data_exp_3127 _audit_creation_date 2014-03-25 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _publ_contact_author_address ? _publ_contact_author_email ? _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. (2008). Acta Cryst. A64, 112-122 ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H24 O5' _chemical_formula_sum 'C21 H24 O5' _chemical_formula_weight 356.40 _chemical_melting_point ? _chemical_oxdiff_formula C21H24O5 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' _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 9.9111(4) _cell_length_b 14.8737(8) _cell_length_c 12.4145(5) _cell_angle_alpha 90 _cell_angle_beta 90.895(3) _cell_angle_gamma 90 _cell_volume 1829.84(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3438 _cell_measurement_temperature 180.01(10) _cell_measurement_theta_max 29.0020 _cell_measurement_theta_min 3.8770 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour '' _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description '' _exptl_crystal_F_000 760 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_unetI/netI 0.0356 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 8136 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.022 _diffrn_reflns_theta_min 2.948 _diffrn_ambient_temperature 180.01(10) _diffrn_detector_area_resol_mean 10.3914 _diffrn_measured_fraction_theta_full 0.9973 _diffrn_measured_fraction_theta_max 0.8370 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -77.00 42.00 1.0000 2.6500 omega____ theta____ kappa____ phi______ frames - 10.8579 0.0000 -90.0000 119 #__ type_ start__ end____ width___ exp.time_ 2 omega -94.00 -62.00 1.0000 2.6500 omega____ theta____ kappa____ phi______ frames - -11.7173 178.0000 150.0000 32 #__ type_ start__ end____ width___ exp.time_ 3 omega -20.00 23.00 1.0000 2.6500 omega____ theta____ kappa____ phi______ frames - -11.7173 -99.0000 -60.0000 43 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0690027000 _diffrn_orient_matrix_UB_12 -0.0087109000 _diffrn_orient_matrix_UB_13 0.0118221000 _diffrn_orient_matrix_UB_21 0.0140814000 _diffrn_orient_matrix_UB_22 0.0467032000 _diffrn_orient_matrix_UB_23 -0.0030882000 _diffrn_orient_matrix_UB_31 -0.0127115000 _diffrn_orient_matrix_UB_32 0.0044009000 _diffrn_orient_matrix_UB_33 0.0558011000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2813 _reflns_number_total 3593 _reflns_odcompleteness_completeness 99.73 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790' _refine_diff_density_max 0.251 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.043 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 3593 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0431 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.5481P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.1077 _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: C4(H4) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B) 2.c Aromatic/amide H refined with riding coordinates: C7(H7), C17(H17) 