data_TPAPO _audit_creation_date 2020-07-08 _audit_creation_method ; Olex2 1.2 (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _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 'C30 H24 N O P' _chemical_formula_sum 'C30 H24 N O P' _chemical_formula_weight 445.47 _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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 '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 'orthorhombic' _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.0526(6) _cell_length_b 16.6684(6) _cell_length_c 17.1822(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4597.5(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9811 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 68.198 _cell_measurement_theta_min 5.149 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.7015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1151 before and 0.0716 after correction. The Ratio of minimum to maximum transmission is 0.9315. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 1872 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1065 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 60551 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.295 _diffrn_reflns_theta_min 4.610 _diffrn_ambient_temperature 153.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type Bruker _diffrn_measurement_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3146 _reflns_number_total 4171 _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 0.421 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.109 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 4171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0472 _refine_ls_restrained_S_all 1.092 _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^)+(0.1230P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1370 _refine_ls_wR_factor_ref 0.1783 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C17(H17), C26(H26), C30(H30), C8(H8), C6(H6), C20(H20), C16(H16), C14(H14), C12(H12), C4(H4), C24(H24), C21(H21), C9(H9), C27(H27), C15(H15), C28(H28), C10(H10), C11(H11), C29(H29), C22(H22), C2(H2), C23(H23), C5(H5), C3(H3) ; _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 P1 P 0.49656(3) 0.76745(3) 0.21747(3) 0.0219(2) Uani 1 1 d . . . . . O1 O 0.54073(10) 0.82814(10) 0.26580(10) 0.0283(4) Uani 1 1 d . . . . . N1 N 0.36205(11) 0.77335(11) 0.34668(11) 0.0252(4) Uani 1 1 d . . . . . C13 C 0.33507(14) 0.80093(14) 0.27147(13) 0.0236(5) Uani 1 1 d . . . . . C17 C 0.35697(14) 0.81613(14) 0.13331(14) 0.0257(5) Uani 1 1 d . . . . . H17 H 0.3910 0.8093 0.0886 0.031 Uiso 1 1 calc R . . . . C25 C 0.50902(14) 0.66634(14) 0.25124(14) 0.0241(5) Uani 1 1 d . . . . . C7 C 0.36356(13) 0.83204(14) 0.40706(14) 0.0253(5) Uani 1 1 d . . . . . C19 C 0.53853(13) 0.76445(14) 0.11957(14) 0.0259(5) Uani 1 1 d . . . . . C1 C 0.34143(14) 0.69245(14) 0.36703(14) 0.0266(5) Uani 1 1 d . . . . . C18 C 0.38681(13) 0.79134(13) 0.20624(13) 0.0227(5) Uani 1 1 d . . . . . C26 C 0.45282(15) 0.60453(15) 0.23577(15) 0.0301(5) Uani 1 1 d . . . . . H26 H 0.4019 0.6160 0.2100 0.036 Uiso 1 1 calc R . . . . C30 C 0.58369(15) 0.64818(15) 0.28858(14) 0.0302(5) Uani 1 1 d . . . . . H30 H 0.6231 0.6895 0.2985 0.036 Uiso 1 1 calc R . . . . C8 C 0.32418(15) 0.81992(14) 0.47837(14) 0.0294(5) Uani 1 1 d . . . . . H8 H 0.2950 0.7713 0.4879 0.035 Uiso 1 1 calc R . . . . C6 C 0.39246(15) 0.65217(14) 0.42002(14) 0.0288(5) Uani 1 1 d . . . . . H6 H 0.4396 0.6783 0.4418 0.035 Uiso 1 1 calc R . . . . C20 C 0.57323(14) 0.83464(15) 0.08900(15) 0.0309(6) Uani 1 1 d . . . . . H20 H 0.5729 0.8826 0.1189 0.037 Uiso 1 1 calc R . . . . C16 C 0.27836(14) 0.85052(15) 0.12538(14) 0.0288(5) Uani 1 1 d . . . . . H16 H 0.2590 0.8669 0.0756 0.035 Uiso 1 1 calc R . . . . C14 C 0.25690(15) 