13537 16.8462 2 -3 0 16 65.6488 18.4827 2 -2 0 16 266.820 32.6176 2 -1 0 16 9.79578 11.9754 2 0 0 16 2.26876 15.5674 2 1 0 16 17.0300 13.6632 2 -5 -1 16 12.3787 13.5532 2 -5 1 16 84.6913 19.5046 2 -4 -1 16 17.8678 18.9866 2 -4 1 16 46.8743 19.9958 2 -3 -1 16 229.237 29.7419 2 -3 1 16 228.667 31.2933 2 -2 -1 16 -7.3610 15.1072 2 -2 1 16 50.9823 18.6628 2 -1 -1 16 -2.7994 10.1261 2 -1 1 16 -7.1243 10.6486 2 0 -1 16 -12.435 9.85063 2 0 1 16 -13.065 14.4087 2 1 -1 16 291.911 33.6045 2 1 1 16 251.323 30.3235 2 -5 -2 16 23.2998 14.7899 2 -5 2 16 2.94267 16.5604 2 -4 -2 16 90.5281 23.3112 2 -4 2 16 73.9701 21.7507 2 -3 -2 16 92.9587 20.4517 2 -3 2 16 75.7641 23.1316 2 -2 -2 16 31.1452 18.2465 2 -2 2 16 3.59629 15.5592 2 -1 -2 16 33.3941 14.5555 2 -1 2 16 17.8836 13.3883 2 0 -2 16 182.119 25.9438 2 0 2 16 164.093 26.9240 2 1 -2 16 14.4302 16.0414 2 1 2 16 19.2463 17.1840 2 -5 -3 16 33.2686 15.4800 2 -5 3 16 29.8257 17.8886 2 -4 -3 16 29.9122 18.7401 2 -4 3 16 31.2550 17.1778 2 -3 -3 16 24.6285 15.0242 2 -3 3 16 22.5460 18.0700 2 -2 -3 16 10.8993 16.0375 2 -2 3 16 -2.4258 16.1271 2 -1 -3 16 -0.9305 10.7215 2 -1 3 16 14.2724 13.2607 2 0 -3 16 -3.9653 14.6846 2 0 3 16 5.70801 15.6360 2 1 -3 16 71.0281 20.3673 2 1 3 16 83.9879 22.4869 2 -5 4 16 124.986 26.9743 2 -4 -4 16 29.2664 18.7154 2 -4 4 16 29.0455 14.9804 2 -3 -4 16 36.6586 18.9322 2 -3 4 16 8.18773 16.7058 2 -2 -4 16 13.7799 15.7114 2 -2 4 16 22.3038 17.0304 2 -1 -4 16 -8.4346 14.1307 2 -1 4 16 -24.239 8.52444 2 0 -4 16 6.43920 14.4269 2 0 4 16 6.45975 17.5535 2 1 -4 16 199.129 26.5293 2 1 4 16 211.024 30.2506 2 -5 5 16 5.13813 12.6411 2 -4 -5 16 44.7024 20.5409 2 -4 5 16 26.3431 19.2285 2 -3 -5 16 -4.0741 15.6572 2 -3 5 16 4.48474 12.1361 2 -2 -5 16 148.393 26.2419 2 -2 5 16 165.729 26.4160 2 -1 -5 16 -22.206 12.2309 2 -1 5 16 0.73981 11.0777 2 0 -5 16 98.9405 21.8134 2 0 5 16 116.353 24.1245 2 1 -5 16 63.8488 19.4679 2 1 5 16 86.7947 23.7618 2 -4 6 16 -10.262 14.5796 2 -3 -6 16 49.9079 20.0720 2 -3 6 16 47.4198 16.0654 2 -2 -6 16 41.6956 17.8513 2 -2 6 16 -13.588 9.68544 2 -1 -6 16 42.9922 18.4755 2 -1 6 16 31.7260 19.7301 2 0 -6 16 50.9360 18.7061 2 0 6 16 51.8251 20.3370 2 -4 7 16 39.6304 15.8841 2 -3 -7 16 338.946 36.0925 2 -3 7 16 346.047 38.2992 2 -2 -7 16 8.55595 12.2074 2 -2 7 16 -5.6570 16.4691 2 -1 -7 16 7.81714 11.8455 2 -1 7 16 3.71830 16.2262 2 0 -7 16 22.2390 15.7269 2 0 7 16 44.2925 16.8874 2 -4 8 16 12.3199 17.0478 2 -3 -8 16 5.47310 12.6679 2 -3 8 16 -10.141 14.1913 2 -2 -8 16 42.7674 18.8771 2 -2 8 16 51.4693 20.4160 2 -1 -8 16 15.2428 16.0384 2 -1 8 16 3.68740 16.2030 2 0 -8 16 -11.940 13.0412 2 0 8 16 40.9688 16.4864 2 -3 -9 16 18.6503 17.6963 2 -3 9 16 -20.039 9.28845 2 -2 -9 16 44.8616 20.0308 2 -2 9 16 20.4197 17.4546 2 -1 -9 16 36.0950 17.3042 2 -1 9 16 30.7316 18.6079 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6948 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71078 8.706 22.563 13.238 90.001 100.617 90.007 ) ; _shelx_hkl_checksum 73268 _olex2_submission_special_instructions 'No special instructions were received'