2.d Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _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 C1 C 0.25127(15) 0.71833(11) 0.69017(11) 0.0243(4) Uani 1 1 d . . . . . O1 O -0.08600(11) 0.99002(8) 0.68348(8) 0.0305(3) Uani 1 1 d . . . . . C2 C 0.14326(16) 0.71300(12) 0.77598(12) 0.0277(4) Uani 1 1 d . . . . . H2A H 0.1758 0.6735 0.8351 0.033 Uiso 1 1 calc R U . . . H2B H 0.0611 0.6853 0.7441 0.033 Uiso 1 1 calc R U . . . O2 O -0.05877(10) 0.77474(8) 0.57674(8) 0.0245(3) Uani 1 1 d . . . . . C3 C 0.10673(16) 0.80462(12) 0.82265(11) 0.0268(4) Uani 1 1 d . . . . . H3A H 0.0811 0.7974 0.8989 0.032 Uiso 1 1 calc R U . . . H3B H 0.1864 0.8447 0.8204 0.032 Uiso 1 1 calc R U . . . O3 O 0.20646(11) 0.69582(8) 0.58095(8) 0.0291(3) Uani 1 1 d . . . . . C4 C -0.00961(15) 0.84742(11) 0.75971(11) 0.0230(3) Uani 1 1 d . . . . . H4 H -0.0933 0.8132 0.7773 0.028 Uiso 1 1 calc R U . . . O4 O 0.60950(13) 0.51873(10) 0.82043(11) 0.0497(4) Uani 1 1 d . . . . . C5 C -0.03577(16) 0.94851(12) 0.78796(11) 0.0283(4) Uani 1 1 d . . . . . O5 O -0.19929(11) 0.76461(9) 0.43375(9) 0.0377(3) Uani 1 1 d . . . . . C6 C -0.08978(15) 0.92448(12) 0.61028(11) 0.0247(4) Uani 1 1 d . . . . . C7 C -0.16888(16) 0.90668(13) 0.52545(12) 0.0289(4) Uani 1 1 d . . . . . H7 H -0.2271 0.9473 0.4882 0.035 Uiso 1 1 calc R U . . . C8 C -0.14753(15) 0.81198(13) 0.50155(11) 0.0273(4) Uani 1 1 d . . . . . C9 C 0.00226(15) 0.84825(11) 0.63667(11) 0.0219(3) Uani 1 1 d . . . . . C10 C 0.14448(15) 0.86188(11) 0.59338(11) 0.0235(4) Uani 1 1 d . . . . . H10A H 0.1350 0.8768 0.5159 0.028 Uiso 1 1 calc R U . . . H10B H 0.1829 0.9156 0.6297 0.028 Uiso 1 1 calc R U . . . C11 C 0.24852(15) 0.78715(12) 0.60332(11) 0.0246(4) Uani 1 1 d . . . . . C12 C 0.37728(16) 0.81333(14) 0.54687(12) 0.0323(4) Uani 1 1 d . . . . . H12A H 0.4088 0.8718 0.5758 0.039 Uiso 1 1 calc R U . . . H12B H 0.3568 0.8216 0.4692 0.039 Uiso 1 1 calc R U . . . C13 C 0.49094(17) 0.74495(14) 0.55926(13) 0.0361(4) Uani 1 1 d . . . . . H13A H 0.5751 0.7704 0.5300 0.043 Uiso 1 1 calc R U . . . H13B H 0.4680 0.6902 0.5176 0.043 Uiso 1 1 calc R U . . . C14 C 0.51347(16) 0.72022(13) 0.67766(13) 0.0318(4) Uani 1 1 d . . . . . C15 C 0.61953(18) 0.64653(15) 0.69769(16) 0.0437(5) Uani 1 1 d . . . . . H15A H 0.6450 0.6177 0.6291 0.052 Uiso 1 1 calc R U . . . H15B H 0.7016 0.6720 0.7324 0.052 Uiso 1 1 calc R U . . . C16 C 0.55305(18) 0.57936(13) 0.77130(14) 0.0364(4) Uani 1 1 d . . . . . C17 C 0.40839(17) 0.60045(12) 0.77156(12) 0.0304(4) Uani 1 1 d . . . . . H17 H 0.3413 0.5652 0.8055 0.036 Uiso 1 1 calc R U . . . C18 C 0.38493(15) 0.67642(12) 0.71705(11) 0.0259(4) Uani 1 1 d . . . . . C19 C 0.08589(19) 1.00297(14) 0.82367(14) 0.0398(5) Uani 1 1 d . . . . . H19A H 0.0596 1.0660 0.8327 0.060 Uiso 1 1 calc R U . . . H19B H 0.1560 0.9987 0.7691 0.060 Uiso 1 1 calc R U . . . H19C H 0.1209 0.9795 0.8924 0.060 Uiso 1 1 calc R U . . . C20 C -0.14971(19) 0.95800(13) 0.86696(13) 0.0379(4) Uani 1 1 d . . . . . H20A H -0.2326 0.9328 0.8353 0.057 Uiso 1 