0.83620(15) 0.26307(15) 0.0295(5) Uani 1 1 d . . . . . H14 H 0.2226 0.8436 0.3075 0.035 Uiso 1 1 calc R . . . . C12 C 0.40583(15) 0.90432(14) 0.39407(16) 0.0316(5) Uani 1 1 d . . . . . H12 H 0.4332 0.9135 0.3459 0.038 Uiso 1 1 calc R . . . . C4 C 0.30633(17) 0.53411(16) 0.40888(17) 0.0395(6) Uani 1 1 d . . . . . H4 H 0.2941 0.4804 0.4235 0.047 Uiso 1 1 calc R . . . . C24 C 0.53873(15) 0.69546(15) 0.07441(15) 0.0325(6) Uani 1 1 d . . . . . H24 H 0.5144 0.6476 0.0941 0.039 Uiso 1 1 calc R . . . . C21 C 0.60808(16) 0.83463(17) 0.01540(16) 0.0371(6) Uani 1 1 d . . . . . H21 H 0.6315 0.8825 -0.0052 0.045 Uiso 1 1 calc R . . . . C9 C 0.32744(16) 0.87874(16) 0.53551(15) 0.0358(6) Uani 1 1 d . . . . . H9 H 0.3006 0.8700 0.5841 0.043 Uiso 1 1 calc R . . . . C27 C 0.47082(19) 0.52639(15) 0.25779(16) 0.0364(6) Uani 1 1 d . . . . . H27 H 0.4324 0.4845 0.2472 0.044 Uiso 1 1 calc R . . . . C15 C 0.22850(14) 0.86071(15) 0.19051(15) 0.0313(6) Uani 1 1 d . . . . . H15 H 0.1750 0.8844 0.1855 0.038 Uiso 1 1 calc R . . . . C28 C 0.54482(18) 0.50992(16) 0.29517(16) 0.0397(6) Uani 1 1 d . . . . . H28 H 0.5572 0.4563 0.3099 0.048 Uiso 1 1 calc R . . . . C10 C 0.36961(17) 0.95013(16) 0.52229(16) 0.0389(6) Uani 1 1 d . . . . . H10 H 0.3721 0.9901 0.5616 0.047 Uiso 1 1 calc R . . . . C11 C 0.40766(17) 0.96229(16) 0.45166(16) 0.0380(6) Uani 1 1 d . . . . . H11 H 0.4358 1.0115 0.4422 0.046 Uiso 1 1 calc R . . . . C29 C 0.60082(17) 0.56981(16) 0.31141(16) 0.0384(6) Uani 1 1 d . . . . . H29 H 0.6511 0.5578 0.3382 0.046 Uiso 1 1 calc R . . . . C22 C 0.60885(17) 0.76481(17) -0.02826(16) 0.0376(6) Uani 1 1 d . . . . . H22 H 0.6335 0.7647 -0.0785 0.045 Uiso 1 1 calc R . . . . C2 C 0.27380(16) 0.65269(16) 0.33470(16) 0.0356(6) Uani 1 1 d . . . . . H2 H 0.2391 0.6795 0.2983 0.043 Uiso 1 1 calc R . . . . C23 C 0.57398(17) 0.69563(17) 0.00091(15) 0.0380(6) Uani 1 1 d . . . . . H23 H 0.5741 0.6480 -0.0294 0.046 Uiso 1 1 calc R . . . . C5 C 0.37388(17) 0.57361(15) 0.44065(16) 0.0353(6) Uani 1 1 d . . . . . H5 H 0.4082 0.5466 0.4773 0.042 Uiso 1 1 calc R . . . . C3 C 0.25676(17) 0.57379(17) 0.35550(18) 0.0432(7) Uani 1 1 d . . . . . H3 H 0.2106 0.5469 0.3328 0.052 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 P1 0.0207(3) 0.0191(4) 0.0259(4) -0.0009(2) 0.0006(2) -0.0006(2) O1 0.0251(8) 0.0247(9) 0.0351(10) -0.0047(7) -0.0021(7) -0.0028(6) N1 0.0282(9) 0.0230(10) 0.0243(10) 0.0023(8) 0.0010(8) -0.0034(8) C13 0.0245(11) 0.0211(11) 0.0253(12) 0.0007(9) -0.0002(9) -0.0039(9) C17 0.0271(11) 0.0244(12) 0.0255(12) -0.0029(9) 0.0012(9) -0.0032(9) C25 0.0280(11) 0.0205(12) 0.0239(12) -0.0027(9) 0.0021(9) -0.0007(9) C7 0.0240(10) 0.0261(12) 0.0256(12) 0.0014(9) -0.0046(8) 0.0007(9) C19 0.0207(10) 0.0265(12) 0.0305(13) 0.0005(10) 0.0013(8) 0.0012(9) C1 0.0269(11) 0.0273(12) 0.0255(12) 0.0036(10) 0.0041(9) -0.0013(10) C18 0.0236(10) 0.0176(11) 0.0270(11) -0.0015(9) -0.0011(9) -0.0029(9) C26 0.0326(12) 0.0264(13) 0.0312(13) -0.0009(10) 0.0004(10) -0.0013(10) C30 0.0286(12) 0.0299(13) 0.0321(13) -0.0014(10) 0.0019(9) 0.0026(10) C8 0.0308(12) 0.0284(13) 0.0289(13) 0.0030(10) -0.0010(9) 0.0013(10) C6 0.0306(11) 0.0295(13) 0.0264(12) 0.0012(10) 0.0016(9) -0.0001(10) C20 0.0283(11) 0.0291(13) 0.0353(14) 0.0028(11) 0.0038(10) -0.0017(10) C16 0.0265(11) 0.0325(13) 0.0274(12) 0.0012(10) -0.0042(9) -0.0005(10) C14 0.0254(11) 0.0336(14) 0.0295(13) 0.0011(10) 0.0028(9) 0.0014(10) C12 0.0335(11) 0.0273(12) 0.0340(13) 0.0031(10) -0.0041(10) -0.0021(11) C4 0.0471(14) 0.0267(13) 0.0446(16) 0.0087(12) 0.0077(12) -0.0064(12) C24 0.0355(12) 0.0272(13) 0.0349(14) -0.0028(11) 0.0076(10) -0.0003(11) C21 0.0376(13) 0.0370(15) 0.0368(15) 0.0086(12) 0.0057(11) -0.0021(11) C9 0.0389(13) 0.0406(15) 0.0278(13) 0.0003(11) -0.0020(10) 0.0067(12) C27 0.0505(15) 0.0223(12) 0.0365(15) -0.0024(11) 