1 calc R U . . . H20B H -0.1636 1.0218 0.8833 0.057 Uiso 1 1 calc R U . . . H20C H -0.1266 0.9256 0.9335 0.057 Uiso 1 1 calc R U . . . C21 C 0.54573(19) 0.80345(14) 0.74599(14) 0.0409(5) Uani 1 1 d . . . . . H21A H 0.5733 0.7847 0.8187 0.061 Uiso 1 1 calc R U . . . H21B H 0.4654 0.8416 0.7500 0.061 Uiso 1 1 calc R U . . . H21C H 0.6192 0.8373 0.7130 0.061 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0240(8) 0.0266(9) 0.0222(7) 0.0006(6) -0.0037(6) 0.0000(7) O1 0.0376(7) 0.0253(7) 0.0284(6) -0.0019(5) -0.0068(5) 0.0043(5) C2 0.0246(8) 0.0309(10) 0.0277(8) 0.0093(7) -0.0003(6) 0.0030(7) O2 0.0238(6) 0.0260(7) 0.0237(5) -0.0044(4) -0.0045(4) -0.0002(5) C3 0.0273(8) 0.0342(10) 0.0189(7) 0.0020(6) -0.0021(6) -0.0005(7) O3 0.0295(6) 0.0319(7) 0.0256(6) -0.0018(5) -0.0068(4) 0.0005(5) C4 0.0245(8) 0.0245(9) 0.0198(7) 0.0001(6) -0.0017(6) -0.0023(7) O4 0.0402(8) 0.0432(9) 0.0654(9) 0.0084(7) -0.0128(6) 0.0138(7) C5 0.0340(9) 0.0277(10) 0.0229(8) -0.0026(7) -0.0069(6) 0.0022(8) O5 0.0274(6) 0.0522(9) 0.0332(6) -0.0168(6) -0.0076(5) -0.0009(6) C6 0.0248(8) 0.0250(9) 0.0242(7) 0.0020(6) 0.0004(6) -0.0003(7) C7 0.0266(8) 0.0346(11) 0.0254(8) 0.0028(7) -0.0048(6) 0.0046(8) C8 0.0196(8) 0.0393(11) 0.0229(8) -0.0036(7) -0.0020(6) -0.0003(7) C9 0.0227(8) 0.0232(9) 0.0196(7) -0.0011(6) -0.0046(6) -0.0029(7) C10 0.0243(8) 0.0269(10) 0.0193(7) 0.0039(6) -0.0025(6) -0.0012(7) C11 0.0225(8) 0.0308(10) 0.0203(7) 0.0007(6) -0.0037(6) -0.0021(7) C12 0.0247(8) 0.0475(12) 0.0246(8) 0.0095(8) 0.0003(6) 0.0005(8) C13 0.0256(9) 0.0506(13) 0.0323(9) 0.0048(8) 0.0048(7) 0.0029(8) C14 0.0203(8) 0.0407(11) 0.0343(9) 0.0051(8) -0.0030(6) 0.0041(8) C15 0.0261(9) 0.0519(14) 0.0529(11) 0.0083(9) -0.0031(8) 0.0082(9) C16 0.0345(10) 0.0366(11) 0.0378(9) -0.0041(8) -0.0096(7) 0.0089(9) C17 0.0298(9) 0.0320(10) 0.0292(8) -0.0008(7) -0.0056(6) 0.0028(8) C18 0.0245(8) 0.0320(10) 0.0212(7) -0.0030(7) -0.0034(6) 0.0027(7) C19 0.0458(11) 0.0322(11) 0.0411(10) -0.0091(8) -0.0121(8) -0.0045(9) C20 0.0484(11) 0.0351(11) 0.0305(9) -0.0068(8) 0.0030(7) 0.0087(9) C21 0.0359(10) 0.0463(13) 0.0400(10) 0.0063(8) -0.0120(7) -0.0069(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.524(2) . ? C1 O3 1.4592(17) . ? C1 C11 1.487(2) . ? C1 C18 1.497(2) . ? O1 C5 1.5137(18) . ? O1 C6 1.3328(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.527(2) . ? O2 C8 1.3879(18) . ? O2 C9 1.4494(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.522(2) . ? O3 C11 1.447(2) . ? C4 H4 1.0000 . ? C4 C5 1.566(2) . ? C4 C9 1.5339(19) . ? O4 C16 1.220(2) . ? C5 C19 1.513(2) . ? C5 C20 1.514(2) . ? O5 C8 1.2060(19) . ? C6 C7 1.330(2) . ? C6 C9 1.489(2) . ? C7 H7 0.9500 . ? C7 C8 1.456(3) . ? C9 C10 1.530(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.520(2) . ? C11 C12 1.516(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.524(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.528(2) . ? C14 C15 1.536(3) . ? C14 C18 1.519(2) . ? C14 C21 1.531(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.512(3) . ? C16 C17 1.468(2) . ? C17 H17 0.9500 . ? C17 C18 1.336(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? 