0.0038(12) -0.0023(11) C15 0.0245(11) 0.0353(14) 0.0342(13) 0.0038(11) -0.0005(9) 0.0039(10) C28 0.0546(16) 0.0240(13) 0.0404(15) 0.0038(12) 0.0078(12) 0.0092(12) C10 0.0488(14) 0.0328(14) 0.0352(14) -0.0057(12) -0.0105(12) 0.0047(12) C11 0.0438(13) 0.0280(13) 0.0422(15) 0.0017(11) -0.0080(12) -0.0034(12) C29 0.0420(13) 0.0379(15) 0.0355(14) 0.0026(12) -0.0022(11) 0.0145(12) C22 0.0364(14) 0.0473(16) 0.0292(14) 0.0045(12) 0.0077(10) 0.0071(12) C2 0.0326(12) 0.0371(15) 0.0372(14) 0.0094(12) -0.0047(11) -0.0063(11) C23 0.0429(14) 0.0371(15) 0.0340(14) -0.0058(12) 0.0060(11) 0.0056(12) C5 0.0424(13) 0.0314(14) 0.0320(14) 0.0046(11) 0.0051(11) 0.0041(12) C3 0.0421(14) 0.0372(16) 0.0502(18) 0.0061(13) -0.0040(13) -0.0162(12) _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 P1 O1 1.4885(17) . ? P1 C25 1.793(2) . ? P1 C19 1.813(2) . ? P1 C18 1.816(2) . ? N1 C13 1.438(3) . ? N1 C7 1.426(3) . ? N1 C1 1.432(3) . ? C13 C18 1.404(3) . ? C13 C14 1.393(3) . ? C17 H17 0.9500 . ? C17 C18 1.404(3) . ? C17 C16 1.393(3) . ? C25 C26 1.395(3) . ? C25 C30 1.393(3) . ? C7 C8 1.393(3) . ? C7 C12 1.401(3) . ? C19 C20 1.398(3) . ? C19 C24 1.387(3) . ? C1 C6 1.397(3) . ? C1 C2 1.388(3) . ? C26 H26 0.9500 . ? C26 C27 1.387(4) . ? C30 H30 0.9500 . ? C30 C29 1.391(4) . ? C8 H8 0.9500 . ? C8 C9 1.389(4) . ? C6 H6 0.9500 . ? C6 C5 1.389(3) . ? C20 H20 0.9500 . ? C20 C21 1.383(4) . ? C16 H16 0.9500 . ? C16 C15 1.386(3) . ? C14 H14 0.9500 . ? C14 C15 1.389(3) . ? C12 H12 0.9500 . ? C12 C11 1.383(4) . ? C4 H4 0.9500 . ? C4 C5 1.381(4) . ? C4 C3 1.383(4) . ? C24 H24 0.9500 . ? C24 C23 1.384(3) . ? C21 H21 0.9500 . ? C21 C22 1.385(4) . ? C9 H9 0.9500 . ? C9 C10 1.388(4) . ? C27 H27 0.9500 . ? C27 C28 1.378(4) . ? C15 H15 0.9500 . ? C28 H28 0.9500 . ? C28 C29 1.372(4) . ? C10 H10 0.9500 . ? C10 C11 1.374(4) . ? C11 H11 0.9500 . ? C29 H29 0.9500 . ? C22 H22 0.9500 . ? C22 C23 1.376(4) . ? C2 H2 0.9500 . ? C2 C3 1.390(4) . ? C23 H23 0.9500 . ? C5 H5 0.9500 . ? C3 H3 0.9500 . ? 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 O1 P1 C25 113.90(10) . . ? O1 P1 C19 111.06(10) . . ? O1 P1 C18 111.86(10) . . ? C25 P1 C19 103.46(11) . . ? C25 P1 C18 110.40(10) . . ? C19 P1 C18 105.54(10) . . ? C7 N1 C13 116.07(18) . . ? C7 N1 C1 118.18(19) . . ? C1 N1 C13 116.79(18) . . ? C18 C13 N1 120.2(2) . . ? C14 C13 N1 119.9(2) . . ? C14 C13 C18 119.9(2) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C16 C17 C18 121.2(2) . . ? C26 C25 P1 124.08(19) . . ? C30 C25 P1 116.69(18) . . ? C30 C25 C26 118.9(2) . . ? C8 C7 N1 122.2(2) . . ? C8 C7 C12 119.0(2) . . ? C12 C7 N1 118.8(2) . . ? C20 C19 P1 118.27(18) . . ? C24 C19 P1 122.88(18) . . ? C24 C19 C20 118.9(2) . . ? C6 C1 N1 118.4(2) . . ? C2 C1 N1 122.2(2) . . ? C2 C1 C6 119.3(2) . . ? C13 C18 P1 120.92(17) . . ? C17 C18 P1 119.36(17) . . ? C17 C18 C13 118.5(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 C25 120.5(2) . . ? C27 C26 H26 119.8 . . ? C25 C30 H30 119.9 . . ? C29 C30 C25 120.3(2) . . ? C29 C30 H30 119.9 . . ? C7 C8 H8 119.9 . . ? C9 C8 C7 120.2(2) . . ? C9 C8 H8 119.9 . . ? C1 C6 H6 120.2 . . ? C5 C6 C1 119.6(2) . . ? C5 C6 H6 120.2 . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20 119.8 . . ? C17 C16 H16 120.2 . . ? C15 C16 C17 119.6(2) . . ? C15 C16 H16 120.2 . . ? C13 C14 H14 119.6 . . ? C15 C14 C13 120.9(2) . . ? C15 C14 H14 119.6 . . ? C7 C12 H12 120.1 . . ? C11 C12 C7 119.8(2) . . ? C11 C12 H12 120.1 . . ? C5 C4 H4 120.5 . . ? C5 C4 C3 119.1(2) . . ? C3 C4 H4 120.5 . . ? C19 C24 H24 119.7 . . ? C23 C24 C19 120.6(2) . . ? C23 C24 H24 119.7 . . ? C20 C21 H21 120.0 . . ? C20 C21 C22 119.9(2) . . ? C22 C21 H21 120.0 . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.5(2) . . ? C10 C9 H9 119.7 . . ? C26 C27 H27 120.2 . . ? C28 C27 C26 119.6(3) . . ? C28 C27 H27 120.2 . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C27 C28 H28 119.5 . . ? C29 C28 C27 121.0(2) . . ? C29 C28 H28 119.5 . . ? C9 C10 H10 120.4 . . ? C11 C10 C9 119.2(2) . . ? C11 C10 H10 120.4 . . ? C12 C11 H11 119.4 . . ? C10 C11 C12 121.3(2) . . ? C10 C11 H11 119.4 . . ? C30 C29 H29 120.1 . . ? C28 C29 C30 119.7(2) . . ? C28 C29 H29 120.1 . . ? C21 C22 H22 119.9 . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22 119.9 . . ? C1 C2 H2 119.9 . . ? C1 C2 C3 120.2(2) . . ? C3 C2 H2 119.9 . . ? C24 C23 H23 120.0 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C6 C5 H5 119.4 . . ? C4 C5 C6 121.1(2) . . ? C4 C5 H5 119.4 . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? 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 P1 C25 C26 C27 173.95(19) . . . . ? P1 C25 C30 C29 -175.3(2) . . . . ? P1 C19 C20 C21 178.20(19) . . . . ? P1 C19 C24 C23 -177.9(2) . . . . ? O1 P1 C25 C26 155.5(2) . . . . ? O1 P1 C25 C30 -30.9(2) . . . . ? O1 P1 C19 C20 -29.0(2) . . . . ? O1 P1 C19 C24 150.1(2) . . . . ? O1 P1 C18 C13 -57.1(2) . . . . ? O1 P1 C18 C17 110.09(19) . . . . ? N1 C13 C18 P1 -15.2(3) . . . . ? N1 C13 C18 C17 177.52(19) . . . . ? N1 C13 C14 C15 -177.8(2) . . . . ? N1 C7 C8 C9 179.9(2) . . . . ? N1 C7 C12 C11 179.6(2) . . . . ? N1 C1 C6 C5 -179.9(2) . . . . ? N1 C1 C2 C3 179.2(2) . . . . ? C13 N1 C7 C8 127.8(2) . . . . ? C13 N1 C7 C12 -52.0(3) . . . . ? C13 N1 C1 C6 153.3(2) . . . . ? C13 N1 C1 C2 -25.4(3) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C17 C16 C15 C14 -0.4(4) . . . . ? C25 P1 C19 C20 -151.55(18) . . . . ? C25 P1 C19 C24 27.5(2) . . . . ? C25 P1 C18 C13 70.8(2) . . . . ? C25 P1 C18 C17 -121.97(19) . . . . ? C25 C26 C27 C28 0.0(4) . . . . ? C25 C30 C29 C28 1.7(4) . . . . ? C7 N1 C13 C18 123.4(2) . . . . ? C7 N1 C13 C14 -57.5(3) . . . . ? C7 N1 C1 C6 -60.7(3) . . . . ? C7 N1 C1 C2 120.7(3) . . . . ? C7 C8 C9 C10 0.2(4) . . . . ? C7 C12 C11 C10 0.9(4) . . . . ? C19 P1 C25 C26 -83.8(2) . . . . ? C19 P1 C25 C30 89.8(2) . . . . ? C19 P1 C18 C13 -178.02(18) . . . . ? C19 P1 C18 C17 -10.8(2) . . . . ? C19 C20 C21 C22 -0.1(4) . . . . ? C19 C24 C23 C22 -0.4(4) . . . . ? C1 N1 C13 C18 -89.8(2) . . . . ? C1 N1 C13 C14 89.2(3) . . . . ? C1 N1 C7 C8 -18.5(3) . . . . ? C1 N1 C7 C12 161.7(2) . . . . ? C1 C6 C5 C4 0.9(4) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? C18 P1 C25 C26 28.7(2) . . . . ? C18 P1 C25 C30 -157.68(18) . . . . ? C18 P1 C19 C20 92.44(19) . . . . ? C18 P1 C19 C24 -88.5(2) . . . . ? C18 C13 C14 C15 1.3(4) . . . . ? C18 C17 C16 C15 0.1(4) . . . . ? C26 C25 C30 C29 -1.3(4) . . . . ? C26 C27 C28 C29 0.4(4) . . . . ? C30 C25 C26 C27 0.5(4) . . . . ? C8 C7 C12 C11 -0.2(3) . . . . ? C8 C9 C10 C11 0.5(4) . . . . ? C6 C1 C2 C3 0.6(4) . . . . ? C20 C19 C24 C23 1.2(4) . . . . ? C20 C21 C22 C23 0.9(4) . . . . ? C16 C17 C18 P1 -166.67(18) . . . . ? C16 C17 C18 C13 0.9(3) . . . . ? C14 C13 C18 P1 165.78(18) . . . . ? C14 C13 C18 C17 -1.5(3) . . . . ? C12 C7 C8 C9 -0.3(3) . . . . ? C24 C19 C20 C21 -0.9(4) . . . . ? C21 C22 C23 C24 -0.7(4) . . . . ? C9 C10 C11 C12 -1.0(4) . . . . ? C27 C28 C29 C30 -1.3(4) . . . . ? C2 C1 C6 C5 -1.2(4) . . . . ? C5 C4 C3 C2 -0.8(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? _shelx_res_file ; zhangyouzhi20200707_2_0m.res created by SHELXL-2014/7 TITL zhangyouzhi20200707_2_0m_a.res in Pbca REM Old TITL zhangyouzhi20200707_2_0m in Pbca #61 REM SHELXT solution in Pbca REM R1 0.126, Rweak 0.006, Alpha 0.022, Orientation as input REM Formula found by SHELXT: C30 O N P CELL 1.54184 16.0526 16.6684 17.1822 90 90 90 ZERR 8 0.0006 0.0006 0.0007 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O P UNIT 240 192 8 8 8 L.S. 20 PLAN 20 TEMP -120.15 BOND $H list 4 fmap 2 MORE -1 CONF ACTA REM REM REM WGHT 0.123000 FVAR 0.27358 P1 5 0.496558 0.767447 0.217474 11.00000 0.02070 0.01907 = 0.02592 -0.00095 0.00058 -0.00060 O1 4 0.540728 0.828139 0.265799 11.00000 0.02511 0.02475 = 0.03514 -0.00474 -0.00208 -0.00278 N1 3 0.362050 0.773351 0.346684 11.00000 0.02821 0.02300 = 0.02429 0.00232 0.00098 -0.00343 C13 1 0.335068 0.800931 0.271473 11.00000 0.02449 0.02111 = 0.02533 0.00072 -0.00017 -0.00392 C17 1 0.356973 0.816130 0.133312 11.00000 0.02711 0.02441 = 0.02554 -0.00287 0.00125 -0.00321 AFIX 43 H17 2 0.391008 0.809324 0.088566 11.00000 -1.20000 AFIX 0 C25 1 0.509018 0.666343 0.251235 11.00000 0.02795 0.02046 = 0.02388 -0.00271 0.00214 -0.00067 C7 1 0.363558 0.832037 0.407064 11.00000 0.02405 0.02615 = 0.02565 0.00138 -0.00457 0.00073 C19 1 0.538532 0.764446 0.119571 11.00000 0.02072 0.02654 = 0.03049 0.00049 0.00134 0.00120 C1 1 0.341432 0.692451 0.367032 11.00000 0.02690 0.02733 = 0.02551 0.00359 0.00409 -0.00133 C18 1 0.386811 0.791338 0.206243 11.00000 0.02355 0.01759 = 0.02698 -0.00149 -0.00113 -0.00287 C26 1 0.452823 0.604527 0.235770 11.00000 0.03260 0.02638 = 0.03121 -0.00091 0.00042 -0.00129 AFIX 43 H26 2 0.401865 0.616040 0.209969 11.00000 -1.20000 AFIX 0 C30 1 0.583689 0.648176 0.288577 11.00000 0.02861 0.02990 = 0.03213 -0.00137 0.00188 0.00262 AFIX 43 H30 2 0.623082 0.689462 0.298494 11.00000 -1.20000 AFIX 0 C8 1 0.324182 0.819921 0.478370 11.00000 0.03085 0.02839 = 0.02894 0.00305 -0.00100 0.00133 AFIX 43 H8 2 0.295036 0.771304 0.487915 11.00000 -1.20000 AFIX 0 C6 1 0.392456 0.652171 0.420020 11.00000 0.03058 0.02954 = 0.02642 0.00124 0.00164 -0.00008 AFIX 43 H6 2 0.439571 0.678338 0.441815 11.00000 -1.20000 AFIX 0 C20 1 0.573231 0.834636 0.089002 11.00000 0.02830 0.02910 = 0.03525 0.00278 0.00378 -0.00174 AFIX 43 H20 2 0.572863 0.882554 0.118934 11.00000 -1.20000 AFIX 0 C16 1 0.278364 0.850525 0.125384 11.00000 0.02646 0.03250 = 0.02743 0.00115 -0.00422 -0.00051 AFIX 43 H16 2 0.259015 0.866917 0.075611 11.00000 -1.20000 AFIX 0 C14 1 0.256900 0.836200 0.263069 11.00000 0.02544 0.03358 = 0.02946 0.00113 0.00282 0.00137 AFIX 43 H14 2 0.222581 0.843577 0.307540 11.00000 -1.20000 AFIX 0 C12 1 0.405831 0.904321 0.394074 11.00000 0.03351 0.02729 = 0.03404 0.00307 -0.00407 -0.00209 AFIX 43 H12 2 0.433171 0.913507 0.345855 11.00000 -1.20000 AFIX 0 C4 1 0.306326 0.534113 0.408877 11.00000 0.04715 0.02672 = 0.04462 0.00867 0.00773 -0.00641 AFIX 43 H4 2 0.294088 0.480425 0.423493 11.00000 -1.20000 AFIX 0 C24 1 0.538732 0.695460 0.074406 11.00000 0.03553 0.02716 = 0.03491 -0.00285 0.00763 -0.00030 AFIX 43 H24 2 0.514433 0.647633 0.094125 11.00000 -1.20000 AFIX 0 C21 1 0.608084 0.834627 0.015400 11.00000 0.03755 0.03697 = 0.03679 0.00862 0.00570 -0.00213 AFIX 43 H21 2 0.631479 0.882483 -0.005191 11.00000 -1.20000 AFIX 0 C9 1 0.327445 0.878744 0.535515 11.00000 0.03887 0.04062 = 0.02780 0.00030 -0.00198 0.00673 AFIX 43 H9 2 0.300591 0.870047 0.584057 11.00000 -1.20000 AFIX 0 C27 1 0.470824 0.526390 0.257793 11.00000 0.05050 0.02231 = 0.03653 -0.00243 0.00381 -0.00226 AFIX 43 H27 2 0.432374 0.484468 0.247179 11.00000 -1.20000 AFIX 0 C15 1 0.228502 0.860714 0.190515 11.00000 0.02446 0.03527 = 0.03424 0.00376 -0.00055 0.00395 AFIX 43 H15 2 0.174960 0.884441 0.185523 11.00000 -1.20000 AFIX 0 C28 1 0.544820 0.509924 0.295166 11.00000 0.05462 0.02399 = 0.04037 0.00376 0.00777 0.00920 AFIX 43 H28 2 0.557246 0.456311 0.309902 11.00000 -1.20000 AFIX 0 C10 1 0.369610 0.950128 0.522292 11.00000 0.04881 0.03283 = 0.03521 -0.00568 -0.01048 0.00471 AFIX 43 H10 2 0.372136 0.990112 0.561622 11.00000 -1.20000 AFIX 0 C11 1 0.407656 0.962294 0.451662 11.00000 0.04384 0.02802 = 0.04222 0.00169 -0.00805 -0.00344 AFIX 43 H11 2 0.435772 1.011482 0.442176 11.00000 -1.20000 AFIX 0 C29 1 0.600818 0.569806 0.311411 11.00000 0.04198 0.03785 = 0.03551 0.00255 -0.00216 0.01453 AFIX 43 H29 2 0.651097 0.557809 0.338150 11.00000 -1.20000 AFIX 0 C22 1 0.608854 0.764806 -0.028261 11.00000 0.03636 0.04731 = 0.02919 0.00448 0.00766 0.00706 AFIX 43 H22 2 0.633534 0.764653 -0.078514 11.00000 -1.20000 AFIX 0 C2 1 0.273798 0.652688 0.334701 11.00000 0.03255 0.03707 = 0.03723 0.00939 -0.00474 -0.00630 AFIX 43 H2 2 0.239057 0.679472 0.298254 11.00000 -1.20000 AFIX 0 C23 1 0.573980 0.695632 0.000911 11.00000 0.04290 0.03707 = 0.03395 -0.00580 0.00604 0.00564 AFIX 43 H23 2 0.574107 0.647980 -0.029421 11.00000 -1.20000 AFIX 0 C5 1 0.373879 0.573608 0.440653 11.00000 0.04239 0.03136 = 0.03204 0.00458 0.00506 0.00407 AFIX 43 H5 2 0.408231 0.546580 0.477252 11.00000 -1.20000 AFIX 0 C3 1 0.256756 0.573786 0.355502 11.00000 0.04209 0.03724 = 0.05024 0.00606 -0.00402 -0.01618 AFIX 43 H3 2 0.210594 0.546857 0.332819 11.00000 -1.20000 AFIX 0 HKLF 4 REM zhangyouzhi20200707_2_0m_a.res in Pbca REM R1 = 0.0472 for 3146 Fo > 4sig(Fo) and 0.0776 for all 4171 data REM 298 parameters refined using 0 restraints END WGHT 0.1230 0.0000 REM Highest difference peak 0.421, deepest hole -0.515, 1-sigma level 0.109 Q1 1 0.4355 0.7736 0.2054 11.00000 0.05 0.42 Q2 1 0.5420 0.8038 0.2909 11.00000 0.05 0.40 Q3 1 0.5250 0.7695 0.1682 11.00000 0.05 0.39 Q4 1 0.5166 0.8295 0.0195 11.00000 0.05 0.39 Q5 1 0.1866 0.6379 0.3788 11.00000 0.05 0.38 Q6 1 0.5410 0.6561 0.2618 11.00000 0.05 0.36 Q7 1 0.5428 0.8393 0.2402 11.00000 0.05 0.36 Q8 1 0.4114 0.5753 0.5532 11.00000 0.05 0.34 Q9 1 0.4248 0.8569 0.3732 11.00000 0.05 0.34 Q10 1 0.2681 0.9367 0.2801 11.00000 0.05 0.34 Q11 1 0.4497 0.4723 0.4926 11.00000 0.05 0.34 Q12 1 0.5775 0.7770 0.1123 11.00000 0.05 0.34 Q13 1 0.2244 0.8313 0.2856 11.00000 0.05 0.33 Q14 1 0.4755 0.8581 0.3128 11.00000 0.05 0.33 Q15 1 0.4474 0.7079 0.2685 11.00000 0.05 0.33 Q16 1 0.3835 0.9367 0.3250 11.00000 0.05 0.33 Q17 1 0.3406 0.9657 0.4792 11.00000 0.05 0.33 Q18 1 0.3129 0.3906 0.3966 11.00000 0.05 0.33 Q19 1 0.4256 0.4276 0.1769 11.00000 0.05 0.32 Q20 1 0.5006 0.8221 0.3499 11.00000 0.05 0.32 ; _shelx_res_checksum 4593 _shelx_hkl_file ; -1 0 0 0.03 0.28 1 0 0 0.39 0.31 1 0 0 0.01 0.26 -2 0 0 4124.65 123.29 2 0 0 3521.59 121.66 3 0 0 1.12 1.32 -3 0 0 0.95 1.36 -3 0 0 0.74 0.86 3 0 0 0.68 1.33 4 0 0 679.88 26.36 -4 0 0 649.89 26.27 4 0 0 674.11 25.10 -4 0 0 691.19 25.03 5 0 0 0.01 1.48 5 0 0 3.21 2.05 5 0 0 5.68 7.80 -5 0 0 6.34 8.29 -5 0 0 0.14 1.32 -5 0 0 2.44 2.34 6 0 0 186.96 12.48 -6 0 0 196.59 11.22 -6 0 0 191.63 13.02 6 0 0 193.78 11.51 -7 0 0 11.52 9.88 -7 0 0 0.75 7.11 7 0 0 -1.83 1.41 7 0 0 0.01 10.37 7 0 0 -3.54 9.22 8 0 0 601.55 37.98 -9 0 0 2.10 10.38 9 0 0 12.97 13.27 -9 0 0 7.89 3.98 -9 0 0 5.29 3.34 9 0 0 -1.16 2.39 9 0 0 0.22 1.24 -9 0 0 0.48 1.23 9 0 0 -9.82 10.30 9 0 0 1.08 1.41 -9 0 0 0.88 7.04 -10 0 0 11.48 5.16 10 0 0 20.40 15.40 10 0 0 2.73 4.21 -10 0 0 6.53 8.58 -10 0 0 -2.93 9.92 10 0 0 26.61 13.90 -11 0 0 -0.83 12.18 11 0 0 -3.62 11.23 -11 0 0 0.12 1.23 11 0 0 5.33 6.19 -11 0 0 -0.93 9.34 11 0 0 10.06 14.09 11 0 0 -0.52 1.33 11 0 0 -0.56 1.48 12 0 0 47.80 5.57 -12 0 0 53.86 5.13 12 0 0 55.50 5.57 12 0 0 64.50 13.36 13 0 0 -0.55 1.26 -13 0 0 -8.06 16.48 13 0 0 -11.58 18.29 -13 0 0 0.47 1.35 -13 0 0 -3.17 12.61 -13 0 0 -1.50 5.03 13 0 0 2.58 1.63 13 0 0 16.01 10.89 -14 0 0 8.84 29.75 -14 0 0 4.00 1.82 14 0 0 2.35 2.02 14 0 0 5.20 2.22 -14 0 0 -20.53 13.04 15 0 0 -0.01 1.37 -15 0 0 1.19 1.36 15 0 0 1.94 1.69 16 0 0 1.19 1.33 16 0 0 4.43 1.80 -16 0 0 5.35 2.06 17 0 0 -1.66 0.91 17 0 0 -1.76 0.96 -17 0 0 0.51 1.12 17 0 0 1.64 1.43 -18 0 0 107.84 6.48 18 0 0 111.23 6.36 18 0 0 114.17 6.25 18 0 0 108.83 7.79 -18 0 0 116.66 7.45 -19 0 0 -0.09 1.07 19 0 0 0.28 1.10 -19 0 0 1.42 1.06 0 1 0 -0.02 0.13 0 -1 0 -0.08 0.09 0 1 0 0.23 0.35 1 -1 0 0.40 0.44 -1 1 0 -0.09 0.35 -1 -1 0 0.08 0.35 -1 -1 0 0.28 0.32 -1 -1 0 0.28 0.35 1 1 0 0.21 0.33 1 1 0 0.15 