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 O3 C1 C2 115.51(12) . . ? O3 C1 C11 58.81(9) . . ? O3 C1 C18 111.53(12) . . ? C11 C1 C2 122.53(14) . . ? C11 C1 C18 117.04(13) . . ? C18 C1 C2 116.83(12) . . ? C6 O1 C5 106.93(12) . . ? C1 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C1 C2 C3 113.08(14) . . ? H2A C2 H2B 107.8 . . ? C3 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C8 O2 C9 107.41(12) . . ? C2 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C4 C3 C2 111.15(13) . . ? C4 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C11 O3 C1 61.54(10) . . ? C3 C4 H4 107.4 . . ? C3 C4 C5 114.40(13) . . ? C3 C4 C9 116.44(13) . . ? C5 C4 H4 107.4 . . ? C9 C4 H4 107.4 . . ? C9 C4 C5 103.34(12) . . ? O1 C5 C4 104.66(11) . . ? O1 C5 C20 106.17(13) . . ? C19 C5 O1 106.41(14) . . ? C19 C5 C4 116.46(14) . . ? C19 C5 C20 111.06(14) . . ? C20 C5 C4 111.24(14) . . ? O1 C6 C9 113.36(12) . . ? C7 C6 O1 134.08(16) . . ? C7 C6 C9 111.98(15) . . ? C6 C7 H7 127.2 . . ? C6 C7 C8 105.56(15) . . ? C8 C7 H7 127.2 . . ? O2 C8 C7 109.98(13) . . ? O5 C8 O2 119.64(17) . . ? O5 C8 C7 130.23(15) . . ? O2 C9 C4 117.86(13) . . ? O2 C9 C6 102.25(11) . . ? O2 C9 C10 107.40(12) . . ? C6 C9 C4 99.73(12) . . ? C6 C9 C10 112.74(13) . . ? C10 C9 C4 115.87(12) . . ? C9 C10 H10A 107.3 . . ? C9 C10 H10B 107.3 . . ? H10A C10 H10B 106.9 . . ? C11 C10 C9 120.15(14) . . ? C11 C10 H10A 107.3 . . ? C11 C10 H10B 107.3 . . ? C1 C11 C10 124.56(13) . . ? C1 C11 C12 120.40(13) . . ? O3 C11 C1 59.65(10) . . ? O3 C11 C10 118.56(12) . . ? O3 C11 C12 113.23(13) . . ? C12 C11 C10 110.45(14) . . ? C11 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 . . ? C11 C12 C13 114.09(15) . . ? H12A C12 H12B 107.6 . . ? C13 C12 H12A 108.7 . . ? C13 C12 H12B 108.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 C14 110.76(13) . . ? H13A C13 H13B 108.1 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C13 C14 C15 114.63(15) . . ? C13 C14 C21 111.36(16) . . ? C18 C14 C13 107.59(13) . . ? C18 C14 C15 102.54(15) . . ? C18 C14 C21 109.72(14) . . ? C21 C14 C15 110.52(14) . . ? C14 C15 H15A 110.7 . . ? C14 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? C16 C15 C14 105.41(14) . . ? C16 C15 H15A 110.7 . . ? C16 C15 H15B 110.7 . . ? O4 C16 C15 126.16(17) . . ? O4 C16 C17 126.68(18) . . ? C17 C16 C15 107.16(15) . . ? C16 C17 H17 125.0 . . ? C18 C17 C16 110.00(16) . . ? C18 C17 H17 125.0 . . ? C1 C18 C14 119.57(14) . . ? C17 C18 C1 127.71(15) . . ? C17 C18 C14 112.70(14) . . ? C5 C19 H19A 109.5 . . ? C5 C19 H19B 109.5 . . ? C5 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C5 C20 H20A 109.5 . . ? C5 C20 H20B 109.5 . . ? C5 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _shelx_estimated_absorpt_T_max 0.991 _shelx_estimated_absorpt_T_min 0.982 _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. ; _shelxl_version_number 2013-3