0.49 1 1 0 0.38 0.32 1 1 0 0.35 0.31 2 -1 0 2165.97 66.74 -2 -1 0 2012.46 66.88 -2 1 0 2028.59 66.54 2 1 0 2131.28 67.01 -2 1 0 2088.36 67.66 2 1 0 1999.54 66.44 2 -1 0 2086.02 67.64 -2 -1 0 2153.62 66.54 2 1 0 2140.88 66.27 -3 -1 0 0.49 1.33 3 1 0 -0.12 1.19 -3 -1 0 -0.31 1.04 -3 1 0 -0.27 1.48 3 1 0 0.48 0.96 3 -1 0 -0.71 0.92 3 -1 0 -0.94 1.34 3 1 0 -0.04 1.49 -3 1 0 1.15 1.47 -4 -1 0 7556.55 243.15 4 1 0 7618.58 241.85 4 1 0 7759.11 243.05 4 1 0 8066.91 241.82 4 -1 0 7621.09 243.63 -4 1 0 7568.26 243.79 -5 1 0 -1.55 1.70 5 1 0 0.15 1.24 -5 -1 0 -4.60 7.60 -5 -1 0 -1.93 1.50 -5 -1 0 1.51 1.64 5 -1 0 0.25 1.46 -5 1 0 -0.47 1.26 5 1 0 1.09 1.40 5 1 0 -7.41 6.09 5 -1 0 -5.90 7.78 5 1 0 -1.75 1.20 -5 1 0 -3.22 7.10 5 -1 0 -2.13 1.09 -6 -1 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-19 -7.83 13.93 7 3 -19 12.19 2.25 7 -3 19 14.60 2.01 -7 3 19 8.29 1.99 -7 -3 -19 12.54 2.10 7 3 19 12.70 2.15 7 -3 -19 14.08 2.31 -7 3 -19 14.45 2.32 0 -4 -19 4.28 1.54 0 -4 -19 -13.68 29.19 0 4 -19 5.99 1.72 0 4 -19 6.40 1.98 0 -4 -19 5.66 11.17 0 4 19 6.89 1.83 1 4 -19 3.58 1.52 -1 -4 -19 15.13 10.29 -1 -4 -19 1.88 1.14 1 4 19 3.59 1.53 -1 4 -19 3.51 1.51 1 -4 -19 4.30 1.59 -1 4 -19 3.40 1.75 1 -4 -19 8.51 9.97 1 -4 -19 1.40 27.19 2 4 -19 16.81 2.66 2 4 -19 12.17 2.33 -2 -4 -19 18.12 2.51 -2 -4 -19 0.86 9.36 -2 -4 -19 84.24 35.81 -2 4 -19 10.39 2.19 2 -4 -19 17.41 11.11 2 -4 -19 15.32 2.41 -2 4 -19 13.60 2.83 2 4 19 12.33 2.17 2 -4 -19 10.01 33.40 3 4 -19 9.60 2.15 -3 -4 -19 -2.99 10.76 3 4 -19 15.10 2.78 3 -4 -19 8.67 11.44 3 4 19 11.80 2.13 -3 4 -19 10.74 2.52 3 -4 -19 14.24 2.57 -3 4 -19 9.41 2.02 3 -4 -19 -19.84 30.27 4 4 -19 1.54 1.72 -4 -4 -19 -9.87 10.23 -4 -4 -19 -20.59 40.92 4 4 -19 3.05 1.40 4 -4 19 4.07 1.60 4 -4 -19 -2.88 11.57 -4 4 -19 2.14 1.71 4 4 19 4.20 1.50 -4 4 -19 3.74 1.52 5 -4 19 13.42 1.96 5 4 -19 10.20 2.44 5 4 -19 15.89 2.40 -5 -4 -19 17.71 2.52 -5 -4 -19 16.52 12.40 5 4 19 18.87 2.56 -5 4 -19 11.78 2.17 -5 4 -19 15.89 2.94 5 -4 -19 19.59 2.81 6 4 -19 41.96 3.34 6 4 -19 37.48 3.74 -6 -4 -19 41.78 3.47 6 -4 19 43.30 3.11 -6 4 19 30.06 3.04 6 -4 -19 44.91 3.79 6 4 19 44.54 3.51 -6 4 -19 31.75 3.44 -6 4 -19 41.90 3.35 0 5 -19 -1.21 0.84 0 -5 -19 2.72 1.34 0 5 19 0.31 1.45 0 -5 19 -1.63 1.36 0 -5 -19 -10.18 8.98 0 5 -19 1.78 1.31 0 -5 -19 -37.34 25.26 -1 -5 -19 2.22 1.52 1 5 -19 1.67 1.16 1 5 -19 3.46 1.42 -1 -5 -19 -7.18 7.83 -1 -5 -19 -8.49 28.72 1 -5 19 0.96 1.56 1 -5 -19 -0.10 1.18 1 5 19 1.97 1.35 -1 -5 19 2.47 1.52 1 -5 -19 3.98 10.04 -1 5 -19 2.87 1.61 1 -5 -19 -2.89 27.48 -1 5 -19 1.12 1.18 2 5 -19 2.85 1.58 -2 -5 -19 -6.44 9.65 -2 -5 -19 3.79 1.50 -2 -5 -19 35.17 30.17 2 5 -19 2.85 1.14 -2 -5 19 1.58 1.63 2 -5 -19 -2.31 10.19 -2 5 -19 -0.34 1.40 2 -5 -19 0.94 1.40 2 5 19 -1.08 1.09 2 -5 -19 -22.83 29.86 -2 5 -19 1.97 1.27 -3 -5 -19 -3.42 9.51 -3 -5 -19 13.38 31.37 3 -5 -19 -6.55 10.93 3 -5 -19 -32.56 28.30 -4 -5 -19 13.13 10.14 4 5 -19 2.26 1.31 4 5 -19 1.69 1.38 -4 -5 -19 1.87 1.35 -4 5 -19 5.20 1.45 -4 5 -19 1.18 1.41 4 -5 -19 10.53 11.54 4 5 19 2.97 1.23 4 -5 -19 -0.87 1.05 5 -5 19 11.15 1.94 -5 -5 -19 -1.25 11.51 5 5 -19 13.01 2.04 -5 -5 -19 14.93 2.40 5 5 19 12.60 2.09 -5 5 -19 11.24 2.06 5 -5 -19 5.70 11.28 -5 5 -19 15.15 2.20 5 -5 -19 12.47 2.24 6 -5 -19 5.82 12.38 0 6 -19 16.11 2.31 0 6 19 18.75 2.38 0 -6 -19 1.80 28.19 0 -6 -19 15.68 2.88 0 6 -19 12.95 2.53 0 -6 -19 0.67 9.58 0 -6 19 15.66 2.01 1 6 -19 4.24 1.44 -1 -6 -19 3.12 1.46 1 6 -19 5.56 2.02 1 -6 19 6.93 1.40 -1 -6 -19 15.20 10.04 -1 -6 -19 -3.97 28.48 1 -6 -19 45.06 28.17 -1 6 -19 3.77 1.40 -1 6 -19 6.02 1.77 1 -6 -19 11.54 9.34 1 6 19 6.67 1.53 1 -6 -19 6.96 1.92 -1 -6 19 4.70 1.37 -2 -6 -19 -38.96 30.10 2 6 -19 4.03 1.64 -2 -6 -19 -11.74 8.57 2 -6 -19 -40.65 27.03 -2 6 -19 5.60 1.66 3 6 -19 0.15 1.09 -3 -6 -19 7.15 10.33 -3 -6 -19 2.94 1.42 3 6 -19 2.37 1.32 -3 6 -19 0.44 1.08 3 -6 -19 3.02 1.39 3 -6 -19 -6.80 9.92 3 6 19 0.94 1.02 -3 -6 19 3.10 1.41 -3 6 -19 2.18 1.22 4 6 -19 59.74 4.60 4 6 -19 60.40 3.73 -4 -6 -19 69.99 4.33 4 6 19 64.70 4.13 -4 6 -19 64.92 3.88 4 -6 -19 64.93 4.37 -4 6 -19 60.68 4.73 -5 -6 -19 -2.21 9.71 5 6 -19 1.32 1.32 5 6 -19 -0.12 1.09 -5 -6 -19 0.29 1.27 5 -6 -19 -1.61 1.10 5 -6 -19 7.63 11.09 -5 6 -19 -0.88 1.01 0 7 19 1.28 1.19 0 7 -19 0.78 1.33 0 -7 19 1.89 1.16 0 -7 -19 0.38 1.70 0 7 -19 -0.90 0.75 0 -7 -19 -0.64 8.57 1 7 -19 -0.51 1.42 -1 -7 -19 4.20 9.54 1 -7 19 1.15 1.26 -1 -7 -19 5.13 1.61 1 7 -19 0.83 1.12 1 -7 -19 -0.22 1.57 -1 7 -19 0.62 0.97 1 -7 -19 2.10 9.45 -1 -7 19 4.83 1.47 1 7 19 1.73 1.21 -2 -7 -19 -3.10 8.65 2 -7 19 7.38 1.54 -2 -7 -19 12.77 2.07 2 7 -19 5.77 1.65 2 -7 -19 -6.81 9.60 2 7 19 5.99 1.48 -2 -7 19 7.98 1.55 -2 7 -19 5.78 1.57 2 -7 -19 6.57 1.98 -3 -7 -19 14.54 2.36 3 -7 19 12.05 1.76 3 7 19 12.68 1.91 -3 -7 19 16.24 2.17 -3 7 -19 15.21 2.12 3 -7 -19 1.16 11.62 3 -7 -19 15.63 2.30 0 0 -20 30.18 3.32 1 0 -20 0.70 1.18 -1 0 -20 1.14 1.35 2 0 -20 0.95 1.01 -2 0 -20 0.59 0.91 3 0 -20 1.23 1.16 -3 0 -20 1.23 1.30 4 0 -20 14.06 2.47 -4 0 -20 14.37 2.30 4 0 20 17.10 1.97 0 -1 -20 4.59 16.94 0 -1 -20 1.80 1.27 -1 -1 -20 59.95 4.76 1 1 -20 61.23 4.68 -1 1 -20 62.61 4.79 1 -1 -20 58.72 4.63 2 1 -20 -0.47 1.01 -2 -1 -20 2.25 17.19 -2 -1 -20 0.64 0.78 2 -1 -20 0.00 1.09 -2 1 -20 -0.89 0.90 2 -1 -20 -14.83 18.42 -3 -1 -20 34.27 3.45 3 1 -20 33.22 3.45 3 -1 -20 37.94 3.63 -3 1 -20 31.04 3.27 3 1 20 35.39 2.89 4 1 -20 30.98 3.30 -4 -1 -20 30.98 3.22 4 -1 -20 37.16 3.48 4 1 20 32.48 2.70 -4 1 -20 33.83 3.28 0 -2 -20 124.08 6.94 0 2 -20 117.94 6.81 -1 -2 -20 4.24 12.81 -1 -2 -20 0.50 1.22 1 2 -20 0.18 1.08 -1 2 -20 -0.16 0.97 1 -2 -20 -9.97 12.95 1 -2 -20 -1.43 0.82 2 2 -20 20.12 2.76 -2 -2 -20 17.19 2.66 -2 -2 -20 16.15 12.71 2 -2 -20 23.86 15.25 -2 2 -20 19.00 2.71 2 -2 -20 22.25 2.86 -3 -2 -20 1.68 1.16 -3 -2 -20 -3.59 14.46 3 2 -20 1.87 1.22 3 -2 -20 1.02 1.08 3 2 20 1.19 1.21 -3 2 -20 1.44 1.09 -4 -2 -20 34.45 3.29 4 2 -20 38.83 3.46 4 -2 -20 37.31 3.49 -4 2 -20 35.60 3.24 4 2 20 40.34 2.92 0 3 -20 4.14 1.87 0 -3 -20 -9.83 12.52 0 -3 -20 -0.15 0.98 0 3 -20 -0.36 1.09 -1 -3 -20 96.04 5.70 1 3 -20 87.36 5.44 1 3 -20 79.26 5.52 1 -3 -20 91.56 5.55 -1 3 -20 68.30 5.35 -1 3 -20 90.55 5.51 -2 -3 -20 -0.44 10.59 -2 -3 -20 3.66 1.46 2 3 -20 6.36 2.32 2 -3 -20 -7.19 12.24 -2 3 -20 3.12 1.51 2 -3 -20 3.54 1.55 -2 3 -20 -3.28 1.88 3 3 -20 17.52 3.28 3 3 -20 30.56 3.07 -3 -3 -20 31.00 3.07 3 3 20 29.04 2.55 3 -3 -20 20.75 14.43 3 -3 -20 27.38 3.05 -3 3 -20 25.98 2.93 4 3 -20 1.50 1.12 -4 -3 -20 -15.67 12.94 -4 -3 -20 2.32 1.12 -4 3 -20 -0.58 0.93 4 -3 -20 -2.00 19.66 4 3 20 1.64 1.14 4 -3 -20 0.96 1.13 0 -4 -20 3.26 1.45 0 4 -20 2.85 1.78 0 -4 -20 6.47 11.80 0 4 -20 1.97 1.21 -1 -4 -20 11.34 2.06 1 4 -20 9.84 1.87 1 4 -20 8.81 2.44 -1 -4 -20 1.56 10.51 1 -4 -20 10.83 2.14 -1 4 -20 10.02 1.79 -1 4 -20 15.04 2.71 1 -4 -20 5.95 11.03 -2 -4 -20 31.35 3.00 2 4 -20 31.55 2.96 -2 -4 -20 10.51 11.26 2 4 -20 24.49 3.05 2 -4 -20 29.82 3.12 -2 4 -20 36.18 2.99 -2 4 -20 20.05 3.07 -3 -4 -20 -4.56 10.64 3 4 -20 -0.53 0.90 3 4 -20 3.44 1.88 3 -4 -20 6.98 13.60 -3 4 -20 1.57 1.49 -3 4 -20 -0.19 0.94 3 4 20 -0.23 1.12 3 -4 -20 3.78 1.29 0 -5 -20 22.52 11.84 0 -5 -20 0.71 1.11 0 5 -20 3.69 1.10 -1 -5 -20 55.60 3.85 1 5 -20 38.80 3.55 1 5 -20 49.27 3.41 1 -5 -20 50.13 3.71 -1 5 -20 46.92 3.71 -1 5 -20 50.27 3.37 _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 0.7531 _exptl_absorpt_correction_T_min 0.7015 _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 1.54184 16.054 16.658 17.176 90.034 90.019 90.022 ) _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